CN1281787C - 镁及镁合金高耐蚀性复合镀层及其制备工艺 - Google Patents

镁及镁合金高耐蚀性复合镀层及其制备工艺 Download PDF

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CN1281787C
CN1281787C CN 200410018471 CN200410018471A CN1281787C CN 1281787 C CN1281787 C CN 1281787C CN 200410018471 CN200410018471 CN 200410018471 CN 200410018471 A CN200410018471 A CN 200410018471A CN 1281787 C CN1281787 C CN 1281787C
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magnesium
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nickel
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alloy
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刘新宽
胡文彬
丁文江
向阳辉
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Shanghai Jiaotong University
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Abstract

一种镁及镁合金高耐蚀性复合镀层及其制备工艺，用于有色金属材料表面处理领域。复合镀层以化学镀镍层作底层，厚度为20-25微米，电镀锌镍合金层为表层，厚度为8-10微米。工艺如下：镁合金化学镀镍采用美国材料试验协会标准B480-88，施镀时间为1.4-2小时，镀层厚度为20-25微米，镀层磷含量为9-12%；电镀锌镍合金：使用的镀液组成及工艺条件如下：氢氧化钠8-15%，氧化锌2-5%，氯化镍0.5-3%，乙二胺2-4%，三乙醇胺2-4%，酒石酸钾钠0.5-3%，DE 0.2-0.8%，十二烷基磺酸钠0.01-0.1%，余量为水，电流密度为0.5-5A/dm2，电镀时间为30分钟，镀层镍含量为13-18%；采用锌镍合金黑色钝化工艺。本发明复合镀层厚度不超过35微米，耐蚀性很好，中性盐雾耐久时间可达1000小时。利用本发明得到的镀层可以作为苛刻环境中镁及镁合金的保护层。

Description

镁及镁合金高耐蚀性复合镀层及其制备工艺
技术领域
本发明涉及金属复合镀层及其制备工艺，具体是一种镁及镁合金高耐蚀性复合镀层及其制备工艺。用于有色金属材料表面处理领域。
背景技术
镁合金是实际应用中最轻的金属结构材料，具有比重小，比强度、比刚度高，阻尼性、切削加工性、铸造性能好等优点，在汽车、机械、航空航天领域以及便携式电子仪表、计算机、手动工具及照相机部件等方面正得到日益广泛的应用。但是镁合金的耐蚀性很差。已经开发出的几种表面镀层如化学镀或者电镀层，其耐蚀防护效果有限。即使是耐蚀性好的化学镀层，如叶宏等人在《表面处理》2002年31卷第6期，32-35页上发表“镁合金化学镀镍工艺研究”一文，介绍了新开发的镁合金化学镀单一镀层中性盐雾耐久时间约为300小时，显然还无法满足苛刻环境下的耐蚀性要求。为提高镀层耐蚀性，通常采用增加镀层厚度的办法，参见美国材料学会镁及镁合金专用手册，1999年出版(ASM Specialty Handbook Magnesium and Magnesium Alloys.1999)，在苛刻环境中，手册推荐的铬镀层和铜-镍-铬镀层最小厚度为64微米。
在钢铁基体上，已经开发了很多耐蚀性好的镀层，如锌镍合金。但是由于镁高的电化学活性和被大多数镀液快速腐蚀，这些工艺不能直接应用到镁合金上。而且镁的腐蚀电位很低，常用化学镀或者电镀层对镁合金都属于阴极，对钢铁而言的牺牲阳极保护应用到镁合金上就成了阴极保护，镀层的设计原理就要发生变化。对阴极镀层，令人满意的耐蚀性，尤其是苛刻环境下，只有在镀层无孔时才能达到，而镁及镁合金大部分以铸件生产，不可避免地会产生夹杂、疏松、气孔等缺陷，铸件表面的缺陷严重影响镀层的质量，很难避免镀层不出现孔隙，这些孔隙依靠单一的化学镀或电镀过程是很难封闭的。这就是镁合金镀层耐蚀性不高的原因。
发明内容
本发明的目的在于针对现有镁合金镀层耐蚀性差的缺点，提供一种镁及镁合金高耐蚀性复合镀层及其制备工艺，其镀层厚度不超过35微米，而镀层耐中性盐雾时间可达1000小时以上。
本发明是通过以下技术方案来实现的，本发明镁及镁合金高耐蚀性复合镀层包括化学镀镍层、电镀锌镍合金层；化学镀镍层作底层，厚度为20-25微米，电镀锌镍合金层为表层，厚度为8-10微米，镀层总厚度不超过35微米。其中化学镀镍层磷含量为8-12％，电镀锌镍合金层镍含量为13-18％。
采用镁合金化学镀工艺，在镁合金基体上镀覆一层镍作为基底，先把镁基底保护起来。而且镍镀层可与标准电镀层相容，在镍基底上，就可开发高耐蚀性的镀层。
其次解决镀层气孔问题。通过化学镀层，将镀层中的孔隙降低到很低的程度。化学镀镍层的厚度选在20-25微米之间，厚度太薄，孔隙减少的程度有限；厚度太厚，镀层脆性增大，成本还大大增加。而且，有些孔隙靠化学镀覆始终无法遮蔽，镀层厚度增加就失去意义。这些孔隙就靠随后的电镀层封闭。采用碱性镀液电镀锌镍合金，利用镀液强的整平作用和分散作用，可以填没化学镀层的孔隙并将其封闭。化学镀镍层本身就很致密，加上后续电镀锌镍合金，就可解决镀层中孔隙问题。只要将镁合金基体完全包覆起来，表层锌镍合金镀层耐蚀性好的优点就能充分发挥出来。
本发明高耐蚀性复合镀层的制备工艺，包括以下步骤：
(一)镁合金化学镀镍。化学镀工艺采用美国材料试验协会标准B480-88。施镀时间为1.4-2小时，镀层厚度为20-25微米，镀层磷含量约为8-12％。
(二)电镀锌镍合金。电镀锌镍工艺中使用的镀液组成(重量百分比)及工艺条件如下：氢氧化钠8-15％，氧化锌2-5％，氯化镍0.5-3％，乙二胺2-4％，三乙醇胺2-4％，酒石酸钾钠0.5-3％，DE0.2-0.8％，十二烷基磺酸钠0.01-0.1％，余量为水。电流密度为0.5-5A/dm2，电镀时间为30分钟。阳极采用不锈钢板，温度为室温。
电镀锌镍合金工艺中使用的镀液组成(重量百分比)及工艺优选为：氢氧化钠11-13％，氧化锌3-5％，氯化镍1.2-1.7％，乙二胺2.5-3.5％，三乙醇胺2.5-3.5％，酒石酸钾钠1.2-1.7％，DE0.3-0.5％，十二烷基磺酸钠0.02-0.04％，余量为水。电流密度为2.5A/dm2，电镀时间为30分钟。得到的镀层厚度在8-10微米，镍含量约为13-18％。
(三)镀层黑色钝化。黑色钝化处理工艺采用锌镍合金黑色钝化工艺。
与现有镁合金镀层相比，本发明的优点在于复合镀层厚度不超过35微米条件下耐蚀性很好，耐盐雾试验时间可达1000小时。利用本发明得到的镀层可以作为苛刻环境中镁及镁合金的保护层。
具体实施方式
下面通过实施例对本发明作进一步说明。
实施例一：
将镁合金AZ91铸件用化学镀工艺施镀2小时，得到镀层厚度为25微米，化学镀镍层磷含量约为9％。然后按照下面的配方和工艺电镀锌镍合金：氢氧化钠15％，氧化锌5％，氯化镍3％，乙二胺4％，三乙醇胺4％，酒石酸钾钠0.5％，DE0.8％，十二烷基磺酸钠0.03％，余量为水。电流密度为2.5A/dm2，电镀时间为30分钟。阳极采用不锈钢板，温度为室温。得到的锌镍合金镀层厚度为8-10微米，镍含量约为15％。最后镀层经黑色钝化处理。镀层总厚度约35微米。
按照ASTM B117标准进行中性盐雾实验，耐久时间可达1000小时以上。
实施例二
用镁合金AZ91铸件用化学镀工艺施镀1.4小时，得到镀层厚度为20微米，化学镀镍层磷含量约为9％。然后按照下面的配方和工艺电镀锌镍合金：氢氧化钠8％，氧化锌2％，氯化镍0.5％，乙二胺2％，三乙醇胺2％，酒石酸钾钠3％，DE0.2％，十二烷基磺酸钠0.01％，余量为水。电流密度为2.5A/dm2，阳极采用不锈钢板，温度为室温。电镀时间为30分钟，得到的锌镍合金镀层厚度为8-10微米，镍含量约为13％。最后镀层黑色钝化处理。镀层总厚度约为30微米。
按照ASTM B117标准进行中性盐雾实验，耐久时间可达800小时。
实施例三
将镁合金AZ91铸件用化学镀工艺施镀2小时，得到镀层厚度为25微米，化学镀镍层磷含量约为9％。然后按照下面的配方和工艺电镀锌镍合金：氢氧化钠12％，氧化锌4％，氯化镍1.5％，乙二胺3％，三乙醇胺3％，酒石酸钾钠1.5％，DE0.4％，十二烷基磺酸钠0.03％，余量为水。电流密度为2.5A/dm2，电镀时间为30分钟。阳极采用不锈钢板，温度为室温。得到的锌镍合金镀层厚度为8-10微米，镍含量约为16％。最后镀层经黑色钝化处理。镀层总厚度约35微米。
按照ASTM B117标准进行中性盐雾实验，耐久时间可达1000小时以上。
实施例四：
将镁合金AZ91铸件用化学镀工艺施镀2小时，得到镀层厚度为25微米，化学镀镍层磷含量约为9％。然后按照下面的配方和工艺电镀锌镍合金：氢氧化钠11％，氧化锌3％，氯化镍1.2％，乙二胺2.5％，三乙醇胺2.5％，酒石酸钾钠1.7％，DE0.3％，十二烷基磺酸钠0.02％，余量为水。电流密度为2.5A/dm2，电镀时间为30分钟。阳极采用不锈钢板，温度为室温。得到的锌镍合金镀层厚度为8-10微米，镍含量约为15％。最后镀层经黑色钝化处理。镀层总厚度约35微米。
按照ASTM B117标准进行中性盐雾实验，耐久时间可达1000小时以上。
实施例五：
将镁合金AZ91铸件用化学镀工艺施镀2小时，得到镀层厚度为25微米化学镀镍层磷含量约为9％。然后按照下面的配方和工艺电镀锌镍合金：氢氧化钠13％，氧化锌5％，氯化镍1.7％，乙二胺3.5％，三乙醇胺3.5％，酒石酸钾钠1.2％，DE 0.3％，十二烷基磺酸钠0.04％，余量为水。电流密度为2.5A/dm2，电镀时间为30分钟。阳极采用不锈钢板，温度为室温。得到的锌镍合金镀层厚度为8-10微米，镍含量约为15％。最后镀层经黑色钝化处理。镀层总厚度约35微米。
按照ASTM B117标准进行中性盐雾实验，耐久时间可达1000小时以上。

Claims (5)

1、一种镁及镁合金复合镀层，包括：化学镀镍层、电镀锌镍合金层，其特征在于，化学镀镍层作底层，厚度为20-25微米，电镀锌镍合金层为表层，厚度为8-10微米。
2、根据权利要求1所述的镁及镁合金复合镀层，其特征是，化学镀镍层磷含量为8-12％。
3、根据权利要求1所述的镁及镁合金复合镀层，其特征是，电镀锌镍合金层镍含量为13-18％。
4、一种镁及镁合金复合镀层的制备工艺，其特征在于，包括三个步骤：
(1)镁合金化学镀镍：施镀时间为1.4-2小时，镀层厚度为20-25微米，磷含量为8-12％；
(2)电镀锌镍合金：电镀锌镍合金工艺中使用的镀液组成及工艺条件如下：氢氧化钠8-15％，氧化锌2-5％，氯化镍0.5-3％，乙二胺2-4％，三乙醇胺2-4％，酒石酸钾钠0.5-3％，DE 0.2-0.8％，十二烷基磺酸钠0.01-0.1％，余量为水，电流密度为0.5-5A/dm2，电镀时间为30分钟，阳极采用不锈钢板，温度为室温；
(3)镀层黑色钝化：黑色钝化处理工艺采用锌镍合金黑色钝化工艺。
5、根据权利要求4所述的镁及镁合金复合镀层的制备工艺，其特征是，所述的电镀锌镍合金工艺中使用的镀液组成及工艺为：氢氧化钠11-13％，氧化锌3-5％，氯化镍1.2-1.7％，乙二胺2.5-3.5％，三乙醇胺2.5-3.5％，酒石酸钾钠1.2-1.7％，DE 0.3-0.5％，十二烷基磺酸钠0.02-0.04％，电流密度为2.5A/dm2。
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CN100408725C (zh) * 2005-12-30 2008-08-06 东北大学 一种金属镁及镁合金表面复合防护的方法
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CN102312238A (zh) * 2011-09-28 2012-01-11 中国计量学院 一种锌镍镀层的制备及其三价铬钝化工艺
CN103898588A (zh) * 2013-06-04 2014-07-02 无锡市锡山区鹅湖镇荡口青荡金属制品厂 一种预电镀锌镍合金的镁合金表面化学镀镍组合溶液
CN103710692A (zh) * 2013-12-20 2014-04-09 苏州市邦成电子科技有限公司 耐腐蚀sus301不锈钢带的制备方法
CN106282822B (zh) * 2016-08-24 2018-03-13 宁波亚大金属表面处理有限公司 一种输油管的加工工艺
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