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作 者:李良 陈玉奇 朝仓贵一 平井伸治 Li Liang;Chen Yuqi;Asakura Kinyichi;Hirai Shinji(School of Mechanical and Electrical Engineering,Nanyang Normal University,Nanyang,Henan,China;School of Materials Science and Engineering,Shanghai University of Electrical Engineering,Shanghai,,China;School of Engineering,Muroran University of Technology,Muroran,Hokkaido,Japan)
机构地区:[1]南阳师范学院机电工程学院,河南南阳473061 [2]上海电机学院材料学院,上海201306 [3]室兰工业大学工学院,北海道室兰079-1100
出 处:《矿产综合利用》2021年第2期37-43,共7页Multipurpose Utilization of Mineral Resources
基 金:河南省自然科学基金青年基金项目;河南省留学归国人员科技活动项目(208007);南阳师范学院博士专项(2019ZX018)。
摘 要:采用辉锑矿为原料成功制备出Cu_(12)Sb_(4)S_(13)块体。研究以Sb_(2)S_(3)矿物为原料时烧结工艺对Cu_(12)Sb_(4)S_(13)合成的影响。在400~440℃温度区间内均可快速合成Cu_(12)Sb_(4)S_(13)块体且二次烧结能够进一步减小中间相CuSbS_(2)和Cu_(3)SbS_(3)。第二相Cu_(3)SbS_(4)和残留相CuS随着烧结时间的延长而降低。二次烧结前进行机械化球磨处理,干磨比湿磨更容易减小残留相。初次烧结块体的断面SEM和EDS能谱分析表明内部存在Cu或Cu_(2)S颗粒团聚现象。适当降低Cu或CuS摩尔量(化学计量比0.1 mol)能促进烧结块表面反应进行。烧结过程中,硫磺蒸汽压的导致烧结块表面成分和内部粉末的成分不同。Stibnite mineral Sb_(2)S_(3)was employed as starting material for the synthesis of tetrahedrite Cu_(12)Sb_(4)S_(13)bulks by pulse electric sintering.The influences of sintering conditions(temperature and time),secondary sintering,ball milling on the preparation of Cu_(12)Sb_(4)S_(13)compacts were systematically investigated.Highly pure Cu_(12)Sb_(4)S_(13)can be quickly obtained by the optimized sintering condition.Cu_(12)Sb_(4)S_(13)can be synthesized rapidly in the temperature range of 400~440℃,and the secondary sintering can further reduce the mesophases CuSbS_(2)and Cu_(3)SbS_(3).The second phase Cu_(3)SbS_(4)and the residual phase CuS decrease with the increase of sintering time.It is easier to reduce the residual phase in dry grinding than in wet grinding.SEM and EDS analysis of the primary sintering bulk show that there is agglomeration of Cu or Cu_(2)S particles in the matrix.Properly reducing the molar amount of Cu or CuS(stoichiometric ratio 0.1 mol)can promote the surface reaction of agglomerates.In the sintering process,the sulfur vapor pressure results in the difference between the surface composition and the inner composition.
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