FIRAT: A fast and sensitive probe

structure for SPM

F. Levent Degertekin
G.W. Woodruff School of Mechanical
Engineering
Georgia Institute of Technology

Funding sources: NSF and NIH

 Outline
ƒ Force sensing Integrated Readout and Active Tip (FIRAT)
probe structure
ƒ Device fabrication and integration to commercial AFM
system
ƒ Fast imaging with FIRAT
ƒ Experimental setup and initial results
ƒ Quantitative surface characterization with FIRAT
ƒ Time resolved interaction force (TRIF) mode operation
ƒ FIRAT structures with improved dynamics and sensitivity
ƒ Application to biomolecular measurements
ƒ Conclusion and future work
 Some Limitations of AFM
PHOTODETECTOR
ƒ Imaging Speed LASER
ƒ Bulky piezoactuators are slow X, Y
ƒ Integrated piezo or magnetic
actuators can be complex Z PIEZOTUBE

ƒ Material characterization CANTILEVER

ƒ Slope detection leads to tip

rotation
ƒ Point force measurements are
somewhat slow for simultaneous Vibration spectrum of an AFM cantilever
topography imaging
ƒ High Q of cantilever masks tip-
sample interaction forces during
tapping mode imaging
ƒ Array implementation
ƒ Parallel biomolecular
measurements
ƒ Parallel imaging, nanofabrication
 FIRAT Probe Structure
ƒ New AFM probe structure: Sharp tip on micromachined membrane/beam
ƒ Integrated optical interferometer for tip displacement detection
ƒ Phase sensitive grating
ƒ Low-noise, robust interferometer
ƒ Integrated electrostatic actuator for fast tip actuation
ƒ Imaging speed limited by membrane dynamics (fo ~ up to 10MHz)
ƒ Force sensing Integrated Readout and Active Tip Æ FIRAT

Integrated Electrostatic
actuator input

Quartz substrate

Micromachined membrane
and diffraction grating
(bottom electrode)
1st diffraction
order incident
beam

Photodetector Reflected
diffraction orders

Tip displacement
signal
 Diffraction Based Optical Displacement Detection
reflector

d =λ/2 d =λ/4
ƒ Non-moving diffraction
grating on transparent dg substrate
substrate
ƒ Backside illumination:
Reflected diffraction reflection diffraction
pattern Gaussian aperture w0=9µm, λ=850nm, 2µm grating period
ƒ Reflector displacement 50

changes the intensity of 0

h = λ/2
diffraction orders - 50
- 200 - 100 0 100 200

ƒ Photodetectors at fixed y (μm)

50

locations are used to

0
h = λ/4
detect intensity variations - 50

50
- 200 - 100 0 100 200

ƒ Interferometric sensitivity 0

achieved in a small h = λ/8

- 50

volume - 200 - 100 0

x (μm)
100 200

Normalized intensity

0 0.5 1
 Displacement Sensitivity
ƒ Reflection order intensities
1
I0 α cos2(2πd/λ), I1 α sin2(2πd/λ) I0
I1
Output for small deflections Δx + d0 0.8

For d0=nλ/8 (n odd)

Normalized intensity
0.6

∂ (I 0 − αI1 ) 4π
i=R Δx = RI in Δx 0.4
∂d 0 λ0
0.2

• Shot noise limit Î MDD: √ qIR/(4 π IR/λ)

• 1.35x10-4Å/√Hz with 61µW laser power is 0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7
demonstrated Gap thickness (d) (μ m)

¾ Sensitivity depends periodically on the gap

¾ Several diffraction orders can be detected to reduce laser intensity noise
¾ Electrostatic actuation is used to optimize sensitivity
¾ Several methods have been devised to address range limitation
 Device Fabrication
Surface Micromachining On Quartz Substrate
Devices for use in air: Membrane array (100µm diam.)

ƒ Aluminum membrane (0.8-1µm thick)

ƒ Aluminum grating (0.15µm)
ƒ PR sacrificial layer (1.5µm)

Quartz

PECVD
oxide

Photoresist

Aluminum Back side

Originally developed as microphone arrays

 Device Fabrication - Tips
ƒ Focused Ion Beam assisted deposition on membranes
ƒ Platinum and Tungsten tips with 50-70nm tip radius
ƒ Image resolution, attractive force levels depend on tip geometry
ƒ Batch fabrication of silicon devices seems feasible
ƒ Cantilever processes with few extra steps are needed
ƒ Silicon and diamond tip integration is underway

Platinum Tip On Aluminum Membrane Tungsten Tip On Nitride Membrane

10µm
 Device Fabrication – FIRAT chips
ƒ Quartz chips mechanically cut using dicing Wafer edge

saw
ƒ Fully cut for operation in air
ƒ Halfway cut for fluid cell
Electrodes
ƒ Alignment limits the sample geometry
FIRAT chip with Al m./ Pt tip Immersion chip with dielectric m./ W tip

Etch hole to
be sealed

100µm
 Adaptation to Commercial AFM
FIRAT vs. Veeco (commercial) Cantilever holder

ƒ Laser stereo lithography is used to

fabricate the holder with specific
angle to use the 11º standard optics
ƒ FIRAT chip oriented to use first
diffraction order on the
photodetectors
ƒ Nearly plug-and-play with the Veeco
Dimension system with minimal Imaging head with FIRAT on AFM
additional electronics
ƒ Readily adaptable to other
commercial systems
 Experimental Setup
ƒ Used Dimension AFM with Control loop for imaging
custom holder and added material properties
electronics Laser
ƒ Integrated electrostatic actuator Z-input diode
Controller
of FIRAT used as the only Z Control + 2kHz
actuator for fast tapping mode tapping signal Piezo tube:
x-y scan for fast
imaging (lower loop) with RMS RMS imaging,
detector
detector BW ~12kHz A x-y scan & Z motion
for elasticity
ƒ Direct interaction force imaging PD
imaging
(upper loop) for topography and +1st order

material properties with Fast RMS FIRAT probe

detector & holder
Dimension’s RMS detector and
controller
Sample
ƒ Digitizing interaction force signal Controller
Control + 600kHz 10nm
at PD output (A) while using tapping signal

upper loop Control loop for fast tapping mode

ƒ FIRAT actuator is also used as imaging with integrated electrostatic
actuator
equivalent of tapping piezo
 Fast Tapping Mode Imaging With FIRAT
16 x 512 pixel images
1Hz
X-Y scan by piezo tube
5Hz
control oscillation
20Hz

Z motion by 60 Hz
Active Tip

ƒ FIRAT probe used with FIRAT line scans Cantilever line scans
120
commercial AFM system
120

1 Hz 100 1 Hz
ƒ FIRAT tapping frequency 100

600kHz 80
80
5 Hz
Surface height (nm)

Surface height (nm)

5 Hz
ƒ Sample: 20nm high 60
60
20 Hz
calibration grating 20 Hz
40
40
ƒ 60Hz scan rate – limited by 20
60 Hz
X-Y scanner 20
60 Hz 0

ƒ Surface topography limited 0 -20

by interference curve -20 -40

0 0.5 1 1.5 2 2.5 3 3.5 4
0 0.5 1 1.5 2 2.5 3 3.5 4
Lateral position (μ m) Lateral position (μ m)
 Direct Measurement of Interaction Forces
ƒ FIRAT Substrate oscillated, tip displacement recorded
ƒ No tip-sample interaction Î No signal Î Zero background
ƒ Transient signals recorded with high bandwidth of the membrane
ƒ Every tap provides a dynamic force curve
4 Control loop for imaging
material properties
3.5 I V
Laser
Z-input diode
3 Controller
Control + 2kHz
II IV tapping signal
2.5
Piezo tube:
RMS x-y scan & Z motion
Displacement (a.u.)

detector for material property

2
PD
imaging
III
1.5 +1st order

FIRAT probe
1 & holder
I II III IV V
Z- Piezo disp.
0.5 (FIRAT substrate) Electrostatic Sample
actuation port
0

-0.5 Tip displacement

Jump to contact (Photodetector output)
-1
0 50 100 150 200 250 300 350 400 450 500
Time (μs)
 Simultaneous Topography and
Time Resolved Interaction Force (TRIF®) Measurement
2.5nm thick Pt GT logo on silicon Control loop for imaging
Topography material properties

Laser
Z-input diode
Controller
Control + 2kHz
tapping signal
True constant Piezo tube:
RMS x-y scan & Z motion
force tapping detector for material property
PD
imaging
mode imaging
TRIF signal +1st order

FIRAT probe
& holder

Electrostatic Sample
actuation port
Individual tap (TRIF) signals
150

100
• Slope: Stiffness
• Tap shape inversion: Elasticity
Interaction force (nN)

50
• Attractive peaks: Adhesion, capillary
0 hysteresis
• Background: Long range forces
-5 0
• Contact time
-1 0 0

-1 5 0
0 0 .5 1 1 .5
T im e (m s )
 Quantitative Characterization TRIF™ Signals
ƒ Contact mechanics and adhesion hysteresis models are used to fit the
digitized tap signals
ƒ Tip remains normal to the sample during interaction
ƒ Fast nanoindenter with high resolution imaging capability

Simulated vs. measured signals on PR and Si Measured signals on polymers samples and Si
100
150
Si-experiment silicon
Si-simulation 0
100 PR-experiment
PR-simulation -100

stiff polymer
Interaction force (nN)

Interaction force (nN)

50
-200

0
-300

-400
soft polymer
-50

-500

-100
-600

-150 -700
0.68 0.7 0.72 0.74 0.76 0.78 0.8 0.82 150 200 250 300 350 400 450 500 550 600 650
Time (ms) Time (us)

• Polymer samples courtesy of Prof. Ken Gall (GaTech MSE)

Extracting Silicon properties
Extracting PEGDMA properties
 Mapping a feature of TRIF

ƒ Material property imaging

Si substrate
independent of topography Al (140nm) / Si substrate

ƒ Adhesion force peak is used Al (140nm) / Cr (150nm) / Si

as imaging parameter Cr (150nm) / Si substrate

Cr

Topography Peak attractive force

Al

Al Cr
Al Cr
Al Si Al Si
 Mapping properties of CNT over Si
TEM image

• Internal details seen in

the TEM image of a CNT is
1.5 um

observed in stiffness map

Adhesion energy (mJ/m2) Stiffness (N/m) Contact time (%)

• CNT samples courtesy of Prof. Sam Graham (GaTech ME)

 Modeling of Device Dynamics
ƒ The membrane results in
complicated frequency response
Î not ideal for AFM applications
(Because it is a microphone!!)
ƒ Finite element method is used to
model squeeze film stiffening and
damping effects for the complex
membrane structure with vent
1

0.9

holes 0.8

ƒ Simple linear model also

Normalized Amplitude
0.7

0.6

accurately predicts the device 0.5

behavior 0.4

0.3

ƒ Using validated model, 0.2

Experimental

structures with desired 0.1 Linear model fit

ANSYS simulation
0
characteristics can be designed 10
1
10
2
10
3
10
4

Frequency (Hz)
5
10
6
10
7
10
 Other FIRAT Structures
ƒ Cantilever, clamped-clamped
beams can be more suitable for
different applications TRANSPARENT
SUBSTRATE
ƒ The electrodes can be driven to
provide tip motion in 3-D Electrostatic
actuation port

ƒ Interplay between device spring Cantilever

(Silicon nitride
etc.)

constant, stiffness of air in the gap

and damping determines the
frequency response
ƒ Ideal device:
ƒ Flat response until resonance
frequency (f0 ~ 1MHz)
ƒ Reasonable Q (loss) for low
thermal noise limited force
resolution
ƒ Reasonable Q (4-20) for fast
settling time
 Clamped-beam (Bridge) Devices
ƒ Aluminum bridge devices: 60µm long 20µm or 40µm wide, 0.8µm
thick. Air gap thickness 2.5µm
ƒ Targeted Q values 4-15, spring constants in the 10-40N/m range,
resonance frequency ~ 1MHz to result in 100kHz imaging
bandwidth
ƒ Also fabricated devices with 7µm gap for large actuation range
Top view of a bridge device
 Measured Response for Fast Imaging FIRAT
ƒ Simple model predicts device response
ƒ Ideal response for fast tapping mode imaging – flat below resonance
ƒ Thermal noise less than 1nN over 1MHz bandwidth

Calculated response Optically measured response

20 20
60μm x 20μm Bridge simulated 60 μ m x 20 μ m measured
18 60μm x 40μm Bridge simulated 18 60 μ m x 40 μ m measured

16 16

Normalized response
Normalized amplitude

14 14

12 12

10 10

8 8

6 6

4 4

2 2

0 0
3 4 5 6 7
3 4 5 6 7
10 10 10 10 10 10 10 10 10 10
Frequency (Hz) Frequency (Hz)
 Bridge Device with FIB Tip

ƒ Platinum tip built on 60µmx40µm, 0.8µm thick

aluminum beam
ƒ Gap thickness 4.5µm, k ~ 40N/m, Q~ 4-5
 FIRAT for Material Characterization

ƒ Broadband, damped response for clean tap signals

ƒ Device geometry and gap adjusted for desired response

Measured and simulated response of 150μm x 40 μm bridge

5
Measured response
Measured tap signals Simulated response

150 0

Normalized response (dB)

100
-5
Interaction force (nN)

50

0
-10

-50
-15
-100

-150 -20
3 4 5 6
0 0.5 1 1.5 10 10 10 10
Time (ms) Frequency (Hz)
 Structures for Enhanced Sensitivity
ƒ The membrane substrate gap Membrane
(metal+dielectric mirror)
can be converted to a Fabry- Dielectric
mirror
Perot cavity Grating fingers
(metal)

ƒ Reflective part of membrane is

made of alternating stack of
silicon oxide-silicon nitride
quarter wave layers
ƒ With 5-6 pairs slope increases number of dielectric
stack increases
by 10x, shot noise remains the (2,4,6,8)

same Î displacement
sensitivity in the 10-5Å/√Hz
levels with 60μW laser power
ƒ Low dynamic range, but very
high transient tap force
sensitivity
 Experimental Verification of Enhanced Sensitivity

ƒ Fabricated device with 5.5 pairs of

dielectric layers Measured Finesse factor of 10-14
ƒ Four-arm structure Î 3-D forces 0.4
(b) Retracting

Output voltage (V)

ƒ Spring constant can be adjusted by 0.3

arm dimension 0.2

0.1

0.0
Membrane displacement Δx2 (100nm/div.)
Calculated Finesse factor of ~40
0.3

Normalized Intensity
0.2

0.1

0.0
Membrane displacement Δx2(0.25λo/div.)
 Parallel Force Spectroscopy
Not individually actuated Î No force control
ƒ Most parallel molecular force
spectroscopy measurements require
individually controlled force probes
ƒ Individually actuated cantilevers can
be complex to build, can limit the type
of cantilever to be used Individual actuator on cantilever ÎComplex structures

FIRAT based solutions

ƒ Functionalized, elecrostatically
actuated membranes conform to
cantilever array, force measurement
is performed by moving membranes “Locally actuated sample surface”
ƒ Accurate, parallel detection of
membrane displacement with
integrated detector Î accurate
control of force and molecule
extension Transparent
substrate
 Immersion Device Fabrication
Deposit and pattern
Transparent substrate the diffraction grating
20/80 nm Ti/Au
Top view

Spin and pattern the

polymer sacrifical layer
~3 μm of film

Bottom
Deposit and pattern view
The bottom insulator: 0.1 µm SiN/SiO2
The top electrode: 5/80 nm Ti/Au
The top insulator: 1.5 µm SiN/SiO2

Array with separate actuation electrodes:

Decompose polymer layer at

440 °C

Fabricated both nitride and soft parylene membranes:

Spring constant ranging 20-1000N/m
 AFM-FIRAT Combination
ƒ An experimental tool for single molecular force measurements
ƒ Allows for comparison of both methods, calibration of membrane
spring constants etc.

Conventional Motorized
AFM head vertical position
control for AFM
head
10x optical
camera FIRAT ,
regular AFM
PD array cantilever

Laser
Position
adjustment
knobs
 FIRAT Based Devices – Initial Results
ƒ Integrated electrostatic actuator moves the membrane in vertical direction
ƒ Integrated optical interferometer measures displacement with high
resolution
ƒ Nitride and parylene membranes have been coated with PEI cushion and
functionalized with desired proteins
ƒ Electrical isolation ensures proper operation in buffer solutions
AFM Molecular system used in experiments
cant
ile ver

Diffracted beam

Collaborator: Prof. Cheng Zhu (BME/ME)

Incident laser beam
 Experiment with Piezo Actuation
ƒ Membrane is passive sample
substrate Piezo 0.01 N/m
ƒ Commercial AFM piezo is used to Drive: ON AFM Cantilever
move the cantilever for
conventional molecular pulling
ƒ Adhesion-rupture events
recorded
600 800
extend extend
400 retract 600 retract
400
force [pN]

force [pN]
200
200
0
0
-200 -200
Bond rupture
multiple ruptures
-400 -400
0 0.1 0.2 0.3 0.4 0 0.2 0.4 0.6
time [s] time [s]
 Experiment with Membrane Actuation
Piezo
ƒ Piezo driver turned OFF (very small motion)
Drive: OFF
ƒ The membrane is driven with 5Hz triangular
signal to provide tip contact

Continuous tip contact Î tip V

follows periodic membrane
motion with some piezo drift

Force measured by the cantilever (+ve tip pushed up, -ve tip pulled down)

No adhesion No adhesion
Adhesion/ rupture Adhesion/Rupture
 Array of Membrane Sensors
ƒ If membrane is soft enough it can be used for both force sensing
and tip actuation Î Cantilever is eliminated
ƒ High force sensitivity along with soft mechanical structure:
10 fm/√Hz * 1N/m Î 3pN with 1Hz-100kHz BW (need to
check thermal noise)
 Microactuators for Fast Imaging in Liquids
Imaging probe: AFM
cantilever

ƒ Compatible with existing AFMs Sample

ƒ FIRAT membrane is used as Electrostatic

actuation port
active sample holder Substrate: Transparent or

ƒ Devices with > 100kHz BW silicon

have been fabricated and

X-Y scan by separate
actuator

tested
Optically measured frequency response in liquid
ƒ Fast Z-motion provided by the 2500

FIRAT membrane
2000
ƒ Built-in displacement detector
for closed loop operation
PD Out [mVpp]

1500

ƒ Suitable for molecular imaging 1000

in fluids
500

0
10 100 1000 10000 100000 1000000 10000000
Frequency [Hz]
 Conclusion
ƒ A new type of AFM probe tip has been A fully integrated FIRAT probe
developed
ƒ Integrates electrostatic actuation with
interferometric detection in a compact
manner
ƒ Suitable for fast topographic imaging
ƒ Provides sensitive broadband frequency
response for direct measurement of time
resolved interaction forces PD integrated 9x9 membrane array
ƒ Tip motion normal to the sample simplifies MembraneSensor array
quantitative analysis similar to
nanoindentation
ƒ Operation in fluids and application to force
spectroscopy has been demonstrated
ƒ Structure is suitable for miniaturization
and array implementation

1cm
 Challenges & Future Work

ƒ FIRAT structures with integrated sharp tips

ƒ More complex than cantilevers
ƒ Silicon tips are feasible, cost can be an issue
ƒ Robust devices for in liquid operation
ƒ Future work:
ƒ Fast imaging: Improved range and robustness
ƒ Parallel molecular force spectroscopy
ƒ Silicon tip fabrication
ƒ Unique probe structures for specific applications
ƒ Other detection schemes, such as capacitive detection
ƒ ….
 Acknowledgments

ƒ Graduate students and postdocs: Guclu Onaran,

Hamdi Torun, Dr. Mujdat Balantekin, Dr. Krishna
Sarangapani, Wook Lee, Byron Van Gorp, Dr. Jemmy
Sutanto, Dr. Will Hughes (MSE), Brent Buchine (MSE),
Rasim Guldiken, Zehra Parlak
ƒ Prof. Calvin F. Quate (Stanford University)
ƒ Prof. Cheng Zhu
ƒ Prof. Z.L. Wang, Dr. Paul Joseph
ƒ FIB facility, MiRC