CN104835798A - 一种抗氧化键合铜丝及其制备方法 - Google Patents
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Abstract
本发明公开了一种抗氧化键合铜丝,该铜丝表面涂覆有厚度为5-60纳米的有机物层;本发明还公开一种该抗氧化键合铜丝的制备方法,它包括以下步骤:提纯、制作合金、竖式熔炼、拉丝、退火、覆层、包装,通过该方法制作的抗氧化键合铜丝具有较好的低长弧度,可以有效防止了键合铜丝的氧化,使制备出的键合铜丝在储存和运输中保证不产生氧化,并且该覆层材料可以耐受200℃以上的高温,从而有效解决铜线氧化问题。
Description
技术领域
本发明涉及键合丝技术领域,具体涉及一种抗氧化键合铜丝及其制备方法 。
背景技术
键合金丝是用于集成电路或分立器件及LED连接的关键引线材料。近年来随着半导体行业的迅速发展,以及黄金价格的飙涨,给生产和使用公司都带来成本压力。集成电路的集成化程度越来越高,电路板厚度越来越小,器件上的电极数越来越多,电极间距越来越窄,封装密度也相应变得越来越小,键合金丝已经不能满足日益提高的封装要求,键合铜丝是替代键合金丝的理想材料,但是铜线容易氧化的特性阻碍了铜线的应用和发展。这就要求对铜线的储存和应用时的抗氧化性提出了要求。而且,在现有的键合铜丝在制备过程中包装和储存中也要加惰性气体保护;裸铜线的储存和使用寿命都很短,这也增加了生产和储存的成本,也进一步影响最终产品的使用效果。
发明内容
本发明针对现有铜线技术的上述不足,提供一种高抗氧化性的键合铜丝及其制备方法。
为了解决上述技术问题,本发明所采用的技术方案为:一种抗氧化键合铜丝,其特征在于:它包括抗氧化键合铜丝,所述铜丝的纯度≥99.99wt%,所述铜丝表面涂覆有厚度为5-60纳米的有机物层。该有机物覆层能够有效阻断铜和大气或腐蚀气体的接触,并且该覆层耐200℃以上的高温,起到防氧化的作用。
本发明所要解决的另一技术问题是,提供上述抗氧化键合铜丝的制备方法,用该方法制备的抗氧化键合铜丝产品成材率高,抗氧化性好,成本低。
该抗氧化键合铜丝的制备方法,包括以下工艺步骤:
1、提纯-纯度为99.99wt%的铜电解提纯出纯度为99.999wt%的高纯铜;
2、中间合金-制作中间合金,所述中间合金指钙-铜中间合金、银-铜中间合金、锗-铜中间合金;
3、所述制作中间合金,包括以下顺序的工艺步骤:
a.按重量百分比称取步骤2得到的高纯铜98%~99%,称取钙或银或锗1%~2%;
b.投料,高纯铜和钙或银或锗放入坩埚中;
c.真空熔炼:真空熔炼的温度达到铜的熔点后,待完全熔化后保持温度精炼;
d.浇铸,合金液倒入石墨锭模中;
以上步骤制作出一种中间合金,按同样的工艺步骤制作出另外几种中间合金;
4、竖式熔炼:将步骤3得到的中间合金在惰性气体氩气的保护下进行熔炼,拉铸,形成金棒;熔炼温度为900~1300℃;
5、拉丝:将熔铸的铜棒在拉丝机上逐步拉细,直至要求的直径;其拉丝过程中的模具延伸率为5%~18%,拉丝速度为3~15m/s;
6、退火:退火温度为300~600℃,退火速度为0.3~2m/s,退火后进行表面处理;
7、覆层:覆层为本发明的关键工序,退火后的表面处理指在键合铜丝表面涂覆有机物层,该有机物层由表面活性剂、溶剂、凝固剂及高分子化合物组成;
8、包装。
与现有技术相比,本发明的键合铜丝具有以下显著优点和有益效果:
1.本发明的微量元素选用钙、银或锗,铜能提高金属延伸率,提高材料的高温强度;钙主要是降低键合铜丝的弧度;银元素和锗元素的添加与合理配比使制备出的键合铜丝具有较好的低长弧度,满足半导体行业对键合铜丝的高需要。
2.本发明的键合铜丝的制备方法中在退火后进行一个覆层处理,即在键合铜丝表面附上一层有机物层,能在键合铜丝表面形成一层很薄很致密的保护层,这层保护层有效防止了键合铜丝的氧化,使制备出的键合铜丝在储存和运输中保证不产生氧化,并且该覆层材料可以耐受200℃以上的高温,从而有效解决铜线氧化问题。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明,但并不仅限于以下实施例。
实施例1
本发明键合铜丝按以下工艺步骤制备:
1)、纯度为99.99wt%的铜电解提纯出纯度为99.999wt%的高纯铜;原料纯度为99.99wt%的铜为市售的普通纯度的金材料,将此原料通过电解的方式提纯到99.999wt%,具体方法为:将市售的铜作为阳极,挂于阳极导电棒上,惰性碳材料作为阴极,挂于阴极导电棒上,保持阳极和阴极平行;在电解槽中加入硫酸铜溶液作为电解液,电解过程中控制槽压在0.6-1.2V,保证电解液液面高度。电解析出的铜用纯水洗净,洗至中性,最后放入保护气体烘箱中烘干得到99.999wt%的高纯铜;
2)、将高纯铜放入中频感应炉内进行熔炼,使之化成铜液,保温继续精,之后倒入石墨坩埚内进行铸锭;
3)、制作中间合金,本实施例的中间合金包括钙-铜中间合金、锗-铜中间合金和银-铜中间合金,各种中间合金的制作方法及过程完全相同,下面仅以钙-铜中间合金为例:
钙-铜中间合金的制作过程包括以下工艺步骤:
a.按重量百分比称取步骤2)得到的高纯铜98%~99%,钙1%~2%;
b.将高纯铜和钙放入坩埚中;
c.在中频感应炉内进行真空熔炼,待完全熔化后保持温度精炼,使高纯铜与添加元素充分混合均匀;
d.浇铸,将铜液缓慢倒入石墨锭模中,保持真空。待炉内完全冷却下来后,开启注气阀门,并打开炉盖;
e.将生成的中间合金用纯水冷却,再用压缩空气吹干;
然后,再按同样的重量百分比及同样的工艺步骤制作出锗-铜中间合金和银-铜中间合金;
4)、采用竖式熔炼对步骤3)获得的中间合金进行进一步的熔炼:
将部分高纯金放入坩埚内,将中间合金放入合金槽内,装好石英罩加上盖,用密封胶将石英罩及上盖密封好;
开启真空泵,打开抽气阀门,开始抽真空,当压力表显示为-0.1Pa,往炉内充氩气;
设定加热温度为900~1000℃,开始升温,待高纯金完全熔化后,投入中间合金;
启动按钮开始拉铸,形成金棒;
5)、将熔铸的金棒在拉丝机上逐步拉细,直至要求的直径。拉丝过程中的模具延伸率为5%~18%,拉丝速度为3~15m/s;
6)、拉丝的成品线传到退火工序退火,根据性能要求设定合适的温度进行退火;
7)、打开覆层液开关使覆层液缓慢流出,根据直径要求设定相应的覆层速度,速度为1~10m/s;即在键合铜丝表面附上一层有机物层,有机物层由10%表面活性剂、10%溶剂、10%凝固剂及70%高分子化合物组成;具体方式为使键合铜丝从退火炉出线后浸入注满涂敷液体的槽子,依靠液体表面张力的作用使铜线浸润在液面以下,使有机物层均匀涂布于键合铜丝表面;
8)、涂敷了有机物层的铜线直接进入烘烤箱,在150-300℃下进行在线烘干;
9)、将贴好标签的铜丝,低轴每10轴、高轴每6轴放入塑料袋中进行包装,用塑封封口机封好袋口,封口应平整、牢固,放入包装盒内。
实施例2
按以下表1中指定的各组分含量重复实施例1的方法:
表1 实施例1-2产品组分含量以及产品性能指标
表1中通过在键合铜丝表面涂覆有机物层,该有机物层为10%聚乙烯吡咯烷酮表面活性剂、10%异丙醇/正硅酸四乙酯/氨水溶剂、10%聚合氯化铝凝固剂其余为有机硅绝缘漆;该有机物层还可以是10%油烯醇聚氧乙烯醚表面活性剂、20%异丙醇/正硅酸四乙酯/氨水溶剂、15%的聚丙烯酰胺凝固剂其余有机硅绝缘漆的实验对比,各实施例的性能测试参数都说明,本发明的键合铜丝都可以达到指标,具有针涂层结合力高,针孔率低,耐高温,耐氧化的特性。
Claims (4)
1.一种抗氧化键合铜丝,其特征在于:它包括抗氧化键合铜丝,所述铜丝的纯度≥99.99wt%,所述铜丝表面涂覆有厚度为5-60纳米的有机物层。
2.根据权利要求1所述一种抗氧化键合铜丝的制备方法,其特征在于:包括以下步骤:
1)提纯-纯度为99.99wt%的铜电解提纯出纯度为99.999wt%的高纯铜;
2)中间合金-制作中间合金,所述中间合金指钙-铜中间合金、银-铜中间合金、锗-铜中间合金;
3)所述制作中间合金,包括以下顺序的工艺步骤:
a.按重量百分比称取步骤2)得到的高纯铜98%-99%,称取钙或银或锗1%-2%;
b.投料,将高纯铜和钙或银或锗放入坩埚中;
c.真空熔炼:真空熔炼的温度达到铜的熔点后,待完全熔化后保持温度精炼;
d.浇铸,将合金液倒入石墨锭模中;
以上步骤制作出一种中间合金,按同样的工艺步骤制作出另外几种中间合金;
4)、竖式熔炼:将步骤3)得到的中间合金在惰性气体氩气的保护下进行熔炼,拉铸,形成铜棒;熔炼温度为900-1300℃;
5)、拉丝:将熔铸的铜棒在拉丝机上逐步拉细,直至要求的直径;其拉丝过程中的模具延伸率为5%-18%,拉丝速度为3-15m/s;
6)、退火:退火温度为300-600℃,退火速度为0.3-2m/s,退火后进行表面处理;
7)、覆层:覆层为本发明的关键工序,退火后的表面处理指在键合铜丝表面涂覆有机物层,该有机物层由10-12%聚乙烯吡咯烷酮表面活性剂、10-20%异丙醇/正硅酸四乙酯/氨水溶剂、10-15%聚合氯化铝凝固剂其余为有机硅绝缘漆;
8)、包装。
3.根据权利要求2所述一种抗氧化键合铜丝的制备方法,其特征在于:所述有机物层由10%聚乙烯吡咯烷酮表面活性剂、10%异丙醇/正硅酸四乙酯/氨水溶剂、10%聚合氯化铝凝固剂其余为有机硅绝缘漆。
4.根据权利要求2所述一种抗氧化键合铜丝的制备方法,其特征在于:所述有机物层由10%油烯醇聚氧乙烯醚表面活性剂、20%异丙醇/正硅酸四乙酯/氨水溶剂、15%的聚丙烯酰胺凝固剂其余有机硅绝缘漆。
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CN109402445A (zh) * | 2018-11-09 | 2019-03-01 | 上海理工大学 | 一种抗氧化铜基合金键合引线及其制备方法 |
CN109637935A (zh) * | 2018-11-14 | 2019-04-16 | 世纪电缆有限公司 | 一种抗氧化铜丝的制备方法 |
CN111504065A (zh) * | 2020-03-30 | 2020-08-07 | 安徽广宇电子材料有限公司 | 一种银基合金键合线合金材料熔炼设备 |
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