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EP0902849A1 - Scellement thermique rapide de surfaces metalliques anodisees realise au moyen de solutions contenant des tensioactifs - Google Patents

Scellement thermique rapide de surfaces metalliques anodisees realise au moyen de solutions contenant des tensioactifs

Info

Publication number
EP0902849A1
EP0902849A1 EP97923978A EP97923978A EP0902849A1 EP 0902849 A1 EP0902849 A1 EP 0902849A1 EP 97923978 A EP97923978 A EP 97923978A EP 97923978 A EP97923978 A EP 97923978A EP 0902849 A1 EP0902849 A1 EP 0902849A1
Authority
EP
European Patent Office
Prior art keywords
acids
acid
aqueous solution
group
total
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.)
Granted
Application number
EP97923978A
Other languages
German (de)
English (en)
Other versions
EP0902849B1 (fr
Inventor
Torsten Körner
Josef Kresse
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Henkel AG and Co KGaA filed Critical Henkel AG and Co KGaA
Publication of EP0902849A1 publication Critical patent/EP0902849A1/fr
Application granted granted Critical
Publication of EP0902849B1 publication Critical patent/EP0902849B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/18—After-treatment, e.g. pore-sealing
    • C25D11/24—Chemical after-treatment
    • C25D11/246—Chemical after-treatment for sealing layers

Definitions

  • the invention is in the field of producing anti-corrosion and / or decorative coatings on metals by anodic oxidation. It relates to an improved method for compacting the electrochemically produced porous anodizing layers in order to further improve their properties.
  • the electrochemical anodic oxidation of metals in suitable electrolytes is a widespread process for the formation of anti-corrosion and / or decorative coatings on suitable metals. These processes are described, for example, in Ulimann's Encyclopedia of Industrial Chemistry, 5th Edition, Vol. 9 (1987), p. 174 - 176 briefly characterized Accordingly, titanium, magnesium and aluminum as well as their alloys can be anodized, whereby the anodization of aluminum and its alloys is technically of greatest importance.
  • the electrolytically produced anodizing layers protect the aluminum surfaces from the effects of the weather and other corrosive media. Anodizing layers are also applied in order to obtain a harder surface and thus to achieve increased wear resistance of the aluminum.
  • the aluminum is anodized in an acidic electrolyte, with sulfuric acid being the most widespread.
  • Other suitable electrolytes are phosphoric acid, oxalic acid and chromic acid.
  • the properties of the anodizing layers can be varied within wide limits by the choice of the electrolyte, its temperature, the current density and the anodizing time.
  • the anodization is usually carried out with direct current or with an alternating current superimposed direct current
  • the fresh anodizing layers can be subsequently colored by dipping in solutions of a suitable dye or by an alternating current treatment in a metal salt-containing, preferably in a tin-containing, electrolyte.
  • colored anodizing layers can be obtained by so-called color anodizing processes, for which anodizing in solutions of organic acids, such as in particular sulfophthalic acid or sulfanilic acid, optionally in each case in a mixture with sulfuric acid, is used.
  • organic acids such as in particular sulfophthalic acid or sulfanilic acid, optionally in each case in a mixture with sulfuric acid, is used.
  • sealing covering which consists of hydrated aluminum oxide, is visually disturbing, reduces the adhesive strength when such aluminum parts are bonded and requires later contamination and corrosion. Since the subsequent removal of this sealing covering by hand by mechanical or chemical means is attempted to prevent the formation of this sea covering by chemical additives to the sealing bath According to DEC-26 50 989, additions of cyclic polycarboxylic acids with 4 to 6 carboxyl groups in the molecule, in particular cyclohexane hexacarboxylic acid, are suitable for this purpose.
  • DE-A-38 20 650 certain phosphonic acids can also be used Use, for example, 1-phosphonopropane1, 2,3-t ⁇ carbonsaure
  • EP-A-122 129 discloses the use of further phosphonic acids.
  • DE-C-22 11 553 describes a process for compacting anodic oxide layers on aluminum and aluminum alloys in aqueous , Phosphonic acids or their salts and solutions containing calcium ions, the molar ratio of calcium ions to phosphonic acid being set to at least 2 1. A higher ratio of calcium ions to phosphonic acids of about 5 1 to about 500 1 is preferably used.
  • Phosphonic acids which can be used are, for example, 1-hydroxypropane, 1-hydroxybutane, 1-hydroxypentane, 1-hydroxyhexane1, 1-diphosphonic acid and 1-hydroxy-1-phenylmethane-1, 1-diphosphonic acid and preferably 1-hydroxyethane-1, 1-diphosphonic acid, 1-aminoethane, 1- Am ⁇ no-1-phenylmethane, dimethylaminoethane, dimethylaminobutane,
  • the compression time is therefore approximately 3 minutes per ⁇ m layer thickness
  • high temperatures at least 90 ° C.
  • relatively long treatment times in the order of about 1 hour with an anodizing layer of about 20 ⁇ m have hitherto been used for effective compaction required.
  • the compaction process is therefore very energy-intensive and, because of its duration, can be a bottleneck for the production speed.Therefore, additives for the compaction bath were already being sought which support the compaction process so that it works at lower temperatures (so-called Cold compression or cold sealing) and / or takes place with shorter treatment times.
  • nickel salts in particular fluorides
  • it was recommended to make the oxide layer hydrophobic by means of long-chain carboxylic acids or waxes, as well as treatment with acrylamides, which are to be polymerized in the pore space for this purpose the above-mentioned literature by S Wernick et al can be found. With the exception of densification with nickel compounds, these proposals have not been successful in practice
  • a short-term hot compression process is known from US Pat. No. 5,411,607, in which the anodized metal parts are immersed in a lithium-containing aqueous solution.
  • the lithium concentration is preferably in the range from 0.01 to 50 g / l and in particular in the range from 0.01 to 5 g / l.
  • the compaction solution additionally contain a sealant preventing agent.
  • This is preferably present in a concentration between 0.1 and 10 g / l and is preferably an aromatic disulfonate.
  • a short-term hot compaction can be carried out with an aqueous solution which contains at least 0.01 g / l of lithium ions and from 0.1 to 10 g / l of a sealing deposit inhibitor.
  • the sealing deposit inhibitor is preferably an aromatic disulfonate.
  • German patent application 195 38 777.5 discloses a short-term hot compression process in which the anodized metal parts are brought into contact with an anodizing solution which contains a total of 0.1 to 5 g / l of one or more alkali metal and / or alkaline earth metal ions and a total of 0.1 Contains 0005 to 0.2 g / l of a sealing deposit inhibitor in the form of phosphonic acids or cyclic polycarboxylic acids.
  • the teaching of the last three documents enables a significant reduction in hot compression times. Nevertheless, there is a need for short-term compaction processes with improved compaction results.
  • the object of the invention is to provide such a method.
  • the invention relates to a method for compacting anodized metal surfaces, characterized in that the anodized metal is brought into contact with an aqueous solution at a temperature between 75 ° C. and the boiling point for a period of between 0.5 and 2 minutes per micrometer of anodizing layer thickness and has a pH in the range of 5.5 to 8.5 and the a) a total of 0.0004 to 0.05 g / l, preferably 0.005 to 0.02 g / l, of one or more cationic, anionic or nonionic surfactants and
  • the treatment solutions can be brought into contact with the anodized metals by spraying the solutions onto the metal surfaces or preferably by immersing the metal parts in the solutions.
  • the required treatment times are only in the range from 20 to 40 minutes.
  • the temperature of the treatment solution is preferably in the range from 94 to 98 ° C., for example 96 ° C.
  • the pH of the aqueous solution is preferably in the range 5.5 to 7, in particular in the range 5.5 to 6.5. If necessary, the pH can be adjusted with ammonia or with acetic acid. With ammonium acetate as a buffer, it can be kept in the required range.
  • Cationic surfactants of group a) can be selected, for example, from quaternary ammonium salts in which at least one alkyl or arylalkyl radical has at least 8 carbon atoms.
  • An example is C 12 . ⁇ 4 - alkyl dimethyl benzyl ammonium.
  • Pyridinium salts such as dodecylpyridinium chloride can also be used as cationic surfactants.
  • Examples of usable anionic surfactants from group a) are alkyl or alkylaryl sulfates and sulfonates. Linear alkyl sulfates such as lauryl sulfate are preferred for environmental reasons.
  • the anionic surfactants can be used as alkali or ammonium salts, with lithium salts being particularly preferred.
  • nonionic surfactants are preferably used as the surfactants of group a). These can be selected, for example, from alkoxylates such as, for example, ethoxylates and / or propoxylates of fatty alcohols or fatty amines.
  • alkoxylates such as, for example, ethoxylates and / or propoxylates of fatty alcohols or fatty amines.
  • fatty alcohols and fatty amines are understood as meaning compounds with an alkyl radical having at least 8 carbon atoms can consist of pure substances with a defined alkyl radical or of product mixtures as obtained from natural fats and oils.
  • the alkoxylates can also be end group-capped, ie etherified again at the terminal OH group.
  • the nonionic surfactants of group a) are therefore preferably selected from fatty amine ethoxylates at 10 to 18 ° C. -Atoms in the alkyl radical and with 3 to 15 ethylene oxide units in the molecule. Specific examples are coconut fatty amine x 5 EO and coconut fatty amine x 12 EO
  • the organic acids of group b) are selected from saturated, unsaturated or aromatic carbocyclic hexagonal carboxylic acids with 3 to 6 carboxyl groups.
  • Preferred examples of such acids are trimesic acid, t ⁇ mellitic acid, pyromellitic acid, mellitic acid and the particularly preferred cyclohexane hexacarboxylic acid is the total amount preferably in the range 0.001 to 0.05 g / l
  • the preferred cyclohexane hexacarboxylic acid exists in the form of different stereoisomers. As is known from DE-A-26 50 989, preference is given to those cyclohexane hexacarboxylic acids which carry 5 cis and 1 trans or the 4 cis and 2 trans carboxyl groups S
  • the organic acids of group b) are selected from the phosphonic acids 1-phosphonopropane-1, 2,3-t ⁇ carbonsaure, 1, 1-diphosphonopropane-2,3-dicarboxylic acid, 1-hydroxypropane-1, 1-diphosphonic acid , 1 -hydroxybutane-1, 1 -diphosphonic acid, 1 -hydroxy-1 - phenylmethane-1, 1 -diphosphonic acid, 1 -hydroxyethane-1, 1 -diphosphonic acid, 1 - aminoethane-1, 1 -diphosphonic acid, 1 -amino-1 -phenylmethane-1, 1-diphosphonic acid, dimethylamino-ethane-1, 1 diphosphonic acid, propylaminoethane-1,1-diphosphonic acid, butylamine-ethane-1,1-diphosphonic acid,
  • Aminotron methylenephosphonic acid
  • ethylenediamototetra methylenephosphonic acid
  • the aqueous compression solution additionally contains a total of 0.0001 to 5 g / l of one or more alkali metal and / or alkaline earth metal ions.
  • These alkali metal or alkaline earth metal ions can be present as counterions of the acids of group b).
  • the aqueous solution contains a larger amount of alkali metal and / or alkaline earth metal ions than is required for complete neutralization of the acids of group b).
  • these additional alkali metal and / or alkaline earth metal ions, which go beyond the amount required for the complete neutralization of the acids of group b), are selected from lithium and magnesium.
  • the content can the aqueous solution of these alkali metal and / or alkaline earth metal ions as a rule maximum 0.005 g / l can be limited. However, higher contents, for example up to 5 g / l, do not lead to deteriorated compaction results.
  • These alkali metal and / or alkaline earth metal ions such as in particular lithium and magnesium, can be used in the form of their salts which are water-soluble in the concentration range mentioned.
  • the anionic surfactants of group a) can be used as counterions.
  • Acetates, lactates, sulfates, oxalates and / or nitrates are also suitable. Acetates are particularly suitable
  • the compression bath suitable for the compression process according to the invention can in principle be prepared on site by dissolving the constituents in - preferably fully deionized - water in the required concentration range.
  • an aqueous concentrate is preferably used for the preparation of the compression baths, which already contains all the necessary components of the compression bath in the correct proportions contains and from which the ready-to-use solution is obtained by dilution with water, for example by a factor of between about 100 and about 1000.
  • the pH may have to be adjusted to the range according to the invention with ammonia or with acetic acid.
  • the invention accordingly also comprises an aqueous concentrate for the preparation of the aqueous solution for use in the short-term hot compression process according to the invention, the concentrate yielding the ready-to-use aqueous solution by dilution with water by a factor between about 100 and about 1000.
  • the accelerated and energy-saving method according to the invention makes it possible to produce compacted anodizing layers which are not inferior in their layer properties to those conventionally produced.
  • test parameters for the layer quality are of particular importance the acid removal in chromic acid, the apparent conductance as well as the color drop test.
  • the compression method according to the invention is preferably used for anodized aluminum or anodized aluminum alloys. However, it can also be applied to the anodizing layers of other anodizable metals such as titanium and magnesium or their alloys in each case. It can be used both for uncolored anodizing layers and for those based on conventional ones Processes such as, for example, integral coloring, adsorptive coloring using organic dyes, reactive coloring with the formation of inorganic color pigments, electrochemical coloring using metal salts, in particular tin salts, or interference coloring, the process according to the invention has the further advantage that adsorptively colored anodizing layers that the possible bleeding out of the dye in conventional hot compression can be reduced by the shortened compression time
  • Aluminum plates of the type AI 99 5 were conventionally anodized (direct current / sulfuric acid, one hour, layer thickness 20 ⁇ m) and, if necessary, colored electrochemically or with organic dipping paints.Then the plates were immersed for 30 minutes in the compression solutions according to the invention or comparison solutions according to the table g concentrate with demineralized water made up to 1 liter. The solutions had a temperature of 96 ° C. Following the treatment according to the table, the metal sheets were immersed in boiling demineralized water for one minute and then dried Practical quality tests checked The results are also contained in the table. They show that with the The method according to the invention can be obtained after only 30 minutes of compression results, which experience has shown that it can only be obtained after one hour with a conventional hot compression bath. In contrast, the compaction results after half an hour of treatment with comparative solutions are qualitatively inadequate.
  • the admittance Y 2 Q was determined according to the German standard DIN 50949 with a
  • Measuring device Anotest YD 8.1 from Fischer determined.
  • the measuring system consists of two electrodes, one of which is conductively connected to the base material of the sample.
  • the second electrode is immersed in an electrolyte cell that can be placed on the layer to be examined.
  • This cell is designed as a rubber ring with an inner diameter of 13 mm and a thickness of approximately 5 mm, the ring surface of which is self-adhesive.
  • the measuring area is 1.33 cm 2 .
  • a potassium sulfate solution (35 g / l) in deionized water is used as the electrolyte.
  • the apparent conductance readable on the measuring device is converted to a measuring temperature of 25 ° C and a layer thickness of 20 ⁇ m in accordance with the specifications of DIN 50949.
  • the values obtained, which should preferably be in the range between approximately 10 and approximately 20 ⁇ S, are entered in the table.
  • the " residual reflection after dyeing with dye was measured in accordance with the German standard DIN 50946 as a parameter which indicates open-pore and thus poorly compressed layers.
  • the measuring area was delimited with the aid of a self-adhesive measuring cell of the Anotest device described above.
  • the test area is wetted with an acid solution (25 ml / l sulfuric acid, 10 g / l KF). After exactly one minute the acid solution is washed off and the test area is dried.
  • the test area is then wetted with dye solution (5 g / l sanodal blue), which is left for one minute After rinsing under running water, the measuring cell is removed.
  • the stained test area is freed of loosely adhering dye by rubbing with a mild powder cleaner.
  • a relative reflection measurement is carried out by the measuring head of a light reflection.
  • Measuring device Micro Color from Dr. Lange
  • the residual reflection in% is obtained by dividing the quotient from the measurement value of the colored area divided by the measurement value of the uncolored area by hundreds. Residual reflection values between 95 and 100% are evidence of good compression quality, while values below 95% are considered unacceptable The higher the values of the residual reflection, the higher the compression quality. The values found are entered in the table
  • the acid removal was measured in accordance with ISO 3210.
  • the test plate is weighed to the nearest 0.1 mg and then immersed in an acid solution for 15 minutes at 38 ° C, which contains 35 ml of 85% phosphoric acid and 20 g of chromium per liter ( VI) contains ox ⁇ d
  • the sample is rinsed with deionized water and dried in a drying cabinet for 15 minutes at 60 ° C.
  • the sample is then weighed again.
  • the weight difference between the first and the second measurement is calculated and divided by the size the surface in dm 2
  • Example 1 as in comparison 1, additionally 10 g / l coconut paste x 5 EO
  • Example 6 as in comparison 1, additionally:
  • Example 7 additionally: 2 g / l cocosamine x 5 EO
  • Example 8 as cf. 1, additionally: 15 g / l cocosamine x 5 EO

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Gasket Seals (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Paints Or Removers (AREA)

Abstract

L'invention concerne un procédé de scellement de surfaces métalliques anodisées, caractérisé en ce que le métal anodisé est mis en contact, pendant une période comprise entre 0,5 et 2 minutes par micromètre d'épaisseur de couche anodisée, avec une solution aqueuse présentant une température comprise entre 75 °C et le point d'ébullition, ainsi qu'un pH compris dans la plage 5,5 à 8,5, et contenant: a) un total de 0,0004 à 0,05 g/l d'un ou de plusieurs tensioactifs cationiques, anioniques ou non ioniques; et b) un total de 0,0005 à 0,5 g/l d'un ou de plusieurs acides organiques choisis dans le groupe comprenant les acides polycarboxyliques cycliques possèdant 3 à 6 groupes carboxyle et les acides phosphoniques. Les tensioactifs préférés sont les tensioactifs non ioniques et les acides préférés sont les acides polyphosphinocarboxyliques. Ladite solution peut éventuellement contenir des cations de métaux alcalins et/ou alcalino-terreux, de préférence des ions Li et/ou Mg, dans des quantités allant de 0,0001 à 5 g/l.
EP97923978A 1996-05-31 1997-05-22 Scellement thermique rapide de surfaces metalliques anodisees realise au moyen de solutions contenant des tensioactifs Expired - Lifetime EP0902849B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19621818A DE19621818A1 (de) 1996-05-31 1996-05-31 Kurzzeit-Heißverdichtung anodisierter Metalloberflächen mit tensidhaltigen Lösungen
DE19621818 1996-05-31
PCT/EP1997/002620 WO1997046738A1 (fr) 1996-05-31 1997-05-22 Scellement thermique rapide de surfaces metalliques anodisees realise au moyen de solutions contenant des tensioactifs

Publications (2)

Publication Number Publication Date
EP0902849A1 true EP0902849A1 (fr) 1999-03-24
EP0902849B1 EP0902849B1 (fr) 2000-08-09

Family

ID=7795743

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97923978A Expired - Lifetime EP0902849B1 (fr) 1996-05-31 1997-05-22 Scellement thermique rapide de surfaces metalliques anodisees realise au moyen de solutions contenant des tensioactifs

Country Status (15)

Country Link
US (1) US6059897A (fr)
EP (1) EP0902849B1 (fr)
JP (1) JP2000511972A (fr)
KR (1) KR20000016130A (fr)
CN (1) CN1219984A (fr)
AR (1) AR007357A1 (fr)
AT (1) ATE195356T1 (fr)
AU (1) AU719630B2 (fr)
CA (1) CA2257253A1 (fr)
DE (2) DE19621818A1 (fr)
ES (1) ES2150250T3 (fr)
PL (1) PL330016A1 (fr)
TR (1) TR199802338T2 (fr)
WO (1) WO1997046738A1 (fr)
ZA (1) ZA974742B (fr)

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US10920332B2 (en) 2015-01-19 2021-02-16 Council Of Scientific And Industrial Research Process for the preparation of corrosion resistance sealed anodized coatings on aluminum alloy
CN106191959A (zh) * 2015-05-08 2016-12-07 广州市汉科建材科技有限公司 一种环保型铝合金封孔剂
HK1258691A1 (zh) * 2016-03-28 2019-11-15 奥野制药工业株式会社 铝合金的阳极氧化覆膜用封孔处理液、浓缩液和封孔处理方法
US10138566B2 (en) * 2017-01-13 2018-11-27 Macdermid Acumen, Inc. Sealing anodized aluminum using a low-temperature nickel-free process
PL424520A1 (pl) * 2018-02-06 2019-08-12 Cim-Mes Projekt Spółka Z Ograniczoną Odpowiedzialnością Sposób formowania warstwy powierzchniowej aluminium
DE102019101449A1 (de) 2019-01-21 2020-07-23 Carl Freudenberg Kg Oberflächenbehandlung von eloxiertem Aluminium
KR102365724B1 (ko) * 2020-10-16 2022-02-23 주식회사 영광와이케이엠씨 황산 아노다이징 처리된 알루미늄 합금용 봉공처리액 및 이를 이용한 황산 아노다이징 처리된 알루미늄 합금의 고내식성 봉공처리방법
KR102467268B1 (ko) * 2020-10-29 2022-11-17 주식회사 영광와이케이엠씨 옥살산 전해액에서 전류밀도 변화에 따른 아노다이징 처리 방법

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Also Published As

Publication number Publication date
CN1219984A (zh) 1999-06-16
WO1997046738A1 (fr) 1997-12-11
AU2959897A (en) 1998-01-05
ES2150250T3 (es) 2000-11-16
KR20000016130A (ko) 2000-03-25
ZA974742B (en) 1997-12-01
PL330016A1 (en) 1999-04-26
JP2000511972A (ja) 2000-09-12
AU719630B2 (en) 2000-05-11
DE19621818A1 (de) 1997-12-04
EP0902849B1 (fr) 2000-08-09
DE59702148D1 (de) 2000-09-14
ATE195356T1 (de) 2000-08-15
US6059897A (en) 2000-05-09
CA2257253A1 (fr) 1997-12-11
TR199802338T2 (xx) 1999-02-22
AR007357A1 (es) 1999-10-27

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