摘要
研究了金属钼(Mo)在离子液体1-丁基-1-甲基吡咯烷双(三氟甲磺酰)亚胺盐中([BMP]Tf_2N)的电沉积。采用MoCl_5[BMP]Tf_2N离子液体体系作为电沉积的电解质,测定了不同温度下的伏安曲线(CV)。用恒电位法进行电沉积,沉积物通过扫描电镜(SEM)、能谱(EDS)、透射电镜(TEM)和光电子能谱(XPS)进行了观察和表征。结果表明,在25~120℃的温度范围内,当温度高于100℃时,Mo的电化学还原行为发生明显的变化。在120℃,Pt基板上,–2.2和–2.7V恒电位电沉积均能得到金属态的Mo。其中,–2.2V时得到非晶态的Mo,沉积层平整、无裂纹;–2.7V时得到晶态和非晶态混合的Mo,沉积层有裂纹。而在60℃,Mo(Ⅴ)还原后形成难溶产物以致无法得到Mo(0)。最后,对Mo的电化学还原机理进行了讨论。
Electrodeposition of molybdenum in the 1-butyl-1-methylpyrrolidinium bis （trifluoromethylsulfonyl） amide （[BMP]Tf2N） ionic liquid was investigated. MoC15-[BMP]Tf2N was used as the electrolyte of electrodeposition and cyclic voltammetry curves were tested at various temperatures ranging from 25℃ to 120℃. Electrodeposition was carried out using a potentiostatic method. Deposits were observed and characterized by SEM, EDS, TEM and XPS. The results show that the electrochemical reduction behavior of Mo changes significantly when the temperature above 100℃ in the temperature range of 25-120 ℃. The metallic molybdenum can be obtained potentiostatically at -2.2 V and -2.7 V on platinum electrode at 120℃. Deposit obtained at -2.2 V is fiat without cracks, while deposit obtained at -2.7 V contains crystalline molybdenum with cracks in the deposited layer. The reduction product for Mo（V） is insoluble substance so that Mo（0） cannot be obtained at 60 ℃. Mechanism of the electrochemical reduction of molybdenum in the [BMP]Tf2N was also discussed.
作者
杨慧玲
丁晶晶
江奕东
凌国平
Yang Huiling;Ding Jirtgjing;Jiang Yidong;Ling Guoping(Zhejiang University, Hangzhou 310027, China;China Academy of Engineering Physics, Jiangyou 621907, China)
出处
《稀有金属材料与工程》
SCIE
EI
CAS
CSCD
北大核心
2018年第5期1523-1528,共6页
Rare Metal Materials and Engineering
基金
国家自然科学基金(51271166)
