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COMUNICAÇÃO TÉCNICA ______________________________________________________________________________________________________________________________________________________________________________________________________
Nº 176452
Microfluidics Mario Ricardo Gongora-Rubio
Slides apresentado da Palestra da 5.Semana de Inovação, Belo Horizonte, 2019. – FPT Industrial
A série “Comunicação Técnica” compreende trabalhos elaborados por técnicos do IPT, apresentados em eventos, publicados em revistas especializadas ou quando seu conteúdo apresentar relevância pública. ___________________________________________________________________________________________________
Instituto de Pesquisas Tecnológicas do Estado de São Paulo
S/A - IPT Av. Prof. Almeida Prado, 532 | Cidade Universitária ou
Caixa Postal 0141 | CEP 01064-970 São Paulo | SP | Brasil | CEP 05508-901
Tel 11 3767 4374/4000 | Fax 11 3767-4099
www.ipt.br
Eng. Dr. Mário Ricardo Gongora Rubio
Senior Researcher
Micromanufacturing Laboratory
Institute for Technological Research (IPT)
Belo Horizonte - 2019
FTP Innovation Day - CNH Industrial
OUTLINE
IPT Presentation
Bionanomanufacturing Center
Technological Platforms & LMI Infrastructure
What is Microfluidics
Microfluids Phenomena
Microfluidic Unit Operations
Applications in Microreactors
Application in Energy and Automotive Industry
Conclusions
WHO WE ARE
One of the first applied R&D&I institutions in Brazil
Company controlled by São Paulo State Treasury Office - State of São Paulo Government.
TECHNICAL ACTIVITIES
Innovation, research and development
Technological Services Development and metrological support Information and technology education
TECHNICAL CENTERS
CT-Obras Center for Infrastructure Work Technology
CTMM Center for Technology in Metallurgy and Materials
CTGeo Center for Geoenvironmental Technologies
CT-Floresta Center for Forest Resource Technology
CTMetro Center for Mechanical, Electrical and Fluid Flow Metrology
CQuiM Center for Chemistry and Manufactured Goods
CIAM Center for Information Technology, Automation and Mobility
CETAC Center for the Built Environment
CTMNE Center for Mechanical, Naval and Electrical Technologies
NT- BIONANO Nucleus for Bionanomanufacturing
NT – MPE Nucleus for Technological Support to Medium and to Small Enterprises
LEL Light Weight Laboratory
INFRASTRUCTURE
• IPT units in: – São Paulo
– Franca (individual protection equipment))
– São José dos Campos* (composite materials)
14 technology centers
40 laboratories
103.523 m2 of labs area
240.000 m2 of total area
MARKETS
Transportation Infrastructure
Roads
Naval
Pipeline
Metro-railway
Airspace
Cargo
IT & ITS
Metallurgy
Chemistry
Bioproducts
Plastics & Rubber
Composites
Textiles & Leather
Wood
Energy Materials and
Chemistry
Civil Works
Buildings
Environmental
Impacts
Mining
Oil and gas
Ethanol
SOME CUSTOMERS
BIONANOMANUFACTURING CENTER
BIONANOMANUFACTURING CENTER LPP - Lab. Chemical Processes and Particle Technology Nanotechnology and advanced chemical processes LBI - Laboratory of Industrial Biotechnology Development and characterization of biotechnological solutions LMI - Micromanufacturing Lab. Miniaturization of products and processes
TECHNOLOGICAL PLATFORMS &
LMI INFRASTRUCTURE
TECHNOLOGICAL PLATFORMS
Nanotechnology: new possibilities of process intensification (physical, chemical & biological) through scale reduction with gains in product quality
Biotechnology: less aggressive processes to the environment with lower energy consumption and using renewable raw materials
Microtechnology: manufacturing capability for production of miniaturized devices and systems such as microsensors, microreactors and MEMS
LMI/IPT - INFRASTRUCTURE
Microfabrication in Clean Room Technology Equipment Lithography - Mask Aligner EVG620 - Spinner, hot plate, developer Brewer CEE - Maskless Laser Photolithography - Heilderberg µPG 501 Thin Film Deposition - PVD System KJLCLab18 - PECVD Oxford Plasmalab 80 Parylene coater SCS Labcoater 2 Wet Processes - Wafer cleaning bench - Wet Corrosion Bench - HF Vapor phase etcher Dry Corrosion - DRIE-ICP Oxford Plasmalab 100 - Plasma cleaner Diener Nano Wafer Processing - Wafer Bonder AML-AWB -CMP Logitech CM 61 Orbis - Wafer Dicing ADT 7100 Microscopy & Metrology - MEV Zeiss EVO MA 10 - EDS Brucker Quantax 200 - Profilemeter Brucker DEKTAK XT
LMI - MICROMANUFACTURING LAB (CLEAN ROOM)
LMI - MICROMANUFACTURING LAB (CLEAN ROOM)
Interdigital Sensor Application
4 µm gap
Micromachining (Laser)
Thick Film Deposition (Screen Printer)
Lamination
Sintering
Dicing
LTCC Micromixing Device and its internal geometry
LTCC PROCESS AT LMI
LTCC ADVANTAGES FOR MICROSYSTEMS
• Simplicity of tape machining in the green state with feature size of 50 m to several mm;
• Ability of 3D multilayering and high layer count;
• Integration of a wide range of materials with different properties & technologies;
• Adaptability of embedded passive structures;
• 3D Microfluidics are readily implemented;
• Tapes of different compositions can be formulated to obtain desired layer properties;
• Integrated Electronic circuits because of its hybrid nature;
• Possibility of auto-packed devices fabrication;
• Mass production methods can be readily applied;
• Fabrication techniques are relatively simple, inexpensive and environmentally benign.
LMI/IPT – LTCC INFRASTRUCTURE
Equipment for fabrication of LTCC devices:
– Laser Machining
– Screen Printing
– Uniaxial Laminator
– Sintering Oven
– Paste dispenser
– Rework equipment
Micro-
System
Module
TECHNOLOGY VISION
Actuator Micro
Fluidics
I/O
• Microsystems containing Sensors + actuators + Microfluidics & Electronics are feasible to integrate using the LTCC technology.
• The photograph shows a remote controlled microsystem for thermal actuation.
LTCC INTEGRATED MICROSYSTEMS
INITIAL LTCC RESEARCH
S&A Paper published in 2001 with more than 500 citations.
WHAT IS MICROFLUIDICS
MICROFLUIDICS
Behavior of fluids in Microscale: • Control of small fluid volumes,
• Low thermal mass & Fast response time,
• Reaction condition well controlled,
• Efficient mass transport,
• Low energy consumption,
• Continuous processes & Small systems size,
• Laminar flow allows controlled mixing
• Large surface to volume ratio
Microfluidics is a technology which refers to the research
and development of micro-scale devices which handle
small volumes of fluids (as small as micro-, nano-, pico
and even femtolitre volumes)
Some Advantages • Low fluid volumes consumption (less waste, lower reagents costs
and less required sample volumes),
• Faster analysis and response times due to short diffusion distances, fast heating, high surface to volume ratios, small heat capacities,
• Better process control because of a faster response of the system (e.g. thermal control for exothermic chemical reactions),
• Compactness of the systems due to integration of much functionality and small volumes,
• Massive parallelization due to compactness, which allows high throughput production,
• Cost-effective fabrication, allowing disposable devices, fabricated in mass production,
• Safer chemical, energy or biological studies because of integration of functionality, smaller fluid volumes and stored energies.
Traditional
Laboratory
Microfluidic
“Lab-on-
a-chip”
Cost Often very high Low Cost
Equipment Specialized
equipment
Integration on
chip
Time to get
results
Significant time Quick
Benefits of Microfluidics
MICROFLUIDICS SPECTRUM
TODAY MAIN APPLICATIONS
MICROFLUIDICS FABRICATION METHODS
• Soft Lithography
• Silicon Micromachining
• Glass Micromachining
• Plastic Micro-Injection Molding
• 3D Printing
• Green Tape Ceramics (LTCC) Structuring
BATCH Vs. FLOW
MICROREACTOR SCALE-UP
MICROFLUIDS PHENOMENA
LAMINAR AND TURBULENT FLOW
Unstable streamlines
mix fluids in random
and chaotic manner
Well defined streamlines
-adjacent horizontal layers
flow at different speeds
- zero flow at the solid-fluid
interface (no slip condition)
PRESSURE-DRIVEN FLOW
MICROFLUIDS PHENOMENA
Capillarity Surface tension
ElectroWetting Inertial Forces
The force on the fluid
due to a curved
streamline points outwards centrifugally.
DROP GENERATION
• Several structures are used as drop generators with monodisperse dispersion
HYDRODYNAMIC FOCUSING
• Hydrodynamic focusing can be used as drop generator allowing drop frequency and size.
3D FLOW FOCUSING
• 3D Flow focusing can be used to
implement the in-Flow
nanoprecipitation process
MICROFLUIDICS OPERATIONS
MICROFLUIDIC OPERATIONS
MICROMIXING
MIXING PRINCIPLES
Baker transformation as an example of Chaotic
Advection Mixing
3D MICRO MIXERS IN LTCC 3D Serpentine Micromixers can be used for chemical Microreactors in order to fabricate emulsions, particle encapsulation and nanomaterial fabrication
10 mm
MICROFLUÍDIC DEVICES
Aumento 10X Aumento 4X
TURRAX
EMULSIONS USING MICROFLUIDICS
Simple Emulsion Double Emulsion
EMULSION GENERATION
EMULSION PRODUCTION WITH MICROMIXERS • Micromixers can be used to produce emulsions to scale-up the
process in higher flow rates.
Crossing Channels geometry for Micromixer emulsion generator
Straight forward scale-out from bench to industrial
production due to the possibility of mass parallel module
integration to obtain production volume.
EMULSION PRODUCTION USING MICROMIXERS
Scale-Up Scale-out
MICROSEPARATION
SEPARATION TECHNIQUES
SEPARATION VIA LATERAL DISPLACEMENT MAGNETIC SEPARATIONS
GRAVITY SEPARATIONS SEPARATIONS IN PINCHED MICROCHANNELS
APPLICATIONS IN MICROREACTORS
FLOW CHEMISTRY
In flow chemistry, reagents are continuously pumped through the reactor and the product is continuously collected.
A
B
C
Syrris
BATCH AND FLOW
Classic way to do chemistry. • Reagents are loaded into the reactor,
mixed and left to react. • The products is collected at the end, after
the reaction has been completed and worked-up.
New technique. • Reagents streams are continuously
pumped into the flow reactor. • Reagents mix and react in the flow
reactor. • The product leaves the reactor as a
continuous stream. Key factors:
- Concentration - Mixing - Temperature - Reaction time
Key factors: - Residence time (flow rates) - Mixing - Pressure - Temperature
Reaction
Mixture
>5mm
Reagent A Reagent
B
Reagent A
Reaction
Mixture
~100µm
Reagent B
Syrris
FLOW CHEMISTRY PARAMETERS Residence time It can be defined as the time that every fraction of the reaction volume spends in the reactor.
Residence time is equivalent to reaction time in batch chemistry. It is calculated as follows:
Residence Time = Reactor Volume / Flow Rate
There are two ways of controlling the residence time:
• Vary the reactor volume
• Vary the flow rates.
Mixing • In flow chemistry mixing can be turbulent or laminar
Pressure • In a flow reactor the total pressure at any location is made up of two factors:
• Back pressure due to flow & Back pressure intentionally applied
Temperature • Due to a higher surface area to volume ratio, flow reactors enable better heat
transfer and therefore better temperature control.
Syrris
LTCC MICROHEAT EXCHANGE
The major advantage of microchannel heat sinks is the high heat transfer coefficients, up to 60 times higher than the heat transfer coefficient of conventional, macro scale heat exchangers.
• High heat transfer coefficients • Low thermal resistance • High aspect ratios • Occupy less space • Best suited for hot-spots • Increasing the aspect ratio will enhance
the convective heat transfer at fixed flow velocity
ADVANTAGES
Layers
Microchannels
Micro heat exchanger
DEVICE CONCEPT AND IMPLEMENTATION
Vásquez-Alvarez E. ; DegasperI, F. T. ; Morita, L. G. ; Gongora-Rubio M. R. ; Giudici, R. Development Of A Micro Heat Exchanger With Stacked Plates Using LTCC Technology. Brazilian Journal of Chemical Engineering, v. 27, p. 483497, 2010.
HEAT EXCHANGER FLOW ANALYSIS
Several entrance geometries studied
Velocity Results
DROP MICROREACTORS
• New methods for obtaining spatially separated drops for later electro-coalescence allow to perform functions such as Micro-precipitation.
• Extraction of iron oxide nanoparticles in extremely fast reactions.
Active Pharmaceutical
Ingredient (API)
Solubilization Nanoparticle
Formation
Increased bio-availability of poorly soluble drugs
MICROREACTORS FOR NANOPARTICLE PRODUCTION
Crystals Microfluidic device
Characterization
Amorphous Nanoparticles
ϕ ≈ 200 nm
APPLICATIONS IN ENERGY AND AUTOMOTIVE INDUSTRIES
BIODIESEL PRODUCTION IN MICROREACTORS
• Biodiesel is a biodegradable derivative fuel obtained from natural renewable resources. Several processes such cracking, esterification or transesterification can be used and it is produced from animal fats or vegetal oils.
• Several Brazilian vegetal species can be used, such as “mamona”, “dendê” (palm), sunflower, “babaçu”, peanut, tame nut and soy, as raw materials for the process.
Soy Oil
MICROFLUIDICS APPLIED TO BIODIESEL FABRICATION
Methanol
Transesterification Process Biodiesel +
Glycerin
Otimization of Micromixers
LTCC DEVICE FOR BIODIESEL
Microdevices in LTCC technology for the production of Biodiesel using the transesterification process with homogeneous or heterogenous catalyst.
Raw Materials
(oil &alcohol) +
catalyzer
Injection
System
Microreator &
Residence Time
control
Purification System
Measurement and
Control System
Separation System
Glycerin
Biodiesel
Excess
Microfluidic Device for Microreactor
Residence time and heater Microfluidic Module
WATER IN DIESEL EMULSIONS
• The presence of water nanodroplets in diesel causes micro explosions in combustion process; increase the presence of oxygen and in consequence will enhance the fuel performance.
• It was also demonstrated that small amounts of water nanodroplets, something like 5 up to 14%, can reduce the NO, NOx and CO2 emission in a range of 18%
• Water is immiscible in diesel oil and is not possible to obtain an emulsion without the use of a surfactant.
• It is important to use adequate surfactants concentrations to maintain the diesel with the same physical characteristics in terms of energy efficiency.
LTCC DEVICE FOR WATER IN DIESEL EMULSION
Vortex microfluidic device
0
100
200
300
400
500
600
8 10 12 16 20
Pa
rtic
le S
izes
(n
m)
Diesel Flow Rate (mL/min)
10%
5%
Water-in-diesel emulsion: water droplets size in function of diesel flow rate for two surfactant concentration (5 and 10 % v/v).
Particle sizes measurements: results obtained for a solution with 10 % of surfactant
Vortex microfluidic device fabricated in LTCC
OTHER MICROFLUIDICS APPLICATIONS
Reformer MICROFLUIDIC FUEL CELLS
A fuel processor and integrated fuel cell including a
monolithic three-dimensional multilayer ceramic
carrier Structure defining a fuel reformer and including
an integrated fuel cell stack. The reformer includes a
vaporization Zone, a reaction zone including a catalyst,
and an integrated heater. US 6,569,553 B1
A microfluidic vanadium fuel cell system employs graphite rods
commonly used as electrodes. The rods are mounted in a
hexagonal array comprising 12 anodes and 12 cathodes that
share the same fuel and oxidant channel. In this configuration,
the electrodes are connected both fluidically and electrically in
parallel. Connecting the cells electrically in series to achieve
higher voltages. DOI: 10.2478/s13531-011-0012-y
CONCLUSIONS
• At this time, several applications of Microfluidics in various areas of industrial technology were presented.
• We showed as well some applications in Microreactors, Energy and Automotive Industry.
• Microfluidics have been shown to be suitable for the integration of unitary micro-operations (such as mixing, dispensing, separating, diluting, microreacting and analyzing) generating complex functions in continuous flow, creating excellent opportunities for new developments.
LMI/IPT - Team Beatriz Nogueira Messias de Miranda, PhD Chemistry, IQSC, USP 2018
Luciana Ramos, Ph.D. in Mechanical Engineering, U of Michigan, 2005
Mário R. Gongora-Rubio, Ph.D. in Electrical Engineering, USP, 1999
Bruno Verona, B.Sc. in Electrical Engineering, USP, 2013
Martha Lucia Mora Bejarano, Dr. Chemical Engineering, USP, 2003
Karina Ferreira de Noronha Cruz, Dr. Materials Eng. UNIFESP, 2016
Aline Furtado Oliveira, Dr. Chemical Engineering, UNICAMP, 2018
Jaqueline Falchi Rocha, New Talent Program, MSc student at Mackenzie University
Roberta Cardoso, Visiting Researcher, Ph.D. IQ-USP
Ariel Pereira Lima, LTCC technology Trainee
Gabriel Antonieto Gianvecchio, Mechanical Engineering Trainee
Henrique Reis Wisinewski, MicrofabricationTrainee
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