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小木蟲論壇-學術科研互動平臺 » 化學化工區(qū) » 電化學 » 其它 » 鉀固態(tài)電解質(zhì)合成方法
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[求助]
鉀固態(tài)電解質(zhì)合成方法
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 本人想做鉀固態(tài)電解質(zhì)合成，文獻中給的合成方法如下：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. 整個反應在惰性氣體保護下進行，因為涉及到高活性鉀單質(zhì)，所以只能在手套箱中做嗎？可以先在手套箱中用 DEA 把鉀溶解后再拿出來，在Schlenk 中反應可以嗎？求大神指教 |
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