In Situ Growth of a Novel Nanoscaled Rock Salt Titanium Zirconium Nitride Phase in a Silicon Nitride Matrix

M. Bechelany, Abhijeet Lale, Maxime Balestrat, C. Gervais, S. Malo, R. Nishihora, S. Bernard
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Abstract

The first demonstration of a nanoscaled titanium zirconium nitride (TiZrN2) single-phase isolated during the formation of precursor-derived silicon nitride (Si3N4) matrix nanocomposites is highlighted in the present paper. We employed polymethylsilazane (PMSZ) as a Si3N4 precursor, which was chemically modified with Zr[N(CH2CH3)2]4 and Ti[N(CH3)2]4, ammonolyzed and pyrolyzed under ammonia (1000 °C) then annealed in flowing nitrogen (1500 °C). The TiZrN2 phase grew in the temperature range 1000-1500 °C and was isolated - because of its confinement into a Si3N4matrix - as a nanoscaled rock salt structure after annealing at 1500 °C as shown by X-ray diffraction. HRTEM investigations confirmed the unique nanostructural feature of the nanocomposites made of TiZrN2 nanocrystals with a size as low as 9 nm distributed in a- and b-Si3N4 phases.
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新型纳米岩盐氮化钛锆相在氮化硅基体中的原位生长
本文首次展示了在前驱体衍生的氮化硅(Si3N4)基纳米复合材料形成过程中分离出的纳米级氮化钛锆(TiZrN2)单相。以聚甲基硅氮烷(PMSZ)为Si3N4前驱体,用Zr[N(CH2CH3)2]4和Ti[N(CH3)2]4进行化学改性,在氨水(1000℃)下进行氨解和热解,然后在流动氮(1500℃)中进行退火。x射线衍射显示,TiZrN2相在1000 ~ 1500℃的温度范围内生长,并在1500℃退火后被隔离为纳米级岩盐结构,因为它被限制在si3n4基体中。HRTEM研究证实了由尺寸低至9 nm的TiZrN2纳米晶体组成的纳米复合材料的独特纳米结构特征,这些纳米晶体分布在a-和b-Si3N4相中。
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