离子液体中以PAA为模板电沉积镍的研究-化学工程与技术专业论文.docxVIP

Classified Index: O646.54 U.D.C.: 546.57 Dissertation for the Master Degree in Engineering STUDIES ON Ni NANOWIRES ARRAY ELECTRODEPOSITED IN PAA TEMPLATE FROM A IONIC LIQUID Candidate:Li JidanSupervisor: Candidate: Li Jidan Supervisor: Prof. Mao Academic Degree Applied for: Master of Specialty: Chemical Affiliation: Departme Date of Defence: 3 July, 20 Degree-Conferring-Institution: Harbin In Engineering and Technology nt.of Applied Chemistry 07 stitute of Technology 哈尔滨工业大学工学硕士学位论文 哈尔滨工业大学工学硕士学位论文 - - I - 摘 要 以离子液体为电解液，研究了金属镍的电沉积工艺。在EMIC-NiCl2 溶 盐中加入乙腈、乙二醇(EG)、丙三醇、N,N-二甲基甲酰胺后，能够显著地 提高电解液的导电性，乙二醇还具有改善金属沉积层质量的作用。综合研究 了乙二醇加入量、添加剂、电流密度、温度等对镍镀层质量的影响，确定了 电沉积镍的较佳的电解液及工艺条件：EMIC、NiCl2 、EG三者的摩尔比为 2:1:6~2:1:9 、丁炔二醇 0.2~0.4g/L 、阴极电流密度 50~80A/m2 、温度 80~100℃。扫描电子显微镜观察显示：在该条件下，所得镀层结晶细致均 匀、晶粒细小。X射线衍射分析表明，随着电解液中乙二醇加入量的增加， 镍的结晶发生明显的择优取向，晶粒按 (220) 晶面优先生长；当 EMIC- NiCl2-EG体系中加入丁炔二醇后，则 (220) 晶面的择优取向不再发生。通 过阴极极化曲线和计时电流法测试，初步确定离子液体中金属镍的成核符合 三维瞬时成核规律。 以 PAA 为模板，在离子液体中直流电沉积制备了镍纳米线阵列膜。透 射电子显微镜观察表明，离子液体中电沉积得到的镍纳米线粗细均匀、表 面光滑。磁滞回线测试结果表明，组装在硫酸体系制备的 PAA 模板中的镍 纳米线阵列膜的矩形比为 0.72、矫顽力为 646Oe；组装在草酸体系制备的 PAA 模板中的镍纳米线阵列膜的矩形比为 0.36、矫顽力为 522Oe。二者相 比，以硫酸体系制备 PAA 为模板的纳米线阵列膜具有较强的垂直磁各向异 性。 关键词 离子液体；电沉积；镍；多孔阳极氧化铝；纳米线 - - II - Abstract The electrodeposition of Ni from EMIC-NiCl2 ionic liquid was investigated. The addition of acetonitrile, glycol (EG) and glycerin increased the electrolyte conductivity apparently. Simultaneously, glycol can enhance the quality of the deposit. By considering the effect of additional content of glycol, additive, current density, temperature on deposit quality, the optimal electrolyte composition and operating conditions are: the molar ratio of EMIC-NiCl2-EG 2:1:6~2:1:9; 2-butyne-1,4-diol 0.2~0.4 g·L-1; current density 50~80A·m-2; temperature 80~100℃. Under these conditions, FE-SEM indicated that the appearance of Ni plating is pretty wonderful. XRD analysis indicated that the addition of glycol in electrolyte can change the crystal orientation of Ni, and the grains preferred