CN114850471B - Discontinuous layered bimetal composite material and preparation method thereof - Google Patents
Discontinuous layered bimetal composite material and preparation method thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 36
- 238000000498 ball milling Methods 0.000 claims abstract description 24
- 238000007747 plating Methods 0.000 claims abstract description 23
- 238000005245 sintering Methods 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims abstract description 20
- 239000002184 metal Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000009826 distribution Methods 0.000 claims abstract description 12
- 238000004891 communication Methods 0.000 claims abstract description 5
- 238000003475 lamination Methods 0.000 claims abstract description 5
- 230000010355 oscillation Effects 0.000 claims abstract 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 36
- 229910052721 tungsten Inorganic materials 0.000 claims description 24
- 239000010937 tungsten Substances 0.000 claims description 24
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 20
- 229910052802 copper Inorganic materials 0.000 claims description 20
- 239000010949 copper Substances 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000011068 loading method Methods 0.000 claims description 5
- 150000002739 metals Chemical class 0.000 claims description 5
- 238000002490 spark plasma sintering Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 3
- 238000007731 hot pressing Methods 0.000 claims description 3
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 230000008018 melting Effects 0.000 claims description 2
- 238000001338 self-assembly Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 abstract description 38
- 239000007791 liquid phase Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract 1
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 description 24
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- 238000001000 micrograph Methods 0.000 description 7
- 239000000835 fiber Substances 0.000 description 4
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 3
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007772 electroless plating Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 238000004663 powder metallurgy Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- XTYUEDCPRIMJNG-UHFFFAOYSA-N copper zirconium Chemical compound [Cu].[Zr] XTYUEDCPRIMJNG-UHFFFAOYSA-N 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- IXQWNVPHFNLUGD-UHFFFAOYSA-N iron titanium Chemical compound [Ti].[Fe] IXQWNVPHFNLUGD-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- FSVVWABMXMMPEE-UHFFFAOYSA-N molybdenum silver Chemical compound [Mo][Ag][Mo] FSVVWABMXMMPEE-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 239000010955 niobium Substances 0.000 description 1
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000009417 prefabrication Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
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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
- B22F1/17—Metallic particles coated with metal
-
- 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
- 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
-
- 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
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Powder Metallurgy (AREA)
Abstract
A discontinuous layered bimetal composite material and a preparation method thereof belong to the field of metal materials. Preparing flaky powder A with larger length-diameter ratio by taking metal powder A as a raw material through a liquid phase ball milling method; then plating B metal on the surface of the flaky powder A by adopting a chemical plating method to prepare composite powder coated with the B; and finally, placing the obtained flaky composite powder into a mould for oscillation, and then performing vacuum pressure sintering. In the composite material, the phase A is directionally and uniformly distributed in the phase B in a lamellar structure with nano/micron thickness, the phase A and the phase B are in lamination distribution characteristics, and the phase B is in three-dimensional communication distribution. The bimetal composite material of the structure has obvious anisotropism, has the advantage of good strength and toughness of the layered structure, and has higher electric conductivity and thermal conductivity in all directions, and the conductivity of the bimetal composite material in the direction along the A sheet layer is far more than that of other bimetal composite materials with the same components.
Description
Technical Field
The invention belongs to the field of powder metallurgy technology and refractory metal materials, and particularly relates to a discontinuous layered bimetallic composite material and a preparation method thereof.
Background
The bimetal composite material (A is generally refractory metals such as niobium, molybdenum, tantalum, tungsten, titanium, zirconium and the like, and B is generally metals with better conductivity such as copper, silver, iron, nickel and the like, such as tungsten copper, molybdenum silver, zirconium copper, iron titanium and the like) composed of two metals or alloys thereof has the advantages of high electric conduction and high heat conduction of B, high hardness of A, arc erosion resistance, low thermal expansion and the like, and is widely used in the fields of various electric contact materials, electrode materials, heat sink materials, packaging materials, military equipment and the like. These fields generally require composite materials that have both high mechanical and conductive properties. However, the mechanical properties of the current commercial coarse-grain composite materials are lower; although the mechanical properties of the ultra-fine grain or nano-crystal composite material are improved, the conductivity of the ultra-fine grain or nano-crystal composite material is reduced to different degrees. Therefore, new design ideas and preparation methods are needed to improve the comprehensive performance of the bimetal composite material, thereby meeting the requirements of the continuously developed high and new technical fields.
At present, the main preparation method and the structural performance of the bimetal composite material are as follows. The bimetallic composite material prepared by presintering to prepare the A framework and then infiltrating the B metal has higher conductivity but lower mechanical property, wherein the grain sizes of the A phase and the B phase are relatively coarse, and the two phases are mutually interpenetrated and uniformly distributed. The bimetal composite powder is obtained by adopting a chemical method or a mechanical alloying (mechanical ball milling) method, and then the mechanical property of the bimetal composite material prepared by sintering is improved compared with that of a coarse-grain tungsten-copper composite material, but the conductivity is reduced to some extent, wherein the AB two-phase crystal grain size is unequal from nanometer to micrometer and is also in a uniform distribution state. The bimetal composite powder coated with the B and coated with the A is prepared by adopting an electroless plating or electroplating process, and then the bimetal composite material prepared by sintering has higher conductivity and mechanical property influenced by the particle size of the A phase, wherein the B phase is distributed in a three-dimensional network shape, and the A phase is uniformly distributed in a particle shape and is generally coarse. Andr e from the Switzerland nanometallurgy laboratoryTungsten (a phase) frameworks were prepared using an ice template-based method, and then copper-infiltrated (B phase) tungsten-copper composites were shown to be anisotropic, in which the copper phase had continuous channels in one direction, but the tungsten phase was coarser in size, resulting in improved conductivity in a specific direction, but mechanical properties were not high. Duan et al, shanghai engineering university, prepared a tungsten skeleton by sintering a tungsten (A phase) fiber compact, followed by a tungsten copper composite prepared by copper infiltration (B phase), wherein the tungsten phase is continuously distributed in a fibrous form, and the tungsten fiber size is generally in the range of tens to hundreds of micrometers, and the mechanical properties of the composite are not high because the size of the tungsten fiber is difficult to refine. Zhang et al in Chinese national academy of sciences in order to perform a prefabrication of a blank by arranging tungsten meshes (phase A) in a laminated manner and cold pressing, and then copper infiltration (phase B) to prepare a tungsten-copper composite material also shows a certain anisotropy, but has a high copper content, resulting in general mechanical properties, wherein the tungsten phase is in a network-like layered distribution. There are also methods for preparing continuous layered composite materials by laminating and hot-pressing A foil and B foil at home and abroad, and also continuous layered composite materials of AB can be prepared by a method of accumulated and laminated rolling, the materials also show obvious anisotropism, but the thickness of the A phase layer is generally in the order of hundreds of micrometers, and the thickness is difficult to further thin due to the limitation of the preparation process. In addition, the magnetron sputtering method can be used for preparing the AB layered composite material with the nano level, which shows excellent mechanical properties, but the method is difficult to realize industrialized preparation.
Aiming at the problems and structural characteristics, a novel structure-discontinuous layered heterostructure which is obviously different from the existing uniform structure, A fiber reinforced structure, continuous layered structure and the like is provided on the basis of comprehensively considering the performance of the bimetal composite material and the large-scale preparation. In the AB composite material with the structure, the A phase is directionally and uniformly distributed in the B phase in a lamellar structure with nano/micron thickness, the A phase and the B phase are in lamination distribution characteristics, and the B phase is in three-dimensional communication distribution. The AB composite material of the structure has obvious anisotropy, has the advantage of good strength and toughness of the layered structure, and has higher electric conductivity and thermal conductivity in all directions, and the conductivity in the direction along the A sheet layer is far superior to that of other composite materials with the same component reported at present. At present, no research report on discontinuous layered heterostructure bimetallic composite materials and preparation methods thereof exists at home and abroad. Based on the background, the invention provides a bimetal composite material with a discontinuous layered heterostructure, and provides a novel method for preparing the bimetal composite material with the discontinuous layered heterostructure by using a powder metallurgy process, so that macro preparation of the anisotropic bimetal composite material with adjustable and controllable structural components, macroscopically uniform structure, excellent strength and toughness matching property and electric conductivity and thermal conductivity is realized.
Disclosure of Invention
The invention provides a bimetal composite material with a discontinuous layered heterostructure and a preparation method thereof, aiming at the problem of high-efficiency preparation of the bimetal composite material, compared with the existing bimetal composite material, the discontinuous layered heterostructure bimetal composite material has obvious difference in structure, A phase is directionally and uniformly distributed in B phase in a lamellar structure with nano/micron thickness, the A phase and the B phase are in lamination distribution characteristics, and the B phase is in three-dimensional communication distribution. The material has more excellent strength and toughness matching property, electric conductivity and thermal conductivity, and the conductivity of the material in the direction along the A sheet layer is far superior to that of the composite material with the same component and other configurations reported at present.
The technical scheme adopted in the invention is as follows: taking the metal powder A as a raw material, and preparing sheet-shaped metal powder A by a liquid phase ball milling method; plating a certain amount of B metal on the surface of the flaky A metal powder by adopting an electroless plating method; finally, carrying out vacuum pressure sintering on the obtained flaky AB composite powder to obtain the discontinuous layered heterostructure AB bimetallic composite material. Wherein, the mass percentage of B metal in the composite material can be controlled in a large range of 5 to 60 percent, and the balance is A.
The invention provides a discontinuous layered heterostructure bimetallic composite material with controllable components and high strength and high conductivity and a preparation method thereof. The method is characterized by comprising the following steps:
(1) Loading A metal powder (A is tungsten) with the particle size of 1-50 microns into a ball milling tank, adding grinding balls, adding ethanol as a ball milling medium for ball milling, filtering out ethanol, and drying to obtain sheet-shaped A powder with different sheet sizes and thicknesses; in the process, the ball-material ratio is 10:1-30:1, the ball milling rotating speed is 300-600rpm, and the ball milling time is 1-8 days;
(2) Placing the flaky powder A obtained in the step (1) into a plating solution B (B is copper) for plating to obtain flaky bimetal composite powder with a B-package structure A;
(3) Filling the flaky bimetal composite powder obtained in the step (2) into a graphite mold, compacting, and then carrying out spark plasma sintering or hot-pressing sintering under vacuum to obtain a bimetal composite material block with a discontinuous layered heterostructure; the vacuum degree is more than 1X 10 -1 Pa, the sintering temperature is (T m -100) DEG C to T m℃,Tm which is the lower value of the melting points of the two metals, the sintering pressure is 50-150MPa, and the sintering time is 10-120min.
In the step (1), the adjustment and control of the sheet diameter and thickness of the tungsten sheet can be realized according to the particle diameter and ball milling rotating speed of the initial metal powder A and the ball milling time. The plating solution in the step (2) is any plating solution capable of plating B metal on the surface of the metal A, and the content of B can be regulated according to the proportion of the plating solution to the powder A. In the step (3), the construction of the layered structure is realized by the self-assembly stacking effect of the flake powder with large length-diameter ratio under the assistance of vibration.
The method can theoretically regulate and control the contents of two metals in a large range to prepare the discontinuous layered heterogeneous structure bimetallic composite materials with different components and different sizes of the metal sheets A.
The invention has the following characteristics and advantages:
The A phase and the B phase in the AB bimetallic composite material have the characteristic of lamination distribution, the structure can inhibit the growth of the crystal grains of the AB two phases to a certain extent so as to refine the crystal grains, and simultaneously can improve the bearing capacity of the A phase and inhibit crack growth, so that the composite material has excellent strength and toughness matching performance and damage tolerance resistance; meanwhile, the metal sheets A in the composite material are highly oriented, so that the obstruction of movement of electronic phonons and the like in the direction parallel to the sheets A is effectively reduced, and the electric conductivity and the heat conductivity of the material in the direction are greatly improved; the B phase in the composite material is completely distributed in a three-dimensional communication shape, so that the composite material has higher conductivity in the direction vertical to the A sheet, and a three-dimensional network structure can be formed even if the content of B is relatively small; compared with other AB composite materials with the same components, the discontinuous layered heterostructure AB bimetallic composite material prepared by the invention has more excellent toughness and conductivity; the preparation method provided by the invention can realize the regulation and control of the structure and the components of the discontinuous layered heterostructure bimetallic composite material in a large range, thereby regulating and controlling each performance of the bimetallic composite material so as to meet the requirements of different application fields.
Drawings
Fig. 1: the macroscopic morphology (scanning electron microscope image) of the flaky tungsten powder prepared in the step (1) in the example 1;
fig. 2: the side morphology (scanning electron microscope image) of the flaky tungsten powder prepared in the step (1) in the example 1;
fig. 3: the morphology and elemental plane distribution characterization (scanning electron microscope image and energy spectrum analysis) of the flaky tungsten-copper composite powder with the copper-clad structure prepared in the step (2) in the embodiment 1;
Fig. 4: characterization of the cross-sectional structure (scanning electron microscope image) of the discontinuous layered heterostructure tungsten copper composite material prepared in step (3) of example 1;
Fig. 5: the cross-sectional structure and the element plane distribution of the discontinuous layered heterostructure tungsten-copper composite material prepared in the step (3) in the embodiment 1 are characterized (scanning electron microscope image and energy spectrum analysis);
fig. 6: a compressive stress strain curve of the discontinuous layered heterostructure tungsten copper composite material prepared in the step (3) in the embodiment 1 in the direction perpendicular to the tungsten plate;
Fig. 7: a compressive stress strain curve of the discontinuous layered heterostructure tungsten copper composite material prepared in step (3) in example 1 in a direction parallel to the tungsten plate;
Fig. 8: the morphology (scanning electron microscope image) of the flaky tungsten copper composite powder with the copper-clad structure prepared in the step (2) in the embodiment 2;
fig. 9: characterization of the cross-sectional structure (scanning electron microscope image) of the discontinuous layered heterostructure tungsten-copper composite material prepared in step (3) of example 2;
Detailed Description
The following description is provided in connection with two specific embodiments to provide an exemplary illustration and to aid in the further understanding of the present invention. However, the specific details of the embodiments are only for illustrating the present invention, and do not represent all technical solutions under the concept of the present invention, and therefore should not be construed as limiting the technical solutions of the present invention. Insubstantial changes, e.g., simple changes or substitutions of technical features with the same or similar technical effects, without departing from the spirit of the invention are intended to be covered by the claims.
Example 1
(1) Putting 20g of tungsten powder with the average particle size of 15 microns into a ball milling tank, adding 400g of grinding balls, adding ethanol as a ball milling medium, ball milling for 4 days at a rotating speed of 500rpm, and then filtering and drying to obtain flaky tungsten powder with the thickness of about 500 nm;
(2) Placing 6.35g of the flaky tungsten powder obtained in the step (1) into 400ml of copper plating solution (the plating solution contains 6.44g of CuSO 4, 24g of EDTA-2Na, 0.06g of bipyridine and 40ml of formaldehyde), plating for 30 minutes at 60 ℃ under the condition of water bath stirring, and filtering and cleaning the plating solution to obtain flaky tungsten-copper composite powder with a copper coating structure, wherein the copper content of the flaky tungsten-copper composite powder is 30 wt%;
(3) Loading the flaky tungsten-copper composite powder obtained in the step (2) into a graphite mold, and then carrying out spark plasma sintering under vacuum to obtain a W-30Cu composite material block with a discontinuous layered heterostructure; the vacuum degree is about 1X 10 -2 Pa, the sintering temperature is 1000 ℃, the sintering pressure is 100MPa, and the sintering time is 10min.
The prepared W-30Cu composite material has the conductivity of about 56 percent IACS in the direction parallel to the tungsten sheet, about 46.5 percent IACS in the direction perpendicular to the tungsten sheet, and far exceeds 38 percent IACS (GB_T8320-2017) specified in the national standard and other tungsten copper composite materials with the same components. Meanwhile, the compressive strength of the tungsten plate in the direction perpendicular to the tungsten plate can reach 1150MPa, and the compression amount can reach 17%; the compressive yield strength of the alloy is also up to 900MPa in the direction parallel to the tungsten sheet, and the alloy has higher damage tolerance.
Example 2
(1) Putting 20g of tungsten powder with the average particle size of 15 microns into a ball milling tank, adding 400g of grinding balls, adding ethanol as a ball milling medium, ball milling for 4 days at a rotating speed of 500rpm, and then filtering and drying to obtain flaky tungsten powder with the thickness of about 500 nm;
(2) 3.5g of the flaky tungsten powder obtained in the step (1) is placed in 400ml of copper plating solution (the plating solution contains 6.44g of CuSO 4, 24g of EDTA-2Na, 0.06g of bipyridine and 40ml of formaldehyde), plating is carried out for 30 minutes at 80 ℃ under the condition of water bath stirring, and the plating solution is filtered and washed to obtain flaky tungsten-copper composite powder with a copper-coated structure, wherein the copper content of the flaky tungsten-copper composite powder is 40 wt%;
(3) Loading the flaky tungsten-copper composite powder obtained in the step (2) into a graphite mold, and then carrying out spark plasma sintering under vacuum to obtain a W-40Cu composite material block with a discontinuous layered heterostructure; the vacuum degree is about 1X 10 -2 Pa, the sintering temperature is 970 ℃, the sintering pressure is 100MPa, and the sintering time is 10min.
The hardness of the prepared W-40Cu composite material is about 240HV, the conductivity in the direction parallel to the tungsten sheet is about 64.3% IACS, and the hardness far exceeds 47% IACS (GB_T8320-2017) specified in the national standard and other tungsten copper composite materials with the same components.
Example 3
(1) Putting 20g of tungsten powder with the average particle size of 15 microns into a ball milling tank, adding 400g of grinding balls, adding ethanol as a ball milling medium, ball milling for 4 days at a rotating speed of 500rpm, and then filtering and drying to obtain flaky tungsten powder with the thickness of about 500 nm;
(2) Placing 21.2g of the flaky tungsten powder obtained in the step (1) into 400ml of copper plating solution (the plating solution contains 6.44g of CuSO 4, 24g of EDTA-2Na, 0.06g of bipyridine and 40ml of formaldehyde), plating for 30 minutes at 60 ℃ under the condition of water bath stirring, and filtering and cleaning the plating solution to obtain flaky tungsten-copper composite powder with a copper coating structure, wherein the copper content of the flaky tungsten-copper composite powder is 8.5 wt%;
(3) Loading the flaky tungsten-copper composite powder obtained in the step (2) into a graphite mold, and then carrying out spark plasma sintering under vacuum to obtain a W-8.5Cu composite material block with a discontinuous layered heterostructure; the vacuum degree is about 1X 10 -2 Pa, the sintering temperature is 970 ℃, the sintering pressure is 120MPa, and the sintering time is 10min.
The hardness of the prepared W-8.5Cu composite material is up to 496HV, the conductivity in the direction parallel to the tungsten plate is about 36.5% IACS, and the hardness far exceeds 27% IACS (GB_T8320-2017) of W-10Cu and other tungsten copper composite materials with the same components specified in the national standard.
Claims (2)
1. The preparation method of the discontinuous layered bimetal composite material is characterized by comprising the following steps of:
(1) Loading A metal powder with the particle size of 15-50 microns into a ball milling tank, adding grinding balls, adding ethanol as a ball milling medium for ball milling, filtering out ethanol, and drying to obtain sheet A powder with different sheet diameters and thicknesses;
(2) Placing the flaky powder A obtained in the step (1) into a plating solution B, and plating under a certain condition to obtain flaky bimetal composite powder with a B-package structure A;
(3) Filling the flaky bimetal composite powder obtained in the step (2) into a graphite mold, vibrating, and then performing spark plasma sintering or hot-pressing sintering under vacuum to obtain a bimetal composite material block with a discontinuous layered heterostructure; the vacuum degree is more than 1X 10 -1 Pa, the sintering temperature is (T m -100) DEG C to T m℃,Tm which is the lower value of the melting points of the two metals, the sintering pressure is 50-150MPa, and the sintering time is 10-120min;
A is tungsten, B is copper;
In the process of the step (1), the ball-material ratio is 10:1-30:1, the ball milling rotating speed is 300-600rpm, and the ball milling time is 1-8 days;
The step (3) realizes the construction of a layered structure through the self-assembly stacking effect and pressure sintering of the flaky powder with large length-diameter ratio under the assistance of oscillation;
The mass percentage of copper in the composite material obtained by the preparation is 5 to 60 percent, and the balance is tungsten; tungsten in the prepared discontinuous layered bimetal composite material is directionally and uniformly distributed in a copper phase in a lamellar structure with nano/micron thickness, the tungsten and the copper phase are in lamination distribution characteristics, and the copper phase is in three-dimensional communication distribution.
2. A discontinuous layered bimetallic composite prepared according to the method of claim 1.
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