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2 nd International STEM in Education Conference 65 The Development of Physical Vapor Deposition Technology for Use in Experimental Zirconium Nitride Modules in Nanotechnology Courses Ming-Der Jean Department of Mechanical Engineering, Yung-Ta Institute of Technology & Commerce, Ping-Tung [email protected] Abstract: The use of sputtered deposition-based technology in nanotechnology modules in learning and teaching enriches engineering curricula. Nanotechnology courses with a laboratory platform that use physical vapor deposition implemented nanotechnology modules are helpful and enhancing, interesting and contain enough knowledge for students, which helps students to understand nanotechnology concepts and the applications of sputtered deposition-based systems. This project proposes experimental zirconium nitride modules in nanotechnology based on the magnetron sputtering system. This system elucidates the principles, experiments, examination and application of nanotechnology for students, who also learn how to use a sputtered deposition-based system to make experimental zirconium nitride modules. In addition, students can design a magnetron sputtering program to manufacture and control experimental zirconium nitride modules in nanotechnology courses. Furthermore, Students learn, verify and acquire lectured concepts by performing thin film experiments, using zirconium nitride modules, in the laboratory. The most important part of the system is the implementation of the nanotechnology experiments in laboratory sessions, using examples of zirconium nitride modules. The purpose of this project is to develop a sputtered deposition-based technology for implementing the zirconium nitride module experiments in nanotechnology course that supports teaching and learning in engineering education. Keywords Sputtered deposition-based system, magnetron sputtering; nanotechnology course, Questionnaire evaluations, zirconium nitride module 1. Introduction Nanotechnology is not a traditional discipline, but rather a combination of disciplines, involving physics, chemistry, biology, mathematics, engineering and technology (Smith, 1995). Nanotechnology offers cutting-edge applications that will revolutionize the way that disease is detected and treated, the way that the environment is, monitored and protected, energy is produced and stored, crop production and food quality is improved, and will be used to build complex structures as small as an electronic circuit or as large as an airplane(Wasa,2004). Nanotechnology is an essential topic in the current technological world and it has experienced an explosive growth in the last few years, which revolves around precursor materials, fabrication processes and characterization techniques, instrumentation and equipment, theoretical modeling and control and the design and integration of structures into devices and systems(Asmatulu et al., 2010; Roco, 2003; Jean et al., 2010). Nanotechnology has attracted much attention as a process for applying protective coatings in many engineering fields, such as semiconductors, optical devices, tribological functions, displays, decoration, solar power and medical technologies, where their surfaces generate functional layers by thermal spraying, hardening, physical vapor deposition, or

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Page 1: The Development of Physical Vapor Deposition Technology ...stem2012.bnu.edu.cn/data/long paper/stem2012_30.pdf · vacuum-coating techniques can be used to apply coatings that have

2nd

International STEM in Education Conference

65

The Development of Physical Vapor Deposition Technology for Use in

Experimental Zirconium Nitride Modules in Nanotechnology Courses

Ming-Der Jean

Department of Mechanical Engineering, Yung-Ta Institute of Technology & Commerce, Ping-Tung

[email protected]

Abstract: The use of sputtered deposition-based technology in nanotechnology modules in learning and teaching enriches

engineering curricula. Nanotechnology courses with a laboratory platform that use physical vapor deposition

implemented nanotechnology modules are helpful and enhancing, interesting and contain enough knowledge for students,

which helps students to understand nanotechnology concepts and the applications of sputtered deposition-based systems.

This project proposes experimental zirconium nitride modules in nanotechnology based on the magnetron sputtering

system. This system elucidates the principles, experiments, examination and application of nanotechnology for students,

who also learn how to use a sputtered deposition-based system to make experimental zirconium nitride modules. In

addition, students can design a magnetron sputtering program to manufacture and control experimental zirconium nitride

modules in nanotechnology courses. Furthermore, Students learn, verify and acquire lectured concepts by performing thin

film experiments, using zirconium nitride modules, in the laboratory. The most important part of the system is the

implementation of the nanotechnology experiments in laboratory sessions, using examples of zirconium nitride modules.

The purpose of this project is to develop a sputtered deposition-based technology for implementing the zirconium nitride

module experiments in nanotechnology course that supports teaching and learning in engineering education.

Keywords: Sputtered deposition-based system, magnetron sputtering; nanotechnology course, Questionnaire evaluations,

zirconium nitride module

1. Introduction

Nanotechnology is not a traditional discipline, but rather a combination of disciplines, involving physics, chemistry,

biology, mathematics, engineering and technology (Smith, 1995). Nanotechnology offers cutting-edge applications that

will revolutionize the way that disease is detected and treated, the way that the environment is, monitored and protected,

energy is produced and stored, crop production and food quality is improved, and will be used to build complex structures

as small as an electronic circuit or as large as an airplane(Wasa,2004). Nanotechnology is an essential topic in the current

technological world and it has experienced an explosive growth in the last few years, which revolves around precursor

materials, fabrication processes and characterization techniques, instrumentation and equipment, theoretical modeling and

control and the design and integration of structures into devices and systems(Asmatulu et al., 2010; Roco, 2003; Jean et al.,

2010). Nanotechnology has attracted much attention as a process for applying protective coatings in many engineering

fields, such as semiconductors, optical devices, tribological functions, displays, decoration, solar power and medical

technologies, where their surfaces generate functional layers by thermal spraying, hardening, physical vapor deposition, or

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other similar procedures that improve the surface properties and protect the materials from the environment. Of these,

vacuum-coating techniques can be used to apply coatings that have superior surface properties to those of any metal.

Currently, magnetron sputtering is widely preferred for physical vapor deposition technology, due to its greater deposition

efficiency and the reduction in waste of materials. In addition, magnetron sputtering is a useful technique for multilayer

deposition. This technique allows good control of deposition parameters during the deposition process. Almost all types of

materials, including metals, ceramics, polymers, and composites, can be deposited onto similar or dissimilar materials. In

particular, zirconium nitride coatings deposited using magnetron sputtering technologies have been extensively used in a

number of industries, since they can enhance substrate properties and improve surface qualities, for both attractiveness and

durability. Accordingly, physical vapor deposition technology for use in nanotechnology is a widely used technique and

there is a growing interest in engineering education.

Most of the cited literature and current authors on nanotechnology state that adding nanoscale perspectives to teaching

leads to a better fundamental understanding, sharing of similar concepts and courses in various disciplines and areas of

relevance and broader accessibility to science and technology, but not in systematically developing nanotechnology

courses(Corter et al., 2011; Hersam,2004). However, teaching of nanotechnology to undergraduates in science and

engineering can use simulation-based and hands-on educational laboratories. The user of a simulation has argued that

nanotechnology experiments are delicate, limited in availability and expensive to set up and maintain, so knowledge

concerning the best practices in nanoscale science education is limited and current educators are faced with fundamental

questions as to the nature of nanotechnology and where it fits into the already crowded, current curriculum? Conversely,

lectures are supported by laboratory work, where students carry out experiments. This enables them to practically apply the

knowledge they gain from the lecture. Meanwhile, several studies have highlighted the importance of bringing hands-on

experience to integrate nanotechnology into the undergraduate curriculum and several examples have brought practical

nanotechnology module fabrication into the undergraduate curriculum (Jara, 2011; Richard,1988; Felder etal.,1987).

Accordingly, the concept of experience by experimentation favors the introduction of hands-on nanotechnology modules

as an important role in engineering education. In addition, the development of a course in nanotechnology by experimental

instruments such as magnetron sputtering modules in a laboratory has been favorably reviewed in courses with a

significant number of practical activities, where the students could verify and practice all of the analytical concepts and

methods learnt in theoretical courses, in engineering education.

Recently, nanotechnology subjects have not always shown improvement, when classroom teaching is supported by

adequate laboratory courses and experiments, following the learning by doing paradigm, which provides students with a

deeper understanding of theoretical lessons (Mukhopadhyay et al., 2010; Asmatulu & Misak, 2011) It is believed that

developments in nanotechnology will likely change the traditional practices of design, analysis, simulation and

manufacturing of new engineering products. Students prefer a nanotechnology module over the traditional class courses. In

other words, labs for nanotechnology modules are an important academic setting for engineering students and provide

in-depth training in engineering education, as most graduate students majoring in science/engineering must conduct

experiments in a lab. However, the means by which students understand the importance of what they are doing and why

they are doing it is to engage in learning to feel that their experimental work that is valuable and worthy of their efforts.

This is important in a Lab, because cognitively, engagement in learning has been reported to be a robust indicator of

improved student achievement and behavior in engineering education. Moreover, researchers in the field of

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nanotechnology have noted, with alarm, the lack of systematic studies of the technology’s effects on engineering learning

outcomes. Accordingly, understanding the effects of the introduction of new technologies into education in the sciences,

particularly into science laboratory experiences, requires carefully designed study.

The purpose of this study is to emphasize the valuable support for teaching nanotechnologies that experimental

zirconium nitride modules can provide. This study develops an experimental nanotechnology module, using zirconium

nitride thin films that use the magnetron sputtering system at the Institute of Engineering Science and Technology at

National Kaohsiung First University of Science and Technology. This provides the students with a mechanism to observe,

collect, interpret and seek understanding of real-life situations, within the natural setting of the classroom. In this study,

three procedures support the laboratory platform, to provide students with experience in actually creating and

implementing a complete experimental manipulation program in nanotechnology modules. Firstly, the student gleans and

sorts various data and then integrates the experimental nanotechnology module via project work. Secondly, the student

operates a magnetron sputtering system and selects control parameters. Finally, it connects the nanotechnology module

with the magnetron sputtering system devices to produce an experimental nanotechnology course with a group of

integrated learning modules focused on zirconium nitride thin films. Furthermore, this article effectively develops

hands-on experimental nanotechnology modules for magnetron sputtering system fabrication for the undergraduate

curriculum, to offer hands-on experience and to integrate nanotechnology modules for students. The challenge for the

academic community is to imbue undergraduate engineers and science students with all the necessary knowledge to ensure

leadership in this emerging field.

2. Literature Review

Experimentation in an engineering laboratory is one of the most important experiences for undergraduate students,

because it allows them to observe and explore real-world applications of fundamental theories and to develop a deep

understanding of theoretical lessons (Winkelman et al.,2009). Firstly, laboratory instruction helps students develop their

experimental skills and the ability to work in teams, to learn to communicate effectively, to learn from failure and to be

responsible for their own results. Thus, the role of experimentation is a key concept in the education world, particularly in

science and engineering disciplines such as nanotechnology, where practical operation and experience can only be

provided to students by using real equipment such as an industrial physical vapor deposition system or nanotechnology

devices(Nichol and Hutchinson, 2010), which provide a systematic curriculum and effectively assist students to reach a

holistic and meaningful understanding with the application of a knowledge map and curriculum-integrated teaching. In

other words, the implementation of experimentation provides an overview of the engineering knowledge, helping students

to integrate their learning through different courses. Moreover, the knowledge can be represented as an element which is

composed of many of the fundamental knowledge elements that have a complex relationship (Hofstein, et al., 2004). In

engineering education, helping students to associate a lot of theories with different knowledge is a big challenge.

Experimentation in an engineering laboratory is an important resource for students. However, real laboratories cannot be

substituted with some simulated tools, especially in fields such as nanotechnology, in which the actual behavior and

response of the real elements in the experiments is crucial. Recently, nanotechnology teaching has greatly improved when

classroom teaching is supported by adequate laboratory courses and experiments, following the "learning by doing"

paradigm, which provides students with a deeper understanding of theoretical lessons (Tomasi et al.,2009; Bravo et

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al.,2010; Churlyaeva & Kukushkin,2011) In a previous study, students employed their collective knowledge to use PVD in

nanotechnology to develop new modular experiments and pedagogical methods to introduce undergraduates to the field of

nanoscale research. The goals were to cultivate a thin film in nanotechnology, in engineering undergraduate education at

the Institute of Engineering Science and Technology at National Kaohsiung First University of Science and Technology,

using a group of integrated learning modules focused on nanotechnology. The creation of a series of complimentary

courses for undergraduate nanoscience education was envisioned. This development leveraged two programs that employ a

sputtering system (nanofabrication) and hands-on nanotechnology experiments. Currently, the nanotechnology laboratory

courses in experimental modules cover the fabrication, processing, structure, composition and thermal treatment of the

physical and mechanical properties of nanomaterials. Besides the in-class and hands-on nanotechnology modules, students

were also asked to prepare a term paper, discussing a specific application of nanotechnology modules, the term papers

were submitted individually and covered topics such as optical, electrical, magnetic, chemical, mechanical and thermal

properties in engineering applications of nanotechnology.

3. Research and Design

3.1. Sputtering Systems

This section describes magnetron sputtering system requirements for zirconium nitride modules in the experimental

nanotechnology courses. The theoretical background for sputtering deposition techniques is demonstrated and their uses

explained, from the viewpoint of studies on the sputtering phenomena, planar diode glow discharge, balanced and

unbalanced magnetrons and thin film growth. They are being used to develop a wide range of advanced functional

properties, including physical, chemical, electrical, electronic, magnetic, mechanical, wear-resistant and corrosion-resistant

properties at the required substrate surface. The sputtering system is shown generically in Figure1. A magnetron sputtering

equipment that includes magnetron sputtering system with a vacuum subsystem, a cooling subsystem, a sputtering

chamber subsystem and a digital control subsystem allows monitoring of the quality or content of thin films, gathering and

storage of product information and detailed analysis and trouble-shooting of the system. Furthermore, In this context of

deploying a sputtering deposition-based system laboratory, this study focuses on the following three main issues: (1) from

a technological perspective, adaptation of concepts and techniques in PVD modules are explored for possible use in

laboratory settings and (2) from an educational perspective, teaching PVD manipulation principles requires familiarizing

students with mechanical and material engineering concepts and skills (3) from a integrated perspective, nanotechnology

modules in teaching and learning are analyzed for the properties of thin films and the design of a statistical questionnaire

in the laboratory courses. In a lecture on magnetron sputtering systems, the students are taught how to sputter depositions

in the vacuum coating process, using a vacuum of less than one ten millionth of an atmosphere. When the appropriate

pressure has been reached, a controlled flow of an inert gas such as argon is introduced.

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Figure 1. Magnetron sputtering equipment

3.2 Sputtering Deposition Description

The most important part of the system is the implementation of physical vapor deposition technology for experimental

nanotechnology courses that use a laboratory. In this study, magnetron sputtering processes include the creation of material

vapors by evaporation, sputtering, or laser ablation, and their subsequent condensation onto a substrate, to form the film.

This process involves the condensation of the vapor species onto the substrate and subsequent formation of the film by

nucleation and growth processes. However, the examples of experimental zirconium nitride (ZrN) modules for a

magnetron sputtering system are used in nanotechnology courses. In industrial applications, ZrN is becoming the most

promising protective and decorative coating material for metal substrates, mostly due to its warmer golden color and better

corrosion resistance than current commercial counterparts. The students engage in active learning by performing

experiments, which is as important as passive learning through attending a laboratory. For sputtering deposition of

zirconium nitride modules, three basic sputtering systems can be learned: (1) one magnetron with an alloyed target, (2) two

magnetrons equipped with targets made of different elements\alloys\compounds or their combinations, or (3) a pulsed dual

magnetron, which can easily control individual elements in the alloy film or make it possible to deposit non-conductive

Digital control subsystem Vacuum subsystem

Magnetron sputtering system Sputtering chamber

subsystem

Cooling

subsystem

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materials. Furthermore, useful and commercially attractive development in surface engineering using zirconium nitride

modules in their fabrication involves a number of stages (preprocessing, deposition and characterization), which are

interdependent. The flowchart for sputtering deposition procedures is shown in Figure 2. It is clear that development of the

fabrication equipment, process parameters, parameter limits and monitoring/control techniques ensures a good product

yield

Figure 2. the flowchart of sputtering deposition procedures

3.3 Experimental Nanotechnology Courses

Nanotechnology subjects are always greatly improved when classroom teaching is supported by adequate laboratory

courses and experiments, following the learning by doing paradigm, which provides students with a deeper understanding

of theoretical lessons. This study used a curriculum for a PVD system fabricated zirconium nitride, for use in a

nanotechnology module, focusing on a hands-on experimental task, which addresses the problems of traditional

subject-matter curricula. The integrated curriculum emphasizes knowledge in depth and in breadth. The physical vapor

deposition technology for use in nanotechnology in the engineering education curriculum provides integrated knowledge

of surface engineering treatments, helping students to apply their engineering knowledge through different exercises within

experimental nanotechnology courses in zirconium nitride modules. The zirconium nitride thin films are actually

experimental nanotechnology module systems that are suitable for teaching courses in engineering education. The

zirconium nitride thin films laboratory platform is an educational tool for teaching students the basic principles of the

performance of a series of experiments using physical vapor deposition technology. The zirconium nitride thin films in the

laboratory are where elegant scientific theories meet messy everyday reality. This zirconium nitride observation helps

explain why laboratory experiences are at the core of undergraduate education in science and engineering. Practical

nanotechnology examples prepared for this are available. This zirconium nitride module introduces undergraduate students

to the use of nanotechnology techniques for the characterization of materials in the thin films. Such an integrated system

enables students to investigate the principles and application of physical vapor deposition for use in nanotechnology,

which are commonly found in industry. As shown in Figure 3, the procedures for the course are designed with an

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integrated curriculum and the details are organized. The students are given an introduction to the construction, utility and

application of a sputtered deposition-based system in their surface engineering course and/or nanotechnology course.

Figure3 shows the experimental programming for the ZrN module in this nanotechnology course. This study covers all

aspects of sputtered deposition-based system process technology, from characterization and preparation of the substrate

material, through the deposition process and film characterization, to post deposition processing. The emphasis of the

study is on the aspects of the process flow that are critical to the reproducible deposition of films that have the desired

properties.

Figure3. The learning procedures of learning and teaching programs for zirconium nitride modules in nanotechnology courses

Nanotechnology courses

Experimental ZrN modules

Optic Electr Magn ChemMechan

Propert

Surface

Surface Composition

Equipment used

Roughness

Micro/nano structure Film structure

Atomic force

microscopy

Scanning electron

microscopy

X-ray

diffraction

Applicati

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3.4 Design of Statistical Questionnaire

The design of a statistical questionnaire study begins with a discussion of the literature on

nanotechnology related courses offered by colleges and universities and a competency analysis of

zirconium nitride modules in nanotechnology. They are further supported by approaches such as panel

discussions, expert meetings, field work in the PVD industry and student surveys, to explore the

nanotechnology module topic. The assessment tool for this research is a variation of the score chart.

The score chart is designed with a 5-level scoring method (points 1~5). The items being assessed

originates from the essential items of the implementation of basic design courses, including sputtered

deposition-based systems, sputtering design expression, nanotechnology expression, experimental

examination expression and integrity. However, the evaluators include instructors and a group of

engineering undergraduate students. By filling the questionnaire separately, experts have a sense of full

participation. On March 28th, 2012, this study held an expert meeting at which ten experts from the

teaching material courses of universities and institutes reviewed the draft content, structure, usage of

the sputtered deposition-based system and examined the nanotechnology module competences. The

experts’ opinions, obtained in three written documents, were repeatedly analyzed and arranged, until

their opinions reached an agreement. The formal questionnaire that includes 19 questions on the main

function of developing PVD for use with zirconium nitride modules in nanotechnology was finalized.

SPSS20.0 statistical software was used to analyze and process data. In this study, the researchers

designed a structural interview questionnaire, in accordance with literature discussions and qualitative

research experience. Twenty-two engineering undergraduate students finished the nanotechnology

courses in 2012. In-depth interviews were conducted with research objects, who were informed of the

purpose of the interview, and after consent, given an interview questionnaire and agreements designed

according to the respondents’ experience description and research ethics. The results for both teachers

and students scores for the questionnaires show that it is helpful to review the opinions of both groups,

for consistency testing, as a whole and individually.

4. Experimental

4.1 Zirconium Nitride modules

In this study, a zirconium nitride (ZrN) modules was fabricated was developed in a laboratory

experiment. This study used the ZrN films that used the magnetron sputtering system in a laboratory

project. The experimental ZrN modules in nanotechnology can be set up by designing the experimental

contents such as design, system and the interface for experiments and instructions. The students use

control factors to prepare their own control programs for their ZrN modules. In this experiment, a

sputter deposition system with a magnetron gun and pulsed DC power supply was used. The planar

sputtering gun, equipped with a rectangular target (300×100×10 mm), was operated in an unbalanced

mode. The three targets; a zirconium target of 99.5% purity, a chromium target of 99.5% purity and a

titanium target of 99.5% purity, were deposited. The substrates were ultrasonically cleaned in methanol

and acetone, for 10 min each, and fixed on a cylindrical sample holder in the vacuum chamber and then

dried by ion bombardment in an Ar plasma discharge, before deposition. It was coated, in sequence, by

a bonding (Ti,Cr) layer (15 min), and then a top ZrN layer. A system pressure of 4×10-5

torr was used

for each film deposition. Details of the UBM sputtering procedures are described in references. The

experimental schemes used an orthogonal array table. Eight control parameters were chosen for the

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experiments with the magnetic sputtering modules. The deposition conditions for the ZrN thin films

coated onto the stainless steel specimens are listed in Table 1. The substrate matrices used in the

experiment were 306 stainless steel pieces with dimensions of 4cm×4cm×0.7cm. Before film

deposition, the substrate surfaces were cleaned ultrasonically in acetone and ethanol, for 10 minutes,

and then dried. The cross-sectional structures of the composite films were noted, using a field emission

scanning electron microscope (JEOL JSM-6700F). Surface examination of the films involved the use

of a digital instrument nanoscope of the atomic force microscope (Nanoscope Dimension 3100 SPM).

In the experiment, two different spots were chosen for each film surface and a scan area of 5×5 mm2

was measured. From the scanned area, the surface topographies and surface roughness of the various

samples were determined and recorded. The roughness parameters of the root mean square (Rq),

arithmetic mean deviation (Ra) and maximum roughness depth (Rmax) values were obtained at

arbitrarily chosen positions on the film surface. The element depth profiles across both the zirconium

nitride with Ti coatings and zirconium nitride with Cr coatings were researched by glow discharge

optical emission spectroscopy. The elemental species were identified in the films by the assignment of

corresponding signals marked with the high-resolution X-ray photoelectron spectrometer. The

crystalline structures of thin films were identified by X-ray diffraction (XRD), using a CuKα source (λ

= 0.15405 nm) and a scan speed in 2θ of 1°/min.

Table 1. Control factor conditions of experimental ZrN film modules for magnetron sputtering system.

Symbo

l

Factors condition

s A Interlayered element Ti

B Ar (sccm) 25

C Ti+Zr current(A) 3

D N2(sccm) 11

E Sputtering distance (cm) 8

F Substrate Bias voltage (V) 40

G Sputtering time (hr) 2.5

H Rotate speed (rpm) 2

4.2 Structural Analysis of Modules in Nanotechnology Courses

A measurement of thin-film properties is indispensable for the study of thin-film materials and

devices. Several methods are proposed for the measurement of the thin films. Rapid progress was made

in evaluating the surface, structure and thin-film composition of nanotechnology materials. There are

many levels of film analysis, such as physical, chemical, optical and mechanical tests, as shown in

Figure2. The level of the application involves measuring behavioral properties, or how the film

interacts with its environment; light, electrical and magnetic fields, chemicals, mechanical force and

heat, in Figure3. The deeper level involves probing structure and composition, which together

determine film behavior and thus provide a bridge of understanding between the deposition step and

the film behavior. Several examined methods are proposed for the evaluation of the zirconium nitride

modules. Below is a description of the specific techniques for analysis of the film structure,

composition and properties. For example, the AFM images show in Figure 4 show that one is of the

surface morphology of the ZrN coatings on 316 stainless steel substrates, in which the change in the

thin film depends on the different settings of the control parameters.

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Figure 4. AFM images of surface morphology

To examine surface topography features, microscopy is needed. Standard optical microscopy can

reveal prominent features, such as cracks and bubbles and hillocks, but in nanotechnology topography,

a field emission scanning electron microscope (FESEM) is used. The surface morphology of the Ti

nanointerlayer of ZrTiN thin films is examined using FESEM images, as shown in Figure5a. The grain

sizes of the ZrN nanoparticles on the surface of the thin films with a Ti nanointerlayer are much smaller

and the surface is smoother.

(a) (b)

Figure5. Surface and fractured SEM images of nanotechnology modules using ZrN films

Fractured cross-sectional FESEM micrographs of the specimens of the TiZrN thin films are shown

in Figure 5b, in which the vitreous fractured structures of the (Ti, Cr) ZrN films are clearly visible.

There is even an amorphous growth structure on the CrZrN films, where the Cr interface between the

(Ti,Cr) ZrN films and its substrate is well bonded, without any visible flaw. There is no evidence of a

columnar structure. These thin films showed a visible tendency towards forming fractured amorphous

glassy phases. In the experiment, the (Ti, Cr) interface was designed to minimize the variation in

chemical composition and lattice structure between each adjacent layer. It is obvious that after nitrogen

ions attack, some of the chromium atoms are bombarded deep into the substrate and the mixing of film

and substrate is clearly revealed by glow discharge optical spectroscopy (GDOES).

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5

0.0

0.2

0.4

0.6

0.8

1.0

0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5

0.0

0.2

0.4

0.6

0.8

1.0

Fe

Ti

Zr

N

Conc

entra

tion

in %

Depth in um

Fe

N

Zr

Ti

(a)

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Figure 6. Composition analysis (a) GDOE (B) X-RAY of thin films for use ZrN modules in nanotechnology

The film composition and thickness is determined by GDOES. A typical elemental depth profile is

depicted in Figure 6a. The concentration distribution of the Zr, Ti, N, Cr and Fe elements of the films

with depth is determined from the depth profile. The occurrence of elements contained in the films can

be clearly seen, and is in good agreement with the composition studied. As shown in Figure 6, the total

thickness of the TiZrN film is approximately 3.0 m and the titanium intermediate layer with a thickness

value of 0,5 m is visible in the depth profile. The film composition stoichiometry reveals an N

concentration of approximately 40%. It is seen that the relative proportion of the titanium elements

progressively varies, from the surface to the interface to the substrate. It probably provides an efficient

process for diffusion during the magnetron sputtering, which results in a strong mixing of the TiZrN

with the Fe that is present on the stainless steel. Figure 6b shows a series of XRD spectrums with ZrN

modules. These principally exhibit three strong sharp peaks in the thin films, located at 2θ of 33.898,

(b)

(a)

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39.368 and 59.321, which are attributed to diffraction of the ZrN(111), Zr(200) and ZrN(220) planes.

The ZrN(311) peaks and TiN(200) peaks seem to be small. This implies that the film may be composed

of Ti-doped ZrN with preferential orientation in a (111), (200) and (220) direction.

4.3 Questionnaire Evaluations

This section addresses the impact of sputtering deposition-based system with experimental

zirconium nitride modules. The laboratory course included lectures and laboratory experiments. This

course was managed by one teacher and one graduate assistant. Twenty-two students (2 female and 26

male; age between 19 and 21) had participated by the end of the semester in the materials science

courses. They were drawn from the population of undergraduate students. A learning evaluation

system was used to test the efficacy of the system, in terms of teaching, learning and student

achievement. The questionnaire comprised sixteen questions that were designed to evaluate the

usability and effectiveness of the system, on a 5-point Likert scale, from 1 to 5 points, where 1 is

strongly disagree and 5 is strongly agree. The scores for items measuring the effectiveness of the

laboratory platform measured whether the system accomplished its objectives. The evaluations have a

marked impact on student motivation and encourage teachers to explore ways to improve individual

learning attitudes. The laboratory platform was designed for an educational application. It was

determined whether the sputtering deposition-based system with experimental zirconium nitride

modules for nanotechnology evaluation, as shown in Table 2, was very useful, or not at all useful, and

whether the modules met their needs. The platform was first tested and evaluated. The experimental

zirconium nitride modules module was tested for accuracy and completeness and the generated

samples were examined and tested. Further, the teaching and learning platform was evaluated by

measuring teacher and student satisfaction. The scores on the items measuring the usability of the

laboratory platform reflected its usefulness. Student satisfaction was measured from the scores given

to these questions and was used as an indicator of the success of the laboratory platform. Table 2

summarizes the expert and student responses to the questionnaire. Both groups rated the laboratory

platform highly, based on the results of the evaluation. A further analysis was conducted, to

investigate whether experts and potential students differed in their mean ratings of the effectiveness

and usability of the system.

No. Items

Students

(n=28)

Experts

(n=10) t-Test

M SD M SD

1 The sputtering deposition-based system guide was

organized

4.25 0.464 4.40 0.413 0.875

2 The sputtering deposition-based system operating guide

was easy to understand

4.20 0.677 4.10 0,512 -0.415

3 The sputtering deposition-based system goals were clear 3.35 0.371 4.60 0.316 9.222*

4 The sputtered deposition-based system in engineering

undergraduate courses was suitable for students

4.30 0.732 4.70 0.522 1.552

5 The sputtered deposition-based system was helped in the

teaching and learning nanotechnology courses

4.70 0.41 4.60 0.312 -0.684

6 The sputtered deposition-based system was more

interesting than traditional textbook learning

4.65 0.258 4.50 0.152 -1.700

7 The sputtered deposition-based system was well designed 4.10 0.712 3.80 0.356 -1.255

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and processed

8 The background information of sputtered

deposition-based system was helpful to students

4.35 0.611 4.30 0.546 -0.221

9 The operating steps for sputtered nitride zirconium

modules were explained and understandable

4.25 0.892 4.40 0.472 0.498

10 The properties of zirconium nitride modules were

examined and tested in overall

3.70 0.865 4.20 0.324 1.759

11 Typical applications of zirconium nitride modules were

understood and clear

3.55 0.365 3.70 0.415 1.033

12

The analysis of zirconium nitride modules in AFM,

SEM ,X-RAY and GDOE examination was understood

and motivated at whole

3.45 0.882 3.80 0.472 1.174

13

The examination of surface texture, structure feature and

composition in zirconium nitride modules was understood

and clear

4.35 0.322 4.7 0.224 3.100 *

14 The experimental zirconium nitride modules were

interested for use in nanotechnology courses

4.25 0.232 4.4 0.122 1.916

15 The assessments overall provide useful feedback on your

nanotechnology courses

3.95 0.436 4.1 0.215 1.026

16 The learning in nanotechnology courses was useful and

motivating overall

4.10 0.325 3.9 0.324 -1.615

4.4 Evaluation Results

Domain expert evaluations were used to help determine the accuracy of the embedded

nanotechnology knowledge and the effectiveness of the experimental teaching system. The laboratory

platform was validated by ten experts. All were University Professors and/or Researchers, with an

average more than 3 years of experience in teaching surface engineering, so each expert had a strong

background in engineering education. Overall, the expert evaluations were positive. Evaluations by the

students were used to help determine the acceptability of the project, according to the following criteria:

usability of the laboratory platform, the extent to which the students gained hands-on experience in

nanotechnology modules and whether the project helped students learn about zirconium nitride

modules in nanotechnology. The evaluation form was distributed to all students who had taken this

course in the Institute of Engineering Science and Technology at National Kaohsiung First University

of Science and Technology. Most students successfully performed the experiment and responded

positively to the system. They reported that they enjoyed performing the task and found it interesting.

Since the sample size is small, the mean distribution of the difference between students and experts was

used and the results are displayed in Table2. The value, α, called the level of significance of the test, is

usually set in advance, with a commonly chosen value being α = 0.05, for which the corresponding

two-tail critical value is ±1.96. Based on the scores from the test, it was found that there are significant

differences for item3 (t=9.222, P<0.05) and item13 (t=3.100, P<0.05) in the distribution of the

difference between students and experts, but the others are not significantly different. In addition, the

opinion of students on evaluation questionnaire results, at the 2,5,6,7,8 and 16 percent levels, in

learning courses are much less than the experts’ desired results. Further analysis showed that they came

from different engineering backgrounds, which difference in background has a significant effect on

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students’ learning performance in nanotechnology modules class, as verified throughout the world. As

the survey results show, the students’ responses were very positive and encouraging of further

improvement of the nanotechnology courses.

5. Conclusions

This study addressed the development of a physical vapor deposition system, for use in zirconium

nitride modules in nanotechnology courses. This system emphasizes both theory and practice and the

sequence covers general magnetron sputtering devices and technology, as well as new and novel

state-of-the-art design for nanotechnology modules, in which the zirconium nitride thin films use

magnetron sputtering deposition in a laboratory project. Students learn to test and integrate actual

zirconium nitride modules for use in a magnetron sputtering system in nanotechnology, on a design

project. This nanotechnology course will hopefully bridge the gap between university education and

industrial applications. The innovative experimentation and teaching methods have already been

inaugurated in the Institute of Engineering Science and Technology at National Kaohsiung First

University of Science and Technology. The proposed experimental zirconium nitride modules can be

introduced to engineering curricula by incorporating nanotechnology modules in labs, mentoring

undergraduate students in nanotechnology research and introducing a thin film course. The goal of the

system sequence is to use this research and facilities for magnetron sputtering in nanotechnology

modules in engineering education, to give students a comprehensive background in the art and science

of nano/micro technology, design and integration.

Acknowledgments

This work is based upon work supported by National Science Council, Taiwan under grants NSC

101-2511-S-132 -002.

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