Stress-induced microcrack density evolution in β-eucryptite ceramics: Experimental observations and possible route to strain hardening

B. R. Müller, R. C. Cooper, A. Lange, A. Kupsch, M. Wheeler, M. P. Hentschel, A. Staude, A. Pandey, A. Shyam, G. Bruno

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Abstract

In order to investigate their microcracking behaviour, the microstructures of several β-eucryptite ceramics, obtained from glass precursor and cerammed to yield different grain sizes and microcrack densities, were characterized by laboratory and synchrotron x-ray refraction and tomography. Results were compared with those obtained from scanning electron microscopy (SEM). In SEM images, the characterized materials appeared fully dense but computed tomography showed the presence of pore clusters. Uniaxial tensile testing was performed on specimens while strain maps were recorded and analyzed by Digital Image Correlation (DIC). X-ray refraction techniques were applied on specimens before and after tensile testing to measure the amount of the internal specific surface (i.e., area per unit volume). X-ray refraction revealed that (a) the small grain size (SGS) material contained a large specific surface, originating from the grain boundaries and the interfaces of TiO2 precipitates; (b) the medium (MGS) and large grain size (LGS) materials possessed higher amounts of specific surface compared to SGS material due to microcracks, which decreased after tensile loading; (c) the precursor glass had negligible internal surface. The unexpected decrease in the internal surface of MGS and LGS after tensile testing is explained by the presence of compressive regions in the DIC strain maps and further by theoretical arguments. It is suggested that while some microcracks merge via propagation, more close mechanically, thereby explaining the observed X-ray refraction results. The mechanisms proposed would allow the development of a strain hardening route in ceramics.

Original languageEnglish
Pages (from-to)627-641
Number of pages15
JournalActa Materialia
Volume144
DOIs
StatePublished - Feb 1 2018

Funding

Microtensile testing and sample machining were made possible by the U.S Department of Energy, Office of Fossil Energy, Solid State Energy Conversion Alliance (SECA) Program. Research also partially sponsored by the U.S. Department of Energy , Assistant Secretary for Energy Efficiency and Renewable Energy, Office of Vehicle Technologies, as part of the Propulsion Materials Program. The authors thank James E. Webb of Corning Inc. for supplying the uncerammed glass for this study and sharing the devitrification procedures. Authors thank Thomas R. Watkins (ORNL) for reviewing the manuscript.

FundersFunder number
SECA
Solid State Energy Conversion Alliance
U.S Department of Energy
U.S. Department of Energy
Office of Fossil Energy
Office of Energy Efficiency and Renewable Energy
Vehicle Technologies Office

    Keywords

    • Beta-eucryptite
    • Microcracked ceramics
    • Strain hardening
    • Tensile load
    • X-ray refraction

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