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An Investigation of the Long-Range and Local Structure of Sub-Stoichiometric Zirconium Carbide Sintered at Different Temperatures

An Investigation of the Long-Range and Local Structure of Sub-Stoichiometric Zirconium Carbide Sintered at Different Temperatures

Dhan-Sham B K Rana, Eugenio Zapatas Solvas, William E Lee, Ian Farnan

Sci Rep. 2020 Feb 20;10(1):3096.

PMID: 32080236

Abstract:

ZrC1-x (sub-stoichiometric zirconium carbide), a group IV transition metal carbide, is being considered for various high temperature applications. Departure from stoichiometry changes the thermo-physical response of the material. Reported thermo-physical properties exhibit, in some cases, a degree of scatter with one likely contributor to this being the uncertainty in the C/Zr ratio of the samples produced. Conventional, methods for assigning C/Zr to samples are determined either by nominal stochiometric ratios or combustion carbon analysis. In this study, a range of stoichiometries of hot-pressed ZrC1-x were examined by SEM, XRD, Raman spectroscopy and static 13C NMR spectroscopy and used as a basis to correct the C/Zr. Graphite, amorphous, and ZrC1-x carbon signatures are observed in the 13C NMR spectra of samples and are determined to vary in intensity with sintering temperature and stoichiometry. In this study a method is outlined to quantify the stoichiometry of ZrC1-x and free carbon phases, providing an improvement over the sole use and reliance of widely adopted bulk carbon combustion analysis. We report significantly lower C/Zr values determined by 13C NMR analysis compared with carbon analyser and nominal methods. Furthermore, the location of carbon disassociated from the ZrC1-x structure is analysed using SEM and Raman spectroscopy.

Chemicals Related in the Paper:

Catalog Number	Product Name	Structure	CAS Number	Price
AP12070143	Zirconium(IV) carbide		12070-14-3	Price

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