In situ Characterizations of Thin-film Nanostructures with - - PowerPoint PPT Presentation

In situ Characterizations of Thin-film Nanostructures with Large-range Direct g g Force Sensing

Groupe MAP Manipuler Analyser et Manipuler, Analyser et Percevoir les échelles micro & nanoscopiques Gilgueng Hwang Juan Camilo Acosta Juan Camilo Acosta Stéphane Régnier

Large range high accurate force sensing (nN ~ µN)

Background Motivation

Objectives Establish piezoresistive helical nanobelt model considering initial stress Determine design parameters of large range helical nanobelt force sensor A h Investigating of high frequency piezoresistive helical nanobelt force sensor Determine design parameters of large range helical nanobelt force sensor Approaches High resolution force calibration with tunning fork wireless force sensing Force sensing of ultra-flexible nanostructures (graphene DNA) Modeling and design of piezoresistive helical nanobelt scrolling process

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Force sensing of ultra flexible nanostructures (graphene, DNA)

Potential Impacts on Flexible Nanostructures

Range: Range: g 0~1uN Resolution: Range: 0~6uN 30nN

• D. Golberg, Nano Lett. (2007),

V.7 p. 2146

• X. Bai, Nano Lett. (2007),

V.7 p. 632-637

• L. Zhang, APL (2008), V.92 p.

243102

Target Objectives Major Tasks Materials/ NEMS Mechanical characterizations

• f NWs NTs NBs and etc

Buckling, bending, kinking, electromechanical NEMS

• f NWs, NTs, NBs, and etc.

electromechanical measurements Biology DNA, protein, cell, fibre, tissues gecko foot hair and Pulling force measurement, molecular motor adhesion

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tissues, gecko foot hair, and etc. molecular motor, adhesion, Ab/Ag binding force

Related Works

AFM

• Cant. Array

CNTs Nanosprings y p g Sensors

S

Merits

• Resolution
• Sample prep.
• In-situ insp.
• Conformity
• Phase cont. po
• Multiple target

detection

• Compact
• Ultra high resolution
• Very compact
• No need for particular alignment
• Showed high

piezoresistance coefficient from this work

Smart sensor

p

• Not only imag.

Demerits

Lack of real-time response Monodirection

• Limit. to chem.

Biosensing

• Functionalization
• limit. of controlled fabrication
• limit of linear sensing region
• No force sensor yet
• Buckling

Coupled forces Tip-sample inter. Pervasivity Complex setup Small range difficulty

• Short life-time

4 Small range Laser scatt. Liq.

• Int. into nanorob.

I started from

Science Engineering Nanosystem

• Actuation:

Artificial Bacteria Self-scrolling principle Controlled fabrication

=

Artificial Bacteria flagella +

( ) ( )

υ ε + Δ + + + + + = 1 6 4 6 4

2 1 2 1 4 2 1 2 3 2 1 2 2 2 1 2 3 1 4 1 2 1

d d d d d E E d d d d d d d E E r

Sensing: Force sensors (Current Work) R t

Golod et al., APL 84, 3391, 2004 Grundmann et al., APL 83, 2444, 2003 d1, d2: layer thickness. E: Young modulus Δε: mismatch between bilayer. ν: Poisson’s ratio of the bilayer

Resonators Power sourcing: +

Cho et al., Science 313, 1634, 2006 Zhang et al., Nano Lett. 6, 1311, 2006 Bell et al., Nano Lett. 6, 725, 2006

g Nano inductors Resonators Not-controlled process! No device:

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p No known property, No assembly method

Development of Piezoresistive Helical Nanobelt Force Sensor

Schematic Sensing mechanism Force sensing

Sensor

Objectives Characterization of the piezoresistive helical nanobelts D i d bl f th t t i i ti h li l b lt f Design and assembly of the prototype piezoresistive helical nanobelts force sensor Apply to measure force using the developed force sensor Approaches Approaches In-situ SEM nanorobotic manipulation system with teleoperated multi robot configuration Multi-axial piezoresistivity characterization of helical nanobelt with metal connectors

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GILGUENG HWANG GILGUENG HWANG

Force calibration of piezoresistive helical nanobelt force sensor

Objectives and Approaches

MEMS process

InGaAs/GaAs nanobelt obtained by self- scrolling of a strained InGaAs layer Embed metal electrodes

• G. Hwang et al., Nano Lett., vol. 9, no. 2, pp. 554-561, 2009

In-situ Scanning Electron Microscope nanomanipulation Controller outside SEM Inside SEM chamber Nanomanipulation 10 um N p

3 D i l ti

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3-D nanomanipulation Nanometer accuracy

• G. Hwang et al., Int. J. of Optomecha., vol. 2, no. 2, pp. 88-103, 2008

Objectives and Approaches

In-situ SEM nanomanipulation In situ SEM nanomanipulation Nanorobotic assembly Force calibration Characterization

Prototyped helical nanobelt force sensor Giant piezoresistivity (249~890 x higher pie oresistance coefficient Field-assisted alignment Nano-Newton force piezoresistance coefficient than boron P+ Si piezoresistors)

• G. Hwang et al., Nano Lett., vol. 9, no. 2, pp.

554 561 2009

Nanosoldering

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554-561, 2009

Why Helical Nanobelts?

Intrinsic benefit of HNBs Intrinsic benefit of HNBs Wide linear range of sensing Ultra-flexible nanostructures High-resolution

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Parts Fabrications

HNB with metal connectors HNB with metal connectors Objective: Objective: assembly easiness assembly easiness Pipette electrode Pipette electrode Metal electrode Metal electrode Glass micropipette Glass micropipette

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Fabrication of Helical Nanobelts

MBE Deposition of

HNB with metal connectors HNB with metal connectors

GaAs Substrate MBE Deposition of GaAs/AlGaAs/InGaAs/GaAs Cr/Ni/Au Evaporation (a) (e)

Metal connectors

Positive Photolithography Lift-Off (b) (f) Wet Etch Release RIE (c) ( ) Negative Photolithography (g) (d)

Metal (f) Metal connecto rs

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In situ SEM Nanomanipulation System

Nanorobotic manipulators In situ characterization setup

Hwang et al., Intl. J. Optomech. 2, 2008

Nanoassembly Setup Sensing probe with manipulator

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Hwang et al., Proc. IEEE Nano. , 813-818, 2007

Longitudinal Piezoresistivity of Helical Nanobelt

HNB A

Soldered Keithley 6517A 1 2 3 10μm

Hwang et al., Nano Lett., 2009

I ΔL/L L/L 4 A 13 ΔL/L L/L

Longitudinal Piezoresistivity of Helical Nanobelt

R Elongated 27.5% HNB A Elongated 3.7% Compressed p A: 16% of I when 10% of L

Hysteresis due to changes in contact resistance

f f

contact resistance

~150 nN

R+ R+ΔR

The slope is constant increased Rcon

ΔL/L L/L

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Rcon

con

Rcon

con

Rcon

: Contact resistance

3 HNBs showed same behavior

Longitudinal Piezoresistivity of Helical Nanobelt

Further Analyses

Force Characterization Finite-element Simulation Helical Nanobelt in Resonance

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Comparison with Other Piezoresistors

Wide linear range of sensing, high-resolution

• Piezo. Coef.

Πl

ρ[E-10Pa-1]

Fabrication

Hwang et al., ACS Nano Lett., 9, 554, 2009

249~890X higher

l [

] Si Bulk

• 1.7~-9.4

MEMS comp. Bn-si

• 4

MEMS comp.

249~890X higher piezoresistance coefficient than boron doped P+ Si cantilever was found by this work

SiNW

• 3.5~-355

Self-assembly CNT

• 400

Self-assembly

f y

y HNB

• 399~-3560

Robotic assembly

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Assembly Overview

A: ES. Alignment A: ES. Alignment D: Mag. Alignment E: EBID B: Gold nanoink C: RSW A+(B,C): Repeat

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In situ SEM Gold Nanoink Soldering

Ex situ gold nanoink soldering In situ SEM gold nanoink soldering Wetting Wetting Wetting Wetting force force

Dockendorf et al., Appl. Phys. Lett. 2006

Hwang et al., IEEE Nano., 2007 18

Hwang et al., Appl. Phys. Lett. Submitted 2010 Dockendorf, Hwang et al., Appl. Phys. Lett. 2007

In situ SEM Gold Nanoink Soldering

Soldering Process & Stability test Conductivity Improvement Measurement of Axial Piezoresistivity of HNB Mechanically stabile up to 500 Mechanically stabile up to 500 nN nN

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Hwang et al., Appl. Phys. Lett. Submitted 2010

Hwang et al., IEEE Nano., 2007

Helical Nanobelt Force Sensor

Dong et al. Nano lett. pp. 58 Dong et al. Nano lett. pp. 58-

• 63, 2007

63, 2007 Regan et al. Nature, pp. 924 Regan et al. Nature, pp. 924-

• 927, 2004

927, 2004 Dong et al., APL, pp. 1919 Dong et al., APL, pp. 1919-

• 1921, 2002

1921, 2002 Tan et al., J. of Physics D, pp. 1998 Tan et al., J. of Physics D, pp. 1998-2008, 2004 2008, 2004 , J y , pp 998 , J y , pp 998 008, 00 008, 00 HNBs HNBs CNTs CNTs

20 20μm 20μm

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20μm 20μm 20μm

Force Sensor Calibration

ΔLafm

F

i F

F

i

ΔLafm

i

Resolution of SEM: 100 nm Resolution of SEM: 100 nm

ΔR(ε) F ε i(ε)

12 del R/R (%)

13.2 nN of force steps 13.2 nN of force steps Force range: 154 nN Force range: 154 nN

6 8 10 %] de / (%) 2 4 ΔR/R [%

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Force [nN] Hwang et al., IEEE Ind. Elec. Submitted 2010

Applications: Characterization of Tungsten Nanowire Mechanics

• Objectives
• Approaches

Mechanics

• Objectives

– To obtain the mechanical property of TNW for direction

• Approaches

– Use HNB to characterize the TNW`s mechanical control for applying to devices

• Motivation

Th d k property – Indirect calibration using home-made nanoprobe – The need to use as-known mechanical property nanostructures for wide range home made nanoprobe force sensing – The nanostructure should be as flexible as much flexible as much

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Takayama, Hwang et al., J. Prec. Eng. (2008)

Applications: Characterization of Tungsten Nanowire Mechanics Mechanics

Indirect Characterization of TNW kHNB=0.021 N/m Overview of TNW Characterization

TN W Probe

kprobe=0.406N/m

TNWs :7.5Gpa Young`s modulus

wire wire wire

I l k E 3

3

=

wire wire wire

I d Fl 2 = σ

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Rupture stress 18Gpa Brittle fracture

wire wire

I 3

wire

I 2

Applications: Characterization of Silicon Nanowire Mechanics Mechanics

1μm 1μm Nanowire Helical Nanobelt (a) (b) 2μm (c) μ ( )

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Enlarging Force Measurement Range Force

Upper region

Force

Lower region Calibrated region

Nanowire, Nanotube DNA, Protein Cell, Tissue

13.2 nN Upper region 154 nN Lower region Calibrated region pN uN 0 66 pN: min ideal F

L, D, P

L: length

L, D, P

0.66 pN: min ideal F

, , N, R , , N

D: Diameter P: Pitch N: # of turns R: Measurement resolution

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Larger Range Force Calibration

Helical Mechanical Properties Larger range but high Larger range but high resolution force sensor is resolution force sensor is necessary necessary Force characterization tools Nanostructures Larger range but high Larger range but high resolution force sensor is resolution force sensor is necessary necessary

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Assumption: Tunning forks can calibrate Helices? Assumption: Tunning forks can calibrate Helices?

Tuning Forks Force Measurement System

Schematic of Tuning Forks Overview of System Force Measurement Principle

f0

Helice TF

k k f f 2 = Δ

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Mechanical Characterization of Thin-film Nanostructures

3-D Helical nanobelt force sensor Dynamic piezoresistive helical nanobelt Piezoresistivity model Batch fabrication of force sensor Batch fabrication of force sensor Force calibration with CEA Saclay Collaborations with LPN/CNRS Single atomic layer force/position sensor Mechanical property Single atomic film NEMS Å layer Bandgap

R = 2.62 kΩ

Electrical property Tunning by stress Graphene nano electomechanical systems UPMC Internal Participations:

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p y with IMPMC Emergence

Optoelectronic Property Characterization of Graphene

Now from pyrex to TEM grid Electromechanical sensors Incorporating onto other substrate for NEMS Direct device writing

Useful to photovoltaic cell,

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IR gated bandgap tuning

Hwang et al., Filed in Patent 2009 Hwang et al., Int. S. Opto. 2009

Potential Control Applications

• Smart sensing mechanisms

– No external readout systems necessary – Closed loop feedback control

• Large range physical property sensing

P iti l ti f – Position, acceleration, force – Robust sensing

• Wireless sensing
• Wireless sensing

– Non-destructive material characterization – Wireless communication

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Summary of Talk

• Piezoresistive Helical Nanobelt Force Sensors

– Giant piezoresistivity, large range visual detection – Applications: Mechanical characterizations of tungsten/silicon nanowires

• Tuning Fork Force Sensor
• Tuning Fork Force Sensor

– Frequency shift, large range (pN – uN) force sensing – Dynamic force sensing y g

• Property Characterizations of Thin-film Nanostructures

– Graphene, membrane mechanics

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