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帝国小经营家金虫 (小有名气)
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[求助]
求助：{010} and {110}晶面的钒酸铋（BiVO4）合成 已有1人参与
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| 我根据“Spatial separation of photogenerated electronsand holes among {010} and {110} crystal facets of BiVO4”这篇论文的合成方法，合成BiVO4.具体合成方法如下：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. 但是得到的形貌与论文相差甚远，不知道哪个环节出问题。现有几个疑问，望大牛们解答：1.调节 pH到2的过程中，我使用pH计边搅拌边测量，是否需要配合精密pH试纸精准控制？ 2.调节完pH后，我是直接将沉淀溶液转移到反应釜进行水热反应，而论文中是“orange precipitate at the bottom of the beaker was transferred to a Teflon-lined stainless steel autoclave”，是否需要将沉淀过滤，去除溶液水分，然后转移至反应釜进行反应？或者是存在其他合成过程中需要特别注意的问题，希望大牛们能指点一二，感谢！！！！！！ |
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