a research-oriented platform for acoustic wave sensors for

A Research-Oriented Platform

For Acoustic Wave Sensors

Advanced Wave Sensors

www.awsensors.com

Besancon

December 2013

Antonio Arnau

Polytechnic University of Valencia

For Acoustic Wave Sensors

Introducing AWSensors

Spin-off of UPV

Advanced Wave Sensors

www.awsensors.com

7 Persons

2 from UPV (2 PhD)

5 employes (4 PhD)

Introducing the Platform

Why to develop this platform?

We worked on Electronics for QCM applied to

Biosensors

The principle of operation worked fine for 10MHz

sensors, but…

Advanced Wave Sensors

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sensors, but…

LOD was worse in comparison with other label-free

technique like SPR, and much worse in comparison

with ELISA, 3 orders of magnitude;

However from our point of view, AW-Biosensors have

some advantages on the previous techniques.

Introducing the Platform

PIEZOELECTRIC BIOSENSORS

• Easy calibration• Independent of optical properties• Sample preparation unnecessary or simple• Real binding detection• Direct detection

• Increasing the sensitivity, but with…• Increasing the Limit of Detection• Improving the reliability and robustness• Multi-array and multi-analysis detection

Strong Points Needs

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• Direct detection• Real-time monitoring• Low Cost (in principle)

1) To work with VHF resonators2) To improve the S/N ratio at VHF3) To Improve the functional system4) To work with arrays of sensors

CHALLENGES

WORK WITH VHF SENSORS

Acoustic Wave

Devices

Acoustic Wave

Devices

BAWBAW SGAWSGAW

VHF?

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TSM QCM

HFFQCM

TSM QCM

HFFQCM

FBARFBAR SAWSAW

SAW (Rayleigh)

SAW (Rayleigh)

SH-SAW (Leaky orPseudo)

SH-SAW (Leaky orPseudo)

STWSTW LWLW

APMAPM

SH-APMSH-APM LG-APMLG-APM FPWFPW

IMPROVING S/N

SEVERAL ASPECTS TO TAKE INTO ACCOUNT:

a) Characterization Interface – Method and

Technology

b) Solving problems with sensors:

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• Fragility (HFFQCM)

• Sealing (HFFQCM & LW)

without perturbing the sensors response

c) Careful control of all related with fluidics:

• Flow cells, pumps, valves, etc.

IMPROVING S/N

NOISE – SENSITIVITY - LOD

ϕ

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f0 f

SENSITIVITY – LOD OF THE APPLICATIONSample volume – Sensitive surface

Electrode diameter – Thickness of the resonator in Q CM – Fundamental frequencyDistance between ports – Resonant frequency in SAW-L W

Montagut, et al. REV. SCI.INSTRUM. 82, 064702 (2011)

CHARACTERIZATION TECHNIQUE

PHASE-SHIFT VS FREQUENCY SHIFT

1. Oscillators

• Noise of the rest of the elements is absorbed by the sensor, increasing noise with

frequency.

• Problems with HFFQCM

2. Comparing different acoustic techniques

A different point of view:

220

2400,2

0,4

|Z|φ

Z

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DIFFERENT OPERATION MODES SWEEP & TEST

Frequency (kHz)

99800 99820 99840 99860 99880 99900|Z

| (Ω

) 260

280

300

320

φ Z (

rad)

-0,4

-0,2

0,0

0,2

fTEST

Stage 1

Stage 2

SOLVING SENSOR PROBLEMS

HFFQCM

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SOLVING SENSOR PROBLEMS

HFFQCM

Advanced Wave Sensors

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SOLVING SENSOR PROBLEMS

SAW-LW17000 µm

84

00

µm

D = 3480 um

350

0 µ

m

Input RF

signal

Output RF

signal

Ground Ground

L = 7480 µm

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c)

Spring contacts (no wire bonding)

Transparent PMMA

(visual contact)

11Aluminum

PCB

SOLVING SENSOR PROBLEMS

SAW-LW

PDMS

absorber

Sensing area

Upper part of the cell

PDMS absorbers1 mm high × 1mm width

PDMS seal

Spring contacts

Advanced Wave Sensors

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PDMS seal

SOLVING SENSOR PROBLEMS

SAW-LW

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CONTROL FLUIDICS

NOISE DUE TO FLUIDICS

NOISE DUE TO TEMPERATURE

A10

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Research Platform

Three characterization modes are possible:

Sweep Mode

Fast Acquisition Mode

Tracking Mode (Soon)

Allows working simultaneously with classical QCM,

HFF-QCM and SAW Love. Other resonant technologies

are possible.

Integrated research-oriented Platform for AWS

A20 RP

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are possible.

Thermostatic chamberF20 RP

Up to 4 flow-through plug and play modules, each with:

1 Syringe Pump

1 6-5 Distribution Valve (6 ports + syringe port)

1 Injection Valve

1 solenoid pump for sampling

Thermostatic chamber

Research Platform

Three characterization modes are possible:

Sweep Mode

Fast Acquisition Mode

Tracking Mode (Soon)

Allows working simultaneously with classical QCM,

HFF-QCM and SAW Love. Other resonant technologies

are possible.

Integrated research-oriented Platform for AWS

Advanced Wave Sensors

www.awsensors.com

are possible.

Thermostatic chamber

Up to 4 flow-through plug and play modules, each with:

1 Syringe Pump

1 6-5 Distribution Valve (6 ports + syringe port)

1 Injection Valve

1 solenoid pump for sampling

Thermostatic chamber

Research Platform – Operation Modes

Am

plit

ud

eS

US

CE

PT

AN

CE

(B)

SWEEP MODE ON HFFQCM 100MHZ WITH INHARMONICS NEAR THE FUNDAMENTAL MODE

FAST MODE ON HFFQCM 100MHz

Advanced Wave Sensors

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Frequency

Ph

ase

SELECTED FREQUENCY FOR FAST

MODE OPERATION

SU

SC

EP

TA

NC

EC

ON

DU

CT

AN

CE

(G

)

FREQUENCYTIME

Ph

ase

FAST MODE ON HFFQCM 100MHz

IMMUNOSENSOR ASSAY

SAMPLE

INJECTION

HCl

PBST

PBST

FLOW

SPEED

CHANGEPH

AS

E

Research Platform – Operation ModesA

MP

LIT

UD

E

SWEEP MODE ON A LW SENSOR

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SELECTED FREQUENCY FOR

FAST MODE OPERATION

PH

AS

E

FREQUENCY

IMMUNOSENSORS: Fast Acquisition Mode

Carbaryl MAb

Analyte (carbaryl)Love SAW

Pesticide Carbaryl detection: Low molecular weight compound

Advanced Wave Sensors

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Hapten-conjugate

SAM

Au

HFF-QCMQCM

AM

PLI

TU

DE

SWEEP MODE ON A LW SENSOR

IMMUNOSENSORS (LOVE-SAW): Fast Acquisition Mode

Am

plit

ud

eTe

mp

era

ture

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SELECTED FREQUENCY FOR

FAST MODE OPERATION

PH

AS

E

FREQUENCYTime

Ph

ase

Am

plit

ud

e

Sample injection(MAb)

HCl

PBST

Flow speed change

PBST

Am

plit

ud

eTe

mp

era

ture

IMMUNOSENSORS (HFF-QCM): Fast Acquisition Mode

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Time

Ph

ase

Am

plit

ud

e

TIME

Ph

ase

FAST MODE ON HFFQCM 100MHz

IMMUNOSENSOR ASSAY

SAMPLE

INJECTION

HCl

PBST

PBST

FLOW

SPEED

CHANGEPH

AS

E

IMMUNOSENSORS (HFF-QCM): Fast Acquisition Mode

Advanced Wave Sensors

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COMPARISON OF DIFFERENT TECHNIQUES

Comparison between sensitivities and LOD of

Carbaryl Detection Immunoassays using different techniques

Parameters

Calibration

CurveaELISA SPR

QCM LOVE

9b,c 10b,d 50b,d 100b,d 120b,d

LOD 0,051 ; 0,01 2 1,411 30,341 4,001 0,231 0,141 0,271

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I50 0,221 ; 0,062 3,121 13,301 16,701 1,951 0,661 1,281

Wr 0,08-1,101 ; 0,02-0,182 1,91-5,751 18,30-50,301 7,00-35,001 0,50-7,201 0,26-1,721 0,48-3,301

a µg / L

b Fundamental Resonant Frequency (QCM) / Resonant Frequency (LOVE) (MHz)

c Frequency Shift Technique; d Phase-Shift Technique.

1 Standard Immunoassay; 2 Optimized Immunoassay.

IMMUNOSENSORS (HFF-QCM): Fast Acquisition Mode

[Carbaryl]<100 µg/L

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[Carbaryl]

2000µg/L

IMMUNOSENSORS (HFF-QCM): Tracking Mode

[Carbaryl]<100 µg/L

0,0035

0,0040

0,0045

t1t2

Advanced Wave Sensors

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frequency (MHz)

98,5 99,0 99,5 100,0 100,5 101,0 101,5

Con

duct

ance

(S

)

0,0010

0,0015

0,0020

0,0025

0,0030

t2

t1 t2

IMMUNOSENSORS (HFF-QCM): Tracking Mode

[Carbaryl]

2000µg/L

Advanced Wave Sensors

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0,0014

0,0019

0,0024

0,0029

0,0034

0,0039

0,0044

98900000 99400000 99900000 100400000 100900000

Co

nd

uct

an

ce (

S)

Frequency (Hz)

WEElectroactive film

REEs+∆E

solution

WEElectroactive film

REEs+∆E

solutionM

(EQCM) AC-Electrogravimetry: Fast Acquisition Mode

Advanced Wave Sensors

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WE WE

ES∆E

/mV

Time/s 0 500 10001500 2000 2500 3000-6

-4

-2

0

2

4

6

∆ Csp

eci

es/

mm

ole

s cm

-3

Time/s

HFF-QCMC

spec

ies/m

mol

escm

-3

∆m

/ng

∆φ

/rad

(EQCM) AC-Electrogravimetry: Fast Acquisition Mode

1c

L

mm

ϕ∆ ≈ − ∆

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∆C

Time/s Time/sTime/s

FAST ACQUISITION MODE CHARACTERIZATION FITS PERFECTLY!

• Small perturbations

• High resolution is necessary

(EQCM) AC-Electrogravimetry: Fast Acquisition Mode

CE

Vϕϕϕϕ(ω)(ω)(ω)(ω)

∆V(ω) ∆E(ω)

∆I(ω)

Advanced Wave Sensors

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CE

REF

WE

GND

∆I(ω)

Ε+∆V(ω)SET-UP:

• A20RP

• SOLARTRON 1254A FRA

• CUSTOM High BW PSTAT

(EQCM) AC-Electrogravimetry: Fast Acquisition Mode

HFF-QCM

RAW Phase Signal (1mHz - 65KHz)

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(EQCM) AC-Electrogravimetry: Fast Acquisition Mode

HFF-QCM

Electrogravimetric transfer function for 50MHz HFF-QCM

200nm Prussian Blue Film in 0.5M KCl

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A RESEARCH ORIENTED PLATFORM

OPEN PLATFORM:

Adaptable to researcher:

Different Sensors

Software integrable with users software

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Software integrable with users software

Customized cells

Combined with other techniques

FUTURE DEVELOPMENTS

E20 (First term 2014):

Autonomous EQCM with potentiostat integrated

with 3 operation modes:

Sweep, Fast and Tracking Mode

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Sweep, Fast and Tracking Mode

Multisensor platform for HTS:

12, 24, 96 sensores

For Biosensor Applications

THE END

THANKS FOR YOUR ATTENTION!

Advanced Wave Sensors

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THANKS FOR YOUR ATTENTION!