instrumentation and inverse problem solving for impedance ...experimental results in the thesis...

152
Instrumentation and Inverse Problem Solving for Impedance Imaging Xiaobei Li A dissertation submitted in partial fulfillment of the requirements for the degree of Doctor of Philosophy University of Washington 2006 Program Authorized to Offer Degree: Department of Electrical Engineering

Upload: others

Post on 14-Aug-2020

2 views

Category:

Documents


0 download

TRANSCRIPT

Page 1: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

Instrumentation and Inverse Problem Solving for Impedance Imaging

Xiaobei Li

A dissertation submitted in partial fulfillment of the requirements for the degree of

Doctor of Philosophy

University of Washington 2006

Program Authorized to Offer Degree: Department of Electrical Engineering

Page 2: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

University of Washington Graduate School

This is to certify that I have examined this copy of a doctoral dissertation by

Xiaobei Li

and have found it complete and satisfactory in all respects, and that any and all revisions required by the final

examining committee have been made.

Chair of the Supervisory Committee:

_________________________________________

Alexander V. Mamishev

Reading Committee:

_________________________________________

Alexander V. Mamishev

_________________________________________

Brian Otis

_________________________________________

Gunther Uhlmann

_________________________________________

Lloyd Burgess

Date: _________________

Page 3: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

In presenting this dissertation in partial fulfillment of the requirements for the doctoral degree at the University of Washington, I agree that the Library shall make its copies freely available for inspection. I further agree that extensive copying of the dissertation is allowable only for scholarly purposes, consistent with “fair use” as prescribed in the U.S. Copyright Law. Requests for copying or reproduction of this dissertation may be referred to ProQuest Information and Learning, 300 North Zeeb Road, Ann Arbor, MI 48106-1346, 1-800-521-0600, to whom the author has granted “the right to reproduce and sell (a) copies of the manuscript in microform and/or (b) printed copies of the manuscript made from microform.”

Signature_______________________________

Date___________________________________

Page 4: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

University of Washington

Abstract

Instrumentation and Inverse Problem Solving for Impedance Imaging

Xiaobei Li

Chair of the Supervisory Committee:

Associate Professor Alexander Mamishev Department of Electrical Engineering

Fringing electric field (FEF) sensors are widely used for non-invasive measurement

of material properties, such as moisture content, porosity, viscosity, temperature,

hardness, and degree of cure. Impedance spectroscopy using FEF sensors is a viable

process analytical technique for detecting the presence of a material or estimating the

concentration of a material within the test environment. An array of FEF sensors can be

used for electrical impedance tomography (EIT), an effective imaging method for

industrial process control as well as medical monitoring and diagnosis.

This thesis studies the instrumentation and data analysis of fringing electric field

sensing systems, and their application as non-invasive analytical tools in the food and

pharmaceutical industries. A specific emphasis is placed upon multi-channel FEE

sensors. The research work presented in this thesis has several scientific and engineering

challenges. Fringing electric field dielectrometry is a soft-field technique. Sensor

measurements are typically non-linear functions of the distribution of the dielectric or

physical properties of the material under test. The field distribution of FEF sensors is

inherently non-uniform and no generic analytical models exist for FEF sensors. Modeling

of FEF sensors typically relies on finite element simulations, which can be complex and

time-consuming. Interface circuit for FEF sensors typically requires high measurement

Page 5: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

sensitivity, good noise immunity, and broad dynamic range. In imaging applications,

image reconstruction involves solving an ill-conditioned and under-determined non-linear

inverse problem.

The thesis provides guidelines for designing FEF sensor systems, specifically multi-

channel FEF sensor systems for industrial process imaging applications. The majority of

the impedance imaging research focuses on circular electrodes enclosing a cylinder.

Work on the instrumentation of imaging systems based on planar electrodes has been

scarce. The thesis fills in the gap by detailing the various aspects of designing a FEF

sensing system for industrial applications. General rules and principles for designing

multi-channel fringing electric field (FEF) sensors are outlined in the thesis. A non-

dimensionalized parametric modeling method is developed to model FEF sensors, thus

avoiding reconstructing a finite element simulation every time the dimension changes. A

direct non-linear image reconstruction algorithm, the layer stripping algorithm, is used in

the thesis to solve the inverse problem of one-dimensional profiling.

Experimental results in the thesis demonstrate the viability of FEF dielectrometry as

a process analytical sensing technique. FEF dielectrometry complements other traditional

process analytical techniques like NMR and NIR.

Page 6: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

i

TABLE OF CONTENTS page

LIST OF FIGURES ........................................................................................................... iii

LIST OF TABLES............................................................................................................. vi

Chapter 1. Introduction ....................................................................................................... 1

1.1 Motivation and Problem Statement .................................................................... 1 1.2 Scientific and Engineering Challenges ............................................................... 2 1.3 Scope of the Thesis and Contributions ............................................................... 4 1.4 Thesis Outline ..................................................................................................... 6

Chapter 2. Background ....................................................................................................... 9

2.1 Background......................................................................................................... 9 2.2 Basics of Dielectrometry Sensing....................................................................... 9 2.3 Fringing Field Dielectrometry .......................................................................... 13

Chapter 3. Designing Interface Circuits for FEF Dielectrometry..................................... 19

3.1 Introduction....................................................................................................... 19 3.2 AC Impedance Divider ..................................................................................... 21 3.3 AC Current Sense Circuit ................................................................................. 23 3.4 Resonant Impedance Converter ........................................................................ 24 3.5 Charge Discharge Circuit.................................................................................. 26 3.6 Off-the-shelf Impedance Sensing Chips ........................................................... 29 3.7 MOSEFT Switch Charge Injection................................................................... 31 3.8 Excitation .......................................................................................................... 31 3.9 Conclusions....................................................................................................... 33

Chapter 4. Design Principle of Multi-channel FEF Sensors............................................. 35

4.1 Introduction....................................................................................................... 35 4.2 Figures of Merit ................................................................................................ 37 4.3 Major Design Concerns .................................................................................... 42 4.4 Major Design Trade-offs................................................................................... 43 4.5 Examples of Sensor Designs............................................................................. 44 4.6 Conclusion ........................................................................................................ 57

Chapter 5. Non-dimensionalized Parametric Modeling of FEF Sensors.......................... 58

5.1 Introduction....................................................................................................... 58 5.2 Simulation Setup............................................................................................... 59 5.3 Simulation Results ............................................................................................ 61 5.4 Non-dimensionalization.................................................................................... 62 5.5 Conclusions....................................................................................................... 71

Chapter 6. Image Reconstruction Algorithms .................................................................. 73

Page 7: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

ii

6.1 Electrical Impedance Tomography ................................................................... 73 6.2 Background on Inverse Problems ..................................................................... 75 6.3 Modeling of Electrode ...................................................................................... 76 6.4 The Layer Stripping Algorithm ........................................................................ 77 6.5 Problem Description ......................................................................................... 78 6.6 Proof of Concept Study..................................................................................... 79 6.7 Conclusions and Future Work .......................................................................... 80

Chapter 7. Moisture Dynamics in Food Products............................................................. 81

7.1 Review of process analytical technologies in food analysis............................. 81 7.2 Definition of the Problem ................................................................................. 84 7.3 Methodology..................................................................................................... 86 7.4 Experimental Setup........................................................................................... 86 7.5 Experimental Procedure.................................................................................... 88 7.6 Experimental Result and Data Analysis ........................................................... 89 7.7 Conclusions....................................................................................................... 93

Chapter 8. Measuring Physical Properties of Pharmaceutical Samples ........................... 94

8.1 Motivation......................................................................................................... 94 8.2 Measuring Tablet Hardness and Coating Thickness......................................... 97 8.3 Measuring Tablet Coating Thickness ............................................................. 100 8.4 Acquiring Drug Signature Using a FEF Sensor.............................................. 104 8.5 Measuring API Concentration for Powder Samples....................................... 105 8.6 Conclusions..................................................................................................... 107

Chapter 9. Conclusions and Future Work....................................................................... 109

9.1 Conclusions..................................................................................................... 109 9.2 Future Work .................................................................................................... 110

References....................................................................................................................... 112

Appendix A: DiSPEC Hardware Installation Guide....................................................... 124

Appendix B: Matlab Code for the Layer Stripping Algorithm....................................... 136

Page 8: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

iii

LIST OF FIGURES

Figure Number page

1.1. Scope of this thesis and future work. ........................................................................... 6

2.1. Flow diagram of the dielectrometry system............................................................... 11

2.2. A fringing field dielectrometry sensor can be visualized as (a) a parallel plate capacitor whose (b) electrodes open up to provide (c) a one-sided access to the material under test..................................................................................................... 14

2.3. A generic interdigital dielectrometry sensor.............................................................. 16

2.4. Half-wavelength cross-section with a superimposed equivalent π-circuit model. .... 18

2.5. A conceptual view of multi-wavelength dielectrometry............................................ 18

3.1. The fringing electric field sensors are implemented with a vast array of designs. .... 20

3.2. Circuit schematic of an AC impedance divider. ........................................................ 22

3.3. A current-sense impedance converter. ....................................................................... 24

3.4. (a) Parallel and (b) series RLC tanks. ........................................................................ 25

3.5. A resonant impedance converter circuit. ................................................................... 26

3.6. A charge/discharge circuit. ........................................................................................ 28

3.7. The timing diagram for the charge/discharge circuit................................................. 28

3.8. A voltage-divider capacitance sensing circuit. .......................................................... 31

4.1. Evaluation of the effective penetration depth γ3% of an FEF sensor.......................... 38

4.2. Cross-sectional view of a fringing electric field sensor with multiple penetration depth excitation patterns. .......................................................................................... 39

4.3. Top-down view of a concentric fringing electric field sensor head........................... 45

4.4. Top-down view of a concentric fringing field sensor head with shield electrodes between the driving and the sensing electrodes. ....................................................... 46

4.5. Simulated electric field line distribution illustrating the effect of the additional shielding electrode. ................................................................................................... 47

4.6. Layout of a test sample positioned above the unshielded concentric FEF sensor. .... 48

4.7. Layout of a test sample positioned above the shielded concentric FEF sensor ......... 49

4.8. Simulated equipotential plot of the unshielded concentric FEF sensor. .................... 49

4.9. Simulated equipotential plot of the shielded concentric FEF sensor. ........................ 50

4.10. Absolute capacitance value from both sensor designs in the FE simulation. .......... 51

Page 9: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

iv

4.11. Normalized capacitance value from both sensor designs in the FE simulation....... 51

4.12. The effect of change in shielding electrode width on sensor signal strength. ......... 52

4.13. The effect of change in shielding electrode width on sensor penetration depths. ... 53

4.14. Absolute capacitance value of the inner channel of the unshielded sensor. ............ 55

4.15. The effect of change in substrate thickness on sensor penetration depth. ............... 55

5.1. A concentric FEF sensor and its signal conditioning circuit. .................................... 60

5.2. Simulation setup of a concentric FEF sensor in the R-Z plane.................................. 60

5.3. The electric field arrows and equipotential lines for concentric FEF sensors with separate backplanes................................................................................................... 62

5.4. The electric field arrows and equipotential lines for concentric FEF sensors with solid backplanes. ....................................................................................................... 63

5.5. Normalized capacitance between the drive electrode and sense1. ............................ 63

5.6. Normalized capacitance between sense1 and sense2................................................. 64

5.7. Normalized capacitance between sense2 and drive ................................................... 64

5.8. Normalized capacitance between the drive electrode and sense1 ............................. 65

5.9. Electrode pair sensitivity to changes in substrate thickness. ..................................... 66

5.10. Electrode pair sensitivity to changes in the dielectric permittivity of the MUT...... 66

5.11. Fitting residue of the fourth-order polynomial model for C1d/λεs. ........................... 68

5.12. Comparison between finite element simulation results and results from the parametric model. ..................................................................................................... 69

5.13. A half-wavelength portion of the interdigital sensor is shown. ............................... 70

5.14. (a) Finite element simulation results and (b) results estimated by the parametric model......................................................................................................................... 71

6.1. Side-view of the one-dimensional scanner setup....................................................... 79

7.1. Frequency ranges of various types of spectroscopic sensing techniques. ................. 81

7.2. Top and bottom view of the concentric sensor head.................................................. 86

7.3. Side view of the sensor in a voltage divider setup..................................................... 87

7.4. Sensor geometry and experimental setup. ................................................................. 88

7.5. Capacitances and phase measured at different moisture content levels. ................... 89

7.6. Capacitance measurements against the weight of added water at 10 kHz................. 90

7.7. Moisture content distribution across the radius of the sample................................... 92

8.1. Tablet sample weight and thickness against the pressure applied ............................. 98

8.2. Capacitance and phase of tablet samples measured against sample hardness. ........ 100

Page 10: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

v

8.3. Fringing electric field sensor setup for measuring tablet coating thickness.. .......... 100

8.4. Absolute capacitance measurements of tablet samples with different coating thickness using a parallel plate sensor. ................................................................... 101

8.5. Capacitance and phase variations of samples with coating thickness.. ................... 102

8.6. Capacitance variation against sample weight using a parallel plate sensor............. 102

8.7. Absolute capacitance measurements for tablet samples with different coating thickness using a fringing electric field sensor. ...................................................... 103

8.8. Capacitance and phase variations for tablet samples of different coating thickness using a fringing electric field sensor. ...................................................................... 104

8.9. Capacitance variation against sample weight for the fringing electric field setup. . 104

8.10. Capacitance and phase measurements of three different types of tablet samples.. 105

8.11. Capacitance and phase of powder samples of various drying time. ...................... 107

8.12. Capacitance of powder samples against sample drying time measured at two separate frequencies. ............................................................................................... 107

Page 11: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

vi

LIST OF TABLES

Table Number Page

4.1.The effect of increasing shielding electrode width.. ....................................................54

4.2. Penetration depths (mm) of the concentric sensor designs. ....................................... 56

4.3. The effect of increasing substrate thickness. ............................................................. 56

5.1. Polynomial coefficients aij for C1d / (λεs). .................................................................. 67

5.2. Polynomial coefficients aij for C12 / (λεs). ................................................................. 67

5.3. Polynomial coefficients aij for C2d / (λεs). ................................................................. 67

5.4. Polynomial coefficients aij for C12 / εs........................................................................ 71

7.1. Comparison between the actual mass of the moisture added to the sample and the mass of the moisture measured by the sensor. .......................................................... 93

8.1. Tablet sample physical properties: hardness, weight, thickness................................ 99

Page 12: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

vii

ACKNOWLEDGEMENTS

I would like to acknowledge the support of my colleagues at Intel, Dupont,

especially, Dr. Ted Dibene and Dr. Steve Montgomery for their continuing

encouragement of and support.

To my adviser Prof. Alexander Mamishev, who has made the past five years a great

experience for me, who had been patient enough to go through twenty revisions on my

first research paper.

To my fun-loving lab mates Bing Jiang, Nels Jewell Larsen, Abhinav Mathur, Gabe

Rowe, Alanson Sample, Chih-Peng Hsu, and Kishore Sundara-Rajan at SEAL. The

experience at SEAL has been absolutely wonderful.

To the Center of Process Analytical Chemistry, Kraft Foods Inc, and the National

Science Foundation, who funded this research project and provided me with plenty of

opportunities to present my work in front of industrial research communities.

To my parents who have always valued education more than anything else, and who have

encouraged me to set high goals for myself and not to settle for anything less.

Page 13: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

viii

DEDICATION

This thesis is dedicated to my parents Anwen Li, and Heng Zhou.

Page 14: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

1

Chapter 1. Introduction

1.1 Motivation and Problem Statement

The work in the thesis is motivated by the omnipresent need for process control sensing

techniques in the manufacturing industries. This thesis is based on the following

publications by the author [1-7].

Process control is one of the most important tasks of analytical chemists, engineers, and

physicists in manufacturing industries. Product quality is often controlled downstream of

a process. A failed product has to be reworked, sold at a lower price, or even destroyed.

Integrated sensing techniques are the key to industrial process control. Process control

typically involves feedback and feed-forward systems that rely on accurate sensor

measurements to control the manufacturing variables within the desired limit. Variations

in the physical, chemical, and biological properties of a sample need to be closely

monitored to ensure the quality of a product. Faced with increasing cost-reduction

pressure, manufactures are pursuing wider adoption of new process analytical techniques.

Product quality and safety are critical in the food and pharmaceutical industries. Food

industry is seeing great advances in the areas of food biotechnology, food science, and

food engineering [8]. Combinations of new dehydration, food sterilization, freezing, and

separation processes lead to the improvements of safety, convenience, taste, and value of

food products [9]. Sensor technology is at the forefront of the needs of food industry [10].

Existing sensor systems should be updated and improved based on the advances in

computer technology, microelectromechanical systems (especially microfluidics), data

processing algorithms, and material science.

A similar trend is occurring in the pharmaceutical industry. FDA has been steering the

pharmaceutical industry in the direction of a quality–by–design (QbD) approach, and

away from the quality–by–testing (QbT) approach traditionally taken by the

pharmaceuticals sector. The basis of QbT is to test the finished product for quality.

Product specimens that fail to meet the specification are rejected. This approach leads to

Page 15: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

2

a great deal of waste and thus is costly to both the manufacturer and the consumer. The

wastage caused by QbT approach can increase production costs by as much as 10

percent. The basis of the alternative approach QbD is to incorporate the knowledge of the

product and the process to ensure all critical quality parameters are adequately controlled

and that the finished product meets specifications.

FDA started a Process and Analytical Technology (PAT) initiative. Process Analytical

Technology is a system for designing, analyzing, and controlling manufacturing through

timely measurements (i.e., during processing) of critical quality and performance

attributes of raw and in-process materials and processes with the goal of ensuring final

product quality. The desired goal of the PAT framework is to design and develop

processes that can consistently ensure a predefined quality at the end of the

manufacturing process. Such procedures would be consistent with the tenet of quality by

design and could reduce risks to quality and regulatory concerns while improving

efficiency.

This thesis explores the application of fringing electric field dielectrometry to industrial

process control. FEF sensors are non-invasive and can access the sample under test from

only one side. Typically, no sample preparation is required for FEF sensor measurement.

Custom-build FEF sensing systems cost much less than other commercially available

process analytical instruments. These attributes of FEF sensing systems make them very

attractive candidates for real-time industrial process control.

1.2 Scientific and Engineering Challenges

The scientific and engineering challenges are discussed here from three aspects: sensor

modeling and design, sensor interface circuit design, and data analysis.

1.2.1 FEF sensor modeling and design

The field distribution of FEF sensors is inherently non-uniform. Sensor measurements are

typically non-linear functions of the distribution of the dielectric or physical properties of

the material under test. Modeling and design optimization are very complex due to this

inherent non-linearity. The performance of an FEF sensor is largely determined by its

Page 16: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

3

geometry. FEF sensor design is an iterative optimization process of modeling and

redesign, where the sensor geometry is adjusted to meet the design specifications.

There are no generic analytical models for FEF sensors. Analytical models for FEF

sensors are usually based on simplified geometries and idealized assumptions, which

limits their accuracy for real world applications. Finite Element (FE) models can

typically achieve higher accuracy than analytical models. However, modeling accuracy is

heavily dependent on proper mesh and boundary conditions. Therefore, setting up the

models can be time-consuming. An efficient modeling method that is both fast and

accurate can greatly aid the design optimization process.

The design process of FEF sensors and sensor arrays relies on a good understanding of

the fundamental principles and design trade-offs. For imaging applications, the major

goal of sensor design is to achieve the optimum balance of measurement sensitivity,

signal strength, imaging resolution, and measurement speed. The finite area of sensor

head makes it impossible to achieve all design goals simultaneously. The task, therefore,

is to consider the trade-offs and determine the optimal combination of design variables

for a given application.

1.2.2 Sensor interface circuit design

FEF sensors are impedance sensors. They detect changes in the physical properties of the

MUT by measuring the sensor terminal impedance. The challenge is to design an

interface circuit that can accurately measure complex impedance across a wide frequency

range.

For imaging applications, the distribution of the physical parameter of interest is to be

recovered. Local variations in the physical properties of the MUT typically manifest as a

very small change in the terminal impedance of the sensor, while baseline impedance

value can change greatly. Achieving high measurement resolution and wide dynamic

range simultaneously is a challenge.

For industrial process control applications, the sensor measurements tend to vary within a

broad range due to variations in the process parameters such as temperature, humidity,

Page 17: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

4

viscosity, etc. Designing an interface circuit with good dynamic range while maintaining

high measurement accuracy is a challenge. In integrated micro-sensors, the challenge is

to design circuits with good noise immunity so that high measurement sensitivity can be

delivered.

1.2.3 Image reconstruction

Electrical impedance imaging (EIT) is a soft-field imaging technique. Soft-field

modalities are different from ‘hard-field’ techniques like X-ray Computed Tomography

(CT). X-rays propagate in straight lines. Their absorption at any point inside the material

under test (MUT) is completely independent of the absorption at any other point. Image

reconstruction for X-ray CT is a linear problem involving only sparse and well-

conditioned sensitivity matrices. The term sensitivity matrix here refers to the jacobian

matrix relating the parameter of interest with sensor measurements. EIT, on the other

hand, is a low-frequency electromagnetic radiation technique, with the excitation

frequency typically lower than 100 kHz. Due to the long wavelength, an electrostatic

representation is most appropriate for such low frequency techniques. It is inherent to

soft-field methods that the field strength at any point is a non-linear function of the

distribution of the electrical properties throughout the MUT. This makes the associated

reconstruction much more difficult to solve. Image reconstruction for EIT involves

solving an ill-posed inverse problem. Advanced image reconstruction algorithms have

been developed within the mathematical context to tackle the impedance imaging

problem, but few of the advanced algorithms have been used effectively in industrial

process control. The gap between the theoretical algorithms and practical applications

needs to be bridged.

1.3 Scope of the Thesis and Contributions

Figure 1.1 shows the scope of this thesis. Design and modeling of FEF sensors is the

focus of the thesis. The trade-offs and interdependencies of multi-channel FEF sensor

design are described and the general design guidelines are presented within the same

context. In addition, a non-dimensionalized parametric model is developed for FEF

Page 18: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

5

sensors. The model is calibrated based on finite element (FE) simulation results. Once

calibrated, no more FE simulations are necessary. This empirical modeling method

strikes a middle ground between the purely theoretical analytical methods and those

based on FE modeling.

For sensor interface circuits, typical circuit topologies used for impedance sensing are

surveyed, with special focus on those with broadband spectroscopic capabilities suitable

for real-time applications.

In the realm of parameter estimation, this thesis attempts to address the divide between

theoretical algorithms and their applications to solve real world problems. Specifically,

layer-stripping algorithm is used for one-dimensional profiling.

The thesis has two major contributions. First, it provides guidelines for designing FEF

sensor systems, specifically multi-channel FEF sensor systems, for industrial process

imaging applications. Such systems can be used for recovering images of the distribution

of the parameter of interest. The majority of the research on electrical impedance imaging

systems focuses on circular electrodes around an enclosed cylinder. Work on the

instrumentation of imaging systems based on planar electrodes has been scarce. The

thesis fills in the gap by detailing the various aspects of designing a FEF sensing system

for industrial applications.

The second contribution of the thesis is to demonstrate the viability of FEF

dielectrometry as a process analytical sensing technique. Till this day, FEF sensing

systems have not been explored as extensively as other analytical techniques like nuclear

magnetic resonance (NMR) or near-infrared spectroscopy. This phenomenon is

particularly evident in the food and pharmaceutical industry. The thesis presented data

which shows that FEF sensors can be used for determining physical properties of food

and pharmaceutical samples. FEF dielectrometry complements NMR and NIR because

the information it provides is inherently different. NMR and NIR typically provide

information about the molecular or chemical properties of the sample, while FEF

dielectrometry provides information about the physical properties of the sample. In

addition, instrumentation for FEF dielectrometry is less costly and more flexible.

Page 19: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

6

Integration of FEF sensors into the manufacturing process of food and pharmaceutical

industries facilitates better control of product quality at lower cost.

Figure 1.1. Scope of this thesis and future work.

1.4 Thesis Outline

The theoretical background for the thesis work is described first before going into the

details on the instrumentation and parameter estimation for fringing electric field (FEF)

sensing/imaging. Specific applications of FEF sensing in the food and pharmaceutical

industry are then illustrated with experimental results. The outline of the thesis is listed

below:

Page 20: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

7

Chapter 1 describes the motivation, the challenges, and the scope of this thesis.

Chapter 2 reviews the theoretical background of dielectrometry sensing and FEF sensor.

Chapter 3 reviews the state of the art of sensor interface circuits. The operating principles

of various topologies are described and the advantages and disadvantages of each

topology are explained.

Chapter 4 presents the principle of multi-channel fringing electric field sensor design for

imaging applications. The figures of merit for FEF sensor design are presented first. Then

the major design concerns and trade-offs are explained. Finally, the design principles are

illustrated through the example of a concentric FEF sensor design.

Chapter 5 deals with modeling of FEF sensors. Non-dimensionalized parametric models

are developed for both interdigital and concentric FEF sensors. Such models can be used

to estimate the terminal capacitance of a sensor with known dimensions. The accuracy of

the models is tested against finite element simulation results.

Chapter 6 describes the layer stripping algorithm in detail. The algorithm is used to

reconstruct images for a one-dimensional scanner. Numerical simulation results and

analysis are presented in this chapter.

Chapter 7 presents the experimental results of measuring moisture content distribution in

organic food materials. The experimental setup and procedures are explained and a

calibration-based sensing technology is presented. Chapter 9 presents experimental

results of measuring physical properties of pharmaceutical samples. Measurements from

FEF sensors and generic parallel plate sensors with the same set of test samples are

compared to illustrate how the choice of sensors can impact experimental results. The

rationale behind the choice of measurement sensors and experimental setup for such

experiments are dealt with in detail.

Chapter 8 reviews the state of the art of image reconstruction algorithms. The theory of

inverse problem solving is briefly touched upon. Then the various categories of

reconstruction algorithms are introduced. Major concerns such as electrode modeling,

choice of excitation patterns, etc. are also dealt with in this chapter.

Page 21: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

8

Page 22: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

9

Chapter 2. Background

2.1 Background

This need for real-time non-invasive sensing techniques has driven many advances in the

field of dielectrometry. Dielectrometry is widely used for determination of material

physical properties due to its non-invasiveness and wide spectrum of sensing

possibilities. Applications include agricultural products [11], soil [12], paper [13],

transformer board [14], biological sensing [15,16] and hydrophilic polymers [17].

Capacitive sensors are often used for dielectric spectroscopy. They have the advantage of

high measurement accuracy and non-invasiveness. The simplest examples of capacitive

sensors are a guard-ring parallel-plate capacitor and a coaxial cylindrical capacitor. More

complicated examples include fringing electric field sensors, which can assume various

geometries [18,19]. The penetration depth of fringing electric field sensors is proportional

to the distance between coplanar electrodes. By applying different voltage patterns to the

sensor, variable penetration depths can be achieved, thus providing FEF sensors access to

different layers of the material. This characteristic, combined with their one-sided access

capability, makes FEF sensors more flexible in use than their parallel-plate counterparts.

2.2 Basics of Dielectrometry Sensing

2.2.1 Introduction to the theory of dielectrics

Dielectric materials cover the whole spectrum of anything between conductors and

insulators. Dielectrics consist of polar molecules, or non-polar molecules, or very often

both. Due to the asymmetric configuration of polar molecules, material consisting of

these molecules has built-in dipole moments. Under an external electric field, the

polarized dipoles reorient in the electric field and neutralize some of the charges on the

electrodes. The most often used measure of material dielectric properties is the complex

Page 23: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

10

dielectric permittivity. It is a measure of the ability of the dielectric material to reorient

and neutralize charges on the electrodes. This usually depends on how polarized the

material is and the inertial force it has to overcome to reorient. Sometimes, relative

complex dielectric permittivity is used to describe material dielectric properties. It is

defined as the ratio between the dielectric permittivity of the material and that of free

space. The dielectric permittivity of free space is 8.85×10-12 F/m.

The dielectric permittivity of most dielectric materials is frequency-dependent. In the

presence of an alternating electric field, the dipole moments inside the material oscillate

with the direction of the electric field. The higher the frequency the harder it is for the

dipole moments to catch up with the change of field direction. This results in a decreasing

ability of the material to neutralize charges on the electrodes at high frequencies. In

general, the total complex dielectric permittivity ε*(ω) is written as:

*( ) '( ) ''( )iε ω ε ω ε ω= −

(2.1)

where 'ε and ''ε are, respectively, the real permittivity and the dielectric loss factor of

the material.

Jonscher of the Chelsea Dielectric Group has been studying the problem of a universal

relaxation law [20]. Until now, no one has proven the existence of a general model to

describe the dielectric relaxation process. One of the most widely used models for fitting

dielectric relaxation data is the Havriliak-Negami (HN) function, as shown in (2.2),

where 0ε is the dielectric permittivity at dc and ε∞ is its asymptotic value at infinite high

frequency. The term 0ε ε∞− is the total dielectric relaxation strength and 0τ is the

relaxation time of the material. For 1β = , the Cole-Cole model emerges; whereas for

1α = the Davison-Cole model emerges.

( )

0

0

*( )1 i

βα

ε εε ω εωτ

∞∞

−= +

+ (2.2)

''σ ωε=

(2.3)

Page 24: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

11

2.2.2 Principles of dielectric spectroscopy sensing

Dielectric spectroscopy involves the study of the response of a material to an applied

electric field. Typically, the technique is used 1) to gain theoretical understanding of the

dielectric properties of a material/sample, and 2) to relate the dielectric data to other

physical/chemical properties of interest.

Dielectrometry is a versatile sensing technique. Figure 2.1 shows the flow diagram of a

dielectrometry system. Material dielectric permittivity is dependent on various physical

properties such as geometry, texture, temperature, degree of cure, moisture content, and

aging status. Changes in these physical properties will be reflected as changes in such

dielectric property variables as *ε ,σ , and tanδ , where σ is defined in (2.3) and tanδ is

defined as the ratio between the real and imaginary parts of the complex dielectric

permittivity. These parameters variations, in turn, lead to changes in the impedance

measurements from the sensor. The fact that dielectric measurements are sensitive to

changes of a wide range of material physical properties makes dielectrometry sensing

technique a potential candidate for a broad spectrum of sensing applications.

Measurecapacitancesand conductances

Calibration-basedsensing

Differentialsensing

Computedistributionof dielectricproperties

Computedistributionof physicalproperties

Imaging

Faster Slower

ε σ, δ, Μ*, tan ∗

thicknesssurface texturetemperaturedegree of curemoistureporositydensityconcentrationpercolationstructural integrityaging statuscontamination .......

Figure 2.1. Flow diagram of the dielectrometry system.

2.2.2.1 Impedance spectroscopy and dielectric spectroscopy

Rather than focus on details of what happens inside dielectric materials, electrical

engineers often analyze dielectrics from a macroscopic perspective. Impedance

Page 25: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

12

spectroscopy is one such macroscopic approach. It models dielectrics as lumped circuit

elements and uses the terminal electric impedance measurement to represent the physical,

chemical and biological processes happening inside the material.

A proper choice of a circuit model is crucial to obtaining good modeling results. The

dielectric spectra that can be represented by combinations of RC circuits are called

relaxation spectra, whereas those that can be represented by combinations of RL circuits

are called resonance spectra. To determine the choice of circuit models, the frequency

dependency of material dielectric constant should be examined. For relaxation spectra,

the dielectric constant only stays constant or falls with increasing frequency. In these

cases, RC circuit models should be used. If otherwise, RL or RLC circuit model should

be used [21]. In addition to lumped circuit models, distributed circuit models are

sometimes used to model dielectric materials as a distributed dielectric medium in

bounded or unbounded space [22,23].

Dielectric spectroscopy relates material dielectric properties with corresponding physical

properties and investigates the fundamental theoretical link between them. It is often used

for research efforts investigating material dielectric properties. For industrial

applications, where in-depth theoretical knowledge of the dielectric property of the

material is unnecessary, impedance spectroscopy is sufficient.

2.2.2.2 Calibration based sensing

Calibration based sensing works by establishing a quantitative relationship between

material physical property of interest and the resulting impedance measurements. This

functional dependence is usually empirically determined. The algorithms for such

calibration-based approaches are usually quite straightforward, yet these approaches are

not sufficient to gain insight about the physical nature of the material. For real-time

imaging applications, adaptive self-calibration mechanisms are desired to accommodate

variations in the sample or change in the setup.

2.2.2.3 Differential sensing

Differential sensing is a methodology that can be used for monitoring changes.

Page 26: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

13

Systematic measurement errors can be greatly reduced by simply looking at the variation

of the parameters of interest. The system is typically calibrated against baseline

measurements first, and then only the deviations from the baseline measurements are

used for estimation. Examples of such applications include monitoring the aging process

of food product in storage rooms, monitoring the lung/heart activities of patients,

monitoring the drying process of pharmaceutical powder samples, etc.

2.2.2.4 Imaging – electrical impedance and capacitance

tomography (EIT/ECT)

EIT and ECT are the most widely used technologies for imaging the distribution of

material physical properties in industrial applications. Electrical impedance tomography

(EIT) is an imaging modality developed mainly for medical applications. An EIT system

works by applying current to a human body through various electrodes and measuring the

induced voltage at the electrodes. Using the different combinations of current patterns

and the corresponding voltage measurements, the inverse problem is solved to recover

the resistivity distribution of tissue being imaged. Electrical capacitance tomography

(ECT) is a similar modality developed for industrial process control applications. In an

ECT system, electrodes are typically attached to external walls of a pipeline. Similar to

EIT, current is applied and the induced voltage measured. Since the electrodes are not in

direct contact with the sample, the terminal impedance is typically reactive, thus the term

capacitance tomography.

Unlike X-ray or laser imaging, EIT and ECT are “soft field” techniques, because the field

lines that penetrate through the sample do not stay in a straight path. This greatly

increases the complexity of parameter estimation algorithms for image reconstruction.

2.3 Fringing Field Dielectrometry

A fringing field dielectrometry sensor has the same principle of operation as the more

conventional parallel-plate or coaxial cylinder dielectric sensor cell. The voltage is

applied to the electrodes, and the impedance across the electrodes is measured. However,

unlike the parallel-plate cell, the fringing field sensor does not require two-sided access to

Page 27: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

14

material under test. Figure 2.2 shows a gradual transition from the parallel plate capacitor

to a fringing field capacitor. In all three cases, electric field lines pass through the

material under test, therefore the capacitance and conductance between the two electrodes

depends on the material dielectric properties as well as on the electrode and material

geometry.

Figure 2.2. A fringing field dielectrometry sensor can be visualized as (a) a parallel plate capacitor whose (b) electrodes open up to provide (c) a one-sided access to the material under test.

Interdigital dielectrometry is a subset of interdigital electrode sensor applications that

relies on direct measurement of dielectric properties of insulating and semi-insulating

materials from one side [24-26]. The basic idea is to apply a spatially periodic electrical

potential to the surface of the material under test. The combination of signals produced

by the variation of the spatial period of the interdigital comb electrodes combined with

the variation of electrical excitation frequency potentially provides extensive information

about the spatial profiles and dielectric spectroscopy of the material under test. Since the

changes in the dielectric properties are usually induced by changes in various physical,

chemical, or structural properties of materials, the dielectrometry measurements provide

effective means for indirect non-destructive evaluation of vital parameters in a variety of

industrial and scientific applications [27,28].

Usually, the capacitance between two co-planar strips, as shown in Figure 2.2 (c), is

comparable to the stray capacitance of the leads (conductors that connect the electrodes

with the electrical excitation source). Therefore, in order to build-up an easily measurable

electrode structure, the coplanar strip pattern may be repeated many times.

The art and science of designing sensors with multiple interdigital electrode pairs and

Page 28: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

15

processing the output signals to gain knowledge about the material under test is the

subject of multi-wavelength interdigital frequency-wavenumber (ω-k) dielectrometry,

which has been under development for about three decades. The penetration depth of the

fringing quasistatic electric fields above the interdigital electrodes is proportional to the

spacing between the centerlines of the sensing and the driven fingers and is independent

of frequency. Overviews of important concepts related to this technology are available in

[29-35].

One of the most attractive features of multi-wavelength dielectrometry is the ability to

measure complex spatially inhomogeneous distributions of properties from one side. As

the complexity of spatial distribution grows and the number of unknown variables in each

experiment increases, the parameter estimation algorithms become more complicated,

computationally intensive, and less accurate and reliable. Ultimately, every major type of

spatial distribution of material properties requires a different parameter estimation

algorithm. The types of spatial distributions include, but are not limited to, homogeneous

materials, multiple layer materials, local discontinuities (such as cracks and electrical

trees), global discontinuities of micro-structure (such as grains or fibers forming the

material), and, finally, smoothly varying properties. On the electrical properties side,

materials under test may be purely insulating or weakly conductive. Various phenomena

may affect sensor response, including frequency dispersion, electrode polarization due to

an electrochemical double layer, quality of interfacial contact, and many others.

A conceptual schematic of an ω-k dielectrometry sensor measurement is presented in

Figure 2.3. For a homogeneous lossy dielectric medium of semi-infinite extent, periodic

variation of quasistatic electric potential along the surface in the x direction produces an

exponentially decaying pattern of electric fields penetrating into the medium in the z

direction. The variation of shade in the material under test indicates the possible

variation of material properties and thus variations in the complex dielectric permittivity

ε * with the distance z from the surface.

Page 29: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

16

Figure 2.3. A generic interdigital dielectrometry sensor. The black stripes are the electrodes. Underneath the electrodes is the substrate of the sensor (white). At the bottom (black) is the backplane of the sensor. Above the sensor is the sample under test (SUT). The grayscale on the sidewalls of the SUT indicates the non-uniform electrical field that the SUT is subject to.

Concepts of the forward and the inverse problems are widely used in the literature related

to this technology. Here, the forward problem is defined as the task of determining the

electric field distribution and the inter-electrode admittance matrix when the geometry,

material properties, and external excitations are given. Correspondingly, the inverse

problem requires determining either material properties or associated geometry, or both,

when the imposed excitations and experimental values of the sensor admittance matrix

are available. Each application that involves theoretical modeling usually requires solving

the forward problem.

The forward problem can be solved using several approaches. One of them is to use a

continuum model [36]. From the electroquasistatic field point of view, in a homogeneous

lossy dielectric, the electric scalar potential of the field excited by the driven electrode is

a solution to Laplace's equation. At any constant z position, the electric field distribution

far away from the sensor edges is periodic in the x direction and assumed uniform in the y

direction. For a homogeneous dielectric of semi-infinite extent, the scalar potential can be

written as an infinite series of sinusoidal Fourier modes of fundamental spatial

wavelength λ that decays away in the z direction:

Page 30: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

17

0

( sin cos )nk zn n n n n

ne A k x B k x

∞−

=

Φ = Φ +∑ (2.4)

where kn=2πn/λ is the wavenumber of each mode. For j te ω excitations at radian

frequency ω, such that ˆ j tn ne

ωΦ = ℜ Φ , the complex surface capacitance density Cn

relates ε*Êzn at a planar surface z = constant to the potential nΦ at that surface for the n-th

Fourier mode of the homogeneous dielectric of semi-infinite extent as:

* ˆˆˆ

znn

n

EC ε=

Φ (2.5)

where

)/(* ωσεε j−= (2.6)

is the complex permittivity with ε as material dielectric permittivity and σ as ohmic

conductivity. Then, the knowledge of ˆnC at the electrode surface allows calculation of the

terminal current from the potential distribution at that surface. It is also possible to solve

the forward problem with commercial finite-element software [37], with finite-difference

techniques, or by using analytical approximations [38].

Figure 2.4 shows the equivalent circuit of the sensor superimposed onto the schematic

view of a sensor half-wavelength. Note that each wavelength has an opposite conducting

guard plane at the bottom of the substrate. For each wavelength, a follower op-amp drives

the guard plane at the substrate bottom at the voltage VG = VS, thus eliminating any

current between the sensing and guard electrodes through the substrate. Therefore, the

effect of G20 and C20 on circuit response is eliminated, which simplifies response analysis

and improves device sensitivity. The concept of imposed frequency-wavenumber (ω-k)

goes beyond dielectrometry applications. Earlier studies led by J. R. Melcher employed

interdigital electrodes to study electrohydrodynamic surface waves and instabilities [39],

effects on static electrification in insulating liquids [40,41], and electromechanics of

electrochemical double layers in liquid electrolytes [42].

The penetration depth of the fringing electric fields above the interdigital electrodes is

proportional to the spacing λ/2 between the centerlines of the sensing and the driven

Page 31: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

18

fingers. Figure 2.5 illustrates the idea of multiple penetration depths for a three-

wavelength sensor. The variation of the material properties across the thickness of the

material under test in the z direction can be approximately found by simultaneously

solving three complex equations describing this three-wavelength experimental

arrangement as a piece-wise three layer system.

Figure 2.4. Half-wavelength cross-section with a superimposed equivalent π-circuit model.

Figure 2.5. A conceptual view of multi-wavelength dielectrometry. The penetration depth of electric field lines is proportional to the electrode spatial wavelength λ.

Page 32: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

19

Chapter 3. Designing Interface Circuits for FEF Dielectrometry

3.1 Introduction

Fringing electric field sensors are widely used for measurement of material properties in

numerous scientific and industrial applications. Generally speaking, the sensing system

always comprises three main parts: sensor head, interface electronics, and the data

acquisition/signal processing units. The sensor head is a system of electrodes that creates

the electric field for probing the material properties. The complexity of sensor heads

varies from a pair of flat metal strips to multi-electrode three-dimensional arrays. The

interface electronics also varies widely in complexity, from basic op-amp circuits to

complex bench-top instrumentation. The signal processing hardware and algorithms also

vary depending on the need of the application, ranging from an on/off signal indicating

the presence of a material to the inverse-problem solving algorithms that require complex

matrix operations. Figure 3.1 shows the conceptual description of the design domain of

fringing electric field sensing systems. The second column, Interface Electronics, is the

focus of this chapter. The subject matter of other columns is also covered, in order to put

the discussed designs in proper context – but is not the main focus of this chapter.

Extensive tutorials and reviews are available on the subject of electrode design (sensor

head design) [43-50], electrical excitation options [51], and parameter estimation

algorithms [52-55]. The details on these topics will be covered in later chapters.

Page 33: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

20

Electrode design(sensor heads)

Interface electronicsSignal processing

Figure 3.1. The fringing electric field sensors are implemented with a vast array of designs and techniques of widely varying complexity. The connecting lines between the first and the second columns indicate typically encountered combinations. The design of dielectric sensors requires an educated selection of the electronic circuitry

that interfaces sensor electrodes with the data acquisition system. This chapter offers a

comparative review of interface circuit designs for dielectric sensors and a discussion of

their working principles, with a special focus on multi-channel interface circuit for

imaging applications.

Several review and tutorial papers appeared on this subject before. The review by Huang

et. al. [56] offers a balanced review of general principles and circuit examples, but it is

focused only on single-frequency capacitance measurements. Such circuits are not

adequate for biochemical and medical applications where samples have complex

permittivity.

These samples usually have a unique signature in the frequency domain, which can be

used to identify the presence and the concentration of samples. To recover the frequency

domain information, circuits with spectroscopic measurement capabilities are required. It

is difficult to achieve high measurement accuracy across a wide frequency range with a

single interface circuit. Different circuit topologies should be considered for the specific

frequency range of interest. This chapter reviews measurement circuitry that measures

Page 34: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

21

complex impedances at multiple frequencies.

For many imaging applications, the sensor output has a relatively large baseline value

and small variations (variation due to change in test samples). This requires the circuit to

have a high dynamic range and measurement resolution. In addition, since the signal to

be measured is small, noise needs to be suppressed to achieve a sufficient signal to noise

ratio. Interface circuits commonly used for impedance sensing applications are detailed in

the sections below.

3.2 AC Impedance Divider

Impedance divider is one of the simplest AC impedance measurement circuits. It is

typically constructed by connecting an impedance sensor and some known reference

impedance (normally an RC tank) in series. An AC voltage is applied to the combination

of sensor and reference impedance and the gain and the phase of the divider are

measured. The terminal impedance of the sensor is then calculated based on the measured

gain, phase, and the value of the reference impedance.

Figure 3.2 shows a common implementation of impedance divider. In Figure 3.2, GX

and CX are the terminal impedances of the sensor to be measured; GREF and CREF are the

known reference impedances; GS1 and CS1 are the stray impedances at the input side; and

GS2 and CS2 are the stray impedances due to the connecting cables at the output side.

Input AC voltage INV is applied across a series combination of the sensor impedance GX

//CX and the reference impedance GREF //CREF. The signal at the voltage division point

(node 1) is buffered by the voltage-follower opamp 1A . There are two reasons for using

the voltage follower. First, it decouples high-impedance node 1 from usually low-

impedance input of the measurement electronics such as a data acquisition card or a

frequency-response analyzer. Second, it provides a signal for the actively-driven shield.

In the case of the voltage divider in Figure 3.2, node 2 is the cable shielding and is

connected to the output of buffer opamp 1A . By feeding the voltage-follower signal back

to the shield, any effect of the stray impedances 2SG and 2SC is eliminated due to the

zero voltage drop across them. In addition, the stray impedance 1SG and 1SC at the input

Page 35: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

22

side have no effect on the applied voltage. Thus, the described AC impedance divider

circuit is stray-immune.

XG

XC

1SC 1SGINV

1

1AOUTV

REFG

REFC

2SG2SC

2

Figure 3.2. Circuit schematic of an AC impedance divider. GX and CX are the unknown conductance and capacitance of the sample under test, and GREF and CREF are the reference conductance and capacitance respectively. GS1, GS2, CS1, and CS2 are the stray conductance and capacitance due to the sensor substrate and the connecting wires.

The value of GX and CX can be calculated based on equations (3.1) and (3.2).

1

Re ( ) 1( )

X INREF

OUT

G V ZV

ωω

⎧ ⎫⎪ ⎪⎛ ⎞= ⎨ ⎬−⎜ ⎟⎪ ⎪⎝ ⎠⎩ ⎭

%%

% (3.1)

1

1 Im ( ) 1( )

X INREF

OUT

C V ZV

ωω ω

⎧ ⎫⎪ ⎪⎛ ⎞= ⎨ ⎬−⎜ ⎟⎪ ⎪⎝ ⎠⎩ ⎭

%%

% (3.2)

where 1REF

REF REF

ZG j Cω

=+

% and ω is the angular frequency of the input AC signal.

The impedance divider is a non-linear circuit. The changes in the output (the complex

gain) are not linearly proportional to perturbations at the input (sensing impedance). The

dynamic range of the measured gain is between 0 and 1. The circuit is most sensitive

when the value of the reference impedance is close to the sensor impedance to be

measured. Therefore, variable capacitors and resistance are sometimes used to adjust the

reference impedance for the maximum measurement sensitivity.

Page 36: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

23

AC impedance dividers with buffer opamps are not suitable for measuring small

capacitances (for example, XC < 0.1 pF), because state of art opamps typically have an

input capacitance greater than 1 pF. This capacitance is in parallel with the reference

capacitance REFC . Therefore, the effective reference capacitance is always greater than 1

pF, which limits the lowest measurable capacitance of the circuit.

Very low/high input frequency can be used to decouple of the conductance and the

reactance being measured. The upper frequency limit of the AC excitation is limited by

the bandwidth of the buffer opamp. Typically, there is a trade-off between the input

impedance and the frequency bandwidth (BW) of the opamp. High BW opamps tend to

have lower input impedance, while opamps with high input impedance tend to have lower

BW. Low frequency (mHz or µHz) excitation leads to long measurement time, and it

should be used only for detecting loss factors of highly resistive materials.

3.3 AC Current Sense Circuit

Another circuit commonly used for impedance measurements is the current-sense

amplifier. It is used in many commercially available RCL meters, impedance analyzers,

insulation resistance meters, and even microphones. Figure 3.3 shows a typical

implementation of a current sense impedance converter. An AC excitation voltage VIN is

applied across the impedance sensor and the resulting current is measured. An effective

way to measure small AC current is to use an I-V converter (integrator) since it is

difficult to measure current directly. The output of the current to voltage converter is

connected to a high accuracy gain/phase measurement system such as Solartron

frequency analyzer or a data acquisition card. Given the value of the reference impedance

used in the feedback loop, the value of the sensor’s impedance can be calculated from the

gain/phase measurements according to the following equations.

REFOUTXIN ZVZV // −= (3.3)

*// AZVVZZ REFOUTINREFX −=−= (3.4)

where 1REF

REF REF

ZG j Cω

=+

% , XX

X CjGZ

ω+=

1 , and INOUT VVA /* = . Note that A* is the

Page 37: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

24

complex gain measured at the output, which contains both amplitude and phase

information.

XG

XC

1SC 1SG 2SG 2SC

1A

REFC

REFG

OUTVINV

Figure 3.3. A current-sense impedance converter. GX and CX are the unknown conductance and capacitance of the sample under test, and GREF and CREF are the reference conductance and capacitance respectively. GS1, GS2, CS1, and CS2 are the stray conductance and capacitance due to the sensor substrate and the connecting wires.

The current sense circuit is inherently stray-immune. First, the stray impedances at the

input CS1 and GS1 are in parallel with the input voltage source, therefore, they have no

effect on the VOUT; second, the sensor’s sensing electrode (node 1) is held at the virtual

ground through active feedback, thus eliminating the effect of stray impedances CS2 and

GS2 and that of the input capacitance of opamp A1.

The measurement frequency of current sense circuits typically goes from mHz to MHz.

the upper limit of the excitation frequency is determined by the bandwidth of the opamp

used.

3.4 Resonant Impedance Converter

Resonance circuits typically involve an RLC tank, which consists of a known inductance

L and an unknown conductance Gx and capacitance Cx of the test sample. Figure 3.4

shows (a) a parallel RLC tank and (b) a series RLC tank. The frequency of the AC

excitation signal is tuned until the circuit reaches resonance. The resonant frequency is

determined by (3.5). At resonance, the inductive reactance cancels the capacitive

Page 38: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

25

reactance, and the tank becomes purely resistive. The resistance and capacitance of the

test medium are calculated based on the known inductance L and the detected resonant

frequency fR.

12Rf LCπ

= (3.5)

C GL

CGL

(a) (b)

Figure 3.4. (a) Parallel and (b) series RLC tanks. Resonance methods are capable of measuring complex impedances over a wide

frequency range with a very high accuracy. However, they are not suitable for real-time

applications because the frequency tuning is time-consuming. Circuits based on the

resonance methods are widely used for laboratory grade dielectrometry instrumentation

[57,58].

Figure 3.5 shows an example of a resonant impedance converter circuit. The frequency of

the input signal VIN is tuned until the resonance point is reached. At the resonance, the

reactance of LR cancels that of CX. We have

XR

R CLf

π21

= (3.6)

X

REF

IN

OUT

GG

VV

= (3.7)

Therefore, we can calculate the terminal impedance of the sensor based on the following:

2

1(2 )X

R R

Cf Lπ

= (3.8)

Page 39: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

26

A

GV

VGG REF

OUT

INREFX == (3.9)

where INOUT VVA /= is the measured gain.

XG

XC

1SC 1SG 2SG 2SC

RL

REFG

1A

REFC

INVOUTV

Figure 3.5. A resonant impedance converter circuit. GX and CX are the unknown conductance and capacitance of the sample under test, and GREF and CREF are the reference conductance and capacitance respectively. GS1, GS2, CS1, and CS2 are the stray conductance and capacitance due to the sensor substrate and the connecting wires.

As in the case of the current sensing impedance converter, the circuit is immune to the

effect of stray capacitances and resistances. The stray impedances CS1, GS1, CS2, and GS2

have no effect on the measurements of the circuit.

3.5 Charge Discharge Circuit

For applications requiring the measurement of a sensor’s reactance only,

charge/discharge method is often a preferred choice. A charge/discharge circuit operates

by charging the capacitor being measured to some preset voltage and then discharging it

through a charge detector. If the period of this charge/discharge cycle is much shorter

then the time constant of the feedback loop around the charge detector op-amp (for the

voltage feedback I-V converter), then the output voltage will be smoothed to virtually

only a DC component proportional to the magnitude of the average current flowing

through the detector. This method allows an op-amp with bandwidth much lower then the

measurement frequency to be used.

Page 40: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

27

Figure 3.6 shows an stray-immune circuit developed by S. M. Huang [59]. Electronic

switches 1S , 2S , 3S , and 4S are turned on or off according to the timing diagram in Figure

3.7. During “charge” half cycle, 1S and 4S are closed, allowing XC to charge to the

source voltage SV . At the same time, sensor’s stray capacitance 1SC , and combined

parasitic capacitance 12PC of the switches 1S and 2S , are charged to SV as well. During

“discharge” half cycle, 2S and 3S are closed, while 1S and 4S are opened up. The charge

on 1SC and 12PC flows directly to ground through 2S without affecting the measurement.

The charge transferred from the sensor’s capacitance to the detector in a single discharge

is

S XQ V C= (3.10)

The average current entering the detector (at node 1) is

AVE S XI V C f= (3.11)

where 1

C

fT

= is a charge/discharge frequency, and CT is the time of a complete

charge/discharge cycle. The average current AVEI is converted to a DC voltage by the

charge detector:

OUT S X REFV V C f G= (3.12)

It should be noted that throughout the charge/discharge virtually no current flows through

sensor’s stray capacitance 2SC and the combined parasitic capacitance 34PC of the

switches 3S and 4S , thus they have no effect on OUTV . The circuit is, therefore,

intrinsically stray-immune. Furthermore, if the switches 1S through 4S have low “on”

resistance, the circuit is immune to sensor’s conductance as well.

The measurement frequency of Huang’s implementation is in the range of 100 kHz to 5

MHz, which is typical of the charge/discharge technique. The output of the circuit is a

DC voltage proportional to the sensor’s terminal capacitance XC .

Page 41: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

28

OUT REFX

S

V GCV f

= (3.13)

XG

XC

1 S C 1SG 2SG 2SC1 A

REF C

REF G

OUTVS V

2 S

3S

1 S

4S

P12 C

P34CGS1 GS2 CS2CS1

XG

XC

1 S C 1SG 2SG 2SC1 A

REF C

REF G

OUTVS V

2 S

3S

1 S

4S

P12 C

P34CGS1 GS2 CS2CS1

Figure 3.6. A charge/discharge circuit. GX and CX are the unknown conductance and capacitance of the sample under test, and GREF and CREF are the reference conductance and capacitance respectively. GS1, GS2, CS1, and CS2 are the stray conductance and capacitance due to the sensor substrate and the connecting wires. CP12 is the parasitic capacitance of the switches S1 and S2, and CP34 is the parasitic capacitance of the switches of S3 and S4.

S1

S2

S3

S4

On Off

Charge Discharge

Figure 3.7. The timing diagram for the charge/discharge circuit.

Page 42: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

29

3.6 Off-the-shelf Impedance Sensing Chips

3.6.1 Analog Devices AD7745 – 7747 capacitance meter

Analog Devices released a series of single chip solutions for measuring capacitances. The

AD7745 single chip capacitance meter has an accuracy of 4 fF for floating (two-terminal)

capacitance measurements over a dynamic range of 4 pF, and can reject parasitic

capacitances to ground up to 60 pF. This device uses a 32 kHz square-wave excitation, a

second order sigma-delta modulator or charge balancing modulator, and a third order

digital filter. The maximum sampling rate is 90 Hz. A multiplexed two channel device,

the AD7746, is also available from Analog Devices. The AD7747, which is currently

only being sampled, is a single channel capacitance meter like the AD7745, however, the

capacitance being measured can be referenced to ground. The AD7747 also provides a

shield signal to drive the shield conductors to eliminate stray capacitance from cable-

shielding.

3.6.2 Analog Devices AD5933 impedance converter

The AD5933 is a single channel 1 mega-sample-per-second, 12-bit complex impedance

analyzer, operating over a range of 1 to 100 kHz, and can measure impedances between

100 Ohms to 10 MΩ at 0.5% precsion. Impedances are measured by switching into one

of the six modes to measure impedance over a set range, e.g. 100 Ohms to 1000 Ohms.

Frequency resolution is 0.1 Hz and 511 distinct frequencies can be used to measure the

impedance between 1 kHz and 100 kHz during a single sweep. The device consists of a

precise function generator, a programmable gain amplifier, a low-pass filter, a windowing

function, and a 1024 point discrete Fourier transform. As a point of reference, a

capacitance of 16 pF at 1 kHz would be measured as a reactance of approximately 10

MΩ, and at 100 kHz the 16 pF capacitance would be measured as a reactance of

approximately 100 kΩ. The real and imaginary parts of the complex impedance are

stored into separate registers which are then transferred via the I2C bus off the chip. The

frequency sweep feature offers the ability to determine resonant frequency shifts due to a

changes in an RLC network element. Analog Devices also has a single channel 250 kSPS

Page 43: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

30

12-Bit complex impedance analyzer that does not have an internal oscillator, but has

many of the same characteristics as the AD5933, except for a quadrupled sampling

period, 4 ms instead of 1 ms for the AD5933.

3.6.3 Motorola MC33794 electric field imaging device

The Motorola MC33794 Electric Field Imaging Device is a single-chip implementation

that can interface with up to 9 sensors in an array. It was originally developed for

passenger size detection in the case of vehicular air-bag deployment. The device is

ideally suited for capacitances ranging from 10 pF to 100 pF. The device outputs two

signals: a buffered version of the AC signal at the electrode and a DC level indicating the

amplitude of that signal.

With a built-in multiplexer, the device allows the selection and measurement of one of its

nine sensor electrodes, simultaneously grounding all the rest. When an electrode is

selected, the sensor interface topology is that of a voltage divider, where the known

impedance is a 22 kΩ resistor connected to a 5 V p-p 120 kHz sinusoidal voltage source,

as shown in Figure 3.8. The sensed capacitance is that between the selected electrode and

the ground terminals. To eliminate the stray capacitance from the cable shielding, the

shielding is actively driven by the measured signal through a buffer operational amplifier.

The signal from the electrode is also fed into a rectifier followed by a low pass filter so its

amplitude can be determined. This value is then output from the device as a DC voltage,

which varies inversely with capacitance. The internal reference resistance was selected

such that the capacitance values within the range of 10 pF to 100 pF will give a nearly

linear output. For digital processing, this output must be fed to an A/D converter, like

those available in many microcontrollers. Since the output is a DC value, it requires

significantly less processing overhead than reading the AC signal directly from the

electrodes. When connected to a 10 bit A/D converter, a measurement resolution of 0.1

pF is possible.

Because of its design for automotive use, the MC33794 implements many features that

are automotive-specific, including an ISO-9141 to microcontroller translator and an

Page 44: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

31

indicator lamp driver/sensor. In most cases these can and will be left unused. However,

one benefit of its original purpose is that while the device itself requires a 12 V source, it

includes a 5 V regulated output to drive external support circuitry, such as a

microcontroller. In summary, the MC33794 is small and suitable for single frequency

imaging applications. It is best for measuring capacitances ranging from 10 pF to 100 pF

with a resolution around 0.1 pF.

5 V AC

22 K

100 pF

Figure 3.8. A voltage-divider capacitance sensing circuit.

3.7 MOSEFT Switch Charge Injection

The problem of charge injection of MOS switches has been treated extensively in

literature. When the reset switch is active, a conduction channel extends from the source

to the drain of the transistor. When the gate voltage decreases, mobile carriers exit

through both the drain and the source end. The amount of channel charge that is injected

into the input depends on several factors, such as slope of the transient and the

input/output capacitance ratio. The problem can be generally neglected, but if the amount

of channel charge is comparable to the charge amplifier sensitivity, great care has to be

taken to avoid spurious injection of charge into the input.

3.8 Excitation

Excitation waveforms are chosen based on the desired set of excitation frequencies and

the signal to noise ratio (SNR) requirement at each frequency. To achieve a good SNR,

the total energy of the excitation signal needs to be sufficiently high, which requires

Page 45: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

32

either greater amplitude or longer duration for the waveform. The trade-offs are that high

amplitude causes non-linearity, and longer signal duration affects the speed of

measurements. Several possible choices of excitation waveforms are considered below.

3.8.1 Impulse function

An impulse function contains spectral content at all frequencies; therefore, the frequency

characteristics of the entire spectrum of the system under test can be measured

instantaneously.

Since the duration of an impulse function is very short, the amplitude has to be large so

that the signal power is high enough to achieve a sufficient SNR. High amplitude in the

input waveform is hard to accommodate due to non-linearity. Another disadvantage is

that signal energy at the undesired frequencies is wasted.

3.8.2 Step function

Like the impulse function, the step function has spectral content at all frequencies.

However, the excitation energy is spread over the entire duration of the waveform, which

reduces the amplitude required to achieve the same SNR when compared with an impulse

function. On the other hand, unlike the flat spectrum of an impulse, step functions carry

little energy at high frequencies, which makes them unsuitable for cases when high

frequency information is required.

3.8.3 Random noise

Random noise signals also spread the excitation energy over the entire duration of the

waveform. Their spectra can be tailored to match the requirements of the specific

application. The disadvantage is that, due to its randomness, the excitation waveform has

to be sampled in addition to the output waveform, which generates significant overhead

for the analog filters and the digital computation.

3.8.4 Pseudo-random noise

To avoid sampling the excitation waveform, a pseudo-random noise signal can be used

Page 46: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

33

instead of random noise, because pseudo-random signals are deterministic. The downside

is that the extraction of the frequency response of the system requires more computation

than the alternatives described below.

3.8.5 Frequency sweeps

Sequential measurements at frequencies of interest allows for straightforward analysis.

However, it is time consuming, and the transition from one excitation frequency to the

next causes transient that affect the following measurements.

3.8.6 A sum of sinusoids at frequencies of interest

In this case, the excitation energy is exactly matched to the frequency information desired

and the generation of the signal is straightforward. The measurement is faster than the

sequential sinusoid technique and the applied signal does not contain transients from the

transitions between successive single frequency sinusoids. In addition, system

nonlinearity can be checked by the observation of the response signals at frequencies

other than those contained in the excitation set.

3.9 Conclusions

Various aspects of interfacing circuit design for fringing electric field dielectrometry is

discussed in this chapter. Due to the high measurement sensitivity requirement of FEF

sensor applications, the noise floor of the interface circuits needs to be sufficiently

suppressed. Therefore, stray-immunity is one of the most crucial figures of merit for

these circuits. For spectroscopic applications, where the sample under test is evaluated

over a frequency band, the circuit topology optimal for that frequency band should be

used. For circuits interfacing with sensor arrays in imaging applications, parasitics due to

multiplexing need to be carefully addressed.

The future trend is to integrate the interface circuit and the controller with the sensor

electrodes on a silicon-based platform. The planar geometry of FEF sensors facilitates

easy integration into a CMOS process. The sensor electrodes can be placed at the top

metal layers, while the control and measurement circuitry are placed underneath. The

Page 47: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

34

highly-developed and well-controlled CMOS processes can facilitate mass production of

circuits with high precision at low cost.

Page 48: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

35

Chapter 4. Design Principle of Multi-channel FEF Sensors

4.1 Introduction

Multi-channel fringing electric field (FEF) sensors are widely used to measure material

properties as functions of position and time [60-62]. The design process of FEF sensors

and sensor arrays relies on a good understanding of the fundamental principles and

design trade-offs. The purpose of this chapter is to highlight the critical aspects of sensor

design principles and to illustrate the principles with numerical simulations and

experimental results. For imaging applications, the major goal of sensor design is to

achieve the optimum balance of measurement sensitivity, signal strength, imaging

resolution, and measurement speed. The finite area of sensor head makes it impossible to

achieve all design goals simultaneously. The task, therefore, is to consider the trade-offs

and determine the optimal combination of design variables for a given application.

Design variables include the geometry of electrodes and substrate, the choice of materials

for electrodes and substrate, the number of electrodes, and the arrangement of guard

electrodes. The optimization process can rely on either numerical simulations [60] or

analytical methods [63].

Finite element (FE) methods are used extensively for sensor modeling [64], optimization

[65], and performance evaluation [66], especially for structures that are difficult to model

analytically. The quality of the results from finite element methods depends on model

definition as well as mesh generation and refinement. When the right model and mesh are

chosen, FE simulations can generate results with high accuracy.

It is often difficult to construct an analytical model for a three-dimensional electrical

sensor. Analytical models based on conformal mapping were constructed for interdigital

structures in [49,67]. Such model was developed to evaluate the effects of design

parameters such as finger width, substrate thickness, and metallization ratio for thin film

interdigital FEF sensors [49]. The model generated solutions that match closely with

Page 49: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

36

experimental data and FEM simulation results. In geometries where one of the three

dimensions can be considered infinite compared with the other two, a two-dimensional

model approximation can be used [50]. The effect of electric-field-bending on the

linearity of a capacitive position sensor was studied based on an analytical model [68]. A

similar model was constructed for an interdigital FEF sensor designed to detect the

presence of water on a glass surface [5]. Based on analytical calculations, [5] investigated

the effect that electrode width and the width of the gap between the electrodes have on

sensor output. The validity of the analytical model was proven by matching results from

finite difference (FD) simulations. Both the analytical calculation and FD simulation

results showed a trade-off between measurement sensitivity and signal strength. The

paper did not address, however, the penetration depth of the sensor and how it is affected

by sensor geometry. Penetration depth is an important parameter in applications where

bulk measurements (as oppose to surface measurement) of the medium under test are

required.

Among all of the design variables, electrode geometry is the major determining factor for

sensor performance. Therefore, the choice of sensor geometry is critical to meeting the

requirements of an application. Sensors of various geometries were designed previously

for profiling and imaging applications. For example, a multi-segment interdigital FEF

sensor was used for multi-phase interface detection [69]; a multi-segment cylindrical

sensor was used to image continuous flows of materials inside a pipeline [70]; a helical

wound electrode sensor and a concave electrode sensor were developed for void fraction

measurements [71]. For applications where the sample can only be accessed from one

side, FEF sensors can be used. Such applications include, among others, online

measurement of moisture content in food products [72], pharmaceutical products [73],

and paper pulp [34], as well as cure state monitoring in the resin transfer molding process

[48,74].

Aside from sensor geometry, sensor output also depends on the sample of interest. The

optimal design, therefore, is application dependent. The current chapter focuses on the

qualitative effect of design parameters on sensor performance for samples with low

permittivity (< 10) and low conductivity. Design of capacitance tomography sensors for

Page 50: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

37

media with high dielectric permittivity is investigated in [69]. In paper [69], the sensor

was used to measure the media flowing in the pipe through an insulating wall. Simulation

was conducted to determine the effect of wall thickness on sensor output. Although the

simulation results apply only to tomography sensors of similar geometry, [69] provides

insights on how the permittivity of the medium under test affects the performance of

capacitive sensors in general.

The performance of FEF sensors is typically evaluated based on their penetration depth,

signal strength, measurement sensitivity, and linearity. All of these factors depend on

sensor geometry. The effect of electrode geometry on the performance of interdigital FEF

sensors was analyzed in [75], but not in the context of imaging applications. In this

chapter, we provide generalized design principles for multi-channel FEF sensors with a

focus on imaging applications. Most of the principles and results presented here can be

applied to designing multi-channel imaging sensors of other types as well.

The first part of this chapter focuses on the qualitative effect that design variables have

on sensor performance. The second part of the chapter illustrates the method of

simulation-based design optimization through the example of two multi-channel

concentric sensors. The qualitative analysis from the first part provides intuitive design

guidelines for the optimization process shown in the second part of the chapter.

4.2 Figures of Merit

Penetration depth, measurement sensitivity, dynamic range, signal strength, and noise

tolerance are the figures of merit usually used to evaluate the performance of multi-

channel FEF sensors. For imaging applications, imaging resolution and speed are also

considered. All these figures of merit are analyzed in detail in this section.

4.2.1 Penetration depth

Penetration depth is a measure of how quickly the electric field intensity decreases as the

distance from the plane of sensor electrodes increases. There is no strict definition of

penetration depth for FEF sensors. One way to evaluate the effective penetration depth is

to position a sample above the sensor head, move it away from the sensor surface, and

Page 51: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

38

measure the terminal capacitance at each position. Penetration depth γ3% corresponds to

the position z where the difference between the capacitance at that position C(z = γ3%)

and the asymptotic capacitance C(z = ∞) equals to 3% of the difference between the

highest and the lowest values of the terminal impedance [76]. This method is illustrated

in (4.1) and Figure 4.1, where C(z = ∞) represents the sensor terminal capacitance when

the sensor is in direct contact with the sample.

3%( ) ( )100% 3%

( 0) ( )C z C z

C z C zγ= − = ∞

× == − = ∞

(4.1)

Figure 4.1. Evaluation of the effective penetration depth γ3% of an FEF sensor

For an interdigital sensor with a 50% metallization ratio (the ratio of the area of the

electrodes to the total area of the sensor surface), penetration depth γ3% is roughly one

third of its spatial wavelength λ [77]. Spatial wavelength is defined here as the distance

between the centerlines of neighboring electrodes of the same type (e.g. driving or

sensing electrodes). Figure 4.2 shows the cross-sectional view of an interdigital sensor

with electrodes extending into the plane of the paper. In Figure 4.2, the parameters l1, l2,

and l3 represent three different ways of connecting the electrodes. The letter “D”

represents the driving electrodes, “S” represents the sensing electrodes, and “G”

represents the guard electrodes. The function of driving, sensing, and guard electrodes

and their use in different electrode configurations are described in detail in [78]. In the

table below the cross-sectional view of the sensor in Figure 4.2, each row corresponds to

Page 52: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

39

one of the three connection schemes; each column corresponds to the types of connection

used in the different connection schemes for the electrode directly above the column. For

the l1 scheme, an ac voltage signal is applied to every other electrode and the

current/voltage at the rest of the electrodes is measured. For connection schemes l2 and

l3, several fingers are chosen as guard electrodes and the current or voltage at only the

sensing electrodes is measured. The guard electrodes are either connected to ground or

kept at the same voltage potential as the sensing electrodes through unity-gain buffer

amplifiers. By using different connection schemes, the spatial wavelength of the sensor is

increased (λ3 > λ2 > λ1). As a result, sensor penetration depth is also increased. The

variable sensor penetration depth obtained from the different connection schemes

provides the sensor with access to different layers of the test specimen.

Figure 4.2. Cross-sectional view of a fringing electric field sensor with multiple

penetration depth excitation patterns.

4.2.2 Measurement sensitivity

Measurement sensitivity is defined as the ratio between the change in sensor output and

the change in the measured physical parameter of the sample. Because the electric field

of FEF sensors is non-uniform, their measurement sensitivity is position-dependent. As

illustrated in Figure 4.1, sensitivity decreases exponentially with increasing distance from

the plane of electrodes.

Measurement sensitivity also depends on the area of electrodes. For a fixed spatial

wavelength, greater electrode area means higher measurement sensitivity to changes in

Page 53: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

40

the sample under test. In the case of multi-channel sensors, however, increasing the

electrode area will decrease the amount of measurement channels, if the spatial

wavelength for each channel is fixed.

4.2.3 The output dynamic range

The output dynamic range of a sensor is defined as the ratio of the largest to the smallest

sensor output (terminal impedance) [79]. Its value depends on both the sensor geometry

and the sample under test, and it should lie within the input range of the interface circuit.

An impedance divider circuit can take inputs of any value, because its output is always

bounded. However, this circuit is non-linear and its measurement sensitivity is

maximized only when the load and reference impedance are matched. For virtual ground

integrator circuits, adjustable gain is sometimes used to ensure linearity [80].

4.2.4 Signal strength

FEF sensors are generally made of metal strips and the capacitance between the adjacent

two strips is relatively small. This leads to low signal strength. To increase signal

strength, sensors with interdigitated periodical structures can be built. Signal strength is

improved here through adding more ‘fingers’ to a sensor.

The signal strength of an FEF sensor changes exponentially with its distance to the

sample. For capacitive measurements, if the dielectric permittivity of the sample is higher

than that of the medium, the signal strength decays with the increasing distance to the

sample. If the sensor is immersed in a medium that has finite conductivity, its signal

strength can either increase or decrease depending on the dielectric properties of the

medium and the sample.

4.2.5 Noise tolerance

Guard electrodes are usually used to shield sensing electrodes from noise. They can take

the form of a guard ring surrounding the active sensor electrodes (driving and sensing

electrodes), the guard plane beneath the sensor substrate, or a three-dimensional shield

around the sensing area. They need to be positioned properly for optimal sensor

Page 54: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

41

performance. They should also be carefully connected to avoid stray capacitances and

ground loops. The driven-guard technique, where the guard electrodes are kept at the

same voltage potential as the sensing electrodes, is used to remove or reduce any stray

capacitances from the guard electrodes [81].

4.2.6 Imaging resolution

A straightforward approach to produce an image of a physical parameter of a sample is to

let each measurement channel of the sensor correspond to one pixel in the image. The

method has the limitation that the number of channels has to be the same as the number

of desired pixels. To generate an image with high resolution, a large number of

measurement channels is required, which is often difficult to implement. Tomography

imaging, on the other hand, reconstructs images by interpolating measurements from

different channels, and the number of pixels from such interpolation can be much greater

than the number of measurement channels. However, in tomography, it is still desirable

to have as many measurement channels as possible, because the degree of ill-posedness

in image reconstruction can be reduced by increasing the ratio of the number of

independent measurements to the number of output pixels [82].

For a sensor of fixed size, increasing the number of electrodes decreases the area of each

electrode, resulting in a reduced measurement sensitivity and signal strength. If sensor

output gets close to the minimum level measurable by the interface circuit, the resulting

measurement will lose accuracy. The maximum number of electrodes is therefore limited

by the measurement resolution and the noise floor of the interface circuit.

4.2.7 Imaging speed

The speed of imaging systems is important for real time measurement and control

applications. It depends on the total number of measurement channels, the efficiency of

the image reconstruction algorithm, and the frequency of the input driving signal. A

greater number of channels generate more data to process and require longer time for

image reconstruction. In image reconstruction, iterative algorithms are usually slower

than non-iterative ones, but they are more accurate [82]. When the algorithm is not the

Page 55: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

42

bottleneck, imaging speed depends mostly on the frequency of the driving signal, the

faster the imaging speed. The upper limit of operating frequency is determined by the

bandwidth of circuit elements (e.g. operational amplifiers), and by the bandwidth of the

DAQ card (when A/D conversion is performed directly on ac signals).

4.3 Major Design Concerns

4.3.1 Surface contact quality

FEF sensors are highly sensitive to the composition of the volume in the immediate

vicinity of the electrodes. The smaller the spatial wavelength of the sensor, the more

pronounced is this effect. For applications involving contact measurements of solid

samples, surface contact quality between the sample and the sensor is a major source of

uncertainty. Air gaps between the sample and the electrode act as a series capacitance

with the impedance of the sample and lead to inaccurate estimate of sample impedances.

This air capacitance is difficult to determine because its value depends on the surface

roughness of the sample and the electrodes.

To improve sensor-sample contact quality, silver paint can be applied directly to the

specimen as electrodes for macro-scale samples. It conforms to the surfaces of samples,

reducing or eliminating air gaps. However, silver paint electrodes are difficult to pattern

with high resolution and difficult to remove afterwards. Another option for improving the

contact quality is the liquid immersion technique, where the sensor and the sample are

immersed in a liquid that has dielectric properties similar to that of the solid sample under

test [83]. In clinical tomography applications, saline gels are applied to patients’ skin to

improve contact with electrodes [84].

When the sensor and the sample are not in contact, its measurements are much less

sensitive to the surface roughness of the electrode and the sample. However, for micro-

sensors (spatial wavelength from 1 μm to 100 μm), it is important to keep the sensor

surface clean, so that the dust particles and other contaminants do not alter the sensor

output.

Page 56: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

43

4.3.2 Sensor substrate and the geometry of the back plane

The distance between the backplane and the driving electrode depends on the substrate

thickness of the sensor. When the backplane is close to the driving electrodes, it affects

the field distribution pattern, thus influencing the penetration depth and signal strength.

Proper positioning and geometry design of the backplane are critical for optimizing

sensor performance. The effect of substrate thickness on sensor output characteristics is

illustrated with the example of two concentric FEF sensors in Section V.

4.3.3 Cross-talk between difference measurement channels

In general, the closer are individual sensing cells the stronger is the cross-talk between

the corresponding channels. It is therefore desirable to position the sensing cells as far

apart as possible. Cross-talk can also be reduced by inserting shielding electrodes

between neighboring sensing cells. Both of these methods, however, reduce the total

surface area of active electrodes, which in turn reduces measurement sensitivity and

signal strength.

4.4 Major Design Trade-offs

In imaging applications, electrode surface area is limited by the size of the sample. This

makes different output characteristics dependent on each other. Many trade-offs,

therefore, are present in the design process.

4.4.1 The number of channels vs. penetration depth and

measurement sensitivity

For an FEF sensor of a fixed size, increasing the number of measurement channels

decreases the gap between neighboring channels, a change that reduces sensor

penetration depth and causes stronger cross-talk. In addition, the reduced electrode

surface area for each channel results in a drop in measurement sensitivity. A secondary

effect on measurement sensitivity is caused indirectly by the decrease in penetration

depth: at smaller penetration depth, the sensor field energy is much more concentrated

Page 57: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

44

around the sensor electrodes, thus making its output less sensitive to variations in the

sample. These trade-offs limit the number of channels that a FEF sensor can have.

4.4.2 Imaging resolution vs. measurement sensitivity and imaging

speed

Using a larger number of smaller electrodes improves imaging resolution, but leads to

two disadvantages: increased number of measurement channels reduces imaging speed;

smaller size of electrodes reduces measurement sensitivity. The loss in speed and

sensitivity can be compensated by, respectively, higher measurement sensitivity of the

interface circuit and higher system operating frequency. High operating frequency

requires, in turn, the interface circuit to have a sufficient bandwidth. Examples of circuits

with high sensitivity and bandwidth are provided in [80,85].

4.5 Examples of Sensor Designs

Two concentric FEF sensor designs are presented here to illustrate the qualitative design

principles described in the previous sections. Figure 4.3 shows a concentric sensor

designed for measuring moisture content in dough [48]. The rationale for using this type

of sensors in food manufacturing is available in [48]. The electrodes (black in the figure)

were patterned on an insulating substrate (white in the figure). The sensor is configured

as a two-channel FEF sensor, where the middle ring is used as the driving electrode and

the other two electrodes are used as the sensing electrodes. Each sensing electrode needs

individual guarding electrodes (the electrodes beneath the substrate) if the open voltage

measurement scheme is to be used. The readers who need understanding of different

measurement schemes used for this type of sensors are referred to [86].

Page 58: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

45

Figure 4.3. Top-down view of a concentric fringing electric field sensor head. The figures were drawn to scale. The center electrode is 4 mm in diameter as marked.

The Laplace equation of the concentric FEF sensor has the following solution:

( )0 1 2( , ) ( ) z zr z J r c e c eβ βφ β − += +

(4.2)

where β denotes electric potential, r refers to the radial coordinate on the horizontal

plane, z corresponds to the vertical coordinate, J0 is the zero order Bessel function of the

first kind, and β is a scaling constant such that βr is one of the zeros of J0 [65].

The sensor has a spatial wavelength of 8 mm, which corresponds to a penetration depth

of about 2.5 mm, a value insufficient for measuring a broad variety of food products. To

increase the penetration depth, shielding electrodes are added between the driving and the

sensing electrodes, and are kept at the same voltage as their neighboring sensing

electrode. The improved design is shown in Figure 4.4. Figure 4.5 illustrates the effect of

the added shielding electrodes on the penetration depth of the sensor. Without the

shielding electrodes, the backplane draws electric field down toward itself. The shielding

electrodes counteract this effect by pushing the electric field lines upward, which

effectively increases the penetration depth of the sensor. The simulation results were

generated from the FEMLAB software package.

Page 59: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

46

Figure 4.4. Top-down view of a concentric fringing field sensor head with additional shielding electrodes between the driving and the sensing electrodes. The figures were drawn to scale. The center electrode is 3 mm is diameter.

Page 60: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

47

(a)

(b)

Figure 4.5. Simulated electric field line distribution illustrating the effect of the additional shielding electrode. (a) The electric field line distribution of the geometry shown in Figure 4.3. (b) The electric field line distribution of the geometry shown in Figure 4.4.

Page 61: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

48

4.5.1 Finite element analysis

To compare the performance of the two designs, the software package Maxwell 2D

simulator by Ansoft Corp. was used for finite element (FE) simulations. Figure 4.6 and

Figure 4.7 show the layout of the simulation spaces. These spaces were defined in radial

coordinates, with the origin placed at the lower left corner of the simulation space. The

driving electrode is set to 6 volts and all other electrodes (including the backplane) are set

to 0 volts, a Dirichlet boundary condition in nature. A test sample with relative dielectric

permittivity εr = 5.0 and conductivity σ = 0 is positioned above the sensor. FR4 epoxy

with relative dielectric permittivity εr = 4.4 and conductivity σ = 0 is used for the

substrate of the sensor. The boundary of the simulation space is set as a “charge balloon.”

A charge balloon models an electrically insulated system, where the charge at infinity

balances the charge within the simulation space forcing the net charge to be zero. The

convergence criterion for total energy error is set to be within 1%. The equipotential plots

for the two concentric designs are shown in Figure 4.8 and Figure 4.9. In the simulation,

the distance of the sample to the plane of sensor electrodes is varied from 15 mm to 0

mm. The signal strength for each sensor is evaluated based on its absolute terminal

capacitance, while the penetration depth γ3% is evaluated based on normalized terminal

capacitance calculations.

Figure 4.6. Layout of a test sample positioned above the unshielded concentric FEF

sensor in the finite element simulation.

Page 62: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

49

5.0

Figure 4.7. Layout of a test sample positioned above the shielded concentric FEF

sensor in the finite element simulation.

Figure 4.8. Simulated equipotential plot of the unshielded concentric FEF sensor.

Page 63: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

50

Figure 4.9. Simulated equipotential plot of the shielded concentric FEF sensor.

4.5.2 The effect of the shielding electrode

Figure 4.10 and Figure 4.11 show respectively the absolute and normalized terminal

capacitance values obtained from the simulation. “Sensor 1” refers to the design without

the shielding electrodes (Figure 4.3) and “Sensor 2” refers to the design with the

shielding electrodes (Figure 4.4). For both designs, the outer channel has greater signal

strength than its respective inner channel, a difference caused by the larger sensing area

of the outer channel. When the performance of the two designs is compared, the second

design does provide greater penetration depth than the first one. This gain in penetration

depth, however, is obtained at the cost of reduced signal strength, as shown in Figure

4.10.

Page 64: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

51

Figure 4.10. Absolute capacitance value from both sensor designs in the FE

simulation. Absolute capacitance is used here as a metric to evaluate the measurement sensitivity of the sensors. The results indicate that the original sensor design (sensor1) has higher measurement sensitivity than the shielded design (sensor2).

Figure 4.11. Normalized capacitance value from both sensor designs in the FE

simulation. Normalized capacitance is used here as a metric to evaluate the penetration depth of the sensors. The results indicate that the addition of the shielding electrodes increase the penetration depth of the shielded sensor (sensor2).

Page 65: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

52

4.5.3 The effect of the width of the shielding electrode

The width of the shielding electrodes is varied in the second design to evaluate its effect

on sensor output characteristics. Figure 4.12 and Figure 4.13 show respectively the

absolute and normalized capacitance value of the shielded sensor when the width of the

shielding electrode is varied.

(a)

(b)

Figure 4.12. The effect of change in shielding electrode width on the signal strength of the (a) inner sensing channel and (b) outer sensing channel of the shielded sensor. The results show that the sensor signal strength decreases with increasing width of the shielding electrodes.

Page 66: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

53

(a)

(b)

Figure 4.13. The effect of change in shielding electrode width on the penetration depths of the (a) inner sensing channel and (b) outer sensing channel of the shielded sensor. The results show that the sensor penetration depth increases with increasing width of the shielding electrodes.

The same trend exists for the capacitance value from both the inner and the outer sensing

channel: when the width of the shielding electrodes increases, the sensor signal strength

drops and its penetration depth increases. The trend can be explained with the help of

Figure 4.1 (a). Wider shielding electrode diverts electric field energy away from the

sensing electrodes, thus decreasing the signal strength; on the other hand, the field lines

are pushed further up due to the increased surface area of the shielding electrodes, which

increases the penetration depth. The simulation results presented above are summarized

Page 67: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

54

in Table 4.1..

Table 4.1.The effect of increasing shielding electrode width on the performance of the shielded FEF sensor.

Inner2 Outer2

Penetration depth ↑ ↑

Signal strength ↓ ↓

4.5.4 The effect of substrate thickness

As illustrated in Figure 4.5, the sensor backplane draws electric field energy away from

the sensing electrodes. The closer the backplane is to the driving electrode, the more

energy is drawn away. The distance between the driving electrode and the backplane is

determined by the thickness of the substrate. The effect of substrate thickness variation is

therefore important.

The thickness of the sensor substrate is varied from 100% to 25% of its original value in

a series of FE simulations. Figure 4.14 shows the absolute capacitance value from the

inner channel of the unshielded design. The results show that the closer the backplane is

to the driving electrode, the weaker is the signal strength. This same trend exists for the

capacitance value from both channels of the two designs.

In addition to the signal strength, penetration depth is also affected by change in substrate

thickness. The results are shown in Table 4.2 and Figure 4.15. The penetration depth of

the first design decreases with increasing substrate thickness. This can again be explained

with the illustration in Figure 4.1. The farther away the backplane is positioned from the

driving electrode, the further down the electric field lines are drawn away from the top

electrodes, resulting in a decreased penetration depth. Penetration depth for the second

design is relatively stable against variation in substrate thickness because of the shielding

electrodes. There again exits a trade-off between the penetration depth and signal

strength: for greater signal strength, a thicker substrate is desirable, but this decreases the

penetration depth of the sensor. The simulation results are summarized in Table 4.3.

The sensitivity of the sensor terminal measurement to the changes in the substrate

Page 68: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

55

thickness depends on the ratio of the dielectric permittivity of the sample and that of the

sensor substrate. For samples with a much higher dielectric permittivity than the

permittivity of the substrate, variation in substrate thickness will not affect the sensor

performance as much.

Figure 4.14. Absolute capacitance value of the inner channel of the unshielded sensor with different substrate thickness. The results indicate that increasing the substrate thickness improves the measurement sensitivity of the sensor.

Figure 4.15. The effect of change in substrate thickness on sensor penetration depth.

Page 69: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

56

Table 4.2. Penetration depths (mm) of the concentric sensor designs with varying substrate thickness d.

d Inner1 Outer1 Inner2 Outer2 25% 2.78 3.91 3.06 4.63 50% 2.67 3.77 3.04 4.69 75% 2.54 3.67 3.09 4.66

100% 2.47 3.57 3.10 4.72

Table 4.3. The effect of increasing substrate thickness on the performance of the two FEF sensors.

Inner1 Outer1 Inner2 Outer2

Penetration depth ↓ ↓ ↑ ↑

Signal strength ↑ ↑ ↑ ↑

4.5.5 Limitation of simulation results

It is worthy to note that the optimization results presented in this chapter are application-

dependent. The optimal sensor geometry changes with respect to different samples. In the

simulations of this chapter, samples with low permittivity (< 10) and close to zero

conductivity were used. Such samples are representative for a wide range of ceramics and

plastics [64]. Design of sensors specialized for high permittivity dielectrics (10 < εr < 80)

were discussed in [34]. For highly conductive samples, resistance, instead of

capacitance, is measured to estimate sample concentration or distribution within the

sensing zone. In cases where the sample has complex permittivity and displays

frequency-dependent behavior, both the real part and the imaginary part of the complex

impedance have to be measured.

The multi-channel impedance sensors presented in this chapter are designed for imaging

applications. Electrical imaging systems typically operate in the megahertz range.

Therefore, the electrostatic model used in the FE simulations is adequate. For sensors

used in broad-band spectroscopic systems, AC simulations are necessary. Such systems

are usually used for lab-based determination of material properties of samples with

complex permittivity.

Page 70: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

57

4.6 Conclusion

This chapter presents the design principles for multi-channel FEF sensors, with a special

focus on the analysis of figures of merit and the major trade-offs caused by various

design constraints. The effect of design variables, especially sensor geometry, on sensor

performance is analyzed. These qualitative guidelines help to understand the logic behind

the simulation-based design procedures used for the two concentric FEF sensors. The

performance of the two sensors is compared. The shielding electrodes added in the

second design were shown to increase the penetration depth of the sensor. In addition, the

effects of substrate thickness and shielding electrode width were evaluated. The

simulation results demonstrated the effects of sensor geometry on its performance and

provided insights into the design process of multi-channel FEF sensors.

Page 71: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

58

Chapter 5. Non-dimensionalized Parametric Modeling of FEF Sensors

5.1 Introduction

Fringing electric field (FEF) sensors are difficult to model analytically due to their

inherently nonlinear characteristics. Analytical models for FEF sensors are usually based

on simplified geometries and idealized assumptions, which limits their accuracy for real

world applications. For example, ideal electrodes with zero thickness are assumed in

closed-form solutions based on conformal mapping [64,65] and the continuum model

[29]. This assumption is only valid when the electrode thickness is small compared with

the spatial wavelength of the sensor [34]. Therefore, analytical models that assume

infinitesimally thin electrodes do not work well for small FEF sensors with thick

electrodes. The non-idealities of FEF sensors, such as finite finger length, finite electrode

thickness, and the non-uniform electrode surface are analyzed in [34].

Due to this lack of analytical models, FEF sensor design relies heavily on numerical

simulations. Among all numerical methods, the finite element method (FEM) is most

frequently used for FEF sensor design. At low frequency, the sensor is small compared to

the wavelength of the propagating electromagnetic wave. In such cases, electrostatic or

quasi-electrostatic simulations can be used. For sensors with uniform structures along one

dimension, a 2D simulation is sufficient. When none of the above conditions are satisfied,

a full-wave 3D simulation is required for modeling accuracy. A qualitative analysis on

multi-channel FEF sensor design is presented in [1] using 2D electrostatic simulations.

FEM modeling involves a trade-off between run time and accuracy: higher accuracy

requirement demands longer run time, and lower run time reduces modeling accuracy. A

non-parametric model based on artificial neural networks (ANN) for interdigital

capacitors is presented in [87]. To construct an accurate ANN model, a large amount of

simulation is required. Therefore, although the computation time of the ANN model

(after the model is determined) is negligible, the overall modeling throughput is not

Page 72: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

59

reduced.

This chapter presents a parametric modeling method that can predict the output of a wide

range of FEF sensors. The model parameters are determined by polynomial fitting of

prior FEM simulation results. The simulation results were non-dimensionalized to make

the models applicable for FEF sensors with a wide range of dimensions and choice of

substrate materials. Two types of FEF sensors, interdigital sensors and concentric FEF

sensors, are considered here as examples to illustrate the non-dimensionalized modeling

method. Parametric models determined by this method demonstrate high accuracy when

compared to FEM simulation results, while greatly reducing computation time. These

models facilitate fast optimization of sensor design and quick validation of experimental

results.

5.2 Simulation Setup

Figure 5.1 shows a concentric FEF sensor designed for measuring round samples. FEF

sensors of such geometry can also be used when the orientation of the electrode matters,

as in the case of anisotropic samples [18]. The concentric FEF sensor was simulated

using the Ansoft Maxwell 2D software package. Figure 5.2 shows the simulation setup.

The left edge of the simulation space in Figure 5.2 represents the axis of symmetry in the

R-Z plane. The sensor has one driving electrode (drive), two sensing electrodes (sense1

and sense2), a guard electrode above the substrate, and several backplanes. Separate

backplanes are used here because they are each driven by a buffer operational amplifier

to stay in the same voltage as the sensing electrode immediately above. Such a

connection scheme is used to eliminate parasitic capacitance due to the backplanes and

sensing electrodes. A detailed discussion on the geometry of the backplane is presented

later in the chapter.

Page 73: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

60

Figure 5.1. A concentric FEF sensor and a signal conditioning circuit designed for

non-invasive imaging of round samples.

Figure 5.2. Simulation setup of a concentric FEF sensor in the R-Z plane. The left

edge of the simulation space represents the axis of symmetry.

The geometry and dimensions of this sensor were chosen to balance optimal performance

and the simplicity of the design. For an FEF sensor of a fixed size, a trade-off exists

between its penetration depth and measurement sensitivity [3]. Increasing electrode width

improves the measurement sensitivity of the sensor, but reduces its penetration depth. In

the present chapter, the sensors are assumed to have 50% metallization ratio, that is, the

active electrodes (sensing and driving) and the gap between each of them have the same

width. This design is chosen to achieve a balance between penetration depth and

sensitivity. The radius of the sensor is 30 mm. All the electrodes are 0.08 mm thick. The

sensing and driving electrodes are 4 mm wide. The electrodes and backplanes are copper

and the substrate is a dielectric with a relative dielectric permittivity of 10. The relative

dielectric permittivity of the medium under test (MUT) εm varies from 4 to 100 and the

substrate thickness of the sensor d varies from 0.1 mm to 2.5 mm in the simulations.

Page 74: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

61

The following boundary conditions are used for the simulation. All electrodes except for

the drive are set to 0 V; drive is set to 6 V. The boundary of the simulation space is set to

be a charge balloon. The balloon models an electrically insulated space, where the charge

at the infinity balances the internal charges. The simulation was electrostatic, which is

adequate for the low operating frequency of the sensing system.

5.3 Simulation Results

5.3.1 Effect of substrate thickness

Figure 5.3 (a) and (b) show respectively the electric field distribution for a sensor with a

thin substrate (d = 0.1 mm) and a sensor with a thick substrate (d = 2.5 mm). Variations

in the substrate thickness of the sensor have two effects. A thinner substrate causes more

field energy to leak through the gap in the backplane. In the simulation setup used in this

chapter Figure 5.2, the sensor is surrounded by the MUT and the effect of leakage field

on sensor output is minimal. Also, thinner substrates decrease the distance between drive

and the backplane, leading to more rapid decay of the electric field. Reduced substrate

thickness results in weaker signal strength (terminal impedance measurements), but

greater penetration depth [3,4].

5.3.2 Geometry of the backplanes

Separate backplane electrodes, instead of a solid backplane, are used for the sensor

shown in Figure 5.1. This geometry is chosen so that the effect of parasitic capacitances

between the sensing electrodes and backplanes can be eliminated through buffer

operational amplifiers. The widths of the gaps between the backplanes are optimized to

provide sufficient shielding while minimizing the leakage field between drive and the

backplanes.

Since the geometry of the backplanes used here is specific to the driven backplane

technique, we compare this geometry with the case of a solid backplane. Figure 5.4 (a)

and (b) show respectively the electric field distribution for a sensor with a thin substrate

(d = 0.1 mm) and a sensor with a thick substrate (d = 2.5 mm). Comparison of these

Page 75: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

62

figures with Figure 5.3 (a) and (b) shows that difference between the field distribution for

the split-backplane sensor and the solid-backplane sensor is more prominent when the

substrate is thin. This is because for smaller d, more field lines leaked between the gap of

the backplanes in the case of the split-backplane sensor.

(a) (b)

Figure 5.3. The electric field arrows and equipotential lines for concentric FEF sensors with substrate thickness of (a) d = 0.1 mm and (b) d = 2.5 mm, where separate backplanes are used.

5.4 Non-dimensionalization

The normalized electric field radiation pattern of an FEF sensor depends only on the ratio

of the dielectric permittivity of the MUT, εm, to that of the sensor substrate, εs, rather than

on their absolute values. Similarly, only the ratio of the spatial wavelength λ of the sensor

to its substrate thickness d affects the normalized radiation pattern, not their absolute

values. Such properties of FEF sensors justify the use of a non-dimensionalized model to

represent sensors of different sizes.

5.4.1 Concentric ring FEF sensors

Figure 5.5 shows the normalized capacitance between the drive electrode and sense1

electrode plotted against normalized substrate thickness d/λ and normalized dielectric

permittivity of the MUT εm/εs. After normalization, the surface plot is no longer limited to

a sensor with a fixed dimension or choice of substrates, and it can be used for model

Page 76: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

63

calibration.

(a) (b)

Figure 5.4. The electric field arrows and equipotential lines for concentric FEF sensors with substrate thickness of (a) d = 0.1 mm and (b) d = 2.5 mm, where a solid backplane is used.

Figure 5.5. Normalized capacitance between the drive electrode and sense1 plotted

against εm/εs and d/λ.

The capacitance data between other combinations of electrodes have similar trends, as

shown in Figure 5.6 and Figure 5.7 Due to the concentric geometry, the three electrodes

have different surface areas. Because of this variation in surface area, different

combinations of electrodes have different magnitude of capacitances.

Page 77: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

64

Figure 5.6. Normalized capacitance between sense1 and sense2 plotted against εm/εs

and d/λ.

Figure 5.7. Normalized capacitance between sense2 and drive plotted against εm/εs and d/λ

A similar parametric simulation was also conducted for concentric sensors with solid

backplanes. Figure 5.8 shows the normalized capacitance between drive and sense1 of

such sensors. By comparing the results from the split-backplane geometry Figure 5.5 and

those from the solid backplane geometry Figure 5.8, one can see slight differences when

the substrate is thick and large differences when it is thin.

Page 78: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

65

Figure 5.8. Normalized capacitance between the drive electrode and sense1 plotted

against εm/εs and d/λ for concentric sensors with solid backplanes.

5.4.1.1 Electrode pair sensitivity analysis

Figure 5.9 compares the three different pairs of electrodes in terms of their sensitivity to

changes in substrate thickness when the relative dielectric permittivity of the MUT εm is

kept constant at 52. The normalized plot was created by normalizing each value of

C/(λεs) by the minimum value of C/(λεs) (at d = 0.1 mm) as shown in (5.1).

min

%

min

100%s s

s increase

s

C CC

C

λε λελε

λε

⎛ ⎞− ⎜ ⎟

⎛ ⎞ ⎝ ⎠= ×⎜ ⎟⎛ ⎞⎝ ⎠⎜ ⎟⎝ ⎠

(5.1)

The sensitivity to substrate thickness is dependant on how much energy is absorbed from

an electrode pair by the backplanes. Figure 5.9 shows that the sense1-sense2 pair is least

sensitive to changes in substrate thickness. Sense1 and sense2 are separated by drive, and

drive is much closer to both of these electrodes than the backplanes are. Drive acts as a

shielding electrode and absorbs more energy from sense1 and sense2 than the backplanes

do and therefore the distance between the sensing electrodes and the backplanes has a

minimal effect on the capacitance between sense1 and sense2. Similarly, the sense2-

drive pair is less sensitive to substrate variation than the sense1-drive pair. The guard

electrode is in close proximity to the sense2 electrode, so it absorbs some of the energy

that would contribute to the capacitance seen between sense2 and drive. Therefore, the

Page 79: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

66

energy absorbed by the backplanes has a smaller effect.

Figure 5.10 compares the three different electrode pairs in terms of their sensitivity to

changes in dielectric permittivity when the substrate thickness is kept at a constant value

of 1.3 mm. This was done by normalizing C/(λεs) by its initial value (when εm = 4)

according to (5.1). Figure 5.10 show that the sensitivities of different pairs of electrodes

to variations in εm/ εs do not differ much.

Figure 5.9. Electrode pair sensitivity to changes in capacitance as a result of a

changing substrate thickness (εm = 52).

Figure 5.10. Electrode pair sensitivity to changes in capacitance due to changes in the

dielectric permittivity of the MUT (d = 1.3 mm).

5.4.1.2 Determination of polynomial coefficients

The calibration surfaces are fit to the model shown in (5.2), where x = d/λ and y = εm/εs.

The fitting coefficients aij are determined in Matlab and the results are shown in Table

5.3, Table 5.1 and Table 5.2.

Page 80: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

67

0,40,4

i jij

isj

C a x yλε =

=

= ∑ (5.2)

Figure 5.11 shows the residue from the polynomial fit. Within the simulation range, the

residue is shown to be less than 3% of the original simulation results.

Table 5.3. Polynomial coefficients aij for C1d / (λεs).

x4 x3 x2 x 1 y4 -6.436e0 1.940e2 -2.111e3 3.343e3 -1.382e3 y3 2.664e0 -7.847e1 8.267e2 -1.151e3 3.961e2 y2 -3.871e-1 1.106e1 -1.110e2 1.069e2 -1.626e1 y 2.120e-2 -5.798e-1 5.302e0 2.674e0 -1.353e0 1 -9.567e-5 1.859e-3 9.000e-3 2.225e-1 1.384e-2

Table 5.4. Polynomial coefficients aij for C12 / (λεs).

x4 x3 x2 x 1 y4 -7.385e-1 2.314e1 -2.645e2 3.011e2 -9.153e1 y3 3.090e-1 -9.441e0 1.042e2 -9.848e1 2.495e1 y2 -4.646e-2 1.370e0 -1.430e1 7.485e0 -7.787e-1 y 2.758e-3 -7.707e-2 7.249e-1 6.697e-1 -2.156e-1 1 -9.001e-6 1.470e-4 2.554e-3 6.295e-2 9.915e-4

Table 5.5. Polynomial coefficients aij for C2d / (λεs).

x4 x3 x2 X 1 y 4 -1.468e1 4.577e2 -5.132e3 7.698e3 -3.049e3 y3 6.170e0 -1.866e2 2.041e3 -2.631e3 8.510e2 y2 -9.143e-1 2.660e1 -2.715e2 2.353e2 -2.527e1 y 5.115e-2 -1.411e0 1.300e1 8.434e0 -4.019e0 1 -2.262e-4 4.246e-3 2.751e-2 7.129e-1 3.449e-2

Page 81: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

68

Figure 5.11. Fitting residue of the fourth-order polynomial model for C1d/λεs.

5.4.1.3 An example

A practical example is provided here to illustrate how the parametric model can be used.

Suppose a concentric FEF sensor has the geometry shown in Figure 5.1. The substrate is

made from Teflon (εs = 2.08) and it is 4.8 mm thick. The spatial wavelength of the sensor

is 32 mm. The MUT is castor oil (εm = 4.5).

The first step is to calculate the non-dimensionalized parameters d/λ and εm /εs.

/ 4.8 / 32 0.15d λ = = (5.3)

/ 4.5 / 2.08 2.1625m sε ε = = (5.4)

Then, estimate the normalized capacitances based on the coefficients in Table 5.3, Table

5.6 and Table 5.7.

412 3.443 10s

Cελ

−≈ × (5.5)

31 1.994 10d

s

Cελ

−≈ × (5.6)

32 5.402 10d

s

Cελ

−≈ × (5.7)

The capacitances are found to be:

Page 82: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

69

12 0.2029C ≈ pF (5.8)

1 1.1750dC ≈ pF (5.9)

2 3.1834dC ≈ pF (5.10)

5.4.1.4 Model evaluation

To check the validity of the parametric model, results from several test simulations were

compared with the estimated sensor output based on the model. In the test simulations,

the relative dielectric permittivity of the sensor substrate is varied while the spatial

wavelength of the sensor is kept the same as used in the original setup. Figure 5.12 shows

the residue of the estimates from the parametric model. The error is shown to be within

5%.

Figure 5.12. Comparison between finite element simulation results and results

estimated by the parametric model.

When the spatial wavelength of the sensor is varied, the sensor output is shown to scale

linearly with the size of the sensor provided that the electrodes are thin. This matches

well with the prediction of the parametric model. If the thickness of the electrodes is

comparable to the spatial wavelength of the sensor, the parasitic capacitances between the

vertical edges of the electrodes (due to the finite thickness of the electrodes) lead to

nonlinearity, and the sensor output no longer scales linearly with size.

Page 83: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

70

5.4.2 Interdigital FEF sensors

Figure 5.13 shows a typical half-wavelength cross-section of an interdigital FEF sensor,

where εm is the dielectric permittivity of material under test of infinite thickness, and εs is

the dielectric permittivity of the substrate. The substrate thickness d was varied from 20

μm to 2000 μm, in steps of 10 μm, while the relative permittivity of the material, εm was

varied from 4 to 100, in steps of 2. The total height of the simulated region was

maintained at 4000 μm. The permittivity of the substrate, εs, was kept at 10 to permit the

ratio εm/εs to include values above and below 1. Electrode thicknesses are 80 μm.

Capacitance between the drive and sense electrodes was determined as a function of

normalized substrate thickness, d/λ, and normalized dielectric constant, εm/εs as shown in

(5.11), where x = d/λ (substrate thickness/wavelength) and y = εm/εs (material dielectric

constant/ substrate dielectric constant). Table 5.8 shows the polynomial coefficients, aij,

for x = d/λ (substrate thickness divided by the wavelength), and y = εm/εs (material

dielectric constant divided by the substrate dielectric constant).

Figure 5.13. A half-wavelength portion of the interdigital sensor is shown. An

example of a triangular mesh used for computation of capacitance and conductance matrices associated with a half-wavelength section interdigital structure.

12

=0,4=0,4

= i jij

iSj

C a x yε ∑ (5.11)

Page 84: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

71

Table 5.8. Polynomial coefficients aij for C12 / εs.

x4 x3 x2 x 1 y 4 -8.043e-1 2.131e1 -1.885e2 1.066e2 4.542e1 y3 4.865e-1 -1.275e1 1.101e2 -2.736e1 -5.412e1 y2 -9.952e-2 2.559e0 -2.113e1 -1.020e1 2.009e1 y 7.158e-3 -1.763e-1 1.272e0 4.254e0 -1.960e0 1 -1.193e-5 -3.846e-4 2.281e-2 1.004e-1 2.012e-2

(a) (b)

Figure 5.14. (a) Finite element simulation results and (b) results estimated by the parametric model. A practical example is provided here to illustrate how the parametric model can be used.

Suppose an interdigitated FEF sensor has the geometry shown in Figure 5.13. The

substrate is made from Teflon (εs = 2.08) and it is 4.8 mm thick. The spatial wavelength

of the sensor is 32 mm. The MUT is castor oil (εm = 4.5). The non-dimensionalized

parameters d/λ and εm /εs are the same as calculated in (5.3) and (5.4).

Based on the coefficients in Table 5.8, the normalized capacitance is estimated.

12 1.090s

≈ (5.12)

The capacitance is found to be:

12 2.267C ≈ pF/m (5.13)

5.5 Conclusions

Parametric models are constructed for concentric FEF sensors and interdigital FEF

Page 85: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

72

sensors based on non-dimensionalized fitting of FEM simulation results. The models

enable direct estimation of the output of FEF sensors with a good modeling accuracy

(less than 5% error). The modeling method is not restricted to FEF sensors; its concept of

non-dimensionalization can be used for the design optimization of a wide variety of

sensors. For sensors that are difficult to model analytically, the method provides accuracy

comparable to numeric methods while greatly improves the throughput of design

optimization. The models developed by this method can also be used for quick validation

of experimental results.

Page 86: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

73

Chapter 6. Image Reconstruction Algorithms 6.1 Electrical Impedance Tomography

Electrical Impedance Tomography (EIT) produces images of the distribution of complex

electrical impedance within a closed boundary. EIT has been used in various biomedical

[88], geophysical [89], and industrial applications [90,91]. Compared with other imaging

modalities, such as X-ray computed tomography and magnetic resonance imaging (MRI),

EIT has the advantage of being non-invasive, fast, and cost-effective. The theory and

applications of electrical impedance tomography are reviewed in [92].

A typical setup of an EIT system involves an array of electrodes implanted on the surface

of a cylinder. Sinusoidal voltage/current is applied to the electrodes and the induced

voltage/current at the electrodes is measured. The distribution of the complex permittivity

of the medium under test is reconstructed from the excitation signal and electrical

measurements at the electrodes.

The forward problem in EIT is to estimate the induced electrical measurement at the

electrode given an excitation signal and permittivity distribution. The inverse problem

estimates the permittivity distribution based on the excitation signal and the terminal

electrical measurements. The inverse problem involves solving a Fredholm integral

equation of the first kind [93] and it is ill-posed. Ill-posedness means that the solution

does not depend continuously on the measured data, and that small variations in the

measured data can lead to relatively large errors in the reconstruction of the impedance

distribution. The inverse problem of EIT is also underdetermined because the number of

independent measurements is typically much smaller than the number of pixels in the

image.

Image reconstruction algorithms for EIT can be classified into linear algorithms and

nonlinear algorithms. Linear algorithms can not account for the inherent nonlinearities of

EIT and they have to be solved iteratively to generate an image with a reasonable quality.

Iterative algorithms solve both the forward and the inverse problem, where the forward

Page 87: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

74

problem is typically solved by finite element (FE) methods. Because the inverse problem

is ill-posed, the reconstructed image is very sensitive to FE simulation errors. To

minimize the error, accurate electrode modeling and meshing is needed in the FE

calculations. Although iterative linear algorithms have better accuracy than non-iterative

ones, they are more time-consuming and not suitable for real-time applications. Direct

(non-iterative) nonlinear algorithms is the key to fast and accurate image reconstruction

in EIT [94]. A thorough review on the state of art on EIT reconstruction algorithms is

presented in [51].

Image reconstruction for EIT is highly sensitive to measurement errors. Due to the finite

measurement resolution of EIT systems, the images reconstructed from ‘raw’

measurements deviates significantly from the true image. To stabilize the solution to the

ill-posed problem, Tikhonov regularization is often used. It regularizes the solution based

on the prior information about the MUT [95]. A common practice is to assume its

dielectric permittivity to be slow varying. In effect, regularization smoothes out the

highly oscillatory part of the solution caused by measurement noise. The amount of

regularization is controlled by the regularization parameter. Too much regularization

leads to large residues, while not enough regularization leads to unstable solutions. The

generalized cross-validation method, the discrepancy principle, and the L-curve method

[96] are methods for choosing regularization parameters. The ‘smooth’ prior – the

assumption that the dielectric permittivity of the sample is slow-varying – do not work

well if the MUT has sharp discontinuities in its dielectric permittivity distribution.

Regularization based on prior information about the boundary of the discontinuities is

discussed in [97,98].

In traditional 2-D EIT, the electrodes are positioned in the same plane around the cylinder

to image the cross section of the internal medium. Due to the soft-field effect of EIT, the

electric field would not stay confined in the plane of the electrodes. Leakage of electrical

energy outside of the plane leads to reconstruction errors of the permittivity distribution.

A 3-D setup is, therefore, necessary for accurate reconstruction of the interior. Compared

with 2-D systems, 3-D EIT systems require longer data acquisition time and increased

complexity in image reconstruction algorithms.

Page 88: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

75

In EIT, sensor output depends on the excitation signal as well as the permittivity

distribution. The excitation pattern can be optimized to maximize the sensor output for a

particular permittivity distribution. When compared with adjacent electrode excitation

and opposite electrode excitation, optimal excitation is shown to improve

distinguishability of permittivity distribution by 2 to 10 times, however, multi-electrode

excitation requires individual excitation source and measurement devices for each

electrode, thus greatly increasing the complexity and the cost of hardware [99]. Another

concern over multi-electrode excitation is the safety regulation in medical applications of

EIT on the maximum total current that can be applied to a patient’s body. If this

constraint is applied, optimum excitation do not always perform better than single

excitation methods [100].

6.2 Background on Inverse Problems

A problem is said to be well-posed in the Hadamard sense if: (1) the solution exists for all

data; (2) the solution is unique; (3) the solution depends continuously on the data. If a

problem fails to meet any of the above criteria, it is ill-posed. Inverse problems constitute

a broad class of ill-posed problems in real life applications. Such applications include the

inverse scattering problem in communications, image reconstruction in biomedical

sciences and industrial process control, system identification in automatic control, pattern

recognition in signal processing, and so on [93]. The inverse problem in EIT reconstructs

an image of the internal distribution of the dielectric permittivity of the medium under

test (MUT) based on boundary electrical observations. Given complete continuous data

on the boundary, the inverse problem is proven to have unique solutions [101]. Real

world systems deviate from the ideal mathematical assumption in that (1) electrodes do

not cover the entire boundary and (2) the system measurement resolution is finite. A

review of inverse problem theory for electrical impedance tomography is presented in

[102].

Algorithms using for solving ill-posed problems can be divided into statistical methods

(reference), deterministic methods based on linearization (reference), and non-linear

deterministic methods (reference). The linearized and non-linear algorithms can be

Page 89: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

76

subdivided into direct single-step methods (reference), and iterative methods (reference).

Regularization tools are often used to determine a set of solutions for ill-posed problems

based on prior information. The underlying principle of regularization is to minimize the

difference between the measured impedance/capacitance and the calculated

impedance/capacitance, while the calculated solution of permittivity distribution is kept

reasonably close to the true solution.

Tikhonov regularization is one of the most commonly used. It can be expressed in the

general form of finding solution g, which minimizes the following function:

))ˆ((21 22 ggLSg −+− μλ (6.1)

where g is the estimated dielectric permittivity distribution according to prior

information and 2)ˆ( ggL −μ is used as a constraint for the optimization problem.

The quality of Tikhonov regularization strongly depends on the regularization parameter

μ. It is crucial to choose an optimal regularization parameter μ, so that a solution as close

to the true solution as possible can be obtained. In general, a small value of μ gives a

good approximation to the original problem but the influence of errors may make the

solution physically unacceptable. Conversely, a large value of μ suppresses the data

errors but increases the approximation error.

6.3 Modeling of Electrode

Iterative algorithms involve solving the both the forward problem and the inverse

problem. The forward problem predicts the boundary voltages induced by the injected

current for a permittivity distribution; the inverse problem estimates the permittivity

distribution based on the boundary voltage data. First, an initial permittivity distribution

is assumed. The permittivity distribution is modified based on the difference between the

boundary voltage estimated by the forward model and that measured by the sensor.

Iteration continues until the difference converges to zero. Due to the ill-posed nature of

the inverse problem, any errors from forward estimation result in large errors in the

calculated permittivity distribution. It is therefore important to construct an accurate

Page 90: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

77

forward model.

A simple example is the gap model. It assumes constant current on the electrodes and

zero current between the electrodes. Although easy to implement, the model is not

accurate because it does not account for the shunt current and the contact impedance due

to the electrodes.

The shunt effect from the electrodes – the electrodes usually has much higher

conductivity than the material under test (MUT). When current is applies to some

electrodes, the passive electrodes behaves likes an electrical ‘short’ and shunt some of the

current, resulting in less current flowing through the MUT. The shunt current is shown to

increase with increasing metallization ration of the sensor [103].

The contact impedance – a thin high-impedance layer forms between the electrode and

the material under test (MUT). The contact impedance results in bigger boundary voltage

measurement than the actual voltage drop across the MUT, leading to image

reconstruction errors. Such errors can be avoided by using separate electrodes for current

injection and voltage measurement. By connecting the voltage-measuring electrodes to a

high input impedance operational amplifier, the current flowing through the contact

impedance and, therefore, the voltage drop across it is minimized.

The complete electrode model takes into account the effect of both the shunt current and

the contact impedance [104]. The model has demonstrated an accuracy of 0.1% [103].

Reviews on electrode modeling for EIT are presented in [103,105].

6.4 The Layer Stripping Algorithm

The layer stripping algorithm recursively identifies the media by removing the effects of

layers one at a time. It has been used to solve the inverse scattering problems in

geophysical remote sensing for 1-D discrete lossless [106] and lossy [107] media as well

as 2-D lossless media [108]. In remote sensing, layer dielectrics can be used to model

stratified soil, forest canopy, sea ice, and glaciers, where the media can be considered

both homogeneous and infinite in the horizontal plane. Under far-field approximation, the

incident field upon these layered media can be considered a plane wave normal to the

Page 91: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

78

boundary. Inverse scattering theories can only be applied to hyperbolic problems. The

inverse resistivity problem is, however, an elliptic problem. The inverse resistivity

problem is some times solved by transforming it first to an inverse scattering problem.

Layer stripping algorithms bases on this approach are presented in [109-111]. These

algorithms are developed to reconstruct the resistivity distribution in a 1D or 2D media.

Reference [112] presents a layer stripping algorithm developed to directly solve an

inverse resistivity problem for samples with a radial geometry.

The layer stripping algorithm is a direct method of obtaining an approximate solution to

the full non-linear problem, and is therefore immune to extraneous local minima which

can cause iterative methods to become stuck. In addition, the method requires far fewer

computations and storage requirements than iterative schemes.

6.5 Problem Description

The goal of this chapter is to develop a layer stripping reconstruction algorithm for a one-

dimensional imaging scanner. The scanner is designed to reconstruct the 1-dimensional

dielectric permittivity (complex for lossy dielectrics) profile of layered dielectrics based

on electrical measurements from the FEF sensor. The schematic for the scanner is shown

in Figure 6.1. A fringing electric field (FEF) sensor is positioned below a layered

dielectric sample. The sensor is attached to a stepper motor that allows the sensor to

acquire data at different positions along the ‘z’ axis. All the electrodes of the FEF sensor

are independently driven. At each given time, a low frequency ( < 10 MHz) AC electrical

current is applied at the selected pair of electrodes and the induced voltage potentials at

the rest of the electrodes are measured. The dimension of the sample and that of the

sensor along the y direction is finite. The number of electrodes and the geometry of the

backplane of the FEF sensor can be adjusted as needed. The sample under test is assumed

to be homogeneous along the x-y plane. Its dielectric property along the z axis can either

be slowly varying (continuous/smooth) or discrete (has sharp discontinuities). The

present application differs from the above mentioned examples in geophysics in that (1)

the layered dielectric sample is finite along the x-y plane as illustrated in Figure 6.1. (2)

the electromagnetic wave radiated from the FEF sensor can not be considered a plane

Page 92: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

79

wave. These differences necessitate properly defined boundary conditions.

Figure 6.1. Side-view of the one-dimensional scanner setup.

6.6 Proof of Concept Study

As a proof of concept study the layer stripping algorithm presented in [112] is reproduced

using MATLAB. The purpose of the study is to test the validity of the algorithm with

simple test cases. The Matlab code is shown in the Appendix. The test procedure contains

the following steps:

1. A layered medium with known resistivity is constructed.

2. The Fourier basis function for the layer stripping algorithm is calculated based on

the method described in [112].

3. Using the Fourier basis function from step 2 to reconstruct the resistivity profile

of the medium.

For the layer stripping algorithm to converge, some regularization has to be used. In this

case, the algorithm is regularized by truncating higher order Fourier coefficients. It is

critical to determine the order of the coefficients to be truncated. Three different methods

are recommended in [112] to determine the order. All three methods were tried

implemented in the Matlab algorithm, but none of them produced results that are

converging.

Page 93: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

80

6.7 Conclusions and Future Work

The layer stripping algorithm presented in [112] is used here to solve a 1D inverse

resistivity problem. A proof of concept study was done to reproduce the results presented

in the paper. However, the Matlab algorithm failed to converge.

For future work, the first step is to resolve the convergence problem by reinvestigating

the regularization methods. Secondly, the algorithm is originally developed for samples

with radial geometry. The algorithm needs to be modified to be applied to the inverse

resistivity problem in the Cartesian coordinate. Thirdly, the performance of this particular

layer stripping algorithm should be compared with the other layer stripping algorithms

proposed in [109-111].

Page 94: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

81

Chapter 7. Moisture Dynamics in Food Products 7.1 Review of process analytical technologies in food analysis Many of the real-time non-destructive sensing techniques used for food processing are

spectroscopic in nature. Spectroscopic analysis exploits the interaction of electromagnetic

radiation with atoms and molecules to provide qualitative and quantitative chemical and

physical information that is contained within the frequency spectrum of the energy that is

either absorbed or emitted. A thorough review on the various non-destructive

spectroscopic sensing techniques for the measurements of foods is available in [113].

Figure 7.1 shows the frequency spectrums of various types of spectroscopic sensing

techniques often used for food processing.

Figure 7.1. Frequency ranges of various types of spectroscopic sensing

techniques. Dielectric spectroscopy operates at lower frequency range, when compared with other spectroscopic sensing techniques.

7.1.1 Nuclear magnetic resonance spectroscopy (NMR)

In NMR analysis, a constant homogenous magnetic field is applied to the sample and RF

pulses are directed to induce changes in the nuclear spin of atoms. The various spin

responses are frequency-dependent and reflect the number and mobility of hydrogen

atoms. Low resolution instruments associated with 0.23 to 0.95 tesla (T) magnetic fields

uses RF pulses in the range of 10 MHz to 40 MHz. High-resolution instruments with field

strength of roughly 2.35 T uses RF pulses at above 100 MHz. Low-resolution food

analysis are confined to the measurements of hydrogen atom numbers and their mobility.

A wider variety of chemical species can be sensed when stronger magnetic fields are

Page 95: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

82

used. High-resolution NMR is used to measure isotope ratios in foods. Analysis of such

data can be used to confirm authenticity and to detect the presence of adulterants. Many

high-resolution measurements, especially the isotopic ones, require complicated

extraction procedures to enrich the species under study, and therefore cannot be regarded

as truly non-destructive. The major limitation of NMR techniques is their inability to

study ferromagnetic materials and samples containing significant amounts of

paramagnetic species. A review of the applications of NMR to food measurements is

available in [114].

7.1.2 Mid-infrared (mid-IR) spectroscopy

Use of the mid-IR region of the electromagnetic spectrum involves vibrational responses

from the bonds of organic molecules, such as O-H, C-H, C-O, and N-H. When irradiated

by mid-IR electromagnetic waves, these bonds absorb energy from the radiating sources.

The energy absorption is frequency-dependent. The resulting absorption spectrum can be

used to detect the existence of these bonds. Mid-IR radiation impinges only on the

surface of optically dense food materials, which prevent wide-spread application of mid-

IR spectroscopy in food analysis.

7.1.3 Near-infrared (NIR) spectroscopy

Near-infrared (NIR) spectroscopy is based on the absorption of electromagnetic radiation

at wavelengths from 400 nm to 2500 nm. Similar to of mid-IR spectroscopy, NIR is also

based on the principles of vibration spectroscopy. NIR waves have shorter wavelengths

than mid-IR waves, and penetrate deeper into a sample. Thus, NIR can be used to obtain

spectral data of thick samples.

NIR spectroscopy is a relative method that requires calibration against a reference

method for the parameter of interest. Calibration is normally carried out using

multivariate mathematics (chemometrics). The major advantage of NIR is that it requires

no sample preparation. The analysis is, therefore, simple and fast (between 15 and 90 s)

and can be carried out online. In addition, NIR allows several parameters to be measured

concurrently. An excellent review on NIR spectroscopy is available in [115].

Page 96: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

83

Applications of NIR spectroscopy specific to the food industry are reviewed in [116].

7.1.4 Raman spectroscopy

Another non-invasive sensing technique used widely for food process control is Raman

spectroscopy. It is a non-destructive technique that can provide information about the

concentration, structure, and interaction of biochemical molecules within intact cells and

tissues.

Although similar wavelength ranges are used for mid-IR and Raman spectroscopy,

different rules govern the principles of mid-IR absorption spectroscopy and Raman

scattering spectroscopy. The two techniques are, to a certain extent, complementary:

certain atomic bonds that do not produce strong mid-IR vibrational responses produce a

polarizability response that is measurable in Raman spectra and vice versa.

Applications of Raman spectroscopy in food industry was reviewed in [117]. Raman

scattering is a relatively weak optical effect that requires lasers for efficient excitation. In

many materials the fluorescence induced by the incident light is much more intense than

the Raman scattered light, which makes the Raman signals difficult to measure. This

problem can be avoided by using a Fourier transform (FT) Raman system with laser

excitation at 1064 nm, since negligible fluorescence occurs for this low energy excitation

wavelength. However, 1064 nm excitation results in weak Raman signals and requires

long exposure time (typically 30 min) to obtain spectra with a sufficient signal-to-noise

ratio. This approach can therefore be impractical for efficient sample analysis and not

useful for on-line purposes [118].

7.1.5 Ultrasound

Ultrasound is high frequency sound (typically around 1 MHz). An ultrasonic wave is

transmitted as a series of deformations in the medium through which it passes. The

deformations can be either normal (i.e., shear waves) or parallel (i.e., longitudinal waves)

to the direction of propagation. The motion creates alternative compression and

rarefaction of the medium particles. In low-density applications (power density around 1

W/cm2), the deformations are small enough to be within the elastic limit of the material

Page 97: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

84

and the wave is non-destructive. However, in high-density ultrasound (power density

between 10 and 1000 W/cm2), the properties of medium under test are often changed, in

most cases permanently.

The transmission of an ultrasonic wave depends on the compression and extension of

various bonds in the medium. Therefore, ultrasonic properties are related to the number

and strengths of the bonds and hence bulk structure and composition. Ultrasound has

been used for food characterization including the measurement of the concentration of

simple solutions, lipid crystallinity, emulsion droplet size, meat composition, and

temperature [119,120]. Ultrasonic waves can be readily propagated through certain

optically opaque materials including many foods and packaging materials. Because sound

readily passes through steel, it is relatively easy to measure the properties of fluids within

pipes and other process equipment. The most significant limitation of ultrasonic devices

is that it is difficult to make measurements through air. The reflection of a wave at a

surface depends on the acoustic dissimilarity (impedance mismatch) between the two

phases. Because air is so different from food, common container materials, and even the

transducer element itself, most of the energy is reflected rather than passed into the gas.

Furthermore, small air pockets scatter sound very efficiently and the losses make

meaningful transmission measurements impossible. In some cases it is possible to make

measurements at lower frequency but the loss of spatial resolution reduces the value of

this approach [121].

Other analytical techniques that are often used for food analysis are mass spectroscopy,

gas chromatography, atomic spectroscopy, and high-performance liquid chromatography.

They are reviewed in detail in [122].

7.2 Definition of the Problem

The maintenance of food quality is gaining increasing importance as the shelf life of food

products becomes longer. Manufacturers, retailers, and consumers are demanding and

expecting longer shelf life for shelf-stable and refrigerated foods. Moisture content is an

important parameter affecting the shelf life of most food products. In some cases

excessive amounts of water will cause spoilage, while in other cases, loss of water will

Page 98: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

85

render foods unacceptable.

Shelf-stable homogeneous and multi-layer food products represent a rapidly growing

segment of value-added products for the U.S. food industry. These types of foods may be

processed or formulated such that different regions have different moisture saturation

levels and/or different water activity levels. Moisture migration may reduce product

quality and/or decrease its stability [123].

The control of water in foods requires fast and reliable methods of evaluating the

moisture content and the moisture transport activities of foods [124]. In this chapter, a

multi-channel electrical impedance sensor is used for determining the moisture content

and relative distribution of sugar cookies. Moisture concentration is defined here as

follows:

1%

1 2100%MM

M M= ×

+ (7.1)

where M1 is the mass of the moisture contained in the unit volume, and M2 is the mass of

the dry portion of the material in the same unit volume.

Material impedance is a function of many variables, as shown in (7.2), where M% is the

moisture concentration in the material, T is the ambient temperature, D is the sample

density, and ω is the input signal frequency.

%( , , , )s ZZ f M T D ω= (7.2)

System calibration involves solving the inverse problem of determining the following

function:

% ( , , , )M sM f Z T D ω= (7.3)

or

% ( )M sM f Z= (7.4)

where the functional dependence between moisture concentration and the impedance is to

be determined. The effects from variables other than moisture content are either

eliminated or accounted for.

Page 99: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

86

7.3 Methodology

The material contents of food products are usually complex and varying, which renders

direct determination of sample dielectric permittivity difficult and impractical. Under

these circumstances, an indirect parameter estimation approach based on quantitative

mapping between electrical measurements and the physical variable of interest can be

used. The major challenge for such an approach lies in minimizing the effect of variables

other than moisture concentration, such as ambient temperature and sample density,

which are considered here as disturbance factors. The effects of these factors should

either be eliminated or accounted for in the calibration algorithm [125].

7.4 Experimental Setup

7.4.1 The concentric sensor head

Figure 7.2 shows a concentric sensor head, designed for localized measurements. It has

three electrically separated sensing electrodes, each shielded by a guard plane on the back

of the substrate.

Channel 1 BottomTop

Channel 3Channel 2 Figure 7.2. Top and bottom view of the concentric sensor head. The center plate

is 10 mm in diameter. The outer two rings are 5 mm wide. The spacing between adjacent sensing plates is also 5 mm. The guard planes on the back are slightly wider than respective sensing electrodes.

The sensor head can be used as a fringing field sensor by applying an AC sinusoidal

voltage to the middle ring electrode and measuring the voltage at the two neighboring

electrodes. A non-linear model is needed to describe such a setup. The solution to the

Page 100: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

87

Laplace equation of the non-linear model is:

0 1 2( , ) ( )( )z zr z J r c e c eβ βφ β − += + (7.5)

where φ iss electric potential, r is to the radial coordinate on the horizontal plane, z is the

vertical coordinate, J0 is the zero order Bessel function of the first kind and β is a scaling

constant such that βr is one of the zeros of J0 [126].

The fringing field setup provides one-sided access but has limited signal strength. It is

also susceptible to disturbances from the contact quality between the samples and the

surface of the sensors. The parallel plate setup, on the other hand, is a complement to the

fringing field setup. It lacks the one-sided access but offers greater signal strength and is

comparatively less sensitive to surface contact qualities.

Figure 7.3. Side view of the sensor in a voltage divider setup. A cookie is placed

between the sensing and driving plates.

This chapter presents experimental data obtained with the parallel plate arrangement of

Figure 7.3. A barrier made of 300 μm thick Kapton is used to avoid the Debye layer

effect [127]. The parallel plate capacitor can be modeled as a Maxwell capacitor with

three different dielectrics in series: air, polyimide (Kapton), and the material under test.

For a Maxwell capacitor like this, terminal impedance measurements are not sensitive to

vertical displacements of the polyimide and the material under test [128]. This property

makes parallel-plate sensors more robust to surface contact disturbances.

7.4.2 A voltage divider circuit

Figure 7.3 shows a voltage divider circuit, where Vi is the input voltage signal, Vs is the

sensing voltage signal, Zr is the reference impedance, and Zs is the sensing impedance.

Page 101: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

88

The effective impedance of the parallel-plate capacitor is calculated from the voltage

divider relationship 7.6. To maximize circuit sensitivity, Zr is chosen to be close to Zs. In

this investigation, Zr = 8 pF.

s r

i r s

V ZV Z Z

=+

(7.6)

Various connection schemes are available for this voltage divider setup. When there is an

electric potential difference between the sensing electrodes and their respective guard

electrodes, stray capacitances are introduced into the circuit. To prevent these stray

capacitances from affecting measurement accuracy, the guard planes are set to the same

voltage as their respective sensing electrodes by using a unity-gain voltage buffer.

Figure 7.4. Sensor geometry and experimental setup. The moisture content of the

sample is increased by adding increments of 0.2 grams of water to the center of the sample. Measurements are taken at each moisture content level. A 3-channel voltage-divider interface circuit is used to measure the complex terminal impedance of the sensor at three different radial locations.

7.5 Experimental Procedure

To calibrate the moisture sensing system, a quantitative relationship between sample

moisture content and the corresponding impedance measurements needs to be

established. The following experiment was conducted to evaluate this relationship.

1. A test specimen is placed between the sensor plates so that the center of the

specimen is aligned with channel 1 of the sensing plate.

Page 102: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

89

2. A 6 volt, 10 Hz to 10 kHz frequency sweep signal is applied to the circuit in

Figure 7.3 and Vs is measured.

3. The moisture content of the sample is increased by adding increments of 0.2

grams of water to the center point.

4. Measurements are taken at each moisture content level.

7.6 Experimental Result and Data Analysis

Figure 7.5 (a) and Figure 7.5 (b) show respectively the capacitance and phase variations

due to moisture content increase as measured by the center sensing electrode. Change in

moisture content leads to an increase in the capacitance and phase maxima and a shift of

the curves toward higher frequencies.

102

103

1040.14

0.16

0.18

0.2

0.22

0.24

0.26

Cap

acita

nce

(pF)

Frequency (Hz)

0 g

1.0 g

0.8 g

0.6 g

0.4 g

0.2 g

10

210

310

4-12

-10

-8

-6

-4

-2

0

2

4

Frequency (Hz)

Pha

se (d

eg)

0 g

1.0 g0.8 g0.6 g0.4 g0.2 g

(a) (b) Figure 7.5. Capacitances and phase measured at different moisture content levels. The measurement results show that changes in moisture content leads to an increase in the capacitance and phase maxima.

For capacitance measurements, the higher the signal frequency, the greater the

measurement sensitivity to moisture content. To achieve maximum sensitivity,

capacitance data at 10 kHz is used to calibrate the system, which here involves

establishing a quantitative mapping between capacitance values and moisture content.

7.6.1 Compensation for moisture diffusion

The triangles in Figure 7.6 show the channel 1 capacitance data at 10 kHz averaged

across different frequency sweeps. At higher moisture content level, moisture diffusion to

Page 103: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

90

the outer channels reduces the capacitance increase between neighboring samples.

The higher the moisture content gradient between the center channel and the outer rings,

the more intensive the moisture diffusion process. This is reflected in the increasing

discrepancy between the uncompensated and compensated capacitance data as water is

being added to the center of the sample.

0.2 0.4 0.6 0.8 1 1.20

0.02

0.04

0.06

0.08

0.1

0.12

0.14

0.16

0.18

0.2

Moisture (g)

Cap

acita

nce

(pF)

Before compensation

After compensation

*16.4390 0.0028M CΔ = × Δ +

Figure 7.6. Capacitance measurements against the weight of added water at 10

kHz for channel 1. Saturation occurs at high water level.

To compensate for the effect of diffusion, the capacitance increase from channels 2 and 3

is measured and mapped to effective increase in channel 1. This increase, added to the

original capacitance change from channel 1, gives the new channel 1 capacitance data

after compensation, as shown in (7.7), where ∆C is the capacitance increase for each

channel, Cor is the capacitance measurement of the original sample for each channel, and

∆C1* is the channel 1 capacitance increase after compensation.

33

12

2

11

*1 C

CC

CCC

CCor

or

or

or Δ+Δ+Δ=Δ (7.7)

As indicated by the solid line in Figure 7.6, a better linear approximation is achieved after

compensation.

7.6.2 Linear regression

Assuming a linear functional dependence, the following calibration equation is

determined for channel 1 by performing linear regression on the compensated data:

Page 104: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

91

311 108.244.6 −×+Δ×=Δ CM (7.8)

In this configuration, all sensor pixels are parallel-plate capacitors with different area.

Ideally, the functional dependence for channels 2 and 3 can be obtained by scaling (7.8)

with the respective area ratio. However, the existence of a non-uniform air gap has to be

taken into account.

7.6.3 Compensation for non-uniform air gap

The air gap between the material and the top plate of the sensor is non-uniform due to an

uneven shape of the cookie samples. To compensate for this, uniform water distribution

in the original sample is assumed and the ratios of capacitance measurements from

channels 2 and channel 3 with respect to those from channel 1 are measured. This

difference in capacitance measurements from the three channels is caused partly by the

difference in sensing plate area and partly by the non-uniformity in air gap thickness.

Taking the ratios obtained above and using them as scaling factors, the functional

dependence of capacitance measurements on water content from channels 2 and 3 can be

obtained from (7.8).

422 1022.643.1 −×+Δ×=Δ CM (7.9)

433 1095.391.0 −×+Δ×=Δ CM (7.10)

7.6.4 Moisture content distribution

Based on the calibration equations (7.8), (7.9), and (7.10), the absolute mass of moisture

contained in the portion of the sample above each ring is calculated from the capacitance

measurements. The mass of the dry portion of the sample above each ring is determined

from the ratio of the respective sensing electrode area to the area of the whole sample.

Given the absolute mass of moisture and the dry portion of the sample, moisture content

levels for all three channels can be calculated according to (7.1), enabling real-time

imaging of moisture content distribution.

Figure 7.7 shows the moisture content distribution profile of a sample at various moisture

content levels, which is obtained from fitting the moisture content data from the three

Page 105: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

92

channels to scaled Gaussian curves.

2

2%2

)(⎟⎠⎞

⎜⎝⎛−

= σ

πσ

x

eAxM (7.11)

where x is the distance to the center of the sensing plate, σ is a measure of the width of

the curves and A is a scaling factor, which is determined by the moisture diffusion

coefficient of the diffusion process.

Figure 7.7. Moisture content distribution across the radius of the sample when different amount of water is added to the center. The moisture distribution profile is obtained through fitting of measured moisture data to Gaussian curves.

7.6.5 Evaluation of the calibration model

The calibration approach discussed above involves several approximations. To evaluate

the effectiveness of the model obtained through system calibration, the absolute masses

of the moisture measured from all three channels are summed up and compared with the

mass of the moisture added to the sample. As indicated in Table 7.1, measurement error

decreases with increasing moisture content. Further processing of experimental data is

needed to reduce the error at low moisture content levels.

Page 106: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

93

Table 7.1. Comparison between the actual mass of the moisture added to the sample and the mass of the moisture measured by the sensor.

Moisture Added (g) Moisture Measured (g) Error 0.2 0.130 35% 0.4 0.312 22% 0.6 0.570 5% 0.8 0.776 3% 1.0 0.980 2%

7.7 Conclusions

The electrical impedance sensor is used to determine the moisture content and lateral

moisture distribution of cookie samples. The concentric sensor head used here can be

configured as a stand alone FEF sensor. The multi-channel FEF sensor allows three-

dimensional profiling of the sample under test. However, the effects of lateral variation

and those of vertical variation within in the sample could be coupled in the sensor

terminal measurements, which greatly increase the complexity of parameter estimation

algorithms. If moisture activity along only the vertical axis (the axis perpendicular to the

electrode surface) is required, a single channel FEF sensor would be sufficient.

Applications of the electrical impedance moisture sensor described in this chapter are not

limited to the study of shelf life of foods. It can be integrated into the food drying process

to control the moisture endpoint. It can also be used to moisture content of foods during

baking. The latter is a more challenging task in that many other physical parameters

(temperature, texture, porosity, and dimensional) of the sample could be changing

simultaneously. Multivariate analysis methods, such as principle component analysis and

partial least squares regression, are needed to calibrate the system.

Page 107: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

94

Chapter 8. Measuring Physical Properties of Pharmaceutical Samples 8.1 Motivation

The Food and Drug Administration (FDA) has very stringent regulations for

pharmaceutical products in such aspects as active ingredient concentration, tablet

hardness, and coating thickness. Quality control is, therefore, a top priority for

pharmaceutical companies.

A typical pharmaceutical tablet is a complex matrix containing one or more active

pharmaceutical ingredients (APIs), fillers, binders, disintegrants, lubricants, and other

materials. A basic problem in pharmaceutical manufacturing is that a relatively simple

formulation with identical ingredients can produce widely varying therapeutic

performance depending upon how the ingredients are distributed in the final matrix.

Pharmaceutical makers also are developing advanced tablets for drug dosage

management, which can provide longer, flatter, or sometimes complex bloodstream

profiles. Approaches include the use of barrier layers, cored tablets, selective release

microspheres, and even osmotic pumps. These tablets essentially are highly engineered

drug delivery systems in which the physical structure is as critical as the chemical

composition [129].

Existing analytical techniques, such as high performance liquid chromatography (HPLC)

and mass spectrometry (MS), often are used to determine the gross composition of a

dosage form, but they provide no information about the distribution of the individual

components. The manner and duration of component release is examined through

dissolution testing. These techniques require destruction of the sample, making it difficult

or impossible to trace the sources of failures or anomalies. Spectroscopic techniques

enable rapid, nondestructive analysis of samples and can be employed at a number of

points in the pharmaceutical development and manufacturing process. In particular, NIR

spectroscopy and Raman spectroscopy have gained increasing popularity for process

Page 108: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

95

monitoring and control due to its high information content and flexibility of

implementation. It is used widely for the characterization of raw materials, and also has

been used in applications such as blend homogeneity [128-130], moisture measurement

[131-136], and the analysis of intact tablets [137-143].

IR and Raman spectra provide images of the vibrations of the atoms in a compound.

Therefore, both techniques are also referred to as vibrational spectroscopy. IR

spectroscopy is based on the absorption of electromagnetic radiation by a molecular

system, whereas Raman spectroscopy relies on inelastic scattering of electromagnetic

radiation by a molecular system. An IR spectrum is obtained by passing infrared radiation

through a sample and determining what fraction of the incident radiation is absorbed at a

particular frequency. A Raman spectrum is obtained by focusing monochromatic

radiation on a sample and analyzing the scattered light as a function of frequency [144].

Widespread application of Raman spectroscopy has been limited in part by the problem

of fluorescence, especially encountered for colored samples under visible excitation. The

fluorescence signal, when present, is usually much stronger than Raman scattering. To

avoid this problem, spectroscopists commonly employ excitation sources in the near

infrared region (NIR), where the illuminating source has insufficient frequency energy to

reach most fluorescence-producing electronic states. However, certain substances do

fluoresce when irradiated with NIR light sources. Common near infrared fluorescent

substances include iron oxide, which is often utilized in tablet coatings or incorporated in

the tablet core as a colorant and food colorants, such as Alphazurine FG. The use of these

or other NIR fluorescent materials limits the utility of Raman as a tool to support drug

research, development and quality control [142].

In recent years, NIR spectroscopy has superseded traditional methods as an analytical

tool in various fields and [115]. Near-infrared (NIR) spectroscopy is based on the

absorption of electromagnetic radiation at wavelengths in the range of 780 nm to 2500

nm. NIR offers many advantages that make it an attractive candidate for process control

and monitoring. It is a non-invasive, non-destructive technique that requires minimal

sample preparation. Its measurements are fast and relatively accurate. A single NIR

spectrum allows several analytes to be determined simultaneously. The technique allows

Page 109: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

96

determination of non-chemical (physical) parameters such as density, viscosity, or

particle size. In addition, NIR equipment is robust and most suitable for use for process

control at production plants.

However, some characteristics of the technique restrict broader application or preclude

particular uses. NIR measurements are not selective. Therefore, chemometric techniques

have to be used to extract relevant information. Information extraction in NIR often relies

on empirical calibration models because there are no theoretical/analytical models for the

interaction between NIR light and matter. Accurate, robust calibration models are

difficult to obtain because it requires a large number of samples that encompass all

variations in physical and/or chemical properties. In addition, the incorporation of the

physical and chemical variability of samples in the calibration requires as many different

calibration models as there are sample types, and hence more than one model per analyte.

Because NIR spectroscopy is a relative method, model construction often relies on

calibration against a reference method. Measurement accuracy of the constructed NIR

model is thus limited by the accuracy of the reference method. In addition, the technique

is not very sensitive, thus, it can be applied to only major components.

Dielectric analysis methods, though less developed for pharmaceutical applications when

compared with NIR and Raman spectroscopy, have great potential for real time process

control and monitoring. Dielectric analysis is a technique involving the physical, rather

than chemical characterization of samples. Techniques like IR and NMR examine the

molecular structure of samples, while dielectric spectroscopy examines the physical

arrangement and behavior of molecules within structures. A thorough overview of

dielectric analysis for pharmaceutical systems is available in [145].

This chapter investigates the feasibility of using dielectric spectroscopy sensing for

quality control of such physical properties as tablet hardness, coating thickness, and API

content of powder samples. Tests of drug signatures are also carried out to differentiate

between unpolished, polished, and placebo tablet samples. The results show good

measurement sensitivity to parameters of interest. More extensive experiments need to be

conducted to quantify the dependencies between these physical properties and the

electrical measurements and compensate for disturbance factors. Proper choice of a

Page 110: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

97

sensor is very crucial for achieving optimal measurement results. Both FEF sensors and

parallel plate sensors are used in the experiments. Measurements from both types of

sensors are presented and compared to give insight on choosing the right type of sensor

for a particular measurement.

8.2 Measuring Tablet Hardness and Coating Thickness

Film coating is often employed as final and separate operation in the manufacturing of

pharmaceutical or nutritional oral solid dosage forms. A coating barrier offers advantages

to the consumer and in the pharmaceutical manufacturing process. Among the most

important are the controlled release of the active pharmaceutical ingredient (API) and the

durability of the dosage form in production and on the shelf. In addition, coatings can

serve to reduce irritation associated with the exposure of the stomach to high

concentrations of medication, and increase product acceptance by improving the visual

appeal of a tablet while making it easier to swallow and enhancing its taste and odor.

Evaluating the properties of pharmaceutical coatings such as intra- and inter-tablet

thickness and uniformity is important for demonstrating adequate process controls and

for ensuring the optimal performance of the final product. Inter-tablet coating uniformity

is important to ensure that the coating is homogeneously distributed on each tablet

throughout the batch; while intra-tablet uniformity is crucial because the overall

performance of the film will likely be limited by the thinnest location on the tablet.

A number of instrumental methods have received substantial attention as potential means

for coating process monitoring. Techniques like scanning electron microscopy, atomic

force microscopy, and conventional optical microscopy have high spatial resolution.

They are typically used for intra-tablet coating uniformity measurements. These

techniques are, however, tedious and not amenable to rapid at-line analysis of a large

number of samples to obtain reliable statistics on coating uniformity. (Here ‘at-line’

refers to measuring in the manufacturing area after manual sampling. It differs from ‘in-

line’, which refers to when the sample interface is located inside the process vessel, the

chemical analysis is done in situ, thus omitting the need for transport of sample out of the

process vessel.) Laser-induced breakdown spectroscopy (LIBS) can be used as an

Page 111: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

98

alternative technique for the study of coating thickness uniformity [146] and [147]. It has

the potential to provide both rapid at-line analysis of multiple samples as well as the

spatial resolution necessary for intra-tablet uniformity determination. The main drawback

of this approach is that it is destructive. Near infrared spectroscopy is a real-time non-

destructive technique. However, it does not provide the spatial resolution required for

intra-tablet coating uniformity analysis. Non-destructive techniques like near infrared

spectroscopy (NIR) and Raman spectroscopy are typically used for studies of inter-tablet

coating analysis [148,149] and [142].

8.2.1 Information on sample physical properties

Tablet samples of known hardness are used in this feasibility study. Other information,

such as average tablet thickness and weight, are also available. Sample pressure

(hardness) affects both weight and thickness. Figure 8.1 shows the dependence between

these physical parameters. In this case, pressure refers to the pressure applied when the

tablets are being compressed. Increase in pressure leads to increased tablet density, and,

therefore, an increased weight; at the same time, the pressure increase results in a

decrease in tablet thickness. Notice, however, the trend for weight variation is not strictly

monotonic. Table 8.1. shows the average values of hardness, weight and thickness for the

different groups of tablet samples.

Figure 8.1. Tablet sample weight and thickness against the pressure applied to the

sample when the tablets are being compressed. Higher pressure corresponds to reduced thickness and higher weight in the resulting tablets.

Page 112: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

99

Table 8.1. Tablet sample physical properties: hardness, weight, thickness.

Sample Hardness Weight Thickness Sample #1 25.6 (kp) 0.592 (mg) 5.56 (mm) Sample #2 31.5 (kp) 0.607 (mg) 5.53 (mm) Sample #3 34.3 (kp) 0.610 (mg) 5.49 (mm) Sample #4 41.8 (kp) 0.609 (mg) 5.27 (mm) Sample #5 45.1 (kp) 0.615 (mg) 5.26 (mm)

8.2.2 Experimental setup

The experimental results presented here are from a parallel plate setup. Tablet samples of

the same hardness are arranged side by side with the same orientation between the two

electrodes of the sensor. The sensor is driven by a 1 V AC voltage signal from a Fluke

RCL meter. The meter measures the loop AC current and sensor terminal impedance. The

AC signal sweeps from 50 Hz to 100 Hz.

8.2.3 Experimental results

As mentioned previously, the major variables that affect electrical measurements are

sample density and sample thickness. Density affects material dielectric permittivity εr

and conductivity σ while thickness affects d. Therefore, capacitance measurements are

sensitive to changes in both sample density and thickness. Phase measurements, on the

other hand, are determined by the relative ratio of the real and imaginary part of the

impedance. Change in sample geometry affects capacitance and conductance

measurement in the same fashion and leaves their relative ratio constant. Therefore, phase

measurements are only dependent here on density variations.

Figure 8.2 (a) and Figure 8.2 (b) show respectively the capacitance and phase

measurement of the tablet samples against hardness at various frequencies. Conductance

and current measurements are omitted because no additional information is offered.

According to Figure 8.1, increase in hardness results in a rise in sample density and a

drop in sample thickness, which affects the capacitance measurements adversely. The

resulting measurement shown in Figure 8.2 is a trade-off between these two effects,

which explains why the trend is not monotonic. Phase measurement displays a monotonic

dependence on hardness and bears information only about samples density. Using the

Page 113: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

100

combined information from capacitance and phase measurements, samples density and

thickness can be uniquely determined.

(a) (b)

Figure 8.2. Capacitance and phase of 180 mg tablet samples measured against the hardness of the samples.

8.3 Measuring Tablet Coating Thickness

8.3.1 The experimental setup

Experiments are carried out using both a parallel plate sensor and fringing field sensor.

Figure 8.3 shows the FEF setup. For the parallel plate sensor setup, 10 samples are

arranged side by side with the same orientation between the two electrodes of the sensor.

Figure 8.3. Fringing electric field sensor setup for measuring tablet coating

thickness. The spatial wavelength of the chosen sensor is 500 μm.

Page 114: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

101

8.3.2 The experimental results

Figure 8.4 shows the capacitance measurements of the tablet samples. To focus on the

detailed measurement variation between samples of different coating thickness, the

capacitance and phase measurements of the original uncoated sample are used as

references and subtracted from the measurements of all other samples. The results are

shown in Figure 8.5 (a) and Figure 8.5 (b). A clear dependency exists between the

capacitance variation data and sample coating thickness. Note that exact information on

coating thickness is not provided with the test samples used in these experiments. Here,

weight information, which is directly related to coating thickness, is used instead. Figure

8.9 shows the capacitance measurements acquired at 1 kHz plotted against sample

weight. A near-linear dependency is witnessed.

Figure 8.4. Absolute capacitance measurements of tablet samples with different

coating thickness using a parallel plate sensor. Tablets of various thicknesses are grouped here according to their weight. The thickness the coating, the heavier they weigh. The data ‘the original’ corresponds to the bare tablet without any coating.

Page 115: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

102

102 103 104 105-0.5

0

0.5

1

1.5

2

2.5

3

3.5

Frequency (Hz)

Pha

se v

aria

tion

(deg

)

27 mg30 mg33 mg36 mgfinal

(a) (b) Figure 8.5. Capacitance and phase variation between samples with different

coating thickness using a parallel plate sensor. Tablets of various thicknesses are grouped here according to their weight. The thickness the coating, the heavier they weigh.

Figure 8.6. Capacitance variation against sample weight using a parallel plate

sensor. The increase in the weight of the samples is caused by increasing coating layer thickness. The thicker the coating, the heavier the sample weighs. The parallel plate sensor has a near-linear response to variations in sample weight.

Figure 8.7 shows the capacitance measurements of the samples from the fringing field

setup. A much greater difference is witnessed in this case between the measurements of

the original tablets and those of the coated ones than in the case of the parallel plate

setup. This is easily explained by the higher sensitivity of FEF sensors to the layer of

samples in direct contact with the electrodes. Again, using the measurements from the

original tablets as references, the capacitance and phase variations of the coated tablets

are calculated. The results are shown in Figure 8.8 (a) and Figure 8.8 (b). Figure 8.9

Page 116: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

103

shows the capacitance variation data at 1 kHz plotted against sample weight. Compared

with the parallel plate result shown in Figure 8.6, the dependency between capacitance

and sample weight is non-linear in the fringing field setup. This is, however, within

expectation considering the non-uniform field distribution of a FEF sensor. As coating

thickness increases, the electrical measurement sensitivity to thickness variation

decreases. To attain an optimal sensitivity curve, a wavelength of the FEF sensor has to

be carefully chosen. The sensor used here provided three different channels with various

wavelengths. The spatial wavelength of the channel used in the experiments is 500 μm,

which corresponds to a penetration depth of around 160 μm.

102 103 104 1057.2

7.4

7.6

7.8

8

8.2

8.4

8.6

8.8

9

Frequency (Hz)

Cap

acita

nce

(pF)

Original27 mg30 mg33 mg36 mgfinal

Figure 8.7. Absolute capacitance measurements for tablet samples with different

coating thickness using a fringing electric field sensor with spatial wavelength of 500 μm. Tablets of various thicknesses are grouped here according to their weight. The thickness the coating, the heavier they weigh. The data ‘the original’ corresponds to the bare tablet without any coating.

Page 117: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

104

102 103 104 1050.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

1

1.1

1.2

Frequency (Hz)

Cap

acita

nce

varia

tion

(pF) 27 mg

30 mg33 mg36 mgfinal

102 103 104 1050

0.5

1

1.5

2

2.5

3

3.5

Frequency (Hz)

Phas

e va

riatio

n (d

eg) 27 mg

30 mg33 mg36 mgfinal

(a) (b)

Figure 8.8. Capacitance and phase variation for tablet samples with different coating thickness using a fringing electric field sensor with spatial wavelength of 500 μm. Tablets of various thicknesses are grouped here according to their weight. The thickness the coating, the heavier they weigh.

26 28 30 32 34 36 38 40 42

0.44

0.46

0.48

0.5

0.52

Weight (mg)

Cap

acita

nce

var

iatio

n (p

F)

Figure 8.9. Capacitance variation against sample weight for the fringing electric

field setup. The increase in the weight of the samples is caused by increasing coating layer thickness. The thicker the coating, the heavier the sample weighs. Due to the non-uniform field distribution of FEF sensors, the sensor response to variations in tablet coating thickness in non-linear.

8.4 Acquiring Drug Signature Using a FEF Sensor

There exist the need for a non-invasive sensing technique that can differentiate different

types of drugs. One of the solutions is to look at the spectroscopy measurements of the

drug samples in the frequency domain. Information on both the absolute value and the

trend of the frequency dependencies of the electrical measurements can be used to

different types of drugs from each other.

Page 118: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

105

This section investigates the feasibility of acquiring drug signatures using the fringing

field dielectrometry sensing technique. In the experimental setup, eight tablet samples are

positioned on a FEF sensor with spatial wavelength of 500 μm. The goal of the

experiment is to differentiate between three groups of tablet samples: the original, the

polished, and the placebos.

Figure 8.10 (a) and Figure 8.10 (b) show respectively the capacitance and phase

measurements of the three types of tablets. A great difference is witnessed between the

measurements of the original tablets and those of the other two types of tablets, which

makes the original tablets easily distinguishable. The measurement results for the

placebos are close to those of the polished samples, the difference in capacitance

measurements being in the range of 0.01 pF. High measurement resolution is necessary to

differentiate these two groups of samples.

102 103 104 105

6.5

6.6

6.7

6.8

6.9

7

7.1

7.2

7.3

Frequency (Hz)

Cap

acita

nce

(pF)

OriginalPolishedPlacebo

102 103 104 105

-90.5

-90

-89.5

-89

-88.5

-88

-87.5

Frequency (Hz)

Pha

se (d

eg)

OriginalPolishedPlacebo

(a) (b)

Figure 8.10. Capacitance and phase measurements of three different types of tablet samples using a fringing electric field sensor with spatial wavelength of 500 μm. The results show that the FEF sensor has high measurement sensitivity to the surface textures of the sample under test.

8.5 Measuring API Concentration for Powder Samples

Fluid bed dryers are used during the manufacture of many products, including minerals,

polymers, fertilizers, crystalline materials, and pharmaceuticals. In pharmaceutical

processing, the fluid bed drying unit operation is often used to remove water or other

solvents added to dry powder mixtures during wet granulation prior to further processing

Page 119: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

106

(lubrication, compression, etc.). Poorly controlled moisture endpoints can affect

downstream processablilty, tablet dissolution characteristics, mass balance required for

accurate dosing, and long-term chemical stability. The pharmaceutical industry has

traditionally relied on loss on drying (LOD) and Karl Fischer (KF) titration to measure

moisture content in pharmaceutical granulation and drying processes. These techniques

are time-consuming and usually limited to analyzing only a few samples during the

process. Furthermore, sampling and preparation can lead to significant analytical errors

[132].

This section investigates the feasibility of non-invasive monitoring of the drying process

for pharmaceutical powder samples using FEF sensors. The electrical impedance of

powder samples that have been subject to different period of drying time are measured

using the impedance spectroscopy sensing system. Figure 8.11 (a) and Figure 8.11 (b)

show the capacitance and phase measurement of the various powder samples. It can be

inferred from the big difference between the measurements of ‘0 hour’ samples and ‘2

hours’ samples that most API is removed in the first two hours of the process. Figure 8.12

shows the capacitance measurements of the powder samples plotted against drying time

at two different frequencies. The exponentially decaying profile resembles that of a

diffusion process, which matches with what is expected of the drying process. This result

indicates the feasibility of the technique. More extensive experiments have to be

conducted to quantify the functional dependence between the electrical measurements

and API content.

Page 120: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

107

(a) (b)

Figure 8.11. Capacitance and phase of powder samples of various drying time.

Figure 8.12. Capacitance of powder samples against sample drying time

measured at two separate frequencies. The trend of exponential decay approximates that of a moisture diffusion process. These measurement curves can be used to calibrate the sensor to monitor moisture endpoints during the power drying process.

8.6 Conclusions

The dielectric sensors used here demonstrated good sensitivity to the variations in the

physical properties of pharmaceutical tablet and powder samples. The feasibility of using

such sensors for rapid at-line measurements is proved. Selecting the sensor with a proper

geometry is crucial to obtaining good experimental results. Parallel plate sensors measure

a sample in bulk. Any local variations are averaged across the whole sample in the

terminal impedance measurements. The electric field distribution of FEF sensors is non-

uniform. An FEF sensor with the proper spatial wavelength can be used to detect

variations within a localized region of the sample. Measurements from parallel plate

Page 121: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

108

sensors are, in general, more stable and less noise-prone than those from FEF sensors,

which makes parallel plate sensors good candidates for proof-of-concepts experiments.

FEF sensors are more attractive in cases where high measurement sensitivity is desired.

Page 122: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

109

Chapter 9. Conclusions and Future Work

9.1 Conclusions

9.1.1 Parametric Modeling of FEF Sensors

Parametric models are constructed for concentric FEF sensors and interdigital FEF

sensors based on non-dimensionalized fitting of FEM simulation results. A 50%

metallization ratio is assumed when constructing the unit cell, but the methodology can

be used for modeling FEF sensors with metallization ratio other than 50% as well. Only

the terminal capacitance of the FEF sensors is considered here. To extend the results for

applications where complex impedance is of interest, the variable C can be replaced by

the complex admittance Y* and the dielectric constant ε can be replaced by the complex

dielectric permittivity ε*. In the case of interdigital FEF sensors, the model is constructed

to evaluate the terminal capacitance per unit finger length. Here the end effect of finite

finger length is ignored. For interdigital FEF sensors with finger length much greater than

its spatial wavelength (more than 10 times greater), this simplification is valid.

The modeling method is not restricted to FEF sensors; its concept of non-

dimensionalization can be used for the design optimization of a wide variety of sensors.

For sensors that are difficult to model analytically, the method provides accuracy

comparable to numeric methods while greatly improves the throughput of design

optimization.

9.1.2 Interfacing Circuits for FEF Sensors

Various aspects of interfacing circuit design for fringing electric field dielectrometry is

discussed in this chapter. Due to the high measurement sensitivity requirement of FEF

sensor applications, the noise floor of the interface circuits needs to be sufficiently

suppressed. Therefore, stray-immunity is one of the most crucial figures of merit for

these circuits. For spectroscopic applications, where the sample under test is evaluated

Page 123: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

110

over a frequency band, the circuit topology optimal for that frequency band should be

used. For circuits interfacing with sensor arrays in imaging applications, parasitics due to

multiplexing need to be carefully addressed.

9.1.3 FEF Sensor Design Optimization

The optimal sensor geometry changes with respect to different dielectric properties of the

samples. In this thesis, the samples are assumed to have low permittivity (< 10) and close

to zero conductivity. Such samples are representative for a wide range of ceramics and

plastics [86]. Design of sensors specialized for high permittivity dielectrics (10 < εr < 80)

were discussed in [50]. For highly conductive samples, resistance, instead of

capacitance, is measured to estimate sample concentration or distribution within the

sensing zone. In cases where the sample has complex permittivity and displays

frequency-dependent behavior, both the real part and the imaginary part of the complex

impedance have to be measured.

The multi-channel impedance sensors presented in this chapter are designed for imaging

applications. Electrical imaging systems typically operate in the megahertz range.

Therefore, the electrostatic model used in the FE simulations is adequate. For sensors

used in broad-band spectroscopic systems, AC simulations are necessary. Such systems

are usually used for lab-based determination of material properties of samples with

complex permittivity.

9.2 Future Work

Instrumentation for FEF systems is developing toward custom-designed silicon-based

integrated systems. The planar geometry of FEF sensors allows easy integration into a

CMOS process. Complete systems can be fabricated with the sensor electrodes on the top

metal layers, and the interface and control circuitry underneath. The highly developed

and well-controlled CMOS processes can facilitate mass fabrication of the sensors with

high spatial resolution at low cost. The elimination of wiring and connection help to

minimize the stray impedance. In some cases, the signal conditioning circuits can be

replaced by digital signal processing units. For example in spectroscopic applications, the

Page 124: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

111

frequency response acquired by the sensor can be analyzed by an integrated DSP unit

built-in to the sensor. Finger print sensors based on integrated FEF electrodes have been a

relative active field of research in the last decade [150-152].

As MEMS and nanotechnology reach maturity, integrated FEF sensors at the nanometer

to micrometer scale are no longer a remote reality. Due to the small electrode surface area

for FEF sensors at this scale, the sensor measurement signal can be very weak. The key to

such systems lies in highly sensitive interface circuits. Bio-chemical coatings can be used

to enhance the selectivity and sensitivity of the sensing system. Since FEF sensor

measurements are highly dependent on surface contact quality, measuring solids with

FEF sensors at the nanometer to micrometer scale may be challenging. Noise due to

surface roughness of the sample can be minimized if the test sample is placed in a

solution.

In the area of data analysis, many chemometrics methods, often used by analytical

chemists, can be applied here directly for multivariate calibration of FEF sensing

systems. Dielectric sensors typically respond to variations in several physical parameters

simultaneously. Although the dielectric properties of a sample can be measured directly

through dielectric spectroscopy, the relation between dielectric measurements and

physical properties are typically not well defined, especially when several physical

parameters are changing simultaneously. Therefore, determination of sample physical

properties typically relies on empirical calibration against results from other measurement

methods. For the FEF sensing systems described here to be used effectively in industrial

processes where many environmental variables (such as temperature during the baking

process for foods) are changing, multivariate analysis has to be used to extract useful

information from experimental data.

Page 125: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

112

References

[1] X. B. Li, S. D. Larson, A. S. Zyuzin, and A. V. Mamishev, "Design Principles for Multichannel Fringing Electric Field Sensors," Sensors Journal, IEEE, vol. 6, no. 2, pp. 434-440, 2006.

[2] X. B. Li, V. V. Inclan, G. I. Rowe, and A. V. Mamishev, "Parametric Modeling of Concentric Fringing Electric Field Sensors," IEEE Conference on Electrical Insulation and Dielectric Phenomena, 2005, pp. 617-620.

[3] X. B. Li, S. D. Larson, A. S. Zyuzin, and A. V. Mamishev, "Design of Multichannel Fringing Electric Field Sensors for Imaging. Part I. General Design Principles," IEEE International Symposium on Electrical Insulation, 2004, pp. 406-409.

[4] X. B. Li, C. Kato, A. S. Zyuzin, and A. V. Mamishev, "Design of Multichannel Fringing Electric Field Sensors for Imaging. Part II. Numerical Examples," IEEE International Symposium on Electrical Insulation, 2004, pp. 410-413.

[5] X. Li, A. Zyuzin, and A. V. Mamishev, "Measuring Moisture Content in Cookies Using Dielectric Spectroscopy," IEEE Conference on Electrical Insulation and Dielectric Properties, 2003.

[6] X. Li, "Real-time Impedance Spectroscopy Sensing of Material Physical Properties," Master of Science, Department of Electrical Engineering, University of Washington, Seattle, Washington, 2003.

[7] K. Sundara-Rajan, X. Li, N. Semenyuk, and A. V. Mamishev, "Moisture Measurement in Paper Pulp Using Fringing Field Impedance Spectroscopy," IEEE Sensors Conference, Toronto, Canada, 2003.

[8] R. K. Singh, "Research Directions for Food Engineering," Journal of Food Engineering, vol. 23, no. 4, pp. 491-499, 1994.

[9] N. H. Mermelstein, O. R. Fennema, C. A. Batt, H. D. Goff, M. W. Griffiths, D. G. Hoover, F. H. Hsieh, V. K. Juneja, M. Kroger, D. B. Lund, D. D. Miller, D. B. Min, P. A. Murphy, S. A. Palumbo, M. A. Rao, E. T. Ryser, B. O. Schneeman, H. Singh, H. Stone, R. Whiting, J. S. B. Wu, A. E. Yousef, J. N. BeMiller, C. Dennis, M. P. Doyle, F. E. Escher, T. Klaenhammer, D. Knorr, J. L. Kokini, W. Iwaoka, G. W. Chism, F. M. Dong, R. Hartel, C. Reitmeier, S. J. Schmidt, and R. E. Wrolstad, "Food Research Trends - 2003 and Beyond," Food Technology, vol. 56, no. 12, pp. 30-+, Dec. 2002.

[10] N. H. Mermelstein, D. J. O'Sullivan, E. A. Baldwin, V. B. Alvarez, M. A. Swanson, F. M. Aramouni, W. C. Ellefson, D. Craig-Petsinger, and D. L. Park, "A Look into the Future of Food Science & Technology - Representatives of IFT's 26 Divisions Tell What

Page 126: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

113

They Foresee Happening in Their Respective Division's Area of Expertise Over the Next Few Years," Food Technology, vol. 56, no. 1, pp. 46-+, Jan. 2002.

[11] S. O. Nelson, S. Trabelsi, and A. W. Kraszewski, "RF Sensing of Grain and Seed Moisture Content," IEEE Sensors Journal, vol. 1, no. 2, pp. 119-126, Aug. 2001.

[12] P. M. Johnson, D. V. Thiel, and D. A. James, "Contributions to the Measured Capacitance by the Dielectric Properties of Water in Insulated Electrode Soil Moisture Sensors," Sensors Proceedings of IEEE, vol. 1, 2002, pp. 495-498.

[13] S. Simula, S. Ikalailen, K. Niskanen, T. Varpula, H. Seppa, and A. Paukku, "Measurement of the Dielectric Properties of Paper," Imaging Science and Technology, vol. 43, no. 5, pp. 472-477, 1999.

[14] A. V. Mamishev, Y. Du, B. C. Lesieutre, and M. Zahn, "Measurement of Moisture Spatial Profiles in Transformer Pressboard," IEEE Conference on Electrical Insulation and Dielectric Phenomena, Atlanta, GA, 1998, pp. 323-326.

[15] H. Beving and G. Eriksson, "Dielectric-Spectroscopy of Human Blood," European Journal of Surgery, pp. 87-89, 1994.

[16] K. Asami, T. Yonezawa, H. Wakamatsu, and N. Koyanagi, "Dielectric Spectroscopy of Biological Cells," Bioelectrochemistry and Bioenergetics, vol. 40, no. 2, pp. 141-145, Aug. 1996.

[17] D. D. Denton, J. B. Camou, and S. D. Senturia, "Effects of Moisture Uptake on the Dielectric Permittivity of Polyimide Films," Proceedings of the 1985 International Symposium on Moisture and Humidity, Washington, D.C, 1985, pp. 505-513.

[18] I. C. Shay and M. Zahn, "Cylindrincal Geometry Electroquasistatic Dielectrometry Sensors," IEEE Conference on Electrical Insulation and Dielectric Phenomena, 2002, pp. 126-129.

[19] A. V. Mamishev, Y. Du, B. C. Lesieutre, and M. Zahn, "Development and Applications of Fringing Electric Field Sensors and Parameter Estimation Algorithms," Journal of Electrostatics, pp. 109-123, 1999.

[20] A. K. Jonscher, Universal Relaxation Law, Chelsea Dielectrics Press London, 1996.

[21] A. R. von Hippel, Dielectrics and Waves, John Wiley & Sons, 1954.

[22] A. K. Jonscher, Dielectric Relaxation in Solids, Chelsea Dielectrics Press London, 1983.

[23] w. R. Westphal, "Permittivity, Distributed Circuits," in A. von Hippel (ed.) Dielectric materials and applications, Cambridge: The M.I.T. press, 1961, pp. 63-122.

[24] M. C. Zaretsky, P. Li, and J. R. Melcher, "Estimation Of Thickness, Complex Bulk Permittivity And Surface Conductivity Using Interdigital Dielectrometry," IEEE Transactions on Electrical Insulation, vol. 24, no. 6, pp. 1159-1166, Dec. 1989.

Page 127: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

114

[25] J. O. Simpson and S. A. Bidstrup, "Modeling Conductivity and Viscosity Changes During Epoxy Cure Using TEA DMA and DSC," Proceedings of the American Chemical Society Division of Polymeric Materials: Science and Engineering Fall Meeting, vol. 69, no. 3, pp. 451-452, 1993.

[26] M. C. Zaretsky, J. R. Melcher, and C. M. Cooke, "Moisture Sensing In Transformer Oil Using Thin-Film Microdielectrometry," IEEE Transactions on Electrical Insulation, vol. 24, no. 6, pp. 1167-1176, Dec. 1989.

[27] Y. K. Sheiretov and M. Zahn, "Dielectrometry Measurements of Moisture Dynamics in Oil-Impregnated Pressboard," IEEE Transactions on Dielectrics and Electrical Insulation, vol. 2, no. 3, pp. 329-351, June 1995.

[28] N. J. Goldfine, A. P. Washabaugh, J. V. Dearlove, and P. A. von Guggenberg, "Imposed Omega-k Magnetometer and Dielectrometer Applications," Review of Progress in Quantitative Nondestructive Evaluation, vol. 12, New York, 1993.

[29] M. C. Zaretsky, L. Mouayad, and J. R. Melcher, "Continuum Properties From Interdigital Electrode Dielectrometry," IEEE Transactions on Electrical Insulation, vol. 23, no. 6, pp. 897-917, Dec. 1988.

[30] J. Melcher, Y. Daben, and G. Arlt, "Dielectric Effects of Moisture in Polyimide," IEEE Transactions on Electrical Insulation, vol. 24, no. 1, pp. 31-38, Feb. 1989.

[31] P. A. von Guggenberg and M. C. Zaretsky, "Estimation of One-Dimensional Complex-Permittivity Profiles: a Feasibility Study," Journal of Electrostatics, vol. 34, no. 2-3, pp. 263-277, Mar. 1995.

[32] P. Li, "Low Frequency, Millimeter Wavelength, Interdigital Dielectrometry of Insulating Media in a Transformer Environment," Master of Science Thesis, Department of Electrical Engineering and Computer Science, Massachusetts Institute of Technology, Cambridge, MA, 1987.

[33] N. F. Sheppard, D. R. Day, H. L. Lee, and S. D. Senturia, "Microdielectrometry," Sensors and Actuators, vol. 2, no. 3, pp. 263-274, July 1982.

[34] A. V. Mamishev, B. C. Lesieutre, and M. Zahn, "Optimization of Multi-Wavelength Interdigital Dielectrometry Instrumentation and Algorithms," IEEE Transactions on Dielectrics and Electrical Insulation, pp. 408-420, 1998.

[35] M. C. Zaretsky, "Parameter Estimation Using Microdielectrometry with Application to Transformer Monitoring," Ph.D. Thesis, Department of Electrical Engineering and Computer Science, Massachusetts Institute of Technology, Cambridge, MA, 1987.

[36] A. V. Mamishev, B. A. Berdnikov, J. P. Rivenc, B. C. Lesieutre, and M. Zahn, "Surface Contact Effects in Interdigital Dielectrometry," 10th International Symposium on High Voltage Engineering, vol. 6, Montreal, Canada, 1997, pp. 357-360.

Page 128: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

115

[37] S. D. Senturia, N. F. Sheppard, S. Y. Poh, and H. R. Appelman, "The Feasibility of Electrical Monitoring of Resin Cure With the Charge-Flow Transistor," Polymer Engineering and Science, vol. 21, no. 2, pp. 113-118, Feb. 1981.

[38] J. R. Melcher, "Electrohydrodynamic Surface Waves," Waves on Fluid Interfaces, Academic Press: New York, NY, 1983, pp. 167-200.

[39] S. M. Gasworth, J. R. Melcher, and M. Zahn, "Induction Sensing of Electrokinetic Streaming Current," Conference on Interfacial Phenomena In Practical Insulating Systems, National Bureau of Standards, Gaithersburg, MD, 1983.

[40] J. R. Melcher, "Charge Relaxation on a Moving Liquid Interface," Physics of Fluids, no. 10, pp. 325-331, 1967.

[41] J. C. Zuercher and J. R. Melcher, "Double-Layer Transduction At a Mercury-Electrolyte Interface With Imposed Temporal and Spatial Periodicity," Journal of Electrostatics, vol. 5, pp. 21-31, Oct. 1978.

[42] G. Brasseur, "Design Rules for Robust Capacitive Sensors," IEEE Transactions on Instrumentation and Measurement, vol. 52, no. 4, pp. 1261-1265, 2003.

[43] C. W. Coln, "A High Performance Dielectric Measurement System," Ph.D. Dissertation, Department of Electrical Engineering and Computer Science, Massachusetts Institute of Technology, Cambridge, MA, 1985.

[44] O. Isaksen, "A Review of Reconstruction Techniques for Capacitance Tomography," Measurement Science & Technology, vol. 7, no. 3, pp. 325-337, 1996.

[45] W. C. Heerens, "Application of Capacitance Techniques in Sensor Design," Journal of Physics E-Scientific Instruments, vol. 19, no. 11, pp. 897-906, 1986.

[46] J. C. Newell, Y. Peng, P. M. Edic, R. S. Blue, H. Jain, and R. T. Newell, "Effect of Electrode Size on Impedance Images of Two- and Three-Dimensional Objects," IEEE Transactions on Biomedical Engineering, vol. 45, no. 4, pp. 531-534, 1998.

[47] N. Polydorides and H. McCann, "Electrode Configurations for Improved Spatial Resolution in Electrical Impedance Tomography," Measurement Science & Technology, vol. 13, no. 12, pp. 1862-1870, 2002.

[48] A. V. Mamishev, K. Sundara-Rajan, F. Yang, Y. Q. Du, and M. Zahn, "Interdigital Sensors and Transducers," Proceedings of the IEEE, vol. 92, no. 5, pp. 808-845, May 2004.

[49] H. X. Wang, W. L. Yin, W. Q. Yang, and M. S. Beck, "Optimum Design of Segmented Capacitance Sensing Array for Multi-Phase Interface Measurement," Measurement Science & Technology, vol. 7, no. 1, pp. 79-86, 1996.

[50] A. J. Jaworski and G. T. Bolton, "The Design of an Electrical Capacitance Tomography Sensor for Use With Media of High Dielectric Permittivity," Measurement Science & Technology, vol. 11, no. 6, pp. 743-757, 2000.

Page 129: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

116

[51] W. Q. Yang and L. H. Peng, "Image Reconstruction Algorithms for Electrical Capacitance Tomography," Measurement Science and Technology, vol. 14, pp. R1-R13, 2003.

[52] M. D. Benadda, J. C. Carru, and C. Druon, "A Measuring Device for the Determination of the Electric Permittivity of Materials in the Frequency-Range 0.1-300 Mhz," Journal of Physics E-Scientific Instruments, vol. 15, no. 1, pp. 132-136, 1982.

[53] S. M. Huang, A. L. Stott, R. G. Green, and M. S. Beck, "Electronic Transducers for Industrial Measurement of Low Value Capacitances," Journal of Physics E - Scientific Instruments, vol. 21, no. 3, pp. 242-250, 1988.

[54] A. H. Sayed and S. Chandrasekaran, "Parameter Estimation With Multiple Sources and Levels of Uncertainties," IEEE Transactions on Signal Processing, vol. 48, no. 3, pp. 680-692, 2000.

[55] A. V. Mamishev, A. R. Takahashi, Y. Du, B. C. Lesieutre, and M. Zahn, "Parameter Estimation in Dielectrometry Measurements," Journal of Electrostatics, vol. 56, pp. 465-492, 2002.

[56] R. Courteau and T. K. Bose, "Dielectric Measurements With A Resonance Method for Comparing Low-Value 3-Terminal Capacitors," Review of Scientific Instruments, vol. 58, no. 6, pp. 1096-1103, June 1987.

[57] N. F. Sheppard Jr, S. L. Garverick, D. R. Day, and S. D. Senturia, "Microdielectrometry: a New Method for In Situ Cure Monitoring," Proceedings of the 26th SAMPE Symposium, Los Angeles, CA, 1981, pp. 65-76.

[58] V. Shtrauss, A. Kalpinsh, U. Lomanovskis, and J. Rotbahs, "Tomographic Imaging By Electrical Methods," Latvian Journal of Physics and Technical Sciences, no. 3, pp. 23-47, 1995.

[59] S. M. Huang, A. L. Stott, R. G. Green, and M. S. Beck, "Electronic Transducers for Industrial Measurement of Low Value Capacitances," Journal of Physics E - Scientific Instruments, vol. 21, no. 3, pp. 242-250, 1988.

[60] S. H. Khan and F. Abdullah, "Finite-Element Modeling of Multielectrode Capacitive Systems for Flow Imaging," IEE Proceedings-G Circuits Devices and Systems, vol. 140, no. 3, pp. 216-222, 1993.

[61] M. H. W. Bonse, C. Mul, and J. W. Spronck, "Finite-Element Modeling As A Tool for Designing Capacitive Position Sensors," Sensors and Actuators A-Physical, vol. 46, no. 1-3, pp. 266-269, 1995.

[62] X. J. Li, G. deJong, and G. C. M. Meijer, "The Application of the Capacitor's Physics to Optimize Capacitive Angular-Position Sensors," IEEE Transactions on Instrumentation and Measurement, vol. 46, no. 1, pp. 8-14, 1997.

[63] S. H. Khan, L. Finkelstein, and F. Abdullah, "Investigation of the Effects of Design Parameters on Output Characteristics of Capacitive Angular Displacement Sensors by

Page 130: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

117

Finite Element Field Modeling," IEEE Transactions on Magnetics, vol. 33, no. 2, pp. 2081-2084, 1997.

[64] S. S. Gevorgian, T. Martinsson, P. L. J. Linner, and E. L. Kollberg, "CAD Models for Multilayered Substrate Interdigital Capacitors," IEEE Transactions on Microwave Theory and Techniques, vol. 44, no. 6, pp. 896-904, June 1996.

[65] R. Igreja and C. J. Dias, "Analytical Evaluation of the Interdigital Electrodes Capacitance for a Multi-Layered Structure," Sensors and Actuators A-Physical, vol. 112, no. 2-3, pp. 291-301, 2004.

[66] X. J. Li, G. de Jong, and G. C. M. Meijer, "The Influence of Electric-Field Bending on the Nonlinearity of Capacitive Sensors," IEEE Transactions on Instrumentation and Measurement, vol. 49, no. 2, pp. 256-259, 2000.

[67] N. Boules and T. W. Nehl, "Design Optimization of Glass-Embedded Capacitive-Type Water Sensors," IEEE Transactions on Industry Applications., vol. 24, no. 3, pp. 402-410, 1988.

[68] K. J. Elkow and K. S. Rezkallah, "Void Fraction Measurements in Gas-Liquid Flows Under 1-g and Mu-g Conditions Using Capacitance Sensors," International Journal of Multiphase Flow, vol. 23, no. 5, pp. 815-829, 1997.

[69] M. Craig, "Dielectric Spectroscopy As a Novel Analytical Technique Within the Pharmaceutical Sciences," STP-Pharma-Pratiques, vol. 5, no. 6, pp. 421-42, 1995.

[70] K. Sundara-Rajan, L. Byrd, and A. V. Mamishev, "Moisture Content Estimation in Paper Pulp Using Fringing Field Impedance Spectroscopy," IEEE Sensors Journal, pp. 378-383, 2004.

[71] A. A. Ogale, M. C. Hegg, A. Mescher, A. V. Mamishev, and B. Minae, "Fill Front Detection Using Dielectric Sensors In Resin Transfer Molding Processes," International Conference on Composites/Nano Engineering, 2003, pp. 529-530.

[72] C. W. Lee, B. P. Rice, M. Buczek, and D. Mason, "Resin Transfer Process Monitoring and Control," SAMPE Journal, vol. 34, no. 6, pp. 48-55, Nov. 1998.

[73] A. V. Mamishev, A. R. Takahashi, Y. Du, B. C. Lesieutre, and M. Zahn, "Assessment of Performance of Fringing Electric Field Sensor Arrays," IEEE Conference on Electrical Insulation and Dielectric Phenomena, 2002, pp. 918-921.

[74] A. V. Mamishev, Y. Du, J. H. Bau, B. C. Lesieutre, and M. Zahn, "Evaluation of Diffusion-Driven Material Property Profiles Using Three-Wavelength Interdigital Sensor," IEEE Transactions on Dielectrics and Electrical Insulation, vol. 8, no. 5, pp. 785-798, Oct. 2001.

[75] J. G. Webster, The Measurement, Instrumentation, and Sensors Handbook, The CRC PRESS, IEEE PRESS, 1999.

Page 131: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

118

[76] R. Pallas-Areny and J. G. Webster, Sensors and Signal Conditioning, 2nd ed., John Wiley & Sons., 2001.

[77] G. Demoment, "Image-Reconstruction and Restoration - Overview of Common Estimation Structures and Problems," IEEE Transactions on Acoustics Speech and Signal Processing, vol. 37, no. 12, pp. 2024-2036, 1989.

[78] A. V. Mamishev, "Interdigital Dielectrometry Sensor Design and Parameter Estimation Algorithms for Nondestructive Materials Evaluation," Ph.D. Dissertation, Department of Electrical Engineering and Computer Science, Massachusetts Institute of Technology, Cambridge, MA, 1999.

[79] J. G. Webster, "Electrodes," in J. G. Webster (ed.) Electrical Impedance Tomography, Bristol and New York: Adam Hilger, 1990, pp. 21-28.

[80] D. M. G. Preethichandra and K. Shida, "A Simple Interface Circuit to Measure Very Small Capacitance Changes in Capacitive Sensors," IEEE Transactions on Instrumentation and Measurement, vol. 50, no. 6, pp. 1583-1586, 2001.

[81] R. Pallas-Areny and J. G. Webster, Sensors and Signal Conditioning, 2nd ed., John Wiley & Sons., 2001.

[82] G. Demoment, "Image-Reconstruction and Restoration - Overview of Common Estimation Structures and Problems," IEEE Transactions on Acoustics Speech and Signal Processing, vol. 37, no. 12, pp. 2024-2036, 1989.

[83] A. V. Mamishev, "Interdigital Dielectrometry Sensor Design and Parameter Estimation Algorithms for Nondestructive Materials Evaluation," Ph.D. Dissertation, Department of Electrical Engineering and Computer Science, Massachusetts Institute of Technology, Cambridge, MA, 1999.

[84] J. G. Webster, "Electrodes," in J. G. Webster (ed.) Electrical Impedance Tomography, Bristol and New York: Adam Hilger, 1990, pp. 21-28.

[85] W. Q. Yang, A. L. Stott, and M. S. Beck, "High-Frequency and High-Resolution Capacitance Measuring Circuit for Process Tomography," IEE Proceedings - Circuits Devices and Systems, vol. 141, no. 3, pp. 215-219, 1994.

[86] A. von Hippel, Dielectric Materials and Applications, Artech House, 1995.

[87] R. S. Chen, X. Zhang, K. F. Tsang, and K. N. Yung, "Modeling and Design of Interdigital Capacitor Based on Neural Networks and Genetic Algorithm," Microwave and Optical Technology Letters, vol. 38, no. 3, pp. 231-235, Aug. 2003.

[88] D. Isaacson, J. Mueller, and S. Siltanen, "Biomedical Applications of Electrical Impedance Tomography," Physiological Measurement, vol. 24, no. 2, May 2003.

[89] W. Daily, A. Ramirez, and A. Binley, "Remote Monitoring of Leaks in Storage Tanks Using Electrical Resistance Tomography: Application at the Hanford Site," Journal of Environmental and Engineering Geophysics, vol. 9, no. 1, pp. 11-24, Mar. 2004.

Page 132: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

119

[90] C. G. Xie, N. Reinecke, M. S. Beck, D. Mewes, and R. A. Williams, "Electrical Tomography Techniques for Process Engineering Applications," Chemical Engineering Journal and the Biochemical Engineering Journal, vol. 56, no. 3, pp. 127-133, 1995.

[91] C. G. Xie, S. M. Huang, B. S. Hoyle, R. Thorn, C. Lenn, D. Snowden, and M. S. Beck, "Electrical Capacitance Tomography for Flow Imaging - System Model for Development of Image-Reconstruction Algorithms and Design of Primary Sensors," IEE Proceedings-G Circuits Devices and Systems, vol. 139, no. 1, pp. 89-98, 1992.

[92] M. Cheney, D. Isaacson, and J. C. Newell, "Electrical Impedance Tomography," SIAM Review, vol. 41, no. 1, pp. 85-101, Mar. 1999.

[93] A. N. Tikhonov, Solutions of ill-posed problems, Washington; Winston; New York; Halsted Press, 1977.

[94] W. R. B. Lionheart, "EIT Reconstruction Algorithms: Pitfalls, Challenges and Recent Developments," Physiological Measurement, vol. 25, no. 1, pp. 125-142, Feb. 2004.

[95] M. Vauhkonen, D. Vadasz, P. A. Karjalainen, E. Somersalo, and J. P. Kaipio, "Tikhonov Regularization and Prior Information in Electrical Impedance Tomography," IEEE Transactions on Medical Imaging, vol. 17, no. 2, pp. 285-293, 1998.

[96] P. C. Hansen, "Analysis of Discrete Ill-Posed Problems by Means of the L-Curve," SIAM Review, vol. 34, no. 4, pp. 561-580, 1992.

[97] W. R. B. Lionheart, "Boundary Shape and Electrical Impedance Tomography," Inverse Problems, vol. 14, no. 1, pp. 139-147, 1998.

[98] J. P. Kaipio, V. Kolehmainen, M. Vauhkonen, and E. Somersalo, "Inverse Problems With Structural Prior Information," Inverse Problems, vol. 15, no. 3, pp. 713-729, 1999.

[99] D. Isaacson, "Distinguishability of Conductivities by Electric-Current Computed-Tomography," IEEE Transactions on Medical Imaging, vol. 5, no. 2, pp. 91-95, June 1986.

[100] B. M. Eyuboglu and T. C. Pilkington, "Comments on Distinguishability in Electrical-Impedance Imaging," IEEE Transactions on Biomedical Engineering, vol. 40, no. 12, pp. 1328-1330, Dec. 1993.

[101] J. Sylvester and G. Uhlmann, "A Global Uniqueness Theorem for an Inverse Boundary-Value Problem," Annals of Mathematics, vol. 125, no. 1, pp. 153-169, Jan. 1987.

[102] L. Borcea, "Electrical Impedance Tomography," Inverse Problems, vol. 18, no. 4, pp. 99-136, 2002.

[103] K. Paulson, W. Breckon, and M. Pidcock, "Electrode Modeling in Electrical-Impedance Tomography," SIAM Journal on Applied Mathematics, vol. 52, no. 4, pp. 1012-1022, 1992.

Page 133: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

120

[104] N. Hyvonen, "Complete Electrode Model of Electrical Impedance Tomography: Approximation Properties and Characterization of Inclusions," SIAM Journal on Applied Mathematics, vol. 64, no. 3, pp. 902-931, 2004.

[105] K. S. Cheng, D. Isaacson, J. C. Newell, and D. G. Gisser, "Electrode Models for Electric-Current Computed-Tomography," IEEE Transactions on Biomedical Engineering, vol. 36, no. 9, pp. 918-924, 1989.

[106] A. M. Bruckstein and T. Kailath, "Inverse Scattering for Discrete Transmission-Line Models," SIAM Review, vol. 29, no. 3, pp. 359-389, 1987.

[107] J. Frolik, "On the Feasibility of Impulse Reflection Response Data From One-Dimensional Multilayered Lossy Media," IEEE Transactions on Antennas and Propagation, vol. 51, no. 2, pp. 184-194, 2003.

[108] A. E. Yagle and J. L. Frolik, "On the Feasibility of Impulse Reflection Response Data for the Two-Dimensional Inverse Scattering Problem," IEEE Transactions on Antennas and Propagation, vol. 44, no. 12, pp. 1551-1564, 1996.

[109] A. E. Yagle, "A Layer Stripping Fast Algorithm for the Two-Dimensional Direct-Current Inverse Resistivity Problem," IEEE Transactions on Geoscience and Remote Sensing, vol. 25, no. 5, pp. 558-563, 1987.

[110] A. E. Yagle, "Discrete Layer-Stripping Algorithms and Feasibility Conditions for the 2D Inverse Conductivity Problem," Inverse Problems, vol. 16, no. 5, pp. 1157-1171, 2000.

[111] B. C. Levy, "Layer by Layer Reconstruction Methods for the Earth Resistivity From Direct-Current Measurements," IEEE Transactions on Geoscience and Remote Sensing, vol. 23, no. 6, pp. 841-850, 1985.

[112] E. Somersalo, M. Cheney, D. Isaacson, and E. Isaacson, "Layer Stripping - A Direct Numerical-Method for Impedance Imaging," Inverse Problems, vol. 7, no. 6, pp. 899-926, 1991.

[113] C. N. G. Scotter, "Non-Destructive Spectroscopic Techniques for the Measurement of Food Quality," Trends in Food Science & Technology, vol. 8, no. 9, pp. 285-292, 1997.

[114] I. L. Pykett, "NMR - A Powerful Tool for Industrial Process Control and Quality Assurance," IEEE Transactions on Applied Superconductivity, vol. 10, no. 1, pp. 721-723, 2000.

[115] M. Blanco and I. Villarroya, "NIR Spectroscopy: a Rapid-Response Analytical Tool," Trac-Trends in Analytical Chemistry, vol. 21, no. 4, pp. 240-250, 2002.

[116] B. osborne, "Near-infrared spectroscopy in food analysis," 2006. Encyclopedia of Analytical Chemistry.

[117] E. C. Y. Lichan, "The Applications of Raman Spectroscopy in Food Science," Trends in Food Science & Technology, vol. 7, no. 11, pp. 361-370, 1996.

Page 134: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

121

[118] B. J. Marquardt and J. P. Wold, "Raman Analysis of Fish: a Potential Method for Rapid Quality Screening," Lebensmittel-Wissenschaft Und-Technologie-Food Science and Technology, vol. 37, no. 1, pp. 1-8, 2004.

[119] D. Knorr, M. Zenker, V. Heinz, and D. U. Lee, "Applications and Potential of Ultrasonics in Food Processing," Trends in Food Science & Technology, vol. 15, no. 5, pp. 261-266, 2004.

[120] M. N. K. Prakash and K. V. R. Ramana, "Ultrasound and Its Application in the Food Industry," Journal of Food Science and Technology-Mysore, vol. 40, no. 6, pp. 563-570, 2003.

[121] R. Saggin and J. N. Coupland, "Non-Contact Ultrasonic Measurements in Food Materials," Food Research International, vol. 34, no. 10, pp. 865-870, 2001.

[122] E. Ibanez and A. Cifuentes, "New Analytical Techniques in Food Science," Critical Reviews in Food Science and Nutrition, vol. 41, no. 6, pp. 413-450, 2001.

[123] T. P. Labuza and C. R. Hayman, "Moisture Migration and Control in Multi-Domain Foods," Trends in Food Science and Technology, vol. 9, pp. 47-55, 1998.

[124] C. H. Mannheim, J. X. Liu, and S. G. Gilbert, "Control of Water in Foods During Storage," Journal of Food Engineering, vol. 22, no. 1-4, pp. 509-532, 1994.

[125] B. S. Mohamed, R. Z. Morawski, A. W. Kraszewski, A. Brawicz, and S. O. Nelson, "Calibration of a Microwave System for Measuring Grain Moisture Content," IEEE Transactions on Instrumentation and Measurements, vol. 48, no. 3, pp. 778-783, June 1999.

[126] A. K. Vijh, "Electrochemical Nature of Metal-Insulator Interfaces," IEEE International Symposium on Electrical Insulation, Montreal, Que., Canada, 1996, pp. 870-873.

[127] E. N. Lewis, J. Schoppelrei, and E. Lee, "Molecular Spectroscopy Workbench - Near-Infrared Chemical Imaging and the PAT Initiative," Spectroscopy, vol. 19, no. 4, pp. 26-+, 2004.

[128] O. Berntsson, L. G. Danielsson, B. Lagerholm, and S. Folestad, "Quantitative in-Line Monitoring of Powder Blending by Near Infrared Reflection Spectroscopy," Powder Technology, vol. 123, no. 2-3, pp. 185-193, 2002.

[129] A. S. El-Hagrasy and J. K. Drennen, III, "A Process Analytical Technology Approach to Near-Infrared Process Control of Pharmaceutical Powder Blending. Part III: Quantitative Near-Infrared Calibration for Prediction of Blend Homogeneity and Characterization of Powder Mixing Kinetics," Journal of Pharmaceutical Sciences, vol. 95, no. 2, pp. 422-434, Feb. 2006.

[130] G. J. Vergote, T. R. M. De Beer, C. Vervaet, J. P. Remon, W. R. G. Baeyens, N. Diericx, and F. Verpoort, "In-Line Monitoring of a Pharmaceutical Blending Process Using FT-Raman Spectroscopy," European Journal of Pharmaceutical Sciences, vol. 21, no. 4, pp. 479-485, 2004.

Page 135: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

122

[131] J. Rantanen, E. Rasanen, J. Tenhunen, M. Kansakoski, J. P. Mannermaa, and J. Yliruusi, "In-Line Moisture Measurement During Granulation With a Four-Wavelength Near Infrared Sensor: an Evaluation of Particle Size and Binder Effects," European Journal of Pharmaceutics and Biopharmaceutics, vol. 50, no. 2, pp. 271-276, 2000.

[132] R. L. Green, G. Thurau, N. C. Pixley, A. Mateos, R. A. Reed, and J. P. Higgins, "In-Line Monitoring of Moisture Content in Fluid Bed Dryers Using Near-IR Spectroscopy With Consideration of Sampling Effects on Method Accuracy," Analytical Chemistry, vol. 77, no. 14, pp. 4515-4522, 2005.

[133] T. A. Lestander and C. Rhen, "Multivariate NIR Spectroscopy Models for Moisture, Ash and Calorific Content in Biofuels Using Bi-Orthogonal Partial Least Squares Regression," Analyst, vol. 130, no. 8, pp. 1182-1189, Aug. 2005.

[134] J. Rantanen, S. Lehtola, P. Ramet, J. P. Mannermaa, and J. Yliruusi, "On-Line Monitoring of Moisture Content in an Instrumented Fluidized Bed Granulator With a Multi-Channel NIR Moisture Sensor," Powder Technology, vol. 99, no. 2, pp. 163-170, 1998.

[135] J. G. White, "Online Moisture Detection for A Microwave Vacuum Dryer," Pharmaceutical Research, vol. 11, no. 5, pp. 728-732, 1994.

[136] A. Gupta, G. E. Peck, R. W. Miller, and K. R. Morris, "Real-Time Near-Infrared Monitoring of Content Uniformity, Moisture Content, Compact Density, Tensile Strength, and Young's Modulus of Roller Compacted Powder Blends," Journal of Pharmaceutical Sciences, vol. 94, no. 7, pp. 1589-1597, 2005.

[137] M. Blanco and M. Alcala, "Content Uniformity and Tablet Hardness Testing of Intact Pharmaceutical Tablets by Near Infrared Spectroscopy - A Contribution to Process Analytical Technologies," Analytica Chimica Acta, vol. 557, no. 1-2, pp. 353-359, 2006.

[138] W. Bonawi-Tan and J. A. S. Williams, "Online Quality Control With Raman Spectroscopy in Pharmaceutical Tablet Manufacturing," Journal of Manufacturing Systems, vol. 23, no. 4, pp. 299-308, 2004.

[139] M. Donoso, D. O. Kildsig, and E. S. Ghaly, "Prediction of Tablet Hardness and Porosity Using Near-Infrared Diffuse Reflectance Spectroscopy As a Nondestructive Method," Pharmaceutical Development and Technology, vol. 8, no. 4, pp. 357-366, 2003.

[140] J. Petri, A. Kaunzinger, A. Niemoller, and M. Karas, "Quality Control of Tablets by Near Infrared (NIR)-Spectroscopy," Pharmazie, vol. 60, no. 10, pp. 743-746, Oct. 2005.

[141] S. Romero-Torres, J. D. Perez-Ramos, K. R. Morris, and E. R. Grant, "Raman Spectroscopic Measurement of Tablet-to-Tablet Coating Variability," Journal of Pharmaceutical and Biomedical Analysis, vol. 38, no. 2, pp. 270-274, 2005.

[142] S. Romero-Torres, J. D. Perez-Ramos, K. R. Morris, and E. R. Grant, "Raman Spectroscopy for Tablet Coating Thickness Quantification and Coating Characterization in the Presence of Strong Fluorescent Interference," Journal of Pharmaceutical and Biomedical Analysis, vol. 41, no. 3, pp. 811-819, 2006.

Page 136: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

123

[143] C. Abrahamsson, J. Johansson, S. ndersson-Engels, S. Svanberg, and S. Folestad, "Time-Resolved NIR Spectroscopy for Quantitative Analysis of Intact Pharmaceutical Tablets," Analytical Chemistry, vol. 77, no. 4, pp. 1055-1059, Feb. 2005.

[144] S. Wartewig and R. H. Neubert, "Pharmaceutical Applications of Mid-IR and Raman Spectroscopy," Advanced Drug Delivery Reviews, vol. 57, no. 8, pp. 1144-1170, June 2005.

[145] D. Q. M. Craig, Dielectric Analysis of Pharmaceutical Systems, Taylor & Francis Group, 1995.

[146] Y. Mouget, P. Gosselin, M. Tourigny, and S. Bechard, "Three-Dimensional Analyses of Tablet Content and Film Coating Uniformity by Laser-Induced Breakdown Spectroscopy (LIBS)," American Laboratory, vol. 35, no. 4, pp. 20-22, Feb. 2000.

[147] M. D. Mowery, R. Sing, J. Kirsch, A. Razaghi, S. Bechard, and R. A. Reed, "Rapid at-Line Analysis of Coating Thickness and Uniformity on Tablets Using Laser Induced Breakdown Spectroscopy," Journal of Pharmaceutical and Biomedical Analysis, vol. 28, no. 5, pp. 935-943, June 2002.

[148] J. D. Kirsch and J. K. Drennen, "Determination of Film-Coated Tablet Parameters by Near-Infrared Spectroscopy," Journal of Pharmaceutical and Biomedical Analysis, vol. 13, no. 10, pp. 1273-1281, Sept. 1995.

[149] J. D. Kirsch and J. K. Drennen, "Near-Infrared Spectroscopic Monitoring of the Film Coating Process," Pharmaceutical Research, vol. 13, no. 2, pp. 234-237, Feb. 1996.

[150] S. M. Jung, J. M. Nam, D. H. Yang, and M. K. Lee, "A CMOS Integrated Capacitive Fingerprint Sensor With 32-Bit RISC Microcontroller," IEEE Journal of Solid-State Circuits, vol. 40, no. 8, pp. 1745-1750, 2005.

[151] J. M. Nam, S. M. Jung, D. H. Yang, and M. K. Lee, "Design and Implementation of 160 x 192 Pixel Array Capacitive-Type Fingerprint Sensor," Circuits Systems and Signal Processing, vol. 24, no. 4, pp. 401-413, 2005.

[152] M. Tartagni and R. Guerrieri, "A Fingerprint Sensor Based on the Feedback Capacitive Sensing Scheme," IEEE Journal of Solid-State Circuits, vol. 33, no. 1, pp. 133-142, 1998.

Page 137: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

124

Appendix A: DiSPEC Hardware Installation Guide

List of Instruments

The instruments listed below are necessary for the dielectric spectroscopy system: • National Instruments PCI-GPIB, NI-488.2 with Cable • Tektronix AFG310 Arbitrary Function Generator • National Instruments PCI-6035E/PCI-6036E DAQ board • National Instruments BNC-2120 terminal block • National Instruments SH-68-68-EP shielded cable • Tektronix PS280 Triple Output Power Supply

The following is a complete list of the items provided by SEAL:

• 3-channel sensor-interface circuit • Two 2-channel fringing field electric sensors with connectors attached • A K-type thermocouple • Five SMA male – BNC male cables • 5-pin male – 3 Banana plug power cable for sensor-interface circuit • 5-pin male – single wire for relay-control signal connection • Two short stripped wires for power supply lead-to-lead connection • Kapton covers for sensor heads • DiSPEC custom software CD • A user’s manual

Installing the Hardware Step 1: Install the GPIB and the DAQ Cards

Plug the NI GPIB and the NI-DAQ boards into the experimental computer and install

all recommended drivers.

Step 2: Connect BNC-2120 to the DAQ Board

Page 138: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

125

Connect BNC-2120 breakout box to the DAQ card in the computer using the shielded

SH-68-68-EP cable.

Step 3: Connect Thermocouple to BNC-2120

Plug thermocouple into the thermocouple socket of the BNC-2120 breakout box.

Check that the row switches for ACH0 and ACH1 are set to the right, the “Temp.Ref.” and “Thermocouple” positions.

Page 139: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

126

Step 4: Connect the Sensor Box to BNC-2120 Attach the BNC-ends of four BNC-SMA cables to BNC-2120’s channels ACH2-

ACH5. The switches under all ACH connectors should be in GS position.

Switch ACH3 selector (above the thermocouple connector) to BNC position.

Using the BNC-SMA cables to connect the ADC0 to ADC3 terminals on the sensor interface box to the ACH2 to ACH5 of BNC-2120.

Page 140: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

127

Place the sensor interface box and the sensor as far away as possible from the

computer, the monitor and other electronic devices to minimize noise interference.

Step 5: Connect the Relay Control Lead to BNC-2120 Connect the relay-control wire from the “Cntrl.” socket of sensor interface box to

DIO0 of BNC-2120 using a 5-pin to single wire connector.

To connect the wire to BNC-2120 DIO0 port, untighten a screw (on the right), let the wire end into the hole and re-tighten the screw.

Page 141: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

128

Step 6: Set up the Power Supply To properly set the polarity of the power supply, two short wires should be

connecting the outputs as shown in the picture below:

Set the power supply to independent mode by adjusting the two buttons in the middle

of the front panel. Set the display-mode switches to Voltage position. The current dial should be set to the twelve-o’clock position (halfway). Use voltage dials to set both outputs to 10 volts. DO NOT CHANGE THE VOLTAGE SETTINGS WHILE THE SENSOR INTERFACE IS CONNECTED TO THE POWER SUPPLY! Once the voltage is set, connect the interface box to the power supply using 5-pin to 3 banana plug cable.

The plug labeled GND can be connected to either of the two ground sockets available on the power supply. Connect the “+” plug to the “+” terminal of the right 0-20V supply and “-“ plug to the “-“ terminal of the left 0-20V supply.

Page 142: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

129

Step 7: Connect the Function Generator Using the fifth BNC-SMA cable, connect the function generator to the sensor

interface box.

Use the GPIB cable to connect the function generator to the GPIB card in the computer. Note that you don’t need to change the settings of the function generator manually. The program DiSPEC will tell it what to do. AlWAYS TURN ON THE FUNCTION GENERATOR BEFORE OPENING the DiSPEC PROGRAM.

Step 8: Connect the Sensor to the Interface Box

Page 143: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

130

The sensor is connected to the interface as follows: The cable labeled as “drive” of the sensor is connected to any of the Drive terminals of the board. The ones labeled as “inner sense” and “outer sense” are connected to the S. 1 and S. 2 terminals on the sensor interface box respectively. DiSPEC software guide Installing the Software This LABVIEW application is for viewing data in real time as well as recording data to a file. Start by opening the DiSPEC folder on the CD. Go to folder “Installer” and double click on the “setup” icon. Follow the setup guide step by step and the software will be installed on your computer. After installation, the program will show up in your computer’s start up menu as DiSPEC. Using the Software After all the hardware is installed, go to the start up menu of your computer and open the program DiSPEC. The following steps need to be followed to run the software.

1. Connect all the instruments according to the instructions in the hardware guide. 2. Open the NI software “Measure & Automation Explorer” (MAX). (The software

should be provided the DAQ board). Find out the device number for the function generator and the DAQ board. Specific instructions are available below under Device Number of the Function Generator and the DAQ Board.

3. Go to the system settings tab in the front panel and enter the device numbers found from step 1. The same values need to be manually entered each time the program is opened if they are found to be different from the default values.

4. Find out the time delay for each channel of the circuit board. For detailed instructions, go to Time Delay.

5. Enter the time delay values obtained from step 3 in the system settings tab. Note that if found to be different from the default values, these time delay constants have to be reentered each time the program is opened.

6. Go to the Controls tab, and configure the entries in the tab. For detailed instructions, go to Controls.

7. Turn on the function generator and the power supply. 8. Press the “Run” and the “Acquire” button. If an arrow appears on the top left

corner of the front panel, click on the arrow and the program will start running. If the arrow doesn’t appear, the code should already be running after the “Run” and the “Acquire” button is pressed down.

9. Go to the different tabs on the front panel to look at the data and the graphs. 10. To monitor change in sample capacitance more visually, go to the Real-time

Imaging tab. 11. To stop the program, press the “Acquire” button again.

Page 144: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

131

Configure the System In the front panel, go to the “System Settings” tab, a window like the following will show up.

Upon starting LABVIEW, the 'System settings' has all its entry values set to their defaults for the 2 channel fringing field sensor. These default values should be used unless specified otherwise below. Description of the entries can be obtained by right-clicking on an entry and selecting “Descriptions and Tips” on the menu.

Device Number of the Function Generator and the DAQ Board The device numbers of the function generator and the DAQ board are dependent on the particular setup, therefore values different from those specified as default may need to be used. To get the device numbers, open the NI software “Measurement & Automation Explorer” that is provided with the DAQ board. Double click on “Devices and Interfaces”, the DAQ board and the NI GPIB card will show up. The number listed for the DAQ board is the device number for the DAQ and the number listed for the GPIB card is the device number for the function generator.

Channel Numbers on the DAQ board

Page 145: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

132

This entry specifies the channel numbers on the DAQ board that the input and the three output signals of the circuit are connected to. The default values are “2,3,4,5”. Channels 0 and 1 on the DAQ board are saved for the thermocouple. The first channel number is the input to the DAQ board, and the following numbers are output channels, displayed in front channel as channels 1, 2, and 3 respectively. All numbers must be separated by commas. (Channel 3 is most often used in the parallel plate setup rather than the fringing field system)

Reference Capacitance The “Reference Capacitance” entries specify the reference capacitance used for each channel of the sensor circuit board. Note that these values are not the same as the values of the reference capacitors on the board. The effect of the stray capacitances (e.g. that introduced by the Op-Amp has to be accounted for.) The default values are obtained through careful calibration of the system. These values should be used unless some circuit elements are changed. Recalibration of the system is necessary if changes are made to the circuit.

Time Delay Multiplexing of the DAQ board introduces a time delay between the data stream from its different channels. The time delay causes significant phase distortion, therefore its effect has to be eliminated. Unfortunately, the time delay values are device dependent. A different computer and DAQ board will cause a change in these values, which means that these values have to be fine-tuned for each particular setup. The following procedure can be used to find the time delay constants:

1. Connect the input and all the outputs of the circuit board to the function generator. Note that since all channels are connected to the same source, ideally there should be no phase delay between the channels.

2. Run the program at the highest frequency (30 kHz). Ideally, the gain should be 1 and the phase should be zero for all channels. Adjust the time delay for each channel of the sensor in the “systems and setting” tab until the phase delays for all channels are 0.

3. The new time delay constants must be typed in manually each time the program is started.

The Settings for the Thermocouple

Page 146: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

133

Channel 0 and 1 of the DAQ board should always be used for the thermocouple as is specified in the default setting. The sampling rate for the thermocouple could be increased if an improvement in the speed of the program is desired. Otherwise, use the default value. Averaging is used here to remove noise. The number of samples for temperature averaging can be changed for different application. Controls The controls tab should look like the following window.

Mass Real-time monitoring of sample mass is not necessary at this point. This function is included for possible future applications. By pressing the “mass” button down, the

Page 147: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

134

program will acquire data from a scale that is connected to the computer through a serial port.

Temperature A K type thermocouple is connected to the computer. By pressing the “Temperature” button down, the system starts acquiring data from the thermocouple and saving the temperature data to the output file if “Saving to file” is also enabled.

Sweep When the “Sweep” button is not pressed, the system runs at a single frequency specified by the “Start Frequency” entry. The system performs frequency sweeps when the “Sweep” button is enabled. The range of the frequency sweep is defined by the start and the stop frequency. The minimum and maximum frequencies allowed by the current version of the program are 1 Hz and 30 kHz respectively. Measurements at frequencies lower than 1 Hz are comparably noisy, thus we limit the frequency to above 1 Hz. The frequency range can be easily extended for future applications.

Save to File If you wish to record the data to a file, the “Save to File” button should be pressed down. You can enter the file name and the saving directory in the “File Name” entry. If the entry is left blank, a file saving window will automatically pop up when the program starts running. The file can be saved as an Excel spreadsheet or a ‘.txt’ file.

Real-time Imaging

The following is a picture of the real-time imaging tab.

Page 148: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

135

The tab provides a profile of the sample by displaying the capacitance of all channels of the sensor. Note that in a 2-channel fringing field setup, the information shown for channel 3 should be ignored. Channel 3 is included here mainly for the consideration that a 3-channel sensor might be used in the future. The capacitance values displayed in the vertical bars are all scaled to be within 0 to 1. The “Maximum Capacitance” knobs on the right refer to the actual capacitance value in “pF” when the bar displays a value of “1”. The knobs could be adjusted for the best visual effect.

Page 149: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

136

Appendix B: Matlab Code for the Layer Stripping Algorithm

% this code generates the data that feeds the layer stripping algorithm. % vector of the radius of the concentric discs function w = data_gen(N, d, sigma) K = length(d); % in this case K=4; w = zeros(N, K-1); % calculate the w_n(1), that is the w_n for the outer boundary for n = 1:N w(n, 1) = 1/n/sigma(1); for k = 2:K-1 L0 = (d(k)/d(k+1))^(2*n); L = n*sigma(k)*w(n, k-1); H = (1-L)/(1+L); L1 = L0*H; H = (1-L1)/(1+L1); w(n, k)=1/sigma(k)/n*H; end end

% this code solve the inverse problem of electrical % impedance imaging using the layer stripping algorithm. clear all %close all clc % this code takes matrix w as the input %format long % % d1 d2 d3 d4 % d = [0, 0.08, 0.6, 1]; % sig = [1, 1, 1]; % sig2 = [2, 1, 0.5];

Page 150: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

137

% sig3 = [0.5, 0.5, 2]; % N=16; % w = data_gen(N, d, sig2) % w2= data_gen(N, d, sig2) % w3 = data_gen(N, d, sig3) d1 = [0, 0.2, 1]; d2 = [0, 0.4, 1]; d3 = [0, 0.6, 1]; d4 = [0, 0.8, 1]; sig1 = [1, 1]; sig2 = [2, 1]; sig3 = [1, 2]; sig4 = [2, 2]; N=16; w11 = data_gen(N, d1, sig1); w21= data_gen(N, d2, sig1); w31 = data_gen(N, d3, sig1); w41 = data_gen(N, d4, sig1); w12 = data_gen(N, d1, sig2); w22= data_gen(N, d2, sig2); w32 = data_gen(N, d3, sig2); w42 = data_gen(N, d4, sig2); w13 = data_gen(N, d1, sig3); w23= data_gen(N, d2, sig3); w33 = data_gen(N, d3, sig3); w43 = data_gen(N, d4, sig3); w14 = data_gen(N, d1, sig4); w24= data_gen(N, d2, sig4); w34 = data_gen(N, d3, sig4); w44 = data_gen(N, d4, sig4); w = w42; [N, K]= size(w); % step 1, choose mode-drooping radii: alpha=0.2; H=10 n=1:H; %a = alpha+(1-alpha)/(N-1).*(N-1-n); %a = alpha.^(2./(N+1-n)); a=((H+1-n)./2*alpha^2).^(1./(N+1-n)); a=[1, a,0]; delta = 1e-2; L = length(a); % reconstruction at the boundary sigma(1) = a(1)/N/w(N,K);

Page 151: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

138

% iterate to reconstruct at the subsurface. a_p = a(1); w_p = w(:,K); sigma_p= sigma(1); n = (1:N)'; for h = 2:L while a_p > a(h) delta_w=delta/a_p.*(1/sigma_p-(n.^2).*sigma_p.*(w_p.^2)); w_p=w_p-delta_w; a_p = a_p-delta; sigma_p = a_p/16/w_p(N); end sigma(h)=sigma_p; %N=N-1; end sigma for i = 1:length(sigma); if abs(sigma(i))>5; sigma(i)=5; end end sigma plot(a, sigma, 'x-') grid on hold on

Page 152: Instrumentation and Inverse Problem Solving for Impedance ...Experimental results in the thesis demonstrate the viability of FEF dielectrometry as a process analytical sensing technique

139

Vita

Xiaobei Li received her B.S. degree in controls theory from Northwestern Polytechnical

University, Xi’an, China, in 1999; and a M.S. in Electrical Engineering from the

University of Washington, Seattle, in 2003. She joined the Sensors, Energy and

Automation Laboratory (SEAL) at the department of Electrical Engineering, University

of Washington at 2002 as a graduate research assistant. Her research interests include

dielectric spectroscopy sensor design, sensor signal conditioning circuit design, and

image reconstruction for soft-field sensing. Xiaobei Li is currently working for the

INTEL Corporation in Dupont, WA.