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小木虫论坛-学术科研互动平台 » 材料区 » 微米和纳米 » 合成表征 » 纳米棒合成pH值调节问题
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一一8778

铜虫 (小有名气)

[求助] 纳米棒合成pH值调节问题

目前有俩篇文献提到了氧化钨纳米棒的合成。方法如下：
1、WO 3 nanorods were synthesized by the recently reported hydrothermal process with (NH 4 ) 2 SO 4  as a capping agent 。 In a typical synthesis, Na 2 WO 4 · 2H 2 O (0.6597 g,) and (NH 4 ) 2 SO 4 (0.5286 g, Sigma-Aldrich) were dissolved in deionized water (15 mL), then HCl (3 M ) aqueous solution was added to adjust the pH value to 2.0. The solution obtained was transferred into a Tefl onlined stainless autoclave where the reaction was maintainedat 180 ° C for 8 h. Then the precipitate was isolated by fi ltration 。
2、WO3 nanowire arrays were synthesized by a sulfate-assisted hydrothermal method. Briefly, 3.29 g sodium tungstate powder was dissolved in 76 ml de-ionized water, and a 3MHCl aqueous solution was used to adjust the pH value to 2.0. Afterwards,ammonium sulfate (2.64 g) was added to the reaction precursor
to control the morphology of the WO3 product. After stirring for 1 h, the clear solution obtained was transferred into a Teflonlined stainless autoclave. The FTO-coated glass with the WO3 seed layer was placed vertically in the autoclave, and then the autoclave was sealed and heated at 180 C for 4 h. The obtained film with a thickness of 1.5 mm was washed and dried in a vacuum oven at 60 C for 12 h.

在这两种方法中，调节pH值一个在ammonium sulfate加入后，一个在其加入前，这样的结果会有区别吗？
另外无机纳米材料的合成重复性很poor吗？还是文章中的条件存在一定的玄机？

[ Last edited by 一一8778 on 2013-6-20 at 14:27 ]
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1楼 2013-06-20 14:26:22
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004411cyy

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根据目前文章的形势来看，大部分的精华，尤其是实验步骤的关键点，都被作者握在手里，藏在心里，所以很多条件不可能完全模拟重复得来~~
关于顺序滴加不同，再水热中影响还是蛮大的。也看到有文章，用氯化钠作为导向剂合成纳米棒的~~
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2楼2014-06-30 20:33:20
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