Observation of monocrystallic silicone crystal using TEM

Kristian Sagmo
NTNU, 22. april 2013

Abstract
The distance d022 was measured to be 1.853 0.067 .

Introduction
The purpose of this report will be to briey summarize the observation of a multicrystalline silicone crystal using Bright Field (BF) and High resolution (HR) TEM
modes, as well as to exhibit a basic understanding of some of the physics involved
in the mechanisms of the microscope and basic observation theory. The rst TEM
microscope was invented by Max Knoll and Ernst Ruska in 1931 shoving promise of
higher resolutions than that possible with light. This remains one of the main benets of the instrument to date, being capable of resolutions down to around 0,05 nm
[2]. Problematically, lens imperfections leading to unwanted optical eects caused by
spherical and chromatic abberration, is now one of the main limiting factors of the
resoluton power of TEM.
For simplicity, no section regarding method will be included in this report, as it is
largely described here in the introduction and the theory section.

Theory
About TEM
TEM is a method of imaging using engergized electrons, oscillating with a specic

wavelength, to penetrate a thin sample of material. The wavelength, , may be

modeled by the De Broglie relation and the relativistic momentum of the electron (for
high voltage), to produce the equation
= q

h
2m0 E(1 +

.
E
2m0 c2 )

(1)

Here, h is the planck constant, m0 the rest mass of an electron, c the speed of light
and E the energy of the accelerated electron. We may then begin to appreciate the
practicality of using a charged particle for imaging, as one may by applying a specic
voltage across the electron accelerator, produce probing particles with wavelengths
smaller than that of light.
As electrons are highly interactive particles, the material needs to be thin, 200
nm or less, to prevent too many scattering events in the sample. A specifc ray of
transmitted electrons may then be selected by the use of a specic aperture in the
back of the sample, usually after the electrons have been focused. This selction of
transmitted electrons denes the dierent imaging modes commonly used.

Lab assignment in course TFY 4220; Solid State Physics, S2013

BF-TEM is among the most commonly used modes. It involves selecting only the

directly transmitted electrons by the positioning of a magnetic gathering lens, and

an aperture in its focal plane. An area of the sample with a denser concentration
of atoms, as seen by the electron, will appear darker than an area with less atoms
along the linear path of the electron. In addition, in a crystal structure, braggs law
suggests that areas oriented more symmetrically towards line of motion for a particle,
will diract, meaning it will appear darker than more randomized areas.

HR-TEM involves selecting all transmitted electrons to produce an image.

Diraction-mode TEM, involves selecting only diracted electrons to form an image.

In a crystal structiure this provides an image of the diraction pattern formed by the
electrons, giving information of the alignment of the symmetry planes in the sample.
By selecting dierent incoming waves, tilting the sample, and selcting diracted waves,
one may for instance identify imperfections in a crystal structure, as well as identify
the dierent orientations in a multicrystalline structure.

Diraction and diraction pattern indexing

By introducing Miller indexes (hkl), the real space distance between atomic planes in
a cubic crystal might be described
dhkl =

a
,
h2 + k 2 + l2

(2)

where a is the lattice constant of the cubic planes. Further, the vector in the reciprocal
space indexed ghkl = hi a + ki a + li a is related with the real space distance by
1
,
| ghkl |

dhkl =

(3)

thus illustrating that the interplanar atomic spacings and the diraction pattern image is inversely related [1].
In indexing diraction patterns, dierent approaches may be used, but here preered
is the relationship between the ratio of the lengths between two diraction points and
their respective hkl values. By exploiting that tan 2 = 2 for very small angles and
thereby 2 = RLhkl , Braggs law gives
(4)

Rhkl dhkl = L.

The value Rhkl is the distance of the diraction point hkl from the origin, so again
this illustrates that the distance between diraction points in a diraction image is
inversely related to the real space between lattice planes in the crystal. Using the
above equation for dhkl one arrives at the desired equation
d2
h2 + k12 + l12
R12
.
= 22 = 12
2
R2
d1
h2 + k22 + l22

The vector relation

cos 12 =

R1 R2
,
R1 R2

(5)
(6)

may be used as a check. Lastly to calculate the zone axis of an indexed diraction
pattern


i

R1 R2 = h1
h2

j
k1
k2

k 
l1 
l2 

(7)

Results
Indexing of diraction patterns
For the diraction pattern shown in gure 1 , given that our silicone sample is a diamond crystal with a fcc Bravais lattice with a two atom basis, all visible points must
fulll Fhkl = 4f , meaning that h, k and l are all even or all odd. Furthermore, in
the image, R is measured R1 = R2 = 2 cm, so equation (5) = 1.The angle between
points gives cos 12 = 12 . Then, by method of trial and error the pattern was indexed
as illustrated, validated with equation (6). By equation (7) this corresponds to a zone
axis [111].

Figure 1: Diraction pattern image 1, with miller indexes

In the second diraction image, gure 2, the fact that cos 12 = 0 equation (6)
gives the only options h1 k1 l1 =[111], [111], [111] and [111]. Again, by trial and error
using equation (5) the indexes were calculated as illustrated in gure... Then the zone
axis was evaluated to [211].

Measurement of real space distance between lattice planes for

a specic crystal orientation
As we see on the HR image, in gure 3, a hexagonial pattern is evident, pointing
toward the [111] lattice family. On the scale 2 nm = 1.4 cm, the distance between
2nm
points in the image was measured to be B = 0.15 1.4cm
, which by equation (2) gives
a real space distance d = 1.853 .

Figure 2: Diraction pattern image 2, with miller indexes, a 2-dim square Bravais lattice

Figure 3: High resolution mode image, illustrating hexagonial symmetry

Discussion
As a comparison to the measured value of d, by the given values of the lattice parameters a = b = c = 5.431 , the real space distances; d111 = 3.136 , d022 = 1.920 ,

Figure 4: BF- TEM image, illustrating oxidation of sample edges

d113 = 1.638 . Thereby we would expect to be looking at the [022]-family, which ts

with the chosen indexing of the diraction pattern.

In gure 4 the edges of the sample is displaying a dark rim. It is suscpected that
this is due to oxidation of the silicone, resulting in a disoriented atomic array close to
the edges. Further, in the indexing of the cubic diraction pattern, index 222 is seen
as an incident of double diraction, due to relative large thickness of the sample.

Conclusion
This exercise has contributed to the basic understanding of TEM, and the operations of
an TE- microscope. Also one has undergone training in miller indexing of diraction
patterns from a crystal, and gained an understanting of its theoretical use. The
distance d022 was measured to be 1.853 0.067 , wich may be used to descibe the
cubic lattice parametres a = b = c of the crystal.

References
[1] Hanne Kauko, TFY4220 Solid State Physics: Electron Diraction. NTNU January
24, 2013.
[2] Transmission electron microscope manufacturer FEI, An introduction to
electron microscopy. http://www.fei.com/resources/student-learning/
introduction-to-electron-microscopy/intro.aspx
[3] Wikipedia, Transmission electron microscopy. http://en.wikipedia.org/wiki/
Transmission_electron_microscopy
[4] Wikipedia, Crystal structure. http://en.wikipedia.org/wiki/Crystal_
structure