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Investigation of mechanism for microstructural changes in hard-brittle materials during cyclic nanoindentation (本文)

香西, 孝司 慶應義塾大学

2021.03.23

概要

Extremely hard-brittle materials are used for a wide range of applications. The quality and service life of products are affected by mechanical properties. In addition, the mechanical properties of hard-brittle materials affect their machining processes; hence, it is imperative to investigate the mechanical properties for the optimization of machining conditions. In particular, owing to the development of ultra-precision machining techniques, mechanical properties on the micron/nanoscale become especially important. Meanwhile, in ultra- precision machining processes, it is difficult to precisely investigate the mechanism of microstructural changes in real time. Therefore, the fundamental analysis of microstructural changes in hard-brittle materials is required.

Nanoindentation is a suitable method for the fundamental analysis of the microstructural changes induced by external forces. Nanoindentation tests permit the accurate investigation of the relationship between loads and material responses by the elimination of error factors compared to real machining processes. Although various nanoindentation studies have investigated microstructural changes, most of them focus on the processes occurring during single nanoindentation. Hence, microstructural changes occurring during cyclic loading/unloading processes, which are similar to situations of real material use and machining processes, have not been sufficiently investigated.

In this study, cyclic nanoindentation tests are performed on representative hard-brittle materials of single-crystal germanium, polycrystalline yttria-stabilized zirconia (YSZ), and amorphous fused silica to narrow the gap and clarify the microstructural changes in hard-brittle materials under repetitive loading/unloading processes. By employing various characterization methods such as cross-sectional observation of indents and load-displacement analysis, new microstructural changes are confirmed, which have not been reported in previous single nanoindentation tests, and the mechanism is clarified.

In the multi-cyclic nanoindentation, where the maximum load on each cycle is constant, of single-crystal Ge, its phase transformation behavior exhibits a strong dependence on the holding load between each indentation cycle. Multi-cyclic nanoindentation with a low holding load promotes phase transformation. In contrast, multi-cyclic nanoindentation with a middle holding load considerably prevents phase transformation. Further increase in the holding load toward the maximum load increases the occurrence of phase transformation.

In case of polycrystalline YSZ, multi-cyclic nanoindentation exhibits location-dependent microstructural changes. Phase transformation is promoted around the indent on unloading processes, whereas beneath the indented surface, grain refinement and the extrusion of the refined layer become dominant. In addition, the diamond-turned surface exhibits cyclic-load- induced fracture due to the spalling of the grain-refinement layer formed by machining processes.

For amorphous fused silica, incremental cyclic nanoindentation, where the maximum load on each cycle increases incrementally, using a sharp indenter promotes brittle fracture via lateral cracking. In addition, some characteristic fractures occur, which are not observed in single indentation, such as secondary spalling far from the indent. The mechanism for such a characteristic brittle fracture is explained.

The mechanism of microstructural changes revealed by multi- and incremental cyclic nanoindentation tests in this study provides new insights into the cyclic-load-induced subsurface damage in hard-brittle materials. This study is expected to help clarify the historical effects related to the subsurface damage mechanism of hard-brittle materials caused by cyclic loads in real material use and precision mechanical processing.

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