WO2016167397A1 - 우수한 내식성 및 크리프 저항성을 갖는 지르코늄 합금과 그 제조방법 - Google Patents

우수한 내식성 및 크리프 저항성을 갖는 지르코늄 합금과 그 제조방법 Download PDF

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WO2016167397A1
WO2016167397A1 PCT/KR2015/004641 KR2015004641W WO2016167397A1 WO 2016167397 A1 WO2016167397 A1 WO 2016167397A1 KR 2015004641 W KR2015004641 W KR 2015004641W WO 2016167397 A1 WO2016167397 A1 WO 2016167397A1
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weight
heat treatment
zirconium alloy
vacuum heat
cold
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PCT/KR2015/004641
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English (en)
French (fr)
Korean (ko)
Inventor
최민영
목용균
김윤호
나연수
이충용
정태식
고대균
이승재
김재익
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한전원자력연료 주식회사
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Priority to JP2017553426A priority Critical patent/JP6588104B2/ja
Priority to CN201580078752.2A priority patent/CN107438675B/zh
Priority to EP15889277.8A priority patent/EP3284836B1/en
Publication of WO2016167397A1 publication Critical patent/WO2016167397A1/ko

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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D7/00—Casting ingots, e.g. from ferrous metals
    • B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals

Definitions

  • the present invention relates to a zirconium alloy having excellent corrosion resistance and creep resistance, and a method of manufacturing the same, and more particularly, to a composition and heat treatment condition of a zirconium alloy used in nuclear fuel cladding and support grids of light and heavy water reactors.
  • Zirconium alloys are alloys with low neutron absorption cross-sectional area, good corrosion resistance and mechanical properties. They are materials for nuclear cladding, fuel assembly support grids, and structures within reactors. It has been widely used in BWR (Boiling Water Reactor) reactors.
  • Zircaloy-2 developed so far (Zircaloy-2, Sn 1.20-1.70 wt%, Fe 0.07-0.20 wt%, Cr 0.05-1.15 wt%, Ni 0.03-0.08 wt%, 0 900-1500 ppm, Zr balance)
  • Zircaloy-4 Zircaloy-4, Sn 1.20 to 1.70 wt%, Fe 0.18 to 0.24 wt%, Cr 0.07 to 1.13 wt%, 0 900 to 1500 ppm, Ni ⁇ 0.007 wt%, Zr balance) most widely It is used.
  • US Patent No. 4,649,023 is made of zirconium with 0.5 to 2.0% by weight of niobium, 0.9 to 1.5% by weight of tin, one element of iron, chromium, molybdenum, vanadium, copper, nickel, tungsten
  • a zirconium alloy containing 0.09 to 0.11% by weight and 0.1 to 0.16% by weight of oxygen was proposed.
  • the alloy is proposed a method for producing a product in which precipitates of fine size of 80 nm or less are homogeneously distributed in the matrix.
  • U. S. Patent No. 5,648, 995 proposes a cladding tube using a zirconium alloy composed of 0.8 to 1.3 wt% niobium, 50 to 250 ppm iron, 1600 ppm or less oxygen, and 120 ppm or less silicon.
  • the alloy is heat-treated at 600 to 800 ° C. and then extruded, cold rolling is performed 4 to 5 times, and an intermediate heat treatment between cold rolling is performed at a temperature range of 565 to 605 ° C. for 2 to 4 hours.
  • the final heat treatment was performed at 580 ° C. to prepare a nuclear fuel coated tube.
  • iron is limited to 250 ppm or less and oxygen is limited to 1000 to 1600 ppm in the composition of the alloy.
  • U.S. Patent No. 6,325,966 discloses 0.15 to 0.25% by weight of niobium, 1.10 to 1.40% by weight of tin, 0.35 to 0.45% by weight of iron, and 0.15 to 0.25% by weight of chromium and 0.08% of one of molybdenum, copper and manganese.
  • the zirconium alloy composition for high combustion degree improved corrosion resistance and mechanical properties by changing the type and amount of added elements or by changing the heat treatment conditions I'm continuing my research.
  • the optimum conditions having excellent corrosion resistance and mechanical properties of the zirconium alloy is affected by the type of additive element, the amount of addition, processing conditions and heat treatment conditions, etc., it is necessary to establish the alloy design and heat treatment conditions.
  • Zr-Nb alloy system can remove the Sn and add P, Ta, etc. to adjust the composition and the heat treatment temperature to improve creep resistance while significantly improving creep resistance.
  • the present invention has been made to solve the above problems, considering the optimized heat treatment conditions by removing the tin that adversely affects the corrosion resistance, by adding niobium, phosphorus, tantalum, etc. to maintain creep resistance
  • the purpose of the present invention is to provide a zirconium alloy composition and final heat treatment conditions with improved creep resistance while improving corrosion resistance.
  • the zirconium alloy according to the present invention for achieving this purpose is basically composed of niobium 1.1 to 1.2% by weight, phosphorus 0.01 to 0.2% by weight, iron 0.2 to 0.3% by weight and zirconium balance.
  • phosphorus is preferably characterized in that from 0.02 to 0.07% by weight.
  • the zirconium alloy may be added 0.01 to 0.15% by weight of tantalum (Ta) in order to improve the corrosion resistance and resistance to creep deformation.
  • Ta tantalum
  • tantalum (Ta) is 0.03 to 0.1 weight%.
  • the method for producing a zirconium alloy according to the present invention is prepared by dissolving a mixture composed of 1.1 to 1.2% by weight of niobium, 0.01 to 0.2% by weight of phosphorus, 0.2 to 0.3% by weight of iron and the zirconium balance. Stage 1;
  • the seventh step of the final vacuum heat treatment of the third cold rolled rolling material in the sixth step at 440 ⁇ 650 °C for 7 to 9 hours.
  • the phosphorus in the first step is preferably 0.02 ⁇ 0.07% by weight
  • the temperature of the final vacuum heat treatment is preferably 460 ⁇ 600 °C in the seventh step to optimize the corrosion resistance and resistance to creep deformation have.
  • the corrosion resistance may be further improved.
  • the tantalum (Ta) is 0.03 ⁇ 0.1% by weight
  • the temperature of the final vacuum heat treatment in the seventh step is 460 ⁇ 530 °C by which the corrosion resistance and the resistance to creep deformation can be improved to the highest.
  • the zirconium alloy according to the present invention completely removes tin and has superior corrosion resistance compared to zircaloy-4 by controlling the type, amount and final heat treatment conditions of additive elements such as P and Ta, and also has high creep resistance. And it can be very useful as a nuclear fuel coating pipe in the reactor core of the heavy water reactor type nuclear power plant.
  • the zirconium alloy according to the present invention is composed of 1.1 to 1.2% by weight of niobium, 0.02 to 0.05% by weight of phosphorus, 0.2 to 0.3% by weight of iron and zirconium balance.
  • niobium is 1.1 to 1.2% by weight, phosphorus 0.02% by weight, iron 0.2-0.3% by weight and zirconium balance.
  • niobium is 1.1 to 1.2% by weight, phosphorus 0.05% by weight, iron 0.2-0.3% by weight and the zirconium balance.
  • tantalum is added to the zirconium alloy and is composed of 1.1 to 1.2% by weight of niobium, 0.05% by weight of phosphorus, 0.03 to 0.04% by weight of tantalum, 0.2 to 0.3% by weight of iron, and zirconium balance.
  • tantalum is added to the zirconium alloy and is composed of 1.1 to 1.2% by weight of niobium, 0.05% by weight of phosphorus, 0.09 to 0.1% by weight of tantalum, 0.2 to 0.3% by weight of iron, and zirconium balance.
  • a first step of dissolving a mixture of zirconium alloy composition elements into an ingot A second step of ⁇ -quenching (quenching) the ingot prepared in the first step by quenching in water after solution heat treatment for 30 to 40 minutes at 1,000 to 1,050 ° C ( ⁇ phase section); A third step of preheating the ingot heat-treated in the second step for 20 to 30 minutes at 630 to 650 ° C., followed by hot rolling at a 60 to 65% reduction ratio; A fourth step of first cold rolling the hot rolled material in the third step at 570 to 590 ° C.
  • the first step is ingot using 1.2% by weight of niobium, 0.02 to 0.05% by weight of phosphorus, 0.03 to 0.1% by weight of tantalum, 0.2% by weight of iron and the balance of zirconium by vacuum arc melting (VAR) method. To prepare.
  • the zirconium used was a nuclear grade zirconium sponge as specified in ASTM B349, and the added elements such as niobium, phosphorus, tantalum, and iron used high purity elements of 99.99% or more.
  • the ingot was prepared by maintaining the vacuum sufficiently in the chamber of the arc melting apparatus at 10 -5 torr or less and then dissolving the alloy.
  • phosphorus (P) was pressed and melted differently from other alloy elements in order to prevent precipitation.
  • an inert gas such as argon was injected and cooled.
  • the second step is a process of ⁇ -solution heat treatment and ⁇ -quenching, and the solution was water cooled at a rate of about 300 ° C./sec or more after solution treatment for 30 minutes in the ⁇ phase temperature range of 1,000 to 1,050 ° C.
  • a stainless steel plate of 1mm thickness spot welding was performed. This process is performed to homogenize the alloy composition in the manufactured ingot and to uniformly distribute the size of the secondary phase particles (SPP) in the base metal.
  • the hot rolling of the specimen in which ⁇ -annealing is completed is performed.
  • the hot rolled rolled material was removed from the coated stainless steel plate, and then the oxide film and impurities were removed using a pickling solution having a volume ratio of 50:40:10 of water: nitric acid: hydrofluoric acid. The oxide film was completely removed.
  • the intermediate vacuum heat treatment it is preferable to heat up the recrystallization heat treatment temperature. If the temperature is out of the temperature range, the corrosion resistance may be degraded.
  • the rolled material which was subjected to the first intermediate vacuum heat treatment, was subjected to primary cold rolling at a rolling reduction rate of about 40 to 50% at intervals of about 0.3 mm per pass.
  • the first cold rolled rolled material was subjected to a secondary intermediate vacuum heat treatment at 570-580 ° C. for about 2-3 hours.
  • the corrosion resistance may be reduced.
  • the secondary cold rolled rolled material was subjected to a third intermediate vacuum heat treatment at 570-580 ° C. for 2-3 hours.
  • If out of the intermediate heat treatment temperature may cause a problem that the corrosion resistance is lowered.
  • a third cold rolling was performed at a rolling reduction rate of about 30 to 40% at an interval of about 0.3 mm per pass.
  • Final heat treatment of the third cold rolled rolled material is carried out in a high vacuum atmosphere of 10 ⁇ 5 torr or less.
  • a plate corrosion test specimen having a size of 20 mm ⁇ 20 mm ⁇ 1.0 mm was manufactured, and stepwise using SiC abrasive paper of # 400 to # 1200. Mechanical polishing was performed.
  • the surface area and initial weight of the alloy were measured before the autoclave was charged.
  • the loaded specimens were subjected to a corrosion test for 100 days using static autoclave in pure water and 70 ppm Li water at 360 ° C. and 18.6 MPa.
  • the results of the corrosion test are as follows: 1) 0.02% by weight and 0.05% by weight of phosphorus in the absence of tantalum; and 2) 0.03% and 0.1% by weight of tantalum when the phosphorus component is 0.05% by weight. Let's take a look at each of the results when added in%. In this case, in the above 1) and 2), all the experiments were carried out for the three cases when the final heat treatment temperature is 460 °C, 520 °C, 580 °C, respectively.
  • the significant improvement in corrosion resistance can be seen that the experimental value of 0.02% to 0.07% by weight.
  • the phosphorus component is 0.05% by weight, but an increase in corrosion resistance is observed when phosphorus is 0.05% by weight rather than 0.02% by weight, so at least a significant improvement in corrosion resistance can be maintained even at 0.07% by weight. It can be predicted enough.
  • Examples 2, 6, and 10 are cases in which only phosphorus is added without tantalum
  • Examples 3, 7, and 11 are cases in which 0.03% by weight of tantalum is added
  • Examples 4, 8 and 12 are tantalum. 0.1 weight% is added.
  • Tantalum has a significant increase in corrosion resistance in Example 4 at 460 ° C. and Example 8 at 520 ° C., with a slight increase in tantalum at 0.03% by weight. Is observed.
  • tantalum will have an increase in corrosion resistance when the component ratio is 0.01% by weight to 0.15% by weight, and further remarkable increase in corrosion resistance is proved by the experiment that it is the case of 0.03% by weight to 0.1% by weight.
  • the zirconium alloys of Examples 1 to 4 were fabricated in the above-described manufacturing process, and then creep specimens were prepared.
  • Comparative Example 1 In addition, in order to compare the creep characteristics, a commercial cladding tube of Comparative Example 1 was simulated to prepare Zircaloy-4 specimen of Comparative Example 2 in the form of a plate in the same process. In this case, the final heat treatment of Comparative Example 2 was carried out at 460 ° C. under the same conditions as those of Examples 1 to 4 and Comparative Example 1 to perform creep tests.
  • Example 1-4 consisting of a zirconium alloy composition according to the present invention was evaluated for 10 days at 350 °C, 120 MPa stress conditions, the creep deformation was measured in the range of 0.22 ⁇ 0.34.
  • the amount of Ta increases, the amount of creep deformation is greatly reduced.
  • the creep deformation amount of Comparative Example 2 is 0.46, it can be seen that the deformation amount is much larger than Example 1-4.
  • the resistance to creep deformation is effective when even a small amount of phosphorus is added. As the amount of tantalum is increased, the resistance to creep deformation is remarkably higher.

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  • Chemical & Material Sciences (AREA)
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  • Mechanical Engineering (AREA)
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  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
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PCT/KR2015/004641 2015-04-14 2015-05-08 우수한 내식성 및 크리프 저항성을 갖는 지르코늄 합금과 그 제조방법 WO2016167397A1 (ko)

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Application Number Priority Date Filing Date Title
JP2017553426A JP6588104B2 (ja) 2015-04-14 2015-05-08 優れた耐食性及びクリープ抵抗性を有するジルコニウム合金、及びその製造方法
CN201580078752.2A CN107438675B (zh) 2015-04-14 2015-05-08 具有优异的耐腐蚀性和抗蠕变性的锆合金及其制备方法
EP15889277.8A EP3284836B1 (en) 2015-04-14 2015-05-08 Zirconium alloy having excellent corrosion resistance and creep resistance, and method for manufacturing same

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KR10-2015-0052711 2015-04-14
KR1020150052711A KR101604105B1 (ko) 2015-04-14 2015-04-14 우수한 내식성 및 크리프 저항성을 갖는 지르코늄 합금과 그 제조방법

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EP (1) EP3284836B1 (ja)
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WO (1) WO2016167397A1 (ja)

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CN108251698A (zh) * 2018-01-15 2018-07-06 燕山大学 一种耐腐蚀锆合金及其制备方法和应用
AR110991A1 (es) 2018-02-21 2019-05-22 Comision Nac De Energia Atomica Cnea Aleaciones de circonio con resistencia a la corrosión y temperatura de servicio mejoradas para usar en el revestimiento del combustible y las partes estructurales del núcleo de un reactor nuclear
US20220184706A1 (en) * 2019-04-30 2022-06-16 Westinghouse Electric Company Llc Improved corrosion resistance of additively-manufactured zirconium alloys
EP4082685A4 (en) * 2019-12-26 2024-01-17 Joint Stock Company Tvel METHOD FOR MANUFACTURING TUBULAR ARTICLES FROM A ZIRCONIUM ALLOY
CN115011822B (zh) * 2022-06-13 2023-07-18 国核宝钛锆业股份公司 一种外方内圆锆合金型材的制备方法
CN115652237B (zh) * 2022-08-16 2023-11-24 重庆大学 含三次孪晶的锆合金及其制备方法

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EP3284836A1 (en) 2018-02-21
CN107438675B (zh) 2020-04-07
JP6588104B2 (ja) 2019-10-09
KR101604105B1 (ko) 2016-03-16
JP2018514650A (ja) 2018-06-07
CN107438675A (zh) 2017-12-05
EP3284836B1 (en) 2020-07-01
US20160304991A1 (en) 2016-10-20
EP3284836A4 (en) 2018-09-26

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