CN114921780A - 一种铝合金用环保钝化液及其制备方法和处理工艺 - Google Patents
一种铝合金用环保钝化液及其制备方法和处理工艺 Download PDFInfo
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- 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
- C23C22/06—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 using aqueous acidic solutions with pH less than 6
- C23C22/40—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 using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates
- C23C22/44—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 using aqueous acidic solutions with pH less than 6 containing molybdates, tungstates or vanadates containing also fluorides or complex fluorides
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- 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
- C23C22/73—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 characterised by the process
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- C—CHEMISTRY; METALLURGY
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- 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
- C23C22/73—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 characterised by the process
- C23C22/76—Applying the liquid by spraying
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- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/20—Use of solutions containing silanes
Abstract
本发明针对已有技术存在的钝化液稳定性差,钝化膜抗腐蚀性差,钝化膜不均匀,厚度薄和致密性低等问题,提出一种高效环保的钝化液及其制备方法和处理铝合金的工艺,该钝化液稳定性高,钝化膜均一致密,耐腐蚀性高,制备过程和处理工艺操作短时简便、能耗低。本环保无铬钝化液,不含铬等有害物质,从根本上消除了铬盐对水质的污染;且槽液稳定,使用寿命长,维护管理简单。
Description
技术领域
本发明属于材料表面处理与金属防护技术领域,尤其涉及一种铝合金用环保钝化液及其制备方法和处理工艺。
背景技术
作为轻质合金的代表,铝合金具有密度低、强度高、高度可回收的特点,广泛应用于航空航天、汽车工业、轨道交通等领域。对于铝合金来说,其表面的天然氧化膜虽然具有一定的耐蚀性能,但远远无法满足工业应用需求。因此,为了提高铝合金的耐蚀性能,铝合金表面天然形成的氧化膜必须被去除,同时被一种新的耐蚀的膜层取代。因此,铝合金在工业应用中必须要进行表面处理。化学转化法表面处理技术,设备操作简单,成本低廉,成膜速度快,能源消耗小,尤其适用于复杂零部件。
传统的化学转化法主要为铬酸盐转化法,膜层中的主成膜物质为六价铬化合物,所形成的铬酸盐转化膜具有良好的耐蚀性且与有机涂层的结合力优良。但铬酸盐转化膜工艺最大的缺点是环保问题和毒性,被严格限制使用。最有希望替代铬酸盐转化膜工艺的主要研究方向主要有:三价铬转化膜、钛锆转化膜、硅烷转化膜及稀土盐转化膜。三价铬转化膜工艺目前在工业中应用较多,虽然在成膜溶液和制得的转化膜中均未检测到Cr6+的存在,是一种环保型的铝合金化学转化处理工艺,但研究表明三价铬转化膜在腐蚀环境中提供长期腐蚀保护时,会生成六价铬的中间产物,存在六价铬造成污染的可能。钛锆钝化技术是目前市场上主要的无铬钝化产品技术,利用化学转化反应在铝合金表面形成一层保护膜层,然而在成膜过程中,由于成核、生长的不均匀性,易导致转化膜产生裂纹或孔隙,形成不规则的钝化层,所以需要添加有机物进行填充,但填充后形成的钝化膜层成分不均一,且有机物与氧化物之间的附着力也对膜层的耐蚀性能起到重要的影响。最终导致钝化裸膜的耐蚀性能难以令人满意。
发明内容
本发明的目的是针对已有技术存在的钝化液稳定性差,钝化膜抗腐蚀性差,钝化膜不均匀,厚度薄和致密性低等问题,提出一种高效环保的钝化液及其制备方法和处理铝合金的工艺,该钝化液稳定性高,钝化膜均一致密,耐腐蚀性高,制备过程和处理工艺操作短时简便、能耗低。
本发明的第一个目的是提供一种高效环保耐腐蚀铝合金用无铬钝化液,按照质量百份数计由以下原料组成:
其中,氟锆酸溶液为质量浓度45%的氟锆酸水溶液;硅烷偶联剂为3-缩水甘油醚氧基丙基三甲氧基硅烷;稳定剂为1-氨基-2-丙醇;碱金属硅酸盐溶液为模数为3.3的钠水玻璃溶液、钾水玻璃溶液中的至少一种;缓蚀剂为偏钒酸钠。
本发明的第二个目的是提供一种上述高效环保耐腐蚀铝合金用无铬钝化液的制备方法:首先向反应釜中添加适量去离子水,加入乙酸,调节pH值至3.0~4.0,在搅拌状态下加入硅烷偶联剂,搅拌1h至充分水解,加热至50~55℃,然后缓慢滴加稳定剂,滴加时间为0.5h,滴加完毕后继续搅拌反应0.5h,然后缓慢加入碱金属硅酸盐溶液,升温至80~85℃,搅拌反应2h,再加入缓蚀剂,搅拌至完全溶解,降温至室温,缓慢加入氟锆酸溶液,搅拌均匀,得到铝合金用无铬钝化液。
此外,本发明还提供一种无铬钝化液处理铝合金的工艺,包括如下步骤:铝合金工件经过脱脂、出光后,用质量浓度为3%~10%的本发明制备的无铬钝化液在25~40℃的条件下以喷淋法或浸渍法处理1~8min;水洗烘干,烘干温度为100-120℃,烘干时间为10-30min,烘干后即获得具有良好耐蚀性的钝化膜。
与现有技术相比,本发明所具有的有益效果是:
1、本发明提供的铝合金用环保无铬钝化液,不含铬等有害物质,从根本上消除了铬盐对水质的污染;且槽液稳定,使用寿命长,维护管理简单。
2、本发明提供的钝化液中氟锆酸、硅化合物(硅烷偶联剂和碱式硅酸盐)及缓蚀剂偏钒酸钠能够通过协同作用,在铝合金表面形成复合型钝化膜,提高了钝化膜的厚度及致密性,且硅化合物的加入提高了钝化膜与铝合金表面的附着力,钒盐的加入改善了钝化膜的自修复功能,有利于提高钝化膜的耐蚀性能。
3、本发明处理工艺简单,处理时间短,施工方便,适用于规模化工业生产。
附图说明
图1为实施例2的铝合金钝化膜的表面形貌图即SEM图和元素分析图谱
具体实施方式
下面结合实施例,对本发明作进一步的详细说明,但本发明的实施方式不限于此。
实施例1:
一种高效环保耐腐蚀铝合金用无铬钝化液,由以下重量百份数的原料组分制成:45%的氟锆酸溶液3份,3-缩水甘油醚氧基丙基三甲氧基硅烷8份,1-氨基-2-丙醇2.5份,钠水玻璃溶液1份,偏钒酸钠1.0份,乙酸0.8份,余量为去离子水。
制备方法:首先向反应釜中添加适量去离子水,加入乙酸,调节pH值至3.0~4.0,在搅拌状态下加入3-缩水甘油醚氧基丙基三甲氧基硅烷,搅拌1h至充分水解,加热至50~55℃,然后缓慢滴加1-氨基-2-丙醇,滴加时间为0.5h,滴加完毕后继续搅拌反应0.5h,然后缓慢加入钠水玻璃溶液,升温至80~85℃,搅拌反应2h,再加入偏钒酸钠,搅拌至完全溶解,降温至室温,缓慢加入45%的氟锆酸溶液,搅拌均匀,得到铝合金用无铬钝化液。
使用上述铝合金用无铬钝化液进行钝化,具体步骤如下:铝合金工件经过脱脂、出光后,用质量浓度为8%的本发明钝化液在25℃的条件下浸泡处理7min。水洗烘干,烘干温度为100℃,烘干时间为30min),得到表面钝化的铝合金。
本实施例对上述铝合金表面的钝化膜进行中性盐雾试验,通过了120h,证明本实施例制备的钝化膜具有良好的耐蚀性;并且在经过静电喷涂后,涂层也具有良好的附着力。
实施例2:
一种高效环保耐腐蚀铝合金用无铬钝化液,由以下重量百份数的原料组分制成:45%的氟锆酸溶液5份,3-缩水甘油醚氧基丙基三甲氧基硅烷12份,1-氨基-2-丙醇3.5份,钠水玻璃溶液2份,偏钒酸钠0.8份,乙酸1.0份,余量为去离子水。
制备方法:首先向反应釜中添加适量去离子水,加入乙酸,调节pH值至3.0~4.0,在搅拌状态下加入3-缩水甘油醚氧基丙基三甲氧基硅烷,搅拌1h至充分水解,加热至50~55℃,然后缓慢滴加1-氨基-2-丙醇,滴加时间为0.5h,滴加完毕后继续搅拌反应0.5h,然后缓慢加入钠水玻璃溶液,升温至80~85℃,搅拌反应2h,再加入偏钒酸钠,搅拌至完全溶解,降温至室温,缓慢加入45%的氟锆酸溶液,搅拌均匀,得到铝合金用无铬钝化液。
使用上述铝合金用无铬钝化液进行钝化,具体步骤如下:铝合金工件经过脱脂、出光后,用质量浓度为5%的本发明钝化液在35℃的条件下浸泡处理6min。水洗烘干,烘干温度为110℃,烘干时间为15min),得到表面钝化的铝合金。图1为本实施例制备的铝合金钝化膜的SEM图和EDX分析图,从图中可知,钝化膜表面无裂纹存在,但其表面具有一定的粗糙度,有利于与后续喷涂层形成良好的结合力,锆、硅及钒三种元素均匀分布在钝化膜中,说明氟锆酸、硅化合物(硅烷偶联剂和碱式硅酸盐)及缓蚀剂偏钒酸钠通过协同作用在铝合金表面形成致密的复合钝化膜。
本实施例对上述铝合金表面的钝化膜进行中性盐雾试验,通过了168h,证明本实施例制备的钝化膜具有良好的耐蚀性;并且在经过静电喷涂后,涂层也具有良好的附着力。
实施例3:
一种高效环保耐腐蚀铝合金用无铬钝化液,由以下重量百份数的原料组分制成:45%的氟锆酸溶液5份,3-缩水甘油醚氧基丙基三甲氧基硅烷8份,1-氨基-2-丙醇3份,钠水玻璃溶液3份,偏钒酸钠0.5份,乙酸1.0份,余量为去离子水。
制备方法:首先向反应釜中添加适量去离子水,加入乙酸,调节pH值至3.0~4.0,在搅拌状态下加入3-缩水甘油醚氧基丙基三甲氧基硅烷,搅拌1h至充分水解,加热至50~55℃,然后缓慢滴加1-氨基-2-丙醇,滴加时间为0.5h,滴加完毕后继续搅拌反应0.5h,然后缓慢加入钠水玻璃溶液,升温至80~85℃,搅拌反应2h,再加入偏钒酸钠,搅拌至完全溶解,降温至室温,缓慢加入45%的氟锆酸溶液,搅拌均匀,得到铝合金用无铬钝化液。
使用上述铝合金用无铬钝化液进行钝化,具体步骤如下:铝合金工件经过脱脂、出光后,用质量浓度为3%的本发明钝化液在40℃的条件下浸泡处理3min。水洗烘干,烘干温度为120℃,烘干时间为10min),得到表面钝化的铝合金。
本实施例对上述铝合金表面的钝化膜进行中性盐雾试验,通过了120h,证明本实施例制备的钝化膜具有良好的耐蚀性;并且在经过静电喷涂后,涂层也具有良好的附着力。
实施例4:
一种高效环保耐腐蚀铝合金用无铬钝化液,由以下重量百份数的原料组分制成:45%的氟锆酸溶液4份,3-缩水甘油醚氧基丙基三甲氧基硅烷10份,1-氨基-2-丙醇3份,钠水玻璃溶液1份,偏钒酸钠1.0份,乙酸1.0份,余量为去离子水。
制备方法:首先向反应釜中添加适量去离子水,加入乙酸,调节pH值至3.0~4.0,在搅拌状态下加入3-缩水甘油醚氧基丙基三甲氧基硅烷,搅拌1h至充分水解,加热至50~55℃,然后缓慢滴加1-氨基-2-丙醇,滴加时间为0.5h,滴加完毕后继续搅拌反应0.5h,然后缓慢加入钠水玻璃溶液,升温至80~85℃,搅拌反应2h,再加入偏钒酸钠,搅拌至完全溶解,降温至室温,缓慢加入45%的氟锆酸溶液,搅拌均匀,得到铝合金用无铬钝化液。
使用上述铝合金用无铬钝化液进行钝化,具体步骤如下:铝合金工件经过脱脂、出光后,用质量浓度为6%的本发明钝化液在35℃的条件下浸泡处理5min。水洗烘干,烘干温度为110℃,烘干时间为20min),得到表面钝化的铝合金。
本实施例对上述铝合金表面的钝化膜进行中性盐雾试验,通过了168h,证明本实施例制备的钝化膜具有良好的耐蚀性;并且在经过静电喷涂后,涂层也具有良好的附着力。
实施例5:
一种高效环保耐腐蚀铝合金用无铬钝化液,由以下重量百份数的原料组分制成:45%的氟锆酸溶液4份,3-缩水甘油醚氧基丙基三甲氧基硅烷12份,1-氨基-2-丙醇3份,钠水玻璃溶液2份,偏钒酸钠1.0份,乙酸0.9份,余量为去离子水。
制备方法:首先向反应釜中添加适量去离子水,加入乙酸,调节pH值至3.0~4.0,在搅拌状态下加入3-缩水甘油醚氧基丙基三甲氧基硅烷,搅拌1h至充分水解,加热至50~55℃,然后缓慢滴加1-氨基-2-丙醇,滴加时间为0.5h,滴加完毕后继续搅拌反应0.5h,然后缓慢加入钠水玻璃溶液,升温至80~85℃,搅拌反应2h,再加入偏钒酸钠,搅拌至完全溶解,降温至室温,缓慢加入45%的氟锆酸溶液,搅拌均匀,得到铝合金用无铬钝化液。
使用上述铝合金用无铬钝化液进行钝化,具体步骤如下:铝合金工件经过脱脂、出光后,用质量浓度为6%的本发明钝化液在30℃的条件下浸泡处理6min。水洗烘干,烘干温度为110℃,烘干时间为30min),得到表面钝化的铝合金。
本实施例对上述铝合金表面的钝化膜进行中性盐雾试验,通过了144h,证明本实施例制备的钝化膜具有良好的耐蚀性;并且在经过静电喷涂后,涂层也具有良好的附着力。
Claims (4)
1.一种高效环保耐腐蚀铝合金用无铬钝化液,其特征在于,按照质量百份数计由以下原料组成:
氟锆酸溶液3~5.0份,
硅烷偶联剂8~12份,
稳定剂2~4份,
碱金属硅酸盐溶液1~3份,
缓蚀剂0.5~1.0份,
乙酸0.8-1份,
去离子水余量。
2.根据权利要求1所述的一种高效环保耐腐蚀铝合金用无铬钝化液,其特征在于,所述的氟锆酸溶液为质量浓度45%的氟锆酸水溶液;硅烷偶联剂为3-缩水甘油醚氧基丙基三甲氧基硅烷;稳定剂为1-氨基-2-丙醇;碱金属硅酸盐溶液为模数为3.3的钠水玻璃溶液、钾水玻璃溶液中的至少一种;缓蚀剂为偏钒酸钠。
3.一种上述高效环保耐腐蚀铝合金用无铬钝化液的制备方法,其特征在于,由以下步骤组成:
首先向反应釜中添加适量去离子水,加入乙酸,调节pH值至3.0~4.0,在搅拌状态下加入硅烷偶联剂,搅拌1h至充分水解,加热至50~55℃,然后缓慢滴加稳定剂,滴加时间为0.5h,滴加完毕后继续搅拌反应0.5h,然后缓慢加入碱金属硅酸盐溶液,升温至80~85℃,搅拌反应2h,再加入缓蚀剂,搅拌至完全溶解,降温至室温,缓慢加入氟锆酸溶液,搅拌均匀,得到铝合金用无铬钝化液。
4.一种无铬钝化液处理铝合金的工艺,其特征在于,包括如下步骤:铝合金工件经过脱脂、出光后,用质量浓度为3%~10%的权利要求2制备的无铬钝化液在25~40℃的条件下以喷淋法或浸渍法处理1~8min;水洗烘干,烘干温度为100-120℃,烘干时间为10-30min,烘干后即获得具有良好耐蚀性的钝化膜。
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