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[求助]
兩相法合成3nm左右金顆粒
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最近合成3nm左右 Au顆粒,用的是兩相法,參考文獻(xiàn)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 問題是:每次拿出來(lái)轉(zhuǎn)到離心管里還分散性好,但離心下來(lái)就團(tuán)聚了,分也分不開,我已經(jīng)注意控制轉(zhuǎn)速了。而且即使加硫醇超聲也分散不了了。 這種兩相法合成應(yīng)該很成熟了啊, 求問做過的XDJM們?cè)趺椿厥掳?你們都怎么操作的,還是文獻(xiàn)中把有些關(guān)鍵性步驟省略掉了???? 要奔潰了 |
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