β-SiC粉体中常见金属杂质的亚临界水热去除工艺  

Subcritical Hydrothermal Removal of Common Metal Impurity in β-SiC Powder

作　　者：王波 段晓波[1,2,3] 邓丽荣 王嘉博[1,2,3] 陆树河 王晓刚[1,2,3] WANG Bo;DUAN Xiaobo;DENG Lirong;WANG Jiabo;LU Shuhe;WANG Xiaogang(College of Materials Science and Engineering,Xi’an University of Science and Technology,Xi’an 710000,China;Shaanxi Engineering Research Center of Energy Saving and Polygeneration in Silicon and Magnesium Industry,Xi’an 710000,China;Xianyang Industrial Technology Research Institute of New Energy Materials,Xianyang 712000,China)

机构地区：[1]西安科技大学材料科学与工程学院,西安710000 [2]陕西省硅镁产业节能与多联产工程技术研究中心,西安710000 [3]咸阳新能源材料产业技术研究院,咸阳712000

出　　处：《硅酸盐通报》2021年第8期2713-2718,共6页Bulletin of the Chinese Ceramic Society

基　　金：国家自然科学基金青年科学基金(51602254);陕西省自然科学基础研究计划(2020JQ-737);咸阳市重大科技专项计划(2019K01-13)。

摘　　要：高纯β-SiC粉体作为原料,广泛应用于半导体晶圆、半导体窑具、半导体芯片设备用陶瓷器件等产品。高温高压可以促进水热反应,采用亚临界水热法可去除工业合成β-SiC粉体中的金属杂质。研究不同酸体系下β-SiC粉体中常见金属杂质的去除效果。利用电感耦合等离子原子发射光谱仪(ICP-OES)检测微量元素的含量,通过X射线衍射仪(XRD)和扫描电镜(SEM)对β-SiC粉体的物相组成和微观结构进行表征。结果表明,对于Cr和Zr去除效果较好的是HCl体系,对于Ca、Fe、Mg和Ti去除效果较好的是HCl+HF+HNO_(3)体系,对于Al和K去除效果较好的是H_(2)SO_(4)+(NH_(4))2SO_(4)体系。采用HCl体系处理的最佳反应温度为200℃,采用HCl+HF+HNO 3体系处理的最佳反应温度是220℃,采用H_(2)SO_(4)+(NH_(4))2SO_(4)体系处理的最佳反应温度是200℃。其中,H_(2)SO_(4)+(NH_(4))2SO_(4)体系可将β-SiC粉体中常见金属杂质含量降低至最少(杂质总含量为920.31 mg/L),因此该体系为β-SiC粉体除杂的最优方案。High-purity β-SiC powders are used as raw materials for semiconductor wafers,semiconductor kiln furniture and ceramic devices used in semiconductor chip equipment.A subcritical hydrothermal method was used to remove metal impurities in β-SiC powders synthesized by high-temperature and high-pressure,which promotes the hydrothermal reaction.The removal effect of common metal impurities in β-SiC powders under different acid systems was studied.The content of trace elements was detected by inductively coupled plasma optical emission spectrometry spectrometry(ICP-OES),and the phase composition and microstructure of β-SiC powders were characterized by X-ray diffraction(XRD)and scanning electron microscope(SEM).The results are as follows:the HCl system is better for Cr and Zr removal than the other two;the HCl+HF+HNO_(3) system is better for Ca,Fe,Mg and Ti,and H_(2)SO_(4)+(NH_(4))2SO_(4) system is better for Al and K.The best reaction temperature for treatment with HCl system is 200℃,the best reaction temperature for treatment with HCl+HF+HNO_(3) system is 220℃,and the best reaction temperature for treatment with H_(2)SO_(4)+(NH_(4))2SO_(4) system is 200℃.Among them,H_(2)SO_(4)+(NH_(4))2SO_(4) system reduces the content of common metal impurities in β-SiC powders to the minimum,and the total content of impurities is 920.31 mg/L.Therefore,H_(2)SO_(4)+(NH_(4))2SO_(4) system is the optimal scheme for β-SiC powders impurity removal.

关 键 词：β-SiC粉体 水热法 金属杂质 电感耦合等离子体 提纯 

分 类 号：TQ163[化学工程—高温制品工业]