Silicon-Based Resonant Microsensors O. Brand, K. Naeli, K.S. Demirci, S. Truax, J.H. Seo, L.A. Beardslee

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Silicon-Based Resonant Microsensors O. Brand, K. Naeli, K.S. Demirci, S. Truax, J.H. Seo, L.A. Beardslee School of Electrical and Computer Engineering g Georgia Institute of Technology Atlanta, GA 30332-0250, USA E-mail: oliver.brand@ece.gatech.edu http://mst.ece.gatech.edu

Outline Resonant Microsensors Operation Principles and Applications Frequency-Output Sensors Operation in Feedback Loop Device vs. System-Level Resonant Sensor Frequency Resolution and Drift Drift Compensation Techniques (Bio)Chemical Resonant Microsensor Platform Disk-Type Microstructure t Optimization i Chemical Sensing Summary and Outlook Nano@Tech, October 21, 2008 O. Brand, Slide 2 of 34

Resonant Sensors Measurand affects characteristic of resonant behavior of microstructure 1.5 1.0 A f f ~ Q -1 0.5 Resonance frequency Quality factor 0 0 Vibration amplitude Phase -100 [µm] Am mplitude Phase [degree es] -200 43 45 47 49 Frequency f [khz] Nano@Tech, October 21, 2008 O. Brand, Slide 3 of 34

Resonant Sensors Nano@Tech, October 21, 2008 O. Brand, Slide 4 of 34

Why Resonant Sensors? Resonant Sensors Quasi-digital output signal Frequencies can be measured precisely If Combined with CMOS Technology Established fabrication base On-chip circuitry Fabrication outsourcing Analog Devices ADXRS 150 Nano@Tech, October 21, 2008 O. Brand, Slide 5 of 34

Frequency-Output Sensors Working Principle d2 x dx m dt 2 + b dt + k x = F i Device-Level Frequency Sensor F = F 1 = b dx dt f = 1 2π k m Δf f = 1 Δk 2 k Δm m System-Level Frequency Sensor F = F 1 + F 2 + F 3 = b dx + k d 2 x add x + m add f = 1 k k add dt dt 2 2π m m add Δf f = 1 2 m add m k add k Nano@Tech, October 21, 2008 O. Brand, Slide 6 of 34

Device-Level Frequency Sensor In steady state, the excitation force compensates for damping loss and microstructure vibrates with constant amplitude Changes of the effective spring constant or mass result in a measurable frequency change Nano@Tech, October 21, 2008 O. Brand, Slide 7 of 34

System-Level Frequency Sensor Excitation force component proportional to deflection (or acceleration) is modulated by measurand Feedback loop introduces measurable frequency change Nano@Tech, October 21, 2008 O. Brand, Slide 8 of 34

Resonant Magnetic Field Sensor Working Principle Current through coil I = k B x generates Lorentz force F L proportional to the cantilever deflection x in presence of magnetic field F L = qv B ( )= IL C B = k B xl C B Assume: resonator damping compensated by thermal bimorph actuation m d2 x dt 2 = kx +F L = (k B L C B k)x f = 1 2π k m = 1 2π k k B L C B m Nano@Tech, October 21, 2008 O. Brand, Slide 9 of 34

Resonant Magnetic Field Sensor Microstructure Design Coil L C Thermal Actuator Wheatstone Bridge R. Sunier et al., IEEE J. MEMS, 15 (2006) 1098-1107 Nano@Tech, October 21, 2008 O. Brand, Slide 10 of 34

Magnetic Field Detection Sensor Sensitivity Resonance freq.: 176 khz Quality factor: 600 (in air) Short-term freq. stab.: 25 mhz Sensitivity: 60 khz/t Resolution: 1 µt Sensor offset compensation by switching off magnetic feedback Nano@Tech, October 21, 2008 O. Brand, Slide 11 of 34

Resonant Sensor Resolution Sensor resolution is limited by sensor sensitivity S [Hz/ measurand change ] and minimal detectable frequency change f min [Hz] c min = Δf min S Limit of Detection (LOD) is measurand amplitude that generates three times the noise amplitude, i.e. LOD = 3 Δf min S Minimizing f min generally demands maximizing quality factor Q; e.g. for cantilever in amplifying i feedback loop Δf min = f 0 k B TB Albrecht et al., 2πk Q x 2 J. Appl. Phys. 69 (1991) 668 Nano@Tech, October 21, 2008 O. Brand, Slide 12 of 34

Silicon Cantilever Beam Q-Factor Optimization Support loss Air damping K. Naeli et al., Proc. Transducers 07, L/t 15-20 pp. 245-248 Nano@Tech, October 21, 2008 O. Brand, Slide 13 of 34

Silicon Disk-Resonators Allan Variance vs. Gate Time Increase due to Long-Term Drift σ 2 m 1 ( τ,mm )= γ 2m n+1 γ n n=1 γ n = f n+1 f n f n ( ) 2 Nano@Tech, October 21, 2008 O. Brand, Slide 14 of 34

Drift Compensation: Method I Controlled Stiffness Modulation Compensation in closed-loop operation! Δk k ΔQ Q J.H. Seo et al., J. Appl. Phys. 104 (2008) 014911 Nano@Tech, October 21, 2008 O. Brand, Slide 15 of 34

Q-Factor Tracking via Periodic Stiffness Modulation 2 ω POS = α ω NEG Q = α+1 α 1 Nano@Tech, October 21, 2008 O. Brand, Slide 16 of 34

Temperature Compensation via Q-factor Tracking Uncompensated: df/dt - 33 ppm/ C Compensated: df/dt < 2 ppm/ C J.H. Seo et al, Proc. Hilton Head Workshop, pp. 190-193, 2008 Nano@Tech, October 21, 2008 O. Brand, Slide 17 of 34

Drift Compensation: Method II Overtone Analysis in Prismatic Beams Goal: Compensation for environmental effects in cantilever-based mass-sensitive sensors Idea: Explore flexural resonances of partly-covered beams Key: Flexural resonance frequencies of prismatic, homogeneous beam only differ by i f i = i t 2π 12 L 2 λ i 2 Assumption: added mass does not affect k! Difference of relative frequency changes f i /f i f j /f j only depends on added mass but NOT on environmental changes! E ρ Nano@Tech, October 21, 2008 O. Brand, Slide 18 of 34

Temperature Compensation via Overtone Analysis O. Brand, K. Naeli et al., Proc. MME 2008 Workshop, pp. 121-127, 2008 Nano@Tech, October 21, 2008 O. Brand, Slide 19 of 34

Temperature Compensation via Overtone Analysis f i /f i f j /f j Uncompensated: df/dt - 20 ppm/ C Compensated: df/dt 0.2 02 ppm/ C O. Brand, K. Naeli et al., Proc. MME 2008 Workshop, pp. 121-127, 2008 Nano@Tech, October 21, 2008 O. Brand, Slide 20 of 34

Resonant BioChemical Sensors Approach: Recognition film deposited onto microresonator ad- /absorbs analyte, thus lowering the microstructure s s resonance frequency Implementations: Acoustic wave devices, tuning forks, cantilevers Applications: Chemical safety, surveillance applications, environmental monitoring, medical diagnosis Sensor Arrays: Sensor selectivity through sensor arrays coated with different recognition films D. Lange et al., Anal. Chem. 74 (2002) 3084-3095 Nano@Tech, October 21, 2008 O. Brand, Slide 21 of 34

Resonant Sensor Platform for BioChemical Sensing Goal: Develop mass-sensitive sensitive sensor platform for biochemical applications in air/liquid Large sensing area High Q-factor Dynamic instead of static sensing principle Approach: Investigate in-plane (instead of out-of-plane) vibration modes to improve Q-factor Performance achieved so far: Q 5800 in air at f 620 khz Nano@Tech, October 21, 2008 O. Brand, Slide 22 of 34

Disk-Shape Resonator Semi-discs to be coated with sensitive layer Center of rotation with sensing/actuation elements Support beam J.H. Seo, O. Brand, IEEE J. of MEMS 17 (2008) 483-493 493 Frequency 400-600 khz Sensitivity 1 Hz/pg Nano@Tech, October 21, 2008 O. Brand, Slide 23 of 34

Driving and Sensing Structure Thermal Actuation Asymmetric arrangement of two heating resistors Thermal expansion coefficient difference of Al and Si Piezoresistive Sensing Wheatstone bridge sensitive only to desired in-plane vibration mode EX1 VCC RD+ RD- GND EX2 Nano@Tech, October 21, 2008 O. Brand, Slide 24 of 34

2 Fabrication Flow 3 Substrate : Epi-wafer (5-10 μm nlayer) n-layer) 4 1. Wet thermal oxidation 2. Pattern oxide & boron diffusion 3. Thermal oxidation (Drive-in & oxidation) 4. RIE etching of contact openings 5. DC sputter & pattern Al 6. PECVD oxide & nitride deposition 7. Pattern back side nitride & oxide layer 8. Anisotropic KOH etch 9. Release structure with RIE 5 6 8 9 N-Epi P-Si SiO2 P-Diff. Al SiNx Nano@Tech, October 21, 2008 O. Brand, Slide 25 of 34

Transfer Characteristic Quality factor in air up to 5,800; in water up to 100 Nano@Tech, October 21, 2008 O. Brand, Slide 26 of 34

Resonance Frequency J.H. Seo, O. Brand, IEEE J. of MEMS 17 (2008) 483-493 Nano@Tech, October 21, 2008 O. Brand, Slide 27 of 34

Quality Factors in Air & Water AIR WATER = ω 0 ρ Q t 2 ν ρ fluid Nano@Tech, October 21, 2008 O. Brand, Slide 28 of 34

Sensitive Layer Coating Polymers for VOC enrichment PIB: poly(isobutylene) PECH: poly(epichlorohydrin) Polymer coating techniques Drop Coating: Dispensing from syringe or BioForce Nano enabler Spray Coating: Dispensing with spray gun Polymer film thickness 2-5 µm in air < 1 µm in water Disk resonator drop-coated with polymer film Nano@Tech, October 21, 2008 O. Brand, Slide 29 of 34

Gas-Phase VOC Sensing Exposure to different concentrations of o-xylene 4 µm spray-coated polymer films Turn-on and turn-off transients t < 5 sec Short-term frequency stability 80 mhz (at 710 khz & Q = 940) LOD 2 ppm for PIB/o-xylene S. Truax et al., Proc. MEMS 2008, pp. 220-223 Nano@Tech, October 21, 2008 O. Brand, Slide 30 of 34

Sensitivities in Gas Phase S. Truax et al., Proc. MEMS 2008, pp. 220-223 Nano@Tech, October 21, 2008 O. Brand, Slide 31 of 34

Summary & Outlook Resonant Microsensors Benefit from wide applicability and (potentially) excellent resolution Frequency modulation can be introduced d on device or system -level Effective methods for compensating long-term drift are essential and available Resonant Chemical Microsystem Demonstrated Q up to 5,800 in air and 100 in water Demonstrated gas (and liquid-phase) chemical sensing with ppm resolution Demonstrated drift compensation via controlled stiffness modulation Nano@Tech, October 21, 2008 O. Brand, Slide 32 of 34

Acknowledgements Applied Sensors Laboratory, Georgia Tech Prof. B. Mizaikoff, Y. Luzinova, G. Dobbs ETH Zurich, Switzerland Prof. A. Hierlemann, Dr. P. Kurzawski for help with gas-phase measurements NSF for funding part of the work Cantilever work: 0304009 Gas-phase Chemical Sensor: ECCS-0601467 Liquid-phase Chemical Sensing: CBET-0606981 Nano@Tech, October 21, 2008 O. Brand, Slide 33 of 34