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linxiaoxia

金虫 (初入文坛)

[求助] 纳米粒子如何提纯? 已有1人参与

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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吴国庆

金虫 (小有名气)

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【答案】应助回帖

感谢参与,应助指数 +1
你的情况是单分散性不好,可以试试用油胺或油酸钠做分散剂试试,祝成功。
努力奋斗,不然别人看不起!
2楼2013-12-11 23:08:49
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linxiaoxia

金虫 (初入文坛)

引用回帖:
2楼: Originally posted by 吴国庆 at 2013-12-11 23:08:49
你的情况是单分散性不好,可以试试用油胺或油酸钠做分散剂试试,祝成功。

你好,我整个合成过程都没用到分散剂,之前也没有做过类似的实验,没什么经验。。。想问下分散剂在什么时候加入呢?是在配成溶液后再加入吗?而且我合成的粒子只溶于极性较小的有机溶剂如二氯甲烷等。。。
3楼2013-12-12 09:04:30
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吴国庆

金虫 (小有名气)

平静

【答案】应助回帖

引用回帖:
3楼: Originally posted by linxiaoxia at 2013-12-12 09:04:30
你好,我整个合成过程都没用到分散剂,之前也没有做过类似的实验,没什么经验。。。想问下分散剂在什么时候加入呢?是在配成溶液后再加入吗?而且我合成的粒子只溶于极性较小的有机溶剂如二氯甲烷等。。。...

你用的什么方法?
努力奋斗,不然别人看不起!
4楼2013-12-12 14:38:34
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linxiaoxia

金虫 (初入文坛)

引用回帖:
4楼: Originally posted by 吴国庆 at 2013-12-12 14:38:34
你用的什么方法?...

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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吴国庆

金虫 (小有名气)

平静

【答案】应助回帖

不好意思,咱们做得方法不一样,爱莫能助啊
努力奋斗,不然别人看不起!
6楼2013-12-12 23:13:39
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linxiaoxia

金虫 (初入文坛)

引用回帖:
6楼: Originally posted by 吴国庆 at 2013-12-12 23:13:39
不好意思,咱们做得方法不一样,爱莫能助啊

还是谢谢哈
7楼2013-12-18 09:15:47
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