采用有机合成的方法制备配位化合物FeSe2粉末,然后将该前驱粉末在650℃下真空环境退火得到β-FeSe0.93粉末,经烧结最终制得具有超导性能的FeSe0.93体材料.采用扫描电镜、X射线衍射及能谱仪对两种粉末进行了成分和形貌分析,结果表明,化学合成得到的FeSe2粉末颗粒呈八面体状,粒度均匀,尺寸约0.5 μm.而FeSe2粉末经高温退火后发生分解,铁硒比随着硒单质的逸出而增大,最终获得粉末成分为FeSe0.93,颗粒发生融合使得粒度增大,由于分解反应的无序性使得产物中有少量的非超导相(α-FeSex).粉末经压制成锭后750℃下烧结,对FeSe0.93粉末制块材进行了超低温下电输运测量的研究,多物性测量系统(PPMS)测试结果表明该体材料初始超导转变温度(Tc,onset)约为11K,同时存在零电阻特性(Tc,0=4 K),超导性能得到较好的表现.因为非超导的杂相存在对铁硒化学计量比产生微扰,没能获得更好的输运测量结果.
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