激波等离子法制备纳米氧化锆及表征
发布时间:2018-04-10 02:34
本文选题:激波等离子 切入点:负氧平衡炸药 出处:《中北大学》2011年硕士论文
【摘要】:采用激波等离子法制备了高纯纳米多晶氧化锆粉末。借助热重分析(TG-DTA)、煅烧试验研究了气相氧化温度对最终粉体性能的影响,通过x衍射、拉曼光谱、透射电镜(TEM)等手段对前驱体和最终产品的性能进行了表征,探讨了制备过程中团聚控制机理。结果表明:激波等离子体法通过对粉体生长时间的控制,实现了对超微粉体高温制备过程中团聚的控制,不同的煅烧温度对最终产物的相组成影响较大,而对颗粒的尺寸影响较小,通过调整煅烧温度,可以控制最终粉体的相组成,所制备出粉末为纳米四方/单斜氧化锆多晶,纯度高,分散性好,粒径范围在11.5nm~16.55nm。 主要研究工作和成果如下: 1).设计了TNT与锆源的混合药柱以爆轰的方式合成纳米氧化锆,初步证明了激波等离子法合成纳米氧化物技术路线和研究方法。 2).采用激波等离子制备技术实现了对粉体生长时间的控制,达到了对超微粉体高温制备过程中团聚的控制。制备出的前驱体为单质碳微粒和纳米ZrO_2的混合颗粒粉末,颗粒尺寸在10 nm左右呈球形,ZrO_2的主体相为四方相。 3).气相氧化可有效地去除前驱体中单质碳微粒,不同的煅烧温度对最终产物的相组成影响较大,而对颗粒的尺寸影响较小,600℃~800℃条件下,得到的最终粉体粒径范围在11.5nm~16.55nm,为四方相和单斜相的混晶,通过调整煅烧温度,可以改变最终粉体的晶相组成。
[Abstract]:High purity polycrystalline zirconia powder was prepared by shock plasma method.The influence of gas phase oxidation temperature on the properties of the final powder was studied by means of TG-DTAC, and the properties of the precursor and the final product were characterized by means of x diffraction, Raman spectroscopy and transmission electron microscopy (TEM).The agglomeration control mechanism in the preparation process was discussed.The results show that the shock wave plasma method can control the agglomeration during the preparation of ultrafine powder at high temperature by controlling the growth time of the powder. Different calcination temperature has a great influence on the phase composition of the final product.By adjusting the calcination temperature, the phase composition of the final powder can be controlled. The prepared powder is a nanometer tetragonal / monoclinic zirconia polycrystal with high purity and good dispersion. The particle size ranges from 11.5 nm to 16.55 nm.The main research work and results are as follows:1.A hybrid column of TNT and zirconium source was designed to synthesize nano-zirconia by detonation. The technical route and research method of preparing nano-oxide by shock wave plasma method were preliminarily proved.2.The shock wave plasma technology was used to control the growth time of the powder and to control the agglomeration during the preparation of ultrafine powder at high temperature.The precursor is a mixed particle powder of single carbon particle and nanometer ZrO_2. The particle size is about 10 nm and the main phase of ZZrO _ 2 is tetragonal.Three.Gas phase oxidation can effectively remove the single carbon particles from the precursor. The phase composition of the final product is greatly affected by different calcination temperatures, but the effect on the particle size is smaller at 600 鈩,
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