EP0951582B1 - Traitement de surface de l'acier ou d'un alliage au nickel et acier ou alliage au nickel ainsi traites - Google Patents

Traitement de surface de l'acier ou d'un alliage au nickel et acier ou alliage au nickel ainsi traites Download PDF

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Publication number
EP0951582B1
EP0951582B1 EP97954726A EP97954726A EP0951582B1 EP 0951582 B1 EP0951582 B1 EP 0951582B1 EP 97954726 A EP97954726 A EP 97954726A EP 97954726 A EP97954726 A EP 97954726A EP 0951582 B1 EP0951582 B1 EP 0951582B1
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EP
European Patent Office
Prior art keywords
process according
peroxide
water
treated
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.)
Expired - Lifetime
Application number
EP97954726A
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German (de)
English (en)
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EP0951582A1 (fr
Inventor
Erhard Schenker
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.)
Areva GmbH
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Framatome ANP GmbH
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Publication date
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Publication of EP0951582A1 publication Critical patent/EP0951582A1/fr
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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
    • C23C22/68—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 solutions with pH between 6 and 8

Definitions

  • the invention relates to a method for preventing a radioactive substances enriched oxide layer on a Surface of stainless steel and / or of a nickel alloy.
  • the steel or the nickel alloy are of the type, for example Incoloy 800, Inconel 600 or the like.
  • An application of the The process can be done in nuclear technology for reduction the later activity (contamination) of components the primary circuit of water-cooled nuclear power plants a new installation or after decontamination.
  • the surface of the steel be by means of Peroxide or by means of a water-peroxide mixture or with peroxide solution at a temperature of max. 180 ° C is treated, with an at least 20 nm thick oxide layer is produced.
  • per peroxide also stands for one Water-peroxide mixture or a peroxide solution. In place of hydrogen peroxide can always occur “peroxide” and vice versa.
  • the treatment takes place e.g. under water, e.g. thereby, that hydrogen peroxide is added to the water.
  • water e.g. thereby, that hydrogen peroxide is added to the water.
  • surface treatment of stainless steel and / or nickel alloys, e.g. Incoloy type 800, Inconel 600, and the like, particularly in steam generators used by pressurized water reactors before that the surface to be treated initially with the usual Techniques such as chemical treatment is cleaned and degreased.
  • the real deal can with a peroxide solution with a peroxide concentration of 0.1 up to 200 mmol H202 in e.g. pure or deionized water.
  • This treatment can be in an open or closed System.
  • concentrations are higher than 10 mmol H202 not used but can still be used but bring no significant advantages in the sense of the invention more, because excess hydrogen peroxide quickly becomes thermal and is catalytically decomposed, i.e. for the target Layer formation remains ineffective.
  • the peroxide solution is e.g. a solution of peroxide in pure or deionized water.
  • the method is used for the treatment of in water-cooled Nuclear power plants wet surfaces which are used for mostly stainless steel and / or nickel alloys, e.g. of type
  • Incoloy 800, Inconel 600, or the like which are special are used in steam generators of pressurized water reactors, and which in the past due to cantamination have led to the problems mentioned at the beginning.
  • the layer created using hydrogen peroxide differs fundamentally different in their composition and structure atmospheric or formed only with hot water. While at atmospheric oxidation mainly chromium-rich oxide layers and predominantly in hot water without hydrogen peroxide Nickel spinels are formed with hydrogen peroxide almost pure iron III oxides. Oxide layers without Hydrogen peroxide provides little or no protection further oxidation in hot water / steam (the spinel layers continue to form) while layers covered by hydrogen peroxide were formed, are very stable and in particular when used later under the conditions of the prima circle of a nuclear power plant not allow spinel formation.
  • An advantage of the present invention is that the Parts that have surfaces to be treated, either can be expanded or treated separately.
  • Systems like Containers, pipes, pumps, can also be built in Condition to be treated by being on your water Be coated on the inside.
  • Another advantage of treating steel with hydrogen peroxide is that the surface treatment of the steel can be checked visually by changing the color. As a result of interference, the process is colored surface of deep gold treated according to the invention to dark blue-violet. Basically there are all spectral colors, depending on the layer thickness and the type of Light reflection.
  • the coloration of stainless steel is over not known in the prior art. So that's the procedure according to the invention also generally suitable for coloring stainless steel or nickel alloys by cleaning the Surface e.g. treated with peroxide under water becomes.
  • the coloring is not only interesting in connection with the specified uses of the method in nuclear technology, but also in non-nuclear areas.
  • Suitable layer thicknesses are those from approx. 20 nm to approx. 300 nm or between approx. 0.02 to approx. 0.3 ⁇ m. Such Layer thickness is e.g. with a treatment time between 10h and achieved 300h.
  • the pre-oxidation with hydrogen peroxide takes place in the Way that the coating at below-100 ° C in an open or closed container, or at temperatures above 100 ° C in a closed container.
  • coated Systems e.g. in nuclear technology
  • the latter is the Case when the systems, tanks, piping, pumps etc. to be coated on the inside exposed to water are, for example, in cooling systems in nuclear power plants the case is.
  • the procedure is as follows:
  • the container or the systems are filled with pure water or deionized water.
  • the pure water is preferably circulated or metered in continuously.
  • the water is brought to the desired treatment temperature and maintained by suitable devices.
  • a dilute solution of hydrogen peroxide is metered in, so that the desired concentration of hydrogen peroxide can be maintained at all times.
  • effective ventilation is expediently applied in order to remove the oxygen gas which is formed during the thermal and catalytic decomposition of excess hydrogen peroxide and to avoid a gas cushion. which could prevent the complete coating of the systems / containers.
  • Example 1 Open container (depressurized) temperature ⁇ 100 ° C print atmospheric concentration 0.1 to 100 mmol H 2 O 2 * water speed 0 to ⁇ 10 m / s treatment time 10 to ⁇ 300 h
  • Example 2 Closed container or system temperature > 100 ° C print > 1 bar, depending on the temperature, so that no steam cushion is created, respectively. the system remains completely filled with pressurized water.
  • the present invention proposes a method for the surface treatment of steel, such as in particular stainless steel, as well as nickel alloys, e.g. of type Incoloy 800, Inconel 600, and similar ones, particularly as in Steam generators from pressurized water reactors are used before, treatment with peroxide or a water-peroxide mixture or solution. It depends that a protective layer on the treated surface Oxide is formed.
  • the surface can be the surface of a Container, a pipeline, a pump, etc. at Boiling water reactors could e.g. also the feed water preheaters be treated using the method mentioned here, to prevent corrosion products from entering the reactor reduce.

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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)
  • Chemical Treatment Of Metals (AREA)

Claims (14)

  1. Procédé pour empêcher la présence d'une couche d'oxyde enrichie en substances radioactives sur une surface d'acier inoxydable et/ou d'un alliage de nickel,
       caractérisé    en ce que l'on forme sur la surface une couche d'oxyde d'une épaisseur d'au moins 20 nm, en traitant la surface par du peroxyde comme agent oxydant ou par un mélange d'eau et de peroxyde à une température de 180° C au maximum, avant que la surface ne vienne en contact avec des substances radioactives.
  2. Procédé suivant la revendication 1, caractérisé en ce que l'on nettoie d'abord et/ou dégraisse la surface à traiter.
  3. Procédé suivant la revendication 1 ou 2, caractérisé en ce que l'on effectue le traitement sous l'eau.
  4. Procédé suivant la revendication 3, caractérisé en ce que l'on ajoute du peroxyde à l'eau.
  5. Procédé suivant l'une des revendications 1 à 4, caractérisé en ce que l'on traite la surface par une solution de peroxyde ayant une concentration en peroxyde de 0,1 à 200 mmoles de H2O2, de préférence une concentration de 0,1 à 100 mmole de H2O2.
  6. Procédé suivant l'une des revendications 1 à 5, caractérisé en ce que la solution de peroxyde est une solution dans de l'eau pure ou dans de l'eau déminéralisée.
  7. Procédé suivant l'une des revendications 1 à 6, caractérisé en ce que l'on fait circuler en circuit fermé la solution de peroxyde et/ou on l'additionne de manière dosée en permanence.
  8. Procédé suivant l'une des revendications 1 à 7, caractérisée en ce que la durée de traitement est comprise entre 10 et 300 heures.
  9. Procédé suivant l'une des revendications 1 à 8, caractérisé en ce que l'on effectue le traitement dans une cuve ou dans un système ouvert à une température de la solution < 100° C ainsi que sous la pression atmosphérique et avec une vitesse de la solution le long de la surface de 0 à < 10m/s et en ce que l'on maintient constamment une concentration souhaitée de peroxyde par addition de manière dosée de peroxyde.
  10. Procédé suivant l'une des revendications 1 à 8, caractérisé en ce que l'on effectue le traitement dans un récipient ou un système fermé à une température > 100° C, de préférence de l'ordre de 100 à 200° C, sous une pression supérieure à 1 bar et en ce qu'il est prévu une purge de l'oxygène gazeux qui se forme par la décomposition thermique et catalytique du peroxyde en excès.
  11. Procédé suivant la revendication 10, caractérisé en ce que l'on effectue le traitement dans une plage de température de 120 à 180° C et dans une plage de pression de 5 à 15 bar, ainsi qu'à une vitesse de la solution le long de la surface de 0 à 10m/s.
  12. Procédé suivant l'une des revendications 1 à 11, caractérisé en ce que l'on revêt de l'oxyde la surface à traiter d'un système à l'état monté sur la face intérieure, soumise à l'eau, du système.
  13. Procédé suivant l'une des revendications 1 à 12, caractérisé en ce que l'on traite la surface d'un élément mouillé, par exemple du circuit primaire, d'une centrale nucléaire à refroidissement par de l'eau.
  14. Procédé suivant l'une des revendications 1 à 13, caractérisé en ce que l'on traite la surface pour la colorer.
EP97954726A 1996-12-06 1997-12-08 Traitement de surface de l'acier ou d'un alliage au nickel et acier ou alliage au nickel ainsi traites Expired - Lifetime EP0951582B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
CH03001/96A CH691479A5 (de) 1996-12-06 1996-12-06 Oberflächenbehandlung von Stahl.
CH300196 1996-12-06
PCT/EP1997/006839 WO1998024948A1 (fr) 1996-12-06 1997-12-08 Traitement de surface de l'acier ou d'un alliage au nickel et acier ou alliage au nickel ainsi traites

Publications (2)

Publication Number Publication Date
EP0951582A1 EP0951582A1 (fr) 1999-10-27
EP0951582B1 true EP0951582B1 (fr) 2004-05-19

Family

ID=4246409

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97954726A Expired - Lifetime EP0951582B1 (fr) 1996-12-06 1997-12-08 Traitement de surface de l'acier ou d'un alliage au nickel et acier ou alliage au nickel ainsi traites

Country Status (8)

Country Link
US (1) US6277213B1 (fr)
EP (1) EP0951582B1 (fr)
JP (1) JP3607705B2 (fr)
CA (1) CA2274072C (fr)
CH (1) CH691479A5 (fr)
DE (1) DE59711648D1 (fr)
ES (1) ES2221080T3 (fr)
WO (1) WO1998024948A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6633623B2 (en) * 2000-11-29 2003-10-14 General Electric Company Apparatus and methods for protecting a jet pump nozzle assembly and inlet-mixer
JP2003105557A (ja) * 2001-10-01 2003-04-09 Matsumoto Shika Univ 金属部材の酸化膜形成方法
GB0124846D0 (en) * 2001-10-16 2001-12-05 Unilever Plc Corrosion protection process
CN105483733A (zh) * 2015-12-08 2016-04-13 无锡华工薄板有限公司 一种带钢用酸洗槽的除氢系统

Family Cites Families (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE710733C (de) 1937-10-16 1941-09-19 Schering Ag Verfahren zum Beizen von Eisen und Eisenlegierungen
DE740432C (de) 1938-10-14 1943-10-20 Schering Ag Verfahren zum Beizen von Eisen und Eisenlegierungen
US2890974A (en) * 1957-12-02 1959-06-16 Fairchild Engine & Airplane Passivation of stainless steel alloys
DE1928307B2 (de) 1969-06-03 1971-10-21 Bad und verfahren zum glaenzen von werkstuecken mit ober flaechen aus eisen oder eisenlegierungen
NL164328C (nl) * 1970-04-02 1980-12-15 Stamicarbon Werkwijze voor het verhogen van de weerstand tegen cor- rosie van austenitische chroom-nikkelstalen, alsmede werkwijze voor de bereiding van ureum in apperatuur waarvan de weerstand tegen corrosie aldus is verhoogd.
US3888702A (en) * 1973-11-19 1975-06-10 Gen Motors Corp Hydrogen peroxide treatment of nickel surfaces for silicone rubber bonding
US4581074A (en) * 1983-02-03 1986-04-08 Mankina Nadezhda N Method for cleaning internal heat transfer surfaces of boiler tubes
JPS59157285A (ja) * 1983-02-25 1984-09-06 Hitachi Ltd マルテンサイト系ステンレス鋼の前処理法
JPH0658437B2 (ja) * 1984-11-06 1994-08-03 株式会社日立製作所 原子力プラントの放射能低減方法
DE3871143D1 (de) 1988-07-28 1992-06-17 Voest Alpine Stahl Verfahren zur chemischen nachbehandlung von stahlblechoberflaechen.
US4946518A (en) * 1989-03-14 1990-08-07 Motorola, Inc. Method for improving the adhesion of a plastic encapsulant to copper containing leadframes
DE4135029A1 (de) * 1990-10-23 1992-04-30 Nalco Chemical Co Verfahren zur kontrollierten passivierung der innenwaende eines kuehlkreislaufsystems aus kohlenstoffstahl
DE4424638A1 (de) * 1994-07-13 1996-04-11 Univ Dresden Tech Verfahren zur Herstellung von oxidischen Korrosionsschutzschichten auf hoch chromlegierten Stählen
EP0708295B1 (fr) * 1994-10-21 1999-01-07 Energy Support Corporation Appareil pour former des films de protection dans des conduites d'alimentation d'eau pour chaudière
US5532024A (en) * 1995-05-01 1996-07-02 International Business Machines Corporation Method for improving the adhesion of polymeric adhesives to nickel surfaces

Also Published As

Publication number Publication date
DE59711648D1 (de) 2004-06-24
ES2221080T3 (es) 2004-12-16
JP2000514565A (ja) 2000-10-31
WO1998024948A1 (fr) 1998-06-11
CH691479A5 (de) 2001-07-31
US6277213B1 (en) 2001-08-21
CA2274072A1 (fr) 1998-06-11
JP3607705B2 (ja) 2005-01-05
EP0951582A1 (fr) 1999-10-27
CA2274072C (fr) 2005-04-19

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