Scanning Probe Microscopy

By:

MUKESH Kumar
IIT Ropar
[email protected]
 Scanning Probe microscopy

 Powerful tool because of good magnification and not limited to topography.

 Nanoscale electrical, magnetical, mechanical, optical properties can be

investigated

This dimension not

accessible for imaging!!!!

3-D imaging is possible!!!!

 Lennard-jones potential: AFM
 van der Waals forces

Sharp tip in contact with sample

 Lennard-jones potential: AFM
 At distances few Å apart
attractive van der Waals
forces act between the atoms
of the tip and the sample.
 When the tip approaches
closer and electron clouds repel
each other the attractive van der
Waals forces decrease in
strength.
When the two forces balance
each other at distances ~
chemical bond, the force goes
A general Force-distance curve to zero.

REGIME OF  At even closer distances repulsive

CONTACT MODE van der Waals forces come into play.
AFM
 Scanning Probe Microscope
 Piezo scanner | vertical moment detection | Feedback system | Tip

Means of sensing
vertical position of tip.
A coarse
positioning
system to
bring the
A probe tip
tip into
general
vicinity of
A feedback system to sample
control the vertical
position of the tip.

A PZT scanner to
move either tip or A computer system to drive the scanner,
sample on the other measure data and to process It into an
in a raster pattern. image
 More insight
 How tip approached on the sample

 How and where to focus the laser on different

tips

 Role of PSPD

Position of PSPD
Positionof laser on tip
 More insight

 The pixel size of the image and image resolution

 Scanner range
 Find a specific location for scanning on a bigger image
 Position sensitive Photodetector
Photo sensitive
Laser
Photodetector

ro r
Mir

Light received
from different
segments
is processed
electronically Four-segment
to convert into photodiode
height signal. Cantilever

Reflective coating on
the back-side of the
cantilever
 Instrumentation Overview
Scanner Probe Photodetector Feedback

Scanners consist of Piezoelectric materials

0V +V -V

No applied voltage Extended Contracted

Design of a scanner tube

y
z
z
Metal
Electrod
y e x x
PZT
x y x material

Ground
y
 Instrumentation Overview
ac voltages applied at different segments of scanner tube

x-axis y-axis

+V +V

X 0 t Y 0 t

-V Sample -V

+V
+V

t
X 0 Y 0
t

-V
-V
 Instrumentation Overview
There is a reflective coating at the Probes
back side of the cantilever.

The cantilever moves on the sample

surface. It follows the contours on
the sample i.e. bumps or pits present
on the surface.

Tip

Sample Usually Si or Si3N4 tips are used.

The cantilevers obey Hooke’s law for small

displacements. So, the interaction force
between tip and sample can be found out.
Position sensitive Photodetector

i. Initial position of laser spot.

ii. On reaching a height, spot
gets deflected.
iii. Feedback operates, brings
spot to initial position.
iv. On descent spot deflects
again, but now to a different
position.
v. Feedback again operates to
bring the spot to the initial
position.
 LATERAL FORCE MICROSCOPY (LFM)

 Lateral force microscopy images for PZT samples

 Feedback system

Constant Force mode Constant Height mode

 Feedback is on.
 Piezo responds
to any changes
detected & alters
tip-sample gap.
 Fairly faithful
topography. Feedback is off.
Tip moves at a
constant height
above sample.
High resolutions
are achieved.
 Modes of AFM
 Tip-sample remain close
while scanning.
 Mode is in the repulsive Contact Mode
regime of force-plot.
 Large lateral forces exist-
causing tip to drag. AFM’s Most Common Operating Modes
 Strong repulsive forces act.
 Cantilever oscillates at/near
its resonance frequency.
 Tip taps the surface TAPPING Mode
occasionally.
 Lateral forces are
dramatically reduced.
 Better for softer samples.
 Cantilever vibrates near
the surface of the sample.
 No physical contact with
sample surface.
NON-Contact Mode  Changes in resonant freq,
vibration amplitude are
detected.
 Cantilevers used are stiffer.
 Modes of AFM
Difference between Contact and Non-contact Mode

Contact Mode AFM Non-Contact Mode AFM

Surface covered with

a water droplet

Image of the surface

as scanned by the tip

Tapping mode provides the best resolution. The lateral forces present in the
contact mode are dramatically reduced in this mode giving a higher lateral
resolution.
Effect of Tip-Shape on Imaging

Effect of a tip-shape.

Shows the effect of missing atom.

Effect visible,
though small.

Superposition of signals nullifies

the effect of missing atom.
Images Follow!!
Indium nano particles
Bad Imaging due to a bad tip.
Particles sticking onto the tip spoil the imaging.
Cu nanorods 3-D image
Cu nanorods
 Current sensing-AFM
• CS-AFM measures the local
electrical conductivity of a material
at nanoscale

• Current flow direction in the sample

can be controlled: either lateral or
transverse direction through
appropriate electrode configuration

• Local Electron/hole mobility can be

estimated from local I-V plots

• Local photocurrent can be measured

by conducting I-V spectroscopy
under light illumination

• Standard sample: Au or ITO coated

glass
 Current Sensing-AFM
Chlorobenzene 1 2 dichlorobenzene 1 3 dichlorobenzene

 Brighter regions (higher hole current)

correspond to P3HT
 Darker regions (lower hole current)
correspond to PCBM
 Nanoscale charge transport pathways
are clearly defined in 12 DCB film,
which also has higher electrical
conductivity as compared to CB and
13 DCB films
 Local I-V measurements by CS-AFM
Local dark I-V plots Local I-V under Illumination

0.15
0.15 CB based film
CB based film
12 DCB based film 12 DCB based film
0.12
0.12
13 DCB based film 13 DCB based film

Current (nA)
0.09
Current (nA)

0.09

0.06
0.06

0.03
0.03

0.00
0.00

-0.03
-0.03

-0.06
-0.06

-1.0 -0.5 0.0 0.5 1.0 -1.5 -1.0 -0.5 0.0 0.5 1.0 1.5

Bias Voltage (V) Bias voltage (V)

 Local I-V spectroscopy

 Local Current in all the films increased
with illumination
 Dark current and illuminated photo-current
was maximum in 12 DCB based film
 Hole mobility calculations from local I-V plots
• Space charge limited current density
(SCLC) J= current density
Tip radius = 20 nm
ε = dielectric constant
µ = hole mobility
V = bias
L = thickness of film
(Mott, N. F. Gurney, R. W. Electronic
Processes in Ionic Crystals,Oxford
University Press, London, 1948) 0.056
CB
0.048
• Hole mobility (dark) obtained by fitting 12 DCB
13 DCB
the above equation

Current (nA)
0.040

 CB 4.64 x 10-3 cm2/V-s 0.032

 1 3 DCB 6.89 x 10-3 cm2/V-s 0.024
 1 2 DCB 1.40 x 10-2 cm2/V-s 0.016

0.008
• Highest hole mobility in 1 2 DCB film
0.2 0.4 0.6 0.8 1.0 1.2 1.4
2
V
CS-AFM and selective carrier dynamics
 Tapping mode: Phase Imaging
 Atomic force microscope is
commonly used to determine
the surface morphology
• Phase image: The phase lag of
the cantilever oscillation,
relative to drive signal
 Simultaneously imaged
with topography
• Phase lag is dependent on
factors such as: viscoelastic
properties of the surface,
composition, adhesion and
friction
• Helpful in identifying multi-
phase morphology of polymer
blends
 Tapping mode: Phase Imaging
Lift mode: Double pass

Single pass mode

EFM mode requires a MAC III controller to provide the drive signals. Lock-in
1 is used to drive the cantilever. The input to Lock-in 1 is the amplitude of
the cantilever deflection at a specific frequency. Lock-In 2 operates at a
different frequency, providing the AC bias, also with the Deflection channel
as its input.
 Topography and phase imaging

Topography images of P3HT: PCBM blended films spin cast from CB and
1,2-DCB solvents, respectively. (b and d) shows the corresponding phase images
 Tapping mode: EFM

 EFM measures electric field gradient distribution above the sample surface,
through measuring local electrostatic interaction between a conductive tip and a
sample
 In EFM, a voltage is applied between the tip and the sample to create and
modulate an electrostatic field between the tip and the substrate.
 The cantilever’s resonance frequency and phase change are used to construct the
EFM image
 Tapping mode: EFM

 The standard sample for EFM, FLUOROALKANES F14H20 which produces a

fixed amount EFM signal
 Tapping mode: KPFM

Electronic energy levels of the sample and AFM tip for three cases: (a) tip
and sample are separated by distance d with no electrical contact, (b) tip
and sample are in electrical contact, and (c) external bias (V dc ) is applied
between tip and sample to nullify the CPD and, therefore, the tip–sample
electrical force. Ev is the vacuum energy level. Efs and Eft are Fermi
energy levels of the sample and tip, respectively
Tapping mode: KPFM
STM and STS
Scanning Tunneling Microscope: STM

The Scanning Tunneling Microscope works like a record player…

Scanning Tunneling Microscopy
 Allows for the imaging of the surfaces of metals and
semiconductors at the atomic level.
 Developed by Gerd Binnig and Heinrich Rohrer at the
IBM Zurich Research Laboratory in 1982.

Binnig Rohrer

 STM has fathered a host of new scanning probe techniques:

Scanning Tunneling Spectroscopy, Atomic Force Microscopy
(AFM), Magnetic Force Microscopy, Near-field Scanning Optical
Microscopy (NSOM) etc.
What is Tunneling?
Quantum Tunneling

de broglie
wavelength
 Quantum Mechanical Tunneling

V(x)
V0 T  16 (1   )e 2d

e x
 (x)
e

x=0 x=a
x
 STM-Tunneling (No PSPD)

 The 90% of the current is contributed from the top and front
atom
 Modes of Scanning

Constant
Height Mode

Constant
Current Mode
STM Does NOT Probe The Nuclear Position Directly
Scanning Tunnelling Spectroscopy
Scanning Tunnelling Spectroscopy
Scanning Tunnelling Spectroscopy
 Some practical examples of STS: Si

Scanning tunneling microscopy and spectroscopy (STM & STS)

measurement of a B and P co-doped Si-NC (7 nm in dia.). (a)
STM topography image of Si-NC before performing the
spectroscopic measurements. (b) Height cross section of NC
size. (c) dI/dV–V characteristics, which is proportional to the DOS
Some practical examples of STS: PSC
Band alignment across 2D/3D perovskite
hetero interfaces using STM. (a) in the
dark and (b) under 515 nm laser
illumination. The sample archi-tecture is
ITO glass/2D perovskite/3D perov-skite.
Mapping images of current spectra
across2D/3D perovskite heterointerfaces
probed at a sample bias of +0.8 V (c) in
the dark and (d)under 515 nm radiation.
Point-to-point evoluation of electronic
dI/dV curves across 2D perovskite/ 3D
perovskite interfaces (e) in the dark and
(f) under 515 nm illumination. Map-ping
images of the band alignment across
2D/3D perovskite heterointerfaces (g) in
the darkand (h) under 515 nm
illumination

NanoEnergy 2021, 89, 106362

Thank You