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Substructure Measurements by Statistical Fluctuations in X-Ray Diffraction Intensity

Published online by Cambridge University Press:  06 March 2019

E. F. Sturcken ,
W. E. Gettys  and
E. M. Bohn
E. F. Sturcken
Affiliation:
E. I.du Pont de Nemours & Co. Aiken, South Carolina
W. E. Gettys
Affiliation:
E. I.du Pont de Nemours & Co. Aiken, South Carolina
E. M. Bohn
Affiliation:
E. I.du Pont de Nemours & Co. Aiken, South Carolina
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Abstract

The substructures of a bet a-quenched and a recrystallized form of high-purity uranium were measured by a method based on statistical fluctuations in X-ray diffraction intensity. For these measurements, Warren's statistical equation for determining grain size was modified to make the equation applicable to materials with high absorption coefficients or moderate-to-large grain size ( > 20 microns) or both, since many metals fall into this category, and to allow for defocusing of the X-ray beam which occurs as a natural consequence of the experiment.

The beta-quenched uranium was found to have numerous subgrains with a range of misorientation angles that was smaller and larger than the limits of the X-ray measurements (Ω = 10−4 to 10−2 steradians). The presence of the large subgrains was corroborated by optical microscopy. The presence of very small subgrains was corroborated by transmission electron microscopy which showed 0.1- to 1-micron subgrains relatively free of dislocations bounded by dense dislocation networks, and by micro Laue diffraction patterns (30-micron beam diameter) which showed partial rings similar to a powder pattern.

The recrystallized uranium had no misorientation within the grains greater than 5.5 × 10−3 steradians. In contrast to the beta-quenched case, no subgrains were found either by transmission electron microscopy (TEM) or micro Laue diffraction patterns. The TEM micrographs showed a uniform distribution of dislocation networks. Since no other substructural elements were observed, the dislocations are believed to be the cause of the misorientation within the grains for solid angles of less than 5 × 10−3 steradiflns.

These preliminary experiments show that the statistical method may be used in conjunction with transmission electron microscopy and micro Laue diffraction for the study of substructure. The statistical method gives quantitative data on “bulk” specimens that can be given a meaningful interpretation with the aid of the other techniques.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 9: Fourteenth Annual Conference on Applications of X-ray Analysis, August 25-27, 1965 , 1965 , pp. 74 - 90
Copyright
Copyright © International Centre for Diffraction Data 1965

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References

1. Warren, B. E., “X-Ray Measurements of Grain Size,” J. Appl. Phys. 31: 2237–2239, 1960.Google Scholar
2. Barrett, C. S., Structure of Metals, McGraw-Hill Book Company, Inc., New York, 1952, Chapter V.Google Scholar
3. Taylor, A., X-Ray Metallography, John Wiley & Sons, Inc., New York, 1961, Chapter 14.Google Scholar
4. Hirsch, P. B. and Kellar, J. N., “A Study of Cold-Worked Aluminum by an X-Ray Micro-Beam Technique. II. Measurement of Particle Volume and Misorientations,Acta Cryst. 5: 162, 1952.Google Scholar
5. Hirsch, P. B., “A Study of Cold-Worked Aluminum by an X-Ray Micro-Beam Technique. II. Measurement of Shapes of Spots,” Acta Cryst. 5: 168, 1952.Google Scholar
6. Hirsch, P. B., “The Reflection and Transmission of X-Rays in Perfect Absorbing Crystals,” Acta Cryst. 5: 176, 1952.Google Scholar
7. Hirsch, P. B., “Mosaic Structures,” in: B. Chalmers and R. King (eds.), Progress in Metal Physics, Vol. 6, Pergamon Press Ltd., London and New York, 1956, pp. 236–339.Google Scholar
8. Barrett, C. S., “Determining Recrystallization by a Diffractometer Technique,” in: J. B. Newkirk and J. H. Wernick (eds.), Direct Observations of Imperfections in Crystals, Interscience Publishers, Inc., New York, 1962, p. 395.Google Scholar
9. Barrett, C. S., “X-Ray Diffraction Studies at Low Temperatures,” in: W. M. Mueller, G. R. Mallett, and M. J. Fay (eds.), Advances in X-Ray Analysis, Vol. 5. Plenum Press, New York, 1961, p. 33.Google Scholar
10. Sturcken, E. F. and Croach, J. W., “Predicting Physical Properties in Oriented Metals,” Tram. AIME 227: 934–940, 1963.Google Scholar
11. Sturcken, E. F. and Gettys, W. E., Determination of Grain Sise in Uranium from Statistical Fluctuations in X-Ray Diffraction Intensity, E. I. du Pont de Nemours and Co., DP-904, July 1964.Google Scholar
12. Angerman, C. L., “Transmission Electron Microscopy of Uranium.” J. Nucl. Mater. 9: 109–110, 1963.Google Scholar
13. Crank, N. and Thudium, R. N., Effects of Etching on Preferred Orientation Measurements, Hanford Atomic Products Operation, HW-74429, August 1962.Google Scholar
14. Margenau, H. and Murphy, G. M., The Mathematics of Physics and Chemistry, D. Van Nostrand Company, Inc., New York, 1943, pp. 422–425.Google Scholar
15. Seeman, H., Ann. Physik 59: 455, 1919.Google Scholar
16. Eohlin, H., Ann. Phytik 61: 421, 1920.Google Scholar
17. Ogilvie, R. E., Stress Measurement with the X-Ray Spectrometer, M.S. Thesis, Department of Metallurgy, MIT, 1952.Google Scholar
18. Schwartz, M., J. Appl. Phys. 26: 1507, 1955.Google Scholar