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X-ray Diffraction

  

Points to ponder:

How are the x-rays generated?
Give a diagram of the machine and a description of how it works.
Why are there two peaks for some orders?  Whay do they only show up at large diffraction angles?
Why do the peaks for graphite appear so different from the peaks for tungsten?
Why, in the electron diffraction experiment, do we only get two peaks? Which ones are they?  Do we see them with the X-rays?

You will want to determine values such as

d- spacings
Unit cell size
Crystal type
Atomic size
Density
The location of the next peak

(For a NYT article, you may not need to calculate all of these values, depending on the focus of your report).

References:

Kingery, Bowen, Uhlmann, Introduction to Ceramics, excerpt.
ASM, Metals Handbook.
Kittel, Charles, Solid State Physics, excerpt.
Trigg, Landmark Experiments in 20th Century Physics, "The Wave Nature of X-rays."
Atkins, Physical Chemistry. (Useful for background and has a good description of spin-orbital coupling).
Zumdahl, Introduction to Chemistry. A good introductory chemistry text.
CRC Press, Handbook of Chemistry and Physics.

 

Data Analysis


For your data analysis, you should probably download the full size image (in Adobe Acrobat format) and print them out:
Tungsten diffraction graph.
Graphite diffraction graph, filtered.
Graphite diffraction graph.

 

Tungsten


Scan Parameters

Search Parameters

Radiation CU 1.54059 Filter length (pts) 9
Scan Range 35 - 120 (2theta.gif (975 bytes)) Noise level (sigmas) 5.0
Step Size 0.05 Intensity Cutoff (%) 0.5-100
Count Time 1 s 2theta.gif (912 bytes) zero 0

 

Peak Data (Extracted from the graph)
# 2theta.gif (912 bytes)
(Peak)
2theta.gif (912 bytes)
(Centroid)
d
spacing
Local Bkgrd Peak Height % of max Area
% of max FWHM
1 40.246 40.244 2.xxx 26 100070 100.0 2518 100.0 0.225
2 58.206 58.232 1.xxx 28 2053 20.4 618 24.5 0.271
3 73.107 73.115 1.xxx 38 4670 46.4 1223 48.6 0.236
4 86.905 86.909 1.xxx 34 1517 15.1 409 16.2 0.243
5 87.185 87.175 1.xxx 33 819 8.1 238 9.5 0.262*
6 100.510 100.530 1.xxx 36 2183 21.7 736 29.2 0.303
7 100.850 100.845 0.xxx 37 1266 12.6 448 17.8 0.318
8 114.797 114.812 0.xxx 30 699 6.9 245 9.7 0.315
9 115.209 115.203 0.xxx 36 354 3.5 151 6.0 0.384*

* - Likely Kalpha.gif (913 bytes),2 peaks.

 

Tungsten X-ray Line card

JCPDS-ICDD PDF-2, Sets 1-45.  (Quality: *)
Swanson, Tatge, NIST Circ. 529, 1 28 (1953)
Radiation Cu Kalpha.gif (913 bytes)1  dA  Int.  h k l
Lambda 1.54505  2.238  100  1 1 0
System Cubic  1.582  15  2 0 0
Molecular Wt. 183.85  1.292  23  2 1 1
a 3.1648  1.1188  8  2 2 0
 1.0008  11  3 1 0
Color Gray metallic 0.9137  4  2 2 2
CAS # 7440-33-7 0.8459  18  3 2 1
Merck Index 8th ed. p. 1087 0.7912  2  4 0 0
Pattern @ 26C.  Sample prepared at Westinghouse Electric Corp.  Analysis of sample showed SiO2 0.04%, K 0.05%, Mo and Al2O3 0.01%.

 

TungstenFull.gif (34178 bytes)


Graphite

  

Scan Parameters

Search Parameters

Radiation CU 1.54059 Filter length (pts) 9
Scan Range 20 - 90  (2theta.gif (975 bytes)) Noise level (sigmas) 5.0
Step Size 0.05 Intensity Cutoff (%) 0.5-100
Count Time 1 s 2theta.gif (912 bytes) zero 0

 

Peak Data (Extracted from the graph)
# 2theta.gif (912 bytes) (Peak) 2theta.gif (912 bytes) (Centroid) D spacing Local Bkgrd Peak Height % of max Area
% of max FWHM
1 26.494 26.465 3.xx 116 6299 100.0 3960 100.0 0.566
2 35.043 35.020 2.xx 54 123 2.0 37 0.9 0.271
3 42.825 42.325 2.xx 161 123 2.0 29 0.7 0.212
4 43.898 43.902 2.xx 144 158 2.5 145 3.7 0.826
5 54.499 54.496 1.xx 117 418 6.6 310 7.8 0.667
6 61.752 61.758 1.xx 99 75 1.2 23 0.6 0.276
7 73.003 72.984 1.xx 63 73 1.2 18 0.5 0.22
8 77.398 77.403 1.xx 80 352 5.6 197 5.0 0.504
9 83.501 83.500 1.xx 110 211 3.3 120 3.0 0.512
10 86.718 86.720 1.xx 116 36 0.6 8 0.2 0.200

* - Likely Kalpha.gif (913 bytes)2 peaks.

Carbon (Graphite) X-ray Line card

JCPDS-ICDD PDF-2, Sets 1-45.  (Quality: C)  dA  Int.  h k l
Holcombe, Private Communication, 1974  3.348  100  0 0 3
 2.081  11  1 0 1
Radiation Cu Kalpha.gif (913 bytes)  1.958  9  0 1 2
System Rhombohedral (Hex)  1.674  6  0 0 6
Molecular Wt. 12.01  1.623  4  1 0 4
Lambda 1.54178  1.460  2  0 1 5
a, b 2.456  1.228  4  1 1 0
c 10.044  1.190  1  1 0 7
1.153  6  1 1 3
1.116 1 0 0 9
1.081 1 0 1 8
0.9902 4 1 1 6
0.8370 1 0 0 12
0.8259 4 1 1 9
0.8014 1 2 1 1
0.7938 1 1 2 2

GraphiteFiltered.gif (24351 bytes)

GraphiteFull.gif (19114 bytes)

 

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