CN104164587A - Compact dispersion-strengthened copper-base composite material - Google Patents
Compact dispersion-strengthened copper-base composite material Download PDFInfo
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Abstract
The invention relates to a compact dispersion-strengthened copper-base composite material and a preparation method thereof. The compact dispersion-strengthened copper-base composite material is composed of a copper alloy base and Al2O3 particles which are uniformly dispersed in the copper alloy base. Composite metals are added into the copper-alumina master alloy, and a vacuum induction hot-pressing furnace or low-pressure isostatic sintering furnace is adopted for sintering to maximally eliminate the residual porosity and defects in the alloy, so that the sintered billet basically reaches the theoretical density. The prepared dispersion-strengthened copper product has the advantages of high electric conductivity, high softening temperature resistance and high compactness, and can achieve more than 99.5% of theoretical density.
Description
Technical field
The present invention relates to dispersed and strengthened copper-based composite material of a kind of densification and preparation method thereof, belong to metal-base composites science and technology field.
Background technology
By adding oxide particle as wild phase, and make being distributed in copper matrix of its even dispersion in copper matrix, can improve mechanical property and the anti-softening power of high temperature of Cu-base composites, electroconductibility can not reduce again too much simultaneously.Not only room temperature strength is high for copper-alumina composite material, conduction and heat conductivility good, and there is good anti-electric-arc erosion, wear resistance and high-temperature stability, be a kind of matrix material having a extensive future.Because the manufacturing processed of copper-alumina composite material is a kind of powder metallurgy process, density is difficult to reach 100%, so workpiece surface exists many minute apertures.In hot-work heat-processed, easily cause surperficial grain boundary oxidation, cause grain-boundary strength low, in hot forging process, cause cracking.Due to a forge hot difficult problem, be substantially confined at present, on resistance welding Material Field and electronics miniature parts, limit the application of this material.
But the general density of dispersed and strengthened copper-based composite material sintered blank that traditional production method is prepared is not high, when particularly section is large, cannot further realize large deformation ratio, generally can only reach 97.5% left and right theoretical density, goods inside has a certain amount of hole and exists, and makes the machinery of the finished product, physicals not good.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of dispersed and strengthened copper-based composite material with high conductivity, high resistance softening temperature and high compactness and preparation method thereof.
The technical scheme that the present invention solves the problems of the technologies described above is as follows:
A dispersed and strengthened copper-based composite material for densification, is distributed in the Al in described copper alloy matrix by copper alloy matrix and even dispersion
2o
3ultrafine particles composition; Wherein,
Described copper alloy matrix is the alloy that copper and following one or more metals form: Ag, Cd, Ca, Zr, Mg, La, Ce single rare earth metal or norium;
Described Al
2o
3content be 0.1～1.5wt%; The content summation < 2.0wt% of one or more of described Ag, Cd, Ca, Zr, Mg, La, Ce single rare earth metal or norium, all the other are Cu.
Another technical scheme that the present invention solves the problems of the technologies described above is as follows:
A preparation method for the dispersed and strengthened copper-based composite material of densification, comprises the following steps:
1) in vacuum induction furnace, add electrolytic copper to carry out melting, after melting clearly, add copper-phosphorus master alloy to carry out deoxidation, add again copper-aluminium intermediate alloy to proceed melting, then with nitrogen or the water smoke of 5～15Mpa, carry out powder by atomization, make copper-Al alloy powder;
2) by step 1) in the copper-Al alloy powder that makes first under air atmosphere, be oxidized, then pass into nitrogen and carry out again interior oxidation, obtain the powder after interior oxidation;
3) by step 2) in powder after the described interior oxidation that obtains pass into hydrogen or decomposed ammonia reduces, reduce complete cool to room temperature, obtain copper-aluminium oxide alloy powder;
4) by step 3) in described copper-aluminium oxide alloy powder of obtaining and single rare earth metal or two or more norium or in mixer, mix with one or more powder in the copper alloy of Cu-Ag, Cu-Cd, Cu-Ca, Cu-Zr, Cu-Mg, Cu-La, Cu-Ce arbitrarily in Ag, Cd, Ca, Zr, Mg, La, Ce, obtain mixed powder;
5) by step 4) in the described mixed powder that obtains carry out briquetting, obtain preformed compact;
6) by step 5) in the described preformed compact that obtains be placed in vacuum induction hot pressing furnace or low pressure isostatic sintering stove carries out sintering alloying, obtain disperse distribution Al on copper alloy matrix
2o
3the sintered blank of particle, i.e. the dispersed and strengthened copper-based composite material of described densification.
The invention has the beneficial effects as follows:
The present invention adds composition metal in copper-aluminum oxide master alloying, adopts vacuum induction hot pressing furnace or low pressure isostatic sintering stove to carry out sintering, eliminates to greatest extent the inner residual porosity of alloy and defect, makes sintered blank substantially reach theoretical density.The dispersion-strengthened brass work that adopts the inventive method to prepare has high conductivity, high resistance softening temperature and high compactness, can reach 99.5% above theoretical density.
Copper-alumina composite material electric conductivity > the 80%IACS that adopts the present invention to prepare, hardness > 126HB, density > 99.5% theoretical density, 920 ℃ of softening temperature >.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in step 1) in, described in carry out deoxidation time be 3～5 minutes.
Further, in step 1) in, described in add copper-aluminium intermediate alloy to carry out melting processing condition be: at the temperature of 1200～1300 ℃, melting is 5～10 minutes.
Further, in step 2) in, the described processing condition that are oxidized under air atmosphere are: be to be oxidized 60～180 minutes at the temperature of 300～400 ℃.
Further, in step 2) in, described in carry out interior oxidation processing condition be: at the temperature of 800～950 ℃, carry out interior oxidation, and be incubated 90～180 minutes.
Further, in step 3) in, described in the processing condition of reducing be: at the temperature of 800～950 ℃, reduce, and be incubated 90～180 minutes.
Further, in step 5) in, the density of described preformed compact is 70～90% theoretical densities.
Further, in step 6) in, described in to carry out the processing condition of sintering alloying as follows: sintering temperature is 950～1020 ℃, and the vacuum tightness of described vacuum induction hot pressing furnace is not less than 5.0 * 10
-1mpa, the pressure of described low pressure isostatic sintering stove is 25～35MPa, sintering time 1～3 hour.
Further, described sintered blank density be greater than 99.5% theoretical density.
Embodiment
Below principle of the present invention and feature are described, example, only for explaining the present invention, is not intended to limit scope of the present invention.
A dispersed and strengthened copper-based composite material for densification, is distributed in the Al in described copper alloy matrix by copper alloy matrix and even dispersion
2o
3ultrafine particles composition; Wherein,
Described copper alloy matrix is the alloy that copper and following one or more metals form: Ag, Cd, Ca, Zr, Mg, La, Ce single rare earth metal or norium;
Described Al
2o
3content be 0.1～1.5wt%; The content summation < 2.0wt% of one or more of described Ag, Cd, Ca, Zr, Mg, La, Ce single rare earth metal or norium, all the other are Cu.
A preparation method for the dispersed and strengthened copper-based composite material of densification, comprises the following steps:
1) in vacuum induction furnace, add electrolytic copper to carry out melting, after melting clearly, add copper-phosphorus master alloy to carry out deoxidation 3～5 minutes, add again the melting 5～10 minutes at the temperature of 1200～1300 ℃ of copper-aluminium intermediate alloy, then with nitrogen or the water smoke of 5～15Mpa, carry out powder by atomization, make copper-Al alloy powder;
2) by step 1) in the copper-Al alloy powder that makes first under air atmosphere, at the temperature of 300～400 ℃, be oxidized 60～180 minutes, then pass into nitrogen and at the temperature of 800～950 ℃, carry out interior oxidation, and be incubated 90～180 minutes, obtain the powder after interior oxidation;
3) by step 2) in powder after the described interior oxidation that obtains pass into hydrogen or decomposed ammonia reduces at the temperature of 800～950 ℃, and be incubated 90～180 minutes, reduce complete cool to room temperature, obtain copper-aluminium oxide alloy powder;
4) by step 3) in described copper-aluminium oxide alloy powder of obtaining and single rare earth metal or two or more norium or in mixer, mix with one or more powder in the copper alloy of Cu-Ag, Cu-Cd, Cu-Ca, Cu-Zr, Cu-Mg, Cu-La, Cu-Ce arbitrarily in Ag, Cd, Ca, Zr, Mg, La, Ce, obtain mixed powder;
5) by step 4) in the described mixed powder that obtains carry out briquetting, obtain preformed compact, the density of preformed compact is 70～90% theoretical densities;
6) by step 5) in the described preformed compact that obtains be placed in vacuum induction hot pressing furnace or low pressure isostatic sintering stove carries out sintering alloying, sintering temperature is 950～1020 ℃, the vacuum tightness of described vacuum induction hot pressing furnace is not less than 5.0 * 10
-1mpa, the pressure of described low pressure isostatic sintering stove is 25～35MPa, sintering time 1～3 hour obtains disperse distribution Al on copper alloy matrix
2o
3the sintered blank of particle, described sintered blank density be greater than 99.5% theoretical density, i.e. the dispersed and strengthened copper-based composite material of described densification.
Below by several specific embodiments so that the present invention is specifically described.
Embodiment 1
Percentage composition in Cu-base composites gross weight: aluminum oxide accounts for 0.58%, silver accounts for 2.0%, and copper accounts for 97.42%, and theoretical density is 8.864g/cm
3.
The preparation method of the dispersed and strengthened copper-based composite material of above-mentioned densification, comprises the following steps:
1) in vacuum induction furnace, add electrolytic copper to carry out melting, after melting clearly, add copper-phosphorus master alloy to carry out deoxidation 3 minutes, add again the melting 10 minutes at the temperature of 1200 ℃ of copper-aluminium intermediate alloy, then with nitrogen or the water smoke of 5Mpa, carry out powder by atomization, make copper-Al alloy powder;
2) by step 1) in the copper-Al alloy powder that makes first under air atmosphere, at the temperature of 300 ℃, be oxidized 180 minutes, then pass into nitrogen and at the temperature of 800 ℃, carry out interior oxidation, and be incubated 180 minutes, obtain the powder after interior oxidation;
3) by step 2) in powder after the described interior oxidation that obtains pass into hydrogen or decomposed ammonia reduces at the temperature of 800 ℃, and be incubated 180 minutes, reduce complete cool to room temperature, obtain copper-aluminium oxide alloy powder;
4) copper-aluminium oxide alloy powder is mixed in mixer with accounting for powder total mass 2.0% silver powder, obtain mixed powder;
5) by step 4) in the described mixed powder that obtains carry out briquetting, obtain preformed compact, the density of preformed compact is 7.868g/cm
3theoretical density;
6) by step 5) in the described preformed compact that obtains be placed in vacuum induction hot pressing furnace or low pressure isostatic sintering stove carries out sintering alloying, sintering temperature is 950 ℃, the vacuum tightness of described vacuum induction hot pressing furnace is not less than 5.0 * 10
-1mpa, the pressure of described low pressure isostatic sintering stove is 25MPa, sintering time 3 hours obtains disperse distribution Al on copper alloy matrix
2o
3the sintered blank of particle, the base specification φ 150 * 300mm of described sintered blank, the density of sintered blank is 8.829g/cm
3.
Embodiment 2
Percentage composition in Cu-base composites gross weight: aluminum oxide accounts for 0.58%, silver accounts for 0.36%, and copper accounts for 99.06%, and alloy theory density is 8.841g/cm
3.
The preparation method of the dispersed and strengthened copper-based composite material of above-mentioned densification, comprises the following steps:
1) in vacuum induction furnace, add electrolytic copper to carry out melting, after melting clearly, add copper-phosphorus master alloy to carry out deoxidation 5 minutes, add again the melting 5 minutes at the temperature of 1300 ℃ of copper-aluminium intermediate alloy, then with nitrogen or the water smoke of 15Mpa, carry out powder by atomization, make copper-Al alloy powder;
2) by step 1) in the copper-Al alloy powder that makes first under air atmosphere, at the temperature of 400 ℃, be oxidized 60 minutes, then pass into nitrogen and at the temperature of 950 ℃, carry out interior oxidation, and be incubated 90 minutes, obtain the powder after interior oxidation;
3) by step 2) in powder after the described interior oxidation that obtains pass into hydrogen or decomposed ammonia reduces at the temperature of 950 ℃, and be incubated 90 minutes, reduce complete cool to room temperature, obtain copper-aluminium oxide alloy powder;
4) copper-aluminium oxide alloy powder is mixed in mixer with the copper-6wt% silver powder that accounts for powder total mass 6%, obtain mixed powder;
5) by step 4) in the described mixed powder that obtains carry out briquetting, obtain preformed compact, the density of preformed compact is 7.871g/cm
3;
6) by step 5) in the described preformed compact that obtains be placed in vacuum induction hot pressing furnace or low pressure isostatic sintering stove carries out sintering alloying, sintering temperature is 1020 ℃, the vacuum tightness of described vacuum induction hot pressing furnace is not less than 5.0 * 10
-1mpa, the pressure of described low pressure isostatic sintering stove is 35MPa, sintering time 1 hour obtains disperse distribution Al on copper alloy matrix
2o
3the sintered blank of particle, the base specification φ 150 * 300mm of described sintered blank, the density of sintered blank is 8.797g/cm
3.
Embodiment 3
Percentage composition in Cu-base composites gross weight: aluminum oxide accounts for 0.72%, lanthanum accounts for 0.42%, and copper accounts for 98.86%, and alloy theory density is 8.805g/cm
3.
The preparation method of the dispersed and strengthened copper-based composite material of above-mentioned densification, comprises the following steps:
1) in vacuum induction furnace, add electrolytic copper to carry out melting, after melting clearly, add copper-phosphorus master alloy to carry out deoxidation 4 minutes, add again the melting 7 minutes at the temperature of 1250 ℃ of copper-aluminium intermediate alloy, then with nitrogen or the water smoke of 10Mpa, carry out powder by atomization, make copper-Al alloy powder;
2) by step 1) in the copper-Al alloy powder that makes first under air atmosphere, at the temperature of 350 ℃, be oxidized 100 minutes, then pass into nitrogen and at the temperature of 850 ℃, carry out interior oxidation, and be incubated 100 minutes, obtain the powder after interior oxidation;
3) by step 2) in powder after the described interior oxidation that obtains pass into hydrogen or decomposed ammonia reduces at the temperature of 850 ℃, and be incubated 120 minutes, reduce complete cool to room temperature, obtain copper-aluminium oxide alloy powder;
4) copper-aluminium oxide alloy powder is mixed in mixer with the copper-6wt% lanthanum powder that accounts for powder total mass 7%, obtain mixed powder;
5) by step 4) in the described mixed powder that obtains carry out briquetting, obtain preformed compact, the density of preformed compact is 7.925g/cm
3;
6) by step 5) in the described preformed compact that obtains be placed in vacuum induction hot pressing furnace or low pressure isostatic sintering stove carries out sintering alloying, sintering temperature is 970 ℃, the vacuum tightness of described vacuum induction hot pressing furnace is not less than 5.0 * 10
-1mpa, the pressure of described low pressure isostatic sintering stove is 30MPa, sintering time 2 hours obtains disperse distribution Al on copper alloy matrix
2o
3the sintered blank of particle, the base specification φ 300 * 600mm of described sintered blank, the density of sintered blank is 8.770g/cm
3.
Embodiment 4
Percentage composition in Cu-base composites gross weight: aluminum oxide accounts for 1.05%, silver accounts for 0.24%, and cerium accounts for 0.12%, and copper accounts for 98.59%, and alloy theory density is 8.785g/cm
3.
The preparation method of the dispersed and strengthened copper-based composite material of above-mentioned densification, comprises the following steps:
1) in vacuum induction furnace, add electrolytic copper to carry out melting, after melting clearly, add copper-phosphorus master alloy to carry out deoxidation 4 minutes, add again the melting 8 minutes at the temperature of 1250 ℃ of copper-aluminium intermediate alloy, then with nitrogen or the water smoke of 12Mpa, carry out powder by atomization, make copper-Al alloy powder;
2) by step 1) in the copper-Al alloy powder that makes first under air atmosphere, at the temperature of 370 ℃, be oxidized 120 minutes, then pass into nitrogen and at the temperature of 900 ℃, carry out interior oxidation, and be incubated 140 minutes, obtain the powder after interior oxidation;
3) by step 2) in powder after the described interior oxidation that obtains pass into hydrogen or decomposed ammonia reduces at the temperature of 900 ℃, and be incubated 150 minutes, reduce complete cool to room temperature, obtain copper-aluminium oxide alloy powder;
4) copper-aluminium oxide alloy powder is mixed in mixer with accounting for copper-6wt% silver powder of powder total mass 4% and copper-6wt% cerium powder of 2%, obtain mixed powder;
5) by step 4) in the described mixed powder that obtains carry out briquetting, obtain preformed compact, the density of preformed compact is 7.730g/cm
3;
6) by step 5) in the described preformed compact that obtains be placed in vacuum induction hot pressing furnace or low pressure isostatic sintering stove carries out sintering alloying, sintering temperature is 1000 ℃, the vacuum tightness of described vacuum induction hot pressing furnace is not less than 5.0 * 10
-1mpa, the pressure of described low pressure isostatic sintering stove is 32MPa, sintering time 2 hours obtains disperse distribution Al on copper alloy matrix
2o
3the sintered blank of particle, the base specification φ 400 * 800mm of described sintered blank, the density of sintered blank is 8.749g/cm
3.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a fine and close dispersed and strengthened copper-based composite material, is characterized in that, by copper alloy matrix and even dispersion, is distributed in the Al in described copper alloy matrix
2o
3ultrafine particles composition; Wherein,
Described copper alloy matrix is the alloy that copper and following one or more metals form: Ag, Cd, Ca, Zr, Mg, La, Ce single rare earth metal or norium;
Described Al
2o
3content be 0.1～1.5wt%; The content summation < 2.0wt% of one or more of described Ag, Cd, Ca, Zr, Mg, La, Ce single rare earth metal or norium, all the other are Cu.
2. a preparation method for fine and close dispersed and strengthened copper-based composite material, is characterized in that, comprises the following steps:
1) in vacuum induction furnace, add electrolytic copper to carry out melting, after melting clearly, add copper-phosphorus master alloy to carry out deoxidation, add again copper-aluminium intermediate alloy to proceed melting, then with nitrogen or the water smoke of 5～15Mpa, carry out powder by atomization, make copper-Al alloy powder;
2) by step 1) in the copper-Al alloy powder that makes first under air atmosphere, be oxidized, then pass into nitrogen and carry out again interior oxidation, obtain the powder after interior oxidation;
3) by step 2) in powder after the described interior oxidation that obtains pass into hydrogen or decomposed ammonia reduces, reduce complete cool to room temperature, obtain copper-aluminium oxide alloy powder;
4) by step 3) in described copper-aluminium oxide alloy powder of obtaining and single rare earth metal or two or more norium or in mixer, mix with one or more powder in the copper alloy of Cu-Ag, Cu-Cd, Cu-Ca, Cu-Zr, Cu-Mg, Cu-La, Cu-Ce arbitrarily in Ag, Cd, Ca, Zr, Mg, La, Ce, obtain mixed powder;
5) by step 4) in the described mixed powder that obtains carry out briquetting, obtain preformed compact;
6) by step 5) in the described preformed compact that obtains be placed in vacuum induction hot pressing furnace or low pressure isostatic sintering stove carries out sintering alloying, obtain disperse distribution Al on copper alloy matrix
2o
3the sintered blank of particle, i.e. the dispersed and strengthened copper-based composite material of described densification.
3. the preparation method of the dispersed and strengthened copper-based composite material of densification according to claim 2, is characterized in that, in step 1) in, described in carry out deoxidation time be 3～5 minutes.
4. the preparation method of the dispersed and strengthened copper-based composite material of densification according to claim 2, it is characterized in that, in step 1) in, described in add copper-aluminium intermediate alloy to carry out melting processing condition be: at the temperature of 1200～1300 ℃, melting is 5～10 minutes.
5. the preparation method of the dispersed and strengthened copper-based composite material of densification according to claim 2, is characterized in that, in step 2) in, the described processing condition that are oxidized under air atmosphere are: at the temperature of 300～400 ℃, be oxidized 60～180 minutes.
6. the preparation method of the dispersed and strengthened copper-based composite material of densification according to claim 2, it is characterized in that, in step 2) in, described in carry out interior oxidation processing condition be: at the temperature of 800～950 ℃, carry out interior oxidation, and be incubated 90～180 minutes.
7. the preparation method of the dispersed and strengthened copper-based composite material of densification according to claim 2, is characterized in that, in step 3) in, described in the processing condition of reducing be: at the temperature of 800～950 ℃, reduce, and be incubated 90～180 minutes.
8. the preparation method of the dispersed and strengthened copper-based composite material of densification according to claim 2, is characterized in that, in step 5) in, the density of described preformed compact is 70～90% theoretical densities.
9. the preparation method of the dispersed and strengthened copper-based composite material of densification according to claim 2, it is characterized in that, in step 6) in, described in to carry out the processing condition of sintering alloying as follows: sintering temperature is 950～1020 ℃, and the vacuum tightness of described vacuum induction hot pressing furnace is not less than 5.0 * 10
-1mpa, the pressure of described low pressure isostatic sintering stove is 25～35MPa, sintering time 1～3 hour.
10. the preparation method of the dispersed and strengthened copper-based composite material of densification according to claim 2, is characterized in that, described sintered blank density be greater than 99.5% theoretical density.
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