Zhang Lipeng, Wang Enqi, Mu Jiechen, Yu Xianjin, Wang Qiannan, Yang Lina, Zhao Zengdian
J Nanosci Nanotechnol. 2014 Aug;14(8):6287-93. doi: 10.1166/jnn.2014.8856.
An efficient microwave enhanced synthesis of ambient temperature chloroaluminate ionic liquid ([EMIM]Br) that preceeds reaction of 1-methylimidazolium with bromoethane in a closed vessel, was described in our work. The reaction time was drastically reduced as compared to the conventional methods. The electrochemical techniques of impedance spectroscopy, cyclic voltammetry and chronoamperometry were used to investigate the mechanism of Al electrodeposition from 2:1 (molar ratio) AlCl3/[EMIM]Br ionic liquid at room temperature. Results indicated that Al electrode- position from this ionic liqud was a quasi-reversible process, and the kinetic complications during the reaction was probably attributed to the electron transfer or mass transport cooperative controlled processes, instantaneous nucleation with diffusion-controlled growth was also investigated. Electrodepositon experiment was conducted using constant current density of 40 mA·cm(-2) for 20 minutes at room temperature and the qualitative analysis of the deposits were performed using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and energy dispersive spectroscope (EDS). The deposits obtained on copper cathode were dense and compact and most Al crystal shows granular structure spherical with high purity.
我们的工作描述了一种高效的微波增强合成室温氯铝酸盐离子液体（[EMIM]Br）的方法，该方法在密闭容器中使1-甲基咪唑鎓与溴乙烷发生反应。与传统方法相比，反应时间大幅缩短。采用阻抗谱、循环伏安法和计时电流法等电化学技术研究了室温下从2:1（摩尔比）的AlCl₃/[EMIM]Br离子液体中电沉积Al的机理。结果表明，从这种离子液体中电沉积Al是一个准可逆过程，反应过程中的动力学复杂性可能归因于电子转移或传质协同控制过程，还研究了瞬时成核与扩散控制生长。在室温下以40 mA·cm⁻²的恒定电流密度进行电沉积实验20分钟，并使用X射线衍射（XRD）、扫描电子显微镜（SEM）和能量色散光谱仪（EDS）对沉积物进行定性分析。在铜阴极上获得的沉积物致密且紧凑，大多数Al晶体呈现高纯度的颗粒状球形结构。
