CN1125885C - Zirconium based alloy - Google Patents

Zirconium based alloy Download PDF

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Publication number
CN1125885C
CN1125885C CN99816580A CN99816580A CN1125885C CN 1125885 C CN1125885 C CN 1125885C CN 99816580 A CN99816580 A CN 99816580A CN 99816580 A CN99816580 A CN 99816580A CN 1125885 C CN1125885 C CN 1125885C
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alloy
niobium
zirconium
iron
chromium
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CN1350597A (en
Inventor
A·V·尼库里那
P·V·谢巴多夫
V·N·希肖夫
M·M·派里古德
L·E·阿吉恩科娃
V·V·罗兹德斯特万斯基
P·P·马克洛夫
M·I·索罗尼
J·K·比比拉施维利
P·I·拉夫伦朱克
A·F·罗斯特斯基
N·A·甘扎
N·V·库兹门科
V·A·克特里克霍夫
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Gosudarstvenny Nauchny Tsentr Rossiiskoi Federatsiii Vserossiisky Nauchno-=issle
Tvel JSC
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Gosudarstvenny Nauchny Tsentr Rossiiskoi Federatsiii Vserossiisky Nauchno-=issle
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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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
  • Materials For Medical Uses (AREA)

Abstract

A zirconium-based alloy have ( according to weight percent ): from 0.5 to 3.0 wt % of niobium; from 0.5 to 2.0 wt % of tin; from 0.3 to 1.0 wt % of iron; from 0.002 to 0.2 wt % of chromium; from 0.003 to 0.04 wt % of carbon; from 0.04 to 0.15 wt % of oxygen; from 0.002 to 0.15 wt % of silicon; from 0.001 to 0.4 wt % of tungsten or molybdenum or vanadium; the balance consisting of zirconium. The structure of this alloy is characterised in that it has a alpha -hardness temper and in that it contains particles of iron- and niobium-containing intermetallic compounds of the Zr(Nb, Fe)2 type. The structure of this alloy may also include particles of iron- and niobium-containing intermetallic compounds of the Zr[Nb, Fe (W or Mo, or V)]2, Zr[Fe, Cr, Nb, (W, or Mo, or V)]2, [Zr, Nb, (W, or Mo, or V)]2Fe, Zr(Fe, Cr, Nb)2 or (Zr, Nb)2Fe types having a particle size not exceeding 0.3 mu m.

Description

Zirconium base alloy
Technical field
The present invention relates to metallurgy, especially relate to zirconium base alloy.
Background technology
People have proposed considerable requirement to above-mentioned alloy, promptly as corrosion resisting property, strength characteristics and resistance of oxidation, anti-hydrogenation ability, radioprotective energy for growth and creep resistance in water and high-temperature water vapor.In addition, because this alloy mainly is the sheet-metal duct that is used for other member of the work runner of fuel jacket and nuclear reactor and radioactivity core thereof at manufacturing, so it must have high processability.
Up to now, a kind of zirconium base alloy of prior art and preparation technology thereof and have been known by its method that manufactures a product (referring to U.S. Pat 4649023).Alloy contains the following composition that wherein accounts for following ratio (by weight percentage): niobium, 0.5-2.0; Tin, 0.9-1.5; A kind of element in iron, chromium, molybdenum, vanadium, copper, nickel, the tungsten, 0.09-0.11; Surplus is a zirconium.
But it is comprehensive to be by the feature of the product of this alloy manufacturing that it has wide inadequately corrosion resisting property with currently known methods, comprising not high enough anti-dross corrosive nature in boiling water.The product iron composition that obtained reduce hindered obtain between each ferrous metal between the compound fixedly than, thereby influence the intensity and the corrosion resisting property of alloy unfriendly.
Another kind of zirconium base alloy contains (by weight percentage) as everyone knows: niobium, 0.5-2.0; Tin, 0.7-1.5; At least a element in iron, chromium, the nickel, 0.07-0.28; Surplus is zirconium (referring to a U.S. Pat 5125985).
But described alloy has run into the trouble of processability difference, and this is because at the processing initial stage, formed compound such as ZrFe between stable metal in alloy structure 3The macrobead arranged of elongation, described intermetallic compound has influenced the resistance to cleavage of being made product by this alloy unfriendly, and this has hindered in the use intensive cold working of processing final stage and has limited in fact and made the used large-scale component of nuclear reactor radioactivity core.
Another kind of zirconium base alloy contains (by weight percentage) as everyone knows: niobium, 0.5-1.5; Tin, 0.9-1.5; Iron, 0.3-0.6; Chromium, 0.005-0.2; Carbon, 0.005-0.04; Oxygen, 0.05-0.15; Silicon, 0.005-0.15, this alloy structure are by containing niobium and ferruginous intermetallic compound hardened metal matrix, and described intermetallic compound has such intermetallic compound total amount volume ratio, promptly Zr (Fe, Nb) 2+ Zr (Fe, Cr, Nb)+(Zr, Nb) 3Fe accounts at least that 60% and its intermediary gap of total amount of compound equals 0.32 ± 0.09 μ m (referring to U.S. Pat 2032759) between ferrous metal.
This from technical spirit the alloy of approaching alloy described herein be chosen as prototype.
Product by the manufacturing of this prototype alloy has high strength characteristics, anti-boiling water corrosive nature and radiation hardness growth performance and creep-resistant property.
But people need be used to make some products that are used for nuclear reactor radioactivity core to the alloy that has higher strength characteristics, creep-resistant property and radiation hardness growth performance under near 350 ℃ of long-time radiation as being used for the pipe of its guide groove or work runner.
Summary of the invention
The purpose of this invention is to provide a kind of zirconium base alloy, the product characteristics of being made by described alloy is that it has higher intensity and radiation hardness energy for growth and creep resisting ability under 300 ℃-350 ℃, this is because set up the microtexture of determining in described product, and its strong solidity to corrosion and fracture-resistant can not be affected.
Realize above-mentioned purpose by such fact, the zirconium base alloy of the present invention that promptly contains niobium, tin, iron, chromium, carbon, oxygen, silicon also contains the element that another kind is selected from one of tungsten, molybdenum and vanadium, its percentage composition is such (by weight percentage): niobium, 0.5-3.0; Tin, 0.5-2.0; Iron, 0.3-0.1; Chromium, 0.002-0.2; Carbon, 0.003-0.04; Oxygen, 0.04-0.15; Silicon, 0.002-0.15; Tungsten, molybdenum or vanadium, 0.001-0.4; Surplus is a zirconium.
Product by this alloy manufacturing is practical, this is because at first cancelled the alloy pre-treatment is come to form the work of big intermetallic compound particle, secondly is because considered that the blank technology extension limit in the cold working section that can use sizable deflection in its initial stage is wideer.Utilize aximal deformation value to make material structure more even and help to form fixed composition, dispersity and the dispersing uniformity of two second phase particles in zirconium matrix, obtained thus near the higher processing characteristics under 350 ℃ the temperature, comprising intensity, corrosion resisting property, resistance to rupture, radiation hardness growth performance and creep-resistant property.
According to the present invention, the characteristics of this alloy microtexture be it have size less than the Zr of 0.2-0.3 μ m (Nb, Fe) 2The type iron content contains the particle and the αGu Rongti of the intermetallic compound of niobium, and it can also have the Zr[Nb of size less than 0.2-0.3 μ m, Fe (W or Mo or V)] 2, Zr[Fe, Cr, Nb (W or Mo or V)] 2, [Zr, Nb (W or Mo or V)] 2Fe, Zr (Fe, Cr, Nb) 2, (Zr, Nb) 2Fe type iron content contains the particle and the αGu Rongti of the intermetallic compound of niobium.
Above-mentioned intermetallic compound sum surpasses 80% (volume percent) in the segregation composition total amount of two second phases.
Add a kind of element and its addition that is selected from one of tungsten, molybdenum and vanadium to alloy and reach 0.001 weight %-0.4 weight %, this has improved the intensity of α zirconium matrix, thus one, there not be formation is big in finished product β zirconium compound between the binary metal of particle and zirconium and iron and zirconium and chromium mutually by making the sealing of iron, chromium and comparing the content that improves niobium, tin, iron with prototype, thereby prevented that the intermetallic compound that iron content contains chromium from condensing, compound has reduced the corrosion resisting property of material between described binary metal, causes the finished product disintegration and its processability is descended.
0.001 the interpolation material quantity of weight %-0.4 weight % is selected according to the following fact, promptly when the content of tungsten, molybdenum or the vanadium of material during less than 0.001 weight %, α zirconium matrix can reduce with feeling and ferruginous intermetallic compound no longer strengthens in manufacturing processed, decomposes and stablizes, as a result, the corrosion resisting property of material has been subjected to disadvantageous effect.
When the content of described element in alloy surpasses 0.4 weight %, this caused compound between bimetal (zirconium and iron or zirconium and chromium) macrobead group formation with and particle between the gap excessively condense above other iron of 0.3 μ m and two second phase particles of niobium.As a result, the material processability in the worse cold working process and the resistance to cleavage of finished product have been obtained.
Tungsten, molybdenum and vanadium have also formed the part that iron content contains the intermetallic compound of niobium, have increased its dispersiveness and density thus.
With make all relevant above-mentioned factors of the used product of nuclear reactor radioactivity core with above-mentioned materials and facilitated and in finished product, form thin brilliant α zirconium matrix uniformly, it has and is characterized in having high-density and the dispersed iron content and the intermetallic compound of niobium, and the characteristics of these intermetallic compounds of the overwhelming majority are that it has less than the particle size of 0.1 μ m-0.3 μ m and the particle gap of 0.1 μ m-0.3 μ m.It is intermetallic compound that total amount surpasses 80% described particle performance, as its particle size less than the Zr of 0.2 μ m-0.3 μ m (Nb, Fe) 2And Zr[Nb, Fe (W or Mo or V)] 2, Zr[Fe, Cr, Nb (W or Mo or V)] 2, [Zr, Nb (W or Mo or V)] 2Fe, Zr (Fe, Cr, Nb) 2, (Zr, Nb) 2Fe.
In the time of in being used to nuclear reactor radioactivity core, in finished product, forming such microtexture and guaranteed its high job stability and pursued high corrosion resisting property in view of the above and especially anti-dross corrosive nature, high strength and resistance to rupture and near creep-resistant property under 450 ℃ of temperature and radiation hardness growth performance.
The preferred forms of invention
In order to promote to understand the present invention, particular exemplary embodiment more of the present invention have below been provided.
Example 1
Utilize the vacuum arc melting method that alloy of the present invention is made ingot.Then, forge ingot casting under 1070 ℃-900 ℃ temperature, the ingot casting diameter has reduced 5 times as a result, and forging stock is heated to 1050 ℃ and accept water quenching.In case removed surperficial gas saturated zone, the quenching base carries out the scale cutting and is being drilled with a hole on each blank and is annealing under 620 ℃.Then, scale blank with holes carries out pressure forming under 620 ℃.Then, the pressure forming pipe is quenched and under 425 ℃, anneal since 950 ℃ of speed with 500 ℃/s, and the annealing blank is accepted cold forging according to multi-pass with depressing rolling pattern in first rolling pass and follow-up rolling pass, its total draft is 50 (with regard to wall thickness and base footpaths), and accepts process annealing under 620 ℃.Final annealing after cold rolling carries out under 580 ℃.After finishing finishes, obtained external diameter and be 9.15 millimeters, wall thickness and be 0.65 millimeter production tube.
Example 2
Utilize the vacuum arc melting method that alloy of the present invention is made ingot.Then, forge ingot casting under 1070 ℃-900 ℃ temperature, the ingot casting diameter has reduced 1.6 times as a result.Subsequently, forging stock is heated to 1050 ℃ and accept water quenching.In case removed surperficial gas saturated zone, the quenching base is become multistage and be drilled with a hole on each blank by fixed ruler cutting.Then,, scale blank with holes carries out pressure forming and annealed two hours down at 620 ℃ under 735 ℃ ± 10 ℃.Then, blank is accepted twice cold rolling repeatedly and two hours process annealing under 630 ℃, and following by draught is that the final cold rolling one-tenth in 20%-25% ground limits size.Final annealing after cold rolling carries out under 580 ℃-590 ℃.The external diameter that finishing operation has caused being used as the workflow deferent in the nuclear reactor is that 88 millimeters and wall thickness are 4 millimeters production tube.
Utilize table 1,2 listed examples to show to abide by embodiments of the invention, wherein table 1 expression alloy of the present invention and according to the composition (No. 10) of prototype, sample composition (No. 11) and the composition of microtexture characteristic with the content value that transfinites.Table 2 expression material property: at the workflow deferent (example 2) of fuel jacket under 350 ℃ (example 1) and the nuclear reactor radioactivity core under 300 ℃.
Table 1
Sample number into spectrum Alloying constituent Two second phase particulate characteristics in finished product tubing
Niobium Tin Iron Chromium Carbon Oxygen Silicon Tungsten Molybdenum Vanadium Average grain gap μ m Zr(Nb，Fe，W/Mo/V) 2, Zr (Fe, Cr, Nb, W/Mo/V) two second phase proportion of particles
1 2 3 4 5 6 7 8 9 10 11 12 13
Example 1
1 0.5 0.5 1.0 0.003 0.003 0.05 0.003 0.4 0.16 91
2 3.0 2.0 0.3 0.2 0.04 0.15 0.15 0.001 0.21 80*
3 1.5 1.3 0.8 0.1 0.01 0.12 0.1 0.01 0.19 85*
4 1.5 1.3 0.8 0.1 0.02 0.1 0.1 0.4 0.17 90
5 2.0 1.0 0.7 0.08 0.03 0.09 0.009 0.001 0.22 80*
6 1.0 1.7 0.9 0.15 0.08 0.07 0.07 0.01 0.18 87
7 1.5 1.3 0.8 0.1 0.02 0.1 0.1 0.4 0.17 90
8 2.0 1.0 0.7 0.08 0.03 0.09 0.009 0.001 0.22 81*
9 1.0 1.7 0.9 0.15 0.08 0.03 0.09 0.01 0.19 82*
10 1.5 1.2 0.3 0.2 0.04 0.15 0.15 0.28 72
11 0.4 2.2 1.2 0.22 0.002 0.004 0.002 0.43 0.38 60
Example 2
12 1.5 1.3 1.0 0.1 0.01 0.1 0.1 0.05 0.17 85*
13 1.0 1.7 0.9 0.15 0.02 0.07 0.07 0.01 0.19 87*
14 2.0 1.7 0.9 0.15 0.02 0.07 0.07 0.01 0.20 81*
15 2.8 1.0 0.4 0.2 0.003 0.007 0.4 0.2 0.19 87
16 0.7 0.7 1.2 0.18 0.005 0.14 0.008 0.3 0.18 89
17 2.8 1.0 0.4 0.2 0.003 0.007 0.4 0.01 0.21 81*
* tissue characteristic be have Zr (Nb, Fe) 2Compound between shaped metal
Table 2
Sample number into spectrum The finished product pipe performance
Final strength Weightening finish mg/dm in autoclave water 2 Creep rate σ=100MPa * 3000h.10 -5％/h 5.4 * 10 -26m -2(influence of E＞0.1MeV) radiation growth down is out of shape %
Example 1 (350 ℃)
1 360 46 1.5 0.31
2 390 48 1.65 0.32
3 390 45 1.4 0.30
4 380 48 1.55 0.31
5 370 51 1.6 0.33
6 350 46 1.5 0.30
7 380 47 1.55 0.33
8 350 51 1.6 0.34
9 360 48 1.5 0.32
10 280 55 1.7 0.35
11 - - - -
Example 2 (300 ℃)
12 510 16 1.15 0.30
13 490 18 1.25 0.32
14 520 15 1.27 0.33
15 520 16 1.21 0.31
16 480 17 1.2 0.32
17 550 16 1.28 0.32
As described above shown in the example, use described alloy to guarantee to form a kind of have uniform subdivision tissue and equally distributed two second phase particulate products, 80 volume % of described two second phases by size less than the Zr of 0.2 μ m-0.3 μ m (Nb, Fe) 2Intermetallic compound particle constitutes.Owing to formed such microtexture, so the characteristics of finished product are that it has high intensity, resistance to rupture, corrosion resisting property, creep-resistant property and radiation hardness growth performance.
For the purpose of contrasting, table 1,2 (No. 11 samples) has been expressed its component content and has been surpassed its content ultimate alloy and prototype alloy (No. 10 samples) in alloy of the present invention.
Defective because of forming tiny crack when accepting flaw detection by all products that No. 11 samples are made.Add tungsten, molybdenum or vanadium for the alloy that is proposed as alloying constituent (different) and guaranteed higher intensity, creep-resistant property and radiation hardness growth performance, and strong corrosion resisting property and resistance to rupture are unaffected with No. 10 samples.
Industrial applicibility
When being used to make the used workflow deferent of the used product of nuclear reactor radioactivity core such as fuel encapsulation light-wall pipe and large-sized object such as nuclear reactor radioactivity core and other member, the present invention may be the most applicable. In addition, described alloy need can also be used to strong corrosion resisting property, cracking resistance, the high temperature resistant service life of prolongation and chemical industry, field of medicaments and other engineering field of strong capability of resistance to radiation.

Claims (3)

1. zirconium base alloy, it contains niobium, tin, iron, chromium, carbon, oxygen, silicon, it is characterized in that, and it also contains the element that another kind is selected from one of tungsten, molybdenum and vanadium, and its composition weight percent is such: niobium, 0.5-3.0; Tin, 0.5-2.0; Iron, 0.3-1.0; Chromium, 0.002-0.2; Carbon, 0.003-0.04; Oxygen, 0.04-0.15; Silicon, 0.002-0.15; Tungsten, molybdenum or vanadium, 0.001-0.4; Surplus is a zirconium.
2. zirconium base alloy as claimed in claim 1 is characterized in that, the characteristics of this alloy microtexture be it have size be no more than 0.3 μ m Zr (Nb, Fe) 2The type iron content contains the particle and the αGu Rongti of the intermetallic compound of niobium.
3. zirconium base alloy as claimed in claim 1 is characterized in that, the characteristics of this alloy microtexture are that it has the Zr[Nb of size less than 0.2 μ m-0.3 μ m, Fe (W or Mo or V)] 2, Zr[Fe, Cr, Nb (W or Mo or V)] 2, [Zr, Nb (W or Mo or V)] 2Fe, Zr (Fe, Cr, Nb) 2, (Zr, Nb) 2Fe type iron content contains the particle and the αGu Rongti of the intermetallic compound of niobium.
CN99816580A 1999-04-22 1999-10-08 Zirconium based alloy Expired - Lifetime CN1125885C (en)

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RU99107803A RU2141540C1 (en) 1999-04-22 1999-04-22 Zirconium-base alloy

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WO (1) WO2000065117A1 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101260528B (en) * 2007-03-07 2011-04-06 西屋电气有限责任公司 Removal of niobium second phase particle deposits from pickled zirconium-niobium alloys
CN104911378A (en) * 2015-05-25 2015-09-16 常熟锐钛金属制品有限公司 Preparation method of zirconium pipe special for nuclear reactor

Families Citing this family (6)

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Publication number Priority date Publication date Assignee Title
RU2227171C1 (en) 2002-12-23 2004-04-20 Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт неорганических материалов им. акад. А.А. Бочвара" Zirconium niobium oxygen-containing alloy and method of production of such alloy
DE10332239B3 (en) * 2003-07-16 2005-03-03 Framatome Anp Gmbh Zirconium alloy and components for the core of light water cooled nuclear reactors
CN101665886B (en) * 2008-09-04 2011-06-22 中国核动力研究设计院 High temperature overheated steam corrosion resistant zirconium alloy material
CN105018758B (en) * 2015-07-03 2017-03-08 宝鸡市三立有色金属有限责任公司 Srgery grafting zirconium and the preparation method of Zirconium alloy material
RU2675178C1 (en) * 2018-08-15 2018-12-17 Федеральное государственное унитарное предприятие "Всероссийский научно-исследовательский институт авиационных материалов" (ФГУП "ВИАМ") Method of obtaining a semi-finished product from a zirconium based alloy (options)
CN110904359A (en) * 2019-12-18 2020-03-24 佛山科学技术学院 Corrosion-resistant zirconium alloy

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JPH01301830A (en) * 1988-05-30 1989-12-06 Sumitomo Metal Ind Ltd High corrosion-resistant zirconium alloy
JP2726299B2 (en) * 1989-02-14 1998-03-11 日本核燃料開発株式会社 High corrosion resistant zirconium alloy for nuclear reactors
US5125985A (en) * 1989-08-28 1992-06-30 Westinghouse Electric Corp. Processing zirconium alloy used in light water reactors for specified creep rate
SE9103052D0 (en) * 1991-10-21 1991-10-21 Asea Atom Ab Zirconium-based alloys carry components in nuclear reactors
RU2032759C1 (en) * 1993-03-04 1995-04-10 Всероссийский научно-исследовательский институт неорганических материалов им.А.А.Бочвара Zirconium-base material
FR2723965B1 (en) * 1994-08-30 1997-01-24 Cezus Co Europ Zirconium PROCESS FOR THE MANUFACTURE OF ZIRCONIUM ALLOY SHEETS WITH GOOD RESISTANCE TO NODULAR CORROSION AND DEFORMATION UNDER IRRADIATION

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101260528B (en) * 2007-03-07 2011-04-06 西屋电气有限责任公司 Removal of niobium second phase particle deposits from pickled zirconium-niobium alloys
CN104911378A (en) * 2015-05-25 2015-09-16 常熟锐钛金属制品有限公司 Preparation method of zirconium pipe special for nuclear reactor

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UA57878C2 (en) 2003-07-15
CA2365779A1 (en) 2000-11-02
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CN1350597A (en) 2002-05-22
KR20020001838A (en) 2002-01-09
WO2000065117A1 (en) 2000-11-02

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Patentee before: Gosudarstvenny nauchny Tsentr Rossiiskoi Federatsiii Vserossiisky Nauchno-=Issle

CX01 Expiry of patent term
CX01 Expiry of patent term

Granted publication date: 20031029