Y_2O_3纳米颗粒催化氮化Si粉制备Si_3N_4粉体
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摘要
以聚乙二醇为表面活性剂,以氨水为沉淀剂,先采用沉淀法将氧化钇(Y_2O_3)纳米颗粒催化剂原位沉积于Si粉表面,再通过催化Si粉氮化工艺制备Si_3N_4粉体。研究了催化剂Y_2O_3的用量及氮化温度等对Si_3N_4粉体合成的影响。采用X射线衍射、扫描电子显微镜及能谱仪对产物的物相组成及显微结构进行了表征。结果表明:当Y_2O_3纳米颗粒的加入量为1%(质量分数,下同)时,试样于1350℃/2 h催化氮化后产物中残余单质Si含量最小,低于1%;氮化后产物中存在着长度约为几个微米,直径在20~200 nm的晶须状Si_3N_4,其生长机理主要为气相-气相-固相(VVS)机理。
Using PEG as surfactant and NH_3·H_2O as precipitant,Y_2O_3 nanoparticle(NP)catalysts were homogeneously deposited on the surface of Si powders by an in-situ precipitation method and Si_3N_4 was then prepared by nitridation of Si powders.The effects of various processing parameters including the amount of catalyst and nitridation temperature on the synthesis of Si_3N_4 powders were investigated.Phase composition and microstructure of the Si_3N_4 were characterized by X-ray diffraction and field emission-scanning electron microscopy equipped with EDS,respectively.The results show that when the sample is nitrided at 1350℃/2 h with 1 wt%of Y_2O_3 NPs as catalysts,the residual Si content in the final sample is less than 1wt%.Many of Si_3N_4 whiskers with 20~200 nm in diameter and several microns in length form in the final products.Vapor-vapor-solid(VVS)growth mechanism is responsible for the growth of Si_3N_4 whiskers.
Using PEG as surfactant and NH_3·H_2O as precipitant,Y_2O_3 nanoparticle(NP)catalysts were homogeneously deposited on the surface of Si powders by an in-situ precipitation method and Si_3N_4 was then prepared by nitridation of Si powders.The effects of various processing parameters including the amount of catalyst and nitridation temperature on the synthesis of Si_3N_4 powders were investigated.Phase composition and microstructure of the Si_3N_4 were characterized by X-ray diffraction and field emission-scanning electron microscopy equipped with EDS,respectively.The results show that when the sample is nitrided at 1350℃/2 h with 1 wt%of Y_2O_3 NPs as catalysts,the residual Si content in the final sample is less than 1wt%.Many of Si_3N_4 whiskers with 20~200 nm in diameter and several microns in length form in the final products.Vapor-vapor-solid(VVS)growth mechanism is responsible for the growth of Si_3N_4 whiskers.
引文
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