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帝國小經營家金蟲 (小有名氣)
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[求助]
求助:{010} and {110}晶面的釩酸鉍(BiVO4)合成 已有1人參與
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| 我根據(jù)“Spatial separation of photogenerated electronsand holes among {010} and {110} crystal facets of BiVO4”這篇論文的合成方法,合成BiVO4.具體合成方法如下:All chemicals were analytical grade and were used without further purification. BiVO4 sample was synthesized by a hydrothermal procedure. Typically, the precursors NH4VO3 (36 mmol) and Bi(NO3)3·5H2O (36 mmol) were dissolved in 300 mL of 2.0 M nitric acid solution, and the pH value of the solution was then adjusted to 2.0 with ammonia solution under stirring until formation of an orange precipitate. After about 2 h aging, the orange precipitate at the bottom of the beaker was transferred to a Teflon-lined stainless steel autoclave with a capacity of 100 mL and hydrothermally treated at 200 oC for 24 h. After the autoclave was cooled to room temperature, a vivid yellow powder was separated by filtration, washed with de-ionized water for more than 3 times, and then dried at 60 oC in air for overnight. 但是得到的形貌與論文相差甚遠,不知道哪個環(huán)節(jié)出問題,F(xiàn)有幾個疑問,望大牛們解答:1.調節(jié) pH到2的過程中,我使用pH計邊攪拌邊測量,是否需要配合精密pH試紙精準控制? 2.調節(jié)完pH后,我是直接將沉淀溶液轉移到反應釜進行水熱反應,而論文中是“orange precipitate at the bottom of the beaker was transferred to a Teflon-lined stainless steel autoclave”,是否需要將沉淀過濾,去除溶液水分,然后轉移至反應釜進行反應?或者是存在其他合成過程中需要特別注意的問題,希望大牛們能指點一二,感謝。。。。! |
至尊木蟲 (著名寫手)

鐵蟲 (初入文壇)
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