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作 者:杨博 郝清滨[2] 肖鹏[1] 刘国庆[2] 焦高峰[2] 姚凯[2] 徐晓燕[2] 崔利军[2] 张胜楠[2] 李成山[2] 冯建情[2] Yang Bo;Hao Qingbin;Xiao Peng;Liu Guoqing;Jiao Gaofeng;Yao Kai;Xu Xiaoyan;Cui Lijun;Zhang Shengnan;Li Chengshan;Feng Jianqing(School of Materials Science and Engineering,Xi’an University of Technology,Xi’an 710048,China;Northwest Institute for Nonferrous Metal Research,Xi’an 710016,China)
机构地区:[1]西安理工大学材料科学与工程学院,陕西西安710048 [2]西北有色金属研究院,陕西西安710016
出 处:《稀有金属材料与工程》2023年第9期3163-3169,共7页Rare Metal Materials and Engineering
基 金:国家重点研发计划(2021YFB3800201,2017YFE0301402);陕西省科技重大专项(2020zdzx04-04-02);国家自然科学基金(52277029,52002333);中国科学院战略性先导科技专项(XDB250020200)。
摘 要:采用喷雾热分解法制备了Bi_(2)Sr_(2)CaCu_(2)Ox(Bi-2212)初级粉末,系统地研究了热处理温度对粉末成相和性能的影响。使用TG-DSC分析初级粉末的失重和相变情况,采用XRD分析粉末的相组成,通过SEM观察粉末的微观形貌,采用磁化法对样品的超导物理性能进行判定。结果发现,535~570℃,喷雾热分解初级粉末中的硝酸盐残留物逐渐分解;605~640℃,Bi-2201相形成;温度达到775℃时,Bi-2212相开始形成,随热处理温度的提高,粉末结晶度持续增加,Bi-2212相含量先增加后减少,860℃是最佳的成相烧结温度。另外,通过对DSC曲线和M-T曲线的深入分析发现,先进行640℃的低温预分解,再进行860℃的高温成相烧结,可进一步改善最终粉末的质量。Bi_(2)Sr_(2)CaCu_(2)Ox(Bi-2212)primary powder was prepared by spray pyrolysis method.The effect of heat treatment temperature onpowderphase formation and properties was studied.The mass loss and phase transformation of the primary powder were analyzed by TG-DSC,thephasecomposition of the powder was analyzed by XRD,the microstructure of the powder was observed by SEM,and the superconductingphysical properties of the samples were determined by the magnetization method.It is found that at 535-570°C,the nitrate residues in the primarypowderof spray pyrolysis gradually decompose;the Bi-2201 phase is formed at 605-640°C;when the temperature reaches 775°C,the Bi-2212phasebegins to form.With the increase in heat treatment temperature,the crystallinity of the powder continues to increase,and the content of Bi-2212phase first increases and then decreases.The best phase-forming sintering temperature is 860°C.In addition,through the in-depth analysis of theDSC curve and the M-T curve,it is found that the schedule of low-temperature pre-decomposition at 640°C followed by high-temperaturephase-forming sintering at 860°C can further improve the quality of the powder.
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