Scanning Probe Microscopes:

Scanning Tunneling Microscope (STM)

and Atomic Force Microscope (AFM)

Dr Rakesh G Mote - Dr. Suhas S. Joshi

Department of Mechanical Engineering, Indian Institute of Technology, Bombay,
Powai, MUMBAI 400 076 (India)
ssjoshi@me.iitb.ac.in; rakesh.mote@iitb.ac.in

Optical Microscopes

The optical microscopy has been one of the earliest methods of analysis.
The electron microscope was built in 1931.
The electrons are the particles that can be accelerated, focused and detected.
They have shorter wavelength than visible lights and illuminate the specimen
giving higher resolutions than the optical microscope.
The transmission electron microscopes (TEM) is similar to optical microscopes
involving a light source and image plane, but uses electrons instead of light
source. Electrostatic and magnetic lenses are replaced by glass lenses in TEM.
In SEM (1938), an electron beam is focused onto a small spot and scanned in
parallel linear scans over the surface of the specimen. The electrons going back
and forth from the surface are detected simultaneously with an electron
detector.

Scanning Probe Microscopes

SPM uses a sharp probe to
measure a sample at localized
points with nanometer resolution.

Resolution:
Lateral dimension: nanometer
Vertical dimension: sub-nano
SPM family members:
Scanning Tunneling Microscope (STM)
Atomic Force Microscope (AFM)
Near-field Scanning Optical Microscope
(NSOM)
Magnetic Force Microscope (MFM)
etc.

Schematic of a generalized SPM

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Scanning Probe Microscopes

The basic method of the scanning probe microscopes was to be able to move a tip
over the substrate surface with a sensor (probe) with molecular sensitivity (nm) in
the longitudinal and height directions.
This is something similar to the act of probing over a surface with a finger.
If the sensor movement is controlled under highly sensitive feedback system,
when coupled to a variety of signals, it could provide atomic surface details.
Originally, two types scanning probe microscopes
were invented: these are - scanning tunneling
microscope (STM) and atomic force microscope
(AFM).
STM can be used for conducting materials whereas,
AFM can be used for non-conducting materials.
The STM was invented by Binnig and Rohrer in 1982
(for which they were awarded the Noble prize in
1986).

Scanning Probe Microscopes

STM and AFM proved to be powerful tools for obtaining information on
the packing order of molecular adsorption on a surface, relative importance
of molecule-molecule and molecule-substrate interactions, also types of
forces responsible for the packing order at the surface.
This is important in growth of thin films, lubrication and microelectronics
fabrication, each of which involves interactions between molecules on a
surface and can be investigated by using these procedures.

Scanning Probe Microscopes

Scanning Tunneling Microscope

The STM can image the surface of conducting materials with atomic-scale
detail.
Similar to the other microscope, where image of the surface is recorded, in STM,
a map of trajectory of a probe tip over a surface is recorded, where the height of
the probe is constantly adjusted to maintain a constant tunneling current between
the tip and the surface.
The object points are in the range of atomic dimensions i.e. 1 nm = 10-9 m =
10A0. This corresponds to the magnification around 10 million times.
In general, resolution of an object is determined by the smallest distinguishable
distance between two closely spaced features in the sample.
The samples could be analyzed in the ambient conditions and no preparation
(like drying or treatment) of the work surfaces is necessary.

Scanning Tunneling Microscope

In STM, two conducting electrodes are separated
by some isolator (air or liquid) form a barrier for
the electrons inside the electrodes.
If the barrier is thin (around 1 nm) enough,
electrons can pass through it by quantummechanical process called tunneling.
The probe is made of W or Pt-Ir alloy and scans
the surface of a sample with the help of a
piezoelectric device.
At very small distances, the wave functions of
molecules at the surfaces of the sample and the tip
overlap.
If a bias voltage is applied to the sample, an electron
tunneling current flows between the two phases.
The tunneling current between the conductive sample
and the tip is measured as a function of distance
traveled in X and Y directions.

If two conductors are so close that their leak

out electron wavefunctions overlap. The
electron wavefunctions at the Fermi level have
a characteristic exponential inverse decay
length K given by

When a small voltage, V is applied

between the tip and the sample, the
overlapped electron wavefunction
permits quantum tunnelling current

m is mass of electron, is the local tunneling barrier height or the average

work function of the tip and sample, h is Plancks constant

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Scanning Tunneling Microscope

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Scanning Tunneling Microscope

The two modes of operation of STM are: 1. Constant current mode. The tip is
moved to maintain the current constant to a preset value. 2. Constant height mode:
the distance is kept constant and the variation in current is measured to find out
the variation in the distance.
Constant current
mode

Constant height
mode

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Scanning Tunneling Microscope

The tip-sample separation can be controlled very exactly.

The tunneling current is only carried by the outermost tip atom; the atoms that
are second nearest carry only an negligible amount of the current: The sample
surface is scanned by a single atom.
The resolution in the image is defined in the vertical direction and laterally on
the plane of the sample. The size and shape of the probe will determine the
lateral resolution.
The tip moves at 10A/V applied to the translator. Typically, a lead Zirconatelead titanate (PZT) polycrystalline ceramic is used. It has strong piezoelectric
properties.
The sample is mounted on a scanner that enables movement in all three
dimensions x, y and z with a resolution better than 1 A and a maximum scan
length of the order of a few hundred micrometers.
The movements are controlled by voltage applied over different segments of the
piezoelectric tube.
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Scanning Tunneling Microscope

For a typical barrier heights of 4eV, the tunneling current decays one order of
magnitude when the distance z is increased by 1 A0. Therefore, the tunneling
tip is at close proximity to the sample.
The tunneling detection method is sensitive to contaminants such as oxides or
hydrocarbons.
The presence of contaminants causes the tip to press and lever to oscillate until
the nominal tunneling current is achieved.
Forces as high as 10-6 N have been reported in such cases. But for the ideal
conditions, the forces are reduced to 10-9 N (nN).

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STM Tips
The most common types of STM tips are electrochemically etched tungsten wires
and cut platinumiridium wires.
Use of materials that do not oxidise in air such as Pt-Ir or Au might be
advantageous as far as the stability of tunneling in air.

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Scanning Tunneling Microscope

STM image, 7 nm x 7 nm, of a single zig-zag

chain of Cs atoms (red) on the GaAs(110)
surface (blue).

The barriers were assembled by individually

positioning Fe adatoms using the tip of a low
temperature (STM). A circular corral of radius
71.3 A0 was constructed in this way out of 48
Fe adatoms.
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Atomic Force Microscope

Atomic Force Microscope

After the STM was invented, it was felt that similar type of scanning
microscope is needed for non-conducting surfaces.
AFM was developed 5 years after the invention of STM. The AFM can
operate on non-conducting as well as conducting surfaces.
AFM work Principle: It works on the principle of separation dependency
force between any two bodies. This force can be attractive or repulsive, which
depends upon the separation distance.
In AFM, It is the force between the tip and the substrate that is present at close
separations.
Pyramidal silicon nitride tips are used, which have a radius of curvature of
100A0.
These are made by an etching process that removes silicon from the substrate,
leaving an etched and sharpened tip behind.
The force is detected by placing the tip on a flexible cantilever that deflects
proportionally to the exerted force.
The deflection is then measured by some convenient procedure, such as laser
reflection or some other device.
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Atomic Force Microscope

A Si3N4 cantilever of an approximately 200 m in length and a spring constant
of 0.06 N/m or 0.12 N/m is generally used.
The biggest advantage of AFM is that most of the samples can be investigated
in their natural state including biological samples in an aqueous environment,
which otherwise is not possible by electron microscopy.

AFM Apparatus principle

Schematic of beam deflection

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Atomic Force Microscope

Construction of an AFM: requires a force sensor to measure forces between a
small probe and the surface being imaged.
A common type of sensor utilizes a relation between motion of a cantilever and
the applied force given by Hooks law
F=-KxD
K is a constant depends upon the material and dimensions of the cantilever, D is
the deflection of the cantilever.

For a cantilever of length L = 100 m, W = 20 m and T = 1 m, the force

constant is 1 N/m. Thus, if the cantilever is moved by 1nm, a force of 1 nN
is required.
The measurement of deflection of the cantilever (as small as 1nm) is
possible by light lever method.
In this light is reflected into a photo-detector from the back of the cantilever.

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Atomic Force Microscope:

Cantilever Deflection Detection

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Atomic Force Microscope

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Atomic Force Microscope

A feedback control is used to keep the probe in a fixed relationship with the
surface while the scan is measured.
In principle, the theory and operation of a AFM is similar to a stylus profiler.
Only difference being, in AFM, the forces are of much smaller magnitude. Also,
since the AFM uses much smaller probe, the resolution is much higher.
A constant force is maintained between the probe and the sample while the
probe raster scans the surface.
A constant force is maintained by
measuring the force by the light lever
sensor and using a feedback circuit to
control the position of the z
piezoelectric ceramic.
The motion of the probe in X and Y
directions is generated by the
piezoelectric ceramic.
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Atomic Force Microscope

AFM Resolution: The traditional microscopes have resolution in only in the
plane of the image.
The AFM has resolution in two directions: one in the plane of measurement and
other in the direction perpendicular to the surface.
The in-plane resolution depends upon the geometry of the probe used for
scanning.
In general, the sharper the probe, the higher the resolution of the AFM image.
The vertical resolution in an AFM is established by relative vibrations of the
probe above the surface.
Sources of vibration are: acoustic noise, floor vibrations, thermal vibrations and
so on. To obtain maximum vertical resolution requires minimization of vibrations
of the instrument.

Dull probe: Low

resolution

Sharp probe:
High resolution

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Atomic Force Microscope

Scanning speeds estimated in AFM are: 0.1 m/s in vacuum and 2 m/s in
water.
The increase in speed in water arises from the damping effect provided by water
on the cantilever as the density of water is 1000 times that of the air.

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Atomic Force Microscope

Scanning Modes: When scanning a sample, a constant force is applied to the
surface at the end of cantilever. The measurement of force with the cantilever is
achieved by two methods:
In the first method, deflection of the cantilever is directly measured. It is also called
as contact mode.
In the second method, the cantilever is vibrated and a change in its vibration
properties is measured. It is also called as Tapping mode.

The interaction between the probe and sample surface is one of the important
aspect of the AFM, which affects its resolution.

Deflection or
contact mode

Vibration or
tapping Mode
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Atomic Force Microscope

The interactive forces can be attractive or repulsive and are as small as a few nN.
A force curve starts at a point where the difference between the tip and the sample
are negligible, and the cantilever is not deflected.
As the tip touches the sample,
this region is called non-contact
region.
But when they are brought very
close to each other, then they
contact. This is called contact
region.
In the non-contact region, the
net force detected is attractive.
Whereas, in the contact region, it
is repulsive.

Contact region

Non-contact region
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AFM
Probe

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Atomic Force Microscope

Contact mode: It is the most common method of operation of the AFM. As
the name suggests, the tip and sample remain in close contact as the scanning
proceeds. But, in this mode, forces are in the repulsive regime of the intermolecular force curve (see figure). The repulsive region of the curve lies
above the x-axis.
Since the deflection of the cantilever is directly proportional to the force on
the surface, a constant force is applied to the surface during the scan.
The cantilever in such cases has spring constant in the range of 0.01 to 10
N/m. Since the forces are of the order of nN, the probe touches minimally to
the surface of the sample.
The contact mode can also be operated under fluids with similar high
resolution that in air.

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Atomic Force Microscope

Tapping mode: It is the next most common mode used in AFM. In this, a
cantilever is operated at its resonant frequency, which is often 70-400 KHz.
It can be operated in air or other gases. The probe is positioned above the surface
so that it only taps the surface for a very small fraction during its oscillation
period.
The probe operates in a contact mode, but for a very short time due to
oscillations. This contact ensures that the lateral forces are dramatically reduced
as the tip scans over the surface.
When a vibrating cantilever comes close to
the surface, the amplitude and phase of
vibrating cantilever may change. The
changes in the vibration amplitude or phase
are easily measured and the changes can be
related to the force on the surface.
This mode is a better choice when poorly
immobilized or soft samples are imaged.
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Tapping Mode

Atomic Force Microscope

Non-contact Mode: In this method, the cantilever must be oscillated above
the surface of the sample at such a distance that the resulting force is no
longer in the repulsive regime of the inter-molecular force curve.
This is a very difficult mode to operate in ambient conditions with the
AFM.
The thin layer of water contamination which exists on the surface on the
sample will invariably form a small capillary bridge between the tip and the
sample and cause the tip to "jump-to-contact".

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Atomic Force Microscope: Resolution

The lateral resolution is determined by two factors:
step size of the image
minimum radius of the tip

A probe tip with a 40nm diameter was used to measure the left image and a
probe tip with 5 nm diameter

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Atomic Force Microscope: Resolution

Atomic Resolution

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Atomic Force Microscope: Calibration

Calibration and Image Analysis of STM and AFM: The calibration of STM and
AFM in X and Y- directions can be done using suitable grids available
commercially.
The calibration in Z-direction is more difficult. At this stage, the best
procedures are:

Use of gold samples with steps of one layer of gold

Use of lipid layers deposited as LB films
Use of macromolecules with known dimensions
Use of highly oriented pyrolytic graphite

2D and 3D STM image of Highly Oriented Pyrolytic

Graphite (23.2 A x 23.2 A x 2.19 A

AFM image of commercially

available grid (90,000 A x 90,000
A and max height of 7289 A
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AFM: Applications

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AFM: Appln - Lateral Force Microscopy

Polished polycrystalline silicon carbide

Lateral Force Microscopy (LFM) (right) and
topographical (left) images of the surface
of a polished polycrystalline silicon carbide
film. The polishing process obscures the
grain structures in the topographical image
but it is clearly visible in the LFM image.
30m scan.

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AFM: Appln Phase Detection Microscopy

Phase detection microscopy (PDM) is another technique which can be
used to map variations in surface properties such as elasticity, adhesion
and friction.
Phase detection images can be produced while an instrument is operating
in any vibration cantilever mode.
Phase detection refers to the monitoring of the phase lag between the
signal that drives the cantilever to oscillate and the cantilever oscillation
output signal.
Changes in the phase lag reflect changes in the mechanical properties of
the sample surface.

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AFM: Appln - Contact Lens Characterization

Power Spectral
Density (PSD):
Section analysis
reveals a 1.5 m
periodicity and
nanometer-sized
peak-to-valley
heights of the
grooves at various
locations
AFM measurement of the grooves on the lens surface
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AFM: Appln - Contact Lens Characterization

Prominent linear feature on the lens surface (a) 47 m, (b) 10 m, (c) 4 m

A surface defect, measured of 170 in

width and 150 nm in depth, is large
enough to trap proteins and other
contaminants.

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