EP2358922A1 - Couches de conversion pour surfaces contenant du zinc - Google Patents

Couches de conversion pour surfaces contenant du zinc

Info

Publication number
EP2358922A1
EP2358922A1 EP09760833A EP09760833A EP2358922A1 EP 2358922 A1 EP2358922 A1 EP 2358922A1 EP 09760833 A EP09760833 A EP 09760833A EP 09760833 A EP09760833 A EP 09760833A EP 2358922 A1 EP2358922 A1 EP 2358922A1
Authority
EP
European Patent Office
Prior art keywords
acid
treatment solution
group
solution according
aqueous treatment
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
EP09760833A
Other languages
German (de)
English (en)
Other versions
EP2358922B1 (fr
Inventor
Björn Dingwerth
Andreas Noack
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.)
Atotech Deutschland GmbH and Co KG
Original Assignee
Atotech Deutschland GmbH and Co KG
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 Atotech Deutschland GmbH and Co KG filed Critical Atotech Deutschland GmbH and Co KG
Priority to PL09760833T priority Critical patent/PL2358922T3/pl
Publication of EP2358922A1 publication Critical patent/EP2358922A1/fr
Application granted granted Critical
Publication of EP2358922B1 publication Critical patent/EP2358922B1/fr
Not-in-force legal-status Critical Current
Anticipated expiration legal-status Critical

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
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/08—Orthophosphates
    • C23C22/12—Orthophosphates containing zinc cations
    • C23C22/17—Orthophosphates containing zinc cations containing also organic acids
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/08—Orthophosphates
    • C23C22/10—Orthophosphates containing oxidants
    • 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
    • C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
    • C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
    • 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

Definitions

  • the invention relates to the corrosion protection of metallic materials, in particular of those which are provided with a conversion layer.
  • the coating of the metallic workpiece to be protected with a coating of another metal is a widely used and established method in the art.
  • the coating metal can behave in the corrosive medium either electrochemically nobler or less noble than the material base metal alone. If the coating metal behaves less noble, it acts as a sacrificial anode in the corrosive medium in the sense of cathodic protection against the base metal. Although this is associated with the formation of corrosion products of the coating metal protection function is indeed desirable, but the corrosion products of the coating often lead even to undesirable decorative and often to functional impairments of the workpiece.
  • so-called conversion layers are often used especially on cathodically protective base coating metals such as zinc and its alloys. These are reaction products of the base metal which are insoluble in aqueous media over a wide pH range with the reaction solution.
  • conversion layers are, for example, so-called phosphating and chromating.
  • phosphating the layer to be protected is dipped in an acidic solution containing phosphate ions.
  • the acidic medium leads to the partial dissolution of zinc from the coating.
  • the liberated Zn 2+ cations form a sparingly soluble zinc phosphate layer on the surface with the phosphate ions of the reaction solution. Since zinc phosphate coatings themselves form only a comparatively bad corrosion protection, but an excellent primer for this On applied paints and paints, their main application is in the function of a primer for coatings and paints.
  • the surface to be treated is dipped in an acidic solution containing chromium (VI) ions.
  • chromium (VI) ions For example, if it is a zinc surface, some of the zinc will dissolve.
  • chromium (VI) is reduced to chromium (III), which in the hydrogenation more alkaline surface film i.a. as chromium (III) - hydroxide or as sparingly soluble ⁇ -oxo or ⁇ -hydroxo-bridged chromium (III) - complex is deposited.
  • sparingly soluble zinc chromate (VI) is formed. Overall, a tightly closed, very well protects against corrosion attack by electrolytes conversion coating on the zinc surface.
  • chromium (VI) compounds are distinguished by their high carcinogenic potential, so that it is necessary to replace the processes associated with these compounds.
  • chromating processes with hexavalent chromium compounds a large number of processes have now been established which use different complexes of trivalent chromium compounds.
  • a decisive step in the course of the deposition is a reaction by which the pH at the interface of the zinc surface or zinc-containing surface to the solution increases to such an extent that the deposition of the conversion layer takes place.
  • Chromium (III) is not suitable in the sense described above as an oxidizing agent for zinc. Reduction to chromium (II) is possible due to redox potential, but does not increase the pH at the interface. It is therefore necessary, in order to build up a conversion layer from an aqueous acidic solution of chromium (III) ions, to additionally add a suitable oxidizing agent which increases the concentration of zinc ions as well as the pH at the zinc or zinc alloy interface in that the components of the conversion layer which are soluble in the inside of the solution in solution on the metal surface are converted into a sparingly soluble hydrolysis form.
  • Nitrate is first reduced to nitrite under the usual reaction conditions of the treatment solutions.
  • nitrite is in the acidic medium of the treatment solutions, the pH is usually between pH 1 and pH 3.5, not stable but tends to disproportionation in nitrate and nitrogen monoxide:
  • Nitrogen oxides are toxic gases and must be extracted by suction above the surface of the solution.
  • Patent EP 1 816 234 A1 describes an aqueous reaction solution and a process for the passivation of zinc and zinc alloys.
  • the reaction solutions contain nicotinic acid, its salts or their derivatives. From such reaction solutions, colored passivation layers are produced on zinc and zinc alloys. Nicotinic acid is not suitable as an oxidizing agent in chromium (III) -containing treatment solutions for producing conversion coatings on zinc-containing surfaces.
  • the patents EP 1 005 578 B1 and GB 715,607 describe processes for the production of phosphating layers.
  • the accelerators used here are organic nitro compounds and organic N-oxides.
  • the phosphating layers described here are porous and therefore offer no corrosion protection.
  • organic oxidizing agents of the invention selected from aliphatic nitro compounds, aromatic nitro compounds, N-oxides and quinones. Substitution of nitrates by water-soluble, organic oxidants does not result in gaseous, toxic reaction products.
  • nitrate ions can be present in the solution without the negative properties being problematic.
  • the solution does not contain nitrate.
  • an aqueous treatment solution for producing substantially chromium (VI) -free black conversion layers on zinc or zinc alloy layers which contains, inter alia, the following components:
  • R 1 to R 5 are independent of one another
  • Preferred organic compounds are selected from the group consisting of compounds according to formulas I, III, IV and V where R 1 to R 5 are independently of one another
  • Particularly preferred organic compounds are selected from the group consisting of compounds of the formula I., wherein R 1 to R 5 independently
  • Suitable classes of compounds are e.g. Nitrobenzoic acids, nitrosalicylic acids, nitrophenols, dinitrophenols, trinitrophenols, nitropropionic acid, pyridine-N-oxides, morpholine-N-oxides and benzoquinones.
  • Suitable compounds in the meaning of the invention are therefore, e.g. m-nitrobenzoic acid, 2-hydroxy-5-nitrobenzoic acid, 3,5-dinitrosalicylic acid, 2,4-dinitrophenol, m-nitrobenzenesulfonic acid, N-methylmorpholine N-oxide, pyridine N-oxide and p-benzoquinone.
  • Equation 1 Examples of reduction reactions of suitable organic oxidants in an acidic medium.
  • Another advantage of the components of the invention is that they have no free nitrate and thus can be used in solutions for the production of conversion layers containing dyes with amino groups.
  • the disadvantage of the use of nitrate ions known in the art for producing the conversion layer is that the nitrate is reduced to nitrite. This nitrite can undergo diazotization reactions in the strongly acidic solution to form the conversion layer with amino-containing dyes, which react to Undefined dye products, which no longer give the desired surface color of the conversion layer. Such reactions go organically bound NO groups according to the formulas I. - III. not a.
  • Aqueous treatment solutions according to the invention contain between 0.2 g / l and 20 g / l chromium (III), preferably between 0.5 g / l and 15 g / l chromium (III) ions and more preferably between 1 g / l and 5 g / l chromium (III) ions.
  • no Cr (VI) salts are added to the solution.
  • Suitable anions are methanesulfonate, sulfate, hydrogensulfate, borates and the anions of acidic boric esters, phosphate, hydrogenphosphate, dihydrogenphosphate, nitrate, nitrite, chloride, iodide, fluoride, hexafluorosilicate, hexafluorotitanate, tetrafluoroborate, hexafluoroantimonate, hexafluorophosphate, phosphate, Hydrogen phosphate, dihydrogen phosphate or corresponding anions of esters of phosphoric acid.
  • Chromium (III) may be added to the solutions either in the form of a chromium (III) salt such as basic chromium (III) sulfate, chromium (III) hydroxide, chromium (III) dihydrogen phosphate, chromium (III) chlorite, potassium chromium ( III) sulfate or chromium (III) salts of organic acids such as chromium (III) methanesulfonate, chromium (III) citrate.
  • a chromium (III) salt such as basic chromium (III) sulfate, chromium (III) hydroxide, chromium (III) dihydrogen phosphate, chromium (III) chlorite, potassium chromium ( III) sulfate or chromium (III) salts of organic acids such as chromium (III) methanesulfonate, chromium (III) citrate.
  • complexing agents can be used, such as, for example, polycarboxylic acids, hydroxycarboxylic acids, hydroxypolycarboxylic acids, aminocarboxylic acids or hydroxyphosphonic acids.
  • carboxylic acids are oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, sebacic acid, maleic acid, phthalic acid, terephthalic acid, tartaric acid, citric acid, malic acid, ascorbic acid, ethylenedinithlotetraacetic acid, tetrahydrofuran-2-carboxylic acid, maleic acid , Ethylenediaminetetraacetic acid, diethylenediaminopentaacetic acid, nithlotriacetic acid, lactic acid, adipic acid, 4-aminohippuric acid, 4-aminobenzoic acid, 5-aminoisophthalic acid, L-aspartic acid, L
  • Dihydroxybenzoic acid 4- (dimethylamino) benzoic acid, glucuronic acid, citrazinic acid, indole-3-carboxylic acid, indole-5-carboxylic acid, butane-1, 2,3,4-tetracarboxylic acid, DL-leucine, 2,2-bis- (hydroxymethyl) propionic acid, quinoline-2,4-dicarboxylic acid, 2-aminopyridine-3-carboxylic acid, 5-amino-2-hydroxybenzoic acid, anthranilic acid, benzene-1, 2,4-tricarboxylic acid, 3,5-diaminobenzoic acid, 4,8-dihydroxyquinoline-2-carboxylic acid, 3,3-dimethylglutaric acid, trans, trans-2,4-haxadienoic acid, 3-hydroxybutyric acid, o-hydroxyhippuric acid, (4-hydroxyphenyl) -acetic acid, imidazole-4-acrylic acid, indole
  • the concentration of complexing agents in The treatment solutions may be between 0.05 g / l and the solubility limit of the complexing agents.
  • the treatment solutions may further comprise one or more surfactants such as e.g. Oxo alcohol ethoxylates (eg Lugalvan ON110, BASF), fatty alcohol ethoxylates (eg Ethylan CPG 660, Julius Hoesch GmbH), or surfactants with fluorinated radicals (eg Novec FC-4432, 3M) and between 0.01 g / l and 10 g / l another metal ion or metalloidion such as Sc, Y, Ti, Zr, Mo, W, Mn, Fe, Co, Ni, Zn, B, Al, Si, P.
  • surfactants such as e.g. Oxo alcohol ethoxylates (eg Lugalvan ON110, BASF), fatty alcohol ethoxylates (eg Ethylan CPG 660, Julius Hoesch GmbH), or surfactants with fluorinated radicals (eg Novec FC-4432, 3M) and between 0.01 g / l and
  • An aqueous treatment solution is prepared which contains 3.0 g / l Cr 3+ (from chromium (III) chloride hexahydrate), 2 g / l Co 2+ (from cobalt sulfate heptahydrate) and 8 g / l PO 4 3 " (from ortho Phosphoric acid) and 2.5 g / l Fe 2+ (from iron (III) sulfate heptahydrate) and a compound according to the invention or nitrate according to the comparative example according to Table 1.
  • the treatment solution is adjusted to a pH of 1.6 with nitric acid / sodium hydroxide
  • nitric acid / sodium hydroxide In an alkaline galvanizing process (Protolux 3000, Atotech Deutschland GmbH), a sheet of low-alloy steel is coated with 10 ⁇ m zinc
  • the sheet is activated in 0.3% by weight nitric acid for 10 s, washed three times with demineralized water and left for 60 s immersed in the above-described treatment solution. the solution is stirred in this case. After removal of the plate, this is rinsed three times with demin. water at 80 0 C for 10 min in a circulating air oven.
  • the black sheet is in the neutral salt spray according to DIN EN ISO 9227 after 6 h initial approaches to zinc corrosion.
  • a analogously prepared sheet is treated with an organic-silicate sealant (eg Corrosil Plus 501, Atotech Germany GmbH) and dried in a circulating air oven at 80 0 C for 10 min.
  • the sheet is tested in the neutral salt spray test according to DIN EN ISO 9227. The time in h, until the first signs of zinc corrosion are visible, is shown in Table 1.
  • Table 1 Experiments with conversion coatings

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Chemical Treatment Of Metals (AREA)

Abstract

L'invention concerne un procédé de production d'une couche de revêtement anticorrosion, procédé selon lequel une surface à traiter est mise en contact avec une solution de traitement aqueuse qui renferme, en plus d'au moins une source d'ions chrome(III), au moins un composé organique qui agit, vis-à-vis du zinc, comme agent oxydant, dans une solution acide ou faiblement acide. On obtient ainsi, ou on améliore, les propriétés décoratives et fonctionnelles des surfaces. En outre, on évite les inconvénients connus lors de l'utilisation de composés renfermant du chrome(VI).
EP09760833.5A 2008-11-27 2009-11-23 Couches de conversion pour surfaces contenant du zinc Not-in-force EP2358922B1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL09760833T PL2358922T3 (pl) 2008-11-27 2009-11-23 Powłoki konwersyjne dla powierzchni zawierających cynk

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102008044143A DE102008044143B4 (de) 2008-11-27 2008-11-27 Wässrige Behandlungslösung und Verfahren zur Erzeugung von Konversionsschichten für zinkhaltige Oberflächen
PCT/EP2009/065646 WO2010060883A1 (fr) 2008-11-27 2009-11-23 Couches de conversion pour surfaces contenant du zinc

Publications (2)

Publication Number Publication Date
EP2358922A1 true EP2358922A1 (fr) 2011-08-24
EP2358922B1 EP2358922B1 (fr) 2016-01-27

Family

ID=41479326

Family Applications (1)

Application Number Title Priority Date Filing Date
EP09760833.5A Not-in-force EP2358922B1 (fr) 2008-11-27 2009-11-23 Couches de conversion pour surfaces contenant du zinc

Country Status (9)

Country Link
US (1) US20110217476A1 (fr)
EP (1) EP2358922B1 (fr)
JP (1) JP5562347B2 (fr)
KR (1) KR20110089304A (fr)
CN (1) CN102227516B (fr)
DE (1) DE102008044143B4 (fr)
ES (1) ES2565839T3 (fr)
PL (1) PL2358922T3 (fr)
WO (1) WO2010060883A1 (fr)

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US9499700B2 (en) * 2010-09-14 2016-11-22 Yuken Industry Co., Ltd. Finishing agent for chemical conversion coating and method for producing same
WO2016104703A1 (fr) * 2014-12-26 2016-06-30 ディップソール株式会社 Liquide de conversion chimique à base de chrome trivalent pour bases de zinc ou d'alliage de zinc et film de revêtement de conversion chimique
US20160348245A1 (en) * 2015-05-28 2016-12-01 Macdermid, Incorporated Method of Pretreatment for Electroless Plating
EP3156518A1 (fr) * 2015-10-14 2017-04-19 Helmholtz-Zentrum Geesthacht Zentrum für Material- und Küstenforschung GmbH Composition inhibitrice de corrosion pour alliages de magnésium ou magnésium
CN105937031B (zh) * 2016-06-29 2018-10-30 周少霞 一种热镀锌板用钝化液的制备方法
KR101998606B1 (ko) * 2018-11-21 2019-07-10 주식회사 지에스켐텍 아연-니켈 도금용 3가 크로메이트계 흑색 내식성 향상제 및 이를 이용한 아연-니켈 도금층의 표면처리방법
CN114592186B (zh) * 2022-04-27 2024-03-12 上海库曜新材料有限公司 一种锌粉的无铬钝化方法

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Also Published As

Publication number Publication date
CN102227516A (zh) 2011-10-26
EP2358922B1 (fr) 2016-01-27
PL2358922T3 (pl) 2016-07-29
JP5562347B2 (ja) 2014-07-30
KR20110089304A (ko) 2011-08-05
JP2012509994A (ja) 2012-04-26
DE102008044143A1 (de) 2010-06-02
DE102008044143B4 (de) 2011-01-13
WO2010060883A1 (fr) 2010-06-03
US20110217476A1 (en) 2011-09-08
CN102227516B (zh) 2015-07-22
ES2565839T3 (es) 2016-04-07

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