CN1067729C - Method for preparing zirconium niobium alloy - Google Patents

Method for preparing zirconium niobium alloy Download PDF

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Publication number
CN1067729C
CN1067729C CN98117560A CN98117560A CN1067729C CN 1067729 C CN1067729 C CN 1067729C CN 98117560 A CN98117560 A CN 98117560A CN 98117560 A CN98117560 A CN 98117560A CN 1067729 C CN1067729 C CN 1067729C
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zirconium
niobium
electrode
alloy
bar
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CN1213008A (en
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刘建章
薛祥义
李佩志
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Northwest Institute for Non Ferrous Metal Research
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Northwest Institute for Non Ferrous Metal Research
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Abstract

The present invention relates to a method for preparing a zirconium-niobium alloy, which is used for the preparation process of a non-ferrous binary alloy. The present invention comprises: zirconium sponge is pressed into zirconium electrodes; the present invention is characterized in that prepared niobium bars, which have the length of equal to that of the zirconium electrode, and the zirconium electrodes are welded into zirconium-niobium composite electrode bars; the zirconium niobium composite electrode bars are welded into consumable electrodes, and then the consumable electrodes are smelted. The present invention has simple technical process, the prepared zirconium-niobium alloy has accurate ingredient, and the present invention is an ideal method for preparing a zirconium-niobium alloy.

Description

A kind of preparation method of zirconium-niobium alloy
A kind of preparation method of zirconium-niobium alloy relates to a kind of preparation method who is used for the non-ferrous metal binary alloy of nuclear reactor, particularly adds the method for niobium in the zirconium metal.
At present, in the preparation process of existing zirconium-niobium alloy, the adding of niobium is to add with the form of Zr-Nb master alloy in its alloy.Its concrete grammar is at first selected short grained atomic level zirconium sponge and the pure niobium of scutellate refining, press the proportioning of 60%Nb-40%Zr, in the non-consumable arc furnace or the copper crucible in the weldering case of vacuum argon filling, with electric arc make that it is melt-blended, solidify, melt-blended, resolidification again, repeated multiple times, till be sure oing both mix, be cooled to room temperature.Be machined into chip after the taking-up.When the compacting electrode, be the centre that strip is clipped in zirconium sponge by the amount of calculating with pure zirconium paper tinsel parcel master alloy, be pressed into electrode, be smelted into ingot twice through vacuum consumable electrode arc furnace then.This alloy preparation method at first needs preparation and melting master alloy, and complex process is wanted artificial spreading master alloy during the compacting electrode, and the granulous master alloy drops out easily, influences the accuracy of alloy ingredient.And the master alloy alloy only is present on the medullary ray of electrode, is not easy to stir, and easily causes the segregation of alloy ingredient.
Purpose of the present invention is exactly the complex process that exists among the preparation method who overcomes above-mentioned zirconium-niobium alloy, be difficult to accurately control alloying constituent, cause the shortcoming of composition segregation easily, provide a kind of new method simple, can accurately control alloy ingredient, effectively reduce the preparation method of the existing zirconium-niobium alloy of composition segregation.
The objective of the invention is to be achieved through the following technical solutions.
A kind of preparation method of zirconium-niobium alloy, the weight ratio that this zirconium-niobium alloy contains niobium is 0.35%-2.8%, it is characterized in that preparation process is: a. selects the zirconium sponge of atomic level, through removing impurity, cleaning, vacuum drying, being pressed into zirconium electrode; B. with atomic level niobium bar, purify, become ingot, pass through forging, hot rolling, cold rolling one-tenth niobium plate then through electron beam furnace; C. the niobium plate is cut into the niobium bar identical, the niobium bar tightly is attached on the zirconium electrode with zirconium electrode length, in vacuum argon filling weldering case, that the niobium bar is welded together with zirconium electrode then, make zirconium niobium combined electrode rod; D. the zirconium niobium combined electrode rod that makes is welded into consumable electrode, will makes consumable electrode and in consumable electrode vacuum furnace, carry out melting, obtain zirconium-niobium alloy.
The preparation method of a kind of zirconium-niobium alloy of the present invention, its technological process is simple, saved the process of preparation master alloy in the prior art, adopt alloy preparation method of the present invention, overcome artificial spreading master alloy, the granulous master alloy drops out the shortcoming of the inaccurate and composition segregation of the alloy ingredient that causes, and the zirconium-niobium alloy composition of preparation is accurate, being evenly distributed, is a kind of preparation method of more satisfactory zirconium-niobium alloy.
Below in conjunction with example method of the present invention is described further.
A kind of preparation method of zirconium-niobium alloy, the weight ratio that this zirconium-niobium alloy contains niobium is 0.35%-2.8%, preparation process is: a. selects the zirconium sponge of atomic level, through removing impurity, cleaning, vacuum drying, being pressed into zirconium electrode; B. with atomic level niobium bar, purify, become ingot, pass through forging, hot rolling, cold rolling one-tenth niobium plate then through electron beam furnace; C. the niobium plate is cut into the niobium bar identical with zirconium electrode length; The niobium bar tightly is attached on the zirconium electrode, in vacuum argon filling weldering case, that the niobium bar is welded together with zirconium electrode then, make zirconium niobium combined electrode rod; D. the zirconium niobium combined electrode rod that makes is welded into consumable electrode, will makes consumable electrode and in consumable electrode vacuum furnace, carry out melting, obtain zirconium-niobium alloy.
Embodiment 1
The preparation of Zr-1.0% (weight) Nb alloy is an example with the alloy pig of preparation 27kg.
Get atomic level zirconium sponge 2970g, on 500 tons of oil presses, be pressed into the electrode bar of long 300mm, amount to 9.
Get atomic level niobium bar, after the electron beam furnace purification, becoming ingot, through forging, hot rolling, cold rolling one-tenth niobium plate; The niobium plate is cut into the niobium bar identical with zirconium electrode length, and every is of a size of 1mm * 5.8mm * 300mm, and weight is 15g, amounts to 18.
Get two niobium bars and tightly invest on the zirconium electrode surface, in vacuum argon filling weldering case, the niobium bar is welded together with zirconium electrode then, make zirconium niobium combined electrode rod;
The zirconium niobium compound bar welding that makes is fused into electrode, in consumable electrode vacuum furnace, carries out melting.Through twice vacuum melting, the zirconium-niobium alloy niobium content analytical results that obtains is 0.93%~1.10% (weight).Satisfy the composition scope (containing niobium 0.90%~1.10%) of alloy requirement.
Embodiment 2
The preparation of Zr-2.5% (weight) Nb alloy is an example with the alloy pig of preparing 27kg.
Get the atomic level zirconium sponge, be pressed into the electrode bar of long 300mm on 500 tons of oil presses, every heavy 2925g amounts to 9.
Get atomic level niobium bar, after the electron beam furnace purification, becoming ingot, pass through forging, hot rolling, cold rolling one-tenth niobium plate again; The niobium plate is cut into the niobium bar identical with zirconium electrode length, and every is of a size of 1mm * 14.6mm * 300mm, and weight is 37.5g, amounts to 18.
Get two niobium bars and tightly invest on the electrode surface, in vacuum argon welding case, the niobium bar is welded together with zirconium electrode then, make zirconium niobium combined electrode rod;
The zirconium niobium compound bar welding that makes is fused into electrode, in consumable electrode vacuum furnace, carries out melting.Through three vacuum melting, the zirconium-niobium alloy niobium content analytical results that obtains is 2.45%~2.60%.Satisfy the composition scope (containing niobium 2.40%~2.80%) of alloy requirement.
Embodiment 3
The preparation of Zr-0.5% (weight) Nb alloy is an example with the alloy pig of preparing 27kg.
Get atomic level zirconium sponge 2985g, get pure niobium bar 15g and make and be of a size of 0.5mm * 11.6mm * 300mm niobium bar.
The 1493g zirconium sponge is poured in the electrode pressing mold, put into pure niobium sheet after shakeouing, pour other 1493g zirconium sponge again into, be placed on the combined electrode rod that is pressed into long 300mm on the 500t oil press, every heavy 300g amounts to 9.
The zirconium niobium compound bar that makes is welded into consumable electrode, in consumable electrode vacuum furnace, carries out melting.Through twice vacuum melting, the zirconium-niobium alloy niobium content interpretation of result that obtains is 0.48%~0.55%, satisfies the composition scope (containing niobium 0.35%~0.65%) of alloy requirement.

Claims (1)

1. the preparation method of a zirconium-niobium alloy, the weight ratio that this zirconium-niobium alloy contains niobium is 0.35%-2.8%, it is characterized in that preparation process is:
A. select the zirconium sponge of atomic level, through removing impurity, cleaning, vacuum drying, being pressed into zirconium electrode;
B. with atomic level niobium bar, purify, become ingot, pass through forging, hot rolling, cold rolling one-tenth niobium plate then through electron beam furnace;
C. the niobium plate is cut into the niobium bar identical, the niobium bar tightly is attached on the zirconium electrode with zirconium electrode length, in vacuum argon filling weldering case, that the niobium bar is welded together with zirconium electrode then, make zirconium niobium combined electrode rod;
D. the zirconium niobium combined electrode rod that makes is welded into consumable electrode, will makes consumable electrode and in consumable electrode vacuum furnace, carry out melting, obtain zirconium-niobium alloy.
CN98117560A 1998-08-25 1998-08-25 Method for preparing zirconium niobium alloy Expired - Fee Related CN1067729C (en)

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CN1067729C true CN1067729C (en) 2001-06-27

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103650658B (en) * 2004-12-27 2010-11-10 西北有色金属研究院 A kind of Zr-Sn-Nb-Fe-Cr alloys homogenize method of smelting

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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
CN100529150C (en) * 2007-12-17 2009-08-19 西部金属材料股份有限公司 Method for preparing niobium sheet metal strip
CN101701298B (en) * 2009-10-29 2012-10-24 国核宝钛锆业股份公司 Manufacture method of nuclear grade zirconium-niobium alloy cast ingot
CN101831565A (en) * 2010-05-17 2010-09-15 宝鸡市众邦稀有金属材料有限公司 New process for preparing niobium-zirconium 10 alloy
CN102000806B (en) * 2010-12-13 2012-10-17 西安群德新材料科技有限公司 Industrial preparation method of titanium alloy casting ingot with high niobium content
CN103498062B (en) * 2013-09-05 2015-10-28 宝鸡天博金属材料有限公司 A kind of preparation method of niobium-zirconium 10 alloy
CN105950912B (en) * 2016-06-30 2017-12-22 西部超导材料科技股份有限公司 A kind of preparation method of medical Zr 2.5Nb alloy cast ingots
CN106676297A (en) * 2017-03-24 2017-05-17 南昌专腾科技有限公司 Smelting method and system for zirconium niobium lead alloy
CN106801155B (en) * 2017-03-24 2019-05-21 南昌专腾科技有限公司 A kind of smelting process and system of zirconium-niobium alloy
CN112011700B (en) * 2020-09-03 2022-03-22 西部新锆核材料科技有限公司 Method for adding zirconium alloy ingot casting alloy elements
CN114645148B (en) * 2022-03-28 2023-05-05 西部钛业有限责任公司 Preparation method of intermediate alloy for R60705 zirconium alloy cast ingot

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0065816A2 (en) * 1981-04-20 1982-12-01 Comisiòn Nacional de Energia Atòmica Zirconium based alloy

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0065816A2 (en) * 1981-04-20 1982-12-01 Comisiòn Nacional de Energia Atòmica Zirconium based alloy

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103650658B (en) * 2004-12-27 2010-11-10 西北有色金属研究院 A kind of Zr-Sn-Nb-Fe-Cr alloys homogenize method of smelting

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