A Research-Oriented Platform For Acoustic Wave Sensors For ...
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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
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Introducing AWSensors
Spin-off of UPV
Advanced Wave Sensors
www.awsensors.com
7 Persons
2 from UPV (2 PhD)
5 employes (4 PhD)
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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
www.awsensors.com
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.
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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
Advanced Wave Sensors
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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
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WORK WITH VHF SENSORS
Acoustic Wave
Devices
Acoustic Wave
Devices
BAWBAW SGAWSGAW
VHF?
Advanced Wave Sensors
www.awsensors.com
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
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IMPROVING S/N
SEVERAL ASPECTS TO TAKE INTO ACCOUNT:
a) Characterization Interface – Method and
Technology
b) Solving problems with sensors:
Advanced Wave 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.
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IMPROVING S/N
NOISE – SENSITIVITY - LOD
ϕ
Advanced Wave Sensors
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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)
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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
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SOLVING SENSOR PROBLEMS
HFFQCM
Advanced Wave Sensors
www.awsensors.com
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SOLVING SENSOR PROBLEMS
HFFQCM
Advanced Wave Sensors
www.awsensors.com
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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
Advanced Wave Sensors
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c)
Spring contacts (no wire bonding)
Transparent PMMA
(visual contact)
11Aluminum
PCB
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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
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SOLVING SENSOR PROBLEMS
SAW-LW
Advanced Wave Sensors
www.awsensors.com13
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CONTROL FLUIDICS
NOISE DUE TO FLUIDICS
NOISE DUE TO TEMPERATURE
A10
Advanced Wave Sensors
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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
Advanced Wave Sensors
www.awsensors.com
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
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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
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
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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
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Research Platform – Operation ModesA
MP
LIT
UD
E
SWEEP MODE ON A LW SENSOR
Advanced Wave Sensors
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SELECTED FREQUENCY FOR
FAST MODE OPERATION
PH
AS
E
FREQUENCY
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IMMUNOSENSORS: Fast Acquisition Mode
Carbaryl MAb
Analyte (carbaryl)Love SAW
Pesticide Carbaryl detection: Low molecular weight compound
Advanced Wave Sensors
www.awsensors.com
Hapten-conjugate
SAM
Au
HFF-QCMQCM
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AM
PLI
TU
DE
SWEEP MODE ON A LW SENSOR
IMMUNOSENSORS (LOVE-SAW): Fast Acquisition Mode
Am
plit
ud
eTe
mp
era
ture
Advanced Wave Sensors
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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
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Am
plit
ud
eTe
mp
era
ture
IMMUNOSENSORS (HFF-QCM): Fast Acquisition Mode
Advanced Wave Sensors
www.awsensors.com
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
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IMMUNOSENSORS (HFF-QCM): Fast Acquisition Mode
Advanced Wave Sensors
www.awsensors.com
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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
Advanced Wave Sensors
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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.
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IMMUNOSENSORS (HFF-QCM): Fast Acquisition Mode
[Carbaryl]<100 µg/L
Advanced Wave Sensors
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[Carbaryl]
2000µg/L
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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
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IMMUNOSENSORS (HFF-QCM): Tracking Mode
[Carbaryl]
2000µg/L
Advanced Wave Sensors
www.awsensors.com
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)
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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
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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
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(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
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(EQCM) AC-Electrogravimetry: Fast Acquisition Mode
HFF-QCM
RAW Phase Signal (1mHz - 65KHz)
Advanced Wave Sensors
www.awsensors.com
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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
Advanced Wave Sensors
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A RESEARCH ORIENTED PLATFORM
OPEN PLATFORM:
Adaptable to researcher:
Different Sensors
Software integrable with users software
Advanced Wave Sensors
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Software integrable with users software
Customized cells
Combined with other techniques
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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
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THE END
THANKS FOR YOUR ATTENTION!
Advanced Wave Sensors
www.awsensors.com
THANKS FOR YOUR ATTENTION!