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Crystallization behaviour of Yb-doped and undoped YAG nanoceramics synthesized by microwave-assisted urea precipitation

机译:微波辅助尿素沉淀法合成掺Yb和掺YAG纳米陶瓷的结晶行为

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摘要

Yb-doped and undoped Y_3Al_5O_(12) (YAG) nanometric powders were synthesized by microwave assisted liquid synthesis from nitrate precursors and calcination. The homogeneous and rapid heating of the reaction volume of this synthesis process allowed a precise control on particle nucleation and growth and the formation of nanometric primary particles with a narrow size distribution. The chemical composition of synthesized powders was checked by ICP and FTIR analysis. The morphology of the precursor and calcined powders as well as the microstructurc after sintering were analysed by SEM. High temperature XRD and TG-DTA analyses, performed in the 800-1200 ℃ range, with two temperature ramps, made it possible for a thorough investigation of the crystallization behaviour of YAG and Yb: YAG precursors. The results show that the crystallization of Yb:YAG from the powder precursors started at 900 ℃ and that both the presence of Yb and a high heating rate accelerate the YAG formation through the intermediate YAH (hexagonal YAlO_3 phase). The intermediate phases Y_4Al_2O_9 (YAM) and YAlO_3 (YAP) that are generally observed during the calcination step of nanometric YAG powder did not form. Pellets of pressed powders were sintered under high vacuum in clean atmosphere at 1700 ℃ for 16 h and a full density translucent material with grain size from 3 to 5 was obtained.
机译:通过硝酸盐前驱体的微波辅助液相合成和煅烧,合成了掺Yb和未掺杂Y_3Al_5O_(12)(YAG)纳米粉末。对该合成过程的反应体积进行均匀且快速的加热,可以精确控制颗粒的成核和生长以及形成具有窄尺寸分布的纳米级初级颗粒。通过ICP和FTIR分析检查合成粉末的化学组成。通过SEM分析了前体和煅烧粉末的形态以及烧结后的微观结构。在800-1200℃范围内进行的高温XRD和TG-DTA分析具有两个温度梯度,这使得有可能彻底研究YAG和Yb:YAG前体的结晶行为。结果表明,Yb:YAG从粉末前体开始在900℃结晶,并且Yb的存在和较高的加热速率都加速了YAG通过中间YAH(六方YAlO_3相)的形成。没有形成在纳米YAG粉末的煅烧步骤中通常观察到的中间相Y_4Al_2O_9(YAM)和YAlO_3(YAP)。在高真空下于1700℃的清洁气氛中将压制成粉的颗粒烧结16 h,得到粒度为3至5的全密度半透明材料。

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