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氨磺酸体系电镀锡工艺及锡沉积过程的研究

发布时间:2018-11-08 13:59
【摘要】:目前广泛应用的酚磺酸电镀锡体系和甲磺酸电镀锡体系分别存在酚类对环境与人体有害和甲磺酸易腐败变质、价格高的缺点,本文试图开发一种新型电镀锡体系来代替甲磺酸体系或酚磺酸体系。氨磺酸属于固体强酸,受运输条件限制小,对仪器设备腐蚀小,氨磺酸溶液有一定的还原性,对于氨磺酸电镀锡体系国内外鲜有报道,可以说氨磺酸体系是一种有发展前景的电镀锡体系。本文主要对氨磺酸电镀锡体系的工艺及锡沉积过程进行研究,通过电化学工作站,SEM,XRD等方法,确定亚光和光亮电镀锡的添加剂及工艺参数,并考察两种镀液的镀液性能。通过电化学工作站和SEM研究锡在两种镀液的成核过程及其动力学参数。从氨磺酸镀液的物理化学性质和量子化学水平分析,符合酸性镀锡的基本要求,通过连续电镀测定Sn2+浓度可得氨磺酸镀锡稳定性良好。通过Hull槽筛选氨磺酸体系镀亚光锡添加剂为EPE9400,通过电化学工作站,SEM和XRD方法分析EPE9400无整平能力,工艺参数为:EPE9400的浓度为0.56g/L,电流密度为1-2A/dm2,Sn2+浓度为15-30g/L,温度为45℃。在低电流密度下锡沉积的电流效率在95%左右,当电流密度达到4A/dm2时,电流效率只有77%。在25-45℃下电流效率都在95%左右,氨磺酸亚锡镀液分散能力30%左右,其深度能力极佳。通过电化学工作站和SEM确定氨磺酸体系镀光亮锡镀液的分散剂为TX-100,主光亮剂为苄叉丙酮,辅助光亮剂为乙二醛。通过Hull槽实验,SEM和XRD方法,确定TX-100浓度为2g/L,苄叉丙酮浓度为1g/L,乙二醛浓度为0.128g/L,电流密度为4-6A/dm2。在1-5A/dm2范围内,电流效率都在99%左右,沉积速率随电流密度成线性增加,氨磺酸光亮镀锡液的分散能力在28%左右,其深度能力较差。锡电极在亚光镀液中的电沉积属于扩散控制,锡在不同电位下的电沉积更近于三维瞬时成核。锡在氨磺酸亚光镀锡液的成核位点数在108cm-2左右,成核速率在100s-1左右,临界成核吉布斯自由能在10-20J左右,临界成核尺寸在0.5atom左右。锡在氨磺酸光亮镀锡液中锡的成核过程更接近于三维瞬时成核。锡在氨磺酸光亮镀液的成核位点数在109cm-2左右,成核速率在70s-1左右,临界成核吉布斯自由能在10-20J左右,临界成核尺寸在1atom左右。
[Abstract]:At present, the widely used tin electroplating system with phenol sulfonic acid and tin electroplating system with methyl sulfonic acid have the disadvantages of harmful to the environment and human body respectively, and are prone to corruption and deterioration of Mesosulfonic acid, so the price is high. This paper attempts to develop a new electroplating tin system to replace the mesonic acid system or phenol sulfonic acid system. Ammonia sulfonic acid is a kind of solid strong acid, which is limited by transportation conditions, corrodes little instrument and equipment, and has certain reductivity of ammonia sulfonic acid solution. There are few reports about ammonia sulfonic acid electroplating tin system at home and abroad. It can be said that the ammonia sulfonic acid system is a promising tin electroplating system. In this paper, the process and deposition process of tin electroplating system with ammonia sulfonic acid were studied. The additives and process parameters of glassy and bright tin electroplating were determined by means of electrochemical workstation and SEM,XRD, and the bath properties of the two kinds of plating bath were investigated. The nucleation process and kinetic parameters of tin in two kinds of bath were studied by electrochemical workstation and SEM. According to the physical and chemical properties and quantum chemical level of ammonia sulfonic acid plating solution, the stability of ammonia sulfonic acid tin plating can be obtained by measuring the concentration of Sn2 by continuous electroplating. The Hull bath was used to select the additive of nitrous tin plating in the system of ammonia sulfonic acid as EPE9400,. The electrochemistry workstation, SEM and XRD methods were used to analyze EPE9400 without leveling ability. The technological parameters were as follows: the concentration of EPE9400 was 0.56g / L, the current density was 1-2A / dm2. The concentration of Sn2 is 15-30 g / L and the temperature is 45 鈩,

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