EP1017505A1 - Water-based liquid treatment for aluminum and its alloys - Google Patents
Water-based liquid treatment for aluminum and its alloysInfo
- Publication number
- EP1017505A1 EP1017505A1 EP98923440A EP98923440A EP1017505A1 EP 1017505 A1 EP1017505 A1 EP 1017505A1 EP 98923440 A EP98923440 A EP 98923440A EP 98923440 A EP98923440 A EP 98923440A EP 1017505 A1 EP1017505 A1 EP 1017505A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- protective coating
- aluminum
- titanium
- zirconium
- amount
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- C23C22/48—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 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/56—Treatment of aluminium or alloys based thereon
-
- 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
Definitions
- This invention concerns a novel liquid for the surface treatment of aluminum or aluminum alloy materials for imparting superior corrosion resistance and paint film holding properties to such surfaces.
- Fields in which the invention can be used with particular effectiveness include the surface treatment of aluminum heat exchanger fins and aluminum alloy coils and sheets.
- the liquids used for the surface treatment of aluminum and aluminum alloy materials can be broadly classified as being of the chromate type or the non-c romate type. Chromic acid chromate forming treatment liquids and phosphoric acid chromate forming treatment liquids can be cited as typical examples of chromate type treatment liquids.
- Chromic acid chromate forming treatment liquids have been in practical use since about 1950 and today they are widely used for the surface treatment of heat ex-change fins, aluminum wheels, building materials and aircraft materials. These chromic acid chromate forming treatment liquids contain chromic acid and fluoride as a reaction promotor as essential components, and a formed film which contains some hexavalent chromium is obtained on the metal material surface.
- Phosphoric acid chromate forming treatment liquids are an invention disclosed in U.S. Patent 2,438,877; they contain chromic acid, phosphoric acid and hydrofluoric acid as the main components, and a formed film which has hydrated chromium phosphate as the main component is obtained on the metal material surface. No hexavalent chromium is included in this formed film. Therefore these materials are being widely used at the present time as a paint undercoating treatment for the bodies and lids of beverage cans.
- This surface treatment liquid is an acidic aqueous coating solution, with a pH from about 1.5 to about 4.0, which contains zirconium or titanium or a mixture of the two, phosphate and fluoride.
- a formed film which has zirconium or titanium oxide as the main component is obtained on the metal surface when a metal surface is treated with such a surface treatment liquid.
- the non-chromate type surface treatment liquids do have the advantage of not containing hexavalent chromium, and they are widely used at present for the surface treatment of drawn-and-ironed (hereinafter usually abbreviated as "DI") aluminum cans, but there is a disadvantage in that the corrosion resistance of the film which is formed is not as good as that of a chromate film. Furthermore, the method of treatment disclosed in Japanese Unexamined Patent
- Application (Kokai) 57-41376 involves the surface treatment of the surface of aluminum, magnesium, or an alloy of these metals, using an aqueous solution which contains one type, or two or more types, of titanium salt or zirconium salt and one type, or two or more types, of imidazole derivative.
- the corrosion resistance of the film is such that there is no rusting in 48 hours when tested in accordance with JIS-Z-2371. However, although this performance was satisfactory 15 years ago, it cannot be said to be truly adequate at the present time.
- oxidizing agents such as nitric acid or hydrogen peroxide or potassium permanganate can be used as well, being added in amounts, calculated as compounds, of from 0.01 to 100 grams per liter (hereinafter usually abbreviated as "g/l"), but there are no illustrative examples of oxidizing agents such as potassium permanganate.
- a method of surface treatment whereby a formed film is obtained on the surface of an aluminum material with an aqueous solution which contains potassi- urn permanganate or potassium manganate, or both of these materials, and mineral acid (HN0 3 , H 2 S0 4 , HF), alkali (KOH, NaOH, NH 4 OH), neutral fluoride (KF, NaF), acidic fluoride (NH 4 HF 2 , NaHF 2 , KHF 2 ), silicofluoride (MnSiF 6 , MgSiF 6 ) and the like has been disclosed in Japanese Unexamined Patent Application (Kokai) H8-144063
- a corrosion resistance similar to or better than that of a chromate film cannot be anticipated when long term corrosion resistance tests are carried out with formed films which had been obtained with this liquid.
- the problems of the corrosion resistance of the film which is formed and the treatment of the waste surface treatment liquid remain when the aforementioned conventional non-chromate type surface treatment liquids are used.
- the non-chromate type surface treatment liquids are hardly being used at all at the present time on the surface treatment part of manufacturing lines for aluminum based metal coils and sheets and the aluminum fins for heat exchanges, where especially good corrosion resistance is required.
- the prior art does not provide any surface treatment liquid, for aluminum or aluminum alloy materials, which does not contain hexavalent chromium, which has excellent effluent treatment properties and with which a formed film which has excellent corrosion resistance and paint film adhesion properties is obtained.
- the present invention is intended to resolve the problems described above which are associated with the prior art, and in practical terms it is intended to provide a surface treatment liquid with which a film comprising specified metals can be obtained on an aluminum or aluminum alloy material surface and which can impart excellent corrosion resistance and paint film holding properties.
- a surface treatment liquid of this invention is a water-based liquid which contains from 0.01 to 50 g/l of permanganic acid and/or its salts, and from 0.01 to 20 g/l of at least one compound selected from among water soluble titanium compounds and water soluble zirconium compounds, and which has a pH of from 1.0 to 6.0.
- Permanganic acid and/or its salts can be used to introduce the acid(s) and/or salt(s) thereof into a surface treatment liquid of this invention, and no narrow limitation is imposed upon the particular type of material used.
- the total concentration of permanganic acid and salt(s) thereof must be within the range from 0.01 to 50 g/l, and preferably is within the range from 0.05 to 20 g/l.
- a formed film may be obtained even if the concentration of permanganic acid and/or salt(s) thereof is less than 0.01 g/l, but this is undesirable, because the corrosion resistance and paint film adhesion properties of any such film are poor.
- a good formed film is obtained with a concentration of more than 50 g/l, but the properties of the film are no better than with 50 g/l, the cost of the treatment liquid is increased, and this is economically wasteful.
- One type, or two or more types, of compound selected from among the sulfates, oxysulfates, acetates, ammonium salts and fluorides, for example, of titanium and zirconium can be used to introduce the water soluble titanium compound or water soluble zirconium compound into a surface treatment liquid of this invention, and no limitation is imposed on the type of compound, provided that it is water soluble. Furthermore, the amount included must be within the range from 0.01 to 20 g/l, and preferably within the range from 0.1 to 3 g/l. A formed film can be obtained even if the water soluble titanium compound or water soluble zirconium compound content is less than 0.01 g/l, but this is undesirable since the corrosion resistance of any such film is poor.
- a good formed film is obtained with more than 20 g/l, but the properties of the film are no better than with 20 g/l, the cost of the treatment liquid is increased and this is economically wasteful.
- the pH of a surface treatment liquid of this invention must be within the range from 1.0 to 6.0 and is preferably within the range from 2.0 to 5.0. Excessive etching of the metal material surface occurs at a pH less than 1.0 and irregularities arise in the appearance; this is undesirable. Furthermore, if the pH exceeds 6.0, then it may become difficult to obtain a formed film which has excellent corrosion resistance, and there are cases where problems arise with the stability of the liquid, because the metal ions which are contained in the treatment liquid are likely to form a precipitate; this is undesirable.
- Acids such as nitric acid, sulfuric acid, phosphoric acid, hydrofluoric acid and fluorosilicic acid and alkalies such as sodium hydroxide, sodium carbonate, potassium hydroxide and ammonium hydroxide can be used, as required, when adjusting the pH of a surface treatment liquid of this invention to within the range from 1.0 to 6.0.
- the stability of the treatment liquid is markedly reduced by metal ions, such as copper and/or magnesium ions, derived from the metal component which are dissolved in the surface treatment liquid, so that in this instance organic acids such as gluconic acid, heptogluconic acid, oxalic acid, tartaric acid, organophosphonic acid, ethylenediamine tetra-acetic acid and the alkali metal salts of these acids may advantageously be added as chelating agents to chelate these alloy component metals.
- metal ions such as copper and/or magnesium ions
- tungstic acid molybdic acid and their salts, and water soluble organic peroxides such as tert-butylhydroperoxide, which has the chemical formula (CH 3 ) 3 C-OOH, can be used conjointly in order to promote the formation of a film in this invention.
- water soluble organic peroxides such as tert-butylhydroperoxide, which has the chemical formula (CH 3 ) 3 C-OOH
- the formed films which are obtained by the method described above are comprised of manganese and at least one species selected from among titanium and zircon- ium as structural components, and the ratio by weight of Mn/Ti, Mr/Zr or Mn/(Ti+Zr) is preferably within the range from 0.1 to 20.0, and more preferably within the range from 0.2 to 5.0.
- the mass per unit area of the formed film of these metals independently preferably is from 5 to 500 milligrams per square centimeter of surface coated (hereinafter usually abbreviated as "mg/m 2 ").
- the manganese, tungsten and zirconium which are the structural components of a formed film of this invention are unlimited in terms of the chemical characteristics with which they are present in the film, and they may be present, for example, as the metals, oxides or phosphates.
- a surface treatment liquid of this invention is preferably used in a process sequence such as follows below:
- a surface treatment liquid of this invention is preferably brought into contact with the surface of the aluminum or aluminum alloy material at a temperature of from 20 to 80 °C for a period of from 1 to 120 seconds.
- contact temperatures below 20 °C the reactivity between the treatment liquid and the metal surface is low, so that a good formed film is not usually obtained, and if the temperature exceeds 80 °C, a formed film is obtained but the energy costs are high and this is economically wasteful.
- reaction is usually inadequate with a treatment time of less than 1 second, so that a formed film which has excellent corrosion resistance is not obtained.
- no improvement in the corrosion resistance and paint film adhesion properties of the formed film obtained have been seen if the contact time exceeds 120 seconds.
- any method of contacting the substrate being treated with the surface treatment liquid such as an immersion method or a spraying method, can be used in this invention.
- the amount of formed film deposited on the surface of an aluminum or aluminum alloy material by means of the method of this invention preferably contains from 5 to 300 mg/m 2 of manganese and from 3 to 100 mg/m 2 of titanium, zirconium, or both. If the amount of deposited manganese is less than 5 mg/m 2 , the corrosion resistance and paint film adhesion properties of the formed film obtained usually are inadequate, and if this amount exceeds 300 mg/m 2 , it is undesirable in terms of the irregularity of the appearance of the formed film which is obtained.
- the corrosion resistance of the formed film which is obtained is usually inadequate, and if the amount exceeds 100 mg/m 2 , a formed film which has excellent corrosion resistance, but one which is no better than that obtained at 100 mg/m 2 , is obtained; this is economically wasteful.
- Aluminum or aluminum alloy materials which may be surface treated by means of the method of this invention include pure aluminum and aluminum alloys, and the aluminum alloys include alloys such as Al-Cu, Al-Mn, Al-Mg and Al-Si alloys, for example. Furthermore, no limitation is imposed upon the shape or dimensions of the aluminum or aluminum alloy material with which the method of the invention is used, and the forms include sheets and various moldings, for example. Illustrative examples, which are not to be construed as limiting the invention, are described along with comparative examples below, and the effect of a surface treatment liquid of this invention is described in more detailed terms. SUBSTRATE USED IN THE TESTS
- JIS 3004 Al-Mn alloy sheet according to Japanese Industrial Standard (hereinafter usually abbreviated as "JIS") 3004 was used. Dimensions: 150 mm x 70 mm, Thickness 0.2 mm. TREATMENT CONDITIONS
- a 7 % aqueous solution of a commercial zirconium phosphate based surface treating agent (registered trade name: Arochrome® 713, manufactured by the Nihon Parkerizing Co.) was used for the forming treatment.
- the liquid was used at a 5 temperature of 40 °C for a contact time of 60 seconds by immersion, to treat the aforementioned Al-Mn based alloy sheet.
- a 3 % aqueous solution of a commercial phosphoric acid-chromate forming treatment agent (an aqueous solution of a mixture of 4 % of a product with the registered 15 trade name Alchrome® K702SL, and 0.3 % of a product with the registered trade name Alchrome® K702AC 0.3%, both manufactured by the Nihon Parkerizing Co.) was used for the surface treatment.
- the liquid was used at a temperature of 50 °C for a contact time of 20 seconds, using a spray method, to treat the same type of Al-Mn based alloy sheet as in Comparative Examples 5 and 6.
- a salt water spray test in accordance with JIS Z-2371 was used to evaluate corrosion resistance.
- the state of corrosion of the surface treated sheet after salt water spraying for 1 ,000 hours was assessed visually and is reported by using the following symbols:
- ⁇ Corroded area less than 10 %
- O Corroded area at least 10 % but less than 50 %
- ⁇ Corroded area at least 50 % but less than 90 %
- X Corroded area at least 90 %
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP13185997 | 1997-05-22 | ||
JP13185997 | 1997-05-22 | ||
PCT/US1998/009902 WO1998052699A1 (en) | 1997-05-22 | 1998-05-21 | Water-based liquid treatment for aluminum and its alloys |
Publications (2)
Publication Number | Publication Date |
---|---|
EP1017505A1 true EP1017505A1 (en) | 2000-07-12 |
EP1017505A4 EP1017505A4 (en) | 2000-08-16 |
Family
ID=15067800
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP98923440A Withdrawn EP1017505A4 (en) | 1997-05-22 | 1998-05-21 | Water-based liquid treatment for aluminum and its alloys |
Country Status (5)
Country | Link |
---|---|
EP (1) | EP1017505A4 (en) |
AU (1) | AU744557B2 (en) |
CA (1) | CA2291140A1 (en) |
WO (1) | WO1998052699A1 (en) |
ZA (1) | ZA984335B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US6485580B1 (en) | 1998-05-20 | 2002-11-26 | Henkel Corporation | Composition and process for treating surfaces or light metals and their alloys |
CA2332620A1 (en) * | 1998-05-20 | 1999-11-25 | Henkel Corporation | Composition and process for treating surfaces of light metals and their alloys |
DE10358590A1 (en) | 2003-12-12 | 2005-07-07 | Newfrey Llc, Newark | Process for the pretreatment of surfaces of welded parts of aluminum or its alloys and corresponding welded parts |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1521715A1 (en) * | 1966-12-07 | 1970-02-05 | Collardin Gmbh Gerhard | Process for the production of protective layers on zinc and galvanized surfaces |
JPS56136978A (en) * | 1980-03-26 | 1981-10-26 | Showa Alum Ind Kk | Chemically treating solution for aluminum or aluminum alloy |
JPS5741376A (en) * | 1980-08-26 | 1982-03-08 | Rasa Kogyo Kk | Surface treatment of aluminum, magnesium and their alloy |
JPH03240971A (en) * | 1990-02-16 | 1991-10-28 | Nisshin Steel Co Ltd | Blackening treatment of al, al alloy or steel sheet plated with same |
DE4031710A1 (en) * | 1990-10-06 | 1992-04-09 | Henkel Kgaa | Corrosion protection medium for aluminium@ surfaces - process for making corrosion protecting layers on aluminium |
JPH08144063A (en) * | 1994-11-22 | 1996-06-04 | Matsufumi Takatani | Surface treatment of aluminum based metallic material |
WO1997002369A1 (en) * | 1995-06-30 | 1997-01-23 | Henkel Corporation | Composition and process for treating the surface of aluminiferous metals |
US5707465A (en) * | 1996-10-24 | 1998-01-13 | Sanchem, Inc. | Low temperature corrosion resistant aluminum and aluminum coating composition |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4031817A1 (en) * | 1990-10-08 | 1992-04-09 | Henkel Kgaa | METHOD FOR PASSIVATING POST-TREATMENT OF PHOSPHATED METAL SURFACES |
WO1993005198A1 (en) * | 1991-08-30 | 1993-03-18 | Henkel Corporation | Process for treating metal with aqueous acidic composition that is substantially free from chromium (vi) |
US5449415A (en) * | 1993-07-30 | 1995-09-12 | Henkel Corporation | Composition and process for treating metals |
JP3437023B2 (en) * | 1995-11-20 | 2003-08-18 | 日本ペイント株式会社 | Aluminum-based metal surface treatment bath and treatment method |
US5759244A (en) * | 1996-10-09 | 1998-06-02 | Natural Coating Systems, Llc | Chromate-free conversion coatings for metals |
-
1998
- 1998-05-21 EP EP98923440A patent/EP1017505A4/en not_active Withdrawn
- 1998-05-21 ZA ZA984335A patent/ZA984335B/en unknown
- 1998-05-21 AU AU75734/98A patent/AU744557B2/en not_active Ceased
- 1998-05-21 CA CA002291140A patent/CA2291140A1/en not_active Abandoned
- 1998-05-21 WO PCT/US1998/009902 patent/WO1998052699A1/en not_active Application Discontinuation
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1521715A1 (en) * | 1966-12-07 | 1970-02-05 | Collardin Gmbh Gerhard | Process for the production of protective layers on zinc and galvanized surfaces |
JPS56136978A (en) * | 1980-03-26 | 1981-10-26 | Showa Alum Ind Kk | Chemically treating solution for aluminum or aluminum alloy |
JPS5741376A (en) * | 1980-08-26 | 1982-03-08 | Rasa Kogyo Kk | Surface treatment of aluminum, magnesium and their alloy |
JPH03240971A (en) * | 1990-02-16 | 1991-10-28 | Nisshin Steel Co Ltd | Blackening treatment of al, al alloy or steel sheet plated with same |
DE4031710A1 (en) * | 1990-10-06 | 1992-04-09 | Henkel Kgaa | Corrosion protection medium for aluminium@ surfaces - process for making corrosion protecting layers on aluminium |
JPH08144063A (en) * | 1994-11-22 | 1996-06-04 | Matsufumi Takatani | Surface treatment of aluminum based metallic material |
WO1997002369A1 (en) * | 1995-06-30 | 1997-01-23 | Henkel Corporation | Composition and process for treating the surface of aluminiferous metals |
US5707465A (en) * | 1996-10-24 | 1998-01-13 | Sanchem, Inc. | Low temperature corrosion resistant aluminum and aluminum coating composition |
Non-Patent Citations (5)
Title |
---|
PATENT ABSTRACTS OF JAPAN vol. 006, no. 015 (C-089), 28 January 1982 (1982-01-28) -& JP 56 136978 A (SHOWA ALUM IND KK), 26 October 1981 (1981-10-26) * |
PATENT ABSTRACTS OF JAPAN vol. 006, no. 114 (C-110), 25 June 1982 (1982-06-25) -& JP 57 041376 A (RASA KOGYO KK), 8 March 1982 (1982-03-08) * |
PATENT ABSTRACTS OF JAPAN vol. 016, no. 029 (C-0904), 24 January 1992 (1992-01-24) -& JP 03 240971 A (NISSHIN STEEL CO LTD), 28 October 1991 (1991-10-28) * |
PATENT ABSTRACTS OF JAPAN vol. 1996, no. 10, 31 October 1996 (1996-10-31) & JP 08 144063 A (TAKATANI MATSUFUMI), 4 June 1996 (1996-06-04) * |
See also references of WO9852699A1 * |
Also Published As
Publication number | Publication date |
---|---|
AU744557B2 (en) | 2002-02-28 |
EP1017505A4 (en) | 2000-08-16 |
WO1998052699A1 (en) | 1998-11-26 |
ZA984335B (en) | 1998-11-30 |
AU7573498A (en) | 1998-12-11 |
CA2291140A1 (en) | 1998-11-26 |
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