An investigation of the long-range and local structure of sub-stoichiometric zirconium carbide sintered at different temperatures

Rana, Dhan-sham B. K. and Solvas, Eugenio Zapatas and Lee, William E. and Farnan, Ian (2020) An investigation of the long-range and local structure of sub-stoichiometric zirconium carbide sintered at different temperatures. Scientific Reports, 10 (1). ISSN 2045-2322 DOI https://doi.org/10.1038/s41598-020-59698-6

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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.

Item Type:	Article
Uncontrolled Keywords:	2019AREP, IA76
Subjects:	03 - Mineral Sciences
Divisions:	03 - Mineral Sciences 07 - Gold Open Access 12 - PhD
Journal or Publication Title:	Scientific Reports
Volume:	10
Identification Number:	https://doi.org/10.1038/s41598-020-59698-6
Depositing User:	Sarah Humbert
Date Deposited:	24 Feb 2020 11:11
Last Modified:	24 Feb 2020 11:11
URI:	http://eprints.esc.cam.ac.uk/id/eprint/4632

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