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feiler

新虫 (初入文坛)

[求助] 两相法合成3nm左右金颗粒

最近合成3nm左右 Au颗粒,用的是两相法,参考文献如下:
Synthesis of Au nanoparticles. Typically, 20 ml of 5 mM HAuCl4 aqueous solution was mixed with 10 ml of 25 mM TOAB in toluene. After the Au precursor was transferred to the toluene layer, the toluene layer was mixed with 0.202 g dodecylamine in 5ml toluene. Then, 0.054 g NaBH4 in 3 ml H2O was added to the mixture with vigorous stirring. The mixture turned brown indicating the formation of Au nanoparticles. Au nanoparticles were precipitated from toluene by adding ethanol followed by centrifugation. The nanoparticles were redispersed in 10
ml hexane. For this particular procedure, the Au nanoparticles were about 3 nm in diameter, with nearly spherical shape.
Nano Lett., 2006, 6 (4), pp 875–881
问题是:每次拿出来转到离心管里还分散性好,但离心下来就团聚了,分也分不开,我已经注意控制转速了。而且即使加硫醇超声也分散不了了。  这种两相法合成应该很成熟了啊, 求问做过的XDJM们怎么回事啊?你们都怎么操作的,还是文献中把有些关键性步骤省略掉了????  要奔溃了
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feiler

新虫 (初入文坛)

引用回帖:
3楼: Originally posted by 星汉纳米 at 2012-08-30 08:37:53
先看看TEM是否是3nm的Au颗粒。若不是,先改进实验方法,是3nm以后再来研究分离纯化。

分散不好 看TEM 不好点样
6楼2012-08-30 11:12:35
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feiler

新虫 (初入文坛)

另: 我加硼氢化钠后,剧烈搅拌了 20 min, 然后才加乙醇离心的。
2楼2012-08-20 21:34:03
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星汉纳米

禁言 (小有名气)

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3楼2012-08-30 08:37:53
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bachier

金虫 (职业作家)

【答案】应助回帖

为啥非要用两相法,单相可能会更好些。
4楼2012-08-30 09:17:02
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