CN109136615B - Preparation method of high-strength high-plasticity dispersion-strengthened copper-based composite material - Google Patents
Preparation method of high-strength high-plasticity dispersion-strengthened copper-based composite material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/001—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides
- C22C32/0015—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with only oxides with only single oxides as main non-metallic constituents
- C22C32/0021—Matrix based on noble metals, Cu or alloys thereof
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0063—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on SiC
Abstract
The invention discloses a preparation method of a high-strength high-plasticity dispersion-strengthened copper-based composite material, which can realize the dispersion distribution of nano ceramic particles in an ultrafine-grained copper matrix by adopting a mode of combining multi-step ball milling with multi-step gas-phase reduction and discharge plasma sintering technology and reasonably controlling the process. The method is a brand new preparation method of the copper-based composite material, overcomes the problem that the uniform dispersion of the nano strengthening phase in the matrix can not be effectively realized in the process of directly adding the nano strengthening phase particles and the copper powder for mixing, and can obtain the ceramic particle dispersion strengthening copper-based composite material with excellent mechanical property and good conductivity.
Description
Technical Field
The invention relates to the technical field of copper-based composite materials, in particular to a high-strength high-plasticity dispersion-strengthened ultrafine-grained copper-based composite material and a preparation method thereof.
Background
The particle dispersion strengthened copper-based composite material is a high-performance material which can meet different engineering requirements and is prepared by combining the excellent electric conduction and heat conduction performance of copper with strengthening phase particles with high hardness, high strength, high wear resistance and strong high-temperature thermal stability in a mode of artificial design and synthesis. However, how to effectively realize the excellent combination of the properties between the copper and the reinforcing phase particles is one of the difficulties of research. One important influencing factor is how to uniformly disperse the nano-sized ceramic phase particles in the matrix.
At present, the method for better realizing the uniform dispersion of nano ceramic particles in a copper base is an in-situ synthesis method. Patent publication No.: CN106521205A, published: patent technology published in 2017, 3, month and 22: mixing Cu-x Al (x = 0.2-0.6%) alloy powder with Cu2O is mixed, cold-pressed, molded and sintered, and internal oxidation reaction occurs in the sintering process to prepare the nano Al2O3Composite material uniformly distributed in the copper matrix. Patent publication No.: CN102031401A, published: patent technology disclosed in 2011, 4, month and 27: mixing an aluminum nitrate solution and a copper nitrate solution, adding a chelating agent citric acid to prepare gel, heating to naturally spread to obtain nano aluminum oxide and copper oxide colored powder, reducing in atmosphere, pressing, sintering and molding to obtain Cu-x Al2O3(x = 0.15-3%) composite material. In the method for preparing the copper-based composite material by in-situ synthesis, the strengthening phase bodyThe volume fraction is generally low, and the process control difficulty is gradually increased along with the increase of the volume fraction of the strengthening phase, so that the local coarsening phenomenon of the strengthening phase generated in situ is easy to occur, the strengthening phase is not uniformly distributed in the matrix, and finally, the performance stability of the product is influenced. Therefore, how to realize the uniform distribution of the reinforcing phase particles in the matrix under high volume fraction, further improve the mechanical property of the copper-based composite material on the basis of keeping better conductivity, and have important strategic significance for developing novel high-strength and high-conductivity copper alloy.
Disclosure of Invention
In order to solve the problem of dispersion of nano ceramic particles in a matrix, the invention provides a method for preparing a high-strength high-plasticity dispersion-strengthened ultrafine-grained copper-based composite material, which can effectively realize the dispersion distribution of the nano ceramic particles in the ultrafine-grained copper matrix, and has good conductivity and simultaneously realizes the remarkable improvement of mechanical property and high-temperature softening resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-strength high-plasticity dispersion-strengthened copper-based composite material comprises the following steps:
1) mixing copper oxide powder and ceramic strengthening phase powder in proportion to obtain mixed powder;
2) putting the mixed powder, the hard alloy balls and the absolute ethyl alcohol into a hard alloy ball milling tank;
3) putting the ball milling tank into a planetary ball mill for first high-energy ball milling to obtain precursor powder with uniformly dispersed nano ceramic strengthening phase in nano copper oxide;
4) putting the precursor powder into a quartz tube furnace, vacuumizing, heating to a heat preservation temperature point, introducing reducing gas CO, carrying out primary reduction on the precursor powder, and cooling to room temperature along with the furnace after heat preservation is finished to obtain first-grade copper-based composite powder with nano-scale copper powder and ceramic particles;
5) mixing the primary copper-based composite powder obtained in the step 4) with a process control agent according to a certain proportion, and then putting the mixture and hard alloy balls into a hard alloy ball milling tank;
6) putting the ball milling tank into a planetary ball mill for secondary ball milling to obtain copper-based composite powder with nano ceramic strengthening phase dispersed on the micron copper powder;
7) putting the copper-based composite powder obtained in the step 6) into a quartz tube furnace, vacuumizing, heating to a heat preservation temperature point, and introducing a reducing gas H2Carrying out secondary deep reduction, and cooling to room temperature along with the furnace after heat preservation is finished to obtain secondary copper-based composite powder;
8) and (3) placing the graphite mould filled with the secondary copper-based composite powder into a spark plasma sintering furnace for sintering, and cooling to obtain the nano ceramic particle dispersion strengthened copper-based composite material.
Further, in the step 1), the copper oxide powder is copper oxide or cuprous oxide, the purity is more than 99%, and the sizes are all nano-scale.
Further, the ceramic strengthening phase powder in step 1) does not need to react with hydrogen and carbon monoxide (such as Al)2O3、Y2O3、SiC、AlN、TiB2Etc.), the purity is more than or equal to 99 percent, the dimension is nano-scale, and the volume fraction of the powder is 1 to 15 percent.
Further, in the step 2), the content of the absolute ethyl alcohol is mPowder×1mL/g。
Further, in the step 2), the ball-material ratio is 10: 1-30: 1, and the ball-milling tank is sealed and then is vacuumized to 15 Pa.
Further, in the step 3), the revolution speed of ball milling is 200-300 r/min, and the ball milling time is 2-12 h.
Further, in the step 4), vacuumizing to ensure that the ambient pressure in the pipe is not more than 15 Pa; then filling high-purity nitrogen or other high-purity inert gases to 1atm, and repeating for 2-3 times.
Further, in the step 4), the heating rate is 4-6 ℃/min, the heat preservation temperature selection interval is 100-150 ℃, the heat preservation time is 0.25-2 h, CO is in a high-purity atmosphere, and the gas flow is 5-10 mL/min.
Further, in the step 4), the process control agent can be selected from organic high polymers such as stearic acid, polyvinyl alcohol and silane coupling agent, the addition amount is 0.5-2% of the total mass of the powder according to different process control agents, and the ball-to-material ratio is 10: 1-30: 1.
Further, in the step 5), the ball milling speed is 100-300 r/min, and the ball milling time is 4-48 h.
Further, in the step 6), vacuumizing to ensure that the ambient pressure in the pipe is not more than 15 Pa; then, high-purity nitrogen or other high-purity inert gases are slowly filled to 1atm, and the process is repeated for 2-3 times.
Further, in the step 6), the heating rate is 6-10 ℃/min, the heat preservation temperature selection interval is 300-500 ℃, the heat preservation time is 0.5-2H, and H2The gas flow is 5-10 mL/min in a high-purity atmosphere.
Further, the pressure of the sintering environment in the step 7) is not more than 10 Pa.
Further, in the step 7), the heating rate is 80-100 ℃/min.
Further, the sintering temperature in the step 7) is 750-900 ℃.
Further, the sintering heat preservation time in the step 7) is 5-10 min.
Further, the sintering pressure in the step 7) is 35-50 MPa.
The invention has the beneficial effects that: the composite material with nano ceramic particles dispersed in the superfine crystal copper matrix can be realized by adopting a mode of combining multi-step high-energy ball milling with multi-step gas-phase reduction and discharge plasma sintering technology and reasonably controlling the process. The method is a brand new preparation method of the copper-based composite material, overcomes the problem that the nano strengthening phase cannot be effectively dispersed in the matrix in the process of directly mixing the nano strengthening phase particles and the copper powder, and finally obtains the ceramic particle dispersion strengthening copper-based composite material with excellent comprehensive performance.
Drawings
FIG. 1 shows Cu-6.9vol% Al prepared by the method of the present invention2O3The back-scattering pattern of the ceramic particles in the composite bulk distributed in the copper matrix (example 1);
Detailed Description
The present invention will now be more fully described with reference to the following examples. This invention may, however, be embodied in many different forms and should not be construed as limited to the exemplary embodiments set forth herein.
To further illustrate the technical means and effects of the present invention for achieving the predetermined technical objectives, the following preferred embodiments 1 to 8 are combined, and the ball milling rotation speed, ball milling time and ball material ratio in step 3) and step 5), the heat preservation temperature and heat preservation time in step 4) and step 6), and the sintering temperature, sintering time and sintering pressure in step 7) are compared with those in comparative examples 1 to 3. The process, features and effects of the present invention will be described in detail hereinafter. The ball-material ratio in the examples is mass ratio.
Example 1
1) Simply mixing 48.75g of nano copper oxide powder and 1.25g of nano alumina powder, wherein the nano alumina powder accounts for 4 percent of the total volume of the mixed powder;
2) and (3) filling the mixed powder, the hard alloy balls and the absolute ethyl alcohol with the ball-to-material ratio of 20:1 and 50mL into a hard alloy ball milling tank.
3) Putting the ball milling tank into a planetary ball mill, and carrying out primary high-energy ball milling at a ball milling revolution speed of 300r/min for 2 h;
4) and taking the ball-milled material as precursor powder. Putting the precursor powder into a quartz tube furnace, vacuumizing to 15Pa, heating to 100 ℃, introducing reducing gas CO, carrying out primary reduction on the precursor powder, keeping the temperature for 120min, and cooling to room temperature along with the furnace to obtain primary copper-based composite powder with copper powder and aluminum oxide particles both in nano scale;
5) mixing the primary copper-based composite powder obtained in the step 4) with 0.5g of stearic acid, and putting the hard alloy balls into a hard alloy ball milling tank at a ball-to-material ratio of 30: 1;
6) putting the ball milling tank into a planetary ball mill, and carrying out secondary ball milling at a ball milling revolution speed of 300r/min for 8 hours to obtain copper-based composite powder with nano ceramic strengthening phases dispersed on the micron copper powder;
7) putting the copper-based composite powder obtained in the step 6) into a quartz tube furnace, vacuumizing to 15Pa, heating to 400 ℃, and introducing reducing gas H2Carrying out secondary deep reduction, keeping the temperature for 1h, then cooling to room temperature along with the furnace to obtain secondary copper-based composite powder;
7) and placing the graphite die filled with the secondary copper-based composite powder into a discharge plasma sintering furnace, sintering at the initial pressure of 45MPa, the heating rate of 80 ℃/min and the heat preservation time of 850 ℃, and cooling to obtain the dispersion-strengthened copper-based composite material with the volume fraction of the nano aluminum oxide of 6.9 percent, wherein the measured microhardness is HV185, the compressive yield strength is 560MPa, the maximum compressive strength is 802MPa, the compression ratio is 41 percent, and the electrical conductivity at normal temperature is 64 percent IACS.
Example 2
The preparation method is basically the same as that of the example 1, except that:
the powder mixture of 49.49g of nanometer copper oxide powder and 0.51g of nanometer silicon carbide powder in the step 1), wherein the nanometer silicon carbide powder accounts for 2% of the total volume of the powder mixture;
in the step 3), the revolution speed of one-time ball milling is 250r/min, and the ball milling time is 4h;
in the step 4), the primary reduction temperature is 120 ℃, and the reduction heat preservation time is 70 min.
After spark plasma sintering, the copper-based composite material with the volume fraction of nano silicon carbide of 3.5 percent is obtained, the microhardness is HV146, the compressive yield strength is 426MPa, the maximum compressive strength is 580MPa, the compressibility is 48 percent, and the electrical conductivity is 72 percent IACS at normal temperature.
Example 3
The preparation method is basically the same as that of the example 1, except that:
the mixed powder of 47.59g of nano copper oxide powder and 2.41g of nano yttrium oxide powder in the step 1) accounts for 6 percent of the total volume of the mixed powder;
in the step 3), the revolution speed of one-time ball milling is 200r/min, the ball milling time is 6h, and the ball-material ratio is 15: 1.
After spark plasma sintering, the copper-based composite material with the volume fraction of nano yttrium oxide of 10.2 percent is obtained, and the microhardness is HV209, the compressive yield strength is 655MPa, the maximum compressive strength is 932MPa, the compression ratio is 33.2 percent, and the electrical conductivity is 55 percent IACS at normal temperature.
Example 4
The preparation method is basically the same as that of the example 1, except that:
the mixed powder of 46.77g of nano copper oxide powder and 3.23g of nano yttrium oxide powder in the step 1), wherein the nano yttrium oxide powder accounts for 8 percent of the total volume of the mixed powder;
in the step 4), the primary reduction temperature is 150 ℃, and the reduction heat preservation time is 15min;
the ratio of the secondary ball milling balls to the materials in the step 5) and the step 6) is 20:1, the revolution speed of the ball milling is 250r/min, and the ball milling time is 12 h.
After spark plasma sintering, the copper-based composite material with the volume fraction of the nano yttrium oxide being 13.4% is obtained, and the microhardness is HV220, the compressive yield strength is 812MPa, the maximum compressive strength is 980MPa, the compression ratio is 23.2%, and the electric conductivity is 50% IACS at normal temperature.
Example 5
The preparation method is basically the same as that of the example 1, except that:
the powder mixture of 47.04g of nano-copper oxide powder and 3.96g of nano-alumina powder in the step 1), wherein the nano-alumina powder accounts for 12% of the total volume of the powder mixture;
in the step 4), the primary reduction temperature is 150 ℃, and the reduction heat preservation time is 25 mim.
In the step 7), the secondary reduction temperature is 450 ℃, and the reduction time is 1 h.
After spark plasma sintering, the copper-based composite material with the volume fraction of the nano alumina of 19.5 percent is obtained, and the microhardness is HV230, the compressive yield strength is 853MPa, the maximum compressive strength is 986MPa, the compressibility is 10.2 percent, and the conductivity at normal temperature is 47 percent IACS.
Example 6
The preparation method is basically the same as that of the example 1, except that:
in the step 4), the primary reduction temperature is 150 ℃, and the reduction heat preservation time is 15min;
in the step 7), the secondary reduction temperature is 450 ℃, and the reduction time is 1 h.
After spark plasma sintering, the copper-based composite material with the volume fraction of the nano alumina of 6.9 percent is obtained, and the microhardness is HV172, the compressive yield strength is 512MPa, the maximum compressive strength is 756MPa, the compression ratio is 43.2 percent, and the conductivity is 66 percent IACS at normal temperature.
Example 7
The preparation method is basically the same as that of the example 1, except that:
step 5) neutralizing the secondary ball-milling ball-material ratio in step 6) to be 15:1, wherein the ball-milling revolution speed is 200r/min, and the ball-milling time is 48 h;
in the step 7), the secondary reduction temperature is 500 ℃, and the reduction time is 0.5 h.
After spark plasma sintering, the copper-based composite material with the volume fraction of the nano alumina of 6.9 percent is obtained, and the microhardness is HV179, the compressive yield strength is 530MPa, the maximum compressive strength is 789MPa, the compression ratio is 39 percent, and the electrical conductivity is 63 percent IACS at normal temperature.
Example 8
Basically the same as the preparation method of the embodiment 1, except that the SPS sintering temperature in the step 8) is 750 ℃, the heat preservation time is 10min, and the pressure is 50 MPa.
After spark plasma sintering, the copper-based composite material with the volume fraction of the nano alumina of 6.9 percent is obtained, and the microhardness is HV180, the compressive yield strength is 536MPa, the maximum compressive strength is 757MPa, the compression ratio is 38.2 percent, and the electrical conductivity is 60 percent IACS at normal temperature.
Comparative example 1
The difference from the preparation method of the example 1 is that:
in the step 3), the rotation speed of one-time ball milling is 100r/min, the ball milling time is 24 hours, and the ball-to-material ratio is 10: 1.
2) The primary reduction temperature is 250 ℃, and the reduction heat preservation time is 60min;
directly sintering by discharge plasma after primary reduction, and obtaining the copper-based composite material with the volume fraction of the nano alumina being 6.9 percent after the sintering by the discharge plasma, wherein the microhardness is determined to be HV149, the compressive yield strength is 454MPa, the maximum compressive strength is 558MPa, the compression ratio is 34.5 percent, and the electrical conductivity is 48 percent IACS at normal temperature.
Comparative example 2
Basically the same preparation method as that of example 1, except that the direct discharge plasma sintering is carried out after the primary reduction.
After spark plasma sintering, the copper-based composite material with the volume fraction of the nano alumina of 6.9 percent is obtained, and the microhardness is HV96, the compressive yield strength is 159MPa, the maximum compressive strength is 228MPa, the compression ratio is 12.7 percent, and the electrical conductivity at normal temperature is 28 percent IACS.
Comparative example 3
Essentially the same procedure as in example 1 except that secondary H is not conducted2And (4) reducing.
After spark plasma sintering, the copper-based composite material with the volume fraction of the nano alumina of 6.9 percent is obtained, and the microhardness is HV156, the compressive yield strength is 489MPa, the maximum compressive strength is 512MPa, the compression ratio is 14.5 percent, and the electrical conductivity is 42 percent IACS at normal temperature.
The above examples are only for illustrating the present invention, and besides, there are many different embodiments, which can be conceived by those skilled in the art after understanding the idea of the present invention, and therefore, they are not listed here.
Claims (3)
1. A preparation method for preparing a nano ceramic particle dispersion strengthening copper-based composite material by multi-step ball milling and multi-step gas phase reduction is characterized by comprising the following steps:
1) mixing copper oxide powder and ceramic particles in proportion to obtain mixed powder, wherein the copper oxide is copper oxide or cuprous oxide, the purity is higher than 99%, the size is nano-scale, the nano-ceramic particles are one or a mixture of more of Al2O3, Y2O3, SiC, AlN and TiB2, the purity is higher than or equal to 99%, the size is nano-scale, and the mixed powder accounts for 1-15% of the volume fraction of the mixed powder;
2) putting the mixed powder, the hard alloy balls and the absolute ethyl alcohol into a hard alloy ball milling tank;
3) putting the ball milling tank into a planetary ball mill for first high-energy ball milling to obtain precursor powder with uniformly dispersed nano ceramic strengthening phases in the superfine copper oxide, wherein the ball milling rotation speed is 200-300 r/min, the ball milling time is 2-12 h, and the ball-to-material ratio is 10: 1-30: 1;
4) putting the precursor powder into a quartz tube furnace, vacuumizing, heating to a heat preservation temperature point, introducing reducing gas CO, carrying out primary reduction on the precursor powder, cooling to room temperature along with the furnace after heat preservation is finished, and obtaining the first-stage copper-based composite powder with the copper and ceramic particles both being in a nano scale, wherein the heating rate is 4-6 ℃/min, the heat preservation temperature selection interval is 100-150 ℃, the heat preservation time is 0.25-2 h, CO is a high-purity atmosphere, and the gas flow is 5-10 mL/min;
5) mixing the primary copper-based composite powder with a process control agent according to a certain proportion, and then putting the mixture and hard alloy balls into a hard alloy ball milling tank;
6) putting the ball milling tank into a planetary ball mill for secondary ball milling to obtain copper-based composite powder with nano ceramic strengthening phases dispersed on the micron copper powder, wherein the ball milling speed is 100-300 r/min, the ball milling time is 4-48 h, and the ball-to-material ratio is 10: 1-30: 1;
7) putting the copper-based composite powder obtained in the step 6) into a quartz tube furnace, vacuumizing, heating to a heat preservation temperature point, and introducing a reducing gas H2Carrying out secondary deep reduction, cooling to room temperature along with the furnace after heat preservation is finished to obtain secondary copper-based composite powder, wherein the heating rate is 6-10 ℃/min, the heat preservation temperature selection interval is 300-500 ℃, the heat preservation time is 0.5-2H, H2 is high-purity atmosphere, and the air flow is 5-10 mL/min;
8) placing the graphite mould filled with the secondary copper-based composite powder into a discharge plasma sintering furnace for sintering, wherein the pressure of the sintering environment is not more than 10 Pa; the heating rate is 80-100 ℃/min; the sintering temperature is 750-900 ℃; sintering and keeping the temperature for 5 +/-0.5 min; the sintering pressure is 35-50 MPa, and after cooling, the nano ceramic particle dispersion strengthened superfine crystal copper-based composite material is obtained.
2. The preparation method of claim 1, wherein in the step 5), the process control agent is one or a mixture of stearic acid, polyvinyl alcohol and a silane coupling agent, and the addition amount of the process control agent is 0.5-2% of the total mass of the powder.
3. The method according to claim 1, wherein in step 7), the vacuum is applied so that the pressure of the atmosphere in the tube does not exceed 15 Pa; then, high-purity nitrogen or other high-purity inert gases are slowly filled to 1atm, and the process is repeated for 2-3 times.
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| CN107971501A (en) * | 2017-11-29 | 2018-05-01 | 江西理工大学 | The method that secondary atmosphere reduction prepares superfine cupper powder |
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