A Compact Furnace for Synchrotron Powder Diffraction Experiments up to 1800 K

A new electric furnace has been designed and fabricated for measurements of the high-resolution synchrotron radiation powder diffraction profiles from materials at high temperatures up to 1807 K in air, suitable for the multiple-detector system installed at the BL-4B2 experimental station of the Photon Factory, Tsukuba, Japan. In the present study, at 1703 K in air, the whole powder pattern of National Institute of Standard and Technology ceria powder was step scanned at a step interval of 0.004° in 2θ, by the counting time of 1.5 s/step and with a monochromatized 1.205363(5) A X-ray, in just 7 h. The full width at half-maximum of the 111 reflection of the ceria was narrow (0.0139°). The δd/d resolution of the ceria ranged from 0.058% to 0.126% at 1703 K, where d and δd are the lattice spacing and peak width, respectively. Precise unit-cell parameter 5.51259(1) A and the atomic displacement parameters were refined by the Rietveld analysis of the powder data measured at 1703 K. An electron-density map of ceria at 1703 K was obtained by the maximum-entropy method.

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