CN102703740A - Preparation method for Cu-Cr-Zr alloy - Google Patents
Preparation method for Cu-Cr-Zr alloy Download PDFInfo
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- CN102703740A CN102703740A CN2012102069110A CN201210206911A CN102703740A CN 102703740 A CN102703740 A CN 102703740A CN 2012102069110 A CN2012102069110 A CN 2012102069110A CN 201210206911 A CN201210206911 A CN 201210206911A CN 102703740 A CN102703740 A CN 102703740A
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Abstract
The invention belongs to the technical field of alloy and particularly discloses a preparation method for Cu-Cr-Zr alloy. The preparation method comprises the following steps of: firstly at the atmospheric conditions, pouring a pure copper solution into a crucible which contains Zr particles or zirconium sponge, and preparing a copper coating of Zr; afterwards, smelting the copper coating of Zr under a vacuum condition, and preparing Cu-Zr alloy; and mixing the prepared Cu-Zr alloy and Cu-Cr alloy, smelting at the vacuum condition, and preparing the Cu-Cr-Zr alloy. The preparation method for the Cu-Cr-Zr alloy has the advantages that the loss of Zr elements is effectively reduced in the smelting process of the alloy, the yield of the Zr elements is increased, the production cost of the Cu-Cr-Zr alloy is reduced, simultaneously the distribution of the Zr elements in the prepared Cu-Cr-Zr alloy is more uniform, the structural homogenity of the Cu-Cr-Zr alloy is good, and the operational performance of the Cu-Cr-Zr alloy is increased.
Description
Technical field
The present invention relates to the alloy technology field, be specifically related to a kind of preparation method of Cu-Cr-Zr alloy.
Background technology
The Cu-Cr-Zr alloy has under the condition of certain intensity, can keep the very characteristics of high conductivity, is therefore bringing into play huge effect in fields such as power cord, resistance welding electrode, unicircuit and lead frames, has also obtained broad research about its preparation method.
At present the preparation method of Cu-Cr-Zr alloy mainly contains two kinds, and a kind of is to prepare the Cu-Cr-Zr alloy with the direct melting of distribution that pure Cu, pure Zr add pure Cr; Another kind is to prepare the Cu-Cr-Zr alloy with the distribution melting that the Cu-Cr alloy adds pure Zr (or zirc sponge).The difficult point of preparation Cu-Cr-Zr alloy is the yield of active element Zr and evenly interpolation at present.The Zr element is a kind of very active element, and is strong with the avidity of oxygen, in air, very easily forms zirconium white, and except rare gas element, all gas at high temperature can both react with Zr.Therefore, when melting prepared the Cu-Cr-Zr alloy in atmosphere, Zr can react with airborne oxygen, nitrogen etc., causes the loss of Zr element serious, and its yield is lower.In order to overcome the low problem of the Zr element yield that causes owing to reactions such as Zr and airborne oxygen; Industry is at present gone up and is adopted vacuum melting preparation method, controlled atmosphere protection melting preparation method etc. when producing the Cu-Cr-Zr alloy; These preparing method's common characteristic are meltings under vacuum or protective atmosphere, to reduce the loss of Zr element.The method of industrial production Cu-Cr-Zr alloy is at present: adopt the distribution of pure Cr of the pure Zr+ of pure Cu+ or Cu-Cr alloy+pure Zr (or zirc sponge), in crucible, adopt vacuum melting preparation method or controlled atmosphere protection melting preparation method etc. to carry out melting and prepare the Cu-Cr-Zr alloy.But because the fusing point of Cu is 1357K; The fusing point of Cr, Zr is respectively 2176K and 2125K, and under the normal smelting temperature, Cr and Zr are infusible; But the hot stage before the Cu fusing; Vacuum melting preparation method preparation meeting is because the suction function of vacuum condition causes the volatilization of Zr element and causes loss, controlled atmosphere protection melting preparation method preparation meeting because of oxygen in the air and nitrogen through diffusing into shielding gas, in shielding gas or at the interface of shielding gas and melt; Chemical reaction can take place in oxygen and nitrogen and diffusion or the Zr element that evaporates, thereby causes the loss of Zr element.Therefore, the yield of the working method Zr of Cu-CrZr alloy is not very high at present.In addition, that add when preparing the Cu-Cr-Zr alloy owing to melting at present is blocky Zr, and Zr is infusible under normal smelting temperature; Therefore Zr leans on the difference of concentration gradient slowly to spread, if smelting time is too short, the diffusion of Zr alloying element is insufficient; The Zr element will gather with block-shape morphology partially; Cause the inhomogeneous of Cu-Cr-Zr alloying constituent, can cause Zr, the loss of Cr element excessive if smelting time is long, and power consumption increases.
Therefore, when preparation Cu-Cr-Zr alloy, how to reduce the loss of Zr element, improve Zr element yield, realize that simultaneously the homodisperse of Zr element in the Cu-Cr-Zr alloy is problem anxious to be solved in the present Cu-Cr-Zr alloy preparation.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of Cu-Cr-Zr alloy.
In order to realize above purpose, the technical scheme that the present invention adopted is: a kind of preparation method of Cu-Cr-Zr alloy may further comprise the steps:
(1) under atmospheric condition; With the fine copper fusing, process the fine copper liquation, then said fine copper liquation is poured in the crucible that Zr grain or zirc sponge are housed; Zr grain or zirc sponge are coated by the fine copper liquation, and naturally cooling makes the copper clad thing of solid-state Zr under atmospheric condition;
(2) the copper clad thing of the Zr that makes of step (1) carries out melting under vacuum condition, and smelting temperature is controlled to be 1350～1365 ℃, makes the Cu-Zr alloy;
(3) said Cu-Zr alloy mixes with the Cu-Cr alloy, under vacuum condition, carries out melting, and smelting temperature is controlled to be 1360～1370 ℃, makes the Cu-Cr-Zr alloy.
Zr grain or zirc sponge described in the step (1) can adopt Zr grain and pure Cr or zirc sponge and pure Cr to substitute.
For guaranteeing that melting carries out unaffectedly, adopt melting under the vacuum condition during the said melting of step (2) and step (3), its vacuum tightness is preferably 8～12Pa.
Operating under the atmospheric condition in the step (1) carried out, and carries out under the needing no vacuum condition or adopts protection of inert gas, and be easy and simple to handle.
In order to improve the Cr content in the Cu-Cr-Zr alloy that makes, in the time of can in step (1), preparing the copper clad thing of Zr, the Cr that need are added adopts form and the Zr of pure Cr to put together and coats.
Among the preparation method of Cu-Cr-Zr alloy of the present invention; If smelting temperature is low excessively; Can cause the velocity of diffusion of Zr element in the Cu matrix slack-off; Cause Zr element skewness on whole base material easily,, reduce the mechanical property of institute's molten alloy if the too high alloy structure crystal grain that then causes easily of temperature is thick even organize overheatedly.Therefore limiting step 2) smelting temperature of the copper clad thing of Zr is 1350～1365 ℃.
Because exist suddenly Zr and two kinds of alloys of Cr of preparation method of the present invention add element; There is mutual cross influence in its diffusion process; And the increase of alloying element can make the fusing point of alloy slightly improve, and is more abundant for alloying element is spread within a certain period of time, improves final preparation alloy organizing homogeneity; Its smelting temperature has improved about 5 ℃ than the smelting temperature of Cu-Zr master alloy; Can cause alloying element skewness in matrix if smelting temperature is crossed to hang down,, cause the preparation alloy mechanical property to decline to a great extent if smelting temperature is too high can to cause that then alloy grain is thick even it is overheated to organize.Therefore limit step 3) Cu-Zr alloy and Cu-Cr alloy mixed smelting temperature is 1360～1370 ℃.
The preparation method of Cu-Cr-Zr alloy provided by the invention has the following advantages:
One, coats the copper clad thing of Zr granules prepn Zr through copper liquid, Zr particle moment is among copper liquid coats, avoided the loss that the Zr element causes because of volatilization or chemical reaction in the existing melting technology in heat-processed with fusing;
Two, the copper clad thing of melting Zr prepares the Cu-Zr alloy under vacuum condition; Because the Zr particle is by copper clad; In fusion process, the Zr element is to spread to surface or top from the heart portion of the copper clad thing of Zr or bottom, in the most of the time of alloy melting; The Zr constituent content of alloy surface is very low, has effectively reduced the volatilization or the chemical reaction of Zr element;
Three, the distribution that the preparation method who adopts Cu-Cr alloy and Cu-Zr alloy mixed smelting to carry out the Cu-Cr-Zr alloy compares the pure Cr of the pure Zr+ of the pure Cu+ of existing usefulness or Cu-Cr alloy+pure Zr (or zirc sponge) directly prepares the melting method of Cu-Cr-Zr alloy; Because the Zr element has carried out Zr elemental diffusion process one time in preparation Cu-Zr alloy process; The dispersion of Zr element is more uniform in the Cu-Zr alloy; Prepare in the process of Cu-Cr-Zr alloy at next step and Cu-Cr alloy mixed smelting; The homodisperse speed of Zr in the Cu-Cr-Zr alloy will directly prepare the velocity of diffusion of pure Zr grain in the Cu-Cr-Zr alloy in the melting method of Cu-Cr-Zr alloy far above the distribution of the pure Cr of the pure Zr+ of the pure Cu+ of existing usefulness or Cu-Cr alloy+pure Zr (or zirc sponge); Therefore the preparation method of Cu-Cr-Zr alloy provided by the invention has not only significantly shortened the melting soaking time of Cu-Cr-Zr alloy; And then reduced the loss of Zr element in the high melt process, also guaranteed the uniform distribution of Zr element in alloy simultaneously.
The preparation method of Cu-Cr-Zr alloy provided by the invention has effectively reduced the loss of precious metal Zr element in the alloy melting process; The yield of Zr element obviously is provided; Reduced the production cost of Cu-Cr-Zr alloy; Adopt the more even distribution of Zr element in the Cu-Cr-Zr alloy that the preparation method of Cu-Cr-Zr alloy provided by the invention makes simultaneously, Cu-Cr-Zr alloy organizing good uniformity has improved the use properties of Cu-Cr-Zr alloy.
Description of drawings
The ESEM surface analysis figure of the Cu-Cr-Zr alloy that Fig. 1 makes for the embodiment of the invention 1;
The ESEM surface analysis figure of the Cu-Cr-Zr alloy that Fig. 2 makes for Comparative Examples of the present invention.
Embodiment
Embodiment 1
Present embodiment provides a kind of preparation method of Cu-Cr-Zr alloy, and concrete steps are:
(1) under atmospheric condition, with the fine copper fusing, process the fine copper liquation, then the fine copper liquation is poured in the crucible that the Zr grain is housed, the Zr grain is coated by the fine copper liquation, and naturally cooling makes the copper clad thing of solid-state Zr under atmospheric condition;
(2) the copper clad thing of the Zr that makes of step (1) carries out melting under vacuum condition, and vacuum tightness is 8Pa, and smelting temperature is controlled to be 1350 ℃, makes the Cu-Zr alloy;
(3) the Cu-Zr alloy that makes of step (2) mixes with the Cu-Cr alloy, under vacuum condition, carries out melting, and vacuum tightness is 9Pa, and smelting temperature is controlled to be 1365 ℃, makes the Cu-Cr-Zr alloy.
Embodiment 2
Present embodiment provides the preparation method of another kind of Cu-Cr-Zr alloy, and concrete steps are:
(1) under atmospheric condition, with the fine copper fusing, process the fine copper liquation, then the fine copper liquation is poured in the crucible that zirc sponge is housed, zirc sponge is coated by the fine copper liquation, and naturally cooling makes the copper clad thing of solid-state Zr under atmospheric condition;
(2) the copper clad thing of the Zr that makes of step (1) carries out melting under vacuum condition, and vacuum tightness is 10Pa, and smelting temperature is controlled to be 1365 ℃, makes the Cu-Zr alloy;
(3) the Cu-Zr alloy that makes of step (2) mixes with the Cu-Cr alloy, under vacuum condition, carries out melting, and vacuum tightness is 11Pa, and smelting temperature is controlled to be 1370 ℃, makes the Cu-Cr-Zr alloy.
Embodiment 3
Present embodiment provides the preparation method of another kind of Cu-Cr-Zr alloy, and concrete steps are:
(1) under atmospheric condition, with the fine copper fusing, process the fine copper liquation, then the fine copper liquation is poured in the crucible that zirc sponge is housed, zirc sponge is coated by the fine copper liquation, and naturally cooling makes the copper clad thing of solid-state Zr under atmospheric condition;
(2) the copper clad thing of the Zr that makes of step (1) carries out melting under vacuum condition, and vacuum tightness is 12Pa, and smelting temperature is controlled to be 1355 ℃, makes the Cu-Zr alloy;
(3) the Cu-Zr alloy that makes of step (2) mixes with the Cu-Cr alloy, under vacuum condition, carries out melting, and vacuum tightness is 12Pa, and smelting temperature is controlled to be 1360 ℃, makes the Cu-Cr-Zr alloy.
Comparative Examples
Adopt the method for existing industrial production Cu-Cr-Zr alloy to prepare the Cu-Cr-Zr alloy, concrete grammar is: adopt the distribution of Cu-Cr alloy+pure Zr grain, in crucible, adopt the vacuum melting preparation method to carry out melting and prepare the Cu-Cr-Zr alloy.
Embodiment 1 is analyzed comparison with the Cu-Cr-Zr alloy that Comparative Examples makes, and the sem photograph of the Cu-Cr-Zr alloy that embodiment 1 makes is seen shown in Figure 1, and the sem photograph of the Cu-Cr-Zr alloy that Comparative Examples makes is seen shown in Figure 2.
Among the embodiment 1 when preparation Cu-Cr-Zr alloy in the employed raw material consumption proportion of Cu, Cr and three kinds of elements of Zr be: the weight percentage of Zr element is 0.7%, and the weight percentage of Cr element is 1.5%, and surplus is Cu.The Cu-Cr-Zr alloy that embodiment 1 finally makes is through actual detected, and wherein the weight percentage of Zr is 0.52%, and the weight percentage of Cr is 1.13%, and surplus is Cu.The yield of Zr is 74.28%.
In the Comparative Examples when preparation Cu-Cr-Zr alloy in the employed raw material consumption proportion of Cu, Cr and three kinds of elements of Zr be: the weight percentage of Zr element is 0.7%, and the weight percentage of Cr element is 1.5%, and surplus is Cu.The Cu-Cr-Zr alloy that Comparative Examples finally makes is through actual detected, and wherein the weight percentage of Zr is 0.40%, and the weight percentage of Cr is 1.12%, and surplus is Cu.The yield of Zr is 57.14%.
The preparation method of the Cu-Cr-Zr alloy that embodiment 1 provides reaches more than 17% than the yield raising of Comparative Examples preparing method's Zr, and the yield of Zr significantly improves.
Can know according to the Cu-Zr binary alloy phase diagram; The Zr of close-packed hexagonal and face-centred cubic Cu dissolve each other at normal temperatures hardly, and the Zr element mainly is to distribute along crystal boundary in whole C u-Zr binary alloy, when Zr content acquires a certain degree; The Zr element can be enriched in together, in pelletized form or block the existence.Can find out that through Fig. 1 and Fig. 2 the Zr element distributes and all compares evenly in the Cu-Cr-Zr alloy that embodiment 1 and Comparative Examples make, the Zr element is disperse and distributes in whole C u-Cr-Zr alloy, have only a spot of enrichment Zr particulate granular structure to exist.But through Fig. 1 and Fig. 2 are compared and can find out; Though the Cu-Cr-Zr Zr content that the Cu-Cr-Zr Zr content that embodiment 1 makes makes apparently higher than Comparative Examples; But enrichment Zr particulate granular structure does not increase in the Cu-Cr-Zr alloy that embodiment 1 makes; This explanation Zr element distribution in the Cu-Cr-Zr alloy that embodiment 1 makes is the more even distribution in the Cu-Cr-Zr alloy that Comparative Examples makes, the Cu-Cr-Zr alloy that the Cu-Cr-Zr alloy organizing good uniformity that embodiment 1 makes makes in Comparative Examples.
Claims (4)
1. the preparation method of a Cu-Cr-Zr alloy is characterized in that, may further comprise the steps:
(1) under atmospheric condition; With the fine copper fusing, process the fine copper liquation, then said fine copper liquation is poured in the crucible that Zr grain or zirc sponge are housed; Zr grain or zirc sponge are coated by the fine copper liquation, and naturally cooling makes the copper clad thing of solid-state Zr under atmospheric condition;
(2) the copper clad thing of the Zr that makes of step (1) carries out melting under vacuum condition, and smelting temperature is controlled to be 1350～1365 ℃, makes the Cu-Zr alloy;
(3) said Cu-Zr alloy mixes with the Cu-Cr alloy, under vacuum condition, carries out melting, and smelting temperature is controlled to be 1360～1370 ℃, makes the Cu-Cr-Zr alloy.
2. the preparation method of Cu-Cr-Zr alloy according to claim 1 is characterized in that, Zr grain or zirc sponge described in the step (1) can adopt Zr grain and pure Cr or zirc sponge and pure Cr to substitute.
3. the preparation method of Cu-Cr-Zr alloy according to claim 1 is characterized in that, the vacuum tightness of the said melting of step (2) is 8～12Pa.
4. the preparation method of Cu-Cr-Zr alloy according to claim 1 is characterized in that, the vacuum tightness of the said melting of step (3) is 8～12Pa.
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| CN102899521A (en) * | 2012-11-09 | 2013-01-30 | 华东理工大学 | Copper-chromium-zirconium alloy material and preparation method thereof |
| CN103938002A (en) * | 2014-03-17 | 2014-07-23 | 中国船舶重工集团公司第七二五研究所 | Segregation reducing vacuum melting technology of Cu-Cr-Zr alloy cast rod |
| US20170342546A1 (en) * | 2015-05-21 | 2017-11-30 | Jx Nippon Mining & Metals Corporation | Copper alloy sputtering target and method for manufacturing same |
| CN114472904A (en) * | 2022-04-01 | 2022-05-13 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of CuCrZr spherical powder for 3D printing |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899521A (en) * | 2012-11-09 | 2013-01-30 | 华东理工大学 | Copper-chromium-zirconium alloy material and preparation method thereof |
| CN103938002A (en) * | 2014-03-17 | 2014-07-23 | 中国船舶重工集团公司第七二五研究所 | Segregation reducing vacuum melting technology of Cu-Cr-Zr alloy cast rod |
| CN103938002B (en) * | 2014-03-17 | 2016-01-27 | 洛阳双瑞特种合金材料有限公司 | A kind of Cu-Cr-Zr alloy casting rod reduces the vacuum melting technique of segregation |
| US20170342546A1 (en) * | 2015-05-21 | 2017-11-30 | Jx Nippon Mining & Metals Corporation | Copper alloy sputtering target and method for manufacturing same |
| US10494712B2 (en) * | 2015-05-21 | 2019-12-03 | Jx Nippon Mining & Metals Corporation | Copper alloy sputtering target and method for manufacturing same |
| CN114472904A (en) * | 2022-04-01 | 2022-05-13 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of CuCrZr spherical powder for 3D printing |
| CN114472904B (en) * | 2022-04-01 | 2022-07-29 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of CuCrZr spherical powder for 3D printing |
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