CN106222632A - 一种环保型耐蚀、耐磨镁合金镀层的制备方法 - Google Patents

一种环保型耐蚀、耐磨镁合金镀层的制备方法 Download PDF

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CN106222632A
CN106222632A CN201610877506.XA CN201610877506A CN106222632A CN 106222632 A CN106222632 A CN 106222632A CN 201610877506 A CN201610877506 A CN 201610877506A CN 106222632 A CN106222632 A CN 106222632A
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    • C—CHEMISTRY; METALLURGY
    • 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
    • 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
    • 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
    • C23C18/18—Pretreatment of the material to be coated
    • C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
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    • C23C18/1837—Multistep pretreatment
    • C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
    • C—CHEMISTRY; METALLURGY
    • 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
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
    • C23G1/12—Light metals

Abstract

本发明公开了一种环保型耐蚀、耐磨镁合金镀层的制备方法，其特征是采用无铬无氰低氟工艺对镁合金表面进行前处理，包括除油→超声无铬酸洗→低氟活化，再以表面修饰、改性后的(Ni/SiC)P为增强体，优化施镀配方、工艺，制备镁基Ni‑P‑(Ni/SiC)P复合镀层，以提高不同相间的相容性、结合力及金属镍的沉积量，从而进一步提高镁合金的耐蚀及耐磨性能等。经处理后镁合金表面耐蚀性提高2‑4倍，耐磨性提高3‑5倍。该发明属于表面技术、材料制备领域，其结果能广泛应用于电子工业、汽车工业、民用等多个领域。本发明对生产设备要求低，废液中不含Cr6+、CN‑或HF，对环境和人体无污染，所用溶液成分均为常用化学药品，易于购买，所得产品镀层均匀、耐蚀性、耐磨性高。

Description

一种环保型耐蚀、耐磨镁合金镀层的制备方法
技术领域
本发明涉及一种环保型耐蚀、耐磨镁合金镀层的制备方法，特点是采用无铬无氰低氟的环保工艺对镁合金进行前处理，以表面修饰、改性后的碳化硅颗粒 (Ni/SiC)P为增强体，优化施镀工艺，制备Ni-P-(Ni/SiC)P化学复合镀层，以提高镁合金的耐蚀及耐磨性能。该发明属于表面技术、材料制备领域。
背景技术
镁作为最轻的金属结构材料，具有密度低、比强度高、弹性模量大等优势，被誉为“21 世纪的绿色工程材料”，随着镁合金生产技术的逐步完善，其市场需求快速增长。但镁具有很高的化学活性，其标准电位为-2.37V，是工程合金中电位最负的。在室温下镁与空气中的氧易形成MgO 膜层，膜层的致密系数仅为0.79，疏松而多孔，不能阻止镁基体的进一步腐蚀。此外，在腐蚀介质中镁基体容易和合金中的合金元素、杂质以及其他金属构成腐蚀电池，导致电偶腐蚀，严重制约了镁及镁合金的广泛应用。
对镁合金进行适当的表面处理可以提高其耐蚀及耐磨性能。目前采用的表面处理方法主要有化学镀、电镀、化学转化膜等。其中化学镀技术以其设备投资少、不需外加电源、不受工件尺寸和形状限制等优势日益受到关注，成为国内外镁合金表面处理的研究热点.。
(SiC)P具有硬度高、耐磨、耐腐蚀等优点，以其为第二相颗粒制备镍磷化学复合镀层，可以提高金属的硬度和耐蚀、耐磨性等，但裸(SiC)P的共价键与金属基体的金属键之间的本质差别，使界面润湿性能差，颗粒易脱落，性能提高有限。
与铁基材料相比，镁合金化学性质活泼，易氧化，给化学镀镍带来极大困难，属于难镀金属，故施镀前必须对其进行前处理。目前常用的处理方法有浸锌法、转化膜法和直接化学镀镍，但或是步骤繁琐或是施镀效果欠佳，并且多采用铬酐、氰化物、氢氟酸等试剂，六价铬、氰化物和氢氟酸对人体和环境都有严重危害，急需替代改进。
有关这方面的文章或专利如：葛昆等.中温碱性镁合金化学镀镍研究[J].中国铸造装备与技术，2014，3；Chen J L et al．A zinc transition layer in electrolessnickel plating[J]. Surface and Coatings Technology，2006．苗润生等. AZ31 镁合金“两步法”化学镀Ni -P合金组织及性能研究[J].轻金属，2011．成旦红等.镁合金化学镀镍磷方法.申请号：200510110738.4。故简化工艺，替代对环境和人体有害的六价铬和氰化铜等，探索环保型的前处理工艺，增强颗粒与金属基体间的相容性及沉积量，提高镀层的硬度、耐蚀性等，是目前镁合金化学镀镍研究中迫切需要解决的难点问题。
发明内容
本专利的目的是解决现有技术中的不足，探索一种环境友好、无铬无氰、镍沉积量大、镀层结合力强，耐蚀、耐磨镁基镍磷复合镀层的制备方法。
在已积累的实验和理论经验基础上，采用直接化学镀镍法，首先对镁合金 （以AZ91D为例）表面进行前处理，此过程包括试样除油→超声波辅助无铬酸洗→低氟活化，再以(SiC)P表面修饰、改性所得的(Ni/SiC)P为增强体，前处理后镁合金为基体，制备镁基Ni-P-(Ni/SiC)P复合镀层。
本发明采用的技术方案是：
1.AZ91D镁合金表面前处理过程包括：除油处理、超声波辅助无铬酸洗、低氟活化。酸洗配方：HNO320-30ml·L-1，H3PO4 20-30ml·L-1，活化配方：NH4H2PO4 80-100 g·L-1，NH4F 30-50g·L-1。 2.(SiC)P表面修饰、改性，得到(Ni/SiC)P。 3.复合镀液的配制：依次向镀槽中添加硫酸镍20-30g·L-1、还原剂20-35 g·L-1、乳酸15-30ml·L-1、柠檬酸盐10-20g·L-1、氨基乙酸8-15g·L-1、硫脲0.5-1.5mg L-1、稀土及表面活性剂等，用氨水调至适当的pH值。4.复合镀层的制备：将一定质量的(Ni/SiC)P配成浆液，超声分散，使其润湿，加入到已配制好的化学复合镀液中，搅拌，加热镀液至规定温度后，放入前处理后的AZ91D镁合金试样施镀。施镀温度为75-85℃，镀液pH值范围为6.0-8.0，施镀时间为1.5-2h。
本发明的有益技术效果体现在以下几个方面：
（1）本发明一种环保型耐蚀、耐磨镁合金镀层的制备中AZ91D镁合金表面前处理过程，采用无机酸HNO3、H3PO代替铬酐酸洗，NH4H2PO4、NH4F代替HF活化，可有效降低试剂对人体的危害和环境的污染，并且防止基体过腐蚀，同时超声波辅助酸洗可加快去掉镁合金表面的氧化膜；NH4H2PO4、NH4F活化可在镁合金表面生成新膜层，保护基体，促进镍的沉积。（2）本发明一种环保型耐蚀、耐磨镁合金镀层的制备中所使用的增强体(Ni/SiC)P，为纳米(SiC)P经表面修饰、改性而得到，在镀层中分布均匀，颗粒中间为(SiC)P，表层为金属镍，增加了无机纳米颗粒与金属基体的相容性，克服了常规纳米化学复合镀层颗粒表面能高、易团聚的缺点，较常规纳米复合镀层，明显提高了粒子在镀层中的沉积量，可达20-40%。（3）本发明一种环保型耐蚀、耐磨镁合金镀层的制备所用镀液中加入了乳酸、柠檬酸盐、氨基乙酸、稀土混合组成的复合络合剂及加速剂，较现有纳米复合镀液稳定性高、寿命长、沉积速率快。（4）本发明一种环保型耐蚀、耐磨镁合金镀层的制备中所得Ni-P-(Ni/SiC)P复合镀层较原镁合金基体及同条件下所制备的Ni-P镀层，Ni-P-(SiC)P复合镀层，耐蚀性、耐磨性明显增加。可广泛应用于电子工业、汽车工业、民用等多个领域。同时本发明为表面改性技术，降低了生产成本，延长了镁合金的使用性能及寿命。
具体实施方式
下面给出本发明的实施例
实施例1
以AZ91D镁合金为基体制备Ni-P-(Ni/SiC)P复合镀层。
1. AZ91D镁合金基体的前处理：将打磨、除油后的镁合金分别放入25ml·L-1HNO3，25ml·L-1H3PO4和85g·L-1NH4H2PO4，40g·L-1NH4F溶液中酸洗、活化。
2. (SiC)P表面修饰、改性，制得 (Ni/SiC)P。
3. 复合镀液的配制：取硫酸镍20g·L-1、还原剂24 g·L-1、乳酸18ml·L-1、柠檬酸盐15g·L-1、氨基乙酸10g·L-1、硫脲0.8mg·L-1、稀土及表面活性剂等，加蒸馏水配制1L复合镀液。
4. 复合镀层的制备：将1.5g 表面改性后的(Ni/SiC)P配成浆液，超声分散，加入到已配制好的化学复合镀液中，搅拌，加热镀液至规定温度后，放入前处理后的镁合金施镀。施镀温度为76±2℃，镀液中的pH值为6.8±0.2，施镀时间约为1.5-2h。
5. 测试方法
复合镀层中改性(SiC)P的沉积量采用EDS能谱仪测量；镀层表面的形貌及颗粒分散程度采用扫描电子显微镜SEM观察、分析；镀层的耐磨性实验在MM-200摩擦磨损机上进行测试。镀层的结合力根据国家标准GB/T13913-12 中对镀层结合强度的评价方法，采用锉刀实验法检测。耐蚀性采用电化学测试***，用环氧树脂将镀层密封，留出1 cm2 的工作面积做为工作电极，饱和甘汞电极为参比电极，铂电极为辅助电极，将三电极体系通过电化学工作站，在3.5%的NaCl溶液中测量镀层的动电位极化曲线。
6. 测试结果
实验测得Ni-P-(Ni/SiC)P复合镀层中纳米颗粒的沉积量为28%，镀层表面均匀细致，较常规复合镀层中颗粒的沉积量有较大提高。镁合金基体的磨损量是41.2mg，Ni-P化学镀层的磨损量为30.6mg，Ni-P-纳米(SiC)P化学复合镀层的磨损量为19.7mg，Ni-P-(Ni/SiC)P化学复合镀层的磨损量为9.7mg。锉刀实验法检测Ni-P-(Ni/SiC)P复合镀层无起皮脱落现象。镁合金化学镀镍前后的极化曲线显示，基底的自腐蚀电位为-1.68 V，Ni-P化学镀层的自腐蚀电位为-1.03 V，自腐蚀电流降低约2.5个数量级；Ni-P-纳米(SiC)P化学复合镀层的自腐蚀电位为-0.58 V，自腐蚀电流降低约3.1个数量级；Ni-P-(Ni/SiC)P化学复合镀层的自腐蚀电位为-0.12 V，自腐蚀电流降低约4.2个数量级。
从此实施例可见：Ni-P-(Ni/SiC)P复合镀层与同类常规镀层相比较，耐蚀性和耐磨性能都得到了明显提高。
实施例2
以AZ91D镁合金为基体制备Ni-P-(Ni/SiC)P复合镀层。
1. AZ91D镁合金基体试样的前处理
将打磨、除油后的镁合金分别放入28ml·L-1HNO3，28ml·L-1H3PO4和90g·L-1NH4H2PO4，35g·L-1NH4F溶液中酸洗、活化。
2. (SiC)P表面改性，制得(Ni/SiC)P。改性前，需对(SiC)P进行前处理，此过程包括：亲水处理、循环敏化、钯盐活化。
3. 复合镀液的配制
取硫酸镍25g·L-1、次亚磷酸钠30g·L-1、乳酸23ml·L-1、柠檬酸盐18g·L-1、氨基乙酸12g·L-1、硫脲1mg L-1、稀土及表面活性剂等，加蒸馏水配制1L复合镀液。
4. 复合镀层的制备
将2.0g 表面改性后的(Ni/SiC)P配成浆液，超声分散，使其润湿，加入到已配制好的化学复合镀液中，搅拌，加热镀液至规定温度后，放入前处理后的镁合金施镀。施镀温度为80±2℃，镀液中的pH值范围为7.2±0.2，施镀时间约为1.5-2h。
5. 测试结果
实验测得Ni-P-(Ni/SiC)P复合镀层的纳米颗粒沉积量为33%，镀层表面均匀细致，较常规复合镀层中颗粒的沉积量有较大提高。镁合金基体的磨损量是41.2mg，Ni-P化学镀层的磨损量为27.6mg，Ni-P-纳米(SiC)P化学复合镀层的磨损量为15.4mg，Ni-P-(Ni/SiC)P化学复合镀层的磨损量为7.1mg。锉刀实验法检测Ni-P-(Ni/SiC)P复合镀层无起皮脱落现象。镁合金化学镀镍前后的极化曲线显示，基底的自腐蚀电位为-1.68 V，Ni-P化学镀层的自腐蚀电位为-0.94 V，自腐蚀电流降低约2.8个数量级；Ni-P-纳米(SiC)P化学复合镀层的自腐蚀电位为-0.41 V，自腐蚀电流降低约3.5个数量级；Ni-P-(Ni/SiC)P化学复合镀层的自腐蚀电位为-0.06 V，自腐蚀电流降低约4.9个数量级。
从此实施例可见：Ni-P-(Ni/SiC)P复合镀层与同类常规镀层相比较，耐蚀性和耐磨性能都得到了明显提高。

Claims (4)

1.一种环保型耐蚀、耐磨镁合金镀层的制备方法，其特征是采用无铬无氰低氟的环保工艺对镁合金进行前处理，去除镁合金表面的氧化膜，保护基体，促进镍的沉积，同时避免过程对环境和人体的危害；以表面修饰、改性后的纳米碳化硅颗粒(Ni/SiC)P为增强体，制备镁基Ni-P-(Ni/SiC)P复合镀层，降低了纳米粒子的团聚，提高了粒子在镀层中的分散程度、沉积量及镀层的耐蚀性及耐磨性能。
2.根据权利要求1所述的：一种环保型耐蚀、耐磨镁合金镀层的制备方法，其特征是：镁合金施镀前必须前处理，过程包括：除油→超声波辅助无铬酸洗→低氟活化，酸洗配方：HNO320-30ml·L-1，H3PO4 20-30ml·L-1，活化配方：NH4H2PO4 80-100 g·L-1，NH4F 30-50g·L-1。
3.根据权利要求1所述的：一种环保型耐蚀、耐磨镁合金镀层的制备方法，其特征是：(SiC)P需经表面修饰、改性过程，得到(Ni/SiC)P。
4.根据权利要求1所述的：一种环保型耐蚀、耐磨镁合金镀层的制备方法，其特征是：镀液中各成分的浓度是：硫酸镍20-30g·L-1、还原剂20-35 g·L-1、乳酸15-30ml·L-1、柠檬酸盐10-20g·L-1、氨基乙酸8-15g·L-1、硫脲0.5-1.5mg L-1稀土及表面活性剂等。
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