EP1133579B1 - Procede pour produire une couche protectrice sur un acier martensitique et utilisation de l'acier pourvu de ladite couche protectrice - Google Patents

Procede pour produire une couche protectrice sur un acier martensitique et utilisation de l'acier pourvu de ladite couche protectrice Download PDF

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Publication number
EP1133579B1
EP1133579B1 EP99952596A EP99952596A EP1133579B1 EP 1133579 B1 EP1133579 B1 EP 1133579B1 EP 99952596 A EP99952596 A EP 99952596A EP 99952596 A EP99952596 A EP 99952596A EP 1133579 B1 EP1133579 B1 EP 1133579B1
Authority
EP
European Patent Office
Prior art keywords
steel
protective layer
martensitic
temperature
melt
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
EP99952596A
Other languages
German (de)
English (en)
Other versions
EP1133579A1 (fr
Inventor
Heike Glasbrenner
Kathleen Stein-Fechner
Olaf Wedemeyer
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.)
Forschungszentrum Karlsruhe GmbH
Original Assignee
Forschungszentrum Karlsruhe GmbH
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 Forschungszentrum Karlsruhe GmbH filed Critical Forschungszentrum Karlsruhe GmbH
Publication of EP1133579A1 publication Critical patent/EP1133579A1/fr
Application granted granted Critical
Publication of EP1133579B1 publication Critical patent/EP1133579B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • C23C2/00—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor
    • C23C2/04—Hot-dipping or immersion processes for applying the coating material in the molten state without affecting the shape; Apparatus therefor characterised by the coating material
    • C23C2/12—Aluminium or alloys based thereon

Definitions

  • the invention relates to a method for producing a Protective layer on a martensitic steel according to the first Claim and the use of the provided with the protective layer Steel according to the fifth claim.
  • the object of the invention is a further method propose to create a protective layer.
  • the protective layer should be suitable for martensitic steels.
  • the one with the Protective coated martensitic steel is said to be used in nuclear fusion experiments be used, the protective layer Diffusion barrier for the radioactive hydrogen isotope Represents tritium.
  • the steel provided with the protective layer must in this area of application compared to the liquid used here Brood metals such as B. liquid lithium or lithium lead (Pb17% Li).
  • a martensitic steel in particular a Chromium steel, preferably with 8 to 10% chromium, or an unalloyed one or alloy spring steel with the protective layer.
  • the martensitic steel is under a protective gas atmosphere in a melt of aluminum or an aluminum alloy such as B. 90% Al and 10% Si immersed.
  • a Pure aluminum melt preferred.
  • protective gas in particular the noble gases argon and helium, optionally in Combination with a reducing gas like hydrogen.
  • the temperature of the melt is preferably in a temperature range between the melting point and a maximum of 100 ° C above the Melting point.
  • a temperature of 700 ° C is for pure aluminum well suited.
  • the dipping time should be the thickness of the one to be coated Item made of martensitic steel approximately proportional his. Diving times in the range between 5 seconds and 2 minutes are generally well suited.
  • the martensitic steel is then removed from the melt and under the protective gas atmosphere, preferably with natural Cooling rate to a temperature between 100 ° C and cooled to room temperature.
  • the martensitic steel becomes hot isostatic at one Pressure of at least 1500 bar at the austenitizing temperature (Aci final temperature) pressed.
  • the austenitizing temperature is 8 to 10% chromium steels between 1040 ° C and 1075 ° C.
  • the maximum applicable pressure is usually from apparatus Reasons limited to approx. 3000 bar.
  • everyone martensitic components of the steel converted into austenite.
  • the holding time in hot isostatic pressing corresponds to Holding time at austenitizing temperature and should be for 8 to 10 % chromium steels are between 30 and 40 minutes.
  • An approximately 100 to 200 ⁇ m thick protective layer is formed.
  • the steel becomes one Subjected to hardening.
  • the steel is known per se Way quenched and then tempered. Starting can be done in Dependence on the type of steel, for example at a temperature of 750 ° C and a holding time of 1 to 2 hours become. This step will make the martensitic state restored with the desired ductility.
  • the martensitic base body an iron / chrome / aluminum mixed crystal layer which is approx. 100 to 200 ⁇ m thick and its aluminum content is approx. 30% in the areas near the surface, the aluminum content decreases in the direction of the base body.
  • the mixed crystal layer has essentially the same Ductility like the martensitic body.
  • the surface the protective layer is covered by a ceramic layer approx. 1 ⁇ m thick Layer formed from alumina.
  • a major advantage of Invention is that in the event of mechanical damage to the top Aluminum oxide layer in an oxidizing atmosphere can be replicated.
  • the protective layer proves self-healing.
  • Another advantage is that as a result of hot isostatic pressing the pore size and number the pores are greatly reduced.
  • the protective layer turns out as an effective diffusion barrier against hydrogen; the tritium diffusion is compared to uncoated steels reduced by a factor of approx. 1000.
  • the protective layer is also almost against the corrosive attack of liquid metals inert.
  • MANET II is composed as follows: C 0, 10 to 0.11 Si 0.14 to 0.28 Mn 0.75 to 0.96 P 0.003 to 0.007 S 0.004 to 0.005 Cr 10.3 to 10.4 V 0.19 to 0.21 al 0.004 to 0.012 Cu 0.007 to 0.10 B 0.0072 to 0.0089 N 0.027 to 0.032 Ni 0.62 to 0.68 Mo 0.56 to 0.61 Nb 0.14 to 0.16 Zr 0.007 to 0.028 Rest: iron
  • the surface of the steel parts to be coated was initially cleaned by sandblasting. Then the parts in Acetone and ethanol cleaned. To better wettability with to reach the aluminum melt, a flux was created from a saturated saline solution (KCl, NaCl and Na3AlF6 in Ratio 5: 4: 1) applied.
  • the parts prepared in this way were dried before being placed in a box with a protective gas atmosphere (argon with 5% hydrogen), in which there is a crucible with the melt was infiltrated.
  • the temperature of the pure aluminum melt was 700 ° C.
  • the parts were placed in the for 30 seconds Submerged aluminum melt and then under the Protective gas atmosphere cooled to room temperature. after the steel parts coated with aluminum were cooled removed from the box by a lock system.
  • the parts were then placed in a HIP system.
  • the system was first evacuated and then with Ar 4.8 flooded. Then the temperature and pressure were increased at the same time, up to the austenitizing temperature of 1075 ° C and 3000 bar pressure were reached. After a holding time of 0.5 hours the system was switched off, after which the parts with approx. 10 to Cooled 20 K / min at constant pressure. This cooling rate is sufficient to ensure the formation of martensite, d. that is, to harden the parts.
  • the subsequent tempering treatment also took place in the HIP plant. Alternatively, one could other oven can be used.
  • the steel parts were at one Leave the temperature at 750 ° C for 2 hours. Even though the starting step can in principle be carried out without pressure a pressure of 3000 in the HIP system when starting maintain cash. The HIP system was then switched off and the steel parts cooled.

Landscapes

  • 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)
  • Coating By Spraying Or Casting (AREA)
  • Heat Treatment Of Articles (AREA)
  • Heat Treatment Of Steel (AREA)

Claims (5)

  1. Procédé de production d'une couche protectrice sur un acier martensitique comportant les étapes suivantes :
    a) immersion de l'acier martensitique dans une solution d'aluminium ou d'un alliage d'aluminium sous une atmosphère de gaz protecteur,
    b) retrait de l'acier de la masse fondue et refroidissement allant de 100°C à la température ambiante sous l'atmosphère de gaz protecteur ;
    c) pressage isostatique à chaud (HIP) de l'acier à une pression d'au moins 1500 bars à la température d'austénitisation ;
    d) trempage et adoucissement de l'acier.
  2. Procédé selon la revendication 1, avec de l'acier à 8 à 10 % de chrome.
  3. Procédé selon la revendication 1 ou 2 avec une température de la masse fondue située dans un intervalle compris entre le point de fusion et/ou au maximum 100°C au-dessus du point de fusion.
  4. Procédé selon la revendication 1 avec une durée d'immersion située dans un intervalle compris entre 5 secondes et 2 minutes.
  5. Utilisation de l'acier muni de la couche protectrice selon l'une des revendications 1 à 4 comme matériau de structure pour expériences de fusion nucléaire dans laquelle l'acier est mis en contact avec du tritium et/ou un métal liquide.
EP99952596A 1998-11-19 1999-10-18 Procede pour produire une couche protectrice sur un acier martensitique et utilisation de l'acier pourvu de ladite couche protectrice Expired - Lifetime EP1133579B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19853285A DE19853285C1 (de) 1998-11-19 1998-11-19 Verfahren zur Herstellung einer Schutzschicht auf einem martensitischen Stahl und Verwendung des mit der Schutzschicht versehenen Stahls
DE19853285 1998-11-19
PCT/EP1999/007881 WO2000031312A1 (fr) 1998-11-19 1999-10-18 Procede pour produire une couche protectrice sur un acier martensitique et utilisation de l'acier pourvu de ladite couche protectrice

Publications (2)

Publication Number Publication Date
EP1133579A1 EP1133579A1 (fr) 2001-09-19
EP1133579B1 true EP1133579B1 (fr) 2002-09-11

Family

ID=7888280

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99952596A Expired - Lifetime EP1133579B1 (fr) 1998-11-19 1999-10-18 Procede pour produire une couche protectrice sur un acier martensitique et utilisation de l'acier pourvu de ladite couche protectrice

Country Status (5)

Country Link
EP (1) EP1133579B1 (fr)
JP (1) JP2002530536A (fr)
AT (1) ATE223976T1 (fr)
DE (2) DE19853285C1 (fr)
WO (1) WO2000031312A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4990449B2 (ja) * 2001-07-27 2012-08-01 新日本製鐵株式会社 高強度自動車部材用アルミめっき鋼板及びこれを使用した自動車用部材
JP4700263B2 (ja) * 2003-04-25 2011-06-15 新日本製鐵株式会社 高圧水素ガス用タンク及び配管
DE102004010689B3 (de) 2004-02-27 2005-06-30 Schott Ag Absorber mit einer strahlungsselektiven Absorberbeschichtung und Verfahren zu seiner Herstellung
DE102005030231B4 (de) 2005-06-29 2007-05-31 Forschungszentrum Karlsruhe Gmbh Verfahren zum Aufbringen einer hochtemperaturgeeigneten FeCrAl-Schutzschicht, Hüllrohr mit einer derartig aufgebrachten Schutzschicht und Verwendung eines solchen Hüllrohrs
DE102016107152B4 (de) * 2016-04-18 2017-11-09 Salzgitter Flachstahl Gmbh Bauteil aus pressformgehärtetem, auf Basis von Aluminium beschichtetem Stahlblech und Verfahren zur Herstellung eines solchen Bauteils und dessen Verwendung
US10450668B2 (en) 2017-04-11 2019-10-22 Savannah River Nuclear Solutions, Llc Development of a passivated stainless steel surface
CN116968397B (zh) * 2023-09-25 2023-12-15 上海核工程研究设计院股份有限公司 一种防氚渗透的层状复合材料及其制备方法

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1057188A (en) * 1964-07-20 1967-02-01 Murex Welding Processes Ltd An improved method of applying a metal coating to wires, tubes or strips
DE3145941C2 (de) * 1981-11-20 1983-12-01 MTU Motoren- und Turbinen-Union München GmbH, 8000 München Verfahren zur Steigerung der Zuverlässigkeit von bereits kriechbeanspruchten beschichteten Bauteilen von Turbomaschinen
JPS5950177A (ja) * 1982-09-16 1984-03-23 Kobe Steel Ltd 密着性に優れた金属表面処理法
JPS61250130A (ja) * 1985-04-26 1986-11-07 Mitsubishi Motors Corp 繊維強化複合材料の製法
US5447754A (en) * 1994-04-19 1995-09-05 Armco Inc. Aluminized steel alloys containing chromium and method for producing same
JPH08134595A (ja) * 1994-11-11 1996-05-28 Nippon Steel Corp 耐応力腐食割れ特性に優れた高強度ステンレス鋼板
JPH10175081A (ja) * 1996-12-16 1998-06-30 Sumitomo Light Metal Ind Ltd アルミニウム合金クラッド材の製造方法

Also Published As

Publication number Publication date
EP1133579A1 (fr) 2001-09-19
WO2000031312A1 (fr) 2000-06-02
JP2002530536A (ja) 2002-09-17
DE59902693D1 (de) 2002-10-17
ATE223976T1 (de) 2002-09-15
DE19853285C1 (de) 2000-06-15

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