CONTENTS OF TABLE

CONTENTS OF TABLE ..............................................................1

1. Introduction .........................................................................2
1.1 STM and Tunneling effect ..........................................2
1.2 STM modes .................................................................2
1.3 Main factor..................................................................3
1.4 Fast Fourier Transform (FFT) Images ........................3
2. Experiment ..........................................................................3
2.1 Main equipment: .........................................................3
2.2 Experimental part........................................................3
2.3 Layered Structure of HOPG .......................................4
3. Results .................................................................................4
4. Discussion: ..........................................................................7
5. Conclusion ..........................................................................9
6. Refrences:............................................................................9

1. Introduction
1.1 STM and Tunneling effect
Scanning Tunneling Microscope(STM) is a facility of SPM(scanning probe
microscopy). Quantum tunneling effect is the basic concept of STM. And STM is
not limited by environment like UHV(Ultra High Vacuum)
STM consists of a sharp tip on a piezo-electric crystal tube, a mechanism to control
the location of the tip in the x-y plane parallel to the sample surface and a
feedbackloop to control the height of the tip above the sample (the z-axis). [1]

Figure 1. Experimental setup of STM [1]

Tunneling effect is a quantum mechanical phenomenon which is due to the
particle-wave duality [2]
In STM, a narrow gap between metallic tip and the sample occurs when tip
approach towards the sample, this gap is treated as the barrier. A tunneling current
flows from the tip to the sample through the gap.

1.2 STM modes

For a STM, there are three modes could be used, which are called constant current,
constant height and spectroscopy mode.
Constant current and constant height modes are imaging modes which are used for
creating topography. In constant current mode, the tunneling current flows at a
constant number and the tip height is recorded. In the image the brighter regions
shows that the height which is higher than darker part. For constant height, it
applies a constant height by controlling the tunneling current. In the image the

brighter regions shows that the current which is higher than darker part. In the
constant height mode there is a risk of breaking the tip if the samples are not flat.
The spectroscopic mode varies the potential difference between tip and sample, so
that measures the I(V) spectra from which we measure the differential conductance
and from differential conductance we can estimate the local density of states.

1.3 Main factor

The structure of the tip is the most important factor in STM experiment. The size,
shape and chemical identity affect on not only the resolution and topography, but
also on the electronic states.
The radius of curvature of the tip is the crucial point of lateral resolution. The
higher curvature it has, the faster picking rate it gets, as well as the less phase lag it
has. The sharper the tip is, the more stable the tunneling current flows.

1.4 Fast Fourier Transform (FFT) Images

FFT image is the Fast Fourier transformation image showing the symmetry of
sample (graphite) in reciprocal space. The principle working of FFT image is
transforming the image into the reciprocal space using the FFT module.

2. Experiment
2.1 Main equipment:
Tip: Pt-Ir Wire
Sample: Highly Oriented Pyrolytic Graphite (HOPG)
STM device
Tweezers, etc

2.2 Experimental part

The first step of the experiment was the formation of tip (5 mm long piece of Pt-Ir
wire) by mechanical shear force using sharp pliers. Second step involved the
preparation of the sample surface which was done by sticking the tape on the
surface of highly oriented pyrolytic graphite (HOPG) sample and then removing
the upper layer. After that the sample was fixed in the clamps of sample holder by
using tweezers. The sample was then slided on the stage in the z-axis to make
connection between sample and tip. To check that there was proper connection
between sample and the tip an indicator was provided on the machine, which turn
to red if the sample touches the tip and turn to green if desired position was
reached.
After the adjustment of z distance, either manually or by using piezo-motor, by
clicking approach option on the software, the program was started to scan the
sample. In this experiment constant current mode was used. Before scanning, X
and Y orientation of sample was adjusted by using the software, to make it flat.
Easy Scan program was started to take the image and profile (topography) of the
sample. As the surface was scanned by the stylus, zooming in is performed on the

desired area, as well as distance was decreased between sample and tip to get more
detailed image. Z range was also changed relatively to zooming to adjust contrast.
Imaging time was also decreased for fast processing. After imaging, the real images
were converted to Fast Fourier Transform (FFT) images, to determine d spacing
and lattice parameters.
The experiment consists of four different parts.
1. Image of highly oriented pyrolytic graphite (HOPG)
2. Conversion of real image to FFT image.
3. Measuring Crystal lattice spacing and lattice parameter
4. Comparison of values with the standard

2.3 Layered Structure of HOPG

Highly ordered pyrolytic graphite (HOPG) consists of layers of carbon sheets,
forming a semi-metallic system. While the carbons within a sheet are covalently
bonded to form a hexagonal lattice structure, the layers are held together by Van
der Waals forces. The in-plane lattice constant (repeating unit length) and the z-axis
lattice constant are 2.46 and 6.7 respectively and the in-plane atom-to-atom
distance is 1.42 . The sheets are arranged such that every other carbon on a layer
has a carbon in the neighboring sheets, Figure 2. The carbons in the first layer that
have a carbon in the second layer right below are called an A-site carbons, and the
carbons without a carbon directly below are called B-site carbons. [3]

Figure 2. Layered structure of HOPG [3]

3. Results
In the experiment, 3 different regions in the same sample were examined by the
STM.

Figure 3. Region 1, image of HOPG under investigate of STM, left is topography

image and right is the FFT converted image
Calculate from Reciprocal to Real Space is shown as below:
d = 2/d*, whered and d* are real and reciprocal d-spacing respectively. The factor 2
is due to the reason that d* is the distance between subsequent three reflections,
getting inter-planar distance therefore factor is employed.
By measuring two reflections in reciprocal space, in Figure 3, from a to b,
d-spacing value is determined. Then, it is calculated into real space d value.

Table 1. D-spacing values and angles from Sample region 1

Literature
Reciprocal
Real space
Test 1
(from the lab
Deviation
space [1/nm]
[nm]
Manual)
d-spacing
8.533
0.234
0.213 nm
9.8 %
value 1
d-spacing
8.893
0.225
0.213 nm
5.6 %
value 2
d-spacing
8.78
0.228
0.213 nm
7%
value 3
* = 59
angles
* = 62
* = 59
The value of literature is taken from the lab manual, deviation is calculated by
subtracting literature value from the real space and divide by the literature value.
i.e.
Deviation = (Real space Literature) / Literature

Figure 4. Region 2, image of HOPG under investigate of STM, left is topography

image and right is the FFT converted image

As the same measurement and calculation as region 1, d-spacing value and

angles are determined for region 2 and 3.
Table 2. d-spacing values and angles from Sample region 2
Reciprocal
Real space
Test 2
Literature
Deviation
space [1/nm]
[nm]
d-spacing
8.599
0.232
0.213 nm
9%
value 1
d-spacing
8.474
0.236
0.213 nm
10.7 %
value 2
d-spacing
9.052
0.221
0.213 nm
3.75 %
value 3
*=58
Angles
*=62
Angles
*=60
-

Figure 5. Region 3, image of HOPG under investigate of STM, left is topography

image and right is the FFT converted image

Table 3. d-spacing values and angles from Sample region 3

Reciprocal
Real space
Test 3
Literature
Deviation
space [1/nm]
[nm]
d-spacing
8.686
0.230
0.213 nm
8%
value 1
d-spacing
8.489
0.235
0.213 nm
10.3 %
value 2
d-spacing
value 3

8.538

0.234

0.213 nm

9.8 %

angles

*=59
*=60
*=61

4. Discussion:
In Topography image of the HOPG sample each point describe the planes of atom
instead of the individual atom. One can estimate the arrangement of atoms from
topography image as it shown in Figure 6.

Figure 6: Topography Image showing the planes of atoms, right side image
represent the topography image of HOPG by STM whereas the left side image
represent the schematic representation of planes [4]
The topography image of the sample contain bright and dark region, the reason
behind is bright and dark contrasts are due to the un-even surface of HOPG. As the
distance between the HOPG and tip is reduced current density which cause by the
software in the image bright and dark spots.
Another reason of bright and dark contrast may be that in the lattice model of
graphite that there are two different positions of the carbon atoms in the graphite
crystal lattice. One with a neighboring atom in the plane below appear dark and
one without a neighbor in the lattice below appear bright. The reason behind is
atoms without a direct neighbor in the layer beneath have the full electron density
therefore appear as bright spots whereas an atom with a direct neighbor in the layer
beneath loses electron density therefore appear as dark spot. Consequently the
electrical conductivity of the graphite surface varies locally slightly (different
electronic density of states). [4]

Figure 7: the Bright and dark contrast of HOPG in STM image [5]
Variations from the literature values are due to following reasons:
1. Tip preparation error

2. Surface of HOPG is not flat.

3. Effects of surrounding i.e. air flow, direct light or disturbance in
measurement.

5. Conclusion
STM is a characterizing technique used for conducting material to reveal the
structure and topography at the atomic level. It can also be used to find d spacing
and lattice parameter. Experimental results shows that there has been a deviation of
maximum 10% which are due to some reasons which are mention in the
discussion part.

6. Refrences:
[1] http://www.accefyn.org.co/sp/nanociencia/documents/curso/SPM.pdf
[2]http://www.princeton.edu/chemistry/macmillan/group-meetings/DEC_tunneling.
pdf (Date: 22.04.2013)
[3] Atomic resolution images on HOPG, Nanosurf STM Application Note
http://www.nanosurf.com/index.cfm?action=act_getfile&doc_id=100486
[4] STM study of HOPG and Gold films
(http://depts.washington.edu/nanolab/NUE_UNIQUE/Lab_Units/5_Lab_Unit_ST
M.pdf)
[5] Atomic resolution of graphite surface by STM by TESS Experts, PHYWE
System
GmbH
&
Co,
(Dated:
5.3.2000)
(http://grundpraktikum.physik.uni-saarland.de/scripts/PHYWE_STM_Experiments
.pdf)