CN117966053B - Particle reinforced copper-based composite material and preparation method thereof - Google Patents
Particle reinforced copper-based composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 113
- 239000010949 copper Substances 0.000 title claims abstract description 103
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 96
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000002245 particle Substances 0.000 title abstract description 45
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 61
- 238000000498 ball milling Methods 0.000 claims abstract description 46
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000000243 solution Substances 0.000 claims abstract description 39
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- 238000002156 mixing Methods 0.000 claims abstract description 29
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 claims abstract description 18
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 claims abstract description 18
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 claims abstract description 18
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 claims abstract description 18
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 235000005493 rutin Nutrition 0.000 claims abstract description 18
- 229960004555 rutoside Drugs 0.000 claims abstract description 18
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 16
- 238000005245 sintering Methods 0.000 claims abstract description 16
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 13
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000006185 dispersion Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 238000007731 hot pressing Methods 0.000 claims abstract description 10
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 39
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- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 9
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Abstract
The invention discloses a particle reinforced copper-based composite material and a preparation method thereof, and belongs to the technical field of copper-based composite materials. It comprises the following steps: mixing iron, nickel, pretreated aluminum oxide whisker and pretreated graphene with the balance of copper powder raw materials according to weight percentage, performing ball milling treatment, and performing vacuum freeze drying to obtain a mixture; and carrying out hot-pressing sintering treatment on the mixture. According to the preparation method of the particle reinforced copper-based composite material, disclosed by the invention, fewer layers (1-5 layers) of graphene are adopted, rutin is used for dispersion surface modification so as to reduce the agglomeration of graphene in the composite material, sodium dodecyl sulfate solution is adopted for effectively dispersing aluminum oxide whiskers so as to prevent cluster aggregation of the aluminum oxide whiskers, and alloy elements such as Fe are added, so that the effects of solid solution strengthening, grain refinement, reinforcement agglomeration prevention and the like can be achieved, and a coating with good interface bonding performance can be formed by adding Ni-based alloy powder and a copper matrix.
Description
Technical Field
The invention relates to the technical field of copper-based composite materials, in particular to a particle reinforced copper-based composite material and a preparation method thereof.
Background
The particle reinforced copper-based composite material refers to the addition of a copper matrix or in situ generation of second phase particles in a certain process, wherein the second phase particles improve the strength and hardness of the copper-based composite material by blocking dislocation movement. The related studies prove that: the addition of the particles does not lose the electric conductivity and heat conductivity of copper or copper alloy, but can greatly enhance the strength and wear resistance of the copper-based composite material. TiB, alN, graphite particles, tiB 2 particles, etc. are less often incorporated into copper substrates, and much like Al 2O3, WC, siC particles, etc.
The composite material can be reinforced by adding one particle phase into a copper matrix, simultaneously acting as multiphase particles, and even reinforcing the composite material together with a nano phase, such as Al 2O3 particles, carbon nano tubes and rare earth oxide particles. In the aluminum oxide reinforced copper-based composite, al 2O3 particles can refine the structure of the composite material, and the effect of refining the structure is enhanced along with the increase of the content of Al 2O3 particles. However, the content of Al 2O3 is not positively correlated with the effect of reinforcing the copper-based composite material, and the quality fraction of Al 2O3 can be the opposite value when the quality fraction reaches a certain value. The particles with high content are not easy to disperse, and agglomeration worsens the matrix structure, so that the performance of the composite material is affected. In the prior art, the tensile property test is carried out on the Al 2O3/Cu composite material, and the fact that the continuous addition of Al 2O3 to the copper matrix can cause the increase and decrease of tensile strength and elongation is found, because the aluminum oxide whisker is difficult to disperse in the copper matrix composite material and has poor interfacial bonding capability with the copper matrix is found.
Disclosure of Invention
The invention aims to provide a particle reinforced copper-based composite material and a preparation method thereof, which solve the problem that the tensile property of an aluminum oxide composite copper-based composite material is poor.
The invention is realized by the following technical scheme:
The invention provides a preparation method of a particle reinforced copper-based composite material, which comprises the following steps:
According to the weight percentage, 15-20wt% of iron, 1-5wt% of nickel, 0.5-1.5wt% of pretreated alumina whisker and 0.1-1wt% of pretreated graphene are mixed, ball milling treatment is carried out on the powder raw materials with the balance of copper, and a mixture is obtained through vacuum freeze drying; wherein, the alumina whisker is pretreated by sodium dodecyl sulfate; preprocessing graphene by adopting a rutin solution;
Carrying out hot-pressing sintering treatment on the mixture: prepressing at 0.5-1 MPa, heating from room temperature to 600-800 ℃ at a heating rate of 8-12 ℃/min under the vacuum degree of 5-10 Pa, and pressurizing to 1-2 MPa;
under the pressure of 1-2 MPa, the temperature is raised from 600-800 ℃ to 900-1000 ℃ at the temperature rising rate of 4-6 ℃/min, the temperature is kept for 1-5 h, and then the furnace is cooled to the room temperature.
Further, in the method for preparing a particle-reinforced copper-based composite material, the preparation of the pretreated aluminum oxide whisker comprises:
mixing and uniformly stirring the aluminum oxide whisker and sodium dodecyl sulfate with the concentration of 1 g/L-5 g/L to obtain a mixed solution;
And performing ultrasonic dispersion on the mixed solution for 30-60 min, sealing and standing the dispersion liquid for 24-40 h, and performing suction filtration and vacuum freeze drying to obtain the pretreated alumina whisker.
Further, in the preparation method of the particle reinforced copper-based composite material, the doping amount of the alumina whisker in the obtained mixed solution is 0.1 g/mL-0.5 g/mL.
Further, in the method for preparing a particle-reinforced copper-based composite material, the preparing of the pretreated graphene includes:
Mixing graphene and rutin solution with the concentration of (0.5-2) multiplied by 10 -5 g/L, and stirring until the graphene is blended into the rutin solution to obtain a mixed solution;
And (3) performing ultrasonic dispersion for 20-50 min after sealing the mixed solution, standing the dispersion liquid for 24-40 h, and performing suction filtration and vacuum freeze drying to obtain the pretreated graphene.
Further, in the preparation method of the particle reinforced copper-based composite material, the doping amount of graphene in the obtained mixed solution is (0.1-0.5) gGNFs/40mL.
Further, in the preparation method of the particle-reinforced copper-based composite material, the ball milling treatment performed includes:
mixing the pretreated alumina whisker, the pretreated graphene, the copper, the iron and the nickel, performing ball milling under the conditions that the ball milling rotating speed is 300 r/min-500 r/min, the ball milling time is 1 h-5 h, the forward and reverse transfer time is 15 min-30 min, and the acceleration time and the deceleration time are 5 s-20 s, and performing vacuum freeze drying on the obtained ball milling slurry to obtain the mixture.
Further, in the preparation method of the particle reinforced copper-based composite material, the ball-to-material ratio of ball milling is 1-3:1.
Further, in the preparation method of the particle reinforced copper-based composite material, the ball milling medium adopted for ball milling is tertiary butanol.
Further, in the preparation method of the particle-reinforced copper-based composite material, the powder raw materials adopted include: according to the weight percentage, 15-20wt% of iron, 1-5wt% of nickel, 1-5wt% of pretreated aluminum oxide whisker and 0.5wt% of pretreated graphene, and the balance of copper.
The invention also provides a particle reinforced copper-based composite material, which is prepared by the preparation method of the particle reinforced copper-based composite material.
Compared with the prior art, the invention has the following advantages and beneficial effects:
According to the preparation method of the particle reinforced copper-based composite material, disclosed by the invention, fewer layers (1-5 layers) of graphene are adopted, and rutin is used for carrying out dispersion surface modification so as to reduce the agglomeration of the graphene in the composite material. The alumina whiskers were effectively dispersed with a sodium dodecyl sulfate solution to prevent aggregation of their clusters. The alloy elements such as Fe and the like are added, so that the effect of solid solution strengthening can be achieved, grains are refined, aggregation of reinforcements and the like are prevented, and meanwhile, the good electric conductivity and heat conductivity of the Cu matrix can be maintained. Ni and Cu are both face-centered cubic structures, infinite solid solution can be realized by replacing atoms in grains, wettability of Ni and Cu is good, thermal parameters are similar, and Ni-based alloy powder can form a coating with good interface bonding performance with a copper matrix. The particle reinforced copper-based composite material provided by the invention has obviously improved density, the density is more than 98%, the tensile strength is more than 130Mpa, and the shearing strength is more than 130 Mpa.
Drawings
In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the drawings that are needed in the examples will be briefly described below, it being understood that the following drawings only illustrate some examples of the present invention and therefore should not be considered as limiting the scope, and that other related drawings may be obtained from these drawings without inventive effort for a person skilled in the art. In the drawings:
FIG. 1 is a graph showing density comparisons of copper-based composites of test examples 1-4 of the present invention;
FIG. 2 is a graph of tensile test displacement versus test force for copper-based composites of test examples 1-4 of the present invention;
FIG. 3 is an SEM image of copper-based composite powder of test examples 1-4 of the present invention; wherein, (a) a Cu-1/4Fe composite material; (b) Cu-1/16Fe composite material; (c) Cu-1/4Fe-Ni composite material; (d) Cu-1/4Fe-Cr composite material;
FIG. 4 is a SEM image of tensile fracture of copper-based composite of test examples 1-4 of the present invention; wherein, (a) a Cu-1/4Fe composite material; (b) Cu-1/16Fe composite material; (c) Cu-1/4Fe-Ni composite material; (d) Cu-1/4Fe-Cr composite material;
FIG. 5 is a graph (X50) showing the wear scar of Cu-Fe (30N pressure) according to the test example of the present invention;
FIG. 6 is a graph of the grinding marks (. Times.50) of the test example Cu-1/4Fe-Ni of the present invention.
Detailed Description
For the purpose of making apparent the objects, technical solutions and advantages of the present invention, the present invention will be further described in detail with reference to the following examples and the accompanying drawings, wherein the exemplary embodiments of the present invention and the descriptions thereof are for illustrating the present invention only and are not to be construed as limiting the present invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The technical scheme of the invention is as follows:
A method for preparing a particle-reinforced copper-based composite material, comprising:
According to the weight percentage, 15-20wt% of iron, 1-5wt% of nickel, 0.5-1.5wt% of pretreated alumina whisker and 0.1-1wt% of pretreated graphene are mixed, ball milling treatment is carried out on the powder raw materials with the balance of copper, and a mixture is obtained through vacuum freeze drying; wherein, the alumina whisker is pretreated by sodium dodecyl sulfate; preprocessing graphene by adopting a rutin solution;
Carrying out hot-pressing sintering treatment on the mixture: prepressing at 0.5-1 MPa, heating from room temperature to 600-800 ℃ at a heating rate of 8-12 ℃/min under the vacuum degree of 5-10 Pa, and pressurizing to 1-2 MPa;
under the pressure of 1-2 MPa, the temperature is raised from 600-800 ℃ to 900-1000 ℃ at the temperature rising rate of 4-6 ℃/min, the temperature is kept for 1-5 h, and then the furnace is cooled to the room temperature.
Further, the preparation of the pretreated alumina whisker comprises the following steps:
mixing and uniformly stirring the aluminum oxide whisker and sodium dodecyl sulfate with the concentration of 1 g/L-5 g/L to obtain a mixed solution;
And performing ultrasonic dispersion on the mixed solution for 30-60 min, sealing and standing the dispersion liquid for 24-40 h, and performing suction filtration and vacuum freeze drying to obtain the pretreated alumina whisker.
Further, the doping amount of the alumina whisker in the obtained mixed solution is 0.1 g/mL-0.5 g/mL.
Further, the preparation of the pretreated graphene comprises:
Mixing graphene and rutin solution with the concentration of (0.5-2) multiplied by 10 -5 g/L, and stirring until the graphene is blended into the rutin solution to obtain a mixed solution;
And (3) performing ultrasonic dispersion for 20-50 min after sealing the mixed solution, standing the dispersion liquid for 24-40 h, and performing suction filtration and vacuum freeze drying to obtain the pretreated graphene.
Further, the doping amount of graphene in the obtained mixed solution is (0.1-0.5) gGNFs/40mL.
Further, the ball milling treatment performed includes:
mixing the pretreated alumina whisker, the pretreated graphene, the copper, the iron and the nickel, performing ball milling under the conditions that the ball milling rotating speed is 300 r/min-500 r/min, the ball milling time is 1 h-5 h, the forward and reverse transfer time is 15 min-30 min, and the acceleration time and the deceleration time are 5 s-20 s, and performing vacuum freeze drying on the obtained ball milling slurry to obtain the mixture.
Further, ball milling is carried out, and the ball-material ratio is 1-3:1.
Further, the ball milling medium adopted for ball milling is tertiary butanol.
Further, the powder raw materials used include: according to the weight percentage, 15-20wt% of iron, 1-5wt% of nickel, 1-5wt% of pretreated aluminum oxide whisker and 0.5wt% of pretreated graphene are mixed, and the balance is copper.
According to the preparation method of the particle reinforced copper-based composite material, disclosed by the invention, fewer layers (1-5 layers) of graphene are adopted, and rutin is used for carrying out dispersion surface modification so as to reduce the agglomeration of the graphene in the composite material. The hardness, the compactness and the wear resistance of the copper-based composite material can be improved by adopting the graphene with proper content. The alumina whisker is a manually controlled synthetic single crystal material, has high elastic modulus, chemical stability and thermal stability, can be added into a copper-based composite material to improve the strength, and can reduce the friction coefficient of the composite material. The alumina whiskers were effectively dispersed with a sodium dodecyl sulfate solution to prevent aggregation of their clusters. According to the preparation method of the particle reinforced copper-based composite material, the content of graphene in the powder raw material is 0.1-1 wt%, and the content of alumina whisker is 0.5-1.5 wt%, so that the graphene and the alumina whisker in the proportion are well dispersed, the stress can be effectively transmitted, and the overall strength of the composite material is enhanced.
According to the preparation method of the particle reinforced copper-based composite material, the alloy elements such as Fe are added, so that the effect of solid solution strengthening, grain refinement, reinforcement agglomeration prevention and the like can be achieved, and meanwhile, the good electric conductivity and heat conductivity of a Cu matrix can be maintained. Ni and Cu are both face-centered cubic structures, infinite solid solution can be realized by replacing atoms in grains, wettability of Ni and Cu is good, thermal parameters are similar, and Ni-based alloy powder can form a coating with good interface bonding performance with a copper matrix.
For further explanation of the present invention, the particle-reinforced copper-based composite material and the method for preparing the same are described below with reference to examples, but it should be understood that these examples are implemented on the premise of the technical solution of the present invention, and detailed implementation and specific operation procedures are given only for further explanation of the features and advantages of the present invention, and not limitation of the claims of the present invention, and the scope of protection of the present invention is not limited to the examples described below.
Example 1
The preparation method of the particle reinforced copper-based composite material of the embodiment comprises the following steps:
(1) Surface treatment of Al 2O3 whiskers
Mixing the weighed Al 2O3 whiskers with 1g/L concentration sodium dodecyl sulfate, stirring and uniformly mixing by using a glass rod, wherein the mixing amount of the Al 2O3 whiskers is 0.3g/mL, and then placing the uniformly mixed solution in an ultrasonic dispersing machine for ultrasonic dispersion for 40min, and continuing to disperse after cooling if the temperature is higher in the dispersing process. And (3) sealing and standing the solution for 30 hours after the dispersion is finished, and finally, pumping out the solution, drying the solution by using a vacuum freeze dryer and bagging the solution for later use.
(2) Surface treatment of graphene
Mixing weighed graphene with a rutin solution with the concentration of 0.5 multiplied by 10 -5 g/L, continuously stirring with a glass rod until most of the graphene above the liquid is dissolved in the rutin solution, sealing the uniformly mixed solution with a preservative film, then placing the solution in an ultrasonic dispersing machine for ultrasonic dispersion for 35min, and standing the solution for 30h. Finally, the wet powder filtered out by suction is dried by a vacuum freeze dryer YTLGJ-10A and then is packed for standby.
(3) Ball milling mixing material
The powder raw materials of the particle reinforced copper-based composite material comprise: 15 weight percent of iron, 1 weight percent of nickel, 0.5 weight percent of pretreated aluminum oxide whisker and 0.1 weight percent of pretreated graphene are calculated according to the weight percentage, and the balance is copper.
Mixing the powder according to the above proportion, using JC-QM-1 type ball mill, weighing various powders with corresponding mass according to the mass fraction of 300g, loading into a ball milling tank (agate tank), taking 75 g of powder per tank, performing high-energy ball milling in a planetary ball mill at the ball milling speed of 400r/min for 1h, performing forward and reverse alternation for 15min for 5s with the ball material ratio of 1:1, and adding tert-butyl alcohol as a ball milling medium (about 3 g). And then the obtained ball-milling slurry is put into a refrigerator for freezing, and the vacuum freeze dryer is used for drying after the ball-milling slurry is frozen. The final powder was dried using a vacuum freeze dryer without risk of oxidation.
(4) Hot pressed sintering
And (3) sequentially carrying out hot-pressing sintering on the dried powder, wherein the selected sample is a graphite mold with the diameter of 60mm, placing the composite powder into a vacuum-hot-pressing sintering furnace of JZM-1200 for compaction after sample loading according to operation, vacuumizing, continuously heating and pressurizing, preserving heat, and finally cooling along with the furnace. The sintering process is that firstly, the temperature is raised to 600 ℃ from room temperature at the temperature rise rate of 8 ℃/min under the pre-pressure of 0.5MPa and the vacuum degree of 5Pa, and the pressure is increased to 1MPa;
Heating from 600 ℃ to 900 ℃ at a heating rate of 4 ℃/min under the pressure of 1MPa, preserving heat for 1h, cooling to room temperature along with a furnace, demoulding and sampling to obtain a cylindrical sample with the diameter of 60mm and the thickness of about 12mm, and obtaining a formed composite material block.
The particle reinforced copper-based composite material prepared in the embodiment is subjected to performance test, and the compactness is 98.03%, the tensile strength is 131.589Mpa, and the shearing strength is 130.4Mpa.
Example 2
The preparation method of the particle reinforced copper-based composite material of the embodiment comprises the following steps:
(1) Surface treatment of Al 2O3 whiskers
Mixing the weighed Al 2O3 whiskers with the prepared sodium dodecyl sulfate with the concentration of 2g/L, stirring and uniformly mixing by using a glass rod, wherein the doping amount of the Al 2O3 whiskers is 0.1g/mL, then placing the uniformly mixed solution in an ultrasonic dispersing machine for ultrasonic dispersion for 30min, and continuing to disperse after cooling if the temperature is higher in the dispersing process. And (3) sealing and standing the solution for 24 hours after the dispersion is finished, and finally, pumping out the solution, drying the solution by using a vacuum freeze dryer and bagging the solution for later use.
(2) Surface treatment of graphene
Mixing weighed graphene with a rutin solution with the concentration of 2X 10 -5 g/L, continuously stirring with a glass rod until most of the graphene above the liquid is dissolved in the rutin solution, sealing the uniformly mixed solution with a preservative film, then placing the solution in an ultrasonic dispersing machine for ultrasonic dispersion for 20min, and standing the solution for 24h. Finally, the wet powder filtered out by suction is dried by a vacuum freeze dryer YTLGJ-10A and then is packed for standby.
(3) Ball milling mixing material
The powder raw materials of the particle reinforced copper-based composite material comprise: 17.55wt% of iron, 2.83wt% of nickel, 1% of pretreated alumina whiskers and 0.5wt% of pretreated graphene are mixed according to the weight percentage, and the balance is copper.
Mixing the powder according to the above proportion, using JC-QM-1 type ball mill, weighing various powders with corresponding mass according to the mass fraction of 300g, loading into a ball milling tank (agate tank), taking 75 g of powder from each tank, performing high-energy ball milling in a planetary ball mill at the ball milling speed of 300r/min for 2h, performing forward and reverse transition for 18min for 10s, performing ball material acceleration and deceleration for 2:1, and adding tertiary butanol as a ball milling medium (about 3 g). And then the obtained ball-milling slurry is put into a refrigerator for freezing, and the vacuum freeze dryer is used for drying after the ball-milling slurry is frozen. The final powder was dried using a vacuum freeze dryer without risk of oxidation.
(4) Hot pressed sintering
And (3) sequentially carrying out hot-pressing sintering on the dried powder, wherein the selected sample is a graphite mold with the diameter of 60mm, placing the composite powder into a vacuum-hot-pressing sintering furnace of JZM-1200 for compaction after sample loading according to operation, vacuumizing, continuously heating and pressurizing, preserving heat, and finally cooling along with the furnace. The sintering process is that firstly, the temperature is raised to 800 ℃ from room temperature at the temperature rise rate of 10 ℃/min under the pre-pressure of 0.53MPa and the vacuum degree of 6.5Pa, and the pressure is increased to 1.39MPa;
and (3) heating from 800 ℃ to 1000 ℃ at a heating rate of 5 ℃/min under the pressure of 1.39MPa, preserving heat for 2 hours, cooling to room temperature along with a furnace, demoulding, sampling to obtain a cylindrical sample with the diameter of 60mm and the thickness of about 12mm, and obtaining a formed composite material block.
The particle reinforced copper-based composite material prepared in the embodiment is subjected to performance test, and the compactness is 98.62%, the tensile strength is 136.676Mpa, and the shearing strength is 134Mpa.
Example 3
The preparation method of the particle reinforced copper-based composite material of the embodiment comprises the following steps:
(1) Surface treatment of Al 2O3 whiskers
Mixing the weighed Al 2O3 whiskers with 5g/L sodium dodecyl sulfate, stirring and uniformly mixing by using a glass rod, wherein the mixing amount of the Al 2O3 whiskers is 0.5g/mL, and then placing the uniformly mixed solution in an ultrasonic dispersing machine for ultrasonic dispersion for 60min, and continuing to disperse after cooling if the temperature is higher in the dispersing process. And (3) sealing and standing the solution for 40 hours after the dispersion is finished, and finally, pumping out the solution, drying the solution by using a vacuum freeze dryer and bagging the solution for later use.
(2) Surface treatment of graphene
Mixing weighed graphene with a rutin solution with the concentration of 1X 10 -5 g/L, continuously stirring with a glass rod until most of the graphene above the liquid is dissolved in the rutin solution, sealing the uniformly mixed solution with a preservative film, then placing the solution in an ultrasonic dispersing machine for ultrasonic dispersion for 50min, and standing the solution for 40h. Finally, the wet powder filtered out by suction is dried by a vacuum freeze dryer YTLGJ-10A and then is packed for standby.
(3) Ball milling mixing material
The powder raw materials of the particle reinforced copper-based composite material comprise: iron 20wt%, nickel 5wt%, pretreated alumina whisker 1.5wt% and pretreated graphene 1wt% with the balance being copper.
Mixing the powder according to the above proportion, using JC-QM-1 type ball mill, weighing various powders with corresponding mass according to the mass fraction of 300g, loading into a ball milling tank (agate tank), taking 75 g of powder from each tank, performing high-energy ball milling in a planetary ball mill at the ball milling speed of 500r/min for 5h, performing forward and reverse alternation for 30min for 20s, performing ball material acceleration and deceleration for 3:1, and adding tertiary butanol as a ball milling medium (about 3 g). And then the obtained ball-milling slurry is put into a refrigerator for freezing, and the vacuum freeze dryer is used for drying after the ball-milling slurry is frozen. The final powder was dried using a vacuum freeze dryer without risk of oxidation.
(4) Hot pressed sintering
And (3) sequentially carrying out hot-pressing sintering on the dried powder, wherein the selected sample is a graphite mold with the diameter of 60mm, placing the composite powder into a vacuum-hot-pressing sintering furnace of JZM-1200 for compaction after sample loading according to operation, vacuumizing, continuously heating and pressurizing, preserving heat, and finally cooling along with the furnace. The sintering process is that firstly, the temperature is raised from room temperature to 700 ℃ at the temperature rise rate of 12 ℃/min under the pre-pressure of 1MPa and the vacuum degree of 10Pa, and the pressure is increased to 2MPa;
And (3) under the pressure of 2MPa, heating from 700 ℃ to 950 ℃ at a heating rate of 6 ℃/min, preserving heat for 5 hours, cooling to room temperature along with a furnace, demoulding, sampling to obtain a cylindrical sample with the diameter of 60mm and the thickness of about 12mm, and obtaining a formed composite material block.
The particle reinforced copper-based composite material prepared in the embodiment is subjected to performance test, and the compactness is 98.26%, the tensile strength is 133.223Mpa, and the shearing strength is 132.5Mpa.
Test example 1
The preparation of the copper-based composite material of this test example was identical to example 2, except that the powder raw material of the composite material was Cu-1/4Fe, wherein Cu 80.71wt%, fe 17.79wt%, pretreated alumina whisker 1wt% and pretreated graphene 0.5wt%.
Test example 2
The preparation of the copper-based composite material of this test example was identical to example 2, except that the powder material of the composite material was Cu-1/16Fe, wherein Cu 93.36wt%, fe 5.14wt%, pretreated alumina whisker 1wt% and pretreated graphene 0.5wt%.
Test example 3
The preparation of the copper-based composite material of this test example was identical to example 2, except that the powder raw material of the composite material was Cu-1/4 Fe-1/32Ni, in which Cu 78.39wt%, fe 17.55wt%, ni 2.83wt%, pretreated alumina whisker 1% and pretreated graphene 0.5wt%.
Test example 4
The preparation of the copper-based composite material of this test example was identical to example 2, except that the powder raw material of the composite material was Cu-1/4 Fe-1/32 Cr, wherein Cu 78.64wt%, fe 17.34wt%, cr 2.51wt%, pretreated alumina whisker 1% and pretreated graphene 0.5wt%.
The copper-based composite materials of test examples 1 to 4 were subjected to density testing, and the results are shown in FIG. 1. The tensile test was conducted on the copper-based composite materials of test examples 1 to 4, and the results are shown in FIG. 2.
As shown in the results of fig. 1 and fig. 2, the tensile strength of the composite material increases with the increase of the content of the copper matrix added with Fe, and the addition of Fe is beneficial to the distribution of two nano phases of graphene and aluminum oxide whisker in the copper matrix, so that the stress transmission can be improved, and the strength of the copper-based composite material can be improved. The addition of Fe reduces the agglomeration condition of the alumina whisker and the graphene, and introduces a third phase Ni alloy element into the Cu-1/4Fe composite material, so that the density of the composite material and the reinforcing effect of the nano reinforcing phase on a copper matrix can be further improved, the density is 98.62%, the tensile strength is 136.676Mpa, and the shearing strength is 134Mpa. The section of the Cu-1/4 Fe-1/32Ni composite material added with Ni into the Cu-1/4Fe composite material is free of fibrous alumina whiskers and graphene, the distribution of the ductile pits is uniform, and the depth deepening size of the ductile pits is increased. The addition of Ni element can strengthen the interface combination of fibrous alumina whisker and graphene in the composite material and the copper matrix, the size of the ductile fossa becomes larger, the deepening distribution is more uniform, and the plasticity of the composite material is further improved.
The copper-based composite powder and tensile fracture of test examples 1 to 4 were subjected to electron microscopic scanning analysis, and the results are shown in fig. 3 and 4.
In fig. 3, the copper particles and the iron particles are plastically deformed during the mechanical alloying process of the ball mill, and most of them are changed from the original granular shape into a bar shape or an oval shape, and are bonded to each other. The alumina whisker is still distributed in the composite powder in fibrous form, and the alumina whisker is adhered to other powder grains under the grinding action. The addition of Ni element can raise the homogeneous mixing degree of the powder and improve the agglomeration of nanometer powder.
In fig. 4, it is seen that in the fracture morphology of the composite material, the ductile fracture occurs because the plastic denaturation capability of the copper matrix is strong, plastic flow exists, no cleavage plane appears in the fracture, and a large number of ductile pits appear. In general, the greater the number of dimples of a material, the greater the size and the deeper the dimple, the better the plasticity of the material. The number of the ductile pits in the fracture of the Cu-1/4Fe composite material is more, the depth is shallower and more uniform, and the ductile pits contain a small amount of fibrous alumina whiskers and flaky graphene. The ductile fossa in the fracture of the Cu-1/16Fe composite material is less and shallow in depth, uneven in distribution and provided with a large number of tearing edges, a large number of fibrous alumina whiskers exist, the fibrous alumina whiskers and graphene are not contained in the fracture surface of the Cu-1/4Fe-1/32Ni composite material added with Ni into the Cu-1/4Fe composite material, the ductile fossa is evenly distributed, and the depth deepening size of the ductile fossa is increased. On the section of the Cu-1/4Fe-1/32Cr composite material, part of the ductile pits become deep, but the size distribution of the ductile pits is uneven, a large number of tearing edges exist, and a small amount of fibrous alumina still exists.
The phase interface is the origin of crack initiation, and the fracture of the composite material is the bonding interface of the composite material. The Fe in the powder SEM is combined to enable the nano phase to be more uniformly dispersed and strengthen the adsorption of the nano phase and the particles, fibrous alumina whisker and flaky graphene in the composite material are reduced along with the increase of the Fe content, the interface combination of the two nano phases and a copper matrix is strengthened, and the plasticity of the composite material is improved. The interface bonding capability of graphene and a copper matrix is better due to the doping of Cr element in the Cu-1/4Fe composite material, the ductile fossa is deepened, the fibrous alumina whisker in the composite material and the interface bonding of graphene and the copper matrix are enhanced due to the addition of Ni element, the ductile fossa is larger in size, deeper and distributed more uniformly, and the plasticity of the composite material is improved.
The copper-based composite of Cu-Fe (under 30N pressure) and Cu-1/4Fe-1/32Ni was subjected to wear scar testing, and the results are shown in FIGS. 5 and 6.
As shown in the results of FIGS. 5 and 6, the Cu-Fe (under 30N pressure) wear amount was 0.5997 and the Cu-1/4Fe-Ni wear amount was 0.64. The friction and wear performance of Cu-1/4Fe-Ni is better. In the friction process, an adhesive abrasion mechanism is firstly dominant, and can be seen from a tiny line on an abrasion mark graph, an oxide film on the surface of a sample is damaged, the color of abrasive dust is gradually changed from black to a matrix color, the abrasion is oxidized, the existence of a convex peak and the like can lead the initial friction coefficient of a material to be accelerated greatly, the friction coefficient is gradually stabilized along with the experimental process, at the moment, the phenomenon of furrows and falling off is abrasive particle abrasion, the adhesive abrasion is auxiliary, and the abrasion mechanisms are mutually alternated and coexist in the whole process.
The foregoing description of the embodiments has been provided for the purpose of illustrating the general principles of the invention, and is not meant to limit the scope of the invention, but to limit the invention to the particular embodiments, and any modifications, equivalents, improvements, etc. that fall within the spirit and principles of the invention are intended to be included within the scope of the invention.
Claims (5)
1. A method for preparing a particle-reinforced copper-based composite material, comprising:
Mixing 78.39 weight percent of Cu, 17.55 weight percent of Fe, 2.83 weight percent of Ni, 1 weight percent of pretreated alumina whisker and 0.5 weight percent of pretreated graphene according to the weight percent, performing ball milling treatment, and performing vacuum freeze drying to obtain a mixture; wherein, the alumina whisker is pretreated by sodium dodecyl sulfate; preprocessing graphene by adopting a rutin solution;
Carrying out hot-pressing sintering treatment on the mixture: prepressing at 0.5-1 MPa, heating from room temperature to 600-800 ℃ at a heating rate of 8-12 ℃/min under the vacuum degree of 5-10 Pa, and pressurizing to 1-2 MPa;
Heating from 600 ℃ to 800 ℃ to 900 ℃ to 1000 ℃ at a heating rate of 4 ℃/min to 6 ℃/min under the pressure of 1MPa to 2MPa, preserving heat for 1h to 5h, and cooling to room temperature along with a furnace;
The preparation of the pretreated alumina whisker comprises the following steps:
mixing and uniformly stirring the aluminum oxide whisker and sodium dodecyl sulfate with the concentration of 1 g/L-5 g/L to obtain a mixed solution;
Performing ultrasonic dispersion on the mixed solution for 30-60 min, sealing and standing the dispersion liquid for 24-40 h, and performing suction filtration and vacuum freeze drying to obtain the pretreated alumina whisker;
The doping amount of the alumina whisker in the obtained mixed solution is 0.1 g/mL-0.5 g/mL;
the preparation of the pretreated graphene comprises the following steps:
Mixing graphene and rutin solution with the concentration of (0.5-2) multiplied by 10 -5 g/L, and stirring until the graphene is blended into the rutin solution to obtain a mixed solution;
performing ultrasonic dispersion for 20-50 min after sealing the mixed solution, standing the dispersion liquid for 24-40 h, and performing suction filtration and vacuum freeze drying to obtain the pretreated graphene;
The doping amount of graphene in the obtained mixed solution is (0.1-0.5) gGNFs/40mL.
2. The method for preparing a particle-reinforced copper-based composite material according to claim 1, wherein the ball milling treatment comprises:
mixing the pretreated alumina whisker, the pretreated graphene, the copper, the iron and the nickel, performing ball milling under the conditions that the ball milling rotating speed is 300 r/min-500 r/min, the ball milling time is 1 h-5 h, the forward and reverse transfer time is 15 min-30 min, and the acceleration time and the deceleration time are 5 s-20 s, and performing vacuum freeze drying on the obtained ball milling slurry to obtain the mixture.
3. The method for preparing the particle-reinforced copper-based composite material according to claim 2, wherein the ball-milling is carried out at a ball-to-material ratio of 1-3:1.
4. The method for preparing a particle-reinforced copper-based composite material according to claim 2, wherein the ball milling medium used for ball milling is t-butanol.
5. A particle-reinforced copper-based composite material, characterized in that it is produced by the method for producing a particle-reinforced copper-based composite material according to any one of claims 1 to 4.
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