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


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…


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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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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


SAW-LW

PDMS

absorber

Sensing area

Upper part of the cell

PDMS absorbers1 mm high × 1mm width

PDMS seal

Spring contacts


www.awsensors.com12

PDMS seal


SAW-LW


www.awsensors.com13

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


www.awsensors.com

are possible.


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


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


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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


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


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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


IMMUNOSENSOR ASSAY

SAMPLE

INJECTION

HCl

PBST

PBST

FLOW

SPEED

CHANGEPH

AS

E



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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.


[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


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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


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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


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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


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


CE

Vϕϕϕϕ(ω)(ω)(ω)(ω)

∆V(ω) ∆E(ω)

∆I(ω)


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CE

REF

WE

GND

∆I(ω)

Ε+∆V(ω)SET-UP:

• A20RP

• SOLARTRON 1254A FRA

• CUSTOM High BW PSTAT


HFF-QCM

RAW Phase Signal (1mHz - 65KHz)


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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!


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THANKS FOR YOUR ATTENTION!

a research-oriented platform for acoustic wave sensors for

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