电解铜箔添加剂的研究及电解液中各组份浓度的检测
发布时间:2018-01-24 19:14
本文关键词: 电解铜箔 添加剂 电沉积 在线监测 出处:《华南理工大学》2015年硕士论文 论文类型:学位论文
【摘要】:随着锂离子电池行业的迅猛发展,对锂离子电池负极集流体所用的电解铜箔的要求也越来越高。开发优良的添加剂配方是制备高性能电解铜箔的重要途径之一。本文模拟工厂生产电解铜箔的工艺条件,致力于开发能在高电流密度条件下制备光亮整平电解铜箔的添加剂配方,并研究了添加剂作用下铜的电沉积过程。此外,还采取简单有效的方法对电解液中铜离子、硫酸、添加剂浓度进行检测。主要内容如下:1.确定了6组双组份,3组三组分添加剂配方,在高电流密度7500A·m-2条件下,制备电解铜箔。扫描电镜分析表明制备的铜箔显微结构平整致密、无明显缺陷,光泽度测试表明所制备铜箔毛面光亮度都在100-200GS之间,粗糙度测试表明铜箔毛面Ra0.2μm,Rz2.0μm,X射线衍射分析表明镀层均呈现(111)晶面较大择优取向,从而说明所制备铜箔比较平整。2.用线性电势扫描、循环伏安和计时电流法研究50℃下Cl-、BSP、RPE单独存在与同时存在时,在含320g/LCu SO4?5H2O,110g/LH2SO4溶液中,铜在铜电极上的电沉积过程。研究表明Cl-、BSP在铜的电沉积过程中起去极化作用,随着RPE浓度的增大极化作用在增强。添加30mg?L-1Cl-+5mg?L-1BSP+5mg?L-1RPE会增大表观传递系数和扩散系数,加快铜的电沉积过程;RPE会降低成核数密度,而BSP使成核数密度增大,但同时会降低铜离子的扩散系数。在Cl-、RPE、30mg?L-1Cl-+5mg?L-1BSP+5mg?L-1RPE作用下,铜的电沉积都是在开始时接近瞬时成核,随时间延长向连续成核靠近,最终偏离理论模型,而在BSP作用下,始终接近瞬时成核理论。3.结合光电技术,自主设计制作设备,对电解液中铜离子浓度进行在线监测,铜离子浓度与微安表读数有很好的线性关系。此外,校正了温度对铜离子监测的影响。4.用测量电导率的方法,对电解液中硫酸浓度进行检测,电解液中硫酸浓度与电解液的电导率有很好的线性关系,同样校正了温度对电导率的影响。5.沉淀分离电解液中硫酸铜,测含不同浓度DPS的上清液在波长为270nm处吸光度,发现吸光度与DPS浓度有很好的线性关系,从而实现对DPS浓度的检测。
[Abstract]:With the rapid development of lithium ion battery industry. The requirement of electrolytic copper foil for negative electrode collector of lithium ion battery is higher and higher. The development of excellent additive formula is one of the important ways to prepare high performance electrolytic copper foil. This paper simulates the production process of electrolytic copper foil in the factory. Conditions. This paper is devoted to the development of additive formula for the preparation of bright leveling electrolytic copper foil under high current density, and the electrodeposition process of copper under the action of additive. The concentration of copper ion, sulfuric acid and additive in electrolyte was also determined by simple and effective method. The main contents are as follows: 1. Six groups of two-component and three groups of three-component additive formula were determined. Electrolytic copper foil was prepared at high current density of 7500A 路m ~ (-2). SEM analysis showed that the microstructure of the prepared copper foil was flat and compact without obvious defects. The gloss test shows that the luminance of the copper-foil surface is between 100-200GS, and the roughness test shows that the copper foil surface Ra0.2 渭 m Rz 2.0 渭 m. X-ray diffraction analysis shows that the coating exhibits a large preferred orientation on the crystal plane, which indicates that the copper foil prepared is relatively flat. 2. The coating is scanned by linear potential. The cyclic voltammetry and chronoamperometric method were used to study the existence and co-existence of Cl-O BSPN RPE at 50 鈩,
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