CN1619012A - 用于沉积不含镍和铬（vi）的金属消光层的方法 - Google Patents

用于沉积不含镍和铬（vi）的金属消光层的方法 Download PDF

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CN1619012A
CN1619012A CNA2004100952608A CN200410095260A CN1619012A CN 1619012 A CN1619012 A CN 1619012A CN A2004100952608 A CNA2004100952608 A CN A2004100952608A CN 200410095260 A CN200410095260 A CN 200410095260A CN 1619012 A CN1619012 A CN 1619012A
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metal
plating
chromium
nickeliferous
delustring
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安德烈亚斯·默比乌斯
约阿希姆·布雷希特
彼得·皮斯
汉斯-保罗·沙夫
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MacDermid Enthone Inc
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Abstract

本发明涉及一种用于在基材上沉积不含镍和铬(VI)的金属镀层以及制备这种镀层的方法。根据本发明的方法具有下列工艺步骤a)用第一消光层镀覆基材，和b)用吸收第一金属镀层消光效应的第二金属镀层使第一消光金属镀层金属化，以得到具有消光表面的经镀覆的基材，其特征在于，第一消光金属镀层是不含镍的和第二金属镀层是不含镍和铬(VI)的，在此用于制备第一消光金属镀层的金属含有至少一种由铜、银、锡、锌类构成的金属或是一种不含镍的合金，而用于制备第二金属镀层的金属是至少一种由铜、锡、锌、铬(III)、银、金、钌、铂、钯类构成的金属或是这些金属的合金。

Description

用于沉积不含镍和铬(VI)的金属消光层的方法
本发明涉及一种用于在基材上沉积不含镍和铬(VI)的金属消光层的方法。
金属消光层在许多不同领域中用于功能性的或装饰性的表面改善处理。例如在首饰制造中表面出于美观的原因而用相应的消光层镀覆。在家用电器或烹调器具或装置的领域中，表面出于装饰的原因常常带有消光层。
在迄今为止的现有技术中已知的消光层由含镍的-和用于覆盖层大多由含铬(VI)的电解液沉积，从而是含镍的。虽然经仔细小心的操作，特别是在镀铬以后以冲洗的方式时铬(VI)在最终镀层中未能证实，但总是还有一些对于这种由这样的电解液沉积而成镀层的顾虑。
镍可在强烈的皮肤接触或通过食品有微量镍吸收时导致变应原反应。在首饰制品的情况下正是紧密的皮肤接触和通过汗水和湿气促进镍解脱而导致强烈的皮肤刺激。在家用电器或烹调装置或器具的情况下食品与经消光的表面接触可能导致镍的溶解析出，因为铬镀层不足以覆盖显微结构表面。
出于上述的原因，正是在首饰品工业中以及在家用电器和烹调器具或装置的制备领域中力求避免应用这样的表面镀层。
因为经消光的表面具有很大的美观作用，所以现在这种相应的表面尽管有它的缺点还是在上述的领域中有广泛的应用。
所以考虑到上述情况，本发明的任务在于，提出一种用于沉积消光的、不含镍和铬(VI)的金属镀层以及制备这种镀层的方法。
根据本发明该任务通过下述工艺步骤用沉积不含镍和铬(VI)金属消光层的方法而解决
a)用第一消光层镀覆基材
b)用吸收第一金属镀层消光效应的第二金属镀层使第一消光金属镀层金属化，以获得具有消光表面的镀覆基材，
其特征在于，第一消光金属镀层是不含镍的和第二金属镀层是不含镍和铬(VI)的，在此用于制备第一消光金属镀层的金属含有至少一种由铜、银、锡、锌类构成的金属或是一种不含镍的合金；而用于制备第二金属镀层的金属是至少一种由铜、锡、锌、铬(III)、银、金、钌、铂、钯类构成的金属或是这些金属的一种合金。
对于根据本发明的方法应用消光铜镀层作为第一消光金属镀层证明是特别合适的。这样的铜镀层可以通过现有技术已知的电镀金属化或化学金属化的方法而获得。
特别是由含铜-锡的合金，如白青铜构成的金属镀层作为吸收第一金属镀层消光效应的第二金属镀层证明是有利的。这样的镀层使人有经镀铬的消光的镍镀层的美观的印象，然而没有变应原的倾向和具有足够的机械稳定性和耐腐蚀性。
假如出于应用技术的原因而要提高机械稳定性，根据本发明的方法提出，在吸收第一金属镀层消光效应的第二金属镀层上再用具有相应机械性能的第三金属镀层金属化。由含铬(III)的电解液沉积铬镀层或铬合金镀层，如与钒、钼、碳、磷或钨的铬合金，或通过CVD或PVD镀覆的硬镀层，如碳化铬、氮化-/碳化钛、氮化-/碳化锆、二氧化硅或DLC(象碳的金刚石)或由这些层构成的复合层证明是合适的。
下面举例描述了适用于实施本发明方法的电解液，但并不局限于这种电解液，这是酸性的消光铜电解液，其通过加入而生成消光镀层：
实施例1：
18-25g/l           Cu2+
180-210g/l         H2SO4
30-80mg/l          Cl-
1-10ml/l           Enthone公司的Cuprostar LP1添加物
18-35℃            温度范围
1-5A/dm2          电流密度
在根据本发明的方法中其它可用于沉积消光铜镀层的电解液的例子是无电流的铜电解液，如Enthone公司的ENPLATE CU 872。
采用如前举例所述的铜电解液得到的消光铜镀层可以根据本发明在下一步工艺步骤中用铜-锡-合金金属化。优选的用于电镀沉积铜-锡-合金，如白青铜的电解液主要含有以氰化物形式的锡-和铜离子、合适的添加剂碱液和游离氰化物。含有芳族的、非离子交联剂的烷基磺酸的电解液也是可用的。还可在电解液中选择地附加含有稳定剂和/或络合剂、阴离子的和/或非离子的、脂肪族的交联剂、抗氧剂以及其他的金属盐类。
主要用于沉积青铜加入到电解液中的金属锡和铜首先是可作为氰化物存在和在酸性的电解液的情况下可作为烷基磺酸的盐类，优选作为甲基磺酸盐存在或可作为无机酸盐类，优选作为硫酸盐存在。作为锡盐在电解液中特别优选应用的是甲基磺酸锡，其优选以5-195g/l电解质的量加入到电解液中。这相当于加入2-75g/l的2-价锡离子。作为铜盐在电解液中特别优选应用的是甲基磺酸铜，其优选以8-280g/l电解质的量加入到电解液中。这相当于加入2-70g/l的2-价铜离子。
因为在酸性介质中沉积速度要高得多，所以酸，优选是无机酸和/或烷基磺酸以140-382g/l电解质的量加入到电解液中。使用甲基磺酸是特别优选的，因为其一方面决定了金属盐类有卓越的溶解性；而另一方面由于它的酸强度可预先或容易调节对于该方法所必需的pH-值。此外甲基磺酸还具有优越的性能，即主要是有助于电镀槽的稳定。
为了更清楚地解释本发明以下举例示出用于沉积白青铜的电解液，然而其不应限制本发明。
实施例2：
5g/l            Sn2+
10g/l           Cu2+
240g/l          甲基磺酸
32.2g/l         芳族的、非离子交联剂
2g/l            抗氧剂
25g/l           稳定剂/络合剂
实施例3：
18g/l           Sn2+
2g/l            Cu2+
258g/l          甲基磺酸
9g/l            芳族的、非离子交联剂
实施例4：
17.0-25.0g/l    Sn2+
10.0-15.0g/l    Cu2+
1.3-1.9g/l      Zn2+
45.0-60.0g/l    氰化钾
12.4-12.9       pH-值
0.5-2ml/l        交联剂
0.1-1ml/l        抛光添加剂
50.0-60.0℃      温度范围
2.0-4.0A/dm2     电流密度
实施例5：Enthone公司的Bronzex WMF
8.0-12.0g/l      Sn2+
5.0-10.0g/l      Cu2+
1.0-3.0g/l       Zn2+
23.0-30.0g/l     氰化钾
0.1-2ml/l        Enthone公司的四号ATC溶液
0.1-2ml/l        Enthone公司的BRONZEX WMF抛光剂NG
13.2-13.6        pH-值
39.0-45.0℃      温度范围
0.3-0.7A/dm2     电流密度

Claims (11)

1.一种具有下列工艺步骤的用于沉积不含镍和铬(VI)金属消光层的方法
a)用第一消光金属镀层镀覆基材
b)用吸收第一金属镀层消光效应的第二金属镀层使第一消光金属镀层金属化，以得到具有经消光表面的镀覆基材，
其特征在于，第一消光金属镀层是不含镍的和第二金属镀层是不含镍和铬(VI)的，在此用于制备第一消光金属镀层的金属含有至少一种由铜、银、锡、锌类构成的金属或是一种不含镍的合金，而用于制备第二金属镀层的金属是至少一种由铜、锡、锌、铬(III)、银、金、钌、铂、钯类构成的金属或是这些金属的一种合金。
2.根据权利要求1的方法，其特征在于，第一金属层是化学沉积的。
3.根据权利要求1的方法，其特征在于，第一经沉积的金属层是电解沉积的。
4.根据上述权利要求至少之一的方法，其特征在于，第二金属层的金属是化学沉积的。
5.根据权利要求1-3之一或多项的方法，其特征在于，第二层的金属是电解沉积的。
6.根据上述权利要求之一或多项的方法，在此第二金属层用至少一个第三层镀覆，其特征在于，为了制备第三金属层具有至少一种由铬或铬合金类构成的金属，铬合金例如是与钒、钼、碳、磷或钨的合金。
7.铬或具有钒、钼或钨的铬合金被沉积。
8.根据权利要求1-5之一或多项的方法，在此第二金属层用至少一个第三层镀覆，其特征在于，为了制备第三金属层要镀覆至少一单独的硬层或至少一层附加地通过CVD或PVD镀覆的硬层，如碳化铬、氮化-/碳化钛、氮化-/碳化锆、二氧化硅或DLC(象碳的金刚石)或由这些层构成的复合层。
9.一种不含镍和铬(VI)的金属消光层，其通过下列工艺步骤制备
a)用第一消光金属镀层镀覆基材
b)用吸收第一金属镀层消光效应的第二金属镀层使第一消光金属镀层金属化，
其特征在于，第一消光金属镀层是不含镍的和第二金属镀层是不含镍和铬(VI)的，在此用于制备第一消光金属镀层的金属含有至少一种由铜、锡、锌、铬(III)、银、金、钌、铂、钯类构成的金属，或是一种合金；而用于制备第二金属镀层的金属是至少一种由铜、锡、锌、铬(III)、银、金、钌、铂、钯类构成的金属，或是一种合金。
10.根据权利要求7的不含镍和铬(VI)的金属消光层，其特征在于，第二金属层用至少一个第三层镀覆，在此第三层具有至少一种由铬或铬合金类构成的金属，铬合金例如是与钒、钼、碳、磷或钨的合金。
11.根据权利要求7的不含镍和铬(VI)的金属消光层，其特征在于，第二金属层用至少一个第三层镀覆，在此第三层由一单独的硬层或一层附加通过CVD或PVD镀覆的硬层构成，如碳化铬、氮化-/碳化钛、氮化-/碳化锆、二氧化硅或DLC(象碳的金刚石)或由这些层构成的复合层。
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