Rapid, In-Situ, Ultra-High Temperature Investigations of Ceramics using Synchrotron X-Ray Diffraction

In situ studies of oxidation of ZrB2 and ZrB2–SiC composites at high temperatures

“…Plate samples of ZrB 2 and ZrB 2 -SiC composites were heated to T set = 1100 • C in ∼5 minutes, and several HTXRD patterns were acquired over the next ∼1 h duration while the samples were maintained at the T set temperature. Based on prior experience and the location of the control thermocouple (which measures T set ) in the QLF, the sample temperature (T sample ) during these studies was expected to be in the range 1200-1350 • C. [32][33][34][35]37 This temperature was selected for the isothermal studies as it corresponded to oxidizing conditions in a partial protective regime for the materials being evaluated. Therefore, it was anticipated that a pronounced effect of the presence of SiC on oxidation of ZrB 2 could be suitably observed.…”

“…Contingent upon sample properties and incident X-ray beam intensity, high resolution XRD patterns can be acquired in ≤20 s using this detector. 37 For the purpose of this study, the CIP detector was first aligned and calibrated using a Si(1 1 1) analyzer crystal and the LaB 6 powder standard (SRM 660a, National Institute of Standards and Technology, Gaithersburg, MD, USA). Incident monochromatic X-rays of wavelength 0.70087 Å, as calibrated with SRM 660a, were used in this work.…”

“…A specially designed quadrupole lamp furnace (QLF), which allows heating of samples up to 2000 • C in air, [32][33][34][35] was used in conjunction with a high resolution curved image plate (CIP) detector for these studies. 36,37 Using this method, the oxidation of ZrB 2 to ZrO 2 was monitored in real time, independent of other accompanying processes.…”

Effect of transition-metal-ion doping on high temperature thermal expansion of 3:2 mullite—An in situ, high temperature, synchrotron diffraction study

“…The details of the construction, operation and capabilities of the CIP detector are reported elsewhere. 39,40 The CIP detector was aligned and calibrated using a Si(1 1 1) analyzer crystal and the LaB 6 powder standard for XRD (SRM 660a, National Institute of Standards and Technology, Gaithersburg, MD). Incident monochromatic X-rays of two different wavelengths, 0.550784Å and 0.563084Å, as calibrated with SRM 660a, were used in this work.…”

Growth of textured mullite fibers using a quadrupole lamp furnace

“…The details of the experimental apparatus and detector information have been reported in other papers. [18][19][20][21][22] The primary objective of this research was to investigate the possibility of producing single crystal or textured fibers of mullite by controlled texturing or crystallization of polycrystalline or amorphous fibers as precursors. In order to produce textured fibers by extrusion, the use of mullite whiskers as templates was investigated.…”