FR2820152A1 - Coloring of galvanizd metal components by dipping in a pH controlled chemical coloring bath - Google Patents

Coloring of galvanizd metal components by dipping in a pH controlled chemical coloring bath Download PDF

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FR2820152A1
FR2820152A1 FR0101146A FR0101146A FR2820152A1 FR 2820152 A1 FR2820152 A1 FR 2820152A1 FR 0101146 A FR0101146 A FR 0101146A FR 0101146 A FR0101146 A FR 0101146A FR 2820152 A1 FR2820152 A1 FR 2820152A1
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bath
liter
coloring
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chemical coloring
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FR2820152B1 (en
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Thierry Schmitz
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Electro Recherche SARL
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/40—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 molybdates, tungstates or vanadates
    • C23C22/42—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 molybdates, tungstates or vanadates containing also phosphates
    • 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
    • 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
    • C23C22/40—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 molybdates, tungstates or vanadates

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating With Molten Metal (AREA)

Abstract

A method for coloring metal components subjected to galvanisation consists of immersing the components in a chemical coloring bath having a pH between 1 and 3 and containing active elements able to react with the zinc in the galvanization coating to form coloured complexes of a dark color followed by rinsing and drying of the treated components. Independent claims are also included for the chemical coloring bath used in this method and for the metallic component treated by this method.

Description

<Desc/Clms Page number 1> <Desc / Clms Page number 1>

La présente invention concerne un procédé de coloration de pièces métalliques ayant subi un traitement de galvanisation en particulier de galvanisation à chaud.  The present invention relates to a method of coloring metal parts which have undergone a galvanization treatment, in particular hot-dip galvanization.

Il est bien connu que, dans tous les domaines de l'industrie tels qu'à titre d'exemple l'automobile, l'électroménager, la conserverie,... il est nécessaire de protéger les pièces en fer, en fonte ou en acier contre la corrosion.  It is well known that, in all areas of industry such as, for example, the automobile, household appliances, the canning industry, ... it is necessary to protect the iron, cast iron or steel against corrosion.

Parmi les procédés les plus couramment utilisés pour effectuer cette protection, on peut mentionner la galvanisation qui est connue depuis déjà de nombreuses dizaines d'années.  Among the processes most commonly used to perform this protection, mention may be made of galvanization which has been known for many decades.

Cette opération, qui consiste à recouvrir les pièces à protéger d'une couche de protection à base de zinc peut s'effectuer soit par trempage dans un bain de zinc fondu (ou enduction au rouleau), soit par électrozingage.  This operation, which consists of covering the parts to be protected with a zinc-based protective layer, can be carried out either by dipping in a bath of molten zinc (or coating with a roller), or by electrozincing.

Le dépôt qui doit être d'épaisseur contrôlée peut ou non être réalisé sur toutes les faces de la pièce. Il est constitué de zinc pur ou additionné d'éléments tels qu'à titre d'exemple le nickel, l'étain, le cuivre, le plomb, le fer, le cobalt, ou encore l'aluminium.  The deposit which must be of controlled thickness may or may not be carried out on all the faces of the part. It consists of pure zinc or with the addition of elements such as, for example, nickel, tin, copper, lead, iron, cobalt, or even aluminum.

Il est en particulier à noter que l'ajout d'aluminium améliore la brillance des revêtements de galvanisation, réduit l'oxydation superficielle du zinc, améliore la fluidité du bain, et permet de contrôler la réaction zinc/fer qui contribue à l'obtention de l'épaisseur.  It should be noted in particular that the addition of aluminum improves the gloss of the galvanizing coatings, reduces the surface oxidation of zinc, improves the fluidity of the bath, and makes it possible to control the zinc / iron reaction which contributes to obtaining of thickness.

En effet, pour donner satisfaction, les revêtements de galvanisation doivent avoir un aspect uniforme non marbré et en outre avoir une épaisseur homogène en règle gé-

Figure img00010001

nérale de l'ordre de 30 à 80 um. In fact, to give satisfaction, the galvanizing coatings must have a uniform, unblasted appearance and also have a uniform thickness as a rule.
Figure img00010001

general in the range of 30 to 80 µm.

De tels revêtements de galvanisation permettent de garantir des tenues en corrosion très performantes des pièces traitées, et également de les rigidifier.  Such galvanizing coatings make it possible to guarantee highly efficient corrosion resistance of the treated parts, and also to stiffen them.

Ils présentent cependant l'inconvénient d'avoir un aspect métallique brillant qui n'est pas toujours du goût des consommateurs en particulier dans le cadre de l'industrie automobile, lorsque les pièces traitées sont des pièces de  However, they have the drawback of having a shiny metallic appearance which is not always to the taste of consumers, in particular in the context of the automobile industry, when the parts treated are parts of

<Desc/Clms Page number 2><Desc / Clms Page number 2>

sous-bassement de moteurs notamment destinées à être situées à proximité de pièces colorées en noir.  underbody of engines in particular intended to be located near parts colored in black.

La présente invention a pour objet de remédier à ces inconvénients.  The object of the present invention is to remedy these drawbacks.

A cet effet, elle concerne un procédé permettant de doter des pièces métalliques ayant subi un traitement de galvanisation, en particulier de galvanisation à chaud dans un bain à base de zinc fondu allié ou non à différents métaux d'addition d'une couche surfacique d'aspect le plus foncé possible.  To this end, it relates to a process making it possible to provide metal parts which have undergone a galvanization treatment, in particular hot galvanization in a bath based on molten zinc alloyed or not with different metals for the addition of a surface layer d as dark as possible.

Selon l'invention, ce procédé est caractérisé en ce que l'on immerge la pièce à traiter dans un bain de coloration chimique ayant un pH compris entre 1 et 3 et renfermant des éléments actifs susceptibles de réagir avec le zinc présent dans le revêtement de galvanisation pour former des complexes colorés de couleur sombre, puis on rince et on sèche la pièce ainsi traitée.  According to the invention, this process is characterized in that the part to be treated is immersed in a chemical coloring bath having a pH between 1 and 3 and containing active elements capable of reacting with the zinc present in the coating of galvanizing to form dark colored complexes, then rinse and dry the part thus treated.

Ce procédé permet, suite à la réaction entre les cations zinc et les différents cations et anions présents dans le bain de coloration chimique, de former à la surface

Figure img00020001

du revêtement de galvanisation une couche de galvanisation de couleur sombre ayant une épaisseur de l'ordre de 5 um dont la présence ne modifie ni les cotes ni le poids de la pièce galvanisée. This process allows, following the reaction between zinc cations and the different cations and anions present in the chemical coloring bath, to form on the surface
Figure img00020001

of the galvanizing coating a dark colored galvanizing layer having a thickness of the order of 5 μm, the presence of which does not modify either the dimensions or the weight of the galvanized part.

Cette coloration en surface permet d'obtenir un aspect très proche du noir et d'atténuer les effets de grain qui sont très visibles sur les pièces galvanisées par le procédé de galvanisation classique, ce, sans nuire aux tenues en corrosion des pièces ainsi traitées, notamment lors des tests en brouillard salin.  This surface coloring makes it possible to obtain an appearance very close to black and to attenuate the grain effects which are very visible on the parts galvanized by the conventional galvanizing process, without harming the corrosion resistance of the parts thus treated, especially during salt spray tests.

Selon une autre caractéristique de l'invention, la température du bain de coloration chimique est de préférence comprise entre 50 et 90oC.  According to another characteristic of the invention, the temperature of the chemical coloring bath is preferably between 50 and 90oC.

Le temps nécessaire à l'obtention de la couche de galvanisation de couleur sombre à la surface du revêtement de galvanisation est en règle générale de 3 à 7 minutes. Après sa sortie du bain de coloration chimique, la pièce traitée est de préférence rincée à l'eau de ville pendant environ  The time required to obtain the dark-colored galvanizing layer on the surface of the galvanizing coating is generally 3 to 7 minutes. After leaving the chemical coloring bath, the treated part is preferably rinsed with tap water for approximately

<Desc/Clms Page number 3> <Desc / Clms Page number 3>

Figure img00030001

1 minute puis séchée à l'air chaud à température de 70 à 80 C pendant environ 10 minutes.
Figure img00030001

1 minute then dried with hot air at a temperature of 70 to 80 C for about 10 minutes.

Selon une autre caractéristique de l'invention, on agite le bain de coloration chimique de préférence en y insufflant un courant d'air.  According to another characteristic of the invention, the chemical coloring bath is preferably stirred by blowing a stream of air into it.

L'invention se rapporte également à un bain de coloration chimique permettant la mise en oeuvre du procédé susmentionné.  The invention also relates to a chemical coloring bath allowing the implementation of the above-mentioned process.

Selon l'invention, un tel bain est caractérisé en ce qu'il renferme entre 1 et 30 g/litre d'au moins un acide, de préférence d'un mélange d'acide borique et d'acide phosphorique de façon à obtenir un pH compris entre 1 et 3.  According to the invention, such a bath is characterized in that it contains between 1 and 30 g / liter of at least one acid, preferably a mixture of boric acid and phosphoric acid so as to obtain a pH between 1 and 3.

Selon une autre caractéristique de l'invention, le bain de coloration chimique renferme entre 1 et 15 g/litre d'au moins un sel de molybdène.  According to another characteristic of the invention, the chemical coloring bath contains between 1 and 15 g / liter of at least one molybdenum salt.

Selon une autre caractéristique de l'invention, le bain de coloration chimique renferme entre 10 et 50 g/litre d'au moins un sel de nickel.  According to another characteristic of the invention, the chemical coloring bath contains between 10 and 50 g / liter of at least one nickel salt.

On a à titre d'exemple pu obtenir des résultats particulièrement avantageux en mettant en oeuvre un bain de coloration chimique ayant approximativement la composition suivante :

Figure img00030002

molybdat de sodium déshydraté 5 g/litre sulfate de nickel hexahydraté 30 g/litre acide borique 15 g/litre acide phosphorique à 85 % 0, 2 ml/litre chlorure ferrique 2 g/litre. As an example, it was possible to obtain particularly advantageous results by using a chemical coloring bath having approximately the following composition:
Figure img00030002

dehydrated sodium molybdat 5 g / liter nickel sulfate hexahydrate 30 g / liter boric acid 15 g / liter phosphoric acid 85% 0.2 ml / liter ferric chloride 2 g / liter.

L'invention se rapporte également à une pièce métallique traitée dans un tel bain de coloration chimique par le procédé susmentionné.  The invention also relates to a metal part treated in such a chemical coloring bath by the aforementioned method.

Une telle pièce est caractérisée en ce qu'elle présente, à la surface du revêtement de galvanisation une couche de galvanisation de couleur sombre ayant une épaisseur

Figure img00030003

de l'ordre de 5 um. Such a part is characterized in that it has, on the surface of the galvanizing coating, a dark-colored galvanizing layer having a thickness
Figure img00030003

on the order of 5 µm.

On a pu vérifier expérimentalement qu'une telle couche de galvanisation de couleur sombre peut avantageuse- ment avoir la composition suivante : - Zn 60 % It has been experimentally verified that such a dark-colored galvanizing layer can advantageously have the following composition: - Zn 60%

<Desc/Clms Page number 4><Desc / Clms Page number 4>

- Mo 32 % - Ni 2 % - P 5 % - Al 1 % - Fe 0,2 %
La densité d'une telle couche est de 7,68.- Mo 32% - Ni 2% - P 5% - Al 1% - Fe 0.2%
The density of such a layer is 7.68.

Claims (1)

Figure img00050001
Figure img00050001
 REVENDICATIONS 1 ) Procédé de coloration de pièces métalliques ayant subi un traitement de galvanisation, en particulier de galvanisation à chaud dans un bain à base de zinc fondu, caractérisé en ce que l'on immerge la pièce à traiter dans un bain de coloration chimique ayant un pH compris entre 1 et 3 et renfermant des éléments actifs susceptibles de réagir avec le zinc présent dans le revêtement de galvanisation pour former des complexes colorés de couleur sombre puis on rince et on sèche la pièce ainsi traitée. CLAIMS 1) Process for coloring metal parts which have undergone a galvanizing treatment, in particular hot galvanizing in a bath based on molten zinc, characterized in that the part to be treated is immersed in a chemical coloring bath having a pH between 1 and 3 and containing active elements capable of reacting with the zinc present in the galvanizing coating to form colored complexes of dark color, then the part thus treated is rinsed and dried. 2 ) Procédé selon la revendication l, caractérisé en ce que l'on immerge la pièce à traiter dans le bain de coloration chimique pendant 3 à 7 minutes.  2) Method according to claim l, characterized in that the part to be treated is immersed in the chemical coloring bath for 3 to 7 minutes. 3 ) Procédé selon l'une quelconque des revendications 1 et 2, caractérisé en ce que la température du bain de coloration chimique est comprise entre 50 et 90 C.  3) Method according to any one of claims 1 and 2, characterized in that the temperature of the chemical coloring bath is between 50 and 90 C. 4 ) Procédé selon l'une quelconque des revendications 1 à 3, caractérisé en ce que l'on agite le bain de coloration chimique, de préférence en y insufflant un courant d'air.  4) Method according to any one of claims 1 to 3, characterized in that the chemical coloring bath is stirred, preferably by blowing in a stream of air. 5 ) Bain de coloration chimique permettant la mise en oeuvre du procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu' il renferme entre 1 et 30 g/litre d'au moins un acide de préférence d'un mélange d'acide borique et d'acide phosphorique.  5) bath of chemical coloring allowing the implementation of the method according to any one of claims 1 to 4, characterized in that it contains between 1 and 30 g / liter of at least one acid preferably of a mixture boric acid and phosphoric acid. 6 ) Bain selon la revendication 5, caractérisé en ce qu' il renferme entre 1 et 15 g/litre d'au moins un sel de molybdène.  6) Bath according to claim 5, characterized in that it contains between 1 and 15 g / liter of at least one molybdenum salt. <Desc/Clms Page number 6><Desc / Clms Page number 6> 7 ) Bain selon l'une quelconque des revendications 5 et 6, caractérisé en ce qu' il renferme entre 10 et 50 g/litre d'au moins un sel de nickel.  7) Bath according to any one of claims 5 and 6, characterized in that it contains between 10 and 50 g / liter of at least one nickel salt. 80) Bain selon l'une quelconque des revendications 5 à 7, caractérisé en ce qu'  80) Bath according to any one of claims 5 to 7, characterized in that
Figure img00060001
Figure img00060001
 il a approximativement la composition suivante : molybdat de sodium déshydraté 5 g/litre sulfate de nickel hexahydraté 30 g/litre acide borique 15 g/litre acide phosphorique à 85 % 0, 2 ml/litre chlorure ferrique 2 g/litre.  it has approximately the following composition: dehydrated sodium molybdat 5 g / liter nickel sulfate hexahydrate 30 g / liter boric acid 15 g / liter 85% phosphoric acid 0.2 ml / liter ferric chloride 2 g / liter. 9 ) Pièce métallique traitée par le procédé selon l'une quelconque des revendications 1 à 4 dans un bain de coloration chimique selon l'une quelconque des revendications 5 à 8, caractérisée en ce qu' elle est revêtue d'une couche de galvanisation de couleur sombre ayant une épaisseur de l'ordre de 5 um.  9) Metal part treated by the method according to any one of claims 1 to 4 in a chemical coloring bath according to any one of claims 5 to 8, characterized in that it is coated with a galvanizing layer of dark color having a thickness of the order of 5 µm. 100) Pièce métallique selon la revendication 9, caractérisée en ce que la couche de galvanisation a approximativement la composition suivante : - Zn 60 % - Mo 32% - Ni 2 % - P 5 % - Al 1 % -fie 0, 2 %  100) Metal part according to claim 9, characterized in that the galvanizing layer has approximately the following composition: - Zn 60% - Mo 32% - Ni 2% - P 5% - Al 1% -fie 0, 2%
FR0101146A 2001-01-29 2001-01-29 PROCESS FOR COLORING GALVANIZED METAL PARTS AS WELL AS A COLORING BATH FOR CARRYING OUT SAID METHOD AND PARTS OBTAINED BY IMPLEMENTING SAME Expired - Fee Related FR2820152B1 (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3171766A (en) * 1962-10-04 1965-03-02 Conversion Chem Corp Bright polishing of cadmium and zinc
JPS5274541A (en) * 1975-12-17 1977-06-22 Kobe Steel Ltd Process for surface treating zinc or zinc plated products
JPH02122081A (en) * 1988-10-28 1990-05-09 Chubu Electric Power Co Inc Method for coloring zinc and zinc alloy
US5344505A (en) * 1993-08-16 1994-09-06 Betz Laboratories, Inc. Non-chromium passivation method and composition for galvanized metal surfaces
WO1997027001A1 (en) * 1996-01-23 1997-07-31 Henkel Corporation Passivation composition and process for coating
WO1999061681A1 (en) * 1998-05-28 1999-12-02 Bhp Steel (Jla) Pty. Ltd. An anticorrosion treatment
FR2796655A1 (en) * 1999-07-22 2001-01-26 Dacral Sa Aqueous anti-corrosion composition for a metal substrate protected by zinc-based layer contains silane, boric and/or phosphoric acid, micronized silica and wetting agent

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3171766A (en) * 1962-10-04 1965-03-02 Conversion Chem Corp Bright polishing of cadmium and zinc
JPS5274541A (en) * 1975-12-17 1977-06-22 Kobe Steel Ltd Process for surface treating zinc or zinc plated products
JPH02122081A (en) * 1988-10-28 1990-05-09 Chubu Electric Power Co Inc Method for coloring zinc and zinc alloy
US5344505A (en) * 1993-08-16 1994-09-06 Betz Laboratories, Inc. Non-chromium passivation method and composition for galvanized metal surfaces
WO1997027001A1 (en) * 1996-01-23 1997-07-31 Henkel Corporation Passivation composition and process for coating
WO1999061681A1 (en) * 1998-05-28 1999-12-02 Bhp Steel (Jla) Pty. Ltd. An anticorrosion treatment
FR2796655A1 (en) * 1999-07-22 2001-01-26 Dacral Sa Aqueous anti-corrosion composition for a metal substrate protected by zinc-based layer contains silane, boric and/or phosphoric acid, micronized silica and wetting agent

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
CHEMICAL ABSTRACTS, vol. 111, no. 6, 7 August 1989, Columbus, Ohio, US; abstract no. 43517b, KISS J.: "Bath for blackening cast iron, steel and galvanised steel at low temperatures" page 265; XP000058407 *
DATABASE WPI Section Ch Week 197731, Derwent World Patents Index; Class M11, AN 1977-54999Y, XP002182040 *
PATENT ABSTRACTS OF JAPAN vol. 014, no. 334 (C - 0742) 18 July 1990 (1990-07-18) *
WILCOX G. D.: "Chemical molybdate conversion treatments for zinc", METAL FINISHING., vol. 86, no. 9, 1 September 1988 (1988-09-01), ELSEVIER SCIENCE PUBLISHING, NEW YORK, NY., US, pages 71 - 74, XP002182039, ISSN: 0026-0576 *

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