CN1226465C - 一种电沉积平整光亮金属的复合添加剂的生产和使用方法 - Google Patents
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Abstract
一种电沉积平整光亮金属的复合添加剂的生产和使用方法,其由聚丙烯酰胺、硼酸盐、烷基含硫酸盐组成。先将烷基含硫酸盐配制成15~35%百分浓度的水溶液,再加入其他一种或两种,即得到该复合添加剂。其与明胶和硫脲配合使用,控制其在电解液中的浓度为2~10mg/L,可获得平整、光亮的阴极沉积金属,并有效的减少了树枝状结晶在阴极上的生长,具有原料廉价,来源可靠,不污染环境等优点,有直接的工业运用价值。
Description
(一)技术领域:电化学冶金
(二)背景技术:在公知的金属电沉积工艺中,通过外加少量添加剂物质,可以明显改善阴极沉积金属的化学成分和表面结晶质量。
控制阴极极化和电解液中悬浮粒子的含量,使晶粒细化和结晶晶体取向,是添加剂的主要目的。但是,阴极在外观上的几何平整与微观上表面的真实平整存在区别;同样,并非所有细化了的晶粒都能达到外观上光亮效果。表面金属光亮的条件是当晶粒小于可见波长(0.4微米),具有取向晶体结构。
在一般的工艺条件下,明胶和硫脲能够达到平整和光亮的要求,已经在金属电沉积工业中广泛使用。实践中已经发现,目前的动物胶在高温水溶液中容易降解,特别是在酸性水溶液中的降解速度更快。使用的硫脲会与阴极金属形成络合物,导致阴极铜中硫含量升高。在高电流密度下,如何抑制杂质砷、锑、铋的析出和漂浮阳极泥的机械夹杂行为,获得平整光亮的阴极质量,引起了研究人员和工业部门的关注。
在中国专利“用于铜电解提纯和铜电解冶金的聚丙烯酸添加剂,公告号:“1193053”中指出,聚丙烯酸作为添加剂用于电解冶金浴和电解提纯浴中,可以细化晶粒、减少树枝状晶体和减少电镀中的杂质。
在美国专利(U S patent 4336114,Mayer et.al 1982)中,提出了适于电子线路基板金属电镀用添加剂,主要成分有含酞化青染料、聚乙烯亚胺烷基化剂,还含有聚醚化合物。
在美国哥伦比亚大学的博士论文:“在有复合表面活性剂存在下铜的电沉积”,作者Kelly,James John,哥伦比亚大学,公告号:AAT9916887,1999(Copper Deposition in the Presence of Mixed Surfactants,Kelly,James John,Columbia University,Publication No:AAT9916887,1999)中,针对印刷电路板制造,研究了四种添加剂:氯离子、聚乙烯乙二醇(PEG),二-(3-亚砜)-二硫化物(SPS)和JGB(Janus Green B)。研究后发现,聚乙二醇加着色剂及某种二硫化物后,可以得到表面质量很好的阴极铜,聚乙二醇加着色剂的作用次之;明胶和硫脲这两种常规添加剂的作用比前两者的作用都差一些;而效果最差的是明胶加磺基脂肪族有机化合物和二硫化物组成的联合添加剂。
在文献:“一些有机添加剂对从硫酸盐电解液中电解沉积铜的影响”,湿法冶金,2000,54:161-169(The effects of some organic additivsupon copper electrowining from sulphate electrolytes,Hydrometallurgy,2000,54:161-169)中,将HCE(马栗提取物Horse-chestnut extract的缩写)及IT-85(一种乙氧基乙酸乙醇和三乙烷基苯甲基氯化铵的混合物)作为铜电解添加剂进行了研究,并用目测、X-衍射分析阴极铜纯度、X-衍射分析晶粒生长情况等方法进行分析检测后指出,有机添加剂IT-85是一种很好的表面抑制剂,可以获得平整、致密的阴极铜,其作用与硫脲的作用相似。而HCE与动物胶的作用相似,获得的阴极铜有圆形的突起,阴极铜表面质量较差。
至今为止,在众多实际用于铜电解沉积的添加剂中,阿维同-A能显著地改善沉积金属的表面质量,使阴极铜表面光滑、结晶致密,在铜电解精炼工业中得到成功应用。
但是,上述添加剂工艺在不同程度上存在若干限制:原料不容易获得,生产会带来严重的环境污染,工艺流程复杂等。例如,阿维同-A的生产采用氯磺化法(也称Reed法)和磺氧化法(也称I.G.法),工艺流程复杂,环境污染严重。
本发明开发了含聚丙烯酰胺、硼酸盐、烷基含硫酸盐的复合添加剂的生产技术和使用方法。复合添加剂的整体作用机理并不是几个添加剂作用机理的简单迭加,而是几种添加剂的协同作用。该复合添加剂与明胶和硫脲配合使用,生产出的阴极沉积金属致密、平整和光亮,并有效地减少树枝状结晶在阴极的生长。另外,该复合添加剂的平整和光亮的效果类似或优于阿维同-A,原料有可靠的来源,添加剂的生产不会造成环境污染,添加剂的价格不高于目前使用的阿维同-A,具有直接工业应用价值。
(三)发明内容:
1.发明目的:本发明针对高电流密度和高杂质成分金属电沉积,以及电子线路金属电沉积连接技术的要求,为了使阴极上析出的沉积物表面光亮平整、纯度高、结晶致密,减少电解液中的悬浮物,减少结瘤和枝晶生长所引起的短路,减少阳极泥、电解液机械地粘附在阴极上所引起的污染,研制成功的与明胶和硫脲配合使用时效果显著的复合添加剂技术,可获得致密、平整和光亮的阴极电化学沉积金属。
2.复合添加剂的生产方法
1)原料及所占重量百分比:烷基硫酸钠或烷基磺酸钠85~100%;硼酸盐0~10%;聚丙烯酰胺0~15%。
2)配方
复合添加剂1:烷基硫酸钠或烷基磺酸钠90%;聚丙烯酰胺5%;硼酸盐占5%
复合添加剂2:烷基硫酸钠或烷基磺酸钠95%;聚丙烯酰胺5%;硼酸盐0%;
复合添加剂3:烷基硫酸钠或烷基磺酸钠100%;
复合添加剂4:烷基硫酸钠或烷基磺酸钠88%;聚丙烯酰胺8%;硼酸盐4%;
复合添加剂5:烷基硫酸钠或烷基磺酸钠90%;聚丙烯酰胺10%;硼酸盐0%;
3)生产步骤
(1)先将上述三种固体原料磨细至-20目粉末;
(2)烷基硫酸钠或烷基磺酸钠按配方中的数量称量放入水中,配制成15-35%(重量百分浓度)的水溶液,再将配方中的另外一种或两种粉末加入上述水溶液中,搅拌至完全溶解,即得该复合添加剂水溶液。
3.复合添加剂的使用方法
控制复合添加剂在电解液中的体积质量百分浓度为2~10毫克/升或与明胶、硫脲配合使用,先将上述配制好的复合添加剂水溶液再加水稀释成体积质量浓度为0.2~10克/升·水,明胶稀释成1~15克/升·水,硫脲稀释成0.5~15克/升·水的稀释液,再在生产过程中连续均匀的滴入电解液中;
4.与公知技术相比本发明具备的优点及积极效果:复合添加剂与现有明胶和硫脲配合,平整和光亮效果类似或优于阿维同-A,能够应用于各种电化学金属沉积过程。添加剂的生产原料有廉价和可靠的来源保证,生产不会造成环境污染,价格不高于现使用的阿维同-A,具有直接的工业应用价值。
(四)附图说明:图1是本发明的工艺流程图。
(五)具体实施方式
[实施例1]电解液的组成(g/L):Cu 48;H2SO4 180;Cl 0.04;Ni 12;As 5;Sb 0.5;Bi 0.3;悬浮物≤0.07。
电解液温度60~65℃;
电流密度270~300A/m2;
电解液循环量25~35L/min.槽;
取复合添加剂1,其配比为:烷基磺酸钠90%,聚丙烯酰胺5%,硼酸盐5%;取所需之复合添加剂量(由电解过程中电解液的总量来限定),用水稀释至浓度为~5g/L再与稀释好的明胶和硫脲混匀后,再连续均匀的滴入电解液中,并保持电解液中含复合添加剂2~10mg/L,明胶3~10mg/L,硫脲2~8mg/L产出致密,平整、光亮的阴极铜。
[实施例2]电解液的组成(g/L):Cu 49;H2SO4200;Cl 0.04;Ni 8;As 5;Sb 0.5;Bi 0.3;悬浮物≤0.07。
电解液温度60~65℃;
电流密度270~300A/m2
电解液循环量25~35L/min槽;
明胶稀释液浓度为 ~4.5g/L;
硫脲稀释液浓度为 ~2g/L;
复合添加剂3配比:烷基硫酸钠100%,稀释液浓度为~1.5g/L;
添加剂的配制和加入方法与[实施例1]相同。并保持电解液中含有复合添加剂2~8mg/L,明胶3~9mg/L,硫脲2~7mg/L可产出致密、平整、光亮的阴极铜。
Claims (3)
1.一种电沉积平整光亮金属的复合添加剂的生产方法,其特征是:
1)原料及所占重量百分比:烷基硫酸钠或烷基磺酸钠85~100%;聚丙烯酰胺0~15%,硼酸盐0~10%,2)生产方法:先将固体原料磨细至-20目;烷基硫酸钠或烷基磺酸钠按步骤(1)中的重量百分比称量后放入水中,配制成重量百分浓度为15-35%的水溶液,再将上述原料中的另外一种或两种加入该水溶液,搅拌至完全溶解。
2.根据权利要求1所述的复合添加剂的生产方法,其特征是:原料配成5种配方的复合添加剂,复合添加剂1:烷基硫酸钠或烷基磺酸钠90%,聚丙烯酰胺5%,硼酸盐5%;复合添加剂2:烷基硫酸钠或烷基磺酸钠95%,聚丙烯酰胺5%;复合添加剂3:烷基硫酸钠或烷基磺酸钠100%,;复合添加剂4:烷基硫酸钠或烷基磺酸钠88%,聚丙烯酰胺8%,硼酸盐4%;复合添加剂5:烷基硫酸钠或烷基磺酸钠90%,聚丙烯酰胺10%。
3.一种复合添加剂的使用方法,其特征在于:采用由权利要求1或2中的生产方法获得的复合添加剂,控制复合添加剂在电解液中的体积质量百分浓度为2~10毫克/升;或与明胶、硫脲配合使用:先将三种添加剂加水稀释,配制成体积质量浓度为复合添加剂0.2~10克/升·水,明胶1~15克/升·水,硫脲0.5~15克/升·水的稀释液,再连续、均匀地加入电解液中。
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