About Sensors at IMS Bordeaux Labs - CAP’TRONIC fabrication process + ... Whole cell ‐based...

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

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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



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Outline

Introduction on (bio)chemical microsensors

MDA : A versatile transducing platform PRIMS Technological facilities Conclusion and prospects

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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



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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



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Versatile sensing platform

Coupling mechanisms- Mass- Viscosity- Conductivity- Permittivity- Stiffness- ...

Electronics

S1

S2 S3

Sensitivity : S1 x S2 x S3

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Outline


MDA : A versatile transducer PRIMS Technological facilities Conclusion and prospects



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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)



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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



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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



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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



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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



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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 (%)



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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



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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



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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



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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



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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



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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

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Outline





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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

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Some Examples of Research Fields



MEMS Components

Applications




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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)



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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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MEMS Components

Applications




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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

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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

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Outline





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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



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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



MEMS Components

Applications


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About Sensors at IMS Bordeaux Labs - CAP’TRONIC fabrication process + ... Whole cell ‐based...

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