低共熔溶剂中电化学剥离制备GO及脉冲电沉积Ni-GO复合镀层性能研究  

Preparation of Graphene Oxide by Electrochemical Exfoliation and Properties of Pulsed Electrodeposited Ni-Graphene Oxide Composite Coating in Deep Eutectic Solvent

作　　者：郭惠霞 安景花 梁军[2] GUO Hui-xia;AN Jing-hua;LIANG Jun(Key Laboratory of Bioelectrochemistry&Environmental Analysis of Gansu Province,School of Chemistry&Chemical Engineering,Northwest Normal University,Lanzhou 730070,China;State Key Laboratory of Solid Lubrication,Lanzhou Institute of Chemical Physics,Chinese Academy of Sciences,Lanzhou 730000,China)

机构地区：[1]西北师范大学化学化工学院甘肃省生物电化学与环境分析重点实验室,兰州730070 [2]中国科学院兰州化学物理研究所固体润滑国家重点实验室,兰州730000

出　　处：《表面技术》2020年第3期224-233,共10页Surface Technology

基　　金：国家自然科学基金青年基金项目(51405472);甘肃省高等学校科研项目资助(2018D-03)。

摘　　要：目的在低共熔溶剂中实现电化学剥离制备氧化石墨烯(GO)及电沉积制备Ni-GO复合镀层,提高Ni镀层的耐腐蚀和摩擦磨损性能。方法以石墨棒为阴极,铂片为阳极,低共熔溶剂为电解液,采用直流电源电化学剥离石墨制备氧化石墨烯纳米片(GO),然后在此电解液中,采用脉冲电沉积的方式制备Ni-GO复合镀层。采用扫描电子显微镜(SEM)、透射电子电镜(TEM)、紫外分光光度计(UV)、红外光谱仪(IR)、拉曼光谱仪(Raman)、X射线衍射仪(XRD),表征GO的结构和组成。采用扫描电子显微镜(SEM)观察镀层的表面形貌,采用X射线衍射仪(XRD)、X射线光电子能谱仪(XPS)分析镀层的结构特征。采用电化学工作站、纳米压痕仪和摩擦磨损实验机分析镀层的耐腐蚀性能、机械性能和摩擦磨损性能。结果采用电化学剥离法在低共熔溶剂中成功制备了GO,GO呈现大的片层状结构,表面存在褶皱,边缘弯曲,上下表面层含有大量羟基和环氧基。性能检测表明,Ni-GO复合镀层的腐蚀电流密度由纯Ni镀层的6.10×10^-5 A/cm^2降低为5.78×10^-7 A/cm^2,硬度由纯Ni镀层的(8.95±0.43)GPa提高到(13.75±0.75)GPa,弹性模量由纯Ni镀层的(184.55±8.12)GPa提高到(201.38±11.20)GPa,摩擦系数由纯Ni镀层的0.72降低为0.56,磨损率比纯Ni镀层降低了35.16%。结论在低共熔溶剂中实现了电化学剥离石墨制备GO,并用于Ni-GO金属基复合镀层一步制备的电化学途径,为均匀分散的氧化石墨烯的制备和金属基复合镀层的制备提供了新的方法。以此为电解液制备的Ni-GO复合镀层相比于纯Ni镀层,其晶粒细化,耐腐蚀性能增强,机械性能提高,摩擦系数减小,耐磨性能增强。The work aims to improve corrosion resistance and tribological properties of Ni coatings by realizing electrochemical exfoliation of graphene oxide and deposition of Ni-GO composite coating in the deep eutectic solvent(DES).GO was electrochemically exfoliated in DES by DC source with graphite rod as anode and platinum foil as cathode,respectively.The Ni-GO composite coatings were prepared by pulse electrodeposition in this basic electrolyte.Microstructure and composition of GO were characterized by scanning electron microscope(SEM),transmission electron microscope(TEM),UV-Visible absorption spectroscopic(UV),Fourier transform infrared(IR),Raman spectrometer and X-ray diffractometer(XRD).The morphology of coatings was observed by SEM,structural characteristics were analyzed by XRD and XPS and corrosion resistance,mechanical properties and tribological properties of the coatings were investigated by electrochemical workstation,nano-indentation instrument and friction and wear apparatus.GO was successfully prepared by electrochemical exfoliation in DES.GO showed a large sheet structure and had wrinkles on the surface.The edges were curved,and the upper and lower surface layers contained a large amount of hydroxyl groups and epoxy groups.The performance test indicated that the corrosion current density of Ni-GO composite coating was reduced from 6.10×10^-5 A/cm^2 to 5.78×10^-7 A/cm^2,the hardness was improved from(8.95±0.43)GPa to(13.75±0.75)GPa,the elastic modulus was increased from(184.55±8.12)GPa to(201.38±11.20)GPa,the coefficient of frictional was decreased from 0.72 to 0.56 and the wear rate was reduced by 35.16%.One-step electrochemical route for preparation of GO with electrochemical exfoliation is realized in deep eutectic solvents and it can also be used for preparing Ni-GO metal-based composite coatings,which provides a new method for the preparation of uniformly dispersed graphene oxide and the preparation of metal-based composite coatings.Compared with pure Ni coating,Ni-GO composite coating prepar

关 键 词：低共熔溶剂 电化学剥离 氧化石墨烯 Ni-GO复合镀层 脉冲电沉积 

分 类 号：TQ153[化学工程—电化学工业]