Unit for nanoscience and Theme Unit of

Excellence in Nanodevices
S.N. Bose National Centre for Basic Sciences
Kolkata-700098
www.bose.res.in

Basics of Scanning probe microscopy

A.K. Raychaudhuri

SNBNCBS and Bruker School
December 14-15, 2011
Basic concepts
Simple components of SPM
Cantilever Statics and Dynamics
The different modes of SPM
I will assume:
You have used SPM in some form before and
have some acquaintance with it.
However, the talk is not for experts.
SPM
The Scanning Probe Microscope
What are the basic components of a SPM
Localized Probe
that has an
interactionwith
the substrate to
be imaged
A nano-positioning
mechanism that can
position the probe in
close proximity
of the surface
A system to
measure the
interaction of the
probe with the
substrate
A mechanism to
scan the probe
relative to the
substrate and
measure the
interaction as
function of position
STM- Quantum mechanical tunneling between a
tip and the substrate. The contrast comes from
spatial variation of local electronic desnsity of
states.
AFM- Localized mechanical (attraction or
repulsion) interaction between tip and surface.

Physical mechanism and contrast
Any microscopy will depend on some physical
mechanism to create a contrast spatially.
It will also need a way to measure the contrast
with spatial resolution.
If the process of scanning does not measure the
contrast that has a spatial dependence you will not
get any image in any scanning microscope.

Being a computer operated system, any periodic
noise in the system can create images because the
scanning process can add it up to the main signal.
These are plain artifacts.
How to detect artifacts ? A quick thumb rule
In contrast to TEM or Optical microscope there is
no diffraction and reconstruction of diffracted wave
front in SPM.
Advantage:
Resolution is not diffraction limited.
Here the limitation comes from the tip size that
interrogates and of course some fundamental
limitations on detection process and electronics.
Different SPMs and different modes
The nature of the tip surface interaction gives
different types of microscopy.

The way we detect the response gives us the
different modes of SPM.
SPM
The Scanning Probe Microscope (SPM) family
STM (Tunneling)
SFM (Force)
Scanning Thermal
Microscope (Local
Temperature)
STS,STP,Scanning
Electrochemical
Microscope
Scanning Near Field
Optical Microscope
(Optical imaging)
Atomic Force
Microscope (AFM)
Lateral Force (LFM)
Magnetic Force
(MFM)
Electrostatic Force
(EFM)
C-AFM
Scanning Force Microscope
It is nothing but a spring balance (the cantilever)
that is scanned over a surface.
The cantilever is the precision force detection
element- we can detect atomic forces
Type of force of interaction between the tip and
substrate will determine what we are measuring and
the mechanism that makes the contrast.
How large are the atomic forces and can we really
detect them by a cantilever that is much larger?
How big is the Atomic Force
The atomic spring constant
What is the value of the spring
constant of the bond connecting to
atoms ?
e
2
k
eff
/M
e- Is typically in IR range for atomic vibration
e ~ 10
13
- 10
14
cps, M ~ 5 x 10
-26
Kg,
k
eff
= e
2
M ~5 x (1-10
2
) N/m
3
3
Et w
k =
4L
1 k
f =
2 m*
One can make a cantilever as a force measuring element
that can have the same order of k as that of a molecule.
w
L
L

Si elastic modulus (E)
[111] Young's modulus= 185GPa
[110] Young's modulus=170 GPa
[100] Young's modulus= 130 Gpa
Si
3
N
4

~300 Gpa
For a Si cantilever :
t = 5m, w= 20 m, L= 200 m
k=10N/m
It can be softer than atomic
spring constant
L
2

b
w
L
1
t: thickness
m*~0.24(mass of the cantilever)
3 3 3
3
1 2 2
Et wb
k =
2b(L -L ) + 6wL
Engineering cantilevers with different spring
constant k- need for different applications
Advantages:
1.Less prone to vibrational
noise.
2. Can go to lower k or
resonance frequency.
Estimated radius of curvature of the tip R
t
~ 30 nm
K
c
=0.1 N/m
Tip
Engineering cantilevers with different spring
constant k-a real triangular cantilever
Much softer than an
atomic spring !!!!
Cantilever
What ever you do with SFM,
the cantilever is the key.
You need to know it.
Some feeling for numbers
We have a cantilever as a force measuring element.
F = k.

If I want to measure F=1nN, k=1N/m. I should be
able to measure a displacement =1 nm.
Entering the world of nano
At the heart of all scanning probe microscope is the
cantilever with a tip.

How we position the tip?
How we scan the tip?
How we measure deflection of the cantilever?
Demystifying AFM-A simple AFM (Home made)
Laser
QPD
Inertial drive piezo
Scan Piezo
Electronics
L. K. Brar, Mandar Pranjape,
Ayan Guha and
A.K.Raychaudhuri
Design and development of
the scanning force
microscope for imaging and
force measurement with
sub-nanonewton
resolution
Current Science , 83,
1199 (2002)
X-Y micrometer stage
Schematic of SFM
DEFLECTION
SENSOR
FEEDBACK
LOOP
CANTILEVER
Z-PIEZO
PROBE
TIP
COMPUTER
XY-PIEZO SCANNER
Keeps cantilever
deflection or oscillation
amplitude constant
Practical Considerations for AFM/SFM
1. Cantilever deflection detection system.
2. Type of cantilevers that can be used.
3. Coarse and fine approach mechanism.
4. No net relative motion between sample, cantilever and
detection system.
5. Scanner range and type of encoder for large size
scanner.
6. Data acquisition system ,processing and display
software.
7. Accessibility to all the parts of the SFM and capability of
using image processing software on stored data.

Where do the SPM sold by different vendors
differ?
Scanner
Feedback
A-B
Pre-Amplifier
A B
Quadrant
Photo Detector
Tip &
Cantilever
Basic schematic for SPM
To Z-Piezo
Laser
ADC
DAC
Need for
calibration
Keeping something
constant, need for feed back
X-Y scanner
Z-scanner
Coarse approach vs fine approach
Pixels
bits
PID
Calibration of scanning stage of SFM using commercial
2-D grating
The grating has 2160 lines/mm
1000m/2160=0.46m
The calibration: 40nm/V
Brar et.al
(2002)
Topography
Can take care of
image distortion
Arranging spheres of PS in an array by self-assembly
Sub 500nm level calibration, works fine to 20nm
Can find the size by Electron microscope or DLS
Soma Das
(2008)
Mica
Freshly cleaved
7 nm x 7 nm
Calibration in atomic range-
A freshly cleaved surface
Can we assume a linear calibration ?
The piezo -scanner is non-linear and
has hysteresis
Other calibrations:
Z-Calibration- large scale vs small scale
Force calibration-detection of exact k?
Optical head and Detection electronics for scanning
Scanner
Feedback
A-B
Pre-Amplifier
A B
Quadrant
Photo Detector
Tip &
Cantilever
To Z-Piezo
Laser
ADC
DAC

Optical lever =

= 500 -100(for l=100mm)
L(Length of the laser path)
l(Length of the cantilever)
| |
|
\ .
Main components of the optical
stage:
1. Laser diode
2. Cantilever
3. Quadrant photo-detector (QPD)
4. Collimating lenses
5. Mirror
QPD is used as a position
sensitive detector, its output
signal is proportional to the
position of the laser spot.
Why we need smaller cantilever ?
Calibration of the optical stage.
0 1 2 3
-2
0
2


A
-
B
(
V
)
Z-displacement(cm)
Region of Gradient: 1000m
Detects 4V for 1000m movement
1mV electrical noise , positional reolution~1/4m
Using optical lever of 100, we can detect cantilever deflection
of ~ 1/400 m=2.5 nm.
Source of noise in AFM
Atomically resolved steps in Ti terminated SrTiO
3

substrate-reaching the limits
Size of step (1/2 unit cell) ~0.38nm
Courtesy Dr. Barnali Ghosh.
Taken in CP-II
Resolution from optical detection
0 1 2 3
-2
0
2


A
-
B
(
V
)
Z-displacement(cm)
Region of Gradient: 1000m
Detects 4V for 1000m movement, 1mV electrical noise
~1/4m.
Reduce noise to 0.1 mV,
Using optical lever of 100, we can detect cantilever deflection
of ~ 1/4000 m=0.25 nm.
Often it is good to have a
cantilever tip rest on a
surface and record the
output as a function of time
We have the base response
of the QPD, need to enhance
optical lever and reduce
electrical noise to get better
resolution
Quadrant photo-detectors
Why use 4 quadrant detector ?
Vertical deflection of cantilever-
Topography
Lateral deflection of cantilever-
Lateral Force Microscopy (LFM)
Thermal Noise limited resolution
If k is reduced the force sensitivity is increased
Cantilever displacement = Force/k
K ~ 0.1N/m , displacement of 1nm will come from a
force of 100pN
Does any thing limit us ?
Yes it is the thermal noise.
It can be very high for soft cantilevers (those with
very small k)
Thermal Noise limited resolution
For any oscillatory system we can apply
Equi-partition theorem
( )
2 / 1
2 / 1
2
2 * 2
2 * 2
, ,
2
1
|
.
|

\
|
~
=
+ ~
k
T k
z
V m z k system harmonic
V m z k T k
B
B
For a 0.1N/m cantilever the thermal noise induced
root mean-square amplitude 0.14 nm.
For a deflection of 1nm of the cantilever it is a
substantial amount.
Force uncertainty~(10014)pN
I have discussed some of the basic concepts of the
SFM and the main components that go with it and
their functions as well as limitations.
Cantilevers and force detection, Scanner
calibrations, Optical detections and sources of
noise

It will be best if your reflect upon your experience
of using SFM and connect to this presentation
Cantilever Statics and Dynamics
The different modes of SPM
Source: PhD thesis Soma Das , SNBNCBS
Statics and Dynamics of cantilever
Interaction between the tip and the substrate will
decide the nature of force and hence the statics and
dynamics of the cantilever
Tip sample
interaction model
Dynamics of cantilever
Any force velocity will
add to damping and
reduce amplitude of
vibration-dissipation
Any force
displacement will change
the frequency of
vibration
Different types of force microscopy depends on
the dynamics of cantilever and the mode of
detection
t j
Fe kz
dt
dz
dt
z d
m
e
= + I +
2
2
Simple ball and spring model
Driving term
for dynamic
mode
Static mode (contact mode)
AFM
t j
Fe kz
dt
dz
dt
z d
m
e
= + I +
2
2
F kz =
=0
Static mode:
Mostly for contact-mode the cantilever deflection
is such that the bending force is balanced by the
force of interaction:
F(z) =-cU/cz=-k.z
U = Total energy that includes the surface as well as
elastic deformation energy.
2
6
) (
z
HR
z f
t
TS =
5 . 1
0
0
) ( ) ( *
3
4
6
2
z a R E
a
HR
f
t
t
z TS + =
a
0
~Atomic dimension (hard sphere)
E
*
~ Effective elastic constant
R
t
- Tip radius of curvature.
H=Hamakar cosntant
2
6
) (
z
HR
z f
t
TS =
5 . 1
0
0
) ( ) ( *
3
4
6
2
z a R E
a
HR
f
t
t
z TS + =
Elastic force wins
over. The deformation
of the surface should
be larger than the
features you would
like to see
Si tip pressing
on Si substrate
One can evaluate
the contact radius
Herzian contact
The contact area
depends on Elastic
modulus
A thumb rule to select cantilever in contact
mode imaging
Cantilever touching a surface is like two springs
connected back to back, The force applied is
balanced by displacement
The softer spring wins
substrate cantilever eff
eff
appl
substrate
appl
cantilever
appl
substrate cantilever total
k k k
k
F
k
F
k
F
1 1 1
.
+ =
= + = + = o o o
A thumb rule to select cantilever in contact
mode imaging
A surface with mixed k (elastic constants) like a
composite of soft and hard matter will not image the
topography. What you image is actually a mixture
of both
substrate
k
ef f
k
cantilever
k
substrate
k
cantilever
k
ef f
k
cantilever
k
substrate
k
~ <<
~ >>
,
,
Correct
condition for
topography in
contact mode
The softer spring wins
Will image the
elastically
deformed surface
Some tips for good contact mode imaging

Get a soft cantilever that is realistically needed.
Do a force spectr0scopy (F-d) curve
Have some idea about the elastic modulus of the
surface you image.
For soft materials when you cannot have very
soft cantilever use LFM
ODT self-assembled monolayer on Ag
Sai and AKR, J.Phys.D Appl. Phys. 40, 3182 (2007)
Some useful applications of
contact mode AFM

Force spectroscopy
Piezo-force spectroscopy
Conducting AFM
Local charge measurements

t j
Fe kx
dt
dx
dt
x d
m
e
= + I +
2
2
Dynamic mode
Driving force
Controlled by
experimenter
Force of interaction of
tip with substrate and
surrounding
Dynamic mode (all non-contact modes):
Cantilever is modulated at resonance frequency and
the shift in resonance frequency , phase or
amplitude measures the force gradient
-cF/cz=-k+(c
2
U/cz
2
)

2
) ( 6
)) ( (
t z
HR
t z f
t
TS =
5 . 1
0
0
)) ( ( )) ( ( *
3
4
6
2
t z a R E
a
HR
f
t
t
t z TS + =
Dynamic mode -what do we do ?
Oscillate the cantilever at close to resonance
frequency
Interaction with the substrate will change the
resonance frequency and /or amplitude of
oscillation (through the viscous force on the
surface)
Detect the departure from resonance or damping
detected by amplitude, phase or frequency shift as
the cantilever scans the surface
This leads to contrast and the imaging
Dynamics of cantilever
2 2 2 2 2
0
0
2 2 2 2 2
0
2 2
0
0
0
2
2
) (
) / )( (
) Im(
) (
) )( / (
) Re(
) (
I +
I
=
I +

=
=
= + I +
e e e
e
e e e
e e
e
e
m F
z
m F
z
e z t z
Fe kz
dt
dz
dt
z d
m
j
t j
In dynamic mode spectroscopy the resonance curve
and its modifications during imaging provides the
image
what happens to resonance frequency in dynamic
mode when there is additional force
z
U
f
z
f
k
z
U
k k
eff
c
c

c
c
=
c
c
+ = , ) (
0
2
2
0
eff
o
m
k
0
= e
Start with a cantilever that is free
Shift in resonance frequency when the interaction is turned on
eff
eff eff eff
eff
m
f
m
f
m
f
m
k
2
0
'
0
'
0
2
0
'
0
'
2
0
'
0
2
1
2
1
1
e
e e e
e
e e e
~ = A
|
|
.
|

\
|
+ ~ + = =
Force derivative is the
important parameter in
dynamic mode
NC
Tapping
Force Derivative
55
NC
Tapping
Two paradigms of dynamic mode
Detection by amplitude modulation
If the resonant frequency of a cantilever shifts, then the
amplitude of cantilever vibration at a given frequency
changes. Near a cantilevers resonant frequency, this change
is large.
Non-contact (tip does not touch the substrate,) -
This also encompasses the EFM and MFM.
Tapping or IC mode (the tip touches the surface at
some part of the swing)
The set frequency is somewhat larger than the free
resonance frequency.
Non-contact
IC/tapping-mode
The set frequency is somewhat smaller than the free
resonance frequency.
From simulation of data-what happens to the
resonance curve in Tapping mode
Das, Sreeram,AKR , Nanotechnology 18, 035501 (2007),Nanotechnology
21, 045706 (2010),Journal of Nanoscience and Nanotechnology 7, 2167
(2007)
-1.0 -0.5 0.0 0.5 1.0 1.5 2.0
0.000000000
10.000000475
20.000000950
30.000001425
40.000001900
50.000002375
60.000002850
70.000003325
80.000003800
Sample:Mica
A
m
p
l
i
t
u
d
e

(
n
m
)
Tip-sample separation (m)
approach(41nm)
retract(41nm)
approach(70nm)
retract(70nm)
approach(90nm)
retract(90nm)
Amplitude vs. distance curves for mica for three different free vibration amplitude of
the cantilever.
Sample: Mica
K= 0.68N/m
Resonance Frequency = 86KHz
Amplitude vs Height
(in absence of feedback)
61
Application of Non-contact mode
Magnetic Force Microscopy
MFM
Measuring long-range force
Any force that decays slower than
inverse square
2
6
) (
z
HR
z f
t
TS =
2 , ) ( < = n
z
A
z f
n
long
2
6
) (
z
HR
z f
t
TS =
This mode is realized by employing suitable probes
(magnetic tip) and utilizing their specific dynamic
properties.

MFM is an important analytical tool whenever the
near-surface stray-field variation of a magnetic
sample is of interest.

MFM can be used to image flux lines in low- and
high-Tc superconductors . MFM have even
extended local detection of magnetic interactions
to eddy currents and magnetic dissipation
phenomena .
The interpretation of images acquired by
magnetic force microscopy requires some basic
knowledge about the specific near-field
magnetostatic interaction between probe and
sample.

How to take care of the topography ???
The magnetic stray field produced by a magnetized
medium and the contrast mechanism
eff
m
F
2
0
'
0
'
0
2
1
e
e e e ~ = A
The shift in frequency the
MFM detects is the gradient
of the magnetic force
Magnetic Force Microscopy of hard disk
(No applied field)
MFM maps the
magnetic domains on
the sample surface
Stored data in a
hard disk
The stray field is maximum
when the anisotropy is
perpendicular
Magnetic Force Microscopy (with applied field)
Requirements for MFM tips
These tips can be coated with a thin layer of magnetic
material for the purpose of MFM observations.

A lot of effort has been spent on the optimization of
magnetic tips in order to get quantitative information from
MFM data .

The problem is that in the coating of conventional tips, a
pattern of magnetic domains will arrange, which reduces
the effective magnetic moment of the tip. The exact domain
structure is unknown and can even change during MFM
operation.
Best tip is the one that has a single mono-domain
magnetic particle !!!!!

Lorentz Microscopy of field
around a tip
Effect of tip sharpness
Stray field line scan
Observed
Simulated
Ordinary tip
Mono-domain
tip
In SFM , what ever you do the most significant
role is played by the tip and the cantilever
I have tried to give a basic introduction to SFM and
some of its different modes and shared my
experience with you.
SFM images are not just picture gallery

The more knowledge you acquire and more
quantitative you become you can get more value
from your SFM.

Thank you