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Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
L'IMS et ses travaux sur les capteurs - C.Dejous 1
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From the Integration of Innovative Materials to Future Smart Sensing Systems
About Sensors at IMS‐Bordeaux Labs
corinne.dejous@ims‐bordeaux.fr
© IMS Property
Thematic Organization at IMS Lab.
ORGANICS
MICROSYSTEMS
BIOELECTRONICS
AUTOMATIC CONTROL
SIGNAL & IMAGES
PRODUCTION ENGINEERINGY. Ducq
Y. Berthoumieu
A. Oustaloup
S. Renaud
L. Hirsch
NANOELECTRONICS
DEVICES RELIABILITY
CIRCUITS DESIGNJ-B Bégueret
E. Woirgard
T. Zimmer
COGNITICSJ-M André
11 groups
C. Dejous
MATERIALSV. Vigneras
Y. Berthoumieu
ELORGA
MDA
BIO-EM
ARIA
MEID. Chen
A. Zolghadri
I. Lagroye
L. Hirsch
EDMINA
MHYPOP
ELIBIO
CRONE
ICOM. Zolghadri
A. Oustaloup
N. Lewis
L. Bechou
CEMT
MODEST
PSPR. Dupas
D. Rebière
DESTINE. Grivel
VOLTIGEC. Germain
LASER
EC2T. Taris
D. Lewis
PACE
MODEL
CSH
H. Frémont
E. Kerhervé
C. Maneux
POWER
III-V
CSN
J-M. Vinassa
D. Dallet
N. Malbert
AS2NS. Saïghi
CIHJ-M André
ERGOF. Daniellou
FFTGF. Cazaurang
28 teams
D. Rebière
V. Vigneras F. Demontoux
From materialsto devices
Hardware Integration
Systems Integration
Systems and Interactions
Y. Deval
B. Veyret
V. Vigneras
X. Moreau
4 poles
PRIMSI. Dufour
420 members : 150 researchers, 160 PhDs, 15 Post-docs, 70 technical staff, 25 administrative staff
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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Outline
Introduction on (bio)chemical microsensors
MDA : A versatile transducing platform PRIMS Technological facilities Conclusion and prospects
© IMS Property
Smart (bio)chemical Sensor
Structure ofintelligent integrated sensor
Elementto analyze
1
2
transducer
3
signalconditioning
5
responsestreatment
8 calibration
6
results
7 powers
4
responsespre treatment
alarm on alarm
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
L'IMS et ses travaux sur les capteurs - C.Dejous 3
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Food industry
Chemical industry
Environment
Biological andmedical field
Military & Security
Fine chemistrycosmetic
Chemical and biological fields
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Acoustic Sensor Research activity
Interactionmechanisms
Transducingcomponent
Sensingplatform
Detection systemsMicrosystem design & fabrication
for a specific application
Necessary to identifyapplication areas
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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Versatile sensing platform
Coupling mechanisms- Mass- Viscosity- Conductivity- Permittivity- Stiffness- ...
Electronics
S1
S2 S3
Sensitivity : S1 x S2 x S3
© IMS Property
Outline
Introduction on (bio)chemical microsensors
MDA : A versatile transducer PRIMS Technological facilities Conclusion and prospects
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
L'IMS et ses travaux sur les capteurs - C.Dejous 5
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SAW Delay Line
Piezoelectric effect.
Acoustic wave propagation using IDTs (Inter Digital Transducers)
Wave pertubation induces :
– Phase velocity variation
– Attenuation (Insertion Loss)
InterDigital Transducers (IDTs)
Piezoelectric Sunstrate
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STW (BleusteinGulyaev)• SH wave
• Weak trapping energy
STW (BleusteinGulyaev)• SH wave
• Weak trapping energy
SAW (Rayleigh)• Elliptic polarization
(longitudinal & SH • Good mass-loading
sensitivity
SAW (Rayleigh)• Elliptic polarization
(longitudinal & SH • Good mass-loading
sensitivity
FPW (Lamb)•Longitudinal
+ Shear Vertical•h < λ : technological
difficulties
FPW (Lamb)•Longitudinal
+ Shear Vertical•h < λ : technological
difficulties
SH-APM• SH guiding wave
• weak mass-loadingsensitivity
SH-APM• SH guiding wave
• weak mass-loadingsensitivity
Love• Guiding SH SAW
• Guiding layer • High mass-loading
sensitivity
Love• Guiding SH SAW
• Guiding layer • High mass-loading
sensitivity
BAW (QCM)• Shear Honrizontal
(SH) polarization• Low mass-loading
sensitivity(working frequency)
BAW (QCM)• Shear Honrizontal
(SH) polarization• Low mass-loading
sensitivity(working frequency)
A.E.H. Love (1863‐1940, UK)
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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1. Piezoelectric substrate: AT cut ( 0°,121.5°,90°) Shear Horizontal polarization Working in liquid medium
2. Interdigital transducers (IDTs) (λ=40 µm, Lcc=8.4 mm, e=200nm)3. SiO2 guiding layer (4µm, PECVD)
Trapping Energy near free surface : attractive way for sensing applications
Towards Love‐waves devices
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COMSOL Simulation
SH pure Wave
S21 (IL & Phase) vs frequency
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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SiO2 thickness, h (µm)
°(Euler angles
(0°,°,90°))
|Sm
v| (
m²/
kg)
Mass loading sensitivity
AT-cutST-cut
substrate: quartz
wavelength: = 40 µm
guiding layer: SiO2
sensitive coating: PMMA, b = 50 nm, b = 5%
Optimal sensitivity for close to AT-cut and h between
4 and 8 µm
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SAW delay‐line devices
Quartz substrate: AT‐cut
Wavelength = 40 µm
Synchronous frequency
f ≈ 117 MHz
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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Electrical characterizationsusing Network Analyser
f0 = 117 MHz
Insertion Loss: 25 dB
Delay: 1.542µs
Vphase velocity ≈ 4300m.s‐1
Tme Domain, [1] acoustic signal.
S21 (magnitude & phase) LOVE Wave delay line
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Oscillator configuration
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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Acoustic sensors: various applications
Gas sensors
CO, CO2, NO, NO2, …
Volatile organic compounds, organophosphorus & organosulfur, …
Electronic noses Gas mixture, odors, …
Liquid sensors
Viscosity meter, conductivity meter, organic compounds, …
Biosensors
Bacteria, viruses, toxins, heavy metals, hydrocarbons, …
Thin film & complex fluid characterization
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Vapor Detection GB detection
timef0 = 109 MHz
sensitive coating Polysiloxane PLG,
f0 = 138 kHz
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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© IMS PropertyHigh temperature SAW Platform using LGS
Harsh environmental applications
Complete assembly :• Stainless steel shell
• Inlet/Outlet integrated cover for safe gas detection• PCB‐SMA RF connector
PhD G.Tortissier 2009
SAW delay‐line on LGS
Mesoporous sensitive film
Mesoporous : 2 ‐ 50 nm
Sol‐gel technique, spin or dip‐coating
Stability: thermal, mechanical, chemical …
High specific surface : 10 ‐ 1000 m2/g
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Starting value
IV : Filled pores
Disappearance of the curvatureof liquid meniscus
Decrease of P
III : Sharp pore filling
Capillary condensation
II : Film of water
Adsorption of water in grains boundaries
Stress relaxation
I : Micropores (< 2 nm)
Film characterization: mesoporous TiO2Young modulus vs. relative humidity
L. Blanc – PhD, 2011
RH (%)
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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Acoustic Waves & MicrofluidicInterest of both…
Microfluidic
Weak volumes
Parallelization
• Acoustic platforms
High sensitivity
Microelectronic fabrication process
+Weibel, D. B. et al. - Anal. Chem.
77, 4726–4733 (2005).
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PDMS Microfluidic chip
Microfluidic chip
Isolates transducers
Decreases liquid volume (< µL)
Limits acoustic losses
Minimizes acoustic reflections
Low cost and green technology
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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ANALYSISCHAMBER
AIRCAVITIES
VIAS
INLET
OUTLET
ANALYSISCHAMBER
µFLUNETWORK
INLET
OUTLETANALYSISCHAMBER
Hydrostatic configuration
Hydrodynamic configuration
PHS1
PHD1 PHD2
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Biological Micro organisms detection
PDMS chip+PT100Teflon insulationCeramic heatingSAW platform
Prototype
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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© Dissemination of IT for the Promotion of Materials Science –University of Cambridge
Complex fluid characterization
PEG in DIPolymer chain length influence
… Molecular entanglements
PDMS viscoelastic properties : G*G’+jG” from ∆f/f and ∆IL measurements
PhD V.Raimbault Univ. Bordeaux 1 - 2008
Solid lines : modified Huggins model
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Biological Micro organisms detection
Toxins (shellfish Quality)
Bacteria Escherichia Coli
Heavy metals
Cancer biomarkers : nucleosides
Thèse H.Tarbague 2011
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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© IMS PropertySurface Acoustic Wave Biosensors
for Real Time Immunodetection
Sensitive membrane (antibodies)Link layer
Target compound(bacteriophage)
Acoustic wave device
Saturating agent
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Immunodetection : E. Coli
BiofunctionalizationBioreceptive antibodiesSaturating agent
Thèse H.Tarbague 2011
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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Application : Heavy metals
Whole cell‐based biosensor
Trapping of E. coli bacteria
• Perturbation of viscoelastic properties due to modifications
of bacterial metabolism
• Detection threshold lower than 10‐12 M (Cd, Hg)
Cd2+ detection
((PAH-PSS)3-PAH) + E.ColiI.Gammoudi, L.Blanc – Collaboration 2011
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Cancer Biomakers detection (nucleosides)
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N. Omar-Aouled et N. Lebal – Thèses en cours
Molecular imprinting
Molecularly Imprinted Polymer (MIP)– Thin film– Compatible with acoustic propagation
Thin film characterization– Profilometry, SEM– Sensor response to vapor sorption
(toluene, ethanol) Adaptation to target biomarkers
SEM pictures : MIP layer morphologyThickness layer : 500 nm to 1µm
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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Prospects Various resonant transducers
– Acoustic, HF, optic …– Integrability (Mems), multiple detection mechanisms
Innovative materials– Nano- micro- structured, hybrid, organic,
biomaterials, carbon-based materials
Cheap integrated systems– « Green technologies »…
printing, sol-gel, flexible substrates…– Digital microfluidics– Electronic conditioner
© IMS Property
Outline
Introduction on (bio)chemical microsensors
MDA : A versatile transducer PRIMS Technological facilities Conclusion and prospects
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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From materials to devices … in the MEMS fieldAlternative solution to all‐silicon MEMS (‘home‐made’
‘printed’) or silicon MEMS (processed in other Labs)
(Chemists, Physicists, Technologists and Electronicians)
PRIMS: Printed MEMS Team
Materials Patterning
Modeling, Characterization, Optimization
MEMS Components
Applications
Chemical Sensors, Materials Characterization, Physical Sensors, Actuators, Energy Harvesting, Structural Health Monitoring
© IMS Property
Some Examples of Research Fields
Materials Patterning
Modeling, Characterization, Optimization
MEMS Components
Applications
Chemical Sensors, Materials Characterization, Physical Sensors, Actuators, Energy Harvesting, Structural Health Monitoring
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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MEMS Microstructuration
Spray + stencil + sacrificial layerScreen‐printing + sacrificial layer(Univ Bx 1 /IMS Patent)
ADVANTAGES :
•low cost•collective fabrication•large choice of substrates and starting materials•components and electronics•bio‐compatibility (organic) •harsh environment (inorganic)…
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Organic Microcantilevers
SU8 microcantilevers :- Photolithography- Wafer bonding
Methacrylate-based microcantilevers:- Spray and stencil
Epoxy /carbon microcantilevers:- Screen-printing
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PMMA
Biomimetic molecularly imprinted polymer (MIP)
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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Printed Inorganic Microstructures
Electroded piezoelectric microstructuresPZT Au/PZT,BST/Au bridges and disks
Copper, silver and vitroceramiccantilevers
Passive components:- clamped and free-standing Pt resistors
- vitroceramic and silver channels
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Some Examples of Research Fields
Materials Patterning
Modeling, Characterization, Optimization
MEMS Components
Applications
Chemical Sensors, Materials Characterization, Physical Sensors, Actuators, Energy Harvesting, Structural Health Monitoring
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Analytical Modeling of Physical Phenomena in MEMS• Fluid/Structure interaction
• Fluid flow around vibrating structures• Hydrodynamic forces on structures• Fluid viscoelasticity incorporated in the model
• Viscoelastic properties of materials in these components• Influence of the viscoelasticity of the sensitive coatings in static mode
(overshoot)• Influence of the viscoelasticity of a coating on both the resonant
frequency and the quality factor (characterization of mechanical properties of organic thin films)
• Taking into account of the modification the viscoelasticity of the coating during sorption
• Viscoelastic microcantilever
© IMS Property
Some Examples of Research Fields
Materials Patterning
Modeling, Characterization, Optimization
MEMS Components
Applications
Chemical sensors, Materials characterization, Physical Sensors, Actuators, Energy Harvesting, Structural Health Monitoring
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Variation of the resonant frequency
Mass modification
Variation of deflection
Stress/strain modification
Dynamic mode Static mode
Microcantilever for Chemical Detection
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Project: Andra MicH2
L=2mm, b=400µm, h=15µm, f0=5.4kHz
Dynamic mode: Detection with uncoated microcantilevers
Collaboration Andra
Variation of resonant frequency
Modification ofFluid density or viscosity
Dynamic Mode
Fluid
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Project: CTP PiezoBenz (2012‐2013)
Use of in‐plane mode for species detection in liquid or gaz
Benzene detection with CNTs sensitive coating
67552
67553
67554
67555
67556
0 2000 4000 6000 8000 10000 12000 14000
Time (s)
1 ppm benzene
air
30 min 30 min
1 ppm benzene
air air1 ppm benzene
1 ppm benzene
Coll. Spain URV Tarragona and INA Zaragossa
Influence of fluid viscosity Sensor
In‐plane displacementEelecV
Au electrodes
Piezoelectric PZT material
socket Substrate
P
2x8x0.1mm3
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0.00 0.01 0.02 0.03 0.04 0.05
0
1
2
3
4
5
6
Design 1
Design 2
R
/R
Strain,
Project: SoftPiezoRes (2011‐2013)
Design optimization for improved strain sensing
Elaboration of hybrid piezoresistance (CNT/SU-8) for integrated transduction of cantilevers deformation
Collaboration: Philippe Poulin (CRPP, Bordeaux)
D. Thau et al., submitted (2013)
Static mode Dynamic mode
RH=50%RH=60%RH=70%
U-shape bi-layer cantilever patterned by graphtec method
CNT/SU-8 piezoresistance on PET film
Integrated resonance transduction for application to
humidity sensing
100 m100 m
c) d)
Deflection profile and corresponding
piezoresistive response
Gauge factor up to 200
CNT/SU-8 piezoresistance on SU-8
Gold path
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Project: ANR PODCAST (2013‐2016)
Analytes
recognitionSubstrate
Sacrificial layer support
Organic
supporting
layer
Organic
sensitive layerOrganic
passivation layer
Electrodes
Improved organic
FET transducer
All‐organic MEMS for Chemical detection of water pollutants
Static mode FET for strain measurement
Technology Spray + stencil
Sensitive layerMIP
Collaboration UTC Compiègne
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Project: ANR ELENA (2013‐2016)
PRINCIPLEEnvironmental vibrations stress/strain permittivity change of electrostrictive layer capacity change electronics for energy harvesting
Energy Harvesting
Organic cantileverHigh mass part (composite)Low stiffness part (organic)Electrostrictive layer (CNT composite)Electrodes
Technology Screen‐printingSpray + stencil Sacrificial layer technique Ink jet
Collaboration CRPP, LOF Industrial partner : Rhodia-Solvay
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Project: ANR AMOS (2011‐2015)
Advanced Materials for Optical Sensing (T, gas)
Collaboration ICMCB Bordeaux, LCC Toulouse, IPREM Pau
Sensing principleUV radiation + {Temperature, Gas} modified photo‐luminescence
Materials‐ Nanoparticules (NPs) of oxyde semiconductors (<20 nm)‐ Organometallic or supercritical synthesis methods
Patterning‐NPs embedded in resin for screen‐printing‐Dispersion and thickness layer’s influences studied
50nm
5.8 (0.9)
NPs de ZnO (LCC)
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Piezoelectric screen‐printed microceramics for SHM, energy harvesting, sensing, actuating
Easier Shaping: straightforward electroded ceramics,
Thickness: thin film<thick film<ceramic
Project: PICOSSER (2012‐2013)
Sample T33 tanδ kp (%) -d31(pC/N)
fres (kHz)
Printed Au/PZT/Au 9.5mm,
Thick. 190µm634 0.015 14 40 166
Pellet Au/PZT/Au,11.5mm,
Thick. 950µm930 0.015 46 82 140
Commercial Ceramic PIC15110mm,
Thick. 200µm
2900 0.015 66 200
241
Sensor: vibration test
SHM:EMI measurements
Coll. ICMCB, ISAE, Industrial partners : TEMEX-Ceramics , Rescoll
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Collaborations (2008‐2013)
• National academic collaborations: • Bordeaux: Université Bordeaux 1 (CRPP, ISM, ICMCB, LOMA, LOF)• Toulouse: LAAS, LGM (INSA), ISAE, LCC• Compiègne: UTC• Lyon: LGEF (INSA) • Paris: IEF, SATIE• Montpellier: LIRMM • Pau : IPREM
• International academic collaborations: • Austria: Johannes Kepler University, Linz• Spain: Université Rovira y Virgili, Tarragona ; Université Publique de Navarre,
Pamplona; Institut des Nanosciences en Aragon, Zaragossa• United States: Marquette University, Milwaukee ; Georgia Institute of
Technology, Atlanta• Switzerland: ETH Zurich• Thaïland: Prince of Songkla University, Songkla ; MTEC, Bangkok
• Industrials or institutional collaborations: Andra, Ademe, Fondation EADS, NXP, Rhodia, SENSOTRAN, RESCOLL, TEMEX‐Ceramics, SODEMASA
© IMS Property
Outline
Introduction on (bio)chemical microsensors
MDA : A versatile transducer PRIMS Technological facilities Conclusion and prospects
Séminaire CAP’TRONIC “Les capteurs de demain” IMS Bordeaux - 3/10/2013
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• Clean room class 10 000 (hood 100)
• Thin films microprocessing:
spin-coater, spray-coater, Graphtec, mask aligner,
hotplates, wet etching of photoresists
• Thick films processing:
screen printers, ovens, inks formulation
• Wire-bonding assembly:
ball-bonder, wedge-bonder, flip-chip
Technological facilities (TAMIS)
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• Films and devices characterization: profilers, AFM, SEM,
vibrometer, gain/phase analyzer, network analyzer, etc.
• Soft lithography
• Mechanical micro-fabrication
Technological facilities (TAMIS)
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Outline
Introduction on (bio)chemical microsensors
MDA : A versatile transducer PRIMS Technological facilities Conclusion and prospects
© IMS Property
Equipe MDA, en brefMicrosystèmes de Détection à Ondes Acoustiques …et Alternatifs?
Membres– 5 permanents
– 3 doctorant(e)s
Thèmes– Détection en milieu gazeux (composés toxiques à l’état de traces, COV, …),
ambiance sévère haute température– Détection en milieu liquide, bio‐capteurs : détection de micro‐organismes
(bactéries‐virus‐toxines) et de métaux lourds, applications aux domaines de l’environnement, de la santé, du contrôle qualité…
– Mise en œuvre et caractérisation de matériaux en films, détermination dynamique de paramètres viscoélastiques (polymères, hybrides méso‐ et nano‐structurés, biomatériaux)
– Caractérisation de fluides complexes, applications à la chimie haut débit
C.DejousProf.
H.HallilMCF
J.L.LachaudIng.
V.RaimbaultCR2
D.RebièreProf.
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Compétences mobilisées– Propagation d'ondes acoustiques de surface dans des dispositifs multicouches– Intégration de films sensibles de reconnaissance: polymères, matériaux
carbonés, hybrides, méso‐ et nano‐structurés, biomatériaux– Intégration avec des puces microfluidiques– Compréhension et modélisation des mécanismes d'interaction:
onde et gaz‐liquide‐solide, effet de l'immobilisation de composés (bactéries, virus, toxines, métaux lourds, COV...), effet de la température
– Réalisation de prototypes de plateformes ultrasensibles pour la détection précoce et le suivi dynamique
– Nouveaux thèmes:microfluidique digitale, intégration de mesures par microscopie sans lentille en film mince organique, par microrésonateur optique ou HF ‐ low cost and green technologies
Réalisations technologiques– Laboratoire IMS plateforme TAMIS
(Technologies Alternatives aux Microsystèmes Silicium)– LAAS‐CNRS (plateforme RTB)
Equipe MDA, en brefMicrosystèmes de Détection à Ondes Acoustiques …et Alternatifs?
Droplet division ‐ CJ Kim & Sung Kwon Cho ‐ UCLA
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PRIMS: Printed MEMS Team http://www.ims‐bordeaux.fr/equipe.php?guidPage=PRIMS_english
6 Permanent positions 1 senior researcher
2 professors
1 junior researcher
2 associate professors
3 Post-doc,
1 Temporary engineer
5 PhD students
Cédric Ayéla
Benjamin Caillard
Hélène Debéda
Isabelle Dufour
Claude Lucat
Claude Pellet
Damien Thuau
Zouhair Brouzi
Nouha Allouch
Etienne Lemaire
Martin Heinisch
Mohand-Tayeb
Boudjiet
Pierrick Clément
Van Son Nguyen
HusseinNesser
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From materials to devices … in the MEMS fieldAlternative solution to all‐silicon MEMS (‘home‐made’ ‘printed’) or silicon MEMS (processed in other Labs)
(Chemists, Physicists, Technologists and Electronicians)
PRIMS: Printed MEMS Team
Materials Patterning
Modeling, Characterization, Optimization
MEMS Components
Applications
Chemical Sensors, Materials Characterization, Physical Sensors, Actuators, Energy Harvesting, Structural Health Monitoring
© IMS Property
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