CN117604321B - Completely coherent oxide dispersion strengthening copper-based composite material and preparation method thereof - Google Patents
Completely coherent oxide dispersion strengthening copper-based composite material and preparation method thereof Download PDFInfo
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- 239000010949 copper Substances 0.000 title claims abstract description 130
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 126
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 115
- 239000002131 composite material Substances 0.000 title claims abstract description 97
- 238000005728 strengthening Methods 0.000 title claims abstract description 36
- 230000001427 coherent effect Effects 0.000 title claims abstract description 35
- 239000006185 dispersion Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 52
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 33
- 239000000956 alloy Substances 0.000 claims abstract description 33
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000001257 hydrogen Substances 0.000 claims abstract description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 27
- 230000009467 reduction Effects 0.000 claims abstract description 27
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 23
- 239000012535 impurity Substances 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 21
- 239000011159 matrix material Substances 0.000 claims abstract description 18
- 238000005098 hot rolling Methods 0.000 claims abstract description 16
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229940075624 ytterbium oxide Drugs 0.000 claims abstract description 11
- 229910003454 ytterbium oxide Inorganic materials 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 238000001192 hot extrusion Methods 0.000 claims abstract description 9
- 239000002245 particle Substances 0.000 claims description 33
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 11
- 238000001125 extrusion Methods 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 238000005551 mechanical alloying Methods 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000001301 oxygen Substances 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 8
- 238000004886 process control Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000498 ball milling Methods 0.000 claims description 7
- 229910001175 oxide dispersion-strengthened alloy Inorganic materials 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 238000001513 hot isostatic pressing Methods 0.000 claims description 6
- 238000002490 spark plasma sintering Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims description 5
- 235000021355 Stearic acid Nutrition 0.000 claims description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000008117 stearic acid Substances 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 229910052769 Ytterbium Inorganic materials 0.000 abstract description 5
- 229910000881 Cu alloy Inorganic materials 0.000 abstract description 4
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 238000000137 annealing Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000009461 vacuum packaging Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011362 coarse particle Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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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- 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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- 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
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- 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
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
- B22F3/15—Hot isostatic pressing
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- 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
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
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- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
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- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- 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
- C22C1/059—Making alloys comprising less than 5% by weight of dispersed reinforcing phases
-
- 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
-
- 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
- C22C9/01—Alloys based on copper with aluminium as the next major constituent
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
- B22F2003/185—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers by hot rolling, below sintering temperature
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- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention discloses a completely coherent oxide dispersion strengthening copper-based composite material, which comprises the following components in percentage by atom: al 0.2% -6%, yb 2 O 3 0.1% -3%, and the balance of Cu and unavoidable impurities; the preparation method of the material comprises the following steps: 1. performing high-energy ball milling on copper powder, aluminum powder and ytterbium oxide powder to obtain alloy powder; 2. high-temperature hydrogen reduction is carried out on alloy powder; 3. sintering and forming to obtain a copper-based composite material blank; 4. and carrying out hot rolling or hot extrusion on the copper-based composite material blank. The invention adds Al and Yb into copper matrix 2 O 3 To spontaneously generate YbAlO fully coherent with copper 3 As a strengthening phase, the grain boundary and dislocation are effectively pinned, the grain growth is restrained, a higher strengthening effect is provided, the high-temperature tissue stability and the high-temperature strength of the copper-based composite material are improved, and the copper-based composite material is far higher than the traditional oxide dispersion strengthening copper alloy, and meanwhile has higher heat conductivity and electric conductivity.
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a completely coherent oxide dispersion strengthening copper-based composite material and a preparation method thereof.
Background
The high-strength high-conductivity high-heat-resistance copper-based composite material is used as one of key materials for modern high and new technologies, and is widely applied to various fields such as rail transit, electronic communication, navigation control and the like. The insufficient heat-resistant temperature is always the most main problem for limiting the application of the high-temperature copper-based composite material, and the phenomena of insufficient strength, creep failure, high-temperature softening and the like in a high-temperature environment are particularly shown. Oxide Dispersion Strengthened (ODS) copper alloys have been a popular research direction for high-strength, high-conductivity, heat-resistant copper-based composite materials because of their excellent high-temperature creep resistance and high-temperature softening resistance. The research shows that the commonality between the oxide particles and the copper matrix plays a critical role in the strengthening effect of the oxide particles, the better the commonality is, the smaller the lattice mismatch between the copper matrix and the oxide particles is, the less the oxide is easy to grow and aggregate, and therefore the higher the high-temperature strengthening effect is provided. The oxide strengthening particles commonly used at present comprise Al 2 O 3 、Y 2 O 3 And ZrO(s) 2 And the like, the particles and the copper matrix keep different or semi-same interfaces, so that the strengthening effect is limited. In order to further improve the high temperature resistance of the oxide dispersion strengthened copper alloy, oxide particles with higher interfacial commonality with a copper matrix are required to be used as a strengthening phase.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a completely coherent oxide dispersion strengthening copper-based composite material aiming at the defects of the prior art. The copper-based composite material is prepared by adding Al and Yb into a copper matrix 2 O 3 Obtaining high density YbAlO completely coherent with copper 3 As a strengthening phase, the grain boundary and dislocation are effectively pinned, the grain growth is restrained, a higher strengthening effect is provided, the high-temperature tissue stability and the high-temperature strength of the copper-based composite material are improved, and the difficult problem that the strengthening effect provided by the non-coherent or semi-coherent strengthening phase is limited is solved.
To solve the problem ofThe technical scheme adopted by the invention is as follows: the completely coherent oxide dispersion strengthening copper-based composite material is characterized by comprising the following components in percentage by atom: al 0.2% -6%, yb 2 O 3 0.1% -3%, and the balance of Cu and unavoidable impurities.
The copper-based composite material of the invention is prepared by adding Al and Yb into a copper matrix 2 O 3 Based on Gibbs free energy, al and Yb 2 O 3 YbAlO which is completely in line with copper can be spontaneously generated in copper matrix 3 The YbAlO 3 The crystal structure and the lattice parameter are similar to those of copper, and a phase interface which is free of lattice distortion and completely coherent with a copper matrix can be formed, so that the crystal structure has ultralow lattice mismatch, the nucleation barrier of oxide particles is reduced, and high-density nano particles are formed; meanwhile, the interface energy is lower in the completely coherent state, so YbAlO 3 The nano particles are extremely stable and are difficult to grow. Under the high-temperature environment, the high-density fully coherent oxide YbAlO 3 The existence of the particles can effectively pin grain boundaries and dislocation, inhibit grain growth and provide higher strengthening effect, so that the copper-based composite material has extremely excellent high-temperature tissue stability and high-temperature mechanical property, and the high-temperature tissue stability and high-temperature strength of the copper-based composite material are improved.
In addition, al element has a certain solid solubility in the copper matrix, and Yb element has almost no solid solubility in the copper matrix, so Yb is produced in the preparation of the composition of the present invention 2 O 3 The addition amount is slightly excessive, so that the Al element is ensured to be YbAlO 3 In the form of nanoparticles, excess Yb 2 O 3 The thermal conductivity of the copper-based composite material is not greatly influenced, so that the copper-based composite material has higher thermal conductivity and electrical conductivity.
The completely coherent oxide dispersion strengthening copper-based composite material is characterized by comprising the following components in percentage by atom: al 0.2% -1%, yb 2 O 3 0.1% -0.5%, and the balance of Cu and unavoidable impurities. The copper-based composite material composed of the components can maintain extremely high tissue stability and mechanical property below 300 DEG CCan be used.
The completely coherent oxide dispersion strengthening copper-based composite material is characterized by comprising the following components in percentage by atom: al is more than 1 percent and less than or equal to 3 percent, yb is more than 0.5 percent 2 O 3 Less than or equal to 1.5 percent, and the balance of Cu and unavoidable impurities. The copper-based composite material composed of the components can keep extremely high tissue stability and mechanical properties below 500 ℃.
The completely coherent oxide dispersion strengthening copper-based composite material is characterized by comprising the following components in percentage by atom: al is more than 3 percent and less than or equal to 6 percent, yb is more than 1.5 percent 2 O 3 Less than or equal to 3 percent, and the balance of Cu and unavoidable impurities. The copper-based composite material composed of the components can keep extremely high tissue stability and mechanical properties below 800 ℃.
In addition, the invention also discloses a method for preparing the completely coherent oxide dispersion strengthening copper-based composite material, which is characterized by comprising the following steps:
firstly, respectively weighing copper powder, aluminum powder and ytterbium oxide powder according to the atomic percentage composition of a target product copper-based composite material, and then performing high-energy ball milling under the protection of inert atmosphere to realize mechanical alloying to obtain alloy powder;
step two, carrying out high-temperature hydrogen reduction on the alloy powder obtained in the step one, and removing oxygen impurities in the alloy powder;
and thirdly, sintering and forming the alloy powder subjected to the high-temperature hydrogen reduction in the second step to obtain a copper-based composite material blank.
And step four, carrying out hot rolling or hot extrusion on the copper-based composite material blank obtained in the step three to obtain the complete coherent oxide dispersion strengthening copper-based composite material.
The method is characterized in that in the step one, the particle size of the copper powder is 1-150 mu m, the particle size of the aluminum powder is 48-75 mu m, and the particle size of the ytterbium oxide powder is 0.03-1 mu m. The invention is beneficial to obtaining alloy powder with uniform components by limiting the particle size of each raw material powder, and avoids the influence of the excessive coarse particle size of the raw material powder on the high-energy ball milling efficiency, and the increase of oxygen and water impurities caused by the excessive fine particle size of the raw material powder, thereby deteriorating the powder fluidity.
The method is characterized in that the rotating speed of the high-energy ball milling in the first step is 300 rpm-650 rpm, the ball-material ratio is 8:1-15:1, the ball milling time is 36-72 h, and the adopted process control agent is ethanol, n-heptane, acetone or stearic acid.
The method is characterized in that the high-temperature hydrogen reduction temperature in the third step is 400-800 ℃ and the high-temperature hydrogen reduction time is 1-5 h.
The method is characterized in that the sintering and forming method in the third step is hot-press sintering, spark plasma sintering or hot isostatic pressing sintering, wherein the temperature of the hot-press sintering is 750-950 ℃, the pressure is 25-45 MPa, the heat preservation time is 1-3 h, the temperature of the spark plasma sintering is 700-900 ℃, the pressure is 30-50 MPa, the heat preservation time is 5-20 min, the temperature of the hot isostatic pressing sintering is 700-850 ℃, the pressure is 100-200 MPa, and the heat preservation time is 1-3 h.
The method is characterized in that the hot rolling process in the fourth step is as follows: preheating a copper-based composite material blank for 5 minutes to 30 minutes at 700 ℃ to 850 ℃, and then carrying out hot rolling, wherein the pressing amount of each pass in the hot rolling process is 0.5mm to 2mm, and the total rolling deformation amount is 60% -70%; the hot extrusion temperature is 750-950 ℃, the extrusion speed is 220-380 mm/min, and the extrusion ratio is 5-12. The copper-based composite material obtained by the hot rolling process has almost no edge crack.
Compared with the prior art, the invention has the following advantages:
1. the invention adds Al and Yb into copper matrix 2 O 3 To spontaneously generate high density YbAlO fully coherent with copper 3 The ceramic second phase is used as a strengthening phase and is uniformly distributed in crystal grains, so that grain boundaries and dislocation are effectively pinned, the growth of the crystal grains is restrained, a higher strengthening effect is provided, the high-temperature tissue stability and the high-temperature strength of the copper-based composite material are improved, the occurrence of material fracture phenomena of ceramic particles due to stress relaxation at the interface at high temperature is avoided, and the excellent thermal stability of the copper-based composite material is realized.
2. The inventionComplete coherent oxide YbAlO generated in bright copper-based composite material 3 The thermal conductivity of the copper-based composite material is not greatly influenced, so that the copper-based composite material is ensured to have higher thermal conductivity and electrical conductivity, and the copper-based composite material has wide application prospect.
3. The copper-based composite material prepared by the method has extremely excellent high-temperature mechanical properties, the tensile strength at 300 ℃ can reach more than 580MPa, the tensile strength at 450 ℃ can reach more than 440MPa, and the tensile strength at 700 ℃ can reach more than 400MPa, which is far higher than that of the traditional oxide dispersion strengthening copper alloy.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a graph showing the hardness change in the sintered state, the rolled state, the 800 ℃ annealed state and the 900 ℃ annealed state of the copper-based composite materials prepared in example 1 and comparative example 1 according to the present invention.
Fig. 2 is a transmission electron microscope image of the copper-based composite material prepared in example 2 of the present invention.
Detailed Description
Example 1
The copper-based composite material of the embodiment comprises the following components in percentage by atom: al 1.2%, yb 2 O 3 0.6%, the balance being Cu and unavoidable impurities.
The preparation method of the copper-based composite material comprises the following steps:
firstly, respectively weighing copper powder with the particle size of 75 mu m, aluminum powder with the particle size of 48 mu m and ytterbium oxide powder with the particle size of 0.03 mu m according to the atomic percentage composition of a target product copper-based composite material, and then performing high-energy ball milling under the protection of inert atmosphere argon to realize mechanical alloying to obtain alloy powder; the rotating speed of the high-energy ball milling is 600rpm, the ball-material ratio is 8:1, the ball milling time is 60 hours, and absolute ethyl alcohol accounting for 2 percent of the total mass of each raw material powder is added as a process control agent in the high-energy ball milling process;
step two, placing the alloy powder obtained in the step one in a tube furnace for high-temperature hydrogen reduction, and removing oxygen impurities in the alloy powder; the high-temperature hydrogen reduction temperature is 600 ℃ and the high-temperature hydrogen reduction time is 3 hours;
step three, cooling the alloy powder subjected to high-temperature hydrogen reduction in the step two, and then rapidly vacuum packaging to perform spark plasma sintering to obtain a copper-based composite material blank; the temperature of the spark plasma sintering is 900 ℃, the pressure is 45MPa, and the heat preservation time is 8min;
and fourthly, preheating the copper-based composite blank obtained in the third step for 30min at 700 ℃, then carrying out hot rolling, wherein the pressing amount of each pass in the hot rolling process is 0.5mm, the total rolling deformation amount is 70%, and then carrying out stress relief annealing for 3h at 600 ℃ to obtain the complete coherent oxide dispersion strengthening copper-based composite.
The process control agent added in the high energy ball milling in step one of this example may also be replaced with n-heptane, acetone or stearic acid.
Comparative example 1
The copper-based composite material of the comparative example consists of the following components in atomic percent: yb 2 O 3 0.6%, the balance being Cu and unavoidable impurities.
The preparation method of the copper-based composite material of the comparative example is different from that of example 1 in that: in the first step, copper powder with the particle size of 75 mu m and ytterbium oxide powder with the particle size of 0.03 mu m are subjected to high-energy ball milling under the protection of inert atmosphere argon to realize mechanical alloying, so as to obtain alloy powder.
FIG. 1 is a graph showing the hardness change in the sintered state, rolled state, 800 ℃ annealed state and 900 ℃ annealed state of the copper-based composite material prepared in example 1 and comparative example 1 according to the present invention, as can be seen from FIG. 1, yb is selected due to comparative example 1 2 O 3 Yb as a strengthening phase of copper-based composite materials based on differences in crystal structure and lattice constant 2 O 3 Not completely coherent with the copper matrix, so the completely coherent oxide dispersion strengthened copper matrix composite Cu-Al-Yb in example 1 2 O 3 The Vickers hardness number of the alloy is far higher than that of the Cu-Yb of the non-fully coherent oxide dispersion reinforced copper-based composite material in the comparative example 1 2 O 3 While the stability of the copper-based composite in example 1 is much higher than that of the copper-based composite in comparative example 1, sayThe adoption of the completely coherent oxide in the invention leads the copper-based composite material to have excellent high-temperature strength performance.
Example 2
The copper-based composite material of the embodiment comprises the following components in percentage by atom: al 3%, yb 2 O 3 1.5%, the balance Cu and unavoidable impurities.
The preparation method of the copper-based composite material comprises the following steps:
firstly, respectively weighing copper powder with the particle size of 150 mu m, aluminum powder with the particle size of 75 mu m and ytterbium oxide powder with the particle size of 0.03 mu m according to the atomic percentage composition of a target product copper-based composite material, and then performing high-energy ball milling under the protection of inert atmosphere argon to realize mechanical alloying to obtain alloy powder; the rotating speed of the high-energy ball milling is 650rpm, the ball-material ratio is 10:1, the ball milling time is 36h, and n-heptane accounting for 2 percent of the total mass of each raw material powder is added as a process control agent in the high-energy ball milling process;
step two, placing the alloy powder obtained in the step one in a tube furnace for high-temperature hydrogen reduction, and removing oxygen impurities in the alloy powder; the high-temperature hydrogen reduction temperature is 400 ℃ and the high-temperature hydrogen reduction time is 5 hours;
step three, cooling the alloy powder subjected to high-temperature hydrogen reduction in the step two, and then rapidly vacuum packaging to perform hot-press sintering to obtain a copper-based composite material blank; the hot-pressed sintering temperature is 900 ℃, the pressure is 30MPa, and the heat preservation time is 2 hours;
and fourthly, preheating the copper-based composite blank obtained in the third step for 5min at 850 ℃, then carrying out hot rolling, wherein the pressing amount of each pass in the hot rolling process is 2mm, the total rolling deformation is 60%, and then carrying out stress relief annealing for 3h at 600 ℃ to obtain the completely coherent oxide dispersion strengthening copper-based composite.
Fig. 2 is a transmission electron microscopic image of the copper-based composite material prepared in this example, and it can be seen from fig. 2 that there is a high density of fully coherent nano-oxide in the copper matrix.
According to detection, the room-temperature tensile strength of the copper-based composite material prepared by the embodiment is 593MPa, the 300 ℃ tensile strength is 585MPa, the 450 ℃ tensile strength is 449MPa, the 750 ℃ tensile strength is 400MPa, and the annealing mechanical property is not reduced at the temperature below 900 ℃.
Example 3
The copper-based composite material of the embodiment comprises the following components in percentage by atom: al 6%, yb 2 O 3 3%, the balance being Cu and unavoidable impurities.
The preparation method of the copper-based composite material comprises the following steps:
firstly, respectively weighing copper powder with the particle size of 3 mu m, aluminum powder with the particle size of 75 mu m and ytterbium oxide powder with the particle size of 0.1 mu m according to the atomic percentage composition of a target product copper-based composite material, and then performing high-energy ball milling under the protection of inert atmosphere argon to realize mechanical alloying to obtain alloy powder; the rotational speed of the high-energy ball milling is 500rpm, the ball-material ratio is 12:1, the ball milling time is 60 hours, and n-heptane accounting for 2 percent of the total mass of each raw material powder is added as a process control agent in the high-energy ball milling process;
step two, placing the alloy powder obtained in the step one in a tube furnace for high-temperature hydrogen reduction, and removing oxygen impurities in the alloy powder; the high-temperature hydrogen reduction temperature is 500 ℃ and the time is 2 hours;
step three, cooling the alloy powder subjected to high-temperature hydrogen reduction in the step two, and then rapidly vacuum packaging to perform hot-press sintering to obtain a copper-based composite material blank; the hot-pressed sintering temperature is 850 ℃, the pressure is 40MPa, and the heat preservation time is 2 hours;
and fourthly, preheating the copper-based composite blank obtained in the third step for 5min at 800 ℃, then carrying out hot rolling, wherein the pressing amount of each pass in the hot rolling process is 1mm, the total rolling deformation amount is 70%, and then carrying out stress relief annealing for 3h at 700 ℃ to obtain the completely coherent oxide dispersion strengthening copper-based composite.
According to detection, the room-temperature tensile strength of the copper-based composite material prepared by the embodiment is greater than 850MPa, the 300 ℃ tensile strength is greater than 700MPa, the 450 ℃ tensile strength is greater than 600MPa, the 750 ℃ tensile strength is greater than 450MPa, and the annealing mechanical property is not reduced at the temperature below 1000 ℃.
Example 4
The copper-based composite material of the embodiment comprises the following components in percentage by atom: al 0.2%, yb 2 O 3 0.1%, the balance being Cu and unavoidable impurities.
The preparation method of the copper-based composite material comprises the following steps:
firstly, respectively weighing copper powder with the particle size of 1 mu m, aluminum powder with the particle size of 48 mu m and ytterbium oxide powder with the particle size of 1 mu m according to the atomic percentage composition of a target product copper-based composite material, and then performing high-energy ball milling under the protection of inert atmosphere argon to realize mechanical alloying to obtain alloy powder; the rotational speed of the high-energy ball milling is 300rpm, the ball-material ratio is 15:1, the ball milling time is 72 hours, and n-heptane accounting for 2 percent of the total mass of each raw material powder is added as a process control agent in the high-energy ball milling process;
step two, placing the alloy powder obtained in the step one in a tube furnace for high-temperature hydrogen reduction, and removing oxygen impurities in the alloy powder; the high-temperature hydrogen reduction temperature is 800 ℃ and the time is 1h;
step three, cooling the alloy powder subjected to high-temperature hydrogen reduction in the step two, and then rapidly vacuum packaging to perform hot-press sintering to obtain a copper-based composite material blank; the hot-pressed sintering temperature is 850 ℃, the pressure is 40MPa, and the heat preservation time is 2 hours;
and fourthly, performing hot extrusion on the copper-based composite material blank obtained in the third step, wherein the extrusion temperature is 750 ℃, the extrusion speed is 220mm/min, the extrusion ratio is 5, and performing stress relief annealing on the bar obtained by hot extrusion at 700 ℃ for 3 hours to obtain the completely coherent oxide dispersion strengthening copper-based composite material.
According to detection, the room-temperature tensile strength of the copper-based composite material prepared by the embodiment is greater than 400MPa, the 300 ℃ tensile strength is greater than 300MPa, the 450 ℃ tensile strength is greater than 200MPa, the 750 ℃ tensile strength is greater than 150MPa, and the annealing mechanical property is not reduced at the temperature below 700 ℃.
Example 5
The copper-based composite material of the embodiment comprises the following components in percentage by atom: al 5%, yb 2 O 3 2.5%, the balance Cu and unavoidable impurities.
The preparation method of the copper-based composite material comprises the following steps:
firstly, respectively weighing copper powder with the particle size of 150 mu m, aluminum powder with the particle size of 75 mu m and ytterbium oxide powder with the particle size of 0.03 mu m according to the atomic percentage composition of a target product copper-based composite material, and then performing high-energy ball milling under the protection of inert atmosphere argon to realize mechanical alloying to obtain alloy powder; the rotational speed of the high-energy ball milling is 600rpm, the ball-material ratio is 10:1, the ball milling time is 48 hours, and n-heptane accounting for 2 percent of the total mass of each raw material powder is added as a process control agent in the high-energy ball milling process;
step two, placing the alloy powder obtained in the step one in a tube furnace for high-temperature hydrogen reduction, and removing oxygen impurities in the alloy powder; the high-temperature hydrogen reduction temperature is 600 ℃ and the high-temperature hydrogen reduction time is 3 hours;
step three, cooling the alloy powder subjected to high-temperature hydrogen reduction in the step two, and then rapidly vacuum packaging to perform hot isostatic pressing sintering to obtain a copper-based composite material blank; the temperature of the hot isostatic pressing sintering is 800 ℃, the pressure is 150MPa, and the heat preservation time is 2 hours;
and fourthly, performing hot extrusion on the copper-based composite material blank obtained in the third step, wherein the extrusion temperature is 950 ℃, the extrusion speed is 380mm/min, the extrusion ratio is 12, and performing stress relief annealing on the bar obtained by hot extrusion at 700 ℃ for 3 hours to obtain the completely coherent oxide dispersion strengthening copper-based composite material.
According to detection, the room-temperature tensile strength of the copper-based composite material prepared by the embodiment is more than 800MPa, the 300 ℃ tensile strength is more than 700MPa, the 450 ℃ tensile strength is more than 600MPa, the 750 ℃ tensile strength is more than 400MPa, and the annealing mechanical property is not reduced at the temperature below 1000 ℃.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (4)
1. The completely coherent oxide dispersion strengthening copper-based composite material is characterized by comprising the following components in percentage by atom: al 0.2% -6%, yb 2 O 3 0.1% -3%, and the balance of Cu and unavoidable impurities; the fully coherent oxide dispersion strengthening copper-based composite material is prepared by a method comprising the following steps:
firstly, respectively weighing copper powder, aluminum powder and ytterbium oxide powder according to the atomic percentage composition of a target product copper-based composite material, and then performing high-energy ball milling under the protection of inert atmosphere to realize mechanical alloying to obtain alloy powder; the particle size of the copper powder is 1-150 mu m, the particle size of the aluminum powder is 48-75 mu m, and the particle size of the ytterbium oxide powder is 0.03-1 mu m; the rotating speed of the high-energy ball milling is 300 rpm-650 rpm, the ball-material ratio is 8:1-15:1, the ball milling time is 36-72 h, and the adopted process control agent is ethanol, n-heptane, acetone or stearic acid;
step two, carrying out high-temperature hydrogen reduction on the alloy powder obtained in the step one, and removing oxygen impurities in the alloy powder; the high-temperature hydrogen reduction temperature is 400-800 ℃ and the high-temperature hydrogen reduction time is 1-5 h;
step three, sintering and forming the alloy powder subjected to high-temperature hydrogen reduction in the step two to obtain a copper-based composite material blank; the sintering molding method comprises hot press sintering, spark plasma sintering or hot isostatic pressing sintering, wherein the hot press sintering temperature is 750-950 ℃, the pressure is 25-45 MPa, the heat preservation time is 1-3 h, the spark plasma sintering temperature is 700-900 ℃, the pressure is 30-50 MPa, the heat preservation time is 5-20 min, the hot isostatic pressing sintering temperature is 700-850 ℃, the pressure is 100-200 MPa, and the heat preservation time is 1-3 h;
step four, hot rolling or hot extrusion is carried out on the copper-based composite material blank obtained in the step three, so as to obtain a completely coherent oxide dispersion strengthening copper-based composite material; the hot rolling process comprises the following steps: preheating a copper-based composite material blank for 5 minutes to 30 minutes at 700 ℃ to 850 ℃, and then carrying out hot rolling, wherein the pressing amount of each pass in the hot rolling process is 0.5mm to 2mm, and the total rolling deformation amount is 60% -70%; the hot extrusion temperature is 750-950 ℃, the extrusion speed is 220-380 mm/min, and the extrusion ratio is 5-12.
2. The fully coherent oxide dispersion strengthened copper matrix composite of claim 1, comprising the following components in atomic percent: al 0.2% -1%, yb 2 O 3 0.1% -0.5%, and the balance of Cu and unavoidable impurities.
3. The fully coherent oxide dispersion strengthened copper matrix composite of claim 1, comprising the following components in atomic percent: al is more than 1 percent and less than or equal to 3 percent, yb is more than 0.5 percent 2 O 3 Less than or equal to 1.5 percent, and the balance of Cu and unavoidable impurities.
4. The fully coherent oxide dispersion strengthened copper matrix composite of claim 1, comprising the following components in atomic percent: al is more than 3 percent and less than or equal to 6 percent, yb is more than 1.5 percent 2 O 3 Less than or equal to 3 percent, and the balance of Cu and unavoidable impurities.
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