离子液体[BMIM]PF6中铬的电沉积行为

doi:10.7503/cjcu20130278

高等学校化学学报 ›› 2014, Vol. 35 ›› Issue (1): 140.doi: 10.7503/cjcu20130278

离子液体[BMIM]PF₆中铬的电沉积行为

玉山江·哈斯木, 刘瑞泉(), 米红宇

新疆大学化学化工学院, 乌鲁木齐 830046

收稿日期:2013-03-26 出版日期:2014-01-10 发布日期:2013-11-25
作者简介:联系人简介: 刘瑞泉, 男, 教授, 主要从事材料物理化学研究. E-mail:liu.rq@163.com
基金资助:
新疆维吾尔自治区高校科研计划项目(批准号: XJEDU2012I05)和国家自然科学基金(批准号: 21063013)资助

Electrodeposition Behavior of Chromium in Ionic Liquid [BMIM]P $F 6 †$

HASIMU Yushanjiang, LIU Ruiquan^*(), MI Hongyu

College of Chemistry and Chemical Engineering, Xinjiang University, Urumqi 830046, China

Received:2013-03-26 Online:2014-01-10 Published:2013-11-25
Contact: LIU Ruiquan E-mail:liu.rq@163.com
Supported by:
† Supported by the University Scientific Research Project of Xinjiang Uygur Autonomous Region, China(No.XJEDU2012I05) and National Natural Foundation of China(No.21063013)

摘要/Abstract

摘要：

以一氯丁烷、 N-甲基咪唑和KPF₆为原料, 合成了1-丁基-3-甲基咪唑六氟磷酸盐离子液体([BMIM]PF₆), 用红外光谱(IR)对产物进行了结构分析. 用循环伏安法测试该离子液体在85 ℃下的电化学窗口为4.7 V. 考察了[BMIM]PF₆-Cr(Ⅲ)电解液的电化学行为, 结果表明, 在85 ℃下Cr(Ⅲ)的还原过程是受扩散控制的一步还原不可逆过程, Cr(Ⅲ)的传递系数α=0.023, 阴极扩散系数D₀=1.142×10^-6 cm²/s. 在85 ℃和-1.5 V条件下, 用恒电势法在铜片上电沉积Cr(Ⅲ), 并通过扫描电子显微镜(SEM)观察了铜片上镀层的表面结构, 发现该镀层呈颗粒状, 且颗粒的体积随沉积时间的延长而增大. X射线能量色散谱(EDS) 和X射线粉末衍射(XRD)测试结果表明, 该镀层为无定形的金属铬.

关键词: 铬, 离子液体, 循环伏安, 电化学窗口, 电沉积

Abstract:

1-Butyl-3-methylimidazolium hexafluorophosphate([BMIM]PF₆) ionic liquid was synthesized by 1-chlorobutane, N-methylimidazole and KPF₆. The structure of ionic liquid was investigated by IR spectrum. The electrochemical window of [BMIM]PF₆ was determined to be 4.7 V at 85 ℃ by cyclic voltammetry. The electrochemical behavior of the[BMIM]PF₆-Cr(Ⅲ) electrolyte was studied. The reduction of chromium from Cr(Ⅲ) to Cr(0) in the solution is a one-step irreversible growth process which is controlled by diffusion. The cathodal transfer coefficient(α) is 0.023 and the cathode diffusion coefficient(D₀) is 1.142×10^-6 cm²/s. The electrodeposition of chromium on copper substrate from [BMIM]PF₆-Cr(Ⅲ) were experimented by potentiostatic method at -1.5 V. The surface morphology of chromium coating was characterized by means of scanning electron microscopy(SEM) and its morphology was granular structure. The size of granulae increase with the increase of deposition time. The chemical composition and structure of chromium coating were tested by energy dispersive spectrometry(EDS) and X-ray diffraction(XRD). The results indicate that the coating consist of amorphous metallic chromium.

Key words: Chromium, Ionic liquid, Cyclic voltammetry, Electrochemical window, Electrodeposition

中图分类号:

O646

TrendMD:

玉山江·哈斯木, 刘瑞泉, 米红宇. 离子液体[BMIM]PF₆中铬的电沉积行为. 高等学校化学学报, 2014, 35(1): 140.

HASIMU Yushanjiang, LIU Ruiquan, MI Hongyu. Electrodeposition Behavior of Chromium in Ionic Liquid [BMIM]P $F 6 †$ . Chem. J. Chinese Universities, 2014, 35(1): 140.

图/表 11

Scheme 1 Synthesis of [BMIM]PF6 ionic liquid

Fig.1 Schematic diagram of electrochemical device

Fig.2 FTIR spectrum of [BMIM]PF6 ionic liquid

Fig.3 Electrical conductivities of [BMIM]PF6(a) and [BMIM]PF6-Cr(Ⅲ)(b)

Fig.4 Electrochemical window of ionic liquid

Fig.5 Cathodic polarization curves of [BMIM]PF6-Cr(Ⅲ)

Table 1 Data of cathodic polarization of [BMIM]PF6-Cr(Ⅲ)(0.1 mol/L) with various scan rates at 85 ℃

ν/(mV?s^-1)	I_pc/μA	E_pc/V	E_pc/2/V	∣E_pc-E_pc/2∣/V	ν^1/2/(mV?s^-1)^1/2	α
50	-1.52	-1.50	-0.765	0.735	7.071	0.026
80	-3.04	-1.61	-0.771	0.839	8.944	0.023
100	-3.74	-1.65	-0.775	0.875	10.000	0.022
120	-4.51	-1.69	-0.800	0.890	10.954	0.022
180	-6.26	-1.77	0.875	0.895	13.416	0.022
Average						0.023

Fig.6 Relationship between Epc and lgν

Fig.7 Relationship between Ipc and ν1/2

Fig.8 SEM images of Cr deposits from [BMIM]PF6-Cr(Ⅲ) electrolyte at 85 ℃, -1.50 V on Cu substrate (A—C) 0.1 mol/L Cr(Ⅲ); (A'—C') 0.4 mol/L Cr(Ⅲ). Deposition time/min: (A), ( A') 30; (B), (B') 60; (C), (C') 120.

Fig.9 EDS analysis of Cr deposits from [BMIM]PF6-Cr(Ⅲ) on Cu substrate

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离子液体[BMIM]PF₆中铬的电沉积行为

Electrodeposition Behavior of Chromium in Ionic Liquid [BMIM]P $F 6 †$

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