WO1992014862A2 - Procede de traitement des surfaces contenant de l'aluminium - Google Patents
Procede de traitement des surfaces contenant de l'aluminiumInfo
- Publication number
- WO1992014862A2 WO1992014862A2 PCT/US1991/009668 US9109668W WO9214862A2 WO 1992014862 A2 WO1992014862 A2 WO 1992014862A2 US 9109668 W US9109668 W US 9109668W WO 9214862 A2 WO9214862 A2 WO 9214862A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- aluminum
- primary film
- process according
- film
- phosphate
- Prior art date
Links
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 75
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminum Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 23
- 239000010959 steel Substances 0.000 claims abstract description 23
- 229910052742 iron Inorganic materials 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims description 17
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 11
- 150000002500 ions Chemical class 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 229910052803 cobalt Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 6
- 229910000838 Al alloy Chemical group 0.000 claims description 5
- 229910001335 Galvanized steel Inorganic materials 0.000 claims description 4
- 229910045601 alloy Inorganic materials 0.000 claims description 4
- 239000000956 alloy Substances 0.000 claims description 4
- 238000005238 degreasing Methods 0.000 claims description 4
- 239000008397 galvanized steel Substances 0.000 claims description 4
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical class [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000007746 phosphate conversion coating Methods 0.000 claims 3
- 229910004074 SiF6 Inorganic materials 0.000 claims 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims 1
- 239000010941 cobalt Substances 0.000 claims 1
- 150000002739 metals Chemical class 0.000 claims 1
- 229920000136 polysorbate Polymers 0.000 claims 1
- 239000010452 phosphate Substances 0.000 abstract description 50
- NBIIXXVUZAFLBC-UHFFFAOYSA-K [O-]P([O-])([O-])=O Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract description 49
- 239000007788 liquid Substances 0.000 abstract description 31
- HCHKCACWOHOZIP-UHFFFAOYSA-N zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052725 zinc Inorganic materials 0.000 abstract description 11
- 239000011701 zinc Substances 0.000 abstract description 11
- 239000002131 composite material Substances 0.000 abstract description 9
- -1 Cr6+ ion Chemical class 0.000 abstract description 6
- 238000004381 surface treatment Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 80
- 235000021317 phosphate Nutrition 0.000 description 50
- 230000015572 biosynthetic process Effects 0.000 description 10
- 238000005755 formation reaction Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 238000005260 corrosion Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- UKNAYQWNMMGCNX-UHFFFAOYSA-N sodium;[hydroxy(phenyl)methyl]-oxido-oxophosphanium Chemical compound [Na+].[O-][P+](=O)C(O)C1=CC=CC=C1 UKNAYQWNMMGCNX-UHFFFAOYSA-N 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000007654 immersion Methods 0.000 description 4
- 238000010422 painting Methods 0.000 description 4
- 238000003466 welding Methods 0.000 description 4
- OHORFAFFMDIQRR-UHFFFAOYSA-P Hexafluorosilicic acid Chemical compound [H+].[H+].F[Si-2](F)(F)(F)(F)F OHORFAFFMDIQRR-UHFFFAOYSA-P 0.000 description 3
- 239000010960 cold rolled steel Substances 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 239000010687 lubricating oil Substances 0.000 description 3
- 230000001264 neutralization Effects 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 229910000975 Carbon steel Inorganic materials 0.000 description 2
- 229910000737 Duralumin Inorganic materials 0.000 description 2
- 241000201593 Nihon Species 0.000 description 2
- NROKBHXJSPEDAR-UHFFFAOYSA-M Potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 2
- 229910001297 Zn alloy Inorganic materials 0.000 description 2
- 230000002378 acidificating Effects 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 230000000717 retained Effects 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L Cobalt(II) chloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 241001137251 Corvidae Species 0.000 description 1
- NMCUIPGRVMDVDB-UHFFFAOYSA-L Iron(II) chloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910020826 NaAlF6 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229940037003 alum Drugs 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000005591 charge neutralization Effects 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 235000015108 pies Nutrition 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000011698 potassium fluoride Substances 0.000 description 1
- 235000003270 potassium fluoride Nutrition 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000001187 sodium carbonate Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011775 sodium fluoride Substances 0.000 description 1
- 235000013024 sodium fluoride Nutrition 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
Definitions
- This invention concerns a method of treating a surface including metallic aluminum or an aluminum alloy that is at least 45 % by weight, or preferably at least 85 % by weight, aluminum, in order to form on the surface a film which has excellent corrosion resistance, painting proper ⁇ ties and electrodeposition painting properties.
- aluminum is to be understood as including aluminum alloys as specified above, and constitutions specified in percent ⁇ ages are to be understood as percentages by weight unless otherwise stated.
- the process according to the invention is particularly suited to surfaces in sheet or strip form. In recent years, there has been a tendency to use aluminum sheet for parts of an automobile body in order to reduce the weight of automobiles.
- the aluminum sheet or press formed aluminum sheet forms a com ⁇ posite material in which it is joined by welding, bonding or bolting to zinc alloy plated steel sheet, alloyed zinc plated steel sheet, zinc plated steel sheet, or the like.
- This present invention also concerns a method of forming films which have excellent corrosion resistance and paint ⁇ ing properties on these composite materials.
- phosphate treatment liquids which con ⁇ tained fluoride, especially in the form of silicofluoride, were used in the main for forming phosphate films on alum ⁇ inum sheets and formed and worked aluminum sheets.
- Acidic sodium fluoride and acidic potassium fluoride have been added to phosphate treatment liquids as a means of precipitating and removing the Al 3+ ion as K 2 NaAlF 6 com ⁇ pounds in order to prevent the lowering of the forming properties due to the admixture of Al 3+ ions as mentioned above, but fluorine is contained in the precipitate and this is undesirable from the viewpoint of pollution.
- This present invention takes as one of its objects the provision of a method for the formation of phosphate films with which the Al 3+ ion does not substantially increase in the phosphate treatment liquid and with which there is no deterioration of the phosphate film forming properties.
- this present invention discloses a method for the uniform formation of a phosphate film which has ex ⁇ cellent corrosion resistance and painting properties on composite materials in which a press worked aluminum sheet and a steel sheet or a zinc based plated steel sheet are combined.
- a primary film of Ni, Fe or Co, or a composite of two or more of these is formed on the aluminum sheet and washed with water.
- Pure aluminum and aluminum alloys of which aluminum is the principal component for example pure aluminum such as IS and 2S, corrosion resistant aluminum and magnesium based alloys such as 52S and 56S, aluminum and manganese based alloys such as 3S, aluminum and magnesium alloys such as 61S and 63S, duralumin such as 14S, 17S and 24S, and extra super duralumin such as 74S and 75S can be used for the aluminum sheet in this present invention.
- sheets of these aluminum materials are included among the aluminum sheets of this present invention.
- a primary film of Ni, Fe, Co is formed on these aluminum sheets.
- This primary film is obtained by coating Ni, Fe, Co on the aluminum sheet, preferably in an amount calculated as metal of 5 - 100 mg/m 2 using a non-electrolytic or cathodic electrolytic method.
- This primary film can be formed using a simple method, as described hereinafter, and moreover it is not lost on cold forming and working or in the phosphate forming treatment and so it is desirable as a primary film.
- An example of a method of forming a primary film of Ni, Fe, Co or a compositie non-electrolytically is de ⁇ scribed below.
- First of all the aluminum sheet is de- greased and washed, using alkali for example.
- the aluminum sheet is immersed for from 5 seconds to 2 minutes in a warm solution of 15 g/1 of sodium carbonate, 25 g/1 of sodium phosphate and surfactant, the oil and grease and the oxide film are removed from the aluminum sheet and a surface which is suitable for the deposition of Ni, Fe, Co or a combination thereof is obtained.
- the de- greased and washed aluminum film is washed with water, neu ⁇ tralized with nitric acid, sulfuric acid or the like and washed with water.
- the treatment liquid for forming the primary film is an aqueous solution, used at a temperature in the range from normal ambient temperature to 80° C, which contains Fe 2+ , Fe 3+ , Ni 2+ , and/or Co 2+ , and, by immersing the degreased and washed aluminum sheet in this - A - aqueous solution, or by spraying the aqueous solution onto the aluminum sheet, a primary film of Ni, Fe, and/or Co can be formed on the aluminum sheet.
- the aluminum sheet is im ⁇ mersed in an aqueous solution which contains Fe 2+ , Fe 3+ , Ni 2+ , and/or Co 2+ and a thin film is formed on the aluminum sheet, for example by cathode electrolysis at a current density of 0.3 - 30 amps/dm 2 with a quantity of electricity of from 0.3 to 10 coulombs/dm 2 .
- a solution in which from 20 to 50 grams of iron chloride or nickel chlor ⁇ ide or cobalt chloride and 100 milliliters ("ml") of in ⁇ dustrial hydrochloric acid have been dissolved in 1 liter of water can be used for the aqueous solution which con- tains Fe 2+ , Fe 3+ , Ni 2+ , and/or Co .
- nitrates, sulfates, phosphates and condensed phosphates are suitable, non-exclusive counterions for the aforementioned metal ions, and phosphoric acid, sulfuric acid, and nitric acid are suitable, non-exclusive acids for ajusting the acidity of the plating solution.
- the immersion time or cathode electrolysis time in the treatment liquid with which the primary film is formed is selected appropriately according to the composition of the aluminum sheet, but a metal primary film of Ni, Fe, and/or Co of some 5 - 100 mg/m 2 is formed on the aluminum sheet by means of this procedure.
- the aluminum sheet is then washed with water and rinsed, whereupon an aluminum sheet on which a primary film of Ni, Fe or Co, or an alloy of two or more of these, is obtained as part of this present invention.
- a phosphate film is then formed on the aluminum sheet on which the primary film has been formed, using a treat ⁇ ment liquid which contains fluoride.
- the primary film when a phosphate film is formed on an aluminum sheet on which the primary film had been formed, the increase in Al 3+ ion in the treatment liquid is prevented and excellent phosphate film forming properties can be maintained over a long per ⁇ iod of time. Furthermore, after the primary film has been formed on the aluminum sheet, the secondary phosphate film has been formed and an anti-rusting oil has been applied, the product can be obtained as a surface treated aluminum sheet. Furthermore, the primary film is not lost even if the aluminum sheet is press formed using the usual press lubricating oils, and it is retained on the aluminum sheet surface after press forming.
- composite mater- ials comprised of aluminum sheets and zinc plated steel sheets or plain steel sheets using aluminum sheets on which a primary film of Ni, Fe, and/or Co had been formed in an amount calculated as metal of 5 - 100 mg/m 2 , or an aluminum sheet obtained by press forming such a sheet, by joining with spot welding to the zinc based plated steel sheet or steel sheet.
- a phosphate film was formed on these compos ⁇ ite materials using a phosphate film treatment liquid which contained fluorides of sodium and potassium, and good phos ⁇ phate films could be formed on the aluminum sheet and on the zinc plated steel sheet or steel sheet.
- Figure 1 is a drawing which shows the shape and size of the pressed formed product in Examples 2, and Figure 2 is an explanatory drawing of the bonded composite work- pieces in example 3. Details of Some Preferred Embodiments of the Invention
- the inventors prepared in each case 100 aluminum sheets on which a primary film had been formed as shown in Table 1, using commercially pure aluminum sheet (Type 2S)
- Test panels were initially degreased and cleaned by immersion for 5 minutes in a solution of FINECLEANERTM 315, comemrcially available from Nihon Parkerizing Co. , Ltd. , at a temperature of 55 - 60 ° C. Panels were then treated with 1 % aqueous hydrochloric acid solution as a neutral ⁇ izing rinse before the treatments detailed above. with width of 300 mm, length of 300 mm, and thickness of 0.8 mm. These sheets were then subjected to the following process steps: De-grease and wash ⁇ water wash ⁇ neutral ⁇ ization rinse ⁇ water wash ⁇ primary film formation ⁇ wash ⁇ dry ⁇ anti-rusting oil coating ⁇ left to stand for 1 week indoors.
- the de-greasing washing, neutralization and primary film forming treatment conditions were as shown in table 1.
- the sa - pies were phosphated.
- the phosphate film formation results are shown in Table 3.
- the samples were also subjected to a Filiform Corro ⁇ sion Promotion Test Method, as follows: A specimen in which scratches had been made in a cationically electrode- posited paint film surface were immersed for 2 hours in 0.5N HC1 aqueous solution which contained 1% H 2 0 2 at 30°C and then washed with water and dried. Then, they were left to stand for 240 hours in a room at 40°C and 85% relative humidity, and an assessment was made after six of these cycles. The filiform corrosion length was less than 5 mm for Experiments 1. 1 and 1.4, 5 - 10 mm for the remaining Experiments 1.2, 1.3, 1.5, and 1.6, and more than 11 mm for Comparison Experiment 1.7.
- the aluminum ion concentrations are given in parts per million by weight.
- Degreasing Washing Immersed for 2.0 minutes in an aqueous solution of FINECLEANER L4460 (made by Nihon Parkerizing Co.) Furthermore, the press forming was carried out with deep cylindrical pressing as shown in figure 1. Also, the phosphate film forming treatment was carried out with the same immersion time (2.0 minutes/ sheet) using the same treatment liquid as in table 2. The results of phosphate film formation were as shown in Table 4. As shown in Table 4, the aluminum sheets on which a primary film of this invention had been formed and which had been press formed were such that a phosphate film could be formed in roughly the same way as with aluminum sheets which had not been subjected to press forming, as described in Table 3.
- Seams were formed by spot welding formed hot dip gal ⁇ vanized steel sheets which had been press formed and worked, instead of the cold rolled steel sheet as noted in the preceding paragraph, onto aluminum sheet on which a primary film had been formed and a phosphate film forming treatment was carried out using the same procedure, and in this case again a good phosphate film was formed on the zinc plated steel sheet and the aluminum sheet.
- a phosphate film which has excellent corrosion resistance and painting properties is formed uniformly, in a state in which the dissolution of aluminum into the phos ⁇ phate treatment liquid is suppressed, on an aluminum sur ⁇ face or a composite in which an aluminum surface, which may be press worked, is combined with a steel or a galvanized steel surface, which may or may not have been press worked.
Abstract
Un film primaire de Ni, Fe, et/ou Co est constitué sur une surface d'aluminium, un film phosphate est ensuite constitué sur cette surface d'aluminium ayant reçu ce film primaire, ou sur une surface d'un composite d'aluminium sur laquelle un film primaire a été constitué, avant d'être combiné à une tôle d'acier enduite à base de zinc. Cette méthode de traitement de surface n'entraîne pas les problèmes de pollution courants par l'ion Cr6+ et par F-, et l'on constate à l'usage une faible dégradation du liquide de traitement servant à réaliser le film phosphate.
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
BR9107278A BR9107278A (pt) | 1990-12-25 | 1991-12-26 | Processo para revistimento protetor de uma superfície metálica |
AU91713/91A AU655622B2 (en) | 1990-12-25 | 1991-12-26 | Method for treating aluminum containing surfaces |
EP92903444A EP0679200A1 (fr) | 1990-12-25 | 1991-12-26 | Procede de traitement des surfaces contenant de l'aluminium |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2/405446 | 1990-12-25 | ||
JP40544690A JPH04224684A (ja) | 1990-12-25 | 1990-12-25 | アルミニウム板およびその複合物の表面処理法 |
Publications (3)
Publication Number | Publication Date |
---|---|
WO1992014862A1 WO1992014862A1 (fr) | 1992-09-03 |
WO1992014862A2 true WO1992014862A2 (fr) | 1992-09-03 |
WO1992014862A3 WO1992014862A3 (fr) | 2004-04-29 |
Family
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