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[求助]
ZnO纳米粒子的合成 已有2人参与
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我最近按照文献合成氧化锌纳米颗粒,参照文献如下,但是清洗沉淀后,加入氯仿和氯苯得不到透明的溶液,是白色乳浊液,而且容易沉淀,求原因,谢谢! 参考文献如下: Waldo J. E. Beek, Martijn M. Wienk, Martijn Kemerink. Hybrid zinc oxide conjugated polymer bulk heterojunction solar cells. J. Phys. Chem. B, 2005, 109: 9505-9516 制备方法: ZnO Nanoparticles Synthesis:zinc acetate dihydrate (Acros,98%, 2.95 g, 13.4 mmol) was dissolved in methanol (125 mL)at 60 °C, a solution of KOH (Merck, 87%, 1.48 g, 23 mmol) inmethanol (65 mL) was added in 10 min to the zinc acetate dihydrate solution under vigorous stirring. Zinc hydroxides precipitated but dissolved again. After 5 min, the solution became translucent and remained translucent. After 1.5 h, the nanoparticles started to precipitate and the solution became turbid. After 2 h and 15 min, the heater and stirrer were removed and the nanoparticles were allowed to precipitate for an additional 2 h. Precipitate and mother liquor were separated, and the precipitate was washed twice with methanol (50 mL). After the washing steps (5 min), the suspension was left unstirred for a minimum of1hto reach full precipitation. The washed precipitate was treated with chloroform or chlorobenzene (10mL) to dissolve the nanoparticles. This solution was only slightly translucent, almost transparent, and was stable for more than two weeks. The amount of methanol in the resulting solution was determined with 1H NMR. Replacing the last washing step with a centrifugation step (4300 rpm, 5 min) decreased the amount of methanol with a factor 2. [ Last edited by sddtc888 on 2013-8-8 at 23:04 ] |
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