24小时热门版块排行榜    

CyRhmU.jpeg
查看: 350  |  回复: 0
【悬赏金币】回答本帖问题,作者_alphazgy将赠送您 5 个金币

_alphazgy

新虫 (初入文坛)

[求助] 钾固态电解质合成方法

本人想做钾固态电解质合成,文献中给的合成方法如下:The synthesis of the K3SbSe4or Ba-doped K3SbSe4 was carried out in EDA. Typically, 58.5 mg K (1.5 mmol) was dissolved in 5 mL EDA with the formation of a deep  blue  solution.  Elemental  Se  and  Sb  were  added  to  the  above  deep  blue  solution  in  a stoichiometric  proportion  of  K:  Sb:  Se  =  3:1:4.  After  addition,  the  mixture  was  stirred  at  room temperature for 12 hours and then heated at 100 °C for another 12 hours.Theentirereaction was conducted under an inert atmosphere. The solvent was then removed, and the obtained powder was dried under vacuum at 120 °C for 24 hours. The Ba-doped K3SbSe4samples can be prepared in a similar procedure mentioned above just by partially replacing quantitative K with Ba. The synthesized powder after removing EDA solvent was ground for 10 mins and cold-pressed into a pellet. The sample pellet was placed inside a quartz tube under an Ar flow, which was heated to 300 °C for 2 hours, kept at 300°C for 12 hours, and cooled down naturally to room temperature. 整个反应在惰性气体保护下进行,因为涉及到高活性钾单质,所以只能在手套箱中做吗?可以先在手套箱中用 DEA 把钾溶解后再拿出来,在Schlenk 中反应可以吗?求大神指教
回复此楼
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖
相关版块跳转 我要订阅楼主 _alphazgy 的主题更新
不应助 确定回帖应助 (注意:应助才可能被奖励,但不允许灌水,必须填写15个字符以上)
信息提示
请填处理意见