IEMN. Unité Mixte de Recherche 8520 Joint Research Unit Journée Trans GDR, 11 avril 2012 Besançon, France

Transcription

1 IEMN Unité Mixte de Recherche 8520 Joint Research Unit 8520

2 Apport des Microsystèmes pour la Microscopie à Force Atomique B. Walter, M. Faucher, E. Mairiaux, Z. Xiong, L. Buchaillot and B. Legrand IEMN Groupe NAM6 Nano & MicroSystems CNRS UMR 8520 Besançon, April 11 th 2012 NAM6 Group, IEMN UMR 8520 Cité scientifique, Avenue H. Poincaré, Villeneuve d Ascq, France IMPROVE-LM project

3 This is the first AFM! Soft lever in contact mode Detection by STM probe

4 1999 Resonators for mobiles Fabrication process Study of losses Study of damping 2006 ANR Grant for AFM probes GaN MNS new actuation scheme Resonators Process development 2008 ERC Grant for AFM probes AGILENT Grant Lack of interest from the industry for electro mech resonators Journée Trans GDR, 11 avril 2012 Besançon, 6/68 France

5 IEMN-NAM6 background on resonators 7/68

6 2009 AGILENT Grant ERC Grant Laureate Dr. Bernard Legrand in NAM6 Group

7 Context: High sensitive probes for AFM microscopy Opto-electronic sensing 1986: AFM s invention by Binnig + - To signal processing and feedback control Tip Sample Cantilever Piezoelectric driving Surface topography Force spectroscopy Application in material physics, chemistry and biology Piezoelectric scanners Z Y X Challenges: Microscopy on biological systems Imaging in liquid Study of nanobiological system dynamics High imaging rate Bottlenecks: Probe frequency limited to ~100kHz Resolution limited by hydrodynamic forces Optical detection not well adapted to liquid

8 Context: Existing Works Onaran et al., Rev. Sc. Inst., 77, (2006) Torun et al. Nanotechnology, 18, (2008) FIRAT probes Georgia Institute of Technology An et al., Appl. Phys. Lett. 87, (2005) Tokyo University - Nanonis Kolibri sensor, Nanonis Shape Membranes Length extension cantilever Frequency 20 MHz 1MHz Bandwidth 100 khz Noise < 10 fm/ Hz fm/ Hz Measurement In air In air & In liquid Transduction Capacitive actuation/optical detection Piezoelectric actuation/detection Tip process FIB deposition FIB deposition Performance High imaging rate Measurement in liquid

9 Biophysics Group, the Department of Physics, Kanazawa University, Professor Toshio Ando Myosin walking on actin filament 146ms/frame, 130x65nm²

10 Context: Existing Works Biophysics Group, the Department of Physics, Kanazawa University Professor Toshio Ando High speed AFM Cyclic Movement of Dynein C's Tail Driven by ATP Hydrolysis

11 Probe with integrated sensing IBM «Millipede» Thermal actuation Minne et al. APL (1995) 100µm KolibriSensor Quartz extensional mode f 0 = 1 MHz k = 540 kn/m Q = Intégrated actuation/sensing vertical probe Packaging Manual set up 13/68 Can not be batch processed

12 Conventional AFM probe Optical sense laser Piezoelectric drive Context: Our approach MEMS-based AFM probe Integrated Electrostatic driving MEMS ring resonator Elliptic Mode Sample Tip Integrated capacitive sensing Piezoelectric Scanners Z Y X ~100kHz Resonance frequency MHz to 1GHz 500 Quality factor Integrated sense & drive LASERLESS SOI micromachining process compatible Batch fabrication From 5000 to /68

13 Bulk mode resonators overview Square Ring Disk Original shape [1] Elliptic mode [2] Extensional mode Lamé mode [3] [1] Kaajakari, V., Mattila, T., Oja, A. et al. Square-extensional mode single-crystal silicon micromechanical rf-resonator, [2] Li, S-., Lin, YW., Xie, Y. et al. Micromechanical hollow-disk ring resonators, [3] Abdelmoneum, MA., Demirci, MU. and Nguyen, CT-. Stemless wine-glass-mode disk micromechanical resonators, /68

14 Context: Work history Probe concept Tip-liquid interaction «Proposition of Atomic Force Probes Based on Silicon Ring Resonators» Transducers 07, p1529 (2007) «Design and operation of a silicon ring resonator for force sensing application above 1MHz» J. Micromech. Microeng., 19, (2009) Tip-surface interaction 2009/2010: Probe integration in a commercial AFM AFM microscopy demonstration «Tip-Matter interaction measurement using MEMS Ring resonators» Transducers 09, p1638 (2009) 16/68

15 Fabrication Electrical contacts Photolithography and oxide RIE etching Si (20µm) SiO 2 (2µm) DRIE of the device layer Silicon Ring (Resonator) DRIE of the backside Si (300µm) Release of the resonator Electrodes (transduction) Metallic contacts Oxide Silicon SOI process fabrication by DRIE 200µm 50nm Expected frequency: 1MHz Ring radius: 200µm Tip etched by FIB 17/68

16 Probe integration in a commercial AFM Lock-in amplifier Piezo X,Y,Z Piezo controller Multimode Microscope Nanonis Controller Anti-vibration table

17 Probe integration in a commercial AFM Standard AFM probe holder MEMS-based probe holder Capacitive coupling nulling circuit Driving voltage V AC (ref) Bias voltage V DC Amplifier I V To Lock-in amplifier & Nanonis Controller 19/68

18 Output signal amplitude (µv) Probe characterization with the AFM set-up Resonance curve measurement f res =1.101 MHz V DC = 12 V Force curve measurement V AC =500mV V AC =250mV Frequency shift ( Hz) Interaction with a surface With external force Without external force Interaction force ΔA Tip-surface distance Driving frequency = MHz V DC = 12 V Driving frequency

19 AFM microscopy demonstration 2 µm-wide, 250 nm-high lines, spaced by 1 µm f=936khz V AC =250mV V DC =20V Setpoint amplitude 1µm/s 460 nm 2µm/s 460 nm 2 µm 5µm 10 µm 3µm 100 nm-wide, 30 nm-high lines, spaced by 400 nm f=942khz V AC =250mV V DC =20V 100nm/s 200nm/s 39 nm 260 nm 1µm 2µm 55 nm 280 nm

20 Noise measurements Spectral density analysis Signal phase noise analysis Signal amplitude noise: 130 nv/ Hz Signal phase noise: 30 mdeg/ Hz Limited by electronic noise and transduction efficiency 22/68

21 Probe performances Amplitude calibration: 350 µv 4 nm Signal amplitude noise: 130 nv/ Hz 4 nm Amplitude measurement resolution = 1.5 pm / Hz 15 mdeg/hz Phase slope: 15 mdeg/hz 65 Hz/deg = p Signal phase noise: = 30 mdeg / Hz Frequency measurement resolution: f = p f = 2 Hz / Hz Force gradient resolution: k 2k f 0 f = 0.4N.m -1 / Hz Force resolution = ~1 nn/ Hz 23/68

22 Partial conclusion Laserless AFM probes based on MEMS resonators AFM microscopy demonstration with MEMS-based probes 55 nm 2µm 280 nm Force resolution 1 nn/ Hz 24/68

23 Future directions: from micro to nano fab Combined MEMS/NEMS process flow: Integration of batch fabricated nanotips Device downscaling 30µm 10µm 10nm 100 nm gap 15µm 200nm f res =24.88 MHz Q = 850 V DC = 20 V Z mot = 260 kω 25/68

24 26/68 Fabrication I: nanogap

25 Fabrication II: nanotip

26 Fabrication: not yet perfect

27 Measurements 200 résonateurs / wafer Electrical (HP8753 Network Analyser) Optical (Polytech laser vibrometer) 4MHz, 12MHz, 25MHz et 50MHz 29/68

28 AFM set up

29 First AFM images: 4 MHz probe Lignes de 100nm en résine (PMMA) Image 1 : phase Image 2 : Z

30 2011 Latest results

31 Latest results + functionalization

32 3D process for AFM MEMS Probe Signal Input Nanometric capacitive gap fabricated by sacrificial technique Wet etched and batch-fabricated tip Signal output 34/68

33 AFM MEMS Probes Typical AFM MEMS IEMN Characteristic dimension 200µm 60µm Resonance frequency 300kHz 10MHz Quality factor (at atm. pressure) /68

34 HF Measurement Reflection coefficient of a wave reflected on a variable capacity Modulation at the MEMS operation frequency v i n Mixer RF IF OL Signal at the MEMS frequency V DC Coupling Variable capacity C+dC(x) C=~ fF RF source at ω 36/68

35 HF Measurement on a test resonator v i n 10µm HF Measurement HF Measurement on a test sample No coupling High S/N ratio V DC Pin = 10dBm V DC =5V IFBW=100Hz S/N=85dB 37/68

36 Towards AFM imaging 1 cm Resonator setup Device anchoring 1 mm Electric pads Metrology to obtain an overhanging tip 38/68

37 Calibration Purpose: Calibration of vibration amplitude Vibromètre Laser Plans <111> 54,7 x Image optique de la zone de mesure (d) 39/68

38 Calibration 54,7 40/68

39 AFM probe integration 41/68

40 Force resolution V AC +V DC Signal processing Measurement noise level: 7µV/ Hz Probe settings f 0 10,975MHz Q 1300 k e 180kN.m -1 HF measur ement Calibration: 5nm/V AC Scanner control Amplitude measurement resolution: 50fm/ Hz Force resolution: 5pN/ Hz 42/68 42

41 AFM images: 11MHz probe

42 AFM experiment: DNA origamis R ext 30 µm R int 10 µm th. 5 µm f MHz Q k eff 180 kn.m -1 Probe parameters f A 0 Scan size lin. Speed Time/frame MHz 0.2 nm 2 x 2 µm² 19 µm/s 55 s AFM images of DNA Origami on mica (real time) Sample: J.-M. Arbona, J.-P. Aimé, CBMN (Pessac) AFM parameters

43 DNA Origamis on Mica substrate Journée Trans GDR, 11 avril 2012 Besançon, 45/68 France

44 Height measurement Height

45 DNA Origami imaging: image capture

46 Conclusion: AFM experiment on DNA Origamis 1frame/second AFM imaging on DNA Origami No degradation of the bio-molecular structure Proof of concept paving the way for AFM MEMS Probe based of biological applications Z image Phase image Probe f 0 Q relax A min F min Cantilever 250 khz ms 1 pm.hz pn.hz -0.5 MEMS AFM 11 MHz µs 50 fm.hz pn.hz -0.5 Comparing the performance of AFM probes (at ambient pressure) Limitations: Cantilever: thermomechanical noise MEMS Probe: transduction efficiency + electronic noise

47 Y[µm] High frequency AFM: State of the art DNA origamis image done with a probe resonating at 18,4MHz nm 4 3 Settings 2 f 0 A 18,4MHz 0,1nm 1 Scan Size nb of lines x 5 µm² nm Lin Velocity 2µm/s X[µm] Samples: J.-M. Arbo, J.-P. Aimé, CBMN, Pessac 49/68

48 Conclusion - Outlook Amplitude noise <0.5pm/ Hz Phase noise <5m / Hz Force resolution < 10pN/ Hz Outlook High speed imaging is possible (video rate) Give access to real-time protein folding (origami) Piezoresistive sensing Piezoresistive actuation Journée Trans GDR, 11 avril 2012 Besançon, 50/68 France

49 Outlook Piezoresistive detection The piezo-resistances (areas in black) are placed at the zone where the maximal deformation of the same kind (compression or extension) could be attained while vibrating in the elliptic mode. Journée Trans GDR, 11 avril 2012 Besançon, 51/68 France

50 «During MEMS 12, we had» Piezo resistive resonator Piezo-resistance access Excitation access Piezo-resistance access

51 Acknowledgements Fundings SMART Improve-LM Jean-Pierre Aimé, Jean-Michel Arbona, CBMN, Pessac Univ. Bordeaux Permanent staff: E. Algré, M. Faucher, B. Legrand, D. Théron Ph.D. student: B. Walter, Z. Xiong IEMN Laboratory technical staff M. Ozinski, C. Legrand, C. Boyaval, D. Troadec, V. Brandli D. Vandermoere, B. Laurent, D. Ducatteau, E. Mairiaux, Y. Desmedts 53/68

52 54/68