EP0198570A2 - Verfahren zur Herstellung dünnwandiger Röhren aus einer Zirkonium-Niob-Legierung - Google Patents

Verfahren zur Herstellung dünnwandiger Röhren aus einer Zirkonium-Niob-Legierung Download PDF

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Publication number
EP0198570A2
EP0198570A2 EP86300259A EP86300259A EP0198570A2 EP 0198570 A2 EP0198570 A2 EP 0198570A2 EP 86300259 A EP86300259 A EP 86300259A EP 86300259 A EP86300259 A EP 86300259A EP 0198570 A2 EP0198570 A2 EP 0198570A2
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EP
European Patent Office
Prior art keywords
niobium
zirconium
process according
temperature
tube shell
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Granted
Application number
EP86300259A
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English (en)
French (fr)
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EP0198570B1 (de
EP0198570A3 (en
Inventor
George Paul Sabol
Samuel Gilbert Mcdonald Iii
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CBS Corp
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Westinghouse Electric Corp
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Application filed by Westinghouse Electric Corp filed Critical Westinghouse Electric Corp
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Publication of EP0198570A3 publication Critical patent/EP0198570A3/en
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    • 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
    • C21D9/08—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for tubular bodies or pipes
    • 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

Definitions

  • This invention relates to a process for fabricating thin-walled tubing such as nuclear fuel cladding, from a zirconium-niobium alloy such that the alloys of the. resultant products have a particular microstructure which enables the material to resist corrosion in high temperature aqueous environments.
  • Zero-Nb alloys have been traditionally of interest to the nuclear industry because of their high strengths. It is this feature, in conjunction with reasonably good corrosion resistance, which ultimately led to the selection of the alloy of zirconium containing 2.5 per cent by weight niobium, as the standard pressure- tube material for present generation Canadian Deuterium Uranium (CANDU) reactors. Although it was originally believed that the zirconium-niobium alloys had inferior resistance to irradiation enhanced corrosion relative to existing alloys, such as Zircaloy-2 or Zircaloy-4, it ultimately became apparent that they actually had superior in-pile corrosion properties when properly heat treated, as described by J. E. LeSurf, ASTM STP-458, p. 286. As a result of this finding, there has been increasing interest in zirconium-niobium alloys as potential fuel cladding materials in future generation, high performance, light water reactors.
  • zirconium-niobium alloys can be fabricated into thin-walled tubing, of about 0.040 inch or less in wall thickness, which exhibits excellent corrosion resistance, by a process that does not require extensively long final annealing times, by the use of relatively low temperature anneals between cold working steps and a final low temperature anneal.
  • thin-walled tubing can be fabricated that has a microstructure where second phase beta-niobium particles are homogeneously dispersed in the zirconium matrix in extremely fine particle size to provide excellent corrosion resistance of the resultant article under both in-pile and out-of-pile conditions.
  • the present invention resides in a process for fabricating thin-walled tubing from a zirconium-niobium alloy containing from 1 to 2.5 per cent by weight niobium as homogeneously dispersed finely divided particles characterized by beta-treating a zirconium-niobium alloy billet containing from 1 to 2.5 per cent by weight niobium; extruding said beta-treated billet at a temperature no higher than 650°C to form a tube shell; further deforming said tube shell by cold working the same in a plurality of cold working stages; annealing said tube shell, between each of said stages of cold working, at a temperature below 650°C; and final annealing the resultant tubing at a temperature below 600°C, so as to produce a microstructure of the material having niobium particles of a size below about 800 angstroms homogeneously dispersed therein.
  • the fabrication of thin-walled tubing from a zirconium-niobium alloy is effected according to the present invention with the production of tubing exhibiting excellent corrosion resistance and resistance to hydride formation.
  • zirconium alloys containing 1.0 per cent by weight and 2.5 per cent by weight niobium.
  • the zirconium-niobium alloys may contain a minor amount, up to 0.5 per cent by weight of a third element, such as copper, iron, molybdenum, nickel, tungsten, vanadium and chromium.
  • a third element such as copper, iron, molybdenum, nickel, tungsten, vanadium and chromium.
  • An example of such an alloy is one containing zirconium with 2.5 per cent niobium and 0.5 per cent copper.
  • the alloys are first subjected to a beta-treatment by heating the alloy to from 950-1000°C and water-quenching the same to a temperature below the alpha + beta to alpha transus temperature.
  • the billet is then prepared for extrusion by drilling an axial hole along the center line of the billet, machining the outside diameter to desired dimensions, and applying a lubricant to the surfaces of the billet.
  • the billet diameter is then reduced by extrusion at a lower than conventional temperature, below 700°C, through a frustoconical die and over a mandrel.
  • a beta-anneal of the extruded tube shell may then be effected, depending upon the alloy, by heating to from 850-1050°C, followed by rapid cooling.
  • the billet may then be cold worked by pilgering, at a source of primary fabrication, to reduce the wall thickness and outside diameter.
  • This intermediate production is called a TREX (Tube Reduced Extrusion), which may then be sent to a tube mill for fabrication by cold working, intermediate low temperature annealing, and a final anneal under the fabricating steps of the present invention to produce the desired thin-walled tubing.
  • the material is preferably cold worked by pilgering, and 3 to 5 stages of cold working effected, preferably 3 to 4 stages.
  • the present invention produces thin-walled zirconium alloy tubing wherein the alloying elements are homogeneously dispersed throughout the zirconium in a finely divided state.
  • the particles, homogeneously dispersed are of an average particle size below 800 angstroms, and preferably the average particle size is below about 500 angstroms.
  • niobium-containing zirconium alloy (A) ingot containing 1.0 per cent by weight niobium and the balance zirconium, was conventionally broken down in billets of about six inches in diameter (Step 1).
  • a six-inch diameter billet was then given a beta treatment, Step 2, which comprised holding the billet in a furnace at about 968-996°C (1775-1825°F) for about fifteen minutes and then water quenching the billet.
  • the beta-treated billet was machined, bore-holed and inspected in preparation for extrusion.
  • the hollow niobium-containing zirconium alloy billet was then heated to about 649°C (1200°F) and extruded (Step 3) to a hollow tube having an outside diameter of 2.5 inches and a wall thickness of 0.43 inch.
  • the extruded hollow tube was beta-annealed (Step 4) at 954°C (17500F) for a period of fifteen minutes in preparation for a first cold working step (a pilgering reduction), (Step 5).
  • the beta-annealed extrusion was pilgered in Step 5 to a TREX having an outside diameter of 1.75 inches and a wall thickness of 0.3 inch.
  • the TREX was then annealed, (Step 6), at 500°C (932°F) for a period of 8 hours. Following the annealing of the TREX, the same was then cold pilgered to a tube shell having an outside diameter of 1.25 inches and a wall thickness of 0.16 inch, (Step 7).
  • the tube shell was then further annealed and cold worked according to the following sequence.
  • the tube shell was annealed, (Step 8), at about 524°C (975°F) for 7.5 hours and further cold pilgered, (Step 9), to reduce the tube shell to one having an outside diameter of 0.875 inch and a wall thickness of 0.085 inch.
  • This tube shell was again annealed at about 524°C (975°F) for 7.5 hours, (Step 10).
  • the annealed tube shell was again further cold pilgered, (Step 11), to give a tube shell having an outside diameter of 0.602 inch and a wall thickness of 0.045 inch.
  • the tube was then subjected to a final anneal at about 427°C (800°F) for 4 hours, (Step 14).
  • the cold working anneal for the tubes formed from composition B were effected at about 580°C (1076°F) for 8 hours (rather than 524°C (975°F) for 7.5 hours as with A).
  • the remaining treatment steps, including the final anneal were the same as those used with composition A.
  • the TREX was then annealed in Step 6 at 600°C (1112°F) for a period of 8 hours.
  • the material was therefore subjected to an additional anneal for 3 hours at about 685°C (1265°F) and the material then subjected to Step 7 with successful pilgering.
  • the first cold working anneal, Step 8 was carried out at about 593°C (1100 0 F) for a period of 8 hours.
  • Step 13 the tube was subjected to a final anneal, Step 14, for 7.5 hours at about 480°C (896°F).
  • niobium-containing zirconium alloy tubes of the present invention have in-pile corrosion resistance superior to that of Zircaloy-4. This is a property which, in the past, has been attributed only to "heat treated” 2.5% Nb-zirconium alloys (see “The Effect of Aging and Irradiation on the Corrosion of Zr-2.5 wt % Nb", V. F. Urbanic, J. E. LeSurf and A. B. Johnson, Jr.: Corrosion 31 (1975) 15).
  • FIG. 2 Further evidence of the superiority of the tubing prepared according to the present invention is illustrated in Figure 2 where two groups of corrosion data are presented for a zirconium alloy containing 1 per cent by weight niobium.
  • the first group of data (dash lines: 350, 400 and 450°C) were reported for sheet material which was fabricated via standard Russian processing techniques (see A. A. Kiselev, et al., AECL-1724, 1963).
  • the second group of data solid lines: 360 and 427°C
  • the superiority of the present tubing is demonstrated by the fact that the same exhibits lower weight gains at 360 and 427°C than the Russion material does, even though the latter was exposed at lower corrosion temperatures 350 and 400°C respectively.
  • the present processing provides uniform distribution of very fine precipitate particles in the microstructure of niobium-containing zirconium alloys.
  • the microstructure of the fully annealed tubing is illustrated in Figures 3A, B, C and D for composition "A”; 4A, B, C and D for composition "B”; and 5A, B, C and D for composition "C”.
  • TEM transmission electron micrographs

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Metal Extraction Processes (AREA)
  • Heat Treatment Of Nonferrous Metals Or Alloys (AREA)
  • Forging (AREA)
  • Extrusion Of Metal (AREA)
  • Compositions Of Oxide Ceramics (AREA)
EP86300259A 1985-01-22 1986-01-16 Verfahren zur Herstellung dünnwandiger Röhren aus einer Zirkonium-Niob-Legierung Expired - Lifetime EP0198570B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US69354685A 1985-01-22 1985-01-22
US693546 1985-01-22

Publications (3)

Publication Number Publication Date
EP0198570A2 true EP0198570A2 (de) 1986-10-22
EP0198570A3 EP0198570A3 (en) 1987-10-14
EP0198570B1 EP0198570B1 (de) 1990-08-29

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EP86300259A Expired - Lifetime EP0198570B1 (de) 1985-01-22 1986-01-16 Verfahren zur Herstellung dünnwandiger Röhren aus einer Zirkonium-Niob-Legierung

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EP (1) EP0198570B1 (de)
JP (1) JPS61210166A (de)
KR (1) KR930009986B1 (de)
ES (1) ES8708021A1 (de)

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2576322A1 (fr) * 1985-01-22 1986-07-25 Westinghouse Electric Corp Procede pour le formage d'articles a partir d'alliages de zirconium
EP0425465A1 (de) * 1989-10-27 1991-05-02 Sandvik Aktiebolag Verfahren zur Herstellung von Kapselrohren für Brennstäbe von Kernreaktoren
EP0495978A1 (de) * 1990-08-03 1992-07-29 Teledyne Industries Inc Herstellung von zircaloy-mahlprodukten für verbesserte mikrostruktur und eigenschaften
EP0559096A1 (de) * 1992-03-06 1993-09-08 Westinghouse Electric Corporation Zirlo-Legierung und Herstellungsverfahren
EP1223587A1 (de) * 2001-01-09 2002-07-17 Mitsubishi Materials Corporation Brennstoffhüllrohr aus Zr-Nb-Legierung für Kernreaktor
WO2004040587A1 (en) 2002-10-30 2004-05-13 Westinghouse Electric Sweden Ab Method, use and device concerning cladding tubes for nuclear fuel and a fuel assembly for a nuclear pressure water reactor
WO2006004499A1 (en) * 2004-07-06 2006-01-12 Westinghouse Electric Sweden Ab Fuel box in a boiling water nuclear reactor
CN103650659B (zh) * 2005-12-27 2010-03-10 西北有色金属研究院 一种核反应堆用锆基合金板材的制备方法
US8070892B2 (en) 2007-02-09 2011-12-06 Korea Atomic Energy Research Institute High Fe contained zirconium alloy compositions having excellent corrosion resistance and preparation method thereof
US8105448B2 (en) 2004-07-06 2012-01-31 Westinghouse Electric Sweden Ab Fuel box in a boiling water nuclear reactor
US20120145287A1 (en) * 2008-02-29 2012-06-14 Korea Atomic Energy Research Institute Zirconium alloy compositions having excellent corrosion resistance by the control of various metal-oxide and precipitate and preparation method thereof
US8320515B2 (en) 2006-08-24 2012-11-27 Westinghouse Electric Sweden Ab Water reactor fuel cladding tube
CN104550311A (zh) * 2014-12-05 2015-04-29 宁夏东方钽业股份有限公司 一种生产超导铌管材的方法
WO2017131260A1 (ko) 2016-01-27 2017-08-03 한전원자력연료 주식회사 다단 열간압연을 적용한 핵연료용 지르코늄 부품의 제조방법
CN112775203A (zh) * 2020-12-23 2021-05-11 西部新锆核材料科技有限公司 一种锆或锆合金挤压型材的制备方法
WO2021125439A1 (ko) * 2019-12-18 2021-06-24 한전원자력연료 주식회사 페라이트계 합금 및 이를 이용한 핵연료 피복관의 제조방법
CN113201666A (zh) * 2021-04-08 2021-08-03 中广核研究院有限公司 用于燃料组件的锆合金及其制作方法、燃料组件的包壳管
CN113976657A (zh) * 2021-10-21 2022-01-28 西安赛特思迈钛业有限公司 一种超大口径钛合金薄壁无缝管材的制备方法

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62180047A (ja) * 1986-02-03 1987-08-07 Hitachi Ltd ジルコニウム基合金部材の製造法
FR2688232B1 (fr) * 1992-03-04 1994-04-22 Cezus Co Europ Zirconium Procede de fabrication de tubes a base de zirconium formes de couches de composition differente.
KR100382997B1 (ko) † 2001-01-19 2003-05-09 한국전력공사 고연소도 핵연료 용 니오븀 함유 지르코늄 합금 관재 및판재의 제조방법
ITMI20061223A1 (it) * 2006-06-26 2007-12-27 Snam Progetti Tubo bimetallico resistente alla corrosione e suo utilizzo in apparecchiature a fascio tubiwero
KR101552514B1 (ko) 2014-04-25 2015-09-14 한전원자력연료 주식회사 냉간 필거 압연기의 필거 다이 조립체의 갭 조절장치
CN109692880B (zh) * 2018-12-19 2021-01-01 西部超导材料科技股份有限公司 一种Zr-2.5Nb合金棒材及其挤压加工方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2894866A (en) * 1958-01-21 1959-07-14 Marion L Picklesimer Method for annealing and rolling zirconium-base alloys
LU41401A1 (de) * 1961-03-23 1962-05-17
US3341373A (en) * 1962-09-26 1967-09-12 Imp Metal Ind Kynoch Ltd Method of treating zirconium-base alloys
US3865635A (en) * 1972-09-05 1975-02-11 Sandvik Ab Method of making tubes and similar products of a zirconium alloy
EP0071193A1 (de) * 1981-07-29 1983-02-09 Hitachi, Ltd. Verfahren zur Herstellung einer Legierung auf der Basis von Zirkonium
EP0085553A2 (de) * 1982-01-29 1983-08-10 Westinghouse Electric Corporation Herstellungsverfahren für Zirkoniumlegierungen
FR2576322A1 (fr) * 1985-01-22 1986-07-25 Westinghouse Electric Corp Procede pour le formage d'articles a partir d'alliages de zirconium

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2894866A (en) * 1958-01-21 1959-07-14 Marion L Picklesimer Method for annealing and rolling zirconium-base alloys
LU41401A1 (de) * 1961-03-23 1962-05-17
US3341373A (en) * 1962-09-26 1967-09-12 Imp Metal Ind Kynoch Ltd Method of treating zirconium-base alloys
US3865635A (en) * 1972-09-05 1975-02-11 Sandvik Ab Method of making tubes and similar products of a zirconium alloy
EP0071193A1 (de) * 1981-07-29 1983-02-09 Hitachi, Ltd. Verfahren zur Herstellung einer Legierung auf der Basis von Zirkonium
EP0085553A2 (de) * 1982-01-29 1983-08-10 Westinghouse Electric Corporation Herstellungsverfahren für Zirkoniumlegierungen
FR2576322A1 (fr) * 1985-01-22 1986-07-25 Westinghouse Electric Corp Procede pour le formage d'articles a partir d'alliages de zirconium

Cited By (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2576322A1 (fr) * 1985-01-22 1986-07-25 Westinghouse Electric Corp Procede pour le formage d'articles a partir d'alliages de zirconium
EP0425465A1 (de) * 1989-10-27 1991-05-02 Sandvik Aktiebolag Verfahren zur Herstellung von Kapselrohren für Brennstäbe von Kernreaktoren
EP0495978A1 (de) * 1990-08-03 1992-07-29 Teledyne Industries Inc Herstellung von zircaloy-mahlprodukten für verbesserte mikrostruktur und eigenschaften
EP0495978A4 (en) * 1990-08-03 1993-01-27 Teledyne Industries Inc Fabrication of zircaloy mill products for improved microstructure and properties
EP0559096A1 (de) * 1992-03-06 1993-09-08 Westinghouse Electric Corporation Zirlo-Legierung und Herstellungsverfahren
EP1223587A1 (de) * 2001-01-09 2002-07-17 Mitsubishi Materials Corporation Brennstoffhüllrohr aus Zr-Nb-Legierung für Kernreaktor
WO2004040587A1 (en) 2002-10-30 2004-05-13 Westinghouse Electric Sweden Ab Method, use and device concerning cladding tubes for nuclear fuel and a fuel assembly for a nuclear pressure water reactor
US7473329B2 (en) * 2002-10-30 2009-01-06 Westinghouse Electric Sweden Ab Method, use and device concerning cladding tubes for nuclear fuel and a fuel assembly for a nuclear pressure water reactor
WO2006004499A1 (en) * 2004-07-06 2006-01-12 Westinghouse Electric Sweden Ab Fuel box in a boiling water nuclear reactor
US8105448B2 (en) 2004-07-06 2012-01-31 Westinghouse Electric Sweden Ab Fuel box in a boiling water nuclear reactor
CN103650659B (zh) * 2005-12-27 2010-03-10 西北有色金属研究院 一种核反应堆用锆基合金板材的制备方法
US8320515B2 (en) 2006-08-24 2012-11-27 Westinghouse Electric Sweden Ab Water reactor fuel cladding tube
US8070892B2 (en) 2007-02-09 2011-12-06 Korea Atomic Energy Research Institute High Fe contained zirconium alloy compositions having excellent corrosion resistance and preparation method thereof
US20120145287A1 (en) * 2008-02-29 2012-06-14 Korea Atomic Energy Research Institute Zirconium alloy compositions having excellent corrosion resistance by the control of various metal-oxide and precipitate and preparation method thereof
CN104550311A (zh) * 2014-12-05 2015-04-29 宁夏东方钽业股份有限公司 一种生产超导铌管材的方法
WO2017131260A1 (ko) 2016-01-27 2017-08-03 한전원자력연료 주식회사 다단 열간압연을 적용한 핵연료용 지르코늄 부품의 제조방법
WO2021125439A1 (ko) * 2019-12-18 2021-06-24 한전원자력연료 주식회사 페라이트계 합금 및 이를 이용한 핵연료 피복관의 제조방법
US11603584B2 (en) 2019-12-18 2023-03-14 Kepco Nuclear Fuel Co., Ltd. Ferritic alloy and method of manufacturing nuclear fuel cladding tube using the same
CN112775203A (zh) * 2020-12-23 2021-05-11 西部新锆核材料科技有限公司 一种锆或锆合金挤压型材的制备方法
CN112775203B (zh) * 2020-12-23 2024-01-19 西部新锆核材料科技有限公司 一种锆或锆合金挤压型材的制备方法
CN113201666A (zh) * 2021-04-08 2021-08-03 中广核研究院有限公司 用于燃料组件的锆合金及其制作方法、燃料组件的包壳管
CN113976657A (zh) * 2021-10-21 2022-01-28 西安赛特思迈钛业有限公司 一种超大口径钛合金薄壁无缝管材的制备方法
CN113976657B (zh) * 2021-10-21 2024-04-23 西安赛特思迈钛业有限公司 一种超大口径钛合金薄壁无缝管材的制备方法

Also Published As

Publication number Publication date
ES551049A0 (es) 1987-09-01
ES8708021A1 (es) 1987-09-01
EP0198570B1 (de) 1990-08-29
EP0198570A3 (en) 1987-10-14
JPS61210166A (ja) 1986-09-18
KR860005894A (ko) 1986-08-16
KR930009986B1 (ko) 1993-10-13

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