Combined atomic force microscope and acoustic wave devices: application to electrodeposition.

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1 Combined atomic force microscope and acoustic wave devices: application to electrodeposition. J.-M. Friedt, L. Francis, K.-H. Choi, F. Frederix and A. Campitelli October 23, 22

2 Aim Development of biosensors based on acoustic wave devices: requires to understand the sensing mechanism in liquid medium. Biological reactions are too slow: use of electrodeposition (fast, reversible and more reproducible). Look at the nm scale what is happening and relate the observations to the frequency variations.

3 Principle QCM ( c=constant) SAW device ( λ=constant) λ/2 k k QCM: m λ f SAW: m c Φ f } what about additional viscosity effects? Advantages of SAW: higher sensitivity (when properly designed) open back side for adding more sensing techniques sensing electrode is not used/polarized PDMS flow cell air Quartz (c) Love mode device: sensing area (Au) SiO 2 (c <c) PDMS flow cell air

4 MODULEF : 2/11/1 mail coor sol.b friedtj 2862 NOEUDS 9684 FACES 24 PENTAEDRES 128 HEXAEDRES OBSERVATEUR SPHERIQUE : E-1 OUVERTURE : 1. QCM/AFM combination X Z O Y ISOVALEURS : 2 INCONNUE : 4 MNEMO :PHIE E E E E E E E E E E E E E E E E E E E E-7 PEAU + ELIMINATION - static finite element analysis: out of plane displacement A is.1 pm - A dynamic = A static Q out of plane displacement is.3 nm (Q 3) - in plane displacement is at most 3 nm, smaller than AFM pixel size - standing wave pattern between QCM and cantilever holder only disturbs the resonance frequency during approach - fundamental resonance frequency (5 MHz) is unstable and overtones of the QCM must be used Use of commercial instruments: - Q-Sense (Göteborg, Sweden) for QCM-D monitoring (overtones 1, 3, 5, 7+Q factor) - Molecular Imaging (AZ, USA) AFM X X Z O Y DC potential (.5 V) MODULEF : 2/11/1 mail coor sol.b friedtj 2862 NOEUDS 9684 FACES 24 PENTAEDRES 128 HEXAEDRES OBSERVATEUR SPHERIQUE : E-1 OUVERTURE : 1. ISOVALEURS : 2 INCONNUE : 1 MNEMO :VN E E E E E E E E E E E E E E E E E E E E-8 PEAU + ELIMINATION In-plane displacement (1 pm) Z O Y MODULEF : 2/11/1 mail coor sol.b friedtj 2862 NOEUDS 9684 FACES 24 PENTAEDRES 128 HEXAEDRES OBSERVATEUR SPHERIQUE : E-1 OUVERTURE : 1. ISOVALEURS : 2 INCONNUE : 2 MNEMO :VN E E E E E E E E E E E E E E E E E E E E-7 PEAU + ELIMINATION In-plane displacement (.1 pm) X Z O Y MODULEF : 2/11/1 mail coor sol.b friedtj 2862 NOEUDS 9684 FACES 24 PENTAEDRES 128 HEXAEDRES OBSERVATEUR SPHERIQUE : E-1 OUVERTURE : 1. ISOVALEURS : 2 INCONNUE : 3 MNEMO :VN E E E E E E E E E E E E E E E E E E E E-7 PEAU + ELIMINATION Out-of-plane displacements (.1 pm)

5 Measurements d/dt( f 3 ), i d/dt(< f > ) 3 1 i* d/dt( f 3 ), i E (V).1 E (V) D 5 ( 1 6 ) D 5 ( 1 6 ) 2 1 f 5 (Hz) f 5 (Hz) 1 2 D 3 ( 1 6 ) D 3 ( 1 6 ) f 3 (Hz) f 3 (Hz) 1 photodetector laser beam Pt (CE) glass prism (RE) Z 1 nf (15 MHz) Z (25 MHz) =6 Ag =11 Ω Ω AFM cantilever teflon liquid cell viton O ring QCM Q Sense QCM parameters measurement setup Gamry potentiostat L=1 µ H (WE) Z (15 MHz) =942 Ω Z (15 MHz) =1578Ω i*1 4 2 d/dt(< f 3 > 2 ) Cu Rigid layer f n /n m layer (low damping) with n: overtone number Viscous layer f n / n { m liquid, m layer } (large damping)

6 Experimental setup Open loop monitoring Closed loop monitoring Network analyzer Φ, IL I.L. (db) frequency f (f MHz) Φ slope: 36 o /61.38 khz 167 Hz/ o G x 1 5 Open/closed loop operation: requires a 4-port network analyzer PLL setup: compensate for energy losses (and phase shift) Problem: liquid must not reach the IDTs Φ ( o ) f (f MHz) x 1 5

7 Measurements device 11 (1.38 µm SiO 2 ), 1 2 CuSO 4, 1 2 H 2 SO 4 m Cu = I δt N e M Cu n e 1 E(V) N e = 9644 C: 1 Faraday M Cu = 63.5 g/mol, n e = x 1 4 device 11 (1.38 µm SiO 2 ), 1 2 CuSO 4, 1 2 H 2 SO f (MHz) E(V) x x f (MHz) I (ma) x x 1 4 I (ma) 1 time (a.u.) x 1 5

8 Sensitivity estimates S 12 S = f f A m cm2 /g sensitivity (cm 2 /g): S=(A f)/(f m) Love mode: 1.38 µm SiO 2 Love mode: 2.96 µm SiO 2 S 58 QCM (Sauerbrey, 1 MHz): S 23 A: sensing area ( mm 2 ) f : center frequency (123.7 MHz) m: deposited mass (electrochemistry) f: frequency variation 1 QCM (Sauerbrey, 5 MHz): S mass (ng, estimated from electrochemistry) S assumed to be constant, m. Good fit when including offset in the current measurement by the potentiostat rigid mass.

9 AFM combination Monitoring simultaneously Φ f, m and topography at the nm scale S 7..8 for m = µg (S QCM 2 cm 2 /g).

10 Conclusion and perspectives ability to independently measure deposited mass and frequency shift estimation of the sensitivity: constant over the mass range analyzed high sensitivity of Love mode device ( 1 times more sensitive than QCM) - fluidics setup (IDTs protection) - application to biology: replace electrochemical cell by biochemical reactions - combination with other detection methods (SPR) Copies of the slides at

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