CN108385092A - 一种银及银涂层的无铬钝化液及其钝化方法 - Google Patents
一种银及银涂层的无铬钝化液及其钝化方法 Download PDFInfo
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
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Abstract
本发明属于冶金金属材料表面技术领域，公开了一种银及银涂层无铬钝化液及其钝化方法。包括钼酸盐或钨酸盐、去除剂以及络合剂。所述钼酸盐或钨酸盐可选自碱金属钼酸盐或碱金属钨酸盐中的一种或几种，所述去除剂可选自氯化物，所述络合剂可选自次氯酸盐。所述钝化方式为将银及银涂层浸入制备的溶液中，浸渍时间为1～3min，浸渍温度不超过60℃，取出银及银涂层，洗涤干燥，得到银及银涂层钝化膜。所述钝化液不含有对人体和环境有害的六价或三价铬，钝化工艺简单，成本低廉，可控性好，膜层生长迅速以及耐蚀性好，可在工业领域进行产业化推广。
Description
技术领域
本发明涉及冶金金属材料表面技术领域，特别涉及通过钝化在银和银涂层上获得保护性和装饰性涂层的技术领域。
背景技术
银及其制品广泛用于适用于家电行业、电子行业、航空工业、珠宝行业等。尽管银属于贵金属，其化学性质相对比较稳定，但仍然会受到腐蚀。这种现象是由许多外部因素导致的，其中影响因素最大的是硫及其化合物。当金属银被硫及其化合物腐蚀而形成硫化银时，其外观变成黑色或灰色，这对金属银的外观和性能都有非常不利的影响。
现阶段，在保护金属银及银涂层表面免受腐蚀方面，实际运用的方法如：利用其它更稳定的金属膜涂覆银、无机盐溶液钝化、应用有机清漆保护层、在高分子有机化合物溶液中抑制其作用等等。其中，最常用的方法是在盐溶液中钝化银。铬酸盐钝化因其所获钝化膜耐蚀性优良、成本低廉、操作方便而得到广泛的应用，例如铬酸盐、氯化钾和氢氧化铵是常见的银钝化用溶液组分。但铬酸盐含六价铬，毒性高，易致癌，对人体与环境危害严重，随着环保意识的增强，含六价铬废料的排放受到严格的限制，欧盟颁布的法规明令禁止或限制涉及六价铬工艺的使用，铬酸盐工艺将逐步退出应用领域。
因此，开发无毒、环保的绿色钝化技术已成该领域发展的必然趋势。铬酸盐钝化的替代技术开发正受到广泛关注，各种系列的无铬钝化技术如稀土系、钛/锆系、有机/无机复合体系等处理工艺相继出现。然而目前还没有相关报道关于银及银涂层的无铬钝化液的报道。本发明报道了一种银及银涂层表面的无铬钝化工艺，在银和银涂层上产生耐腐蚀氧化物涂层，并且不使用含有有毒成分的物质，成本低廉、膜层生长迅速、简单易行，易于产业化推广。
发明内容
本发明的目的在于提供一种无毒环保的银及银涂层的无铬钝化液。所述钝化液既可解决传统六价铬工艺的毒性环境污染问题，同时高效节能，提高银及银涂层的耐腐蚀性。
本发明的另一目的在于提供一种银及银涂层的无铬钝化方法。本发明采用上述银及银涂层无铬钝化液对银及银涂层进行钝化处理，所述银及银涂层钝化方法成本低廉、操作简单、可控性好、膜层生长迅速以及耐蚀性好，可在工业领域进行产业化推广。
本发明的目的通过以下技术方案实现：
一种银及银涂层用无铬钝化液，包括钼酸盐或钨酸盐、去除剂以及络合剂。
所述银及银涂层用无铬钝化液中钼酸盐或钨酸盐的质量浓度为10～180g/L，优选为15～150g/L，更优选为15～45g/L。
所述银及银涂层用无铬钝化液中去除剂的质量浓度为20～60g/L，优选为30～50g/L，更优选为30～45g/L。
所述银及银涂层用无铬钝化液中络合剂的质量浓度为10～30g/L，优选为10～20g/L，更优选为10～15g/L。
所述钼酸盐或钨酸盐可选自碱金属钼酸盐或碱金属钨酸盐中的一种或几种，所述钼酸盐优选为钼酸钾(K2MoO4)，所述钨酸盐优选为钨酸钾(K2WO4)。所述去除剂可选自氯化物，优选碱金属氯化物，更优选氯化钾。所述络合剂可选自次氯酸盐，优选碱金属次氯酸盐，更优选次氯酸钾。
本发明中通过大量实验研究，发现引入钼酸盐或钨酸盐溶液，是由于需要在银和银涂层表面形成保护性转化膜。测定钼酸盐或钨酸盐溶液含量在10～180g/L范围内的主要依据，是氧化金属与氧化剂组的亲和力。在180g/L以上，溶液中氧化金属酸盐含量的增加，会导致银的急剧发酵，这会降低涂层的保护性能。在10g/L以下，溶液中氧化金属酸盐含量的减少，会导致处理速度的急剧减缓，处理时间倍增，而且所得到的涂层可能会与碱产生不良反应，保护性能低下。
以10～30g/L的次氯酸盐溶液作为配体，与银阳离子形成配合物，并将电极电位转移到负电荷的区域，这使得钼酸盐或钨酸盐可以作为氧化剂，而形成非化学计量的氧化物。在溶液中，超过30g/L的次氯酸盐含量，其增加会导致银阳离子的急剧增加。低于10g/L的次氯酸盐含量，其降低不能够形成上述配合物。均不利于在银及银涂层表面形成耐腐蚀性保护膜。
氯化盐的引入是为了确保氯离子的存在。其作为去除剂，可以消除银表面的天然氧化物膜，这提供了耐腐蚀性涂层形成过程的加速条件。溶液中氯化盐的含量少于20g/L时，会导致形成的涂层性能较差。同时，氯化盐的含量超过60g/L后，并不会改变涂层的特性，反而导致成本增高。此外，氯化盐的含量过高，还将会导致新的腐蚀产生。
所述银及银涂层无铬钝化液，是将钨酸盐或钼酸盐、络合剂和去除剂依次加入水中，待每一种成分溶解完全后加入后续的一种成分，当全部溶解后，调节水量，使其达到实验所需体积，得到所述银及银涂层无铬钝化液。
一种银及银涂层的钝化方法，具体包括以下步骤：
(1)前处理
(2)钝化处理：采用上述银及银合金无铬钝化液将银及银涂层进行钝化处理，所述钝化处理方式为将银及银涂层浸入制备的钝化液中，浸渍时间为1～3min，浸渍温度不超过60℃，取出银及银涂层，洗涤干燥，得到钝化层。本发明在银及银涂层表面获得耐腐蚀性良好的钝化膜。
与现有技术相比，本发明具有如下优点：本发明首次提出了一种用于银及银涂层表面的无铬钝化液，所述钝化液不含有对人体和环境有害的六价或三价铬，钝化工艺简单，成本低廉，可控性好，膜层生长迅速以及耐蚀性好，现有技术中铬钝化层的腐蚀速率为0.42μA/cm2，而本发明钝化液钝化的涂层最佳腐蚀速率可为0.17μA/cm2，优于铬钝化层，可在工业领域进行产业化推广。
具体实施方式
下面结合实施例对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例
一种银及银涂层无铬钝化液的配制及钝化方法：
在含耐化学腐蚀材料例如塑料的浴中，倒入浴2/3体积的60～70℃热水。然后，加入钼酸钾或钨酸钾，搅拌使其溶解，再加入次氯酸钾和氯化钾。调节水量，使其达到实验所需体积。所述钼酸钾或钨酸钾、次氯酸钾和氯化钾的质量浓度如表1所示。将实验部件浸入制备的钝化液，浸渍温度为60℃，钝化时间如表1所示，形成保护涂层。然后，将钝化后的实验部件在清水中洗涤后干燥，并测试各组实验所得涂层的腐蚀速率，测量条件是：工作电极：钝化后的实验部件；辅助电极：石墨电极；参比电极：饱和甘汞电极，30％的盐酸条件下，20℃测得的阳极电流密度。
实验部件在无毒的钼酸钾或钨酸钾钝化液中处理后，形成废水。该废水可以通过引入酸进行纯化，产生不溶性沉淀物，过滤后产生无毒废水。
表1实验涂层各项性能测试
从表1的测试结果中可以看出，3号钝化液的腐蚀速率最低，即耐腐蚀性最强。且各组实验所产生的废水均为无毒。为了在刚性操作条件下，例如在海洋环境或受污染的工业区域中改善涂层的保护性能，可以根据需要在加工零件的表面涂上涂料和清漆。
对比例
一种银及银涂层含铬钝化液的配制及钝化方法：
在含耐化学腐蚀材料(例如塑料)的浴中，按如表2所示配制钝化液。将实验部件浸入制备的钝化液，浸渍温度为60℃，钝化时间如表2所示，形成保护涂层。然后，将钝化后的实验部件在清水中洗涤后干燥，并测试实验所得涂层的腐蚀速率，测量条件是：工作电极：钝化后的实验部件；辅助电极：石墨电极；参比电极：饱和甘汞电极，30％的盐酸条件下，20℃测得的阳极电流密度。
表2实验涂层各项性能测试
| 电解质组成/涂层性质 | 对比钝化液 |
| 铬酸盐，g/L | 100 |
| 氯化钾，g/L | 50 |
| 氢氧化铵，g/L | 15 |
| 溶液酸度，pH值 | - |
| 加工温度，℃ | 60 |
| 处理时间，min | 1 |
| 溶液的毒性 | 有毒 |
| 腐蚀速率，μA/cm2 | 0.42 |
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合和简化，均应为等效的置换方式，都包含在本发明的保护范围之内。
Claims (8)
1.一种银及银涂层无铬钝化液，其特征在于：包括钼酸盐或钨酸盐、去除剂以及络合剂。
2.根据权利要求1所述银及银涂层无铬钝化液，其特征在于：所述钼酸盐可选自碱金属钼酸盐中的一种或几种，所述钨酸盐可选自碱金属钨酸盐中的一种或几种，所述去除剂可选自氯化物，所述络合剂可选自次氯酸盐。
3.根据权利要求1或2所述银及银涂层无铬钝化液，其特征在于：所述钼酸盐为钼酸钾，所述钨酸盐为钨酸钾，所述去除剂为碱金属氯化物，所述络合剂为碱金属次氯酸盐。
4.根据权利要求1或2所述银及银涂层无铬钝化液，所述钼酸盐或钨酸盐的质量浓度为10～180g/L，所述去除剂的质量浓度20～60g/L，所述络合剂的质量浓度为10～30g/L。
5.根据权利要求1或2所述银及银涂层无铬钝化液，所述钼酸盐或钨酸盐的质量浓度为15～150g/L，所述去除剂的质量浓度为30～50g/L，所述络合剂的质量浓度为10～20g/L。
6.根据权利要求1或2所述银及银涂层无铬钝化液，所述钼酸盐或钨酸盐的质量浓度为15～45g/L，所述去除剂的质量浓度为30～45g/L，所述络合剂的质量浓度为10～15g/L。
7.一种使用权利要求1～6任一项所述银及银涂层无铬钝化液的银及银涂层钝化方法，其特征在于：包括如下步骤：
(1)前处理；
(2)钝化处理：采用权利要求1～6中所述银及银合金无铬钝化液将银及银涂层进行钝化处理，所述钝化处理为将银及银涂层浸入制备的钝化液中，浸渍时间为1～3min，浸渍温度不超过60℃，取出银及银涂层，洗涤干燥。
8.根据权利要求7所述的钝化方法，其特征在于：浸渍时间为1min，浸渍温度为60℃。
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