Atomic Force Microscopy (AFM)

1
 Outline

 History of Atomic Force Microscopy (AFM)

 Instrumentation
 Static force-distance curves and force
spectroscopy
 Dynamic AFM and force gradient spectroscopy
 Imaging
 Applications and emerging areas

3
 The starting point- STM
F. Giessibl’s
Rev. Mod. Phys.

 Binnig, Gerber, Rohrer, Wiebel (1982)

 Binnig and Rohrer awarded Nobel Prize in Physics in 1986 for STM
 If |Vt| is small compared to workfunction  , and tunneling current is given
by I t (z)  I 0e 2 t z where z is the gap I0 is a function of the applied voltage
and the density of states in the tip and the sample, and t  2m / 
 For most metals, ˜ 4eV, so that t=1Å-1
 Most current carried by “front atom”blunt tips , so atomic resolution possible
even with relatively blunt tips
 Only electrically conductive samples, restricting its principal use to metals
and semi-conductors

4
 The AFM
G. Binnig, C. F. Quate and Ch. Gerber, PRL 56, 930 (1986)

 Binnig invented the AFM in 1986, and while Binnig and Gerber were on a
Sabbatical in IBM Almaden they collaborated with Cal Quate (Stanford) to
produce the first working prototype in 1986
5
 Early AFM Images
G. Binnig, C. F. Quate and Ch. Gerber, PRL 56, 930 (1986)

6
 Outline

 History of Atomic Force Microscopy (AFM)

 Instrumentation
 Static force-distance curves and force
spectroscopy
 Dynamic AFM and force gradient spectroscopy
 Imaging
 Applications and emerging areas

7
 The microcantilever – the force sensor

Cantilevers can be coated with ‘Cr’ to magnetically excite the sample.

It can also be coated with a fluorescent material to optically excite the
specimen,
8
 Detecting deflection

 STM tip
 Capacitance/laser interferometry
Bending of optical cantilever is
measured by deflection of beam.
 Beam deflection
Bending of optical cantilever is measured
by deflection of beam. The signal is
amplified to improve signal/noise ratio.
9
 The beam deflection method
Photodiode

Laser
Cantilever may
twist due to any
reason, e.g,
atomic/molecular
frictional forces,
so tip moves left
or right.

a) Normal force b)Lateral Force

Up A+B= UP left A+C= LEFT

Down C+D=DOWN Right B+D=Right

10
 AFM Block Diagram
Personal Computer

detector
Signal

z dither piezo SPM Signals

SPM tip

x SFM 3 dimensional image of a

tumor cell HeLa (37x37m2 )
y
z
Piezoelectric
scanner HV Amplifiers and
signal conditioning

Digital
Processor
Signal
11
 Outline

 History of Atomic Force Microscopy (AFM)

 Instrumentation
 Static force-distance curves and force
spectroscopy
 Dynamic AFM and force gradient spectroscopy
 Imaging
 Applications and emerging areas

12
Tip-sample interaction forces in AFM
 Long-range electrostatic and magnetic
forces (upto 100 nm)

Nanosensors Gmbh
 Capillary forces (few nm)
If there are water molecules on the surface
in ambient conditions, the molecules
aggregate forming a neck on the surface.
 Van der Waals forces (few nm) that are
fundamentally quantum mechanical
(electrodynamic) in nature
 Casimir forces
 Short-range chemical forces (fraction of
nm)
Tip-sample  Contact forces
interaction force  Electrostastic double-layer forces (Liquids)
Tip-sample gap
 Solvation forces
Attractive  Nonconservative forces (Dürig (2003)) 13
Repulsive
 Force-displacement curves
k
 
F(d)=k
d Z
F(d) Equilibrium Condition
to Hold.
F(d) Inaccessible region
k

 Snap-in
k
d Z
2
3 2 4’ 1 1
3 4’
2’

2’
4 Z 4
Pull-off
WAdhesion=blue shaded area WCantilever=shaded area above
15
above
 k Force spectroscopy

III II I
Z

 Three distinct regions

 If k is known then from the static-force distance curve, F(d)
can be calculated for all d except for inaccesible range near
snap-in
 It can be shown that WCantilever is related to the WAdhesion
 Slope in III is good measure of repulsive forces (local elasticity)
16
 Outline

 History of Atomic Force Microscopy (AFM)

 Instrumentation
 Static force-distance curves and force
spectroscopy
 Dynamic AFM and force gradient spectroscopy
 Imaging
 Applications and emerging areas

17
 Dynamic AFM
 Cantilever driven near resonance
 Non-contact AFM, Tapping mode AFM, Amplitude
Modulated AFM, Frequency Modulated AFM are all
dynamic AFM
 The cantilever's resonant frequency, phase and
amplitude are affected by short-scale force gradients

18
Dynamic AFM & force gradient spectroscopy
 Variation of amplitude,
resonance frequency, and
phase measured as Z is
decreased
 From this it is possible to
reproduce the Force gradients
between the tip and the sample
 Even non-conservative
interactions can be resolved
 Offers many advantages over
static-force distance curve
based force spectroscopy
 Quantitative information is hard
to come by because the forces
are nonlinear

19
 Outline

 History of Atomic Force Microscopy (AFM)

 Instrumentation
 Static force-distance curves and force
spectroscopy
 Dynamic AFM and force gradient spectroscopy
 Imaging
 Applications and emerging areas

20
 Contact Mode Imaging

y
x

s
s

First tip contacts surface with some setpoint normal force which is kept 21
constant during the scan. For biological samples, keep Normal force smaller.
 Tapping Mode

Surface
interaction

In Tapping mode the tip is oscillated at the resonance frequency and the
amplitude of oscillation is kept constant; any change in amplitude is 22
translated into force and topography.
 Phase Imaging

AFM height (left) and phase (right) images

of poly(methylmethacrylate)

 Regular tapping mode implemented but signal phase monitored

 Phase contrasts are related to differences in local dissipation
 Phase changes in constant amplitude mode tells about dissipation b/w
tip & the sample (for example, visco-elasticity), used for Polymers.

23
 Outline

 History of Atomic Force Microscopy (AFM)

 Instrumentation
 Static force-distance curves and force
spectroscopy
 Dynamic AFM and force gradient spectroscopy
 Imaging
 Applications and emerging areas

24
 Carbon nanotube tips (CNT)

1

Dynamic AFM images of a 100 nm trench

on Si using conventional silicon probe
(left) and a MWCNT probe (right)
 Provide high resolution
 Show little evidence of wear
 Promising technology for critical dimension metrology of
semiconductors, and nanobiological investigations
 Buckling, friction and stiction of CNT become important
25
 CNT tips – tapping mode 120

100 Z gap decrease

Straight MWCNT

Tip amplitude (a.u.)

80

60

40

20
Buckling signature

0
71.5 72 72.5 73 73.5
Excitation f requency (kHz)

CNT attached strongly to buckle and then flex which should be avoided
The Lorentzian resonance curve starts stretching
Straight MWCNT, diameter 10 nm, length 7.5m, Frequency 72.5 kHz
 Repulsive and attractive states do not appear to co-exist for long
CNT tips

26
 Static force-distance curves
D
C E
H F
G
High Adhesion

A I
B
J
Displacement towards sample (nm)

A B C D E

J I H
 CNT buckles, slips, and slides
 High adhesion on the CNT sidewalls 27
 Shorter CNT tips- noncontact mode
 Ringing artifacts associated with CNT adhesion and stiction to sidewalls
300 nm Tungsten nanorods

28
Application to local adhesion estimation: Anharmonicity
3500 nm x 3500 nm scans

Topography Second harmonic ima Seventh harmonic imag

ge e
proteins Lipid deposits
 Clear distinction between lipids and proteins
 Presence of internal resonance critical in the method
 The method shows promise for the measurement of
local attractive forces of soft biomolecules
 Can be extended to electrostatic force microscopy or
capacitance microscopy for dopant profiling
In biology, a lipid is a substance of biological origin that is soluble in nonpolar 30
solvents.