EP0246986B1 - Verfahren zur Herstellung von Bändern aus teilweise rekristallisiertem Zircaloy 2 oder Zircaloy 4 und nach diesem Verfahren hergestellte Bänder - Google Patents

Verfahren zur Herstellung von Bändern aus teilweise rekristallisiertem Zircaloy 2 oder Zircaloy 4 und nach diesem Verfahren hergestellte Bänder Download PDF

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Publication number
EP0246986B1
EP0246986B1 EP87420129A EP87420129A EP0246986B1 EP 0246986 B1 EP0246986 B1 EP 0246986B1 EP 87420129 A EP87420129 A EP 87420129A EP 87420129 A EP87420129 A EP 87420129A EP 0246986 B1 EP0246986 B1 EP 0246986B1
Authority
EP
European Patent Office
Prior art keywords
strip
last
intermediate annealing
heat treatment
zircaloy
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
Application number
EP87420129A
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English (en)
French (fr)
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EP0246986A1 (de
Inventor
Gérard Bunel
Daniel Charquet
Max Dombre
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.)
Compagnie Europeenne du Zirconium Cezus SA
Original Assignee
Compagnie Europeenne du Zirconium Cezus SA
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 Compagnie Europeenne du Zirconium Cezus SA filed Critical Compagnie Europeenne du Zirconium Cezus SA
Publication of EP0246986A1 publication Critical patent/EP0246986A1/de
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Publication of EP0246986B1 publication Critical patent/EP0246986B1/de
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C21—METALLURGY OF IRON
    • C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
    • C21D9/46—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for sheet metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C16/00—Alloys based on zirconium

Definitions

  • the present invention relates to a process for manufacturing a zirconium alloy strip for nuclear use "Zircaloy 2" (specification ASTM B52, grades R 60802 and R 60812) or "Zircaloy 4" (same specification, grades R 60804 and R 60814 ), resulting for this strip in a "restored” state corresponding to a compromise of mechanical strength and ductility.
  • “restored” state one indicates here a heat treated state without there being complete recrystallization as in an annealed state, in which the stresses due to hardening are partly at least relaxed.
  • the present invention also relates to the strip obtained.
  • Zircaloy 2 or 4 strip of thickness typically between 0.3 and 0.9 mm, having both: a good elastic limit at the operating temperature, and good ductility at room temperature (20 ° C) identified by the elongation distributed in the long direction and also in the transverse direction of the strip - so as to behave well vis-à-vis conformations of this manufacture of grids.
  • distributed elongation is the maximum elongation of a test piece during a tensile test, before the necking begins.
  • the characteristics thus sought for this strip are typically: E O , 2 at 315 ° C ⁇ 250 MPa A% distributed long direction sens 4 and if possible * 5 A% distributed direction across k 4 and if possible * 5.
  • the deformation rates (%) corresponding to each rolling or rolling sequence are calculated according to the formula: (1 - final thickness / initial thickness) x 100.
  • the intermediate deformation rates and the intermediate annealing conditions are chosen so that, after each of these intermediate anneals, a just recrystallized state is obtained, while avoiding a grain enlargement, which makes it possible to obtain an extremely equiaxed grain. end by annealing.
  • the rate of deformation and the conditions of final heat treatment are themselves chosen, and these are particularly important points, so that this treatment results in partial recrystallization of the strip.
  • Micrographically the strip then comprises very fine grains obtained by the last intermediate annealing and elongated by the last rolling, grains which often have a length of between 10 and 20 microns.
  • Electron microscope examinations show that in these elongated grains there are locally sub-grains a few microns in diameter which are fully recrystallized, while the surrounding matrix has remained hardened.
  • the fully recrystallized subgrains represent a volume of between 20 and 40% of the total.
  • the final heat treatment is preferably carried out at the runway between 600 and 625 ° C., the constant speed of the strip ensuring maintenance of 2 to 5 min at the processing temperature. And, more preferably, independently of, or in combination with the previous measurement, the strip is laminated between the last intermediate annealing and the final heat treatment with a deformation rate of 35 to 45%.
  • the deformations and the two preceding intermediate anneals also play a role in obtaining and improving the surprising compromise in the characteristics of the strip of the invention.
  • the adjustment of these re intermediate baking is then particularly desirable (obtaining states that are just recrystallized to 100%), and it is preferable to tighten the conditions of duration and temperature of these last two intermediate anneals: each then comprising for the strip a stay of 1 to 3 min between 680 and 720 ° C, whether this is the general case or the process already improved at the level of the final heat treatment or the final deformation rate.
  • An optimum consists in making the last two intermediate anneals as well as the final heat treatment at the constant speed parade, each of these two intermediate anneals is then preferably carried out between 680 and 720 ° C with a scrolling speed ensuring a maintenance of 1 3 min at processing temperature.
  • the final heat treatment is thus preferably carried out in the procession, under a protective atmosphere or possibly in air, and it is then followed either by a pickling, or by a slight brightening of the surface itself followed by a pickling.
  • the protective gas is preferably under slight overpressure in the heating chamber, and at the exit of this heating chamber, the strip enters an airlock or a cooling chamber where it is cooled below 300 ° C by blowing cold inert gas .
  • the subject of the invention is also the strip of the invention which, with its composition and its particular mechanical characteristics, is distinguished in particular from the strips previously known by a particularly fine grain, this grain being in cross section finer than the ASTM index. "11" with partial recrystallization affecting 20 to 40% of the volume.
  • Zircaloy 4 strip (nominal composition: Sn 1.5% - Fe 0.2% - Cr 0.1% - Zr the balance), originating from a flow X of oxygen content 1290 ppm and of carbon 90 ppm, laminated to thickness 0.44 mm.
  • the final deformation rate was 43% and the final heat treatment was done in static under vacuum as it was then usual at 460 ° C for 24 h, the intermediate anneals themselves being 3 to 4 h at 650/700 ° C.
  • the heat-treated samples have a recrystallized grain deformed in the long direction, corresponding on cross section to the ASTM index "10".
  • the parade heat treatments were carried out in an oven operating with a protective argon atmosphere.
  • the running speed of the strip was chosen so as to obtain the desired temperature residence time for each portion of the strip treated.
  • Each of the three intermediate anneals at the parade gives for the strip, according to examinations carried out with the electron microscope, a just state recrystallized with very fine grain.
  • the size of the fine grain recrystallized at the last intermediate annealing measured on cross section is from “11" to "11.5" ASTM.
  • the final recrystallization, assessed with the electron microscope, is very fine and affects 20 to 40% of the volume.
  • this strip is too stiff (E O , 2 strong cross) and difficult to conform (see also A% distributed across).
  • This strip is a little less stiff and a little easier to conform than that of the 2nd series of tests.
  • the method of the invention therefore allows precise quality adjustments, with particularly reproducible results in the case of parade treatments.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Heat Treatment Of Sheet Steel (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Heat Treatment Of Strip Materials And Filament Materials (AREA)
  • Metal Rolling (AREA)

Claims (6)

1. Verfahren zur Herstellung von Bändern aus Zircaloy 2 oder 4 mit einem Sauerstoffgehalt von 900-1600 ppm, in dem ein Block durch Heißkneten transformiert und dann kalt mit Zwischenglühungen in Bänder laminiert wird, dadurch gekennzeichnet, daß
a) bei jeder der beiden letzten Zwischenglühungen die Bänder 0,5-10 min zwischen 650-750°C behandelt werden;
b) die Bänder nach dem letzten Laminieren einer thermischen Endbehandlung von 1,5-7 min zwischen 590 und 630°C unterworfen werden;
c) die Bänder mit folgenden Verformungssätzen zwischen aufeinander folgenden Glühungen oder thermischer Behandlung laminiert werden:
ci) vor der vorletzten Zwischenglühung: 20-55%,
c2) zwischen den beiden letzten Zwischenglühungen: 30-55%,
c3) zwischen der letzten Zwischenglühung und der thermischen Endbehandlung: 30-55%.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß die thermische Endbehandlung im Vorbeilaufen zwischen 600 und 625°C durchgeführt wird, wobei die konstante Geschwindigkeit der Bänder eine Verweilzeit von 2-5 min bei der Behandlungstemperatur gewährleistet.
3. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß die Bänder zwischen der letzten Zwischenglühung und der thermischen Endbehandlung mit einem Verformungssatz von 35-45% laminiert werden.
4. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß in jeder der beiden letzten Zwischenglühungen die Bänder 1-3 min zwischen 680 und 720°C behandelt werden.
5. Verfahren nach Anspruch 2, dadurch gekennzeichnet, daß jede der beiden letzten Zwischenglühungen im Vorbeilaufen zwischen 680 und 720°C durchgeführt wird, wobei die konstante Geschwindigkeit der Bänder eine Verweilzeit von 1-3 min bei der Behandlungstemperatur gewährleistet.
6. Bänder aus Zircaloy 2 oder 4, erhältlich im Verfahren nach einem der Ansprüche 1 bis 5, mit einem Sauerstoffgehalt von 900-1600 ppm und mechanischen Eigenschaften, die den drei Bedingungen genügen:
EO.2 bei 315°C ≥ 250 MPa,
A% "längs" verteilt bei 20°C ≥ 4,
A% "quer" verteilt bei 20°C ≥ 4,
dadurch gekennzeichnet, daß sie im Querschnitt ein feineres Korn als der ASTM-Index "11" und eine Teilrekristallisation, die 20-40% des Volumens betrifft, aufweisen.
EP87420129A 1986-05-21 1987-05-18 Verfahren zur Herstellung von Bändern aus teilweise rekristallisiertem Zircaloy 2 oder Zircaloy 4 und nach diesem Verfahren hergestellte Bänder Expired EP0246986B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8607760A FR2599049B1 (fr) 1986-05-21 1986-05-21 Procede de fabrication d'un feuillard en zircaloy 2 ou zircaloy 4 partiellement recristallise et feuillard obtenu
FR8607760 1986-05-21

Publications (2)

Publication Number Publication Date
EP0246986A1 EP0246986A1 (de) 1987-11-25
EP0246986B1 true EP0246986B1 (de) 1989-11-23

Family

ID=9335806

Family Applications (1)

Application Number Title Priority Date Filing Date
EP87420129A Expired EP0246986B1 (de) 1986-05-21 1987-05-18 Verfahren zur Herstellung von Bändern aus teilweise rekristallisiertem Zircaloy 2 oder Zircaloy 4 und nach diesem Verfahren hergestellte Bänder

Country Status (7)

Country Link
US (2) US4775428A (de)
EP (1) EP0246986B1 (de)
JP (1) JPS6324048A (de)
KR (1) KR920000526B1 (de)
DE (1) DE3761023D1 (de)
ES (1) ES2011818B3 (de)
FR (1) FR2599049B1 (de)

Families Citing this family (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2548773B2 (ja) * 1988-06-06 1996-10-30 三菱重工業株式会社 ジルコニウム基合金とその製造方法
US5194101A (en) * 1990-03-16 1993-03-16 Westinghouse Electric Corp. Zircaloy-4 processing for uniform and nodular corrosion resistance
FR2664907B1 (fr) * 1990-07-17 1997-12-05 Cezus Zirconium Cie Europ Procede de fabrication d'une tole ou feuillard en zircaloy de bonne formabilite et feuillards obtenus.
FR2672057B1 (fr) * 1991-01-30 1994-08-12 Cezus Co Europ Zirconium Procede de fabrication de toles ou tubes en zircaloy 2 ou en zircaloy 4.
FR2673198B1 (fr) * 1991-02-22 1993-12-31 Cezus Cie Europ Zirconium Procede de fabrication d'une bande ou tole en zircaloy 2 ou 4 et produit obtenu.
US5156689A (en) * 1991-05-20 1992-10-20 Westinghouse Electric Corporation Near net shape processing of zirconium or hafnium metals and alloys
US5188676A (en) * 1991-08-23 1993-02-23 General Electric Company Method for annealing zircaloy to improve nodular corrosion resistance
US5266131A (en) * 1992-03-06 1993-11-30 Westinghouse Electric Corp. Zirlo alloy for reactor component used in high temperature aqueous environment
FR2716897B1 (fr) * 1994-03-02 1996-04-05 Cezus Co Europ Zirconium Procédé de fabrication d'un produit plat en alliage de zirconium ou en alliage de hafnium comprenant une poursuite du laminage à chaud après rechauffage par infrarouges et ses utilisations .
FR2729000A1 (fr) * 1994-12-29 1996-07-05 Framatome Sa Procede de fabrication d'un tube pour assemblage de combustible nucleaire et tubes conformes a ceux ainsi obtenus
US6544361B1 (en) 1999-02-15 2003-04-08 Framatome Anp Process for manufacturing thin components made of zirconium-based alloy and straps thus produced
FR2789795B1 (fr) * 1999-02-15 2001-05-25 Framatome Sa Procede de fabrication d'elements minces en alliage a base de zirconium et plaquettes ainsi realisees
FR2791804B1 (fr) * 1999-03-30 2001-06-15 Framatome Sa Procede de fabrication d'elements minces en alliage a base de zirconium et plaquettes ainsi realisees
SE525808C2 (sv) * 2002-10-30 2005-05-03 Westinghouse Atom Ab Förfarande, användning och anordning avseende kapslingrör för kärnbränsle samt en bränslepatron för en nukleär tryckvattenreaktor
US7625453B2 (en) * 2005-09-07 2009-12-01 Ati Properties, Inc. Zirconium strip material and process for making same
SE530783C2 (sv) 2007-01-16 2008-09-09 Westinghouse Electric Sweden Spridargaller för positinering av bränslestavar

Family Cites Families (16)

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Publication number Priority date Publication date Assignee Title
US3567522A (en) * 1965-12-15 1971-03-02 Westinghouse Electric Corp Method of producing zirconium base alloys
US3645800A (en) * 1965-12-17 1972-02-29 Westinghouse Electric Corp Method for producing wrought zirconium alloys
CA1025335A (en) * 1972-09-05 1978-01-31 Ake S.B. Hofvenstam Method of making tubes and similar products of a zirconium alloy
FR2219978B1 (de) * 1973-03-02 1976-04-30 Commissariat Energie Atomique
FR2307884A1 (fr) * 1975-04-15 1976-11-12 Exxon Nuclear Co Inc Procede pour le traitement d'un metal comprenant essentiellement du zirconium et metal obtenu
SU817089A1 (ru) * 1979-06-04 1981-03-31 Государственный Научно-Исследовательскийи Проектно-Конструкторский Институтсплавов И Обработки Цветных Металлов Способ обработки циркони и егоСплАВОВ
US4521259A (en) * 1980-11-03 1985-06-04 Teledyne Industries, Inc. Nitrogen annealing of zirconium and zirconium alloys
SE426891B (sv) * 1981-07-07 1983-02-14 Asea Atom Ab Sett att tillverka kapselror av zirkoniumbaserad legering forbrenslestavar till kernreaktorer
EP0071193B1 (de) * 1981-07-29 1988-06-01 Hitachi, Ltd. Verfahren zur Herstellung einer Legierung auf der Basis von Zirkonium
JPS5822363A (ja) * 1981-07-30 1983-02-09 Mitsubishi Keikinzoku Kogyo Kk 超塑性アルミニウム合金板の製造方法
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FR2540140B3 (fr) * 1983-02-01 1985-10-18 Cezus Co Europ Zirconium Procede de trempe en milieu aqueux d'alliages de zirconium
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FR2575762B1 (fr) * 1985-01-10 1989-03-03 Fragema Framatome & Cogema Procede de fabrication de plaquettes en alliage de zirconium
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US4717428A (en) * 1985-08-02 1988-01-05 Westinghouse Electric Corp. Annealing of zirconium based articles by induction heating

Also Published As

Publication number Publication date
FR2599049B1 (fr) 1988-07-01
KR920000526B1 (ko) 1992-01-14
ES2011818B3 (es) 1990-02-16
DE3761023D1 (en) 1989-12-28
KR870011259A (ko) 1987-12-22
EP0246986A1 (de) 1987-11-25
FR2599049A1 (fr) 1987-11-27
JPS6410590B2 (de) 1989-02-22
US4775428A (en) 1988-10-04
JPS6324048A (ja) 1988-02-01
US4881992A (en) 1989-11-21

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