CN102426938A - Electrical contact material and method for preparing CuZrW electrical contact material by adopting infiltration method - Google Patents

Electrical contact material and method for preparing CuZrW electrical contact material by adopting infiltration method Download PDF

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CN102426938A
CN102426938A CN2011102731436A CN201110273143A CN102426938A CN 102426938 A CN102426938 A CN 102426938A CN 2011102731436 A CN2011102731436 A CN 2011102731436A CN 201110273143 A CN201110273143 A CN 201110273143A CN 102426938 A CN102426938 A CN 102426938A
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powder
cuzrw
tungsten
cast ingot
sintering
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CN102426938B (en
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杨晓红
梁淑华
肖鹏
邹军涛
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Xian University of Technology
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Xian University of Technology
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Abstract

The invention discloses an electrical contact material. A CuZrW composite material is formed by utilizing a CuZr alloy to infiltrate a W framework, wherein the content of Zr in a Cu phase of the material is 1-4.0 wt.% in percentage by mass. The method for preparing the electrical contact material comprises the following steps of: firstly, smelting a certain content of CuZr alloy; adding a certain ratio of induction copper powder into tungsten powder to be uniformly mixed and preparing the mixed powder into a framework green body; and then, sintering the W framework and infiltrating the smelted CuZr alloy into the W framework to prepare the CuZrW material; and finally, carrying out a solution and ageing treatment on the CuZrW material. According to the method provided by the invention, anode spots on the surface of the prepared CuZrW material move rapidly due to strengthening effects on a Cu/W phase interface and a copper-enriched area by the element Zr, electric arcs are effectively dissipated, the splashing of the copper phase is smaller, and the erosion-resistant performance of the material is improved.

Description

Electrical contact material and employing infiltration method prepare the method for CuZrW electrical contact material
Technical field
The invention belongs to technical field of material, relate to a kind of electrical contact material, the invention still further relates to the preparation method of this CuZrW electrical contact material.
Background technology
The CuW material has good heat-conductivity conducting property, good advantages such as arc ablation resistance property, resistance fusion welding and high strength, extensively is used as the electrical contact material in the primary cut-out.Along with the development of high-voltage switch gear, to the higher requirement of combination property proposition of its core component-CuW contact material towards big capacity, high voltage, low overvoltage, miniaturization.Existing research shows that the electrical breakdown of CuW alloy often occurs on the weak puncture phase Cu or on the Cu/W boundary.Through adding the alloying element that can mix with W again with Cu, make the Cu/W boundary produce microalloying on the one hand, reach the effect of strengthening copper matrix phase on the other hand, can play dispersion surface vacuum electric arc, reduce the purpose of the concentrated ablation of electrical contact.
Summary of the invention
The purpose of this invention is to provide a kind of electrical contact material, solved the problem that electrical breakdown takes place existing electrical contact material easily.
Another object of the present invention provides the preparation method of above-mentioned CuZrW electrical contact material.
The technical scheme that the present invention adopted is, this material is made up of CuW alloy and Zr, and the quality percentage composition that described Zr accounts for Cu in the CuW alloy is 1~4.0wt.%.
Another technical scheme that the present invention adopted is, material preparation method carries out according to the following steps,
Preparation CuZr alloy cast ingot
A. get copper powder and Zr powder respectively, the quality percentage composition that Zr accounts for copper is 1~4.0wt%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact;
B. the green compact that step a made are put into corundum crucible, place to carry out melting in the argon gas atmosphere stove, and smelting temperature is 1150~1300 ℃, are incubated and cool to room temperature with the furnace after 0.5~2 hour, make the CuZr alloy cast ingot;
C. the CuZr alloy cast ingot that step b is made is removed the various defectives on the alloy pig through machine work, cleans up;
Preparation tungsten pressed compact
A, get tungsten powder and induce copper powder respectively; Induce copper powder to account for 5~8% of tungsten powder quality, with tungsten powder with induce copper powder to put into mixing tank, add abrading-ball and batch mixing process control agent; The amount that adds the batch mixing process control agent makes powder have moist feeling to get final product, mixing time 5~7 hours;
B, the compound that step a is mixed are poured in the steel die of axial compacting, are molded into the tungsten pressed compact with the pressure of 340 ± 20MPa;
Sintering, infiltration and reprocessing
A, will go up the CuZr alloy cast ingot and the tungsten pressed compact that clean up of step and stack together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 900 ℃~1000 ℃, and sintering time is 1.5~2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1200 ℃~1400 ℃, and the infiltration time is 1.5~2 hours, obtains the CuZrW alloy material;
B, will go up the CuZrW material that obtains of step and place heat-treatment furnace to carry out solution treatment, solid solubility temperature is 900~1000 ℃, and insulation 1~2.5h opens fire door subsequently high temperature CuZrW material is carried out shrend;
C. will go up CuZrW material after the step quenches and place and carry out Ageing Treatment in the heat-treatment furnace, aging temp is 400~500 ℃, be incubated after 3~5 hours to cool off with stove;
D. the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Wherein prepare among the step a of tungsten pressed compact, the mill ball quality of adding is tungsten powder and copper powder gross mass 2~3 times.
Wherein prepare among the step a of tungsten pressed compact, the batch mixing process control agent of adding is an industrial alcohol.
Prepare wherein that the Cu powder is that purity is not less than 99.9% electrolysis Cu powder among the step a of CuZr alloy cast ingot, the Zr powder is that purity is not less than 99% Zr powder.
Electrical contact material of the present invention through adding element Zr, is realized the invigoration effect of Cu/W boundary and the weak breakdown area of copper rich region, the dispersion that helps material surface electric arc with reduce copper splashing mutually, thereby the arc ablation resistance performance of raising electrical contact material.
Description of drawings
Fig. 1 is the flow chart of CuZrW material preparation method of the present invention;
Among Fig. 2, a is the CuZrW contact material microstructure picture figure that the present invention prepares, and b is this line of material scanning ability spectrogram;
Fig. 3 is the first cathode spot movement figure that punctures of existing CuW contact material;
Fig. 4 is the first cathode spot movement figure that punctures of CuZrW contact material of the present invention;
Fig. 5 is the ablation pattern contrast photo after the first puncture of material, and a is the CuW material, and b is the CuZrW material.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is elaborated.
CuZrW electrical contact material of the present invention, this material is made up of CuW alloy and Zr, and the quality percentage composition that Zr accounts for Cu in the CuW alloy is 1~4.0wt.%.
The preparation method of CuZrW electrical contact material of the present invention carries out according to the following steps,
Preparation CuZr alloy cast ingot
A. get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 1~4.0wt%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact;
B. the green compact that step a made are put into corundum crucible, place to carry out melting in the argon gas atmosphere stove, and smelting temperature is 1150~1300 ℃, are incubated and cool to room temperature with the furnace after 0.5~2 hour, make the CuZr alloy cast ingot;
C. the CuZr alloy cast ingot that step b is made is removed the various defectives on the alloy pig through machine work, cleans up;
Preparation tungsten pressed compact
A, get tungsten powder and induce copper powder respectively; Induce copper powder to account for 5~8% of tungsten powder quality, with tungsten powder with induce copper powder to put into mixing tank, add abrading-ball and batch mixing process control agent; The mill ball quality that adds is tungsten powder and copper powder gross mass 2~3 times; The amount that adds the batch mixing process control agent makes powder have moist feeling to get final product, mixing time 5~7 hours, and wherein the batch mixing process control agent is an industrial alcohol;
B, the compound that step a is mixed are poured in the steel die of axial compacting, are molded into the tungsten pressed compact with the pressure of 340 ± 20MPa;
Sintering, infiltration and reprocessing
A, will go up the CuZr alloy cast ingot and the tungsten pressed compact that clean up of step and stack together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 900 ℃~960 ℃, and sintering time is 1.5~2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1200 ℃~1400 ℃, and the infiltration time is 1.5~2 hours, obtains the CuZrW alloy material;
B, will go up the CuZrW material that obtains of step and place heat-treatment furnace to carry out solution treatment, solid solubility temperature is 900~1000 ℃, and insulation 1~2.5h opens fire door subsequently high temperature CuZrW material is carried out shrend;
C. will go up CuZrW material after the step quenches and place and carry out Ageing Treatment in the heat-treatment furnace, aging temp is 400~500 ℃, be incubated after 3~5 hours to cool off with stove;
D. the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 1
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 4.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1150 ℃, is incubated and cools to room temperature with the furnace after 0.5 hour, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 6% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 2 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 5 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 330MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 1000 ℃, and sintering time is 1.5 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1200 ℃, and the infiltration time is 2 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 900 ℃, and insulation 1h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 400 ℃, be incubated after 3 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 2
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 2.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1200 ℃, is incubated and cools to room temperature with the furnace after 1 hour, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 5% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 3 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 6 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 350MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 900 ℃, and sintering time is 2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1300 ℃, and the infiltration time is 1.5 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 950 ℃, and insulation 1.5h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 450 ℃, be incubated after 3.5 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 3
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 3.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1250 ℃, is incubated and cools to room temperature with the furnace after 1.5 hours, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 8% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 2.5 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 7 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 320MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 1000 ℃, and sintering time is 2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1350 ℃, and the infiltration time is 1.7 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 980 ℃, and insulation 2h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 480 ℃, be incubated after 4 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 4
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 4.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1300 ℃, is incubated and cools to room temperature with the furnace after 2 hours, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 7% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 2.3 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 5.5 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 360MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 950 ℃, and sintering time is 1.8 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1400 ℃, and the infiltration time is 1.8 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 1000 ℃, and insulation 1h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 500 ℃, be incubated after 4.5 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 5
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 1.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1150 ℃, is incubated and cools to room temperature with the furnace after 2 hours, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 8% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 2 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 6 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 340MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 980 ℃, and sintering time is 1.5 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1300 ℃, and the infiltration time is 2 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 900 ℃, and insulation 1.5h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 400 ℃, be incubated after 5 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 6
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 2.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1200 ℃, is incubated and cools to room temperature with the furnace after 1.5 hours, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 7% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 2.7 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 7 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 340MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 950 ℃, and sintering time is 2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1250 ℃, and the infiltration time is 1.7 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 950 ℃, and insulation 2h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 450 ℃, be incubated after 3 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 7
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 3.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1250 ℃, is incubated and cools to room temperature with the furnace after 1 hour, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 7% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 2.5 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 5 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 340MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 1000 ℃, and sintering time is 1.5 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1400 ℃, and the infiltration time is 2 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 980 ℃, and insulation 1h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 480 ℃, be incubated after 3.5 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 8
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 4.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1300 ℃, is incubated and cools to room temperature with the furnace after 0.5 hour, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 7% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 2 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 5 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 340MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 1000 ℃, and sintering time is 1.5 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1200 ℃, and the infiltration time is 1.5 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 1000 ℃, and insulation 1.5h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 500 ℃, be incubated after 4 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 9
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 1.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1250 ℃, is incubated and cools to room temperature with the furnace after 2 hours, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 8% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 3 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 6.5 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 350MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 980 ℃, and sintering time is 2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1300 ℃, and the infiltration time is 2 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 900 ℃, and insulation 2h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 400 ℃, be incubated after 4.5 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 10
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 2.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1200 ℃, is incubated and cools to room temperature with the furnace after 1 hour, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 7.5% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 3 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 6 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 360MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 1000 ℃, and sintering time is 2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1400 ℃, and the infiltration time is 2 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 950 ℃, and insulation 1h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 450 ℃, be incubated after 5 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 11
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 3.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1250 ℃, is incubated and cools to room temperature with the furnace after 1.5 hours, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 8% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 3 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 7 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 320MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 900 ℃, and sintering time is 2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1250 ℃, and the infiltration time is 1.5 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 980 ℃, and insulation 2.5h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 480 ℃, be incubated after 4 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
Embodiment 12
At first prepare the CuZr alloy cast ingot, get purity respectively and be not less than 99.9% electrolytic copper powder and purity and be not less than 99% Zr powder, the quality percentage composition that Zr accounts for copper is 4.0wt.%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact; The green compact that make are put into corundum crucible, place and carry out melting in the argon gas atmosphere stove, smelting temperature is 1200 ℃, is incubated and cools to room temperature with the furnace after 0.5 hour, makes the CuZr alloy cast ingot; The CuZr alloy cast ingot that makes is removed the various defectives on the alloy pig through machine work, clean up;
Prepare the tungsten pressed compact then, get tungsten powder respectively and induce copper powder, induce copper powder to account for 5% of tungsten powder quality; With tungsten powder with induce copper powder to put into mixing tank; Add abrading-ball and batch mixing process control agent, the mill ball quality of adding is tungsten powder and copper powder gross mass 3 times, and the amount that adds the batch mixing process control agent makes powder have moist feeling to get final product; Mixing time 7 hours, wherein the batch mixing process control agent is an industrial alcohol; Mixed compound is poured in the steel die of axial compacting, be molded into the tungsten pressed compact with the pressure of 320MPa;
Carry out sintering, infiltration and reprocessing afterwards, CuZr alloy cast ingot that cleans up and tungsten pressed compact are stacked together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 900 ℃, and sintering time is 2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1400 ℃, and the infiltration time is 2 hours, obtains the CuZrW alloy material; Place heat-treatment furnace to carry out solution treatment the CuZrW material that obtains, solid solubility temperature is 1000 ℃, and insulation 2h opens fire door subsequently high temperature CuZrW material is carried out shrend; CuZrW material after quenching placed carry out Ageing Treatment in the heat-treatment furnace, aging temp is 500 ℃, be incubated after 3 hours to cool off with stove; At last the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
The CuZrW material that 12 above-mentioned embodiment are prepared carries out conductivity and the hardness of solid solution aging before and after handling to be tested, during the result is listed in the table below:
The hardness number of CuZrW composite material under the different Zr content, conductivity value
Figure BDA0000091566360000161
Can find out that the hardness of CuZrW material also increases with Zr content and rises, conductivity rises with Zr content and descends.But after solid solution aging was handled, hardness improved, and conductivity also rises to some extent.
The CuZrW material surface was after being polished to minute surface before and after solid solution aging was handled; The vacuum chamber of packing into is interior as negative electrode; The use pure W rod of tip-like that diameter is
Figure BDA0000091566360000162
is as anode; Two interpolars apply the direct voltage of voltage 8kV; Make cathode sample with the speed of 0.2mm/min lentamente near anode, until two interpolar generation electrical breakdowns.Take the vacuum breakdown cathode spot movement situation of moment with high-speed photography, use the arc erosion pattern of scanning electron microscopic observation material surface at last, evidence, the sample of embodiment has been realized effective dispersion of electric arc, material has ablation resistance preferably.
Below only through embodiment 5 prepared CuZrW material structure photo and corresponding energy spectrum analysis; With and the electrical breakdown process in cathode spot movement characteristic and the arc erosion pattern of material surface; Explain that the inventive method prepares the advantage of the static properties of CuZrW material (conductivity, hardness) and arc ablation resistance aspect:
A is the microstructure picture of prepared CuZrW material among Fig. 2; Wherein bright grey is the W phase; The continuous phase of Dark grey is the copper phase, and b is corresponding line sweep ability spectrogram among Fig. 2, can find out by spectrogram from its line sweep; Element Zr all exists in mutually with W mutually at Cu, and Zr the content of W in mutually than Cu mutually in the content height.Therefore, the interpolation of element Zr makes originally immiscible Cu/W boundary realize microalloying, has strengthened weak Cu/W boundary, and Zr is added with the raising that is beneficial to CuW material each item performance.On the other hand, after solid solution aging was handled, Zr element residual in the copper matrix can be separated out, and can not cause the too much reduction of material electric conductivity.
Cathode spot movement picture when Fig. 3 for the CuW material that adopts the high-speed photography shooting first the puncture is taken place; Wherein a, b, c, d corresponding respectively 0 μ s, 200 μ s, 350 μ s; 800 μ s are the moving image of cathode protection constantly; Can find out that CuW material cathode protection is always a bright spot, and almost not move in the horizontal direction, almost puncture repeatedly at the initial point place.
Cathode spot movement picture when Fig. 4 for the CuZrW material that adopts the high-speed photography shooting first the puncture is taken place; Wherein a, b, c, d corresponding respectively 0 μ s; 200 μ s, 350 μ s, 800 μ s are the moving image of cathode protection constantly; Can find out that from Fig. 4 b cathode protection generation cracking disperses when 200 μ s.Along with arcing time prolongation cathode protection cracking further takes place until last disappearance.Through finding out with the comparison of Fig. 3 cathode spot movement, to add alloy element Zr and can reach dispersion electric arc, the effect of cracking cathode protection makes and concentrates arc transfer for disperseing electric arc, and this helps improving the ablation resistance of CuW70 alloy.
The first electricity ablation pattern that punctures back CuW material for taking place in Fig. 5 a; Can find out that electrical breakdown mainly occurs in rich Cu zone and Cu/W boundary, these zones are weak puncture phase, are prone to cause electric arc to concentrate and ablate; Cathode protection is difficult for taking place division and moves; Thereby cause comparatively serious concentrated rhegmalypt in contact surface, and copper liquid splash greatlyyer, this will have a strong impact on the useful life of electrical contact material.
The first electricity ablation pattern that punctures back CuZrW material for taking place in Fig. 5 b; Through finding out with the contrast of Fig. 5 a; Electrical breakdown occurs in the copper rich region territory; The Cu/W boundary is because electrical breakdown no longer takes place in the alloy strengthening effect, and because the separating out of Zr on the copper matrix, and the rhegmalypt that cathode protection forms is more shallow and disperse.Weak district-copper rich region of puncture and Cu/W boundary have been strengthened in the interpolation that shows the Zr element, and the cathode protection that produces during electrical breakdown is easy to move at material surface, and electric arc is effectively disperseed, and helps improving the arc ablation resistance performance of electrical contact material.

Claims (5)

1. an electrical contact material is characterized in that, this material is made up of CuW alloy and Zr, and the quality percentage composition that described Zr accounts for Cu in the CuW alloy is 1~4.0wt.%.
2. a method that adopts infiltration method to prepare the CuZrW electrical contact material is characterized in that, this method is carried out according to the following steps,
Preparation CuZr alloy cast ingot
A. get copper powder and Zr powder respectively, the quality percentage composition that Zr accounts for copper is 1~4.0wt%, after copper powder and Zr powder are fully mixed, in rigid die, is pressed into green compact;
B. the green compact that step a made are put into corundum crucible, place to carry out melting in the argon gas atmosphere stove, and smelting temperature is 1150~1300 ℃, are incubated and cool to room temperature with the furnace after 0.5~2 hour, make the CuZr alloy cast ingot;
C. the CuZr alloy cast ingot that step b is made is removed the various defectives on the alloy pig through machine work, cleans up;
Preparation tungsten pressed compact
A, get tungsten powder and induce copper powder respectively; Induce copper powder to account for 5~8% of tungsten powder quality, with tungsten powder with induce copper powder to put into mixing tank, add abrading-ball and batch mixing process control agent; The amount that adds the batch mixing process control agent makes powder have moist feeling to get final product, mixing time 5~7 hours;
B, the compound that step a is mixed are poured in the steel die of axial compacting, are molded into the tungsten pressed compact with the pressure of 340 ± 20MPa;
Sintering, infiltration and reprocessing
A, will go up the CuZr alloy cast ingot and the tungsten pressed compact that clean up of step and stack together, put into the graphite crucible of completing graphite paper, place high temperature H 2In the atmosphere sintering furnace, earlier tungsten pressed compact skeleton is carried out sintering, sintering temperature is 900 ℃~1000 ℃, and sintering time is 1.5~2 hours; Subsequently the CuZr alloy cast ingot is carried out infiltration to W skeleton, infiltrating temperature is 1200 ℃~1400 ℃, and the infiltration time is 1.5~2 hours, obtains the CuZrW alloy material;
B, will go up the CuZrW material that obtains of step and place heat-treatment furnace to carry out solution treatment, solid solubility temperature is 900~1000 ℃, and insulation 1~2.5h opens fire door subsequently high temperature CuZrW material is carried out shrend;
C. will go up CuZrW material after the step quenches and place and carry out Ageing Treatment in the heat-treatment furnace, aging temp is 400~500 ℃, be incubated after 3~5 hours to cool off with stove;
D. the CuZrW material after the Ageing Treatment of last step is machined to and is finished product.
3. according to the described method of claim 2, it is characterized in that among the step a of said preparation tungsten pressed compact, the mill ball quality of adding is tungsten powder and copper powder gross mass 2~3 times.
4. according to the described method of claim 2, it is characterized in that among the step a of said preparation tungsten pressed compact, the batch mixing process control agent of adding is an industrial alcohol.
5. method according to claim 2 is characterized in that, the Cu powder is that purity is not less than 99.9% electrolysis Cu powder among the step a of preparation CuZr alloy cast ingot, and the Zr powder is that purity is not less than 99% Zr powder.
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