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[求助]
纳米粒子如何提纯？ 已有1人参与
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| 参照文献合成了一种Ru的纳米粒子，文献报道是说粒径大小在5nm左右，可是我测AFM发现里面有微米级的粒子，也有几百纳米的粒子，就是好几种粒径大小的粒子都有，是不是产物不纯？要怎么提纯得到较小粒径的粒子呢？求解答。。。 |
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4楼2013-12-12 14:38:34
吴国庆
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2楼2013-12-11 23:08:49
3楼2013-12-12 09:04:30
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你好，文献中的合成步骤如下：Alkyne-Stabilized Ruthenium Nanoparticles. In a typical reaction, to a two-neck round-bottom flask under dry nitrogen protection was added 1-octyne (0.14 mL, 0.94 mmol) and THF (5 mL,anhydrous). The solution was cooled to -78°C (acetone/dry ice bath) and stirred prior to the dropwise addition of 2.24 M n-BuLi in hexanes (0.42 mL, 0.96 mmol). The reaction was allowed to stir fo r1hto prepare 1-octynyllithium. In a separate flask, ruthenium chloride predried under a vacuum oven and THF (30mL,anhydrous) was stirred and cooled to -78°C.The ruthenium salt solution was added to the cooled 1-octy-nyllithium solution via cannula, and the resulting mixture was allowed to warm to room temperature over a period of 1 h. A 1.0 M solution of lithium triethylborohydride in hexanes (5.0mL, 5.0 mmol) was added dropwise to the reaction mixture,and the resulting solution exhibited an immediate color change from dark red to dark brown, signifying the formation of Ru nanoparticles. The resulting solution was allowed to stir at room temperature over 3 h. The reaction was cooled with an ice-water bath and quenched with Nanopure water. Solvents were then removed under reduced pressure with a rotary evaporator. The resulting sample was washed several times with copious amounts of ethanol to remove any excess of ligands and other impurities, affording purified nanoparticles (denoted as Ru-OC). The particles were found to be readily soluble in typical apolar solvents such as toluene, THF, chloroform, and dichloromethane, and not soluble in polar solvents such as alcohols, acetone, and acetonitrile. |
5楼2013-12-12 17:02:20
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