AlCl_(3)⁃EMIC离子液体中纳米铝粉的制备

Preparation of Nano⁃aluminum Powder in AlCl3⁃EMIC Ionic Liquid

为解决纳米铝粉制备能耗大、粒径控制困难、污染严重的问题,在摩尔比为2∶1的氯化铝‑氯化‑1‑乙基‑3‑甲基咪唑(AlCl_(3)‑EMIC)离子液体中加入二异丁基氢化铝(DIBAL),以液相化学法绿色安全的制备纳米铝粉。采用X射线衍射(XRD)、纳米粒度检测、透射电子显微镜(TEM)、扫描电子显微镜(SEM)、X射线能谱(EDS)和线性扫描伏安法(LSV)等方法对纳米铝粉进行表征,并探究其长大过程及反应机理。结果表明,DIBAL浓度为0.25 mol·L^(-1)、反应时间为0.5 min时获得无团聚且粒径均匀的40~100 nm铝粉,相比其他液相化学法获得粒径更均匀;不同DIBAL浓度下铝粉生长均存在异常长大现象,其原因与Ostwald熟化有关;并且,AlCl_(3)‑EMIC离子液体不仅是反应介质,同时也是纳米铝粉的Al源。

In order to solve the problems of high energy consumption,difficulty in particle size control and serious pollution in the preparation of nano‑aluminum powder.green and safe preparation of nano‑aluminum powder is fulfilled by liquid chemical method through adding diisobutyl aluminum hydride(DIBAL)to aluminum chloride‑1‑ethyl‑3‑methylimidazole chloride(AlCl3‑EMIC)ionic liquid with the molar ratio of 2∶1.By means of X‑ray diffraction(XRD),nano‑particle size detection,transmission electron microscopy(TEM),scanning electron microscopy(SEM),energy dispersive spectrum of X‑ray(EDS)and linear scanning voltammetry(LSV),the nano‑aluminum powder was characterized and its growth process and reaction mechanism were explored The results show that when DIBAL concentration is 0.25 mol·L^(-1) and reaction time is 0.5 min,the non‑agglomerated aluminum powder with uniform particle size of 40-100 nm is obtained,which is more uniform than the one obtained by other liquid chemical methods.The abnormal growth of aluminum powder is observed at different DIBAL concentrations,which is related to the Ostwald ripening.In addition,the AlCl3‑EMIC ionic liquid is not only the reaction medium,but also the Al source of the nano‑aluminum powder.