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Synthesis of AlN Powder by Carbothermal Reduction-Nitridation of Various Al_2O_3 Powders with CaF_2

机译:CaF_2碳热还原氮化处理各种Al_2O_3粉体的合成AlN粉

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The effect of Al_2O_3, properties on the synthesis of AlN powder by the carbothermal reduction-nitridation method with CaF_2 addition was investigated. Four types of Al_2O_3 powders, one type prepared by the Bayer method and three types prepared by the Alkoxide methods, were compared in this work. An Al_2O_3/C molar ratio of 0.29 was selected. The amount of CaF_2 powder added was adjusted to 3wt%. The carbothermal reduction-nitridation was carried out at 1400 and 1450°C in N_2 flow. Nitridation rate tended to increase with decreasing particle size of raw Al_2O_3, and also to depend on synthesizing method of Al_2O_3. The raw Al_2O_3 powder made by the Bayer method was confirmed to form CaF_25·Al_2O_3, as an intermediate. In contrast the intermediates could not be detected by XRD in powders made by the Alkoxide method. The reason is not clear. Particle sizes of the products increased somewhat with increasing reaction temperatures. However, even though different particle sizes of Al_2O_3 powders were used, AlN powders synthesized under the same condition showed nearly equal particle size with round shape and narrow size distribution. This phenomenon suggests that the controlling step determining the size and shape is in the reduction -nitridation process of the intermediate compounds.
机译:研究了添加CaF_2的碳热还原-氮化方法对Al_2O_3性能的影响。在这项工作中,对四种类型的Al_2O_3粉末进行了比较,一种是通过Bayer方法制备的,另一种是通过醇盐方法制备的。选择的Al_2O_3 / C摩尔比为0.29。将CaF_2粉末的添加量调整为3重量%。碳热还原氮化在N_2流中于1400和1450°C进行。随生Al_2O_3颗粒尺寸的减小,氮化率趋于增加,并且取决于Al_2O_3的合成方法。确认通过拜耳法制得的粗Al_2O_3粉末形成CaF_25·Al_2O_3作为中间体。相反,通过烷氧基化法制得的粉末中的XRD无法检测到中间体。原因尚不清楚。随着反应温度的升高,产物的粒度略有增加。然而,即使使用不同粒径的Al_2O_3粉末,在相同条件下合成的AlN粉末也显示出几乎相等的粒径,具有圆形和窄的粒径分布。该现象表明,确定尺寸和形状的控制步骤是在中间体化合物的还原-氮化过程中。

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