CN100529180C - 用于铝和铝合金的预处理 - Google Patents
用于铝和铝合金的预处理 Download PDFInfo
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- CN100529180C CN100529180C CNB2004800027545A CN200480002754A CN100529180C CN 100529180 C CN100529180 C CN 100529180C CN B2004800027545 A CNB2004800027545 A CN B2004800027545A CN 200480002754 A CN200480002754 A CN 200480002754A CN 100529180 C CN100529180 C CN 100529180C
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 75
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 52
- 238000000576 coating method Methods 0.000 claims abstract description 52
- 239000011248 coating agent Substances 0.000 claims abstract description 49
- 239000000203 mixture Substances 0.000 claims abstract description 39
- 239000007864 aqueous solution Substances 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 31
- 230000002378 acidificating effect Effects 0.000 claims abstract description 22
- 239000002562 thickening agent Substances 0.000 claims abstract description 15
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 13
- 150000001845 chromium compounds Chemical class 0.000 claims abstract description 12
- 150000003752 zinc compounds Chemical class 0.000 claims abstract description 5
- 239000004411 aluminium Substances 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 46
- -1 alkali metal tetrafluoroborates Chemical class 0.000 claims description 35
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 32
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 27
- 239000011651 chromium Substances 0.000 claims description 25
- 229910052728 basic metal Inorganic materials 0.000 claims description 23
- 150000003839 salts Chemical class 0.000 claims description 22
- 229910052804 chromium Inorganic materials 0.000 claims description 21
- 230000003628 erosive effect Effects 0.000 claims description 19
- 239000011701 zinc Substances 0.000 claims description 14
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 13
- 239000003513 alkali Substances 0.000 claims description 13
- 150000003818 basic metals Chemical class 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 238000002203 pretreatment Methods 0.000 claims description 13
- 229910052725 zinc Inorganic materials 0.000 claims description 13
- 230000008719 thickening Effects 0.000 claims description 9
- 150000003751 zinc Chemical class 0.000 claims description 9
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 6
- 229910052731 fluorine Inorganic materials 0.000 claims description 6
- 239000011737 fluorine Substances 0.000 claims description 6
- 230000006872 improvement Effects 0.000 claims description 6
- 238000007781 pre-processing Methods 0.000 claims description 6
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000001913 cellulose Substances 0.000 claims description 4
- 229920002678 cellulose Polymers 0.000 claims description 4
- 150000004761 hexafluorosilicates Chemical class 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical group [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- BJZIJOLEWHWTJO-UHFFFAOYSA-H dipotassium;hexafluorozirconium(2-) Chemical compound [F-].[F-].[F-].[F-].[F-].[F-].[K+].[K+].[Zr+4] BJZIJOLEWHWTJO-UHFFFAOYSA-H 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 150000002222 fluorine compounds Chemical class 0.000 claims 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- 239000004094 surface-active agent Substances 0.000 abstract description 7
- 229910045601 alloy Inorganic materials 0.000 abstract description 4
- 239000000956 alloy Substances 0.000 abstract description 4
- 239000000080 wetting agent Substances 0.000 abstract description 2
- 150000001340 alkali metals Chemical class 0.000 abstract 2
- 230000008859 change Effects 0.000 description 10
- 239000002585 base Substances 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 230000007797 corrosion Effects 0.000 description 6
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- 238000007744 chromate conversion coating Methods 0.000 description 4
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 4
- 229960001763 zinc sulfate Drugs 0.000 description 4
- 229910000368 zinc sulfate Inorganic materials 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
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- 239000008399 tap water Substances 0.000 description 3
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- CKAPSXZOOQJIBF-UHFFFAOYSA-N hexachlorobenzene Chemical compound ClC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl CKAPSXZOOQJIBF-UHFFFAOYSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
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- 229940123973 Oxygen scavenger Drugs 0.000 description 1
- 241000978776 Senegalia senegal Species 0.000 description 1
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
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- 150000008055 alkyl aryl sulfonates Chemical class 0.000 description 1
- 125000004422 alkyl sulphonamide group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
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- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
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- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
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- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
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- 229920000151 polyglycol Polymers 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000001570 sorbitan monopalmitate Substances 0.000 description 1
- 235000011071 sorbitan monopalmitate Nutrition 0.000 description 1
- 229940031953 sorbitan monopalmitate Drugs 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
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- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 description 1
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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
- C09D5/084—Inorganic compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/12—Wash primers
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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
- C23C22/82—After-treatment
- C23C22/83—Chemical after-treatment
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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
- C23C2222/00—Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
- C23C2222/10—Use of solutions containing trivalent chromium but free of hexavalent chromium
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- Engineering & Computer Science (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
经预处理的铝和铝合金以及用于预处理所述铝和铝合金的组合物和方法,以提供具有为鉴别目的的颜色识别并且改善耐腐蚀性、电导率和粘附性质。该方法包括用有效量的pH值约为2.5~5.5的酸性水溶液预处理所述铝和铝合金,而所述酸性水溶液包括水溶性三价铬化合物、碱金属六氟锆酸盐、二价锌化合物、碱金属氟化合物以及有效量的水溶性增稠剂、表面活性剂或润湿剂。
Description
发明由来
此处描述的发明是美国政府雇员作出的,因此,为政府目的而由政府或为政府制造和使用本发明不需要支付任何使用费。
继续申请
本申请是共同待决申请序列号10/116,844(申请日为2002年4月5日)的部分继续申请,而10/116,844又是Matzdorf等在2000年10月31日申请的共同待决申请序列号09/702,225的部分继续申请,而09/702,225现在是2002年4月23日发布的专利6,375,726 B1。
发明背景
发明领域
本发明涉及铝和铝合金的保护和预处理、使用新组合物对铝和铝合金进行表面处理以及使用这些组合物在环境和更高温度预处理铝和铝合金的方法。该预处理涂层提供颜色识别,并改进在腐蚀环境中的耐腐蚀性、重叠涂层如涂料之间的粘附,并且保持低的电接触电阻。更具体而言,本发明涉及耐腐蚀性组合物以及在铝和铝合金上使用该组合物的方法,所述组合物包括含有有效量的至少一种水溶性三价铬盐、碱金属六氟锆酸盐、至少一种氟化合物、至少一种锌化合物和至少一种水溶性增稠剂的酸性水溶液。
现有技术的描述
当前很实用的是通过用保护膜初始涂敷或预处理金属表面来改善连续涂层的耐腐蚀性和与铝和铝合金的粘结性。转化涂层提高了未处理金属表面的耐腐蚀性,并制备出包括涂料等在内的修饰涂层的表面。这些转化或预处理涂层最常通过用含六价铬溶液进行涂敷。尽管这些涂层提供了良好的耐腐蚀性,但是因为考虑到六价铬对职业、安全、健康和环境的影响,因此人们尝试获得更受欢迎的非铬酸盐生成的涂层。六价铬是高毒性的,并且是已知的致癌物质。因此,用于沉积这些保护膜的溶液和膜本身是有毒且致癌的。然而,铬酸盐膜通过能提供优异的粘附和耐腐蚀性,并且易于通过包括浸渍、喷涂在内的各种方法或通过擦涂技术(wipe-ontechnique)进行涂敷。而且,环境法和OSH规章强制军事或商业用户寻找其它无毒、无铬酸盐的预处理。此外,由于规章的强制,使用铬酸盐转化涂层变得更加昂贵,而且由于EPA的强加限制,成本变得非常高。例如,某些工艺比如喷涂铬酸盐转化涂层由于OSH规章而被禁止,因此强迫使用没有达到最佳的备选方法。
通常已知铬酸盐水溶液包含部分溶解金属比如铝的表面并已知作为预处理或铬酸盐转化涂层的不溶膜的化学品。这些涂层具有耐腐蚀性,可保护金属避开会导致腐蚀的各种元素。虽然,这些转化涂层提高了耐腐蚀性,并改善了结合或粘附性质,但是该涂层有严重的缺陷,比如制备该涂层的溶液的毒性和涂敷膜中存在六价铬。这对于处理溶液比如处理所使用的铬酸盐溶液、铬酸盐污染的漂洗水和铬酸盐污染的涂层体系的操作者是严重的问题。然而,通过从工艺中除去六价铬可以避免这些问题。然而,该方法昂贵,并且在整个金属处理工艺中为主要的成本因素。因此,非常需要提供没有六价铬的工艺和保护涂层,但同时可以获得能够与传统铬酸盐基转化涂层所赋予的性质相媲美的耐腐蚀性和粘结性能。其中,特别感兴趣的是使用铝和铝合金的铬酸盐转化涂层,如大物体(比如飞机)的涂敷。因此,需要使用作为有毒六价铬涂层的替换物的相对无毒化学品为铝和铝合金提供保护涂层。
发明概述
本发明涉及铝和铝合金的酸性含水三价铬预处理(TCP)和用于提供涂层的颜色识别和涂层的鉴别,并且改善铝表面的粘附和耐腐蚀性的方法。具体地说,本发明涉及预处理铝,涉及在环境温度或更高温度(至高达约200°F)的温度范围预处理铝和铝合金的组合物和方法。所述预处理溶液包括pH值约为2.5~5.5、优选3.7~4.0的酸性水溶液,以每升所述溶液计,它包括约0.01~22克水溶性三价铬化合物;约0.01~12克碱金属六氟锆酸盐;约0.0~12克、优选0.01~1.2克(比如0.12~0.24克)选自由碱金属四氟硼酸盐、碱金属六氟硅酸盐和这两种盐的各种结合物或混合物组成的组中的至少一种氟化合物;约0.001~10克至少一种锌化合物;约0.0~10克/升、优选0.5~1.5克的至少一种水溶性增稠剂以及0.0~10克/升、优选0.5~1.5克的至少一种水溶性非离子、阳离子或阴离子表面活性剂。
由现有TCP涂层描述的组合物和方法的一个缺陷是在处于沉积状态(as deposited)涂层中缺少显著的颜色改变或颜色识别,尤其是用作铝合金的预处理时,存在这样的缺陷。铬酸盐基涂层通常具有易于被操作人员、质量控制人员和本领域中的其它用户识别的闪光金色到棕色。在铝元件上的金色通常表示存在铬酸盐的后处理,并且该颜色对于这种不考虑技术涂层性能如耐腐蚀或涂料粘结力的质量控制是有用的。前面描述的TCP涂层根据处理条件通常具有稍微浅蓝色到略带紫色到棕褐色,这种情况在混合光中诸如在生产设备、在修理仓库或制备工厂内都很难看到。在一些类似包层铝合金表面上的TCP实质上是无色的。因此,为提供涂层的颜色鉴定或识别的方式,本发明涉及用于制备铝和铝合金的耐腐蚀性涂层的组合物和方法。
该组合物包括使用酸性水溶液处理铝基材,所述酸性水溶液包括硫酸三价铬碱(trivalent chromium sulfate basic)、碱金属六氟锆酸盐和任选的纤维素基增稠剂和碱金属四氟硼酸盐和/或碱金属六氟硅酸盐稳定剂。此外,该组合物也必需包含锌基化合物比如二价盐,以使所制备涂层具有颜色识别。
因此,本发明目的是为改善电阻、粘附力和耐腐蚀性且提供用于鉴定被涂敷的铝的颜色识别,通过使用水溶液处理所述铝来提供预处理铝和其合金,所述水溶液包含三价铬化合物、碱金属六氟硅酸盐、有效量的碱金属四氟硼酸盐和/或六氟硅酸盐和至少一种锌化合物。
本发明另一目的是提供使用稳定酸性水溶液预处理铝和铝合金的方法,以获得用于鉴定涂层的颜色识别,所述酸性水溶液的pH值约为2.5~5.5,其包括有效量的三价铬盐、六氟锆酸盐和二价锌盐。
本发明的再一目的是提供具有良好“储藏寿命”的稳定酸性水溶液,该溶液包括三价铬盐、六氟锆酸盐和二价锌盐,其pH值约为2.5~5.5,用于在环境温度预处理铝和其合金,其中所述酸性预处理溶液基本上不包含六价铬。
本发明的这些及其它目的将从本发明进一步且更详细的描述中变得明显。
本发明的详细描述
本发明涉及三价铬化合物的酸性稳定水溶液,其pH值为约2.5~5.5,并优选3.7~4.0,而且涉及在环境温度或更高温度下用于预处理铝和铝合金的用途。所述稳定水溶液包括(以每升溶液计)约0.01~22克、优选约0.01~10克/升(比如5~7克)至少一种水溶性三价铬化合物,约0.01~12克、优选约0.01~8.0克(比如6-8克/升溶液)的至少一种碱金属六氟锆酸盐,约0.001~10克、优选0.1~5.0克/升的至少一种二价锌化合物,约0.0~12克、优选0.01~1.2克(比如0.12~0.24克)至少一种碱金属四氟硼酸盐,0.0~12克、优选0.01~1.2克(比如0.12~0.24克)碱金属六氟硅酸盐和所述硼酸盐和硅酸盐的任意组合,约0.0~10克/升溶液、优选0.5~1.5克/升溶液至少一种水溶性增稠剂(例如,水溶性有机增稠剂)以及0~10克至少一种表面活性剂或润湿剂。
在某些预处理中,碱金属四氟硼酸盐和/或六氟硅酸盐可以以低至0.001克/升到该化合物的溶解极限的量加入到溶液中。例如,以六氟硅酸盐的重量计,可以加入约50重量%的氟硅酸盐。换句话说,对于8克/升的氟锆酸盐,可以向溶液中加入约4克/升的氟硅酸盐。备选方案是以氟锆酸盐的重量计,加入约0.01~100重量%的氟硼酸盐。优选地,以氟锆酸盐的重量计,可以加入约1~10重量%(比如3%)氟硼酸盐。具体实例包括约8克/升的六氟锆酸盐、约6克/升的硫酸铬III碱、约0.1~5.0克/升的硫酸二价锌和约0.12~0.24克/升四氟硼酸钾。加入稳定添加剂比如氟硼酸盐和/或氟硅酸盐的重要结果是溶液稳定,并且pH值保持在约2.5~5.5。然而,在某些情况下,预处理溶液为保持其pH值在约2.5~5.5,需要通过加入有效量的稀酸或碱来轻微调节pH值。
三价铬可以以任意水溶性三价铬化合物形式加入到水溶液中,优选以三价铬盐加入。具体而言,在配置本发明含水涂层过程中,铬盐以其水溶形式便利地加入到溶液中,其中铬的价态是正3价。一些优选铬化合物以Cr2(SO4)3,(NH4)Cr(SO4)2,Cr(OH)SO4,Cr2O3或KCr(SO4)2形式和这些化合物的各种组合的水溶液加入。优选三价铬浓度在约0.01~10克/升水溶液,并且发现当三价铬以该优选范围存在时,经济地获得尤其良好的结果。优选碱金属氟锆酸盐以约0.01~8.0克/升加入到溶液中。
为调节赋予涂层的颜色,锌盐的量可以变化,可以从小至0.001克/升到高达10克/升。Zn2+阳离子或二价锌可以通过溶解在水中的任一化学物供给,并且与组合物中的其它组分相适合。一些特别优选的化合物包括乙酸锌、碲化锌、四氟硼酸锌、钼酸锌、六氟硅酸锌、硫酸锌以及这些化合物任意比例的组合。
铝和铝合金的预处理可以在包括温度范围为环境温度比如约室温到高达约200°F的预处理溶液温度在内的各种温度下进行。然而,优选室温,因为这可以不需要加热设备。涂层可以通过本领域已知的任意方法进行空气干燥,例如烘箱干燥、鼓风干燥、暴露在红外灯下等。就本发明目的而言,术语“铝”拟包括基本上纯的铝和含有各种其它金属的任意铝合金,尤其是铝含量超过60重量%的任意铝合金。
下列实施例解释本发明稳定的预处理溶液以及使用该溶液的方法,该溶液可以在铝和铝合金上提供颜色识别并改善涂层的粘附力和耐腐蚀性。
实施例1
(TCP5P)
pH值约为3.45~4.0的稳定酸性预处理水溶液,用于预处理铝和铝合金,以在铝和铝合金上形成耐腐蚀性涂层,该酸性预处理水溶液包括(以每升溶液计)约3.0克硫酸三价铬碱和约4.0克六氟锆酸钾。
实施例2
(TCP5PZ2)
pH值约为3.45~4.0的稳定酸性水溶液,用于预处理铝和铝合金,以在铝和铝合金上形成耐腐蚀性和颜色识别的涂层,该酸性预处理水溶液包括(以每升溶液计)约3.0克硫酸三价铬碱、约4.0克六氟锆酸钾和约1.0克硫酸锌。
实施例3
(TCP5B3)
用于预处理铝和铝合金以在铝和铝合金上形成耐腐蚀性涂层的稳定酸性水溶液,其包括(以每升溶液计)约3.0克硫酸三价铬碱、约4.0克六氟锆酸钾和约0.12克四氟硼酸钾。
实施例4
(TCP5B3Z4)
用于预处理铝和铝合金以在铝和铝合金上形成耐腐蚀性和颜色识别涂层的稳定酸性水溶液,其包括(以每升溶液计)约3.0克硫酸三价铬碱、约4.0克六氟锆酸钾、约0.12克四氟硼酸钾和约2.0克硫酸二价锌。
实施例5
(TCP5PZA)
用于预处理铝和铝合金以在铝和铝合金上形成耐腐蚀性和颜色识别涂层的稳定酸性水溶液,其包括(以每升溶液计)约3.0克硫酸三价铬碱、约4.0克六氟锆酸钾和约5.0克乙酸二价锌。
实施例6
具有改善的耐腐蚀性和粘附性质的经预处理的铝和铝合金包括用有效量的酸性水溶液处理的所述铝和铝合金,所述水溶液的pH值约为3.7~4.0,并且包含(以每升所述溶液计)约0.01~10克水溶性三价铬盐;约0.01~8克碱金属六氟锆酸盐;约0.01~1.2克选自由碱金属四氟硼酸盐、碱金属六氟硅酸盐和这两种盐的混合物组成的组中的至少一种氟化合物;约0~10克至少一种水溶性增稠剂以及0~10克至少一种水溶性表面活性剂。
实施例7
pH值约为2-6的酸性水溶液,用于在铝和铝合金上制备耐腐蚀性涂层,它基本上由如下物质组成(以每升溶液计):约3.0~22克水溶性三价铬盐;约1.5~11.5克碱金属六氟锆酸盐;约0~10克至少一种水溶性增稠剂以及0~10克至少一种水溶性表面活性剂。
形成三价铬预处理之前,处理铝基材,即用碱性磷酸盐清洗剂Turco4215 NC-LT在约100~140°F温度对铝清洗约15分钟,自来水漂洗,随后在环境条件下在无铬酸盐的去氧剂(Turco Smut Go NC)中浸渍约1~15分钟,然后再用环境自来水漂洗。然后在环境条件下,洁净基材在酸性硫酸三价铬溶液中浸渍约30秒~60分钟,随后以环境自来水漂洗,静置,直到干燥为止。在备选方法中,铝基材在高温用碱性磷酸盐清洗剂喷洗约15分钟,然后用冷自来水漂洗,再在环境条件下用(Turco Smut Go NC)喷洗约30秒。
用本发明的三价铬溶液涂敷铝基材,可以通过喷涂、擦涂或浸渍铝板进行。接触持续时间为约30秒到约5分钟,但当三价铬浓度或溶液温度较低时,也可需要更长的接触时间,例如高达60分钟或更长。水溶液温度通常低于100℃,例如在15~75℃,又如约25℃。铝温度约为15~30℃。
表A-1、A-2和A-3
比色法结果
(所有读数取自Hunterlabs D25PC2色度计)
表A-1
表A-2
表A-3
在表A-1、A-2和A-3中,L是灰度级,其中L=100是纯白,L=0是纯黑,而L=50是灰色。表中“a”是红色到绿色的等级,其中0是中立值,+50是纯红、而-50是纯绿。表中“b”是黄色到蓝色的等级,其中0是中立值,+50是纯黄、而-50是纯蓝。结合“a”和“b”值可给出所需颜色(例如,-b,+a为略带紫色,“b”=-50和“a”=+50为纯紫色),而L值表示板的暗度。
表B
产生涂层的颜色改变和识别的代表性组合物和方法
名称 | 组合物 | 方法 | 评论 | 文件比较 |
TCP5P | 3克/升硫酸铬(III)碱和4克/升六氟锆酸钾实施例1 | 环境条件下,组合物在铝表面上停留2~5分钟 | 产生没有实际颜色改变的涂层的基准组合物和方法 | 实施例7 |
TCP5B3 | TCP5P和0.12克/升四氟硼酸钾实施例3 | 环境条件下,组合物在铝表面上停留2~5分钟 | 产生没有实际颜色改变的涂层的稳定组合物和方法 | 实施例6 |
TCP5PZ2 | TCP5P和1.0克/升硫酸锌实施例2 | 环境条件下,组合物在铝表面上停留1~10分钟 | 产生有实际颜色改变的涂层的基准组合物和方法 | 发明 |
TCP5B3Z4 | TCP5B3和2.0克/升硫酸锌实施例4 | 环境条件下,组合物在铝表面上停留1~10分钟 | 产生有实际颜色改变的涂层的稳定组合物和方法 | 发明 |
TCP5PZA | TCP5P和5.0克/升乙酸锌实施例5 | 环境条件下,组合物在铝表面上停留1~10分钟 | 产生有实际颜色改变的涂层的缓冲基准组合物和方法 | 发明 |
术语“实际颜色改变”表示容易看见、可识别的颜色,它对涂层的腐蚀性能没有不良影响。术语“硫酸铬III碱”定义在Kirk-Othmer Encyclopediaof Chemical Knowledge:第六卷、第三版(95-96页)。
与前面公布的三价铬基铝预处理相比,本组合物和方法的优点是容易看到在沉积状态涂层的颜色改变和识别。表A-1、A-2和A-3详述了在没有锌化合物的情况下,涂敷有本发明描述的TCP溶液的各种铝合金的色度测量,并与以前公开的TCP溶液相比。表B描述了在没有锌盐的情况下,用于沉积本发明预处理涂层的代表性组合物和方法,并与现有的TCP涂层相比较。
当大表面铝不能浸泡或垂直表面喷涂时,加入增稠剂以使水溶液在表面上有充足的接触时间。所使用的增稠剂是已知水溶性或水分散性增稠剂,该增稠剂以约0.0~约10克/升、优选约0.5~1.5克/升水溶液的量加入到本发明的三价铬溶液中。这些增稠剂的具体实例包括优选纤维素增稠剂,例如羟丙基纤维素(例如,Klucel);乙基纤维素;羟乙基纤维素;羟甲基纤维素;甲基纤维素以及一些其它已知的水溶性增稠剂,如胶体二氧化硅、诸如膨润土之类的粘土、淀粉、胶体氧化铝、阿拉伯树胶、黄蓍胶、琼脂以及它们的各种组合。
对本发明来说,以每升TCP溶液计,水溶性表面活性剂可以以约0.0~约10克/升、优选约0.5~1.5克/升的量使用。表面活性剂加入到水溶液中,通过降低表面张力而提供更好的润湿性能,由此确保完全覆盖以及涂层在基材上更均匀。所述表面活性剂包括至少一种水溶性化合物,它选自由非离子、阴离子和阳离子表面活性剂组成的组中。具体水溶性表面活性剂包括单羧基咪唑啉、烷基硫酸钠盐()、十三烷基氧聚(烷撑氧乙醇)、乙氧基化或丙氧基化烷基苯酚()、烷基磺酰胺、烷芳基磺酸盐、棕榈烷基醇酰胺()、辛基苯基聚乙氧乙醇()、脱水山梨糖醇单棕榈酸酯()、十二烷基苯基聚乙二醇醚(例如,)、烷基吡咯烷酮、聚烷氧基化脂肪酸酯、烷基苯磺酸酯(盐)以及它们的混合物。其它已知的水溶性表面活性剂由John Wiley & Sons inKirk-Othmer’s Encyclopedia of Chemical Technology出版的“Surfactants andDetersive Systems”(第三版)公开。
尽管本发明通过大量具体实例进行描述,但是很明显在不背离如所附权利要求详细陈述的本发明精神和范围的情况下,可以进行其它变化和改进。
Claims (25)
1.一种预处理铝或铝合金的方法,所述预处理用以提供具有颜色识别的涂层和改善的耐腐蚀性、电导率和粘附性质,所述方法包括用有效量的pH值为2.5~5.5的酸性水溶液处理所述铝或铝合金,所述酸性水溶液以每升所述溶液计包含:0.01~22克水溶性三价铬化合物;0.01~12克碱金属六氟锆酸盐;大于0.0克但不高于12克选自由碱金属四氟硼酸盐、碱金属六氟硅酸盐和这两种盐的混合物组成的组中的至少一种水溶性氟化合物;0.001~10克至少一种水溶性锌化合物;以及0~10克的至少一种水溶性增稠剂。
2.一种预处理铝或铝合金的方法,所述预处理用以提供具有颜色识别的涂层和改善的耐腐蚀性、电导率和粘附性质,所述方法包括用有效量的pH值为3.7~4.0的水溶液在室温下处理所述铝或铝合金,所述水溶液以每升溶液计包含:0.01~10克水溶性三价铬盐;0.01~8.0克碱金属六氟锆酸盐;大于0.0克但不高于12克选自由碱金属四氟硼酸盐、碱金属六氟硅酸盐和这两种盐的混合物组成的组中的至少一种氟化合物;以及0.001~10克至少一种水溶性二价锌盐。
3.如权利要求1所述的方法,其中所述水溶液的pH值为3.7~4.0,所述水溶液的温度为室温到200°F。
4.如权利要求3所述的方法,其中所述三价铬化合物为5.0~7.0克,所述六氟锆酸盐为6.0~8.0克,所述四氟硼酸盐为0.01~1.2克。
5.如权利要求1所述的方法,其中所述增稠剂为0.5~1.5克的纤维素化合物。
6.如权利要求2所述的方法,其中所述四氟硼酸盐以0.12~0.24克的量存在于溶液中。
7.如权利要求2所述的方法,其中0.5~1.5克的纤维素增稠剂加入到预处理溶液中。
8.如权利要求2所述的方法,其中所述铬盐为硫酸三价铬。
9.如权利要求1所述的方法,其中所述碱金属六氟锆酸盐为六氟锆酸钾。
10.如权利要求2所述的方法,其中所述二价锌盐为硫酸二价锌,其含量为0.01~5.0克/升。
11.经预处理的铝或铝合金,其具有颜色识别涂层,和改善的耐腐蚀性、电导率和粘附性质,其包括用有效量的pH值为2.5~5.5的酸性水溶液处理的所述铝或铝合金,所述酸性水溶液以每升所述溶液计包含:0.01~22克水溶性三价铬化合物;0.01~12克碱金属六氟锆酸盐;大于0.0克但不高于12克选自由碱金属四氟硼酸盐、碱金属六氟硅酸盐和这两种盐的混合物组成的组中的至少一种氟化合物;0.001~10克至少一种水溶性锌化合物;以及0~10克的至少一种水溶性增稠剂。
12.经预处理的铝或铝合金,其具有颜色识别涂层,和改善的耐腐蚀性、电导率和粘附性质,其包括用有效量的pH值为3.7~4.0的酸性水溶液处理的所述铝或铝合金,所述酸性水溶液以每升所述溶液计包括0.01~10克水溶性三价铬盐;0.01~8.0克碱金属六氟锆酸盐;大于0.0克但不高于12克选自由碱金属四氟硼酸盐、碱金属六氟硅酸盐和这两种盐的混合物组成的组中的至少一种氟化合物;0.001~10克至少一种水溶性二价锌盐以及0~10克至少一种水溶性增稠剂。
13.如权利要求11所述的经预处理的铝或铝合金,其中所述增稠剂为0.5~1.5克。
14.如权利要求11所述的经预处理的铝或铝合金,其中所述锌化合物为硫酸二价锌,所述六氟硅酸盐以0.01~1.2克的量存在。
15.如权利要求11所述的经预处理的铝或铝合金,其中所述四氟硼酸盐以0.01~1.2克的量存在于溶液中。
16.如权利要求11所述的经预处理的铝或铝合金,其中所述水溶性增稠剂是以0.5~1.5克的量存在于该溶液中的纤维素增稠剂。
17.如权利要求11所述的经预处理的铝或铝合金,其中所述铬化合物为硫酸三价铬。
18.如权利要求11所述的经预处理的铝或铝合金,其中所述碱金属六氟锆酸盐为六氟锆酸钾。
19.如权利要求12所述的经预处理的铝或铝合金,其中所述锌盐为硫酸二价锌。
20.如权利要求12所述的经预处理的铝或铝合金,其中所述锌盐为乙酸锌。
21.一种组合物,用于预处理铝或铝合金以提供颜色可识别涂层和改善的被涂敷铝的耐腐蚀性、电导率和粘附性质,它包括pH值为2.5~5.5的水溶液,而所述水溶液以每升所述溶液计包含:0.01~22克水溶性三价铬化合物;0.01~12克碱金属六氟锆酸盐;大于0.0克但不高于12克选自由碱金属四氟硼酸盐、碱金属六氟硅酸盐和这两种盐的混合物组成的组中的至少一种水溶性氟化合物;0.001~10克至少一种水溶性锌化合物;以及0~10克的至少一种水溶性增稠剂。
22.如权利要求21所述的组合物,其中pH值为3.7~4.0。
23.如权利要求21所述的组合物,其中所述三价铬化合物为硫酸三价铬碱。
24.如权利要求21所述的组合物,其中所述锌化合物为硫酸二价锌。
25.如权利要求21所述的组合物,其中所述锌化合物为乙酸二价锌。
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