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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.

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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