CN113084166A - Method for preparing tungsten-copper gradient composite material - Google Patents
Method for preparing tungsten-copper gradient composite material Download PDFInfo
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- CN113084166A CN113084166A CN202110342215.1A CN202110342215A CN113084166A CN 113084166 A CN113084166 A CN 113084166A CN 202110342215 A CN202110342215 A CN 202110342215A CN 113084166 A CN113084166 A CN 113084166A
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- 239000002131 composite material Substances 0.000 title claims abstract description 64
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 54
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 144
- 238000005096 rolling process Methods 0.000 claims abstract description 76
- 239000010949 copper Substances 0.000 claims abstract description 69
- 229910052802 copper Inorganic materials 0.000 claims abstract description 68
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 62
- 238000000137 annealing Methods 0.000 claims abstract description 30
- 238000002844 melting Methods 0.000 claims abstract description 28
- 230000008018 melting Effects 0.000 claims abstract description 28
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 21
- 239000010937 tungsten Substances 0.000 claims abstract description 16
- 238000009826 distribution Methods 0.000 claims abstract 2
- 238000001764 infiltration Methods 0.000 claims description 29
- 230000008595 infiltration Effects 0.000 claims description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- 229910002804 graphite Inorganic materials 0.000 claims description 23
- 239000010439 graphite Substances 0.000 claims description 23
- 238000007639 printing Methods 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 20
- 239000011261 inert gas Substances 0.000 claims description 19
- 230000009467 reduction Effects 0.000 claims description 16
- 230000001681 protective effect Effects 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 238000004321 preservation Methods 0.000 claims description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 12
- 229910052593 corundum Inorganic materials 0.000 claims description 12
- 239000010431 corundum Substances 0.000 claims description 12
- 239000004576 sand Substances 0.000 claims description 12
- 238000010146 3D printing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000011049 filling Methods 0.000 claims description 7
- 238000007667 floating Methods 0.000 claims description 7
- 230000004907 flux Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000005098 hot rolling Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 238000011068 loading method Methods 0.000 claims description 7
- 238000009715 pressure infiltration Methods 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000003892 spreading Methods 0.000 claims description 3
- 230000007480 spreading Effects 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims 1
- 238000004506 ultrasonic cleaning Methods 0.000 claims 1
- 238000002679 ablation Methods 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 abstract 1
- 239000001257 hydrogen Substances 0.000 abstract 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 6
- 238000005554 pickling Methods 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010288 cold spraying Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 239000002905 metal composite material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
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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
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y80/00—Products made by additive manufacturing
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
-
- 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
Abstract
The invention discloses a method for preparing a tungsten-copper gradient composite material, which is based on a single-component multi-copper and few-tungsten composite material, prepares a porous tungsten framework with gradient distribution porosity by using a selective laser melting technology, then pressurizes and seeps copper under the protection of hydrogen, finally carries out two times of rolling processes and is assisted with annealing treatment, and can obtain the tungsten-copper gradient composite material with the heat conductivity, the electric conductivity, the strength and the ablation resistance which are synergistically improved. The invention relates to a method for preparing a tungsten-copper gradient composite material, which solves the problem that the heat conductivity and the ablation resistance of the tungsten-copper composite material used for an electromagnetic rail gun guide rail in the prior art can not be simultaneously considered.
Description
Technical Field
The invention belongs to the technical field of metal composite materials, and particularly relates to a method for preparing a tungsten-copper gradient composite material.
Background
The electromagnetic rail gun is a new concept weapon, the bullet is accelerated to the ultra-high speed of 2-3 km/s by using strong electromagnetic energy, the range and the power of the traditional gun are far exceeded, the precision is controllable, and the strong operational efficiency makes the electromagnetic rail gun possibly become a subversive weapon for rewriting future war modes. When the magnetic field magnetic guide rail works, large pulse current flows through the rail and the armature to form a closed loop, and the change rate and the peak value of physical quantities such as electromagnetism, temperature, stress and the like of the guide rail material are extremely large due to the fact that megaampere current is born within a few milliseconds, and huge magnetic field gradient, temperature gradient and stress gradient are formed on the material. At present, the main failure modes of the key guide rail material of the electromagnetic rail gun are material softening and melting, friction and abrasion, edge groove corrosion, high-speed planing and arc ablation. The problem of ablation of guide rail materials is one of key factors for restricting the development of the electromagnetic rail gun to the field of actual combat.
At present, the guide rail of the electromagnetic rail gun mainly adopts a copper-based composite material, wherein the tungsten-copper composite material integrates the respective advantages of W, Cu phases, so that the electromagnetic rail gun has high electrical and thermal conductivity, and good ablation resistance and high-temperature strength. However, the volume fraction of tungsten in the tungsten-copper composite material prepared by the existing traditional powder metallurgy technology, plasma sintering technology, vacuum hot pressing sintering technology, cold spraying technology and the like is over 50 percent, so that the ablation resistance of the composite material is improved at the cost of reducing the thermal conductivity.
Disclosure of Invention
The invention aims to provide a method for preparing a tungsten-copper gradient composite material, which solves the problem that the heat conductivity and the ablation resistance of the tungsten-copper composite material used for an electromagnetic rail gun guide rail in the prior art can not be simultaneously considered.
The technical scheme adopted by the invention is a method for preparing a tungsten-copper gradient composite material, which is implemented according to the following steps:
step 1, designing a porous tungsten skeleton model with gradient porosity;
step 2, 3D printing a porous gradient tungsten framework;
step 3, in H2Under-protection pressure infiltrationCopper (Cu)
Step 3.1, weighing a proper amount of pure copper blocks;
step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten skeleton with graphite paper, then placing the porous gradient tungsten skeleton into a graphite crucible, filling high-purity alumina corundum sand around the porous gradient tungsten skeleton, slightly tamping the graphite crucible to be slightly higher than the top surface of the porous gradient tungsten skeleton, then placing a pure copper block on the upper end surface of the exposed tungsten skeleton, covering a graphite cover, and placing the porous gradient tungsten skeleton into a high-temperature atmosphere protective furnace for pressurized infiltration of copper to obtain a sample;
3.3, removing the floating copper on the surface of the sample through mechanical processing to obtain the tungsten-copper composite material changing along the gradient;
step 4, placing the tungsten-copper composite material changing along the gradient on a hot rolling mill for rolling treatment; and annealing once after each rolling to obtain the tungsten-copper gradient composite material.
The invention is also characterized in that:
the porous tungsten skeleton model comprises three gradient layers, the porosity of the three gradient layers increases from the side contacting with the armature to the side far away from the armature in sequence, and the three gradient layers are respectively k1、k2And k3The volumes of the three gradient layers are respectively V1、V2And V3。
k1＝65％，k2＝80％，k3＝95％。
The shape of the holes in the porous tungsten skeleton model is a cube, a regular octahedron or a hexagonal prism.
The step 2 specifically comprises the following steps:
step 2.1, placing tungsten powder in a powder loading bin of selective laser melting equipment, inputting a porous tungsten skeleton model, starting printing equipment, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to prepare a porous gradient tungsten skeleton;
and 2.2, pickling the porous gradient tungsten skeleton for 1-3 min to remove oil stains and oxide impurities on the surface of the porous gradient tungsten skeleton, and then ultrasonically cleaning the porous gradient tungsten skeleton in alcohol for 3-5 min to obtain the pickled porous gradient tungsten skeleton.
The printing parameters of the selective laser melting equipment are as follows: the diameter of the light spot is 45-100 μm, the scanning distance is 60 μm, and the scanning is performedThe speed is 550-650 mm/s, the powder spreading layer is 25 mu m thick, the laser power is 70-100W, and the laser energy is 80-130J/mm3。
The gas flow of the inert gas is 1-3 m3H; the acid washing solution is as follows: HF. HNO3And H2O is mixed liquid with the volume ratio of 8:1: 21; the ultrasonic frequency is not less than 1MHz, and the ultrasonic temperature is room temperature.
The process of the pressurized melting infiltration of copper in the high-temperature atmosphere protective furnace comprises the following steps: heating to 1300 ℃, and then preserving the temperature for 90 min; introducing H in the temperature rising process2Under a protective atmosphere, the flux is 1-3L/h.
In the step 4, the rolling treatment comprises two rolling and two annealing;
the temperature of the first rolling is 800-830 ℃, the reduction rate is 20-30%, the heat preservation time is 15-30 min, and the unit rolling pressure is 500 MPa; the temperature of the second rolling is 450-500 ℃, the reduction rate is 10-15%, the heat preservation time is 15-30 min, and the unit rolling pressure is 350 MPa;
the annealing temperature after the first rolling is 300 ℃, and the temperature is kept for 2 h; the annealing temperature after the second rolling is 200 ℃, and the temperature is kept for 2 h.
The invention has the beneficial effects that:
(1) according to the method for preparing the tungsten-copper gradient composite material, different properties of W, Cu are combined, and compared with the method for preparing a wear-resistant and ablation-resistant coating on the surface of a copper alloy track, the method can well solve the problems of thermal stress and interface combination caused by large difference of melting points of W, Cu phases; compared with the tungsten-copper composite material with a single component, W, Cu is favorable for giving full play to respective intrinsic characteristics, so that the electrical and thermal conductivity, the strength and the ablation resistance of the composite material are synergistically improved; according to the method for preparing the tungsten-copper gradient composite material, the prepared composite material has good thermal conductivity and ablation resistance;
(2) according to the method for preparing the tungsten-copper gradient composite material, the porosity of the designed porous tungsten skeleton is sequentially increased from the side of the porous tungsten skeleton, which is in contact with the armature, to the side of the porous tungsten skeleton, which is far away from the armature, so that the performance of the composite material obtained after copper infiltration is in gradient change, and the respective advantages of W, Cu phases are fully exerted, thereby obtaining the tungsten-copper gradient composite material with good comprehensive performances such as electrical conductivity, thermal conductivity, strength, ablation resistance and the like;
(3) the invention relates to a method for preparing a tungsten-copper gradient composite material, which uses H during copper infiltration2The pressure infiltration method is adopted to promote the infiltration process, so that the density and the strength of the composite material are improved;
(4) the invention relates to a method for preparing a tungsten-copper gradient composite material, which adopts two-pass rolling and annealing after each rolling to further improve the mechanical property and the ablation resistance of the composite material so as to meet the performance requirement under the actual working condition;
the method for preparing the tungsten-copper gradient composite material can be used for the guide rail material of the electromagnetic rail gun, and has wide application prospect in the fields of pantograph materials, nuclear divertor components, rocket engine cylinder wall materials and the like.
Drawings
FIG. 1 is a microstructure diagram of a porous gradient tungsten skeleton in a tetragonal shape after copper infiltration in example 4;
FIG. 2 a cubic porous gradient tungsten skeleton as in example 1;
FIG. 3 a octahedral porous gradient tungsten skeleton according to example 2;
FIG. 4 the hexagonal-prism porous graded tungsten skeleton of example 3;
FIG. 5 is a graph at H2The charging structure schematic diagram of the porous gradient tungsten framework pressurizing infiltration copper under protection.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The invention provides a method for preparing a tungsten-copper gradient composite material, which is implemented according to the following steps:
step 1, designing a porous tungsten skeleton model with gradient porosity;
wherein the porous tungsten skeleton moldThe type comprises three gradient layers, the porosity of the three gradient layers increases from the side contacting with the armature to the side far away from the armature, and the three gradient layers are respectively k1、k2And k3The volumes of the three gradient layers are respectively V1、V2And V3；k1＝65％，k2＝80％，k395 percent; the shape of the holes in the porous tungsten skeleton model is a cube, a regular octahedron or a hexagonal prism;
step 2, 3D printing a porous gradient tungsten framework;
the method specifically comprises the following steps:
step 2.1, placing tungsten powder in a powder loading bin of selective laser melting equipment, inputting a porous tungsten skeleton model, starting printing equipment, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to prepare a porous gradient tungsten skeleton; wherein the inert gas is argon;
step 2.2, pickling the porous gradient tungsten skeleton for 1-3 min to remove oil stains and oxide impurities on the surface of the porous gradient tungsten skeleton, and then ultrasonically cleaning the porous gradient tungsten skeleton in alcohol for 3-5 min to obtain the pickled porous gradient tungsten skeleton;
the printing parameters of the selective laser melting equipment are as follows: the diameter of a light spot is 45-100 mu m, the scanning distance is 60 mu m, the scanning speed is 550-650 mm/s, the thickness of a powder spreading layer is 25 mu m, the laser power is 70-100W, and the laser energy is 80-130J/mm3；
The gas flow of the inert gas is 1-3 m3H; the acid washing solution is as follows: HF. HNO3And H2O is mixed liquid with the volume ratio of 8:1: 21; the ultrasonic frequency is not less than 1MHz, and the ultrasonic temperature is room temperature;
step 3, in H2Pressure infiltration copper under protection
Step 3.1, weighing a proper amount of pure copper blocks;
mass M of actual infiltrated pure copper block2＝(1.2～1.5)*8.9*(k1*V1+k2*V2+k3*V3) Wherein 1.2-1.5 is infiltration loss coefficient;
step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten skeleton with graphite paper, then placing the porous gradient tungsten skeleton into a graphite crucible, filling high-purity alumina corundum sand around the porous gradient tungsten skeleton, slightly tamping the graphite crucible to be slightly higher than the top surface of the porous gradient tungsten skeleton, then placing a pure copper block on the upper end surface of the exposed tungsten skeleton, covering a graphite cover, and placing the porous gradient tungsten skeleton into a high-temperature atmosphere protective furnace for pressurized infiltration of copper to obtain a sample; as shown in fig. 5.
Wherein, the process of the pressurized melting infiltration of copper in the high-temperature atmosphere protective furnace is as follows: heating to 1300 ℃, and then preserving the temperature for 90 min; introducing H in the temperature rising process2The flux is 1-3L/h under the protection atmosphere, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the particle size of the high-purity alumina corundum sand is 80-100 meshes;
3.3, removing the floating copper on the surface of the sample through mechanical processing to obtain the tungsten-copper composite material changing along the gradient;
step 4, placing the tungsten-copper composite material changing along the gradient on a hot rolling mill for rolling treatment; annealing once after each rolling to obtain the tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling and two annealing;
the temperature of the first rolling is 800-830 ℃, the reduction rate is 20-30%, the heat preservation time is 15-30 min, and the unit rolling pressure is 500 MPa; the temperature of the second rolling is 450-500 ℃, the reduction rate is 10-15%, the heat preservation time is 15-30 min, and the unit rolling pressure is 350 MPa;
the annealing temperature after the first rolling is 300 ℃, and the temperature is kept for 2 h; the annealing temperature after the second rolling is 200 ℃, and the temperature is kept for 2 h.
Wherein, too high rolling temperature can lead to coarse crystal grains, and too low rolling temperature can lead to difficult deformation of tungsten phase with poor plasticity; too high a reduction ratio and rolling pressure may cause cracking of the tungsten phase, and too low a reduction ratio may not exert the function of strengthening performance.
Example 1
The invention relates to a preparation method of a tungsten-copper gradient composite material, which is implemented according to the following steps:
step 1, designing a porous tungsten skeleton model with gradient porosity;
wherein, the porous tungsten skeleton model bagComprises three gradient layers, the porosity of the three gradient layers increases from the side contacting with the armature to the side far away from the armature, and is k1、k2And k3The volumes of the three gradient layers are respectively V1、V2And V3；k1＝65％，k2＝80％，k395 percent; the shape of the hole in the porous tungsten skeleton model is a cube;
step 2, 3D printing a porous gradient tungsten framework;
step 2.1, placing tungsten powder in a powder loading bin of selective laser melting equipment, inputting a porous tungsten skeleton model, starting printing equipment, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to prepare a porous gradient tungsten skeleton; wherein the inert gas is argon;
as shown in fig. 2, the overall size of the printed tungsten skeleton is 10.9 × 10.9mm, and the sizes of the square through holes on each gradient layer are as follows: 1.1 × 1.1mm, 1.3 × 1.3mm, 1.55 × 1.55mm, the wall thicknesses being in the following order: 0.63mm, 0.44mm, 0.24 mm;
step 2.2, HF and HNO with the volume ratio of 8:1:21 are used at room temperature3And H2Pickling the porous gradient tungsten skeleton with the mixed solution of O for 3min to remove oil stains and oxide impurities on the surface of the porous gradient tungsten skeleton, and then ultrasonically cleaning the porous gradient tungsten skeleton in alcohol for 4min at the ultrasonic frequency of 1.2MHz to obtain a bright porous gradient tungsten skeleton;
the printing parameters of the selective laser melting equipment are as follows: the diameter of a light spot is 100 mu m, the scanning interval is 60 mu m, the scanning speed is 550mm/s, the thickness of a powder layer is 25 mu m, the laser power is 90W, and the laser energy is 120J/mm3(ii) a The flow rate of the introduced inert gas is 2m3/h；
Step 3, in H2Pressure infiltration copper under protection
Step 3.1, weighing a proper amount of pure copper blocks (T2 copper);
calculating the mass M of the actual infiltration pure copper block2＝1.2*8.9*(k1*V1+k2*V2+k3*V3)＝19.58g；
Step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten skeleton with graphite paper, then placing the porous gradient tungsten skeleton into a graphite crucible, filling high-purity alumina corundum sand around the porous gradient tungsten skeleton, lightly tamping the porous gradient tungsten skeleton to enable the porous gradient tungsten skeleton to be slightly higher than the top surface of the porous gradient tungsten skeleton, then placing a pure copper block on the upper end surface of the exposed tungsten skeleton, covering a graphite cover, and placing the porous gradient tungsten skeleton in a high-temperature atmosphere protective furnace for pressurized melting and copper infiltration to obtain a sample;
wherein, the process of the pressurized melting infiltration of copper in the high-temperature atmosphere protective furnace is as follows: heating to 1300 ℃, and then preserving the temperature for 90 min; introducing H in the temperature rising process2The flux is 1-3L/h under the protection atmosphere, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the particle size of the high-purity alumina corundum sand is 80-100 meshes;
3.3, removing the floating copper on the surface of the sample through mechanical processing to obtain the tungsten-copper composite material changing along the gradient;
step 4, placing the tungsten-copper composite material changing along the gradient on a hot rolling mill for rolling treatment; annealing once after each rolling to obtain the tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling and two annealing;
the temperature of the first rolling is 800 ℃, the reduction rate is 20%, the heat preservation time is 20min, and the unit rolling pressure is 500 MPa; the temperature of the second rolling is 450 ℃, the reduction rate is 10%, the heat preservation time is 20min, and the unit rolling pressure is 350 MPa; annealing for 2h at 300 ℃ after the first rolling; annealing at 200 ℃ for 2h after the second rolling.
Example 2
The invention relates to a preparation method of a tungsten-copper gradient composite material, which is implemented according to the following steps:
step 1, designing a porous tungsten skeleton model with gradient porosity;
wherein, the porous tungsten skeleton model comprises three gradient layers, the porosity of the three gradient layers is increased from the side contacting with the armature to the side far away from the armature in turn and is k respectively1、k2And k3The volumes of the three gradient layers are respectively V1、V2And V3；k1＝65％，k2＝80％，k395 percent; multiple purposeThe shape of the hole in the hole tungsten framework model is a regular octahedron;
step 2, 3D printing a porous gradient tungsten framework;
step 2.1, placing tungsten powder in a powder loading bin of selective laser melting equipment, inputting a porous tungsten skeleton model, starting printing equipment, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to prepare a porous gradient tungsten skeleton; wherein the inert gas is argon;
as shown in fig. 3, the overall size of the printed tungsten skeleton is 11.1 × 11.1mm, and the diameter and wall thickness of the outer circle on each gradient layer are 2.0 × 0.36mm, 2.0 × 0.24mm and 2.0 × 0.17mm in sequence;
step 2.2, HF and HNO with the volume ratio of 8:1:21 are used at room temperature3And H2Pickling the porous gradient tungsten skeleton with the mixed solution of O for 2min to remove oil stains and oxide impurities on the surface of the porous gradient tungsten skeleton, and then ultrasonically cleaning the porous gradient tungsten skeleton in alcohol for 3min at the ultrasonic frequency of 1.2MHz to obtain a bright porous gradient tungsten skeleton;
the printing parameters of the selective laser melting equipment are as follows: the diameter of a light spot is 80 mu m, the scanning interval is 60 mu m, the scanning speed is 600mm/s, the thickness of a powder layer is 25 mu m, the laser power is 100W, and the laser energy is 100J/mm3(ii) a The flow rate of the introduced inert gas is 3m3/h；
Step 3, in H2Pressure infiltration copper under protection
Step 3.1, weighing a proper amount of pure copper blocks (T2 copper);
calculating the mass M of the actual infiltration pure copper block2＝1.2*8.9*(k1*V1+k2*V2+k3*V3)＝22.14g；
Step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten skeleton with graphite paper, then placing the porous gradient tungsten skeleton into a graphite crucible, filling high-purity alumina corundum sand around the porous gradient tungsten skeleton, lightly tamping the porous gradient tungsten skeleton to enable the porous gradient tungsten skeleton to be slightly higher than the top surface of the porous gradient tungsten skeleton, then placing a pure copper block on the upper end surface of the exposed tungsten skeleton, covering a graphite cover, and placing the porous gradient tungsten skeleton in a high-temperature atmosphere protective furnace for pressurized melting and copper infiltration to obtain a sample;
wherein, the process of the pressurized melting infiltration of copper in the high-temperature atmosphere protective furnace is as follows: heating to 1300 deg.CKeeping the temperature at 90 min; introducing H in the temperature rising process2The flux is 1-3L/h under the protection atmosphere, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the particle size of the high-purity alumina corundum sand is 80-100 meshes;
3.3, removing the floating copper on the surface of the sample through mechanical processing to obtain the tungsten-copper composite material changing along the gradient;
step 4, placing the tungsten-copper composite material changing along the gradient on a hot rolling mill for rolling treatment; annealing once after each rolling to obtain the tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling and two annealing;
the temperature of the first rolling is 810 ℃, the reduction rate is 25%, the heat preservation time is 25min, and the unit rolling pressure is 500 MPa; the temperature of the second rolling is 460 ℃, the reduction rate is 10%, the heat preservation time is 25min, and the unit rolling pressure is 350 MPa; annealing for 2h at 300 ℃ after the first rolling; annealing at 200 ℃ for 2h after the second rolling.
Example 3
The invention relates to a preparation method of a tungsten-copper gradient composite material, which is implemented according to the following steps:
step 1, designing a porous tungsten skeleton model with gradient porosity;
wherein, the porous tungsten skeleton model comprises three gradient layers, the porosity of the three gradient layers is increased from the side contacting with the armature to the side far away from the armature in turn and is k respectively1、k2And k3The volumes of the three gradient layers are respectively V1、V2And V3；k1＝65％，k2＝80％，k395 percent; the shape of the holes in the porous tungsten skeleton model is a hexagonal prism;
step 2, 3D printing a porous gradient tungsten framework;
step 2.1, placing tungsten powder in a powder loading bin of selective laser melting equipment, inputting a porous tungsten skeleton model, starting printing equipment, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to prepare a porous gradient tungsten skeleton; wherein the inert gas is argon;
as shown in fig. 4, the overall size of the printed tungsten skeleton is 11.3 × 9.5 × 12.0mm, and the diameter and wall thickness of the outer circle on each gradient layer are 2.0 × 0.30mm, 2.0 × 0.20mm and 2.0 × 0.10mm in sequence;
step 2.2, HF and HNO with the volume ratio of 8:1:21 are used at room temperature3And H2Pickling the porous gradient tungsten skeleton with the mixed solution of O for 1min to remove oil stains and oxide impurities on the surface of the porous gradient tungsten skeleton, and then ultrasonically cleaning the porous gradient tungsten skeleton in alcohol for 5min at the ultrasonic frequency of 1.2MHz to obtain a bright porous gradient tungsten skeleton;
the printing parameters of the selective laser melting equipment are as follows: the diameter of a light spot is 100 mu m, the scanning interval is 60 mu m, the scanning speed is 550mm/s, the thickness of a powder layer is 25 mu m, the laser power is 100W, and the laser energy is 110J/mm3(ii) a The flow rate of the introduced inert gas is 1m3/h；
Step 3, in H2Pressure infiltration copper under protection
Step 3.1, weighing a proper amount of pure copper blocks (T2 copper);
calculating the mass M of the actual infiltration pure copper block2＝1.2*8.9*(k1*V1+k2*V2+k3*V3)＝20.26g；
Step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten skeleton with graphite paper, then placing the porous gradient tungsten skeleton into a graphite crucible, filling high-purity alumina corundum sand around the porous gradient tungsten skeleton, lightly tamping the porous gradient tungsten skeleton to enable the porous gradient tungsten skeleton to be slightly higher than the top surface of the porous gradient tungsten skeleton, then placing a pure copper block on the upper end surface of the exposed tungsten skeleton, covering a graphite cover, and placing the porous gradient tungsten skeleton in a high-temperature atmosphere protective furnace for pressurized melting and copper infiltration to obtain a sample;
wherein, the process of the pressurized melting infiltration of copper in the high-temperature atmosphere protective furnace is as follows: heating to 1300 ℃, and then preserving the temperature for 90 min; introducing H in the temperature rising process2The flux is 1-3L/h under the protection atmosphere, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the particle size of the high-purity alumina corundum sand is 80-100 meshes;
3.3, removing the floating copper on the surface of the sample through mechanical processing to obtain the tungsten-copper composite material changing along the gradient;
step 4, placing the tungsten-copper composite material changing along the gradient on a hot rolling mill for rolling treatment; annealing once after each rolling to obtain the tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling and two annealing;
the temperature of the first rolling is 820 ℃, the reduction rate is 30%, the heat preservation time is 30min, and the unit rolling pressure is 500 MPa; the temperature of the second rolling is 460 ℃, the reduction rate is 15%, the heat preservation time is 30min, and the unit rolling pressure is 350 MPa; annealing for 2h at 300 ℃ after the first rolling; annealing at 200 ℃ for 2h after the second rolling.
Example 4
The invention relates to a preparation method of a tungsten-copper gradient composite material, which is implemented according to the following steps:
step 1, designing a porous tungsten skeleton model with gradient porosity;
wherein, the porous tungsten skeleton model comprises three gradient layers, the porosity of the three gradient layers is increased from the side contacting with the armature to the side far away from the armature in turn and is k respectively1、k2And k3The volumes of the three gradient layers are respectively V1、V2And V3；k1＝25％，k2＝35％，k355 percent; the shape of the hole in the porous tungsten skeleton model is a cube;
step 2, 3D printing a porous gradient tungsten framework;
step 2.1, placing tungsten powder in a powder loading bin of selective laser melting equipment, inputting a porous tungsten skeleton model, starting printing equipment, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to prepare a porous gradient tungsten skeleton; wherein the inert gas is argon;
step 2.2, HF and HNO with the volume ratio of 8:1:21 are used at room temperature3And H2Pickling the porous gradient tungsten skeleton with the mixed solution of O for 3min to remove oil stains and oxide impurities on the surface of the porous gradient tungsten skeleton, and then ultrasonically cleaning the porous gradient tungsten skeleton in alcohol for 4min at the ultrasonic frequency of 1.2MHz to obtain a bright porous gradient tungsten skeleton;
the printing parameters of the selective laser melting equipment are as follows: the diameter of a light spot is 100 mu m, the scanning interval is 60 mu m, the scanning speed is 550mm/s, the thickness of a powder layer is 25 mu m, the laser power is 90W, and the laser energy is 120J/mm3(ii) a The flow rate of the introduced inert gas is 2m3/h；
Step 3, in H2Pressure infiltration copper under protection
Step 3.1, weighing a proper amount of pure copper blocks (T2 copper);
calculating the mass M of the actual infiltration pure copper block2＝1.2*8.9*(k1*V1+k2*V2+k3*V3)＝6.37g；
Step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten skeleton with graphite paper, then placing the porous gradient tungsten skeleton into a graphite crucible, filling high-purity alumina corundum sand around the porous gradient tungsten skeleton, lightly tamping the porous gradient tungsten skeleton to enable the porous gradient tungsten skeleton to be slightly higher than the top surface of the porous gradient tungsten skeleton, then placing a pure copper block on the upper end surface of the exposed tungsten skeleton, covering a graphite cover, and placing the porous gradient tungsten skeleton in a high-temperature atmosphere protective furnace for pressurized melting and copper infiltration to obtain a sample;
wherein, the process of the pressurized melting infiltration of copper in the high-temperature atmosphere protective furnace is as follows: heating to 1300 ℃, and then preserving the temperature for 90 min; introducing H in the temperature rising process2The flux is 1-3L/h under the protection atmosphere, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the particle size of the high-purity alumina corundum sand is 80-100 meshes;
3.3, removing the floating copper on the surface of the sample through mechanical processing to obtain the tungsten-copper composite material changing along the gradient; as shown in FIG. 1, the volume fraction of tungsten changes from the side in contact with the armature to the side away from the armature as shown in FIG. 1, and the tungsten content is high on the side close to the armature, so the ablation resistance is good, the copper content is high on the side away from the armature, and the conductivity is good, so the ablation resistance and the conductivity of the tungsten-copper composite material are improved.
Step 4, placing the tungsten-copper composite material changing along the gradient on a hot rolling mill for rolling treatment; annealing once after each rolling to obtain the tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling and two annealing;
the temperature of the first rolling is 800 ℃, the reduction rate is 20%, the heat preservation time is 20min, and the unit rolling pressure is 500 MPa; the temperature of the second rolling is 450 ℃, the reduction rate is 10%, the heat preservation time is 20min, and the unit rolling pressure is 350 MPa; annealing for 2h at 300 ℃ after the first rolling; annealing at 200 ℃ for 2h after the second rolling.
Claims (9)
1. A method for preparing a tungsten-copper gradient composite material is characterized by comprising the following steps:
step 1, designing a porous tungsten skeleton model with gradient porosity distribution
Step 2, 3D printing a porous gradient tungsten framework;
step 3, in H2Pressure infiltration copper under protection
Step 3.1, weighing a proper amount of pure copper blocks;
step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten skeleton with graphite paper, then placing the porous gradient tungsten skeleton into a graphite crucible, filling high-purity alumina corundum sand around the porous gradient tungsten skeleton, slightly tamping the porous gradient tungsten skeleton to be slightly higher than the top surface of the porous gradient tungsten skeleton, placing the pure copper block on the upper end surface of the exposed tungsten skeleton, covering a graphite cover, and placing the porous gradient tungsten skeleton into a high-temperature atmosphere protective furnace for pressurized melting and copper infiltration to obtain a sample;
3.3, removing the floating copper on the surface of the sample through mechanical processing to obtain a tungsten-copper composite material changing along a gradient;
step 4, placing the tungsten-copper composite material changing along the gradient on a hot rolling mill for rolling treatment; and annealing once after each rolling to obtain the tungsten-copper gradient composite material.
2. The method for preparing the tungsten-copper gradient composite material as claimed in claim 1, wherein the porous tungsten skeleton model comprises three gradient layers, the porosity of the three gradient layers increases from the side contacting with the armature to the side far away from the armature, and the three gradient layers are respectively k1、k2And k3The volumes of the three gradient layers are respectively V1、V2And V3。
3. The method for preparing the tungsten-copper gradient composite material as claimed in claim 2, wherein k is1＝65％，k2＝80％，k3＝95％。
4. The method for preparing the tungsten-copper gradient composite material as claimed in claim 2, wherein the pore shape in the porous tungsten skeleton model is a cube, a regular octahedron or a hexagonal prism.
5. The method for preparing the tungsten-copper gradient composite material according to claim 1, wherein the step 2 specifically comprises:
step 2.1, placing tungsten powder in a powder loading bin of selective laser melting equipment, inputting a porous tungsten skeleton model, starting printing equipment, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to prepare a porous gradient tungsten skeleton;
and 2.2, carrying out acid washing on the porous gradient tungsten skeleton for 1-3 min to remove oil stains and oxide impurities on the surface of the porous gradient tungsten skeleton, and then carrying out ultrasonic cleaning in alcohol for 3-5 min to obtain the acid-washed porous gradient tungsten skeleton.
6. The method for preparing the tungsten-copper gradient composite material as claimed in claim 5, wherein the printing parameters of the selective laser melting device are as follows: the diameter of a light spot is 45-100 mu m, the scanning distance is 60 mu m, the scanning speed is 550-650 mm/s, the thickness of a powder spreading layer is 25 mu m, the laser power is 70-100W, and the laser energy is 80-130J/mm3。
7. The method for preparing the tungsten-copper gradient composite material as claimed in claim 5, wherein the inert gas has a gas flow rate of 1-3 m3H; the acid washing solution is as follows: HF. HNO3And H2O is mixed liquid with the volume ratio of 8:1: 21; the ultrasonic frequency is not less than 1MHz, and the ultrasonic temperature is room temperature.
8. The method for preparing the tungsten-copper gradient composite material as claimed in claim 1, wherein the process of the high-temperature atmosphere protection furnace pressurized infiltration copper is as follows: heating to 1300 ℃, and then preserving the temperature for 90 min; introducing H in the temperature rising process2Under a protective atmosphere, the flux is 1-3L/h.
9. The method for preparing the tungsten-copper gradient composite material is characterized in that in the step 4, the rolling treatment comprises two rolling and two annealing;
the temperature of the first rolling is 800-830 ℃, the reduction rate is 20-30%, the heat preservation time is 15-30 min, and the unit rolling pressure is 500 MPa; the temperature of the second rolling is 450-500 ℃, the reduction rate is 10-15%, the heat preservation time is 15-30 min, and the unit rolling pressure is 350 MPa;
the annealing temperature after the first rolling is 300 ℃, and the temperature is kept for 2 h; the annealing temperature after the second rolling is 200 ℃, and the temperature is kept for 2 h.
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