1
Contents
Theoretical Basics 2
Experimental setup 5
Carrying out the experiment 6
Analysis 8
Discussion 10
Data sheet 11
2
Basic Theory
X-ray is an electromagnetic radiation with wavelengths between roughly 0.1 and 100,
typically similar to the inter-atomic distances in a crystal. This is convenient as it allows crystal
structures to diffract X-rays.
X-ray diffraction can be used to determine the crystalline structure (i.e. cell parameters, space
group and atomic coordinates) of novel or unknown crystalline materials.
Production and measurement of X-Rays
The laboratory source of X-rays consists of an evacuated tube in which electrons are emitted
from a heated tungsten filament, and accelerated by an electric potential to impinge on a metal
target. When the electrons reach the anode, most of them gradually lose their kinetic energy
during many collisions with the atoms of the anode material. The main part of their kinetic
energy is converted simply into heat, the remaining part is converted into electromagnetic
radiation. The X -rays generated are within a continuous spectrum, the so called
Bremsstrahlung ("white x-ray light") and have wavelengths characteristic of the electronic
levels in the target. A single characteristic radiation is selected using a filter.
Characteristic Radiation
When the energy of the electron beam is above a certain threshold value, called the excitation
potential, an additional set of discrete peaks is observed superimposed on the white radiation
curve. The energies of these peaks are characteristic of the type of the target material (anode).
These peaks are generated by a two-stage process. First an electron from the filament collides
with and removes a core electron from an atom of the target. Then an electron in a higher
energy state "drops down" to fill the lower energy, vacant hole in the atom's structure, emitting
an X-ray photon. These emitted X-ray photons have energies that are equal to the difference
between the upper and lower energy levels of the electron that filled the core hole. The
excitation potential for a material is the minimum energy needed to remove the core electron.
The characteristic lines in an atom's emission spectra are called K, L, M ... and correspond to the
n = 1, 2, 3 ... quantum levels of the electron energy states, respectively. When the two atomic
energy levels differ by only one quantum level then the transitions are described as lines (n =
2 to n = 1, or n = 3 to n = 2). When the two levels are separated by one or more quantum levels,
the transitions are known as lines (n = 3 to n = 1 or n = 4 to n = 2).
3
Figure 1. Characteristic radiation from an X-ray generator.
Figure 2. Electronic energy levels of an atom of the anode.
The characteristic spectrum is thus generated according to the energy levels of the atoms of the
anode material. Both frequency and/or wavelength of these x-ray lines depend on the square of
the atomic number Z of the considered element. For the K
o
line the eq.
v
Ko
=
3/4 (Z - o)
2
Ry , o=1 (Mosleys law)
holds with the Rydberg frequency Ry = 3.29 . 10
15
s
-1
.
Geiger-Muller tube
X rays are detected using a Geiger-Muller tube. A GM tube consists of a very fine central
anode (steel wire) and an insulated shell, which serves as the cathode. The region surrounding
the anode is filled with an inert gas, usually argon or neon, specially selected for the ease with
which it can be ionized and some additional alcohol vapour. A high electrical field is maintained
between the electrodes. The sensitive volume is the portion surrounding the anode responding
to the specific radiation. If the x-rays traverse the tube, they ionize single gas atoms, and the
electrons are accelerated toward the center wire causing more ionization on their way resulting
finally into a complete discharge of the tube (limited in time by the alcohol vapor). The
discharge current across the resistor generates a voltage pulse which is counted.
4
Figure 3. Geiger-Muller tube
Braggs reflection of X- rays
Braggs law of reflection describes the diffraction of plane waves at a monocrystal as the
selective reflection of the waves at a set of lattice planes within the crystal. Due to the
periodicity of the crystal, the lattice planes of a set have a fixed spacing d. An incident wave
with the wavelength is reflected with maximum intensity when the Bragg condition is
fulfilled.
n = 2d sinu
n
, (n = 1, 2, 3...) Braggs law
The "reflection" of radiation at atoms is actually a scattering and an interference process. The
electronic shells (-Ze) of every atom of the crystal subjected to the field of the electromagnetic
radiation are forced to vibrate around the nuclei (+Ze)and thereby emit radiation with the same
frequency as the incoming radiation inalmost all directions. This radiation is intensified by
constructive interference at angles given according to Braggs Law and annihilated at other
angles.
Using Bragg's law one can determine the spacing d of an unknown lattice if the wavelength of
the monochromatic x-ray beam is known, or vice versa , if the lattice spacing d of the crystal is
known.
Figure 4. Braggs reflection
5
Experimental Setup
The x-ray tube T is mounted under a lead glass screening dome within a round experimental
chamber. Having passed through the aperture A, the x-ray beam is incident on the NaCl crystal
Cr (in the center of the apparatus) at an angle u with the crystal surface (parallel to the Bragg
planes). The beam reflected at the angle 2u passes a nickel filter F and enters the detector D.
Both u and 2u are selected by a movable arm on which the detector is mounted. The intensity of
the reflected x-ray beam is monitored by a pulse counter PC with start and stop switches and a
reset button. For acoustic monitoring of the pulses, a small loudspeaker is attached. Since the
intensity of the x-ray beam is very low, the screening of the experimental chamber by a
lead/aluminum plate and the Plexiglas cover is sufficient t o avoid any personal hazard due to
ionizing effects of the primary and scattered beams. The apparatus can be operated only if the
cover is closed. A red lamp indicates the status of operation (high voltage switched on).
6
Carrying out the experiment
At first, the pulse rate (s
-1
) corresponding to the intensity of the background radiation is to be
determined using a counting time of 100 s while the apparatus is switched off. This rate is
subtracted from the rates determined later. In the following, the rate N (2u) is to be measured in
the range 20
o
< 2u < 120
o
,starting at small angles and increasing 2u u sing intervals of 4
o
at a
time. For a more accurate determination of the Bragg angles u
1
, u
2
, N(2u) is determined within
a second run at increasing angles in the close vicinity of the rate maxima observed before, but
now, using smaller intervals of angles (2u = 2
o
; 1
o
; ....).
Background radiation at 100 seconds: 21
Background radiation pulse per second: 0.21 s
-1
Background radiation pulse per 20 seconds (N
0
) ~ 4
Angle (2u) Angle (u) Pulse rate, N (20
sec)
N - N
0
(20 sec) N - N
0
(s
-1
) to
nearest integer
20 10 24
20 1
24 12 68
64 3
28 14 160
156 7
31 15.5 6173
6169 308
31.5 15.75 16720
16716 835
32 16 2069
2065 103
32.5 16.25 480
476 23
33 16.5 418
414 20
36 18 349
345 17
40 20 264
260 13
44 22 184
180 9
48 24 97
93 4
52 26 64
60 3
56 28 58
54 2
60 30 53
49 2
64 32 124
120 6
65.5 32.75 6171
6167 308
7
66 33 6403
6399 319
66.5 33.25 1345
1341 67
67 33.5 284
280 14
67.5 33.75 136
132 6
68 34 111
107 5
72 36 86
82 4
76 38 70
66 3
80 40 59
55 2
84 42 43
39 1
88 44 50
46 2
92 46 41
37 1
96 48 42
38 1
100 50 44
40 2
104 52 36
32 1
108 54 70
66 3
109 54.5 440
436 21
109.5 54.75 1819
1815 90
110 55 1584
1580 79
110.5 55.25 363
359 17
111 55.5 127
123 6
111.5 55.75 69
65 3
112 56 64
60 3
116 58 51
47 2
120 60 49
45 2
8
Analysis
-100
0
100
200
300
400
500
600
700
800
900
0 10 20 30 40 50 60 70
N - N
N - N
9
From the maxima at
n
, (n =1, 2, 3), the Bragg plane distance d
n
is calculated using Braggs
equation with = 154 pm for the Cu Ko. radiation
d
n
= n / (2 sin (u
n
))
Braggs plane distance d
1
= 2.837 x 10
-10
m
(u = 15.75
o
)
Braggs plane distance d
2
= 2.828 x 10
-10
m
(u = 33
o
)
Braggs plane distance d
3
= 2.829 x 10
-10
m
(u = 54.75
o
)
Average Braggs plane distance, d = 2.831 x 10
-10
m
Bragg plane distance from literature, d
NaCl
= 2.820 x 10
-10
m
Deviation, A = , d - d
NaCl
| / ( d
NaCl
)
= 3.9 x 10
-3
= 0.39 %
Uncertainty in measurement of angle :
Combining Braggs equations, you get :
= 1
/ 2sinu
1
= 1
/ sinu
2
= 3
/ 2sinu
3
Therefore :
sinu
2
/ sinu
1
= 2
sinu
3
/ sinu
1
= 3
sinu
3
/ sinu
2
= 3/2
But the values from the recorded data =
sinu
2
/ sinu
1
= 2.00648 Au = 0.00648
sinu
3
/ sinu
1
= 3.00855 Au = 0.00855
sinu
3
/ sinu
2
= 1.49942 Au = 0.00058
Average Au = 0.005
Hence the uncertainty in measurement of angle = 0.5%
Total uncertainties = 0.5% + 0.39%
= 0.89%
Therefore Braggs plane distance for NaCl = 2.831 x 10
-10
m +- 0.89%
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Discussion
Possible errors:
- Uncertainty in the angle measured
- Possibility of a peak at an angle between the measured peak angle
- Not able to stop the counter at exactly 20 seconds
- Only one set of data per angle measured, including background radiation
Safety:
- Do not open the X- ray apparatus while it is turned on. Radiation hazard
- High voltages
