CN115074714A - 镀锡板表面复合转化膜处理液及其制备转化膜的工艺 - Google Patents
镀锡板表面复合转化膜处理液及其制备转化膜的工艺 Download PDFInfo
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- CN115074714A CN115074714A CN202210680888.2A CN202210680888A CN115074714A CN 115074714 A CN115074714 A CN 115074714A CN 202210680888 A CN202210680888 A CN 202210680888A CN 115074714 A CN115074714 A CN 115074714A
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- conversion coating
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- treatment solution
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Classifications
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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
- 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
- C23C22/34—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 fluorides or complex fluorides
- C23C22/36—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 fluorides or complex fluorides containing also phosphates
- C23C22/364—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 fluorides or complex fluorides containing also phosphates containing also manganese cations
-
- 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
- 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
- C23C22/07—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 phosphates
- C23C22/08—Orthophosphates
- C23C22/12—Orthophosphates containing zinc cations
- C23C22/17—Orthophosphates containing zinc cations containing also organic acids
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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
- 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
- C23C22/07—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 phosphates
- C23C22/08—Orthophosphates
- C23C22/18—Orthophosphates containing manganese cations
- C23C22/182—Orthophosphates containing manganese cations containing also zinc cations
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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
- 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
- C23C22/34—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 fluorides or complex fluorides
- C23C22/36—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 fluorides or complex fluorides containing also phosphates
- C23C22/362—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 fluorides or complex fluorides containing also phosphates containing also zinc cations
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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
- 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
- C23C22/74—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 for obtaining burned-in conversion coatings
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Abstract
本发明属于镀锡板表面处理技术领域，具体涉及一种镀锡板表面复合转化膜处理液及其制备转化膜的工艺。本发明镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：钛盐0.25～2.5g/L，锆盐0.025～0.4g/L，磷酸和/或其化合物2～15g/L，双氧水0.25～5g/L，硅烷偶联剂2～20g/L，有机成膜剂100～800g/L。本发明的镀锡板表面复合转化膜处理液不含铬，更加安全、环保；且组成简单，生产成本低。本发明采用涂覆‑烘烤式一步成膜法，无需水洗，没有废水排放，节能减排，有利于环境保护；采用本发明处理液及工艺制备的镀锡板表面复合转化膜具有杰出的耐蚀性、抗酸性、抗硫性等综合性能。
Description
技术领域
本发明属于镀锡板表面处理技术领域，具体涉及一种镀锡板表面复合转化膜处理液及其制备转化膜的工艺。
背景技术
镀锡板(也称马口铁)是指两面镀有一层极薄金属锡的冷轧薄钢板，它将钢的硬度和强度与锡的易焊接性、抗腐蚀性和光亮的外表集于一体。镀锡板具有无味无毒、质量轻、易于加工成型等优点。印制不同的图案还可以美化产品，因此在食品罐头工业、电子器件、化工油漆等行业上得到了广泛应用。在镀锡板的生产过程中，带钢经镀锡软熔以后，为了防止镀锡板在贮存或涂料烘烤时锡层氧化发黄，同时提高镀锡板的抗硫性等性能，要对镀锡板进行处理。
铬酸盐转化处理技术是一种传统的转化处理技术，由于转化液中含有六价铬等毒性物质，对人类健康和环境危害极大，因此开发无铬转化技术是一个必然的趋势。目前已经开发出的无铬化学转化工艺主要分为无机类钝化、有机类化学转化及有机无机复合类化学转化，其中无机类化学转化主要包括钼酸盐和钨酸盐类、稀土金属盐类、钛盐锆盐类、磷酸盐和硅酸盐类等，有机类化学转化主要包括植酸、单宁酸、硅烷偶联剂类和树脂类等。无机类与有机类化学转化在镀锡板表面的成膜机理不同，无机类化合物在镀锡板表面形成化学转化膜是通过自身与镀锡板表面反应，与镀锡板表面形成化学键，形成致密的无机物膜，或者降低镀锡板的表面活性，从而提高镀锡板表面腐蚀防护性能；而有机物化学转化方式是通过有机分子在表面吸附或反应形成一层致密疏水的有机膜层，进而起到改善镀锡板表面耐蚀性能的目的，基体与膜层的结合力大部分为范德华力。研究发现，单一组分化学转化膜的耐蚀效果都无法与重铬酸盐转化膜的耐蚀效果媲美。中国专利申请201210271997.5公开了一种用于铝合金表面防腐蚀的稀土转化膜处理液及其应用方法，其原料成分及其含量为：每升蒸馏水中加入稀土盐10～40g，氯化钠120～400g，氟化钠12～45g。所述的稀土盐为铈盐或镧盐，处理液的pH值在2～6，处理温度为30～70℃，采用浸渍工艺，将铝合金工件浸在上述处理液中40～70min，干燥后即在铝合金表面形成耐腐蚀的稀土转化膜，虽然该稀土转化膜处理液能提高铝合金的耐腐蚀性能，但是其含有稀土盐，成本高，不利于其推广应用。
目前的无铬复合化学转化膜存在成本较高，综合性能不理想等问题。因此，迫切需要开发出一种成本低，且可以提高镀锡板耐蚀效果及综合性能的新型的无铬复合化学转化膜，同时转化膜的制备工艺要简单、节能、减少废水的排放，从而可以应用到工厂的实际生产中。
发明内容
针对现有技术的不足，本发明的目的在于提供一种镀锡板表面复合转化膜处理液及其制备转化膜的工艺。本发明提供的镀锡板表面复合转化膜处理液不含铬，更加安全、环保；且本发明提供的镀锡板表面复合转化膜处理液组成简单，生产成本低。除此之外，本发明制备复合转化膜的工艺采用涂覆-烘烤式一步成膜法，转化液涂到镀锡板基板表面后直接烘干成膜，无需水洗，没有废水排放，节能减排，有利于环境保护；采用本发明提供的镀锡板表面复合转化膜处理液及工艺制备的镀锡板表面复合转化膜具有杰出的耐蚀性；与镀锡板基板之间以及后续涂漆之间具有良好的结合力；且具有良好的抗酸性、抗硫性、可焊性等综合性能，工业应用前景广阔。
本发明的技术方案是：
镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：钛盐0.25～2.5g/L，锆盐0.025～0.4g/L，磷酸和/或其化合物2～15g/L，双氧水0.25～5g/L，硅烷偶联剂2～20g/L，有机成膜剂100～800g/L。
进一步地，所述的镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：钛盐0.5～1.5g/L，锆盐0.05～0.3g/L，磷酸和/或其化合物5～10g/L，双氧水0.5～1.5g/L，硅烷偶联剂5～10g/L，有机成膜剂300～500g/L。
进一步地，所述的镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：钛盐1.2g/L，锆盐0.3g/L，磷酸和/或其化合物6g/L，双氧水0.6g/L，硅烷偶联剂5g/L，有机成膜剂350g/L。
进一步地，所述钛盐为硫酸氧钛、六氟钛酸、二氧化钛中的一种或多种。
进一步地，所述锆盐为碳酸锆、六氟锆酸中的一种或多种。
进一步地，所述磷酸和/或其化合物为磷酸、磷酸二氢锰、磷酸二氢铝、磷酸二氢锌、有机磷酸盐中的一种或多种。
进一步地，所述有机成膜剂为水性树脂和天然聚合物中的一种或两种。
进一步地，所述水性树脂为水性聚氨酯树脂、水性酚醛树脂、水性丙烯酸树脂、水性环氧树脂、水性硅树脂和水性乙烯基树脂中的一种或两种。
进一步地，所述水性聚氨酯树脂为非离子型脂肪族聚氨酯分散液。
进一步地，所述天然聚合物为海藻酸钠、甲壳素中的一种或两种。
本发明还提供了所述的镀锡板表面复合转化膜处理液的制备方法，包括以下步骤：
称取配适量的蒸馏水，开动搅拌器；加入配方量的钛盐，搅拌均匀，加入配方量的双氧水，搅拌均匀，加入配方量的锆盐，搅拌均匀，加入配方量的磷酸和/或其化合物，搅拌均匀，加入配方量的硅烷偶联剂，搅拌均匀；加入配方量的有机成膜剂，搅拌均匀，加入蒸馏水定容至体积为1L，搅拌均匀，即得。
一种利用所述的镀锡板表面复合转化膜处理液制备转化膜的工艺，包括以下步骤：
(1)将基材经前处理后得到镀锡板基板；
(2)调节镀锡板表面复合转化膜处理液的pH值为1.5～4.5，温度为10～40℃；
(3)将步骤(1)得到的镀锡板基板表面涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液；
(4)将经转化处理的镀锡板基板放入热风干燥箱中烘干、冷却，即完成镀锡板表面复合转化膜的制备。
进一步地，所述步骤(3)中采用棒涂、辊涂、浸涂、喷涂、离心式“喷漆器”方法中的一种涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液。
进一步地，所述步骤(4)中烘干是在50～180℃条件下，烘烤2～5min。
本发明通过将无机类与有机类成膜物质进行复配，通过两种不同的耐蚀机理在镀锡板上成膜起到协同化学转化作用，这样得到的复合膜兼顾两者的优点，从而在镀锡板上起到更佳优异的耐蚀效果和综合性能。其中无机盐与基体表面反应生成无机骨架结构转化膜，而有机聚合物通过与无机骨架价键并且镶嵌在无机骨架中固化成膜，二者相结合形成了致密的具有高耐蚀性的复合化学转化膜。
与现有技术相比，本发明具有以下优势：
(1)与传统铬酸盐转化处理技术相比，本发明提供的镀锡板表面复合转化膜处理液避免了使用对环境有害的含铬转化液，更加安全、环保；
(2)本发明提供的镀锡板表面复合转化膜处理液组成简单，无需添加成本高的稀土盐等组分，大大降低了生产成本；
(3)本发明制备复合转化膜的工艺采用涂覆-烘烤式一步成膜法，转化液涂到镀锡板基板表面后直接烘干成膜，无需水洗，没有废水排放，节能减排，有利于环境保护；
(4)采用本发明提供的镀锡板表面复合转化膜处理液及工艺制备的镀锡板表面复合转化膜具有杰出的耐蚀性；与镀锡板基板之间以及后续涂漆之间具有良好的结合力；且具有良好的抗酸性、抗硫性、可焊性等综合性能，工业应用前景广阔。
具体实施方式
以下通过具体实施方式的描述对本发明作进一步说明，但这并非是对本发明的限制，本领域技术人员根据本发明的基本思想，可以做出各种修改或改进，但是只要不脱离本发明的基本思想，均在本发明的范围之内。
实施例1、镀锡板表面复合转化膜处理液
所述镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：六氟钛酸1g/L，六氟锆酸0.25g/L，磷酸5g/L，双氧水(30％)0.5g/L，硅烷偶联剂KH5605g/L，水性丙烯酸树脂300g/L。
所述的镀锡板表面复合转化膜处理液的制备方法，包括以下步骤：
称取配适量的蒸馏水，开动搅拌器；加入配方量的六氟钛酸，搅拌均匀，加入配方量的双氧水，搅拌均匀，加入配方量的六氟锆酸，搅拌均匀，加入配方量的磷酸，搅拌均匀，加入配方量的硅烷偶联剂KH560，搅拌均匀；加入配方量的水性丙烯酸树脂，搅拌均匀，加入蒸馏水定容至体积为1L，搅拌均匀，即得。
一种利用上述的镀锡板表面复合转化膜处理液制备转化膜的工艺，包括以下步骤：
(1)将基材经前处理后得到镀锡板基板；
(2)调节镀锡板表面复合转化膜处理液的pH值为2，温度为20℃；
(3)将步骤(1)得到的镀锡板基板表面采用棒涂涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液；
(4)将经转化处理的镀锡板基板放入热风干燥箱中90℃烘烤3min，冷却，即完成镀锡板表面复合转化膜的制备。
实施例2、镀锡板表面复合转化膜处理液
所述镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：六氟钛酸1.2g/L，碳酸锆0.3g/L，磷酸6g/L，双氧水(30％)0.6g/L，硅烷偶联剂KH5605g/L，水性丙烯酸树脂300g/L。
所述的镀锡板表面复合转化膜处理液的制备方法与实施例1类似。
一种利用上述的镀锡板表面复合转化膜处理液制备转化膜的工艺，包括以下步骤：
(1)将基材经前处理后得到镀锡板基板；
(2)调节镀锡板表面复合转化膜处理液的pH值为2，温度为20℃；
(3)将步骤(1)得到的镀锡板基板表面采用喷涂涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液；
(4)将经转化处理的镀锡板基板放入热风干燥箱中100℃烘烤3min，冷却，即完成镀锡板表面复合转化膜的制备。
实施例3、镀锡板表面复合转化膜处理液
所述镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：六氟钛酸1g/L，碳酸锆0.25g/L，磷酸5g/L，双氧水(30％)0.5g/L，硅烷偶联剂KH560 5g/L，水性聚氨酯树脂350g/L；所述水性聚氨酯树脂为非离子型脂肪族聚氨酯分散液，固含量：30％。
所述的镀锡板表面复合转化膜处理液的制备方法与实施例1类似。
一种利用上述的镀锡板表面复合转化膜处理液制备转化膜的工艺，包括以下步骤：
(1)将基材经前处理后得到镀锡板基板；
(2)调节镀锡板表面复合转化膜处理液的pH值为2，温度为20℃；
(3)将步骤(1)得到的镀锡板基板表面采用棒涂涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液；
(4)将经转化处理的镀锡板基板放入热风干燥箱中90℃烘烤3min，冷却，即完成镀锡板表面复合转化膜的制备。
实施例4、镀锡板表面复合转化膜处理液
所述镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：六氟钛酸1.2g/L，六氟锆酸0.3g/L，磷酸6g/L，双氧水(30％)0.6g/L，硅烷偶联剂KH5605g/L，水性聚氨酯树脂350g/L；所述水性聚氨酯树脂为非离子型脂肪族聚氨酯分散液，固含量：30％。
所述的镀锡板表面复合转化膜处理液的制备方法与实施例1类似。
一种利用上述的镀锡板表面复合转化膜处理液制备转化膜的工艺，包括以下步骤：
(1)将基材经前处理后得到镀锡板基板；
(2)调节镀锡板表面复合转化膜处理液的pH值为2，温度为20℃；
(3)将步骤(1)得到的镀锡板基板表面采用喷涂涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液；
(4)将经转化处理的镀锡板基板放入热风干燥箱中100℃烘烤3min，冷却，即完成镀锡板表面复合转化膜的制备。
对比例1、
镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：六氟钛酸1.2g/L，六氟锆酸0.3g/L，双氧水(30％)0.6g/L，硅烷偶联剂KH560 11g/L，水性聚氨酯树脂350g/L；所述水性聚氨酯树脂为非离子型脂肪族聚氨酯分散液，固含量：30％。
所述的镀锡板表面复合转化膜处理液的制备方法与实施例1类似。
一种利用上述的镀锡板表面复合转化膜处理液制备转化膜的工艺，包括以下步骤：
(1)将基材经前处理后得到镀锡板基板；
(2)调节镀锡板表面复合转化膜处理液的pH值为2，温度为20℃；
(3)将步骤(1)得到的镀锡板基板表面采用喷涂涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液；
(4)将经转化处理的镀锡板基板放入热风干燥箱中100℃烘烤3min，冷却，即完成镀锡板表面复合转化膜的制备。
对比例2、
镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：六氟钛酸1.2g/L，六氟锆酸0.3g/L，磷酸6g/L，双氧水(30％)0.6g/L，水性聚氨酯树脂350g/L；所述水性聚氨酯树脂为非离子型脂肪族聚氨酯分散液，固含量：30％。
所述的镀锡板表面复合转化膜处理液的制备方法与实施例1类似。
一种利用上述的镀锡板表面复合转化膜处理液制备转化膜的工艺，包括以下步骤：
(1)将基材经前处理后得到镀锡板基板；
(2)调节镀锡板表面复合转化膜处理液的pH值为2，温度为20℃；
(3)将步骤(1)得到的镀锡板基板表面采用喷涂涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液；
(4)将经转化处理的镀锡板基板放入热风干燥箱中100℃烘烤3min，冷却，即完成镀锡板表面复合转化膜的制备。
对比例3、
镀锡板表面复合转化膜处理液，包括以下质量浓度的组分：六氟钛酸1.2g/L，六氟锆酸0.3g/L，磷酸6g/L，双氧水(30％)0.6g/L，硅烷偶联剂KH560 5g/L，水性聚氨酯树脂350g/L；所述水性聚氨酯树脂为阴离子型脂肪族聚氨酯分散液，固含量：30％。
该对比例所得溶液破乳沉淀，无法使用。
试验例一、性能测试
1、试验材料：基板：基材为100mm*70mm*0.2mm厚的一次冷轧低碳钢板，钢板牌号为T4-CA。
2、试验方法：
按照表1镀锡板工艺进行前处理，制备84片经前处理后得到的镀锡板基板。
表1镀锡板工艺
取12片经前处理后得到的镀锡板基板作为对照组；将另外72片经前处理后得到的镀锡板基板分成六组，每组12片试样，分别为实施例1组、实施例2组、实施例3组、实施例4组，对比例1组，对比例2组，分别按照实施例1～4和对比例1～2所示组成及工艺在镀锡板表面制备复合转化膜，进行如下测试。
2.1、中性盐雾试验
取对照组、实施例1～4和对比例1～2所制备的试样各三个，进行10h中性盐雾测试验证膜层耐蚀性，中性盐雾试验遵循ASTM B117标准。试验溶液由3.5wt％组成NaCl，pH值为7，实验温度控制在35℃～45℃。每1小时，从盐雾试验箱中取出样品，清洁并观察表面状况，将试片中性盐雾耐蚀等级从好到坏按1～10级分级，取3个平行试片测试结果平均值作为结果。
2.2、附着力测试
取对照组、实施例1～4和对比例1～2所制备的试样各三个，根据QBT2763-2006测试膜层的有机涂层附着力，将试片有机附着力等级从好到坏按1～4级分级，取3个平行试片测试结果平均值作为结果。评级标准：涂膜被撕下的面积为0为1级，涂膜被撕下的面积≤10％为2级，涂膜被撕下的面积≤25％为3级，涂膜被撕下的面积≤50％为4级。
2.3、抗硫性、抗酸性测试
取对照组、实施例1～4和对比例1～2所制备的试样各六个，采用轻工业标准(QBT2763-2006)对试片分别进行抗硫性、抗酸性测试，将试片抗酸性、抗硫性等级从好到坏按1～10级分级，分别取3个平行试片测试结果平均值作为结果。
1～10级评级标准：膜层腐蚀或被破坏了10％以内为1级，10～20％为2级，依次类推。
3、试验结果见下表2。
表2不同性能测试结果汇总表
| 组别 | 耐蚀性等级 | 结合力等级 | 抗酸性等级 | 抗硫性等级 |
| 对照组 | 10 | 4 | 9 | 8 |
| 实施例1组 | 3 | 2 | 3 | 4 |
| 实施例2组 | 2 | 2 | 3 | 3 |
| 实施例3组 | 2 | 1 | 1 | 1 |
| 实施例4组 | 1 | 1 | 1 | 1 |
| 对比例1组 | 6 | 3 | 5 | 6 |
| 对比例2组 | 3 | 3 | 6 | 6 |
由上表2可知，按照本发明实施例1～4所示组成及工艺在镀锡板表面制备的复合转化膜具有优异的耐蚀性、漆膜附着力以及抗酸性、抗硫性等综合性能，其中实施例4的综合性能最优，为本发明的最佳实施例；与对比例1-2相比，本发明在镀锡板表面制备的钛锆/水性树脂复合转化膜具有更为优异的耐蚀性、漆膜附着力以及抗酸性、抗硫性等综合性能。
上述实施例仅例示性说明本发明的原理及功效，而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下，对上述实施例进行修饰或改变。因此，举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变，仍应由本发明的权利要求所涵盖。
Claims (10)
1.镀锡板表面复合转化膜处理液，其特征在于，包括以下质量浓度的组分：钛盐0.25～2.5g/L，锆盐0.025～0.4g/L，磷酸和/或其化合物2～15g/L，双氧水0.25～5g/L，硅烷偶联剂2～20g/L，有机成膜剂100～800g/L。
2.如权利要求1所述的镀锡板表面复合转化膜处理液，其特征在于，包括以下质量浓度的组分：钛盐0.5～1.5g/L，锆盐0.05～0.3g/L，磷酸和/或其化合物5～10g/L，双氧水0.5～1.5g/L，硅烷偶联剂5～10g/L，有机成膜剂300～500g/L。
3.如权利要求1或2所述的镀锡板表面复合转化膜处理液，其特征在于，包括以下质量浓度的组分：钛盐1.2g/L，锆盐0.3g/L，磷酸和/或其化合物6g/L，双氧水0.6g/L，硅烷偶联剂5g/L，有机成膜剂350g/L。
4.如权利要求1-3任一项所述的镀锡板表面复合转化膜处理液，其特征在于，所述钛盐为硫酸氧钛、六氟钛酸、二氧化钛中的一种或多种。
5.如权利要求1-3任一项所述的镀锡板表面复合转化膜处理液，其特征在于，所述磷酸和/或其化合物为磷酸、磷酸二氢锰、磷酸二氢铝、磷酸二氢锌、有机磷酸盐中的一种或多种。
6.如权利要求1-3任一项所述的镀锡板表面复合转化膜处理液，其特征在于，所述有机成膜剂为水性树脂和天然聚合物中的一种或两种。
7.如权利要求6所述的镀锡板表面复合转化膜处理液，其特征在于，所述水性树脂为水性聚氨酯树脂、水性酚醛树脂、水性丙烯酸树脂、水性环氧树脂、水性硅树脂和水性乙烯基树脂中的一种或两种。
8.一种利用权利要求1-7任一项所述的镀锡板表面复合转化膜处理液制备转化膜的工艺，其特征在于，包括以下步骤：
(1)将基材经前处理后得到镀锡板基板；
(2)调节镀锡板表面复合转化膜处理液的pH值为1.5～4.5，温度为10～40℃；
(3)将步骤(1)得到的镀锡板基板表面涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液；
(4)将经转化处理的镀锡板基板放入热风干燥箱中烘干、冷却，即完成镀锡板表面复合转化膜的制备。
9.如权利要求8所述的利用镀锡板表面复合转化膜处理液制备转化膜的工艺，其特征在于，所述步骤(3)中采用棒涂、辊涂、浸涂、喷涂、离心式“喷漆器”方法中的一种涂覆步骤(2)处理后的镀锡板表面复合转化膜处理液。
10.如权利要求8所述的利用镀锡板表面复合转化膜处理液制备转化膜的工艺，其特征在于，所述步骤(4)中烘干是在50～180℃条件下，烘烤2～5min。
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