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High-Temperature Furnaces for X-Ray Diffractometers

Published online by Cambridge University Press:  06 March 2019

William J. Campbell,
Stephan Stecura and
Clark Grain
William J. Campbell
Affiliation:
Bureau of Mines, U.S. Department of the Interior, Metallurgy Research Center, College Park, Maryland
Stephan Stecura
Affiliation:
Bureau of Mines, U.S. Department of the Interior, Metallurgy Research Center, College Park, Maryland
Clark Grain
Affiliation:
Bureau of Mines, U.S. Department of the Interior, Metallurgy Research Center, College Park, Maryland
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Abstract

This paper summarizes developments in the field of high-temperature X-ray diffractometers through 1959, evaluates various furnace designs, and describes briefly the X-ray diffraction facilities of the Federal Bureau of Mines.

X-ray optics, for those furnaces that have precision sample movements, are equivalent in resolution and line profile to conventional X-ray techniques. There is a 10-25% loss of intensity due to absorption of X-rays in the furnace windows, magnitude of which depends on wavelength and type of window used, and a reduction (5–40° 2θ) of useful angular range from limiting X-ray windows, radiation shielding, or the viewport for an optical pyrometer. In oxidizing atmospheres, temperatures up to 1500°C were obtained with furnaces wound with platinum—20% rhodium wire. Under nonoxidizing conditions temperatures of 1800 to 2000°C were obtained with both tantalum-foil and tungsten-wire heaters.

Accurate temperature measurement over the area and depth of samples being studied is the most difficult problem in high-temperature X-ray diffractometry. Below 500°C, there are several furnace designs which are reported to reduce thermal differentials to less than 1°C across the sample. However, at temperatures around 1000°C, there are thermal gradients of 20-30°C/cm across the sample and 100–600°C/cm through the sample holder, making thermocouple location critical. Secondary standards have been used extensively to calibrate the furnaces; however, there is disagreement concerning which are the most reliable data to use. For these reasons, plus others discussed in this report, there is a probable error in the temperature determination of ±10 to 20°C at 1000°C, with the error increasing with temperature.

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Type
Research Article
Information
Advances in X-Ray Analysis , Volume 5: Tenth Annual Conference on Applications of X-ray Analysis, August 7-9, 1961 , 1961, pp. 169 - 190
Copyright
Copyright © International Centre for Diffraction Data 1961

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References

*1. Goldschmidt, H. J., “High Temperature Methods,” in X-Ray Diffraction by Polycrystalline Methods, The Institute of Physics, London, H. S. Peiser et al. (eds.) 1955, p. 242.Google Scholar
*2. Schossberger, F., “High-Temperature X-Ray Diffraction,” in I. E. Campbell (ed.), High Temperature Technology, John Wiley and Sons, New York, 1956, p. 490.Google Scholar
*3. Mauer, F. A. and Bolz, L. H., “Measurement of Thermal Expansion of Cermet Components by High Temperature,”Google Scholar
(a) X-Ray Diffraction: Nai, Bur. of Standards Kept. 3148, 1953, 39 pp.;Google Scholar
(b) X-Ray Diffraction: Nat. Bur. of Standards Kept. 4685, 1956, 11 pp.;Google Scholar
(c) X-Ray Diffraction: WADC Tech. Rept, 55-473, 1955, 57 pp.;Google Scholar
(d) X-Ray Diffraction: WADC Tech. Rept. 55-473, Supp. No, 1, 1957, 47 pp.Google Scholar
*4. Moore, A., “The Application of High-Temperature X-Ray Diffractometer Methods to Solid-State Transformations,” PhD Thesis, University of Birmingham, Birmingham, England, 1955.Google Scholar
*5. Williamson, G. K. and Moore, A., “A Precision High-Temperature Specimen Chamber for an X-Ray Diffractometer,” J. Sci, Instr., Vol. 33, 1956, p. 107.Google Scholar
*6. Birks, L. S., “Apparatus for X-Ray Diffraction Studies of Metals Under Controlled Stress ar Elevated Temperatures,” Rev. Sci. Instr., Vol. 25, 1954, p. 963.Google Scholar
*7. Sowrnan, H. G. and Andrews, A. I., “A Study of the Phase Relations of ZrO2-TiO2 and ZrO2-TiO2-SiO2” J. Am. Ceram. Soc, Vol. 34, 1951, p. 298.Google Scholar
*8. Parker, H., Engineering Ceramics Section, Mineral Products Division, National Bureau of Standards, Washington, D. C, private communication, August 1959.Google Scholar
*9. Kruh, R. F., Department of Chemistry, University of Arkansas, Fayetteville, Ark., private communication, September 1959.Google Scholar
10. Priddis, J. E., “The Design of Platinum-Wound Electric Resistance Furnaces,” Platinum Metals Rev., Vol. 2, 1958, p. 38.Google Scholar
11.Anon., “The Construction of Laboratory Electric Furnaces,” Norton Company, Worcester, Mass, 34 pp.Google Scholar
*12. McKinstry, H. A., Tem-Pres Inc., Box 146N. Atherton Street, State College, Pa., private communication, July 1959.Google Scholar
*13. Ichlkawa, Y., “Construction of a High-Temperature X-Ray-Diffraction Furnace and Studies of Several Reactions at Elevated Temperatures,” M. S. Thesis, New York State College of Ceramics, Alfred, N. Y., 1954.Google Scholar
*14. Kennedy, S. W. and Calvert, L. D., “An Oxidizing Atmosphere Furnace for Use with an X-Ray Diffractometer,” J. Sci, Instr., Vol. 35, 1958, p. 61.Google Scholar
*15. Bassetc, W. A. and Lapham, D. M., “A Thermal-Increment Diffractometer,” Am. Mineralogist, Vol. 42, 1957, p. 548.Google Scholar
*16. Rowland, R. A., Weiss, E. J., and Lewis, D. R., “Apparatus for the Oscillating-Heactng Method of X-Ray Powder Diffraction,” J. Am. Ceram. Soc Vol. 42, 1959, p. 133.Google Scholar
*17. Wood, E. A., “Heated Sample Holder for X-Ray Diffractometer Work,” Rev. Sci. Instr., Vol. 27, 1956, p. 60.Google Scholar
18. Sherwood, E. M., “Metals,” in I. E. Campbell (ed.), High-Temperature Technology, John Wiley and Sons, New York, 1956, p. 17.Google Scholar
19. Wehrmann, R., “Oxidation Resistant Coatings for Molybdenum,” Fansteel Met., November 1956, p. 2.Google Scholar
*20. Perri, J. A., Banks, E., and Post, B., “Study of Phase Transitions in WO3 With a High-Temperature X-Ray Diffractometer,” J. Appl. Phys., Vol. 28, 1957, p, 1272.Google Scholar
21. Bradshaw, W. G. and Matthews, C. O., ‘Properties of Refractory Materials, Collected Data and References,” LMSD-2466, Lockheed Aircraft Corp., Sunnyvale, Calif., 1959, 106 pp.Google Scholar
22.Anon., “AlSiMag Chart No. 591,” American Lava Corporation, Chattanooga, Tenn.Google Scholar
23.Anon., “KT Silicon Carbide,” Advanced Materials Technol., Vol, 1, 1957, p. 2.Google Scholar
24. Campbell, I. E., Rosenbaum, D. M. and Gonser, B. W., “The Availability, Recovery and Properties of Rhenium Metal,” J. Less-Common Metals, Vol. 1, 1959, p. 185.Google Scholar
*25. Birks, L. S. and Friedman, H., “A High-Temperature X-Ray Diffraction Apparatus,” Naval Research Laboratory Rep. N-3081, 1947, 8 pp.Google Scholar
*26. Corvin, L., Schossberger, F. V., and Ticulka, F. A., Armour Research Foundation, Illinois Institute of Technology, Chicago, 111. Proposed Paper “High-Teraperature Attachment for X-Ray Diffractometer,” January 1960, 12 pp.Google Scholar
*27. McKeand, I. J. and Hursti, R. K., “Tungsten-Colt Furnace for High-Temperature X-Ray Diffraction Investigations,” J. Am. Ceram. Soc., Vol. 35, 1955, p. 63.Google Scholar
*28. Das, D. K. and Pitman, D. T., “A Vacuum High-Temperature X-Ray effraction Furnace for the X-Ray Diffractometer,” Pittsburgh Diffraction Conf. November 1959.Google Scholar
*29. Chiotti, P., “Adaption of a Geiger Counter X-Kay Diffrac tome ter for High-Temperature Investigations,” Rev. Sci. Instr., Vol. 25, 1954, p, 683.Google Scholar
*30.Anon., “High-Temperature X-Ray Diffraction Camera,” Johnston, Inc. WADC Tech. Rept. 57-667, 1957, 14 pp.Google Scholar
31. Goode, J. M., Physics Division, Wright Air Development Center, Wright-Patterson Air Force Base, Ohio, private communication, October 1959.Google Scholar
*32. Klein, D. J., “Measurement of the Cry stallographic Thermal Expansion of Alpha -Alum in a and Beryllia to Elevated Temperatures Emphasizing Anisotropic Effects,” NAA-SR-2542, Atomics International, P. O. Box 309, Canoga Park, Calif., 1958, 24 pp.Google Scholar
33. Holzboclc, W. G.. Automatic Control, Principles and Practice, Reinhold Publishing Corporation, New York, 1958, 258 pp.Google Scholar
*34. Spreadborough, J. and Christian, J. W., “High-Temperature X-Ray Diffractometer,” J. Sci. Instr., Vol. 36, 1959, p. 116.Google Scholar
35. Pearson, W. B., Handbook of Lattice Spacing and Structures of Metals and Alloys, Pergamon Press, New York, 1958, 1044 pp.Google Scholar
36. Brand, J. A. and Goldschmidt, H. J., “The Temperature Calibration of a High-Temperature X-Ray Diffraction Camera,” J. Sci. Instr., Vol. 33, 1956, p. 41.Google Scholar
37. Keder, R. and Nowick, A., “Use of Thermal Expansion Measurements to Dstect Lattice Vacancies near the Melting Point of Pure Lead and Aluminum,” Phys. Rev., Vol. 109, 1955, p. 1959.Google Scholar
38. Kelly, H. J. and Harris, H. M., “An Automatically Recording Thermal-Expansion Apparatus,” J. Am. Ceram. Soc Vol. 39, 1956, p. 344.Google Scholar
39. Whittemore, O. J. and Ault, N. N., “Thermal Expansion of Various Ceramic Materials up to 1500°C,” J. Am. Ceram. Soc. Vol. 39, 1956, p. 443.Google Scholar
40. Beals, R. J. and Cook, R. L., “Directional Dilatation of Crystal Lattices at Elevated Temperatures,” J. Am. Ceram. Soc, Vol. 40, 1957, p. 279.Google Scholar
41. Austin, J. B., “The Thermal Expansion of Some Refractory Oxides,” J. Am. Ceram. Soc, Vol. 14, 1931, p. 795.Google Scholar
*42. Parrish, W. and Lowitzsch, K., “Geometry, Alignment and Angular Calibration of X-Ray Diffractometers,” Am. Mineralogist, Vol. 44, 1959, p. 765.Google Scholar
43. Wilson, A. J. C., “Geiger-Counter X-Ray Spectrometer—Influence of Size and Absorption Coefficient of Specimen on Position and Shape of Powder-Diffraction Maxima,” J. Sci. Instr., Vol. 27, 1950, p. 321.Google Scholar
*44. Butters, R. G. and Parr, J. G., “A High-Temperature X-Ray Goniometer,” Can. J. Technol., Vol. 33, 1955, p, 117.Google Scholar
*45. Van Valkenburg, A. Jr. and McMurdie, H. G., “High-Temperature X-Ray Diffraction Apparatus,” J. Nad. Bur. Standards U. S., Vol. 38, 1947, p. 415.Google Scholar
*46. Johnson, J. R. and White, G. D., “Note on a High-Temperature Attachment for an X-Ray Spectrometer,” J. Am. Ceram. Soc, Vol. 39, 1956, p. 227.Google Scholar