CN113337747B - Preparation method of high-strength and high-conductivity copper alloy - Google Patents
Preparation method of high-strength and high-conductivity copper alloy Download PDFInfo
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- 229910000881 Cu alloy Inorganic materials 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 44
- 239000010949 copper Substances 0.000 claims abstract description 38
- 229910052802 copper Inorganic materials 0.000 claims abstract description 38
- 239000002131 composite material Substances 0.000 claims abstract description 25
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000005245 sintering Methods 0.000 claims abstract description 15
- 239000002243 precursor Substances 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 3
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 20
- 239000010439 graphite Substances 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 13
- 229910002530 Cu-Y Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 239000011268 mixed slurry Substances 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 13
- 238000009826 distribution Methods 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000005728 strengthening Methods 0.000 description 7
- 239000000956 alloy Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000013329 compounding Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- 238000001704 evaporation Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 230000001427 coherent effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005088 metallography Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
Abstract
The invention discloses a preparation method of a high-strength high-conductivity copper alloy, which comprises the following steps of 1: preparing a precursor; step 2: calcining and reducing; and step 3: and (4) spark plasma sintering. The preparation method is simple, and only the raw materials of pure copper powder and yttrium nitrate hexahydrate are needed to prepare Y 2 O 3 And (3) sintering the composite powder which is dispersed and distributed on the surface of the copper powder to obtain a compact block. Y is 2 O 3 The distribution of the copper is uniform, the copper crystal grains can be refined, the strength and the hardness of the copper alloy are improved and respectively reach 251.1-303.9 MPa and 101.3HV omega 140.5HV, and simultaneously, the conductivity can be maintained at an extremely high level of 78-98% IACS, so that the invention can be applied to large-scale industrial production, the performance of electrical materials such as an electrical contact is improved, and the service life of the electrical contact is prolonged.
Description
Technical Field
The invention belongs to the technical field of copper-based composite material preparation, and particularly relates to a preparation method of a high-strength and high-conductivity copper alloy.
Background
Copper and its alloy have excellent conductivity and heat conductivity, so that they are widely used in electrical equipment such as electrical contact materials, integrated circuit lead frames and resistance welding electrodes. With the rapid development of modern science and technology, especially in the high-tech industrial fields of aerospace, aviation, electronics, military and the like, the requirements of materials on strength, wear resistance, high temperature resistance and the like are higher and higher, the traditional copper and copper alloy can not meet the requirements of the performances, and the conductivity and the strength of the copper and copper alloy can not be considered at the same time. Therefore, on the premise of ensuring good conductivity, the strength of copper and copper alloy is greatly improved, and the significance of developing copper and copper alloy materials with high strength and high conductivity is great.
Compared with the main solid solution strengthening mechanism in copper alloy, the copper-based composite material is prepared by adding fine dispersed ceramic particles on a copper matrix, wherein the dispersion strengthening mechanism is another important strengthening mechanism. Based on this idea, researchers have conducted many studies on the preparation of copper-based composites and their properties. The predominant ceramic particle strengthening phase at present has Y 2 O 3 、Al 2 O 3 、ZrO 2 、SiC、TiB 2 And AlN and the like. Wherein the strengthening phase Y 2 O 3 The rare earth oxide has extremely high thermodynamic stability, and the fluorite structure of the rare earth oxide can form a coherent interface with a copper matrix under specific conditions, so that the mechanical property of copper can be improved to the maximum extent, and the conductivity can be maintained at a high level. How to handle Y 2 O 3 The proper addition to the copper matrix and the optimal strengthening effect are always a difficult problem. Since the rare earth elements have a very low solid solubility in copper, they often remain as intermetallic compounds at the grain boundaries of copper. Y prepared by internal oxidation 2 O 3 Coarse particles, easy agglomeration, making Y 2 O 3 The strengthening effect is greatly reduced.
Disclosure of Invention
The invention aims to provide a doped Y 2 O 3 A preparation method of a reinforced copper-based composite material. The invention only needs raw materials of pure copper powder and yttrium nitrate hexahydrate, and prepares Y by a simple and convenient process 2 O 3 Copper-based composite material, copper matrix and Y in dispersed distribution 2 O 3 The bonding force between the copper alloy and the metal is good, and the conductivity and the ductility of the traditional ODS copper alloy are improved while the strength is ensured.
A preparation method of a high-strength high-conductivity copper alloy is characterized by comprising the following steps: comprises the following steps:
step 1: precursor preparation
Dissolving pure copper powder and a certain amount of yttrium nitrate hexahydrate in deionized water to ensure that the pure copper powder and the certain amount of yttrium nitrate hexahydrate are completely infiltrated, adding a polytetrafluoroethylene stirrer into the mixed slurry to ensure that the solution has certain fluidity, and carrying out magnetic treatmentStirring, heating in oil bath to evaporate deionized water, and drying the obtained powder to obtain Cu-Y (NO) 3 A precursor;
step 2: calcination and reduction
Putting the precursor obtained in the step 1 in a tube furnace, introducing hydrogen atmosphere, heating to 600 ℃, preserving heat, cooling to 500 ℃ after heat preservation, and then cooling along with the furnace to obtain Cu-Y 2 O 3 Compounding powder;
and step 3: spark plasma sintering
Weighing 12-15 g of Cu-Y obtained in the step 2 2 O 3 Pouring the composite powder into a graphite mold, placing a graphite pressure head at two ends of the composite powder, prepressing the powder in the graphite mold, placing the graphite mold into a sintering furnace, rapidly heating to 900-950 ℃, and preserving heat for 5min to obtain Y 2 O 3 The copper-based composite material is dispersed and distributed and compact.
In the step 1, the pure copper powder is spherical, the granularity is 20 mu m, the purity is 99.5 percent, and the purity of the yttrium nitrate hexahydrate is 99.9 percent.
The content of yttrium nitrate hexahydrate in said step 1 is as follows Cu-1wt% Y 2 O 3 ，Cu-3wt％Y 2 O 3 ，Cu-5wt％Y 2 O 3 And proportioning the final target.
In the step 1, the oil bath temperature is 120-140 ℃, the powder drying temperature is 100-140 ℃, and the drying time is 12-24 h.
The reason why the hydrogen atmosphere is used in step 2 is that it can perform a reducing function in consideration of partial oxidation of copper.
In the step 2, the heating rate is 5 ℃/min, the cooling rate is 5 ℃/min, and the heat preservation time is 2-4 h.
Y (NO) in said step 2 3 ) 3 Decomposition to Y above 400 ℃ 2 O 3 。
The diameter of the graphite die in the step 3 is 20mm.
The heating rate in the step 3 is 100 ℃/min.
In the step 3, the pre-pressure of the powder is 10MPa, and the highest pressure is 50-70MPa.
And 3, the temperature measuring device is a thermocouple, so that the temperature in the furnace cavity is measured more accurately.
And (3) adding carbon paper between the powder and the graphite die in the step (3) to facilitate demoulding after sintering.
And in the step 3, a carbon felt is additionally arranged outside the graphite mould for heat preservation in the sintering process.
The invention has the beneficial effects that: compared with the prior art, the preparation process is simple, and Y can be prepared only by using the raw materials of pure copper powder and yttrium nitrate hexahydrate 2 O 3 And (3) sintering the composite powder which is dispersed and distributed on the surface of the copper powder to obtain a compact block. Y is 2 O 3 The copper alloy has uniform distribution, can refine copper crystal grains, improves the strength and the hardness of the copper alloy, respectively reaches 251.1MPa to 303.9MPa and 101.3HV omega 140.5HV, and simultaneously can maintain the electric conductivity at an extremely high level of 78 to 98% IACS, so that the invention can be applied to large-scale industrial production, improves the performance of electrical materials such as electrical contacts and the like, and prolongs the service life of the electrical materials.
Drawings
Fig. 1 is a morphology diagram of pure copper powder particles.
FIG. 2 is Cu-Y 2 O 3 A composite powder particle morphology map;
wherein: (a), (b) and (c) are Cu-1wt% respectively 2 O 3 Composite powder particles, cu-3wt% 2 O 3 Composite powder particles, cu-5wt% 2 O 3 A morphology of the composite powder particles.
FIG. 3 is Cu-Y 2 O 3 Bulk metallography and their particle size distribution map;
wherein: (a) Respectively, cu-1wt% of 2 O 3 Metallographic phase and particle size distribution map; (c) Respectively, (d) Cu-3wt% of Y 2 O 3 Metallographic phase and particle size distribution map; (e) Respectively, cu-5wt%, (f) 2 O 3 Metallographic phase and particle size distribution.
Detailed Description
The invention is further described with reference to the following figures and detailed description.
Example 1:
(1) Weighing 0.6785g of yttrium nitrate hexahydrate, dissolving in 100ml of deionized water, adding 19.8g of pure copper powder, adding a polytetrafluoroethylene stirrer into the mixed slurry, carrying out magnetic stirring, raising the temperature of an oil bath to 120 ℃, evaporating all deionized water to dryness, and drying the obtained powder in a drying oven for 24 hours at 100 ℃;
(2) The obtained Cu-Y (NO) 3 Placing the powder in a tube furnace, introducing hydrogen at a flow rate of 300ml/min, heating the tube furnace to 600 deg.C at 5 deg.C/min for 2h, cooling to 500 deg.C at 5 deg.C/min, and furnace cooling to obtain Cu-1wt% Y 2 O 3 Compounding powder;
(3) Weighing Cu-1wt% to 2 O 3 Pouring 12g of composite powder into a graphite mold, placing a graphite pressure head at two ends of the composite powder, pre-pressing the powder in the mold, placing the pre-pressed powder into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, setting the sintering procedure to heat to 600 ℃ at 100 ℃/min and preserving heat for 5min, heating to 900 ℃ at 100 ℃/min and preserving heat for 5min (increasing the pressure from 10MPa to 50MPa in the process of heating to 900 ℃ at 600 ℃), and quickly reducing the temperature to room temperature after heat preservation is finished to obtain Cu-1wt% Y 2 O 3 And (3) a block body.
Cu-1wt% after sintering 2 O 3 The Vickers hardness of the alloy material reaches 101.3HV, which is higher than 68HV of pure copper; the material strength reached 251.1MPa, which is higher than 230MPa for pure copper material, and the conductivity was 98% IACS, which is almost equal to pure copper.
Example 2:
(1) Weighing 2.0354g of yttrium nitrate hexahydrate, dissolving the yttrium nitrate hexahydrate in 100ml of deionized water, adding 19.4g of pure copper powder, adding a polytetrafluoroethylene stirrer into the mixed slurry, performing magnetic stirring, raising the temperature of an oil bath to 130 ℃, evaporating all the deionized water to dryness, and drying the obtained powder in a drying box for 16 hours at 120 ℃;
(2) The obtained Cu-Y (NO) 3 Putting the powder in a tube furnace, introducing hydrogen, setting the flow rate to be 300ml/min, setting the temperature rise program of the tube furnace to be increased to 600 ℃ at the speed of 5 ℃/min, preserving the heat for 3h, then reducing the temperature to 500 ℃ at the speed of 5 ℃/min, cooling along with the furnace, and finally obtaining Cu-3wt%％Y 2 O 3 Compounding powder;
(3) Weighing Cu-3wt% of 2 O 3 Pouring 12g of composite powder into a graphite mold, placing a graphite pressure head at two ends of the composite powder, pre-pressing the powder in the mold, placing the pre-pressed powder into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, setting the sintering procedure to heat up to 600 ℃ at 100 ℃/min and preserving heat for 5min, heating up to 920 ℃ at 100 ℃/min and preserving heat for 5min (increasing the pressure from 10MPa to 60MPa in the process of heating up to 920 ℃ at 600 ℃), quickly reducing the temperature to room temperature after the heat preservation is finished, and obtaining Cu-3wt% Y 2 O 3 And (3) a block body.
Cu-3wt% after sintering 2 O 3 The Vickers hardness of the alloy material reaches 125.7HV, which is higher than 68HV of pure copper; the material strength reached 290.7MPa, higher than 230MPa for the pure copper material, the conductivity was 95% IACS, which is essentially equal to that of pure copper.
Example 3:
(1) Weighing 3.3923g of yttrium nitrate hexahydrate, dissolving the yttrium nitrate hexahydrate in 100ml of deionized water, adding 19g of pure copper powder, adding a polytetrafluoroethylene stirrer into the mixed slurry, carrying out magnetic stirring, raising the oil bath temperature to 140 ℃, evaporating all the deionized water to dryness, and drying the obtained powder in a drying oven at 140 ℃ for 12 hours;
(2) The obtained Cu-Y (NO) 3 Placing the powder in a tube furnace, introducing hydrogen gas at a flow rate of 300ml/min, heating the tube furnace to 600 deg.C at 5 deg.C/min, maintaining for 4 hr, cooling to 500 deg.C at 5 deg.C/min, and cooling with the furnace to obtain Cu-5wt% Y 2 O 3 Compounding powder;
(3) Weighing Cu-5wt% of 2 O 3 12g of composite powder, pouring the composite powder into a graphite mold, placing a graphite pressure head at two ends of the composite powder, pre-pressing the powder in the mold, placing the pre-pressed powder into a discharge plasma sintering furnace, vacuumizing the furnace chamber at room temperature, setting the sintering program to heat to 600 ℃ at 100 ℃/min and preserving heat for 5min, heating to 950 ℃ at 100 ℃/min and preserving heat for 5min (the pressure is increased from 10MPa to 70MPa in the process of heating to 950 ℃ at 600 ℃), and quickly reducing to room temperature after the heat preservation is finished to obtain Cu-5wt% Y 2 O 3 And (3) a block body.
Cu-5wt% after sintering 2 O 3 The Vickers hardness of the alloy material reaches 140.5HV, which is higher than 68HV of pure copper; the material strength reached 303.9MPa, which is higher than 230MPa for pure copper material, and the conductivity was 78% IACS, which is a greater reduction compared to pure copper.
As can be seen from Table 1, three kinds of Y 2 O 3 The density of the block body is close to 100 percent, and Y 2 O 3 The hardness of the sample can be increased to 251.1MPa to 303.9MPa and 101.3HV to 140.5HV, respectively, and the conductivity can reach a higher level of 78 to 98% IACS.
TABLE 1 Cu-Y 2 O 3 Mechanical property meter for block
As can be seen from FIG. 1, the pure copper powder is spherical, has a smooth surface and a particle size of about 20 μm.
As can be seen from FIG. 2, fine particles appeared on the surface of the powder, and it was confirmed by the energy spectrum analysis that the surface was uniformly covered with Y 2 O 3 。
It can be seen from FIG. 3 that when Y is 2 O 3 In amounts of 1 and 3wt%, Y 2 O 3 Present at the copper grain boundaries predominantly in the form of polygonal fine particles; and Y is 2 O 3 When it reaches 5wt%, Y 2 O 3 And the copper is wrapped on the copper grain boundary in a net shape. Statistics of their grain sizes revealed that with Y 2 O 3 The increase of the content gradually reduces the size of copper crystal grains, and the minimum size of the copper crystal grains can reach 13 mu m.
The preparation method is simple, and Y can be prepared only by raw materials of pure copper powder and yttrium nitrate hexahydrate 2 O 3 And (3) sintering the composite powder which is dispersedly distributed on the surface of the copper powder to obtain a compact block. Y is 2 O 3 The distribution of (2) is uniform, the copper crystal grains can be refined, the strength and hardness of the copper alloy are improved to 251.1 to 303.9MPa and 101.3 to 140.5HV, respectively, while the conductivity can be maintained at 78 to 98%The high level of the invention can be applied to large-scale industrial production, improve the performance of electrical materials such as electrical contacts and the like, and prolong the service life of the electrical materials.
The above examples merely illustrate specific embodiments of the present disclosure, but embodiments of the present disclosure are not limited by the above. Any changes, modifications, substitutions, combinations, and simplifications which do not materially depart from the spirit and principles of the inventive concepts of this disclosure are intended to be equivalent permutations and to be included within the scope of the invention as defined by the claims.
Claims (6)
1. A preparation method of a high-strength high-conductivity copper alloy is characterized by comprising the following steps: comprises the following steps:
step 1: precursor preparation
Dissolving pure copper powder and yttrium nitrate hexahydrate in deionized water to ensure that the pure copper powder and the yttrium nitrate hexahydrate are completely infiltrated, adding a polytetrafluoroethylene stirrer into the mixed slurry to ensure that the solution has certain fluidity, performing magnetic stirring, performing oil bath heating to evaporate the deionized water to dryness, drying the obtained powder, and finally obtaining Cu-Y (NO) 3 A precursor, the pure copper powder has a particle size of 20 μm, and the content of yttrium nitrate hexahydrate is calculated as Cu-1wt% Y 2 O 3 ，Cu-3wt％Y 2 O 3 ，Cu-5wt％Y 2 O 3 Proportioning the final target;
and 2, step: calcination and reduction
Putting the precursor obtained in the step 2 in a tube furnace, introducing hydrogen atmosphere, heating to 600 ℃, preserving heat, cooling to 500 ℃ after heat preservation, and then cooling along with the furnace to obtain Cu-Y 2 O 3 The heat preservation time is 2-4 h, the heating rate is 5 ℃/min, and the cooling rate is 5 ℃/min;
and 3, step 3: spark plasma sintering
Weighing 12-15 g of Cu-Y obtained in step 2 2 O 3 Pouring the composite powder into a graphite mold, placing a graphite pressure head at two ends of the composite powder, prepressing the powder in the graphite mold, placing the graphite mold into a sintering furnace, rapidly heating to 900-950 ℃, and preserving heat for 5min to obtain Y 2 O 3 The copper-based composite material is dispersed and distributed and compact.
2. The method for preparing the high-strength high-conductivity copper alloy according to claim 1, wherein the method comprises the following steps: in the step 1, the pure copper powder is spherical, the purity is 99.5%, and the purity of the yttrium nitrate hexahydrate is 99.9%.
3. The method for preparing the high-strength high-conductivity copper alloy according to claim 1, wherein the method comprises the following steps: in the step 1, the oil bath temperature is 120-140 ℃, the powder drying temperature is 100-140 ℃, and the drying time is 12-24 h.
4. The method for preparing the high-strength high-conductivity copper alloy according to claim 1, wherein the method comprises the following steps: the diameter of the graphite die in the step 3 is 20mm.
5. The method for preparing the high-strength high-conductivity copper alloy according to claim 1, wherein the method comprises the following steps: the heating rate in the step 3 is 100 ℃/min.
6. The method for preparing the high-strength high-conductivity copper alloy according to claim 1, wherein the method comprises the following steps: in the step 3, the pre-pressure of the powder is 10MPa, and the highest pressure is 50-70MPa.
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| CN107217171B (en) * | 2017-06-07 | 2019-05-24 | 江西理工大学 | A kind of rare earth doped oxide Cu-base composites of liquid liquid and preparation method thereof |
| CN109234557B (en) * | 2018-10-24 | 2020-05-22 | 合肥工业大学 | Superfine high-hardness W-Y2O3Method for preparing composite material |
| CN111057928B (en) * | 2020-01-03 | 2021-04-02 | 合肥工业大学 | WC-Co-Y with excellent comprehensive mechanical properties2O3Hard alloy and preparation method thereof |
| CN111996408B (en) * | 2020-08-27 | 2021-11-09 | 河南科技大学 | Preparation method of oxide ceramic particle reinforced Cu-based composite material |
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