CN104630750B - 一种镁合金表面复合膜层的制备方法 - Google Patents
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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
- 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
- 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
- C23C18/02—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 thermal decomposition
- C23C18/12—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 thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/125—Process of deposition of the inorganic material
- C23C18/1254—Sol or sol-gel processing
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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
- 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
- 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
- C23C18/02—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 thermal decomposition
- C23C18/04—Pretreatment of the material to be coated
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Abstract
一种镁合金表面复合膜层的制备方法，包括：（1）将镁合金构件打磨、上料；（2）进行脱脂、超声波处理、酸洗、碱洗等预处理工艺；（3）进行改性处理、超声波处理、制膜、烧结等复合成膜工艺。本发明复合膜层的表面形貌比单一的磷酸钡膜层更加平整、致密、均匀，抗腐蚀性能比单一的磷酸钡膜层要好；克服了处理过程中溶液不稳定，转化膜层不均匀、易脱落等难题；本发明操作简单方便、通用性强，它可以适用于任何镁合金材料表面处理；本发明整个流程都不使用铬酸或氰化物，无污染，在实际生产中满足环保和可持续发展的要求。而且工艺简单，易形成自动化生产线，而不需大的设备投资，形成产能时间短。
Description
技术领域
本发明属于金属材料技术领域，涉及一种对镁合金材料进行表面化学复合处理的方法。
背景技术
镁合金以其比重小、生物相容性好等诸多优点受到人们的广泛关注。但由于镁非常活泼，耐蚀问题严重地限制了其进一步的推广和应用。在镁合金表面的防腐技术中，磷酸盐转化技术因其工艺简单、成本低、操作方便等优点而成为热点课题。L.Kouisni等研究了AM60镁合金上的磷化膜层，David Hawke 等对AM60B 镁合金进行了磷酸盐-高锰酸盐处理，L.Y.Niu研究的磷酸锌转化膜层，赵明等研究了AZ91D镁合金的多元复合膜（MECC）工艺，Nguyen Van Phuonga等研究了AZ91D镁合金表面的磷酸锌成膜。这些工艺均可在镁合金表面得到厚度不一的磷酸盐膜层，把镁合金基体与外界环境隔绝，不同程度提高镁合金的抗腐蚀能力。然而磷酸盐膜层致密度低、较薄，膜层的内微孔会削弱其耐蚀性，要满足生产应用其抗腐蚀性能还有待提高。因此，提高镁合金表面磷酸盐膜层的抗腐蚀性能成为又一大发展方向。
近年来人们一直在寻求一种既能满足环保要求、提高镁合金的耐蚀性能，又有一定商业价值，又能节省能源的镁及镁合金表面复合处理技术。
中国专利号ZL200610019324.5公开了一种镁合金磷酸钡表面处理方法，包括脱脂、酸洗、碱洗、化学成膜、封闭处理等工序，通过表面改性处理，达到保护镁合金产品表面的目的。
发明内容
本发明的目的是对现有技术进行改进，提出一种镁合金表面复合膜层的制备方法。在镁及其合金构件基体表面生成磷酸钡膜与SiO2 溶胶凝胶膜的复合膜层处理工艺，以显著提高镁合金的耐腐蚀性能，满足环保要求，节省能源。
本发明是通过以下技术方案实现的。
本发明所述的制备方法，包括以下步骤。
（1）将镁合金构件打磨、上料。
（2）预处理工艺：将镁合金构件浸入盛有浓度为5%~10% 氢氧化钠的脱脂槽中，加热到80~98℃，超声波处理20~30 分钟，再进入第一蒸馏水水洗槽中，室温下超声波处理20~50秒，取出热风吹干；然后浸入盛有40~80g/L氢氟酸、30~50g/L乙二醇溶液的酸洗槽中，室温下超声波处理1~2.5分钟，酸洗后进入第二蒸馏水水洗槽中，同样室温下超声波处理20~50秒，取出用热风吹干；再浸入装有20%~30%氢氧化钠的碱洗槽中，室温下超声波处理25~30分钟，然后浸入第三蒸馏水水洗槽中，室温超声波清洗20~50秒，取出用热风吹干。
（3）复合成膜工艺：把镁合金构件放入盛有10~30ml/L磷酸、30~60g/L氢氧化钡、1~5g/L氟化钠改性处理溶液的槽中，加热到40~100℃，超声波处理10~30分钟；然后放入第四水洗槽中超声波振荡清洗，取出热风吹干；最后浸入盛有50-100ml/L正硅酸乙酯、5-20ml/L聚乙二醇-600、1-10ml/L浓硝酸、60-110ml/L无水乙醇的SiO2溶胶凝胶溶液中进行3-6次手动提拉制膜，取出立刻热风吹干，然后放入箱式电阻炉中进行烧结，烧结温度为300 ℃-420℃，烧结时间为4-8小时。
通过采用本发明的方法和配方，以AZ91D镁合金材料为例获得的复合膜层的主要特性如下。
复合膜层外观白色均匀，细腻光滑，膜层更加致密、平整、均匀，裂纹明显减少，由一些无定形相组成（见图1）。
复合膜层抗盐雾性：48小时后，才出现腐蚀，镁合金基体，镀锌、镀镍的转化膜8小时就出现全面腐蚀，可见磷酸钡膜层加SiO2溶胶凝胶膜层形成的复合膜层大大提高了镁合金零件的抗盐雾性能（见图2）。
复合膜层抗潮性：100小时后，才出现腐蚀，镁合金基体7小时后就出现全面腐蚀，可见磷酸钡膜层加SiO2溶胶凝胶膜层形成的复合膜层大大提高镁合金零件的抗潮湿性。
与现有技术相比，本发明具有以下优点。
1、复合膜层的表面形貌比单一的磷酸钡膜层更加平整、致密、均匀，从全浸蚀试验、点滴试验、极化曲线测试都表明复合膜层的抗腐蚀性能比单一的磷酸钡膜层要好。
2、掌握了处理过程中溶液配比、加热温度和处理时间的最优化控制，克服了处理过程中溶液不稳定，转化膜层不均匀、易脱落等难题。
3、复合膜层的制备方法操作简单方便、通用性强，它可以适用于任何镁合金材料表面处理；并能显著提高磷酸钡膜层的表面质量和抗腐蚀性能，完善了镁合金化学转化处理工艺。
4、该工艺整个流程都不使用铬酸或氰化物，无污染，在实际生产中满足环保和可持续发展的要求。而且工艺简单，易形成自动化生产线，而不需大的设备投资，形成产能时间短，能够适应当今社会竞争需要，提高企业竞争力。
附图说明
图1为本发明复合膜层的X-射线衍射图谱。
图2为镁合金试样在5％盐水中腐蚀4 天后照片，其中a为单一磷酸钡膜层，b为复合膜层。
具体实施方式
下面结合实施例对本发明作进一步的说明。
实施例1。材料为手电钻机头外壳。
将手电钻机头外壳打磨、上料。
脱脂：将外壳浸入装有质量百分比为8%、温度为75℃的氢氧化钠脱脂槽中，通过超声波作用20分钟，使油脂与碱性溶液及表面活性物质发生皂化反应和乳化反应而溶解于水中，以达到脱脂的目的，可以明显看见外壳表面变得光亮。之后，进入第一蒸馏水水洗槽中，在室温下用超声波作用40秒，去除残留在外壳表面上的碱性溶液及油脂分子，取出用热风吹干。
酸洗：再将外壳浸入盛有50g/L氢氟酸、40g/L乙二醇的酸洗槽中，在室温下用超声波作用1分钟，微蚀外壳表面以去除外壳表面生成的氧化物，另外还可以中和脱脂后残余在外壳上的碱性物质。酸洗后进入第二蒸馏水水洗槽中，同样在室温下用超声波作用40秒，去除残留在外壳表面上的酸性溶液及氧化物颗粒，取出用热风吹干。
碱洗：将外壳浸入装有质量百分比为25%氢氧化钠的碱洗槽中，在室温下用超声波作用30分钟，中和残留在外壳表面上的酸性物质。然后浸入第三蒸馏水水洗槽中，室温超声波清洗40秒，取出用热风吹干。
磷酸钡成膜：再把外壳放入盛有15ml/L磷酸、50g/L氢氧化钡、5g/L氟化钠，温度为80℃，预加了镁合金浸泡的成膜处理槽中，用超声波作用10分钟，使外壳表面形成一层致密的保护性化学转化膜；然后放入第四水洗槽中超声波振荡清洗，去除外壳表面上残留的化学试剂，取出热风吹干。
SiO2溶胶凝胶成膜：最后浸入盛有50ml/L正硅酸乙酯、5ml/L聚乙二醇-600、1ml/L浓硝酸、60ml/L无水乙醇的SiO2溶胶凝胶溶液中，用细线绑住手电钻机头外壳一端浸没于溶胶溶液之中30秒后开始进行提拉操作，提拉速度大致为3 cm/min，为了使外壳表面形成的膜层更加的致密和均匀，提拉过后在室温下自然风干后再重复上述提拉操作3次，进行4次手动提拉制膜后，取出立刻热风吹干，然后放入箱式电阻炉中进行烧结，烧结温度为300℃，烧结时间为4小时。
Claims (1)
1.一种镁合金表面复合膜层的制备方法，其特征是步骤为：
（1）将镁合金构件打磨、上料；
（2）将步骤（1）的镁合金构件浸入盛有质量百分比浓度为5%~10% 氢氧化钠的脱脂槽中，加热到80~98℃，超声波处理20~30 分钟，再进入第一蒸馏水水洗槽中，室温下超声波处理20~50秒，取出热风吹干；然后浸入盛有40~80g/L氢氟酸、30~50g/L乙二醇溶液的酸洗槽中，室温下超声波处理1~2.5分钟，酸洗后进入第二蒸馏水水洗槽中，同样室温下超声波处理20~50秒，取出用热风吹干；再浸入装有质量百分比浓度为20%~30%氢氧化钠的碱洗槽中，室温下超声波处理25~30分钟，然后浸入第三蒸馏水水洗槽中，室温超声波清洗20~50秒，取出用热风吹干；
（3）将步骤（2）的镁合金构件放入盛有10~30mL/L磷酸、30~60g/L氢氧化钡、1~5g/L氟化钠改性处理溶液的槽中，加热到40~100℃，超声波处理10~30分钟；然后放入第四水洗槽中超声波振荡清洗，取出热风吹干；最后浸入盛有50-100mL/L正硅酸乙酯、5-20mL/L聚乙二醇-600、1-10mL/L浓硝酸、60-110mL/L无水乙醇的SiO2溶胶凝胶溶液中进行3-6次手动提拉制膜，取出立刻热风吹干，然后放入箱式电阻炉中进行烧结，烧结温度为300 ℃-420℃，烧结时间为4-8小时。
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