离子液体的微波合成及铝、铝锌合金的电沉积应用
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摘要
离子液体是基于绿色化学和高效能源利用提出的,氯铝酸离子液体中有关铝及合金的研究较早,但是氯铝酸离子液体的常规制备往往需要大量的反应时间,而且需要大量的溶剂才能得到较高的产率,需要探寻一种新型高效的氯铝酸离子液体的合成方法。尽管氯铝酸离子液体中沉积出了铝及多种合金,但对铝及合金在氯铝酸离子液体中的电沉积机理研究仍不充分,双电层结构、阴阳极反应动力学仍不清楚,制备高质量沉积铝及合金仍需要对其影响因素做进一步的分析探讨。
本文采用新型微波合成方法制备溴代氯铝酸离子液体,测试其物理化学性能,结果表明氯铝酸离子液体的新型微波合成解决了普通微波反应溶剂过热问题,与传统合成方法相比缩短了反应时间,提高了产品品质。溴代氯铝酸离子液体的各项性能取决于氯化铝(AlCl3)与中间体([EMIM]Br)的摩尔比,酸性溴代氯铝酸离子液体除其电化学窗口、电导率稍微低于中性溴代氯铝酸离子液体之外,其余各项物理化学性能优越,为其在铝及合金电沉积制备方向的应用提供了可能。
2AlCl3/[EMIM]Br (AlCl3/[EMIM]Br的摩尔比为2：1)离子液体作为电解质应用于铝的电沉积,通过测定循环伏安曲线、交流阻抗谱、计时电流曲线以及极化曲线探讨铝的电沉积机理。室温下在铜、铝、碳钢基体上进行铝的电沉积实验,沉积层形貌、结构特性以及耐蚀性能分别用扫描电子显微镜(SEM)、X射线衍射(XRD)、电化学测试方法等进行表征。结果表明溴代氯铝酸离子液体中铝的电沉积为准可逆的动力学行为,双电层结构中存在弥散效应,沉积过程非单纯的扩散控制而是复杂动力学限制步骤,铝沉积的时间-电流暂态曲线主要包括三个区域分别对应着三种不同的极化方式,同时也对应着铝的结晶成核及长大的不同阶段,铝在铜基体上结晶成核符合三维瞬时成核模型；铝沉积层大致分为三种典型形貌,对各种形貌产生的原因及各项特征进行分析。
2AlCl3/[EMIM]Br直接溶解ZnCl2进行铝锌合金的共电沉积实验研究。循环伏安分析铝锌共沉积机理,XRD分析电解液组成对合金结构性能的影响,SEM和X射线能谱仪(EDS)分析沉积电压对合金组成的影响。结果表明铜基体上铝锌的沉积有明显的两个峰,纯锌的沉积电位约为-0.42 V(v.A1),铝锌共沉积电位约为-0.63 V；ZnCl2/AlCl3/[EMIM]Br的不同组成对合金相结构有较大影响,随着电解液中锌含量的增加,合金相的衍射峰相比于纯铝的衍射峰有更明显的偏移,合金相衍射峰强度相应减小并不断宽化；沉积电位明显影响着合金相的组成,随着过电位的增加合金相中铝含量相应增加,而锌含量却相应减少。
The concept of ionic liquids is based on green chemistry and efficiency and electrodeposition of aluminium (Al) and its alloys from chloroaluminate ionic liquid has been studied for many years, but the conventional synthesis of this ionic liquid is often time consuming and needs a lot of solvent to get reasonable yield. It is necessary to explore a new and efficient synthesis method about chloroaluminate ionic liquid. Although Al and various of its alloys have been electrodeposited from chloroaluminate ionic liquid, the studies about electrodeposition mechanism is still not sufficient, the structure of double layer and the anode and cathode reaction kinetics is still unclear, further analysis of influencing factors is still needed for high-quality Al and its alloys deposits.
A new microwave synthesis of bromo-chloroaluminate ionic liquid was described in our work and its physical and chemical characteristics were tested. Results indicated that the reaction time of the new microwave synthesis of chloroaluminate ionic liquid was drastically reduced as compared to the conventional methods and chloroaluminate ionic liquid with high properties was achieved;
2AlCl3/[EMIM]Br (the molar ratio of AlCl3/[EMIM]Br is 2:1) ionic liquid was used as the electrolyte in Al electrodeposition. Electrochemical techniques of cyclicvoltammetry, electrochemical impedance spectroscopy, chronoamperometry and potentiodynamic polarization technology (tafel) were used to investigate the mechanism of Al electrodeposition. Constant potential electrodeposition of Al was conducted on Copper substrates at room temperature and the morphology, structure and anti-corrosion behavior analysis of the deposits was performed using Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and electrochemical methods, respectively. Results revealed that Al electrodeposition from this ionic liquid was not a simple linear diffusion controlled process, but a quasi-reversible process with complex kinetic limitations, a slight capacitance dispersion occurred in the chloroaluminate ionic liquid, three different regions occurred on the chronoamperometric curve are responding to the three different polarizations and the different periods of Al nucleation and growth process, instantaneous nucleation growth of Al electrodeposition was proved; Al deposits obtained at different potential were mainly about three typical morphology and the reason for the three typical morphology and their characteristics were analyzed.
Co-deposition of Al-Zn alloy was performed from electrolyte that was prepared by directly dissolving of ZnCl2 into 2AlCl3/[EMIM]Br ionic liquid. Cyclicvoltammetry was used to investigate the mechanism of co-deposition of Al-Zn alloy, co-deposits obtained from different molar ratio of ZnCl2/AlCl3/[EMIM]Br were measured by XRD and the surface morphology and the composition of the co-deposits were measured by SEM and Energy Dispersive Spectrometer(EDS), respectively. Results indicated that bare Zn deposition occurred at the potential of-0.42 V (vs. Al), and Al-Zn coating begin to be co-deposited at the potential of-0.63 V; Zn was solidified as the second phase in the alloys, the co-deposits obtained at higher molar ratio of Zn appears bigger 20 shift, broader reflection centered around a 20 and lower reflections intensity; The applied potential has significantly effects on the composition of Al-Zn alloy, the deposition rate of Zn was more quick than that of Al at less negative potential and was limited when the potential getting more negative.
本文采用新型微波合成方法制备溴代氯铝酸离子液体,测试其物理化学性能,结果表明氯铝酸离子液体的新型微波合成解决了普通微波反应溶剂过热问题,与传统合成方法相比缩短了反应时间,提高了产品品质。溴代氯铝酸离子液体的各项性能取决于氯化铝(AlCl3)与中间体([EMIM]Br)的摩尔比,酸性溴代氯铝酸离子液体除其电化学窗口、电导率稍微低于中性溴代氯铝酸离子液体之外,其余各项物理化学性能优越,为其在铝及合金电沉积制备方向的应用提供了可能。
2AlCl3/[EMIM]Br (AlCl3/[EMIM]Br的摩尔比为2：1)离子液体作为电解质应用于铝的电沉积,通过测定循环伏安曲线、交流阻抗谱、计时电流曲线以及极化曲线探讨铝的电沉积机理。室温下在铜、铝、碳钢基体上进行铝的电沉积实验,沉积层形貌、结构特性以及耐蚀性能分别用扫描电子显微镜(SEM)、X射线衍射(XRD)、电化学测试方法等进行表征。结果表明溴代氯铝酸离子液体中铝的电沉积为准可逆的动力学行为,双电层结构中存在弥散效应,沉积过程非单纯的扩散控制而是复杂动力学限制步骤,铝沉积的时间-电流暂态曲线主要包括三个区域分别对应着三种不同的极化方式,同时也对应着铝的结晶成核及长大的不同阶段,铝在铜基体上结晶成核符合三维瞬时成核模型；铝沉积层大致分为三种典型形貌,对各种形貌产生的原因及各项特征进行分析。
2AlCl3/[EMIM]Br直接溶解ZnCl2进行铝锌合金的共电沉积实验研究。循环伏安分析铝锌共沉积机理,XRD分析电解液组成对合金结构性能的影响,SEM和X射线能谱仪(EDS)分析沉积电压对合金组成的影响。结果表明铜基体上铝锌的沉积有明显的两个峰,纯锌的沉积电位约为-0.42 V(v.A1),铝锌共沉积电位约为-0.63 V；ZnCl2/AlCl3/[EMIM]Br的不同组成对合金相结构有较大影响,随着电解液中锌含量的增加,合金相的衍射峰相比于纯铝的衍射峰有更明显的偏移,合金相衍射峰强度相应减小并不断宽化；沉积电位明显影响着合金相的组成,随着过电位的增加合金相中铝含量相应增加,而锌含量却相应减少。
The concept of ionic liquids is based on green chemistry and efficiency and electrodeposition of aluminium (Al) and its alloys from chloroaluminate ionic liquid has been studied for many years, but the conventional synthesis of this ionic liquid is often time consuming and needs a lot of solvent to get reasonable yield. It is necessary to explore a new and efficient synthesis method about chloroaluminate ionic liquid. Although Al and various of its alloys have been electrodeposited from chloroaluminate ionic liquid, the studies about electrodeposition mechanism is still not sufficient, the structure of double layer and the anode and cathode reaction kinetics is still unclear, further analysis of influencing factors is still needed for high-quality Al and its alloys deposits.
A new microwave synthesis of bromo-chloroaluminate ionic liquid was described in our work and its physical and chemical characteristics were tested. Results indicated that the reaction time of the new microwave synthesis of chloroaluminate ionic liquid was drastically reduced as compared to the conventional methods and chloroaluminate ionic liquid with high properties was achieved;
2AlCl3/[EMIM]Br (the molar ratio of AlCl3/[EMIM]Br is 2:1) ionic liquid was used as the electrolyte in Al electrodeposition. Electrochemical techniques of cyclicvoltammetry, electrochemical impedance spectroscopy, chronoamperometry and potentiodynamic polarization technology (tafel) were used to investigate the mechanism of Al electrodeposition. Constant potential electrodeposition of Al was conducted on Copper substrates at room temperature and the morphology, structure and anti-corrosion behavior analysis of the deposits was performed using Scanning Electron Microscopy (SEM), X-ray diffraction (XRD) and electrochemical methods, respectively. Results revealed that Al electrodeposition from this ionic liquid was not a simple linear diffusion controlled process, but a quasi-reversible process with complex kinetic limitations, a slight capacitance dispersion occurred in the chloroaluminate ionic liquid, three different regions occurred on the chronoamperometric curve are responding to the three different polarizations and the different periods of Al nucleation and growth process, instantaneous nucleation growth of Al electrodeposition was proved; Al deposits obtained at different potential were mainly about three typical morphology and the reason for the three typical morphology and their characteristics were analyzed.
Co-deposition of Al-Zn alloy was performed from electrolyte that was prepared by directly dissolving of ZnCl2 into 2AlCl3/[EMIM]Br ionic liquid. Cyclicvoltammetry was used to investigate the mechanism of co-deposition of Al-Zn alloy, co-deposits obtained from different molar ratio of ZnCl2/AlCl3/[EMIM]Br were measured by XRD and the surface morphology and the composition of the co-deposits were measured by SEM and Energy Dispersive Spectrometer(EDS), respectively. Results indicated that bare Zn deposition occurred at the potential of-0.42 V (vs. Al), and Al-Zn coating begin to be co-deposited at the potential of-0.63 V; Zn was solidified as the second phase in the alloys, the co-deposits obtained at higher molar ratio of Zn appears bigger 20 shift, broader reflection centered around a 20 and lower reflections intensity; The applied potential has significantly effects on the composition of Al-Zn alloy, the deposition rate of Zn was more quick than that of Al at less negative potential and was limited when the potential getting more negative.
引文
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