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EP0257671A1 - Process for removing niobium-containing coatings from a substrate - Google Patents

Process for removing niobium-containing coatings from a substrate Download PDF

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Publication number
EP0257671A1
EP0257671A1 EP87201347A EP87201347A EP0257671A1 EP 0257671 A1 EP0257671 A1 EP 0257671A1 EP 87201347 A EP87201347 A EP 87201347A EP 87201347 A EP87201347 A EP 87201347A EP 0257671 A1 EP0257671 A1 EP 0257671A1
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EP
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Prior art keywords
coating
niobium
substrate
bath
baths
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Granted
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EP87201347A
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German (de)
French (fr)
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EP0257671B1 (en
Inventor
Lucien Clerbois
Gérard Parissis
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Solvay SA
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Solvay SA
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Priority to AT87201347T priority Critical patent/ATE74971T1/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F1/00Etching metallic material by chemical means
    • C23F1/44Compositions for etching metallic material from a metallic material substrate of different composition
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23FNON-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
    • C23F1/00Etching metallic material by chemical means
    • C23F1/10Etching compositions
    • C23F1/14Aqueous compositions
    • C23F1/32Alkaline compositions
    • C23F1/38Alkaline compositions for etching refractory metals

Definitions

  • the present invention relates to pickling baths and a method for removing a coating comprising niobium on a substrate.
  • Niobium and niobium alloys are known for their interesting chemical and electrical properties, in particular their resistance to corrosion vis-à-vis most corrosive substances at room temperature and especially their qualities of excellent conductor of heat and electricity.
  • niobium and its alloys are frequently used for the construction of chemical engineering apparatus and installations and also as a superconductive coating of electrodes.
  • the electrical resistivity of niobium and its alloys becomes almost zero below 8.3 ° K (Revue de la cios Royale Belge des In conurs et des Industriels -n ° 8/9 - 1969: R WINAND, "Properties and uses of refractory metals", pages 381 to 415).
  • the high price of niobium frequently encourages its use in the form of coating on a substrate (R. Lescarts - Dictionary of non-ferrous metals - 1972 - p. 107).
  • the invention therefore aims to provide a pickling bath for quickly and effectively removing a coating comprising niobium on a substrate without giving rise to polluting and toxic discharges and, above all, without damaging the substrate, especially when it is in copper.
  • the invention therefore relates to baths for removing a coating comprising niobium on a substrate, which consists of an aqueous solution of alkali metal hydroxide and hydrogen peroxide.
  • the alkali metal hydroxide can for example be sodium hydroxide or potassium hydroxide.
  • Sodium hydroxide is preferred.
  • the contents of alkali metal hydroxide and hydrogen peroxide in the baths according to the invention depend on various parameters, in particular the temperature at which they are used, the desired attack speed, the thickness of the coating to be remove and material from the substrate.
  • the baths according to the invention contain, per liter, at least 0.4 mole of alkali metal hydroxide and at least 7.5 ml of 100% hydrogen peroxide.
  • Examples of baths which can be used in the process according to the invention are those containing, per liter, between 0.5 and 4 moles of alkali metal hydroxide and between 10 and 155 ml of 100% hydrogen peroxide.
  • the preferred baths are those containing, per liter, between 0.5 and 2 moles of alkali metal hydroxide and between 13 and 75 ml of 100% hydrogen peroxide.
  • the aqueous solution of the baths according to the invention may advantageously contain, in usual proportions, a stabilizer of the hydrogen peroxide such as a derivative of gluconic acid or of a phosphonic acid, for example one of the products known under the brand "DEQUEST" (Monsanto) which are derivatives of phosphonic acid. It may optionally contain additives commonly present in metal pickling baths, such as surfactants and corrosion inhibitors, for example.
  • a stabilizer of the hydrogen peroxide such as a derivative of gluconic acid or of a phosphonic acid, for example one of the products known under the brand "DEQUEST" (Monsanto) which are derivatives of phosphonic acid.
  • additives commonly present in metal pickling baths such as surfactants and corrosion inhibitors, for example.
  • the pickling baths according to the invention are suitable for removing a coating containing niobium on all types of substrates which are not likely to undergo local corrosion in contact with said baths. They are specially adapted for removing a coating comprising niobium on a copper or copper-based alloy substrate.
  • the coating can be pure niobium or a niobium alloy, for example an Nb-C-N alloy or an Nb-Al-Ge alloy, or an Nb-Ti alloy.
  • the invention therefore also relates to a method for removing a coating comprising niobium on a substrate, by treating the coating with a pickling bath according to the invention.
  • the treatment of the coating with the bath can be carried out by any suitable technique, for example by immersion of the substrate with its coating in the bath, by coating or by spraying the bath on the coating.
  • the amount of bath used must be sufficient to dissolve the niobium coating. It depends in particular on the mass of the coating to be removed, its constitution, the composition of the bath and the temperature. It must be determined in each case.
  • the process according to the invention should be carried out at a temperature at which there is no risk of untimely decomposition of the bath.
  • the term of the reaction of the bath with the coating is detected, by a measurement of the electrochemical potential of the substrate in the bath.
  • the method according to the invention finds an application in particular in the construction and maintenance of particle accelerators such as cyclotrons for example, where it can be used to remove a superconductive coating of niobium or of niobium alloy from the wall in copper cavities forming the electrodes supplied with high frequency current (for example an alloy of niobium and titanium as suggested in the document Research and Development - January 1986 - pages 49 and 50: "Physics - Magnet design brings breath of reality to SSC ").
  • particle accelerators such as cyclotrons for example
  • a wafer was immersed in the bath at room temperature and the niobium removal process was followed by a measurement of the electrochemical potential of the wafer relative to a reference electrode of calomel saturated with KCl.
  • the weight of niobium removed was determined by measuring the weight of the wafer, before and after treatment, respectively; knowing the area of the wafer, the thickness of the eliminated niobium film has been deduced therefrom.
  • the platelets collected at the end of the tests were found to be completely stripped of their niobium coating. They had a uniformly polished surface, free of corrosion zones.

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  • Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • ing And Chemical Polishing (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Materials For Medical Uses (AREA)
  • Chemically Coating (AREA)
  • Paints Or Removers (AREA)

Abstract

Baths consisting of an aqueous solution of hydrogen peroxide and alkali metal hydroxide. The coating is treated with the bath in order to remove the substrate by dissolution.

Description

La présente invention concerne des bains décapants et un procédé pour éliminer un revêtement comprenant du niobium sur un substrat.The present invention relates to pickling baths and a method for removing a coating comprising niobium on a substrate.

Le niobium et les alliages de niobium sont connus pour leurs propriétés chimiques et électriques intéressantes, notamment leur résistance à la corrosion vis-à-vis de la plupart des substances corrosives à température ambiante et surtout leurs qualités d'excellent conducteur de la chaleur et de l'électricité. Il en résulte que le niobium et ses alliages sont fréquemment utilisés pour la construction d'appareils et d'installations de génie chimique et aussi comme revêtement supraconducteur d'électrodes. On sait, en effet, que la résistivité électrique du niobium et de ses alliages devient quasi nulle au-dessous de 8,3°K (Revue de la Société Royale Belge des Ingénieurs et des Industriels -n° 8/9 - 1969 : R. WINAND, "Propriétés et usages des métaux réfractaires", pages 381 à 415). Toutefois, le prix élevé du niobium incite fréquemment à l'utiliser sous la forme de revêtement sur un substrat (R. Lescarts - Dictionnaire des métaux non ferreux - 1972 - p. 107).Niobium and niobium alloys are known for their interesting chemical and electrical properties, in particular their resistance to corrosion vis-à-vis most corrosive substances at room temperature and especially their qualities of excellent conductor of heat and electricity. As a result, niobium and its alloys are frequently used for the construction of chemical engineering apparatus and installations and also as a superconductive coating of electrodes. We know, in fact, that the electrical resistivity of niobium and its alloys becomes almost zero below 8.3 ° K (Revue de la Société Royale Belge des Ingénieurs et des Industriels -n ° 8/9 - 1969: R WINAND, "Properties and uses of refractory metals", pages 381 to 415). However, the high price of niobium frequently encourages its use in the form of coating on a substrate (R. Lescarts - Dictionary of non-ferrous metals - 1972 - p. 107).

Dans la construction ou l'entretien d'électrodes ou d'autres organes portant un revêtement comprenant du niobium, on peut être amené à devoir procéder à la dissolution ou au décapage du revêtement afin de libérer le substrat totalement ou en partie.In the construction or maintenance of electrodes or other bodies carrying a coating comprising niobium, it may be necessary to dissolve or pickle the coating in order to release the substrate completely or in part.

Pour effectuer le décapage du niobium, on a proposé d'utiliser, à une température inférieure à 50°C, une solution décapante contenant 45 à 65 parties en volume d'eau, 30 à 50 parties en volume d'acide sulfurique concentré, 0,2 à 3,0 parties en volume d'une solution aqueuse concentrée de peroxyde d'hydrogène et 1,0 à 5,0 parties en volume d'acide fluorhydrique concentré (Central Patents Index, Basic Abstracts Journal, Section L, Week D.19, Derwent Publications Ltd., Londres, abrégé 33525D-L : demande de brevet JP-A-56029324 (Tokyo Shibaura Elec. Ltd)). Le décapage ainsi réalisé est généralement rapide et efficace, mais la présence d'acide fluorhydrique rend ces bains connus, toxiques et dangereux pour les utilisateurs et donne lieu, par conséquent, à des rejets polluants. Ces bains sont par ailleurs contre-indiqués dans le cas d'un substrat en cuivre, qu'ils risquent de corroder.To carry out the pickling of niobium, it has been proposed to use, at a temperature below 50 ° C., a pickling solution containing 45 to 65 parts by volume of water, 30 to 50 parts by volume of concentrated sulfuric acid, 0 , 2 to 3.0 parts by volume of a concentrated aqueous solution of hydrogen peroxide and 1.0 to 5.0 parts by volume of concentrated hydrofluoric acid (Central Patents Index, Basic Abstracts Journal, Section L, Week D .19, Derwent Publications Ltd., London, abstract 33525D-L: Patent Application JP-A-56029324 (Tokyo Shibaura Elec. Ltd)). The pickling thus carried out is generally rapid and effective, but the presence of hydrofluoric acid makes these baths known, toxic and dangerous for the users and gives rise, consequently, to polluting discharges. These baths are also contraindicated in the case of a copper substrate, which they risk corroding.

L'invention vise dès lors à fournir un bain décapant permettant d'éliminer rapidement et efficacement un revêtement comprenant du niobium sur un substrat sans donner naissance à des rejets polluants et toxiques et, surtout, sans endommager le substrat, notamment lorsque celui-ci est en cuivre.The invention therefore aims to provide a pickling bath for quickly and effectively removing a coating comprising niobium on a substrate without giving rise to polluting and toxic discharges and, above all, without damaging the substrate, especially when it is in copper.

En conséquence, l'invention concerne des bains pour éliminer un revêtement comprenant du niobium sur un substrat, qui consistent en une solution aqueuse d'hydroxyde de métal alcalin et de peroxyde d'hydrogène.The invention therefore relates to baths for removing a coating comprising niobium on a substrate, which consists of an aqueous solution of alkali metal hydroxide and hydrogen peroxide.

Dans les bains selon l'invention, l'hydroxyde de métal alcalin peut par exemple être de l'hydroxyde de sodium ou de l'hydroxyde de potassium. L'hydroxyde de sodium est préféré.In the baths according to the invention, the alkali metal hydroxide can for example be sodium hydroxide or potassium hydroxide. Sodium hydroxide is preferred.

Les teneurs en hydroxyde de métal alcalin et en peroxyde d'hydrogène dans les bains selon l'invention dépendent de divers paramètres, notamment de la température à laquelle on les utilise, de la vitesse d'attaque souhaitée, de l'épaisseur du revêtement à éliminer et du matériau du substrat. En pratique, il convient généralement que les bains selon l'invention contiennent, par litre, au moins 0,4 mole d'hydroxyde de métal alcalin et au moins 7,5 ml de peroxyde d'hydrogène à 100 %. Des exemples de bains utilisables dans le procédé selon l'invention sont ceux contenant, par litre, entre 0,5 et 4 moles d'hydroxyde de métal alcalin et entre 10 et 155 ml de peroxyde d'hydrogène à 100 %. Les bains préférés sont ceux contenant, par litre, entre 0,5 et 2 moles d'hydroxyde de métal alcalin et entre 13 et 75 ml de peroxyde d'hydrogène à 100 %.The contents of alkali metal hydroxide and hydrogen peroxide in the baths according to the invention depend on various parameters, in particular the temperature at which they are used, the desired attack speed, the thickness of the coating to be remove and material from the substrate. In practice, it is generally appropriate that the baths according to the invention contain, per liter, at least 0.4 mole of alkali metal hydroxide and at least 7.5 ml of 100% hydrogen peroxide. Examples of baths which can be used in the process according to the invention are those containing, per liter, between 0.5 and 4 moles of alkali metal hydroxide and between 10 and 155 ml of 100% hydrogen peroxide. The preferred baths are those containing, per liter, between 0.5 and 2 moles of alkali metal hydroxide and between 13 and 75 ml of 100% hydrogen peroxide.

La solution aqueuse des bains selon l'invention peut avantageusement contenir, en des proportions usuelles, un stabilisant du peroxyde d'hydrogène tel qu'un dérivé de l'acide gluconique ou d'un acide phosphonique, par exemple un des produits connus sous la marque "DEQUEST" (Monsanto) qui sont des dérivés d'acide phosphonique. Elle peut éventuellement contenir des additifs communément présents dans les bains de décapage des métaux, tels que des agents tensioactifs et des inhibiteurs de corrosion, par exemple.The aqueous solution of the baths according to the invention may advantageously contain, in usual proportions, a stabilizer of the hydrogen peroxide such as a derivative of gluconic acid or of a phosphonic acid, for example one of the products known under the brand "DEQUEST" (Monsanto) which are derivatives of phosphonic acid. It may optionally contain additives commonly present in metal pickling baths, such as surfactants and corrosion inhibitors, for example.

Les bains décapants selon l'invention conviennent pour éliminer un revêtement contenant du niobium sur tous types de substrats qui ne risquent pas de subir des corrosions locales au contact desdits bains. Ils sont spécialement adaptés à l'élimination d'un revêtement comprenant du niobium sur un substrat en cuivre ou en alliage à base de cuivre. Le revêtement peut être du niobium pur ou un alliage de niobium, par exemple un alliage Nb-C-N ou un alliage Nb-Al-Ge, ou encore un alliage Nb-Ti.The pickling baths according to the invention are suitable for removing a coating containing niobium on all types of substrates which are not likely to undergo local corrosion in contact with said baths. They are specially adapted for removing a coating comprising niobium on a copper or copper-based alloy substrate. The coating can be pure niobium or a niobium alloy, for example an Nb-C-N alloy or an Nb-Al-Ge alloy, or an Nb-Ti alloy.

L'invention concerne dès lors aussi un procédé pour éliminer un revêtement comprenant du niobium sur un substrat, par traitement du revêtement avec un bain décapant conforme à l'invention.The invention therefore also relates to a method for removing a coating comprising niobium on a substrate, by treating the coating with a pickling bath according to the invention.

Dans le procédé selon l'invention, le traitement du revêtement avec le bain peut être exécuté par toute technique adéquate, par exemple par immersion du substrat avec son revêtement dans le bain, par enduction ou par pulvérisation du bain sur le revêtement.In the method according to the invention, the treatment of the coating with the bath can be carried out by any suitable technique, for example by immersion of the substrate with its coating in the bath, by coating or by spraying the bath on the coating.

La quantité de bain mis en oeuvre doit être suffisante pour dissoudre le revêtement de niobium. Elle dépend notamment de la masse du revêtement à éliminer, de sa constitution, de la composition du bain et de la température. Elle doit être déterminée dans chaque cas.The amount of bath used must be sufficient to dissolve the niobium coating. It depends in particular on the mass of the coating to be removed, its constitution, the composition of the bath and the temperature. It must be determined in each case.

Il convient d'exécuter le procédé selon l'invention à une température à laquelle on ne risque pas une décomposition intempestive du bain. A cet effet, il est généralement opportun de mettre le bain en oeuvre à une température n'excédant pas 50°C, la température ambiante, comprise entre 15 et 25°C, étant la plus adéquate dans la plupart des cas.The process according to the invention should be carried out at a temperature at which there is no risk of untimely decomposition of the bath. For this purpose, it is generally advisable to carry out the bath at a temperature not exceeding 50 ° C., the ambient temperature, between 15 and 25 ° C., being the most adequate in most cases.

Dans le procédé selon l'invention, il est important de pouvoir suivre l'évolution du processus d'élimination du revêtement du substrat, de manière à déceler avec précision l'instant opportun pour cesser le traitement avec le bain. A cet effet, dans une forme d'exécution avantageuse du procédé selon l'invention, on décèle le terme de la réaction du bain avec le revêtement, par une mesure du potentiel électrochimique du substrat dans le bain. Dans la mise en oeuvre de cette forme d'exécution du procédé, il suffit dès lors de coupler une cellule de mesure de potentiel entre le substrat muni de son revêtement et une électrode de référence, immergée dans le bain.In the process according to the invention, it is important to be able to follow the progress of the process of removing the coating from the substrate, so as to accurately detect the right moment to stop the treatment with the bath. To this end, in an advantageous embodiment of the method according to the invention, the term of the reaction of the bath with the coating is detected, by a measurement of the electrochemical potential of the substrate in the bath. In the implementation of this embodiment of the method, it therefore suffices to couple a potential measurement cell between the substrate provided with its coating and a reference electrode, immersed in the bath.

Le procédé selon l'invention trouve notamment une application dans la construction et l'entretien des accélérateurs de particules tels que les cyclotrons par exemple, où il peut être utilisé pour éliminer un revêtement supraconducteur de niobium ou d'alliage de niobium de la paroi en cuivre des cavités formant les électrodes alimentées en courant à haute fréquence (par exemple un alliage de niobium et de titane comme suggéré dans le document Research and Development - January 1986 - pages 49 et 50 : "Physics - Magnet design brings breath of reality to SSC").The method according to the invention finds an application in particular in the construction and maintenance of particle accelerators such as cyclotrons for example, where it can be used to remove a superconductive coating of niobium or of niobium alloy from the wall in copper cavities forming the electrodes supplied with high frequency current (for example an alloy of niobium and titanium as suggested in the document Research and Development - January 1986 - pages 49 and 50: "Physics - Magnet design brings breath of reality to SSC ").

L'intérêt de l'invention va ressortir des exemples dont la description suit.The advantage of the invention will emerge from the examples, the description of which follows.

Ces exemples concernent des essais dans lesquels des plaquettes en cuivre portant un revêtement de niobium ont été traitées conformément au procédé selon l'invention, pour éliminer le revêtement de niobium.These examples relate to tests in which copper plates carrying a niobium coating were treated in accordance with the method according to the invention, in order to remove the niobium coating.

On a procédé à trois essais avec des bains conformes à l'invention, dont la composition est donnée au tableau I.

Figure imgb0001
Three tests were carried out with baths in accordance with the invention, the composition of which is given in Table I.
Figure imgb0001

Dans chaque essai, on a immergé une plaquette dans le bain à la température ambiante et on a suivi le processus d'élimination du niobium par une mesure du potentiel électrochimique de la plaquette par rapport à une électrode de référence au calomel saturé en KCl. On a déterminé le poids de niobium éliminé au moyen d'une mesure du poids de la plaquette, respectivement avant et après le traitement; connaissant la superficie de la plaquette, on en a déduit l'épaisseur de la pellicule de niobium éliminée.In each test, a wafer was immersed in the bath at room temperature and the niobium removal process was followed by a measurement of the electrochemical potential of the wafer relative to a reference electrode of calomel saturated with KCl. The weight of niobium removed was determined by measuring the weight of the wafer, before and after treatment, respectively; knowing the area of the wafer, the thickness of the eliminated niobium film has been deduced therefrom.

Les résultats des essais sont répertoriés au tableau II.

Figure imgb0002
The results of the tests are listed in Table II.
Figure imgb0002

Les plaquettes recueillies à l'issue des essais se sont avérées entièrement débarrassées de leur revêtement de niobium. Elles présentaient une surface uniformément polie, exempte de zones de corrosion.The platelets collected at the end of the tests were found to be completely stripped of their niobium coating. They had a uniformly polished surface, free of corrosion zones.

Claims (9)

1 - Bains décapants pour l'élimination d'un revêtement comprenant du niobium sur un substrat, comprenant du peroxyde d'hydrogène en solution aqueuse, caractérisés en ce qu'ils consistent en une solution aqueuse de peroxyde d'hydrogène et d'hydroxyde de métal alcalin.1 - Stripping baths for the removal of a coating comprising niobium on a substrate, comprising hydrogen peroxide in aqueous solution, characterized in that they consist of an aqueous solution of hydrogen peroxide and hydroxide alkali metal. 2 - Bains selon la revendication 1, caractérisés en ce que l'hydroxyde de métal alcalin est de l'hydroxyde de sodium.2 - Baths according to claim 1, characterized in that the alkali metal hydroxide is sodium hydroxide. 3 - Bains selon la revendication 1 ou 2, caractérisés en ce que la solution aqueuse contient, par litre, au moins 7,5 ml de peroxyde d'hydrogène et au moins 0,4 mole d'hydroxyde de métal alcalin.3 - Baths according to claim 1 or 2, characterized in that the aqueous solution contains, per liter, at least 7.5 ml of hydrogen peroxide and at least 0.4 mole of alkali metal hydroxide. 4 - Bains selon la revendication 3, caractérisés en ce que la solution aqueuse contient, par litre, entre 13 et 75 ml de peroxyde d'hydrogène et entre 0,5 et 2 moles d'hydroxyde de métal alcalin.4 - Baths according to claim 3, characterized in that the aqueous solution contains, per liter, between 13 and 75 ml of hydrogen peroxide and between 0.5 and 2 moles of alkali metal hydroxide. 5 - Bains selon l'une quelconque des revendications 1 à 4, caractérisés en ce que la solution aqueuse contient un stabilisant du peroxyde d'hydrogène, sélectionné parmi les dérivés de l'acide gluconique et des acides phosphoniques.5 - Baths according to any one of claims 1 to 4, characterized in that the aqueous solution contains a stabilizer of hydrogen peroxide, selected from derivatives of gluconic acid and phosphonic acids. 6 - Procédé pour éliminer un revêtement comprenant du niobium sur un substrat, selon lequel on traite le revêtement avec un bain décapant, caractérisé en ce qu'on met en oeuvre un bain conforme à l'une quelconque des revendications 1 à 5.6 - Method for removing a coating comprising niobium on a substrate, according to which the coating is treated with a pickling bath, characterized in that a bath is used in accordance with any one of claims 1 to 5. 7 - Procédé selon la revendication 6, caractérisé en ce qu'on met le bain en oeuvre à une température comprise entre 15 et 25°C.7 - Method according to claim 6, characterized in that the bath is implemented at a temperature between 15 and 25 ° C. 8 - Procédé selon la revendication 6 ou 7, caractérisé en ce qu'il est appliqué à l'élimination d'un revêtement de niobium ou d'alliage de niobium sur un substrat en cuivre ou en alliage de cuivre.8 - Method according to claim 6 or 7, characterized in that it is applied to the elimination of a coating of niobium or niobium alloy on a substrate of copper or copper alloy. 9 - Procédé selon l'une quelconque des revendications 6 à 8, caractérisé en ce qu'on décèle le terme de la réaction du bain avec le revêtement, par une mesure du potentiel électro-chimique du substrat dans le bain.9 - Process according to any one of claims 6 to 8, characterized in that the term of the reaction of the bath with the coating is detected, by a measurement of the electro-chemical potential of the substrate in the bath.
EP87201347A 1986-07-25 1987-07-14 Process for removing niobium-containing coatings from a substrate Expired - Lifetime EP0257671B1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT87201347T ATE74971T1 (en) 1986-07-25 1987-07-14 METHOD OF REMOVING A NIOBIUM CONTAINING COATING FROM A SUBSTRATE.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8611001A FR2601968B1 (en) 1986-07-25 1986-07-25 STRIPPING BATHS AND METHOD FOR REMOVING A COATING COMPRISING NIOBIUM ON A SUBSTRATE.
FR8611001 1986-07-25

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EP0257671A1 true EP0257671A1 (en) 1988-03-02
EP0257671B1 EP0257671B1 (en) 1992-04-15

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US (1) US4950359A (en)
EP (1) EP0257671B1 (en)
JP (1) JPS6335787A (en)
AT (1) ATE74971T1 (en)
BR (1) BR8605611A (en)
DE (1) DE3778246D1 (en)
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US8836120B2 (en) 2011-04-19 2014-09-16 Infineon Technologies Ag Semiconductor device with a layer including niobium, and/or tantalum overlying a contact pad or a metal layer
CN105018934A (en) * 2015-07-15 2015-11-04 安徽多晶涂层科技有限公司 Coating stripping powder for hard coating, prepared coating stripping liquid and coating stripping method
JP7297623B2 (en) * 2019-09-24 2023-06-26 株式会社東芝 Wire processing method

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DE3778246D1 (en) 1992-05-21
FR2601968B1 (en) 1989-04-14
FR2601968A1 (en) 1988-01-29
JPS6335787A (en) 1988-02-16
US4950359A (en) 1990-08-21
EP0257671B1 (en) 1992-04-15
ATE74971T1 (en) 1992-05-15
BR8605611A (en) 1988-03-29

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