CN103556132A - 一种铝合金用含SiC和石墨烯的镍磷基复合镀液 - Google Patents

一种铝合金用含SiC和石墨烯的镍磷基复合镀液 Download PDF

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CN103556132A
CN103556132A CN201310556604.XA CN201310556604A CN103556132A CN 103556132 A CN103556132 A CN 103556132A CN 201310556604 A CN201310556604 A CN 201310556604A CN 103556132 A CN103556132 A CN 103556132A
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周向志
祁惠光
顾浩
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Hangzhou Guangrong Science & Technology Co Ltd
YUYAO YITONG BRAKE SYSTEM FITTINGS FACTORY
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    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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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
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
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Abstract

本发明公开了一种铝合金用含SiC和石墨烯的镍磷基复合镀液。该镀液由化学镀镍磷镀液和含SiC和石墨烯的分散液组成。其中化学镀镍镀液中由镍盐20-30g/L、络合剂15-25g/L、还原剂15-30g/L、稳定剂2-5mg/L、缓冲剂10-20g/L及余量水组成，分散液由SiC、石墨烯和醇类高分子表面活性剂经磁力搅拌而成。将镍磷镀液和SiC和石墨烯分散液混合搅拌，形成含SiC和石墨烯的镍磷基复合镀层镀液。将含SiC和石墨烯的复合型化学镀镍磷镀液，通过化学镀浴和热处理在铝合金表面得到复合镀层，该镀层在硬度、耐磨性和防粘结性上较一般化学镀镍磷层有很大的提高。

Description

一种铝合金用含SiC和石墨烯的镍磷基复合镀液
技术领域
本发明涉及一种铝合金用含SiC和石墨烯的镍磷基复合镀液配方。主要采用将适用于铝合金表面的化学镀镍磷镀液和含SiC和石墨烯的分散液混合搅拌的方式得到复合镀液，其具有提高镀层硬度、耐磨性和防粘结性等作用。
背景技术
现代科学技术以及工业的发展对材料提出了更加全面和严苛的要求，其中材料表面的保护、改性、强化等方面的处理也变得越来越重要。化学镀镍磷技术因其优良的施镀特点，以及涂层具有硬度高、耐磨性强、耐腐蚀性好等优点，广泛应用于金属、塑料、陶瓷和半导体等非金属材料表面，用以改善材料表面性能。
铝合金因其具有质轻、比强度高等优点，在现代工业中得到广泛应用。但铝合金材料存在质软、摩擦系数高、磨损大、难润滑等缺点，限制了其应用。针对铝合金表面的化学镀镍磷技术是一种新型的改性技术，其能够提高铝合金表面的硬度、耐磨性，耐腐蚀性以及易焊接等性能，已在汽车、军事、机械、航天、计算机等领域得到广泛应用。
而该技术经过多年的发展，其对铝合金表面性能的改善已达到瓶颈，研究人员希望通过寻找理想的添加剂以及合理的工艺条件来得到高质量的镍磷合金镀层。近些年来，通过在化学镀过程中添加某些微粒实现微粒与合金共沉积得到复合镀层的方式，希望复合镀层兼具有基质金属镀层和复合粒子相的特性，提高镀层的综合性能。在此基础上，申请人引入SiC和石墨烯，SiC、石墨烯和镍磷合金复合镀层的综合性能较镍磷合金镀层活或SiC/镍磷复合镀层的体系有较大的提高。
发明内容
本发明针对现有技术的不足，提供了一种铝合金用含SiC和石墨烯的镍磷基复合镀液。
本发明通过将含SiC和石墨烯的分散液加入到化学镀镍磷镀液中，形成复合型化学镀镍磷镀液，该镀液在铝合金表面形成的镀层在硬度、耐磨性和防粘结性等得到提高。
铝合金表面含SiC和石墨烯的镍磷基复合镀液，由化学镀镍磷镀液和含SiC、石墨烯的分散液按体积比1∶1混合搅拌得到。化学镀镍磷镀液，每升由20-30g镍盐、15-25g络合剂、15-30g还原剂、2-5mg稳定剂、10-20g缓冲剂加入到蒸馏水中搅拌得到。其中镍盐为硫酸镍或氯化镍，络合剂为柠檬酸钠或羟基乙酸，还原剂为次磷酸钠或者次亚磷酸钠，稳定剂为硫脲或碘酸钾，缓冲剂为氯化铵。而含石墨烯的分散液，每升由20-80mg醇类高分子为分散剂，将10-20g的SiC粉体和10-25g的石墨烯粉体加入蒸馏水中，经超声分散30分钟，磁力搅拌120分钟得到。其中SiC粒子粒径范围为0.5-1.0μm，石墨烯粉末的平均厚度为3.5nm，直径为0.5-5μm。
本发明具有的有益效果：
(1)该镀液能够提高镀层的硬度。SiC、石墨烯微粒均具有较高的硬度，在镍磷镀层中形成硬质相，能够使复合镀层的承载能力提高。
(2)该镀液提高镀层的耐磨性。SiC、石墨烯粉末的引入可以改善界面的接触状态，使复合镀层的耐磨性得到提高。石墨烯的存在同时降低了镍磷镀层的表面能，有效地提高了镀层的防粘接性能。
(3)该镀液得到的镀层，与镍磷镀液或者单纯含SiC的镍磷复合镀液得到的镀层相比，石墨烯粉末的引入使镀层的硬度及耐磨性有了进一步的提升。
具体实施方式
下面以实施例的形式来说明本发明的效果，但不只是限于实施例。
本发明的配置过程如下：按20-30g/L镍盐、15-25g/L络合剂、15-30g/L还原剂、2-5mg/L稳定剂、10-20g/L缓冲剂的浓度加入到定量蒸馏水中搅拌，经过120分钟得到镍磷镀液。
以20-80mg/L的醇类高分子为分散剂，按10-20g/L和10-25g/L的浓度将粒径范围为0.5-1.0μm的SiC粉体和平均厚度为3.5nm、直径为0.5-5μm的石墨烯粉体加入定量蒸馏水中，经超声分散30分钟，磁力搅拌120分钟得到含SiC和石墨烯的分散液。
将体积比1∶1的镍磷镀液和含SiC、石墨烯分散液混合搅拌，形成铝合金用含SiC和石墨烯的镍磷基复合镀液。
以下结合实施例对本发明作进一步说明。
实施例1
按30g/L硫酸镍、25g/L柠檬酸钠、30g/L次亚磷酸钠、5mg/L硫脲、20g/L氯化铵的浓度加入到定量蒸馏水中搅拌，经过120分钟得到镍磷镀液。
以20mg/L的醇类高分子为分散剂，按10g/L和10g/L的浓度将粒径范围为0.5-1.0μm的SiC粉体和平均厚度为3.5nm，直径为0.5-5μm的石墨烯粉体加入定量蒸馏水中，经超声分散30分钟，磁力搅拌120分钟得到含石墨烯的分散液。
将体积比1∶1的镍磷镀液和含SiC、石墨烯的分散液混合搅拌，形成铝合金用含SiC、石墨烯的镍磷基复合镀液。
同时，将上述镍磷镀液用纯水稀释1倍，作为镍磷基复合镀液的对比液。
将两种镀液按以下工艺流程，使用相同的工艺参数在同样的铝合金汽车阀芯上进行化学镀镍。
超声波脱脂→超声波水洗→水洗→微蚀→水洗→水洗→除渍→水洗→水洗→一次浸锌→水洗→水洗→褪锌→水洗→水洗→二次浸锌→水洗→水洗→化学镀镍→水洗→水洗→热水洗→干燥→热处理
用Micro Pioneer XRF2000测厚仪测量镀层的厚度，用数显维氏硬度计InnovaTest400测试镀层的硬度。相关工作参数及测试结果如下：
Figure BDA0000410860630000031
实施例2
按25g/L硫酸镍、20g/L羟基乙酸、22g/L次磷酸钠、4mg/L的碘酸钾、18g/L氯化铵的浓度加入到定量蒸馏水中搅拌，经过120分钟得到镍磷镀液。
以80mg/L的醇类高分子为分散剂，按20g/L和25g/L的浓度将粒径范围为0.5-1.0μm的SiC粉体和平均厚度为3.5nm，直径为0.5-5μm的石墨烯粉体加入定量蒸馏水中，经超声分散30分钟，磁力搅拌120分钟得到含石墨烯的分散液。
将体积比1∶1的镍磷镀液和含SiC、石墨烯的分散液混合搅拌，形成铝合金用含SiC和石墨烯的镍磷基复合镀液。
同时，将上述镍磷镀液用纯水稀释1倍，作为镍磷基复合镀液的对比液。
将两种镀液按以下工艺流程，使用相同的工艺参数在同样的铝合金汽车阀芯上进行化学镀镍。
超声波脱脂→超声波水洗→水洗→微蚀→水洗→水洗→除渍→水洗→水洗→一次浸锌→水洗→水洗→褪锌→水洗→水洗→二次浸锌→水洗→水洗→化学镀镍→水洗→水洗→热水洗→干燥→热处理
用Micro Pioneer XRF2000测厚仪测量镀层的厚度，用数显维氏硬度计InnovaTest400测试镀层的硬度。相关工作参数及测试结果如下：
Figure BDA0000410860630000041
实施例3
按20g/L氯化镍、15g/L柠檬酸钠、15g/L次磷酸钠、2mg/L硫脲、10g/L氯化铵的浓度加入到定量蒸馏水中搅拌，经过120分钟得到镍磷镀液。
以40mg/L的醇类高分子为分散剂，按13g/L和15g/L的浓度将粒径范围为0.5-1.0μm的SiC粉体和平均厚度为3.5nm，直径为0.5-5μm的石墨烯粉体加入定量蒸馏水中，经超声分散30分钟，磁力搅拌120分钟得到含石墨烯的分散液。
将体积比1∶1的镍磷镀液和含SiC、石墨烯分散液混合搅拌，形成铝合金用含SiC和石墨烯的镍磷基复合镀液。
同时，将上述镍磷镀液用纯水稀释1倍，作为镍磷基复合镀液的对比液。
将两种镀液按以下工艺流程，使用相同的工艺参数在同样的铝合金汽车阀芯上进行化学镀镍。
超声波脱脂→超声波水洗→水洗→微蚀→水洗→水洗→除渍→水洗→水洗→一次浸锌→水洗→水洗→褪锌→水洗→水洗→二次浸锌→水洗→水洗→化学镀镍→水洗→水洗→热水洗→干燥→热处理
用Micro Pioneer XRF2000测厚仪测量镀层的厚度，用数显维氏硬度计InnovaTest400测试镀层的硬度。相关工作参数及测试结果如下：
Figure BDA0000410860630000051
实施例4
按22g/L硫酸镍、18g/L柠檬酸钠、21g/L次亚磷酸钠、3mg/L碘酸钾、12g/L氯化铵的浓度加入到定量蒸馏水中搅拌，经过120分钟得到镍磷镀液。
以60mg/L的醇类高分子为分散剂，按17g/L和20g/L的浓度将粒径范围为0.5-1.0μm的SiC粉体和平均厚度为3.5nm，直径为0.5-5μm的石墨烯粉体加入定量蒸馏水中，经超声分散30分钟，磁力搅拌120分钟得到含石墨烯的分散液。
将体积比1∶1的镍磷镀液和含SiC、石墨烯的分散液混合搅拌，形成铝合金用含SiC和石墨烯的镍磷基复合镀液。
同时，将上述镍磷镀液用纯水稀释1倍，作为镍磷基复合镀液的对比液。
将两种镀液按以下工艺流程，使用相同的工艺参数在同样的铝合金汽车阀芯上进行化学镀镍。
超声波脱脂→超声波水洗→水洗→微蚀→水洗→水洗→除渍→水洗→水洗→一次浸锌→水洗→水洗→褪锌→水洗→水洗→二次浸锌→水洗→水洗→化学镀镍→水洗→水洗→热水洗→干燥→热处理。
用Micro Pioneer XRF2000测厚仪测量镀层的厚度，用数显维氏硬度计InnovaTest400测试镀层的硬度。相关工作参数及测试结果如下：

Claims (9)

1. 一种铝合金用含SiC和石墨烯的镍磷基复合镀液，其特征在于：该镀液由化学镀镍磷镀液和含SiC、石墨烯的分散液组成，化学镀镍磷镀液与分散液
体积比为1:1。
2.如权利要求1所述的镍磷基复合镀液，其特征在于：每升化学镀镍磷镀液由镍盐20-30g、络合剂15-25g、还原剂15-30g、稳定剂2-5mg、缓冲剂10-20g加入到蒸馏水中搅拌得到。
3.如权利要求2所述的镍磷基复合镀液，其特征在于：所述镍盐为硫酸镍或氯化镍。
4.如权利要求2所述的镍磷基复合镀液，其特征在于：所述络合剂为柠檬酸钠或者羟基乙酸。
5.如权利要求2所述的镍磷基复合镀液，其特征在于：所述还原剂为次磷酸钠或者次亚磷酸钠。
6.如权利要求2所述的镍磷基复合镀液，其特征在于：所述稳定剂为硫脲或碘酸钾。
7.如权利要求2所述的镍磷基复合镀液，其特征在于：所述缓冲剂为氯化铵。
8.如权利要求1所述的镍磷基复合镀液，其特征在于：每升分散液由20-80mg醇类高分子为分散剂，10-20g的SiC粉体，10-25g的石墨烯粉体加入蒸馏水中，经超声分散30分钟，磁力搅拌120分钟得到。
9.如权利要求8所述的镍磷基复合镀液，其特征在于：SiC粉体的粒径范围为0.5-1.0μm，石墨烯粉体的平均厚度为3.5nm，直径为0.5-5μm。
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