CN113084166B - Method for preparing tungsten-copper gradient composite material - Google Patents
Method for preparing tungsten-copper gradient composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 62
- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 46
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 121
- 238000005096 rolling process Methods 0.000 claims abstract description 90
- 229910052802 copper Inorganic materials 0.000 claims abstract description 65
- 239000010949 copper Substances 0.000 claims abstract description 65
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 41
- 239000010937 tungsten Substances 0.000 claims abstract description 36
- 238000000137 annealing Methods 0.000 claims abstract description 30
- 238000002844 melting Methods 0.000 claims abstract description 17
- 230000008018 melting Effects 0.000 claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 33
- 229910002804 graphite Inorganic materials 0.000 claims description 33
- 239000010439 graphite Substances 0.000 claims description 33
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 22
- 229910052593 corundum Inorganic materials 0.000 claims description 22
- 239000010431 corundum Substances 0.000 claims description 22
- 239000004576 sand Substances 0.000 claims description 22
- 238000007639 printing Methods 0.000 claims description 21
- 238000004321 preservation Methods 0.000 claims description 20
- 239000011261 inert gas Substances 0.000 claims description 19
- 230000008569 process Effects 0.000 claims description 19
- 230000009467 reduction Effects 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 238000011049 filling Methods 0.000 claims description 13
- 238000009715 pressure infiltration Methods 0.000 claims description 8
- 230000001681 protective effect Effects 0.000 claims description 8
- 238000010146 3D printing Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 7
- 238000007667 floating Methods 0.000 claims description 7
- 230000004907 flux Effects 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
- 238000003892 spreading Methods 0.000 claims description 7
- 230000007480 spreading Effects 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005554 pickling Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 2
- 230000008595 infiltration Effects 0.000 abstract description 17
- 238000001764 infiltration Methods 0.000 abstract description 17
- 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
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 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
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000010304 firing Methods 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
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000002459 sustained effect Effects 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 low-tungsten composite material, adopts a laser selective melting technology to prepare a porous tungsten skeleton with gradient porosity, then carries out copper infiltration under pressure under the protection of hydrogen, and finally carries out two rolling processes and is assisted by annealing treatment, thus obtaining the tungsten-copper gradient composite material with synergistically improved thermal conductivity, electrical conductivity, strength and ablation resistance. The invention discloses a method for preparing a tungsten-copper gradient composite material, which solves the problem that the thermal conductivity and the ablation resistance of the tungsten-copper composite material used for an electromagnetic track gun guide rail in the prior art cannot 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 track gun is a new concept weapon, and the powerful electromagnetic energy is utilized to accelerate the projectile to the ultra-high speed of 2-3 km/s, the firing range and the power of the traditional gun are far exceeded, the precision is controllable, and the powerful fight efficiency makes the gun possible to become a subversion weapon for rewriting the future war mode. In operation, a large pulse current flows through the track and the armature to form a closed loop, since a megaamp current is to be sustained within a few milliseconds, the change rate and peak value of physical quantities such as electromagnetism, temperature, stress and the like of the guide rail material are extremely large, and huge magnetic field gradient, temperature gradient and stress gradient are formed on the material. Currently, the main failure modes of electromagnetic track gun critical rail materials are material softening and melting, frictional wear, edge pitting, high speed gouging and arc ablation. The problem of ablation of the guide rail material is one of key factors for restricting the development of the electromagnetic track gun to the field of actual combat.
At present, the electromagnetic track gun guide rail mainly adopts a copper-based composite material, wherein the tungsten-copper composite material has high electric conductivity and thermal conductivity and good ablation resistance and high-temperature strength because of combining respective advantages of W, cu two phases. However, the volume fraction of tungsten in the tungsten-copper composite material prepared by the traditional powder metallurgy technology, the plasma sintering technology, the vacuum hot-pressing sintering technology, the cold spraying technology and the like is above 50%, so that the ablation resistance of the composite material is improved at the cost of reducing the heat 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 thermal conductivity and the ablation resistance of the tungsten-copper composite material used for an electromagnetic track gun guide rail in the prior art cannot 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 distribution;
step 2,3D printing a porous gradient tungsten skeleton;
step 3, at H 2 Under protection, pressure infiltration copper
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 framework by graphite paper, then filling the graphite paper into a graphite crucible, filling high-purity alumina corundum sand around the graphite crucible, lightly tamping the alumina corundum sand slightly higher than the top surface of the tungsten framework, then placing a pure copper block on the upper end surface of the exposed tungsten framework, covering a graphite cover, and placing the tungsten framework in a high-temperature atmosphere protection furnace for pressurizing and infiltrating copper to obtain a sample;
step 3.3, removing floating copper on the surface of the sample by mechanical processing to obtain a tungsten copper composite material which changes along the gradient;
step 4, placing the tungsten-copper composite material which changes 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, wherein the porosities of the three gradient layers sequentially increase from the side contacted with the armature to the side far away from the armature, and k is respectively 1 、k 2 And k 3 The volumes of the three gradient layers are V respectively 1 、V 2 And V 3 。
k 1 =65%,k 2 =80%,k 3 =95%。
The shape of the holes in the porous tungsten skeleton model is square, regular octahedron or hexagonal prism.
The step 2 is specifically as follows:
step 2.1, placing tungsten powder in a powder loading bin of a laser selective melting device, inputting a porous tungsten skeleton model, starting a printing device, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to obtain a porous gradient tungsten skeleton;
and 2.2, pickling the porous gradient tungsten skeleton for 1-3 min, removing greasy dirt 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 laser selective melting equipment are as follows: the diameter of the light spot is 45-100 mu m, the scanning interval is 60 mu m, the scanning speed is 550-650 mm/s, the thickness of the powder spreading layer is 25 mu m, the laser power is 70-100W, and the laser energy is 80-130J/mm 3 。
The gas flow rate of the inert gas is 1-3 m 3 /h; the acid washing solution is as follows: HF. HNO (HNO) 3 And H is 2 Mixing solution of O 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 high-temperature atmosphere protection furnace for pressure infiltration of copper comprises the following steps: heating to 1300 ℃, and then preserving heat for 90min; h is led in during the heating process 2 The flux is 1-3L/h when the protective atmosphere is used.
In the step 4, the rolling treatment comprises two times of rolling and two times of annealing;
the temperature of the first rolling is 800-830 ℃, the rolling reduction is 20-30%, the heat preservation time is 15-30 min, and the unit rolling pressure is 500MPa; the temperature of the second rolling is 450-500 ℃, the rolling reduction is 10-15%, the heat preservation time is 15-30 min, and the unit rolling pressure is 350MPa;
the annealing temperature after the first rolling is 300 ℃, and the heat preservation is carried out for 2 hours; the annealing temperature after the second rolling is 200 ℃, and the heat preservation is carried out for 2 hours.
The beneficial effects of the invention are as follows:
(1) According to the method for preparing the tungsten-copper gradient composite material, the composite material combines different performances of W, cu, and compared with the method for preparing the wear-resistant and anti-ablation coating on the surface of the copper alloy track, the method can well solve the problems of thermal stress and interface combination caused by larger difference of W, cu two-phase melting points; compared with a tungsten-copper composite material with a single component, the composite material is favorable for W, cu to fully exert respective intrinsic characteristics, so that the electric conduction, the heat conduction, the strength and the ablation resistance of the composite material are synergistically improved; the method for preparing the tungsten-copper gradient 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 which is contacted with the armature to the side which is far away from the armature, so that the performance of the composite material obtained after copper infiltration is also changed in a gradient manner, the respective advantages of W, cu two phases are fully exerted, and the tungsten-copper gradient composite material with good comprehensive performances such as electric conductivity, heat conductivity, strength and ablation resistance is obtained;
(3) The invention relates to a method for preparing a tungsten-copper gradient composite material, which uses H when copper infiltration is carried out 2 The protective atmosphere is used for reducing, promoting infiltration and improving the density of the tungsten framework after copper infiltration so as to improve the conductivity and strength of the composite material;
(4) According to the method for preparing the tungsten-copper gradient composite material, the mechanical property and the ablation resistance of the composite material are further improved by adopting two-pass rolling and annealing after each rolling, so that the performance requirements under actual working conditions are met;
the method for preparing the tungsten-copper gradient composite material not only can be used for electromagnetic track gun guide rail materials, but also has wide application prospects in the fields of pantograph materials, nuclear divertor parts, rocket engine cylinder wall materials and the like.
Drawings
FIG. 1 is a graph of the microscopic morphology of a porous gradient tungsten skeleton copper infiltrated with a square shape in example 4;
FIG. 2 a cube porous gradient tungsten backbone in example 1;
FIG. 3 a regular octahedral porous gradient tungsten framework in example 2;
FIG. 4 a hexagonal-prism porous gradient tungsten backbone of example 3;
FIG. 5 is at H 2 And (3) carrying out pressurized copper infiltration on the porous gradient tungsten skeleton under protection to obtain a schematic diagram of the furnace charging structure.
Detailed Description
The invention will be described in detail below with reference to the drawings and the detailed description.
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 distribution;
wherein the porous tungsten skeleton model comprises three gradient layers, the porosities of the three gradient layers sequentially increase from the side contacted with the armature to the side far away from the armature, and k is respectively 1 、k 2 And k 3 The volumes of the three gradient layers are V respectively 1 、V 2 And V 3 ;k 1 =65%,k 2 =80%,k 3 =95%; the shape of the holes in the porous tungsten skeleton model is square, regular octahedron or hexagonal prism;
step 2,3D printing a porous gradient tungsten skeleton;
the method comprises the following steps:
step 2.1, placing tungsten powder in a powder loading bin of a laser selective melting device, inputting a porous tungsten skeleton model, starting a printing device, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to obtain a porous gradient tungsten skeleton; wherein the inert gas is argon;
step 2.2, pickling the porous gradient tungsten skeleton for 1-3 min, removing greasy dirt 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 a pickled porous gradient tungsten skeleton;
the printing parameters of the laser selective melting equipment are as follows: the diameter of the light spot is 45-100 mu m, the scanning interval is 60 mu m, the scanning speed is 550-650 mm/s, the thickness of the powder spreading layer is 25 mu m, the laser power is 70-100W, and the laser energy is 80-130J/mm 3 ;
The gas flow rate of the inert gas is 1-3 m 3 /h; the acid washing solution is as follows: HF. HNO (HNO) 3 And H is 2 Mixing solution of O 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, at H 2 Under protection, pressure infiltration copper
Step 3.1, weighing a proper amount of pure copper blocks;
mass M of actual infiltrated pure copper block 2 =(1.2~1.5)*8.9*(k 1 *V 1 +k 2 *V 2 +k 3 *V 3 ) Wherein 1.2 to 1.5 are infiltration loss coefficients;
step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten framework by graphite paper, then filling the graphite paper into a graphite crucible, filling high-purity alumina corundum sand around the graphite crucible, lightly tamping the alumina corundum sand slightly higher than the top surface of the tungsten framework, then placing a pure copper block on the upper end surface of the exposed tungsten framework, covering a graphite cover, and placing the tungsten framework in a high-temperature atmosphere protection furnace for pressurizing and infiltrating copper to obtain a sample; as shown in fig. 5.
Wherein, the process of copper infiltration under pressure in the high-temperature atmosphere protection furnace comprises the following steps: heating to 1300 ℃, and then preserving heat for 90min; h is led in during the heating process 2 The flux of the protective atmosphere is 1-3L/h, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the grain diameter of the high-purity alumina corundum sand is 80-100 meshes;
step 3.3, removing floating copper on the surface of the sample by mechanical processing to obtain a tungsten copper composite material which changes along the gradient;
step 4, placing the tungsten-copper composite material which changes along the gradient on a hot rolling mill for rolling treatment; annealing is carried out once for each rolling time to obtain a tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling steps and two annealing steps;
the temperature of the first rolling is 800-830 ℃, the rolling reduction is 20-30%, the heat preservation time is 15-30 min, and the unit rolling pressure is 500MPa; the temperature of the second rolling is 450-500 ℃, the rolling reduction is 10-15%, the heat preservation time is 15-30 min, and the unit rolling pressure is 350MPa;
the annealing temperature after the first rolling is 300 ℃, and the heat preservation is carried out for 2 hours; the annealing temperature after the second rolling is 200 ℃, and the heat preservation is carried out for 2 hours.
Wherein, too high rolling temperature can cause coarse grains, and too low rolling temperature can hardly deform tungsten phase with poor plasticity; too high a reduction rate and rolling pressure may cause cracking of the tungsten phase, and too low a reduction rate may not be effective in strengthening the properties.
Example 1
The invention discloses 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 distribution;
wherein the porous tungsten skeleton model comprises three gradient layers, the porosities of the three gradient layers sequentially increase from the side contacted with the armature to the side far away from the armature, and k is respectively 1 、k 2 And k 3 The volumes of the three gradient layers are V respectively 1 、V 2 And V 3 ;k 1 =65%,k 2 =80%,k 3 =95%; the shape of the middle hole of the porous tungsten skeleton model is square;
step 2,3D printing a porous gradient tungsten skeleton;
step 2.1, placing tungsten powder in a powder loading bin of a laser selective melting device, inputting a porous tungsten skeleton model, starting a printing device, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to obtain a porous gradient tungsten skeleton; wherein the inert gas is argon;
as shown in fig. 2, the overall size of the printed tungsten skeleton was 10.9 x 10.9mm, the sizes of the cube through holes on each gradient layer are as follows: 1.1 x 1.1mm, 1.3 x 1.3mm, 1.55 x 1.55mm, the wall thicknesses are in order: 0.63mm, 0.44mm, 0.24mm;
step 2.2, HF and HNO in a volume ratio of 8:1:21 are used at room temperature 3 And H is 2 Washing the porous gradient tungsten skeleton with mixed solution of O for 3min to remove greasy dirt 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 ultrasonic frequency of 1.2MHz to obtain a bright porous gradient tungsten skeleton;
the printing parameters of the laser selective melting equipment are as follows: the diameter of the light spot is 100 mu m, the scanning interval is 60 mu m, the scanning speed is 550mm/s, the thickness of the powder spreading layer is 25 mu m, the laser power is 90W, and the laser energy is 120J/mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the introduced inert gas is 2m 3 /h;
Step 3, at H 2 Under protection, pressure infiltration copper
Step 3.1, weighing a proper amount of pure copper block (T2 copper);
calculating the mass M of the actual infiltrated pure copper block 2 =1.2*8.9*(k 1 *V 1 +k 2 *V 2 +k 3 *V 3 )=19.58g;
Step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten framework by graphite paper, then filling the graphite paper into a graphite crucible, filling high-purity alumina corundum sand around the graphite crucible, lightly tamping the alumina corundum sand to make the alumina corundum sand slightly higher than the top surface of the tungsten framework, then placing a pure copper block on the upper end surface of the exposed tungsten framework, covering a graphite cover, and placing the tungsten framework in a high-temperature atmosphere protection furnace to pressurize and infiltrate copper to obtain a sample;
wherein, the process of copper infiltration under pressure in the high-temperature atmosphere protection furnace comprises the following steps: heating to 1300 ℃, and then preserving heat for 90min; h is led in during the heating process 2 The flux of the protective atmosphere is 1-3L/h, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the grain diameter of the high-purity alumina corundum sand is 80-100 meshes;
step 3.3, removing floating copper on the surface of the sample by mechanical processing to obtain a tungsten copper composite material which changes along the gradient;
step 4, placing the tungsten-copper composite material which changes along the gradient on a hot rolling mill for rolling treatment; annealing is carried out once for each rolling time to obtain a tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling steps and two annealing steps;
the temperature of the first rolling is 800 ℃, the rolling reduction is 20%, the heat preservation time is 20min, and the unit rolling pressure is 500MPa; the temperature of the second rolling is 450 ℃, the rolling reduction is 10%, the heat preservation time is 20min, and the unit rolling pressure is 350MPa; annealing for 2h at 300 ℃ after the first rolling; annealing at 200 ℃ for 2h after the second rolling.
Example 2
The invention discloses 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 distribution;
wherein the porous tungsten skeleton model comprises three gradient layers, the porosities of the three gradient layers sequentially increase from the side contacted with the armature to the side far away from the armature, and k is respectively 1 、k 2 And k 3 The volumes of the three gradient layers are V respectively 1 、V 2 And V 3 ;k 1 =65%,k 2 =80%,k 3 =95%; the shape of the holes in the porous tungsten skeleton model is a regular octahedron;
step 2,3D printing a porous gradient tungsten skeleton;
step 2.1, placing tungsten powder in a powder loading bin of a laser selective melting device, inputting a porous tungsten skeleton model, starting a printing device, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to obtain a porous gradient tungsten skeleton; wherein the inert gas is argon;
as shown in fig. 3, the overall size of the printed tungsten backbone was 11.1 x 11.1mm, the diameter and the wall thickness of the outer circle on each gradient layer are 2.0 x 0.36mm, 2.0 x 0.24mm and 2.0 x 0.17mm in sequence;
step 2.2, HF and HNO in a volume ratio of 8:1:21 are used at room temperature 3 And H is 2 Washing the porous gradient tungsten skeleton with mixed solution of O for 2min to remove greasy dirt 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 ultrasonic frequency of 1.2MHz to obtain a bright porous gradient tungsten skeleton;
the printing parameters of the laser selective melting equipment are as follows: the diameter of the light spot is 80 mu m, the scanning interval is 60 mu m, the scanning speed is 600mm/s, the thickness of the powder spreading layer is 25 mu m, the laser power is 100W, and the laser energy is 100J/mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the introduced inert gas is 3m 3 /h;
Step 3, at H 2 Under protection, pressure infiltration copper
Step 3.1, weighing a proper amount of pure copper block (T2 copper);
calculating the mass M of the actual infiltrated pure copper block 2 =1.2*8.9*(k 1 *V 1 +k 2 *V 2 +k 3 *V 3 )=22.14g;
Step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten framework by graphite paper, then filling the graphite paper into a graphite crucible, filling high-purity alumina corundum sand around the graphite crucible, lightly tamping the alumina corundum sand to make the alumina corundum sand slightly higher than the top surface of the tungsten framework, then placing a pure copper block on the upper end surface of the exposed tungsten framework, covering a graphite cover, and placing the tungsten framework in a high-temperature atmosphere protection furnace to pressurize and infiltrate copper to obtain a sample;
wherein, the process of copper infiltration under pressure in the high-temperature atmosphere protection furnace comprises the following steps: heating to 1300 ℃, and then preserving heat for 90min; h is led in during the heating process 2 The flux of the protective atmosphere is 1-3L/h, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the grain diameter of the high-purity alumina corundum sand is 80-100 meshes;
step 3.3, removing floating copper on the surface of the sample by mechanical processing to obtain a tungsten copper composite material which changes along the gradient;
step 4, placing the tungsten-copper composite material which changes along the gradient on a hot rolling mill for rolling treatment; annealing is carried out once for each rolling time to obtain a tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling steps and two annealing steps;
the temperature of the first rolling is 810 ℃, the rolling reduction is 25%, the heat preservation time is 25min, and the unit rolling pressure is 500MPa; the temperature of the second rolling is 460 ℃, the rolling reduction is 10%, the heat preservation time is 25min, and the unit rolling pressure is 350MPa; annealing for 2h at 300 ℃ after the first rolling; annealing at 200 ℃ for 2h after the second rolling.
Example 3
The invention discloses 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 distribution;
wherein the porous tungsten skeleton model comprises three gradient layers, the porosities of the three gradient layers sequentially increase from the side contacted with the armature to the side far away from the armature, and k is respectively 1 、k 2 And k 3 The volumes of the three gradient layers are V respectively 1 、V 2 And V 3 ;k 1 =65%,k 2 =80%,k 3 =95%; the shape of the middle hole of the porous tungsten skeleton model is hexagonal prism;
step 2,3D printing a porous gradient tungsten skeleton;
step 2.1, placing tungsten powder in a powder loading bin of a laser selective melting device, inputting a porous tungsten skeleton model, starting a printing device, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to obtain 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 in a volume ratio of 8:1:21 are used at room temperature 3 And H is 2 Washing the porous gradient tungsten skeleton with mixed solution of O for 1min to remove greasy dirt 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 ultrasonic frequency of 1.2MHz to obtain a bright porous gradient tungsten skeleton;
the printing parameters of the laser selective melting equipment are as follows: the diameter of the light spot is 100 μm, the scanning interval is 60 μm, the scanning speed is 550mm/s, the thickness of the powder spreading layer is 25 μm, and the laser power is100W, laser energy 110J/mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the introduced inert gas is 1m 3 /h;
Step 3, at H 2 Under protection, pressure infiltration copper
Step 3.1, weighing a proper amount of pure copper block (T2 copper);
calculating the mass M of the actual infiltrated pure copper block 2 =1.2*8.9*(k 1 *V 1 +k 2 *V 2 +k 3 *V 3 )=20.26g;
Step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten framework by graphite paper, then filling the graphite paper into a graphite crucible, filling high-purity alumina corundum sand around the graphite crucible, lightly tamping the alumina corundum sand to make the alumina corundum sand slightly higher than the top surface of the tungsten framework, then placing a pure copper block on the upper end surface of the exposed tungsten framework, covering a graphite cover, and placing the tungsten framework in a high-temperature atmosphere protection furnace to pressurize and infiltrate copper to obtain a sample;
wherein, the process of copper infiltration under pressure in the high-temperature atmosphere protection furnace comprises the following steps: heating to 1300 ℃, and then preserving heat for 90min; h is led in during the heating process 2 The flux of the protective atmosphere is 1-3L/h, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the grain diameter of the high-purity alumina corundum sand is 80-100 meshes;
step 3.3, removing floating copper on the surface of the sample by mechanical processing to obtain a tungsten copper composite material which changes along the gradient;
step 4, placing the tungsten-copper composite material which changes along the gradient on a hot rolling mill for rolling treatment; annealing is carried out once for each rolling time to obtain a tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling steps and two annealing steps;
the temperature of the first rolling is 820 ℃, the rolling reduction is 30%, the heat preservation time is 30min, and the unit rolling pressure is 500MPa; the temperature of the second rolling is 460 ℃, the rolling reduction is 15%, the heat preservation time is 30min, and the unit rolling pressure is 350MPa; annealing for 2h at 300 ℃ after the first rolling; annealing at 200 ℃ for 2h after the second rolling.
Example 4
The invention discloses 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 distribution;
wherein the porous tungsten skeleton model comprises three gradient layers, the porosities of the three gradient layers sequentially increase from the side contacted with the armature to the side far away from the armature, and k is respectively 1 、k 2 And k 3 The volumes of the three gradient layers are V respectively 1 、V 2 And V 3 ;k 1 =25%,k 2 =35%,k 3 =55%; the shape of the middle hole of the porous tungsten skeleton model is square;
step 2,3D printing a porous gradient tungsten skeleton;
step 2.1, placing tungsten powder in a powder loading bin of a laser selective melting device, inputting a porous tungsten skeleton model, starting a printing device, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to obtain a porous gradient tungsten skeleton; wherein the inert gas is argon;
step 2.2, HF and HNO in a volume ratio of 8:1:21 are used at room temperature 3 And H is 2 Washing the porous gradient tungsten skeleton with mixed solution of O for 3min to remove greasy dirt 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 ultrasonic frequency of 1.2MHz to obtain a bright porous gradient tungsten skeleton;
the printing parameters of the laser selective melting equipment are as follows: the diameter of the light spot is 100 mu m, the scanning interval is 60 mu m, the scanning speed is 550mm/s, the thickness of the powder spreading layer is 25 mu m, the laser power is 90W, and the laser energy is 120J/mm 3 The method comprises the steps of carrying out a first treatment on the surface of the The flow rate of the introduced inert gas is 2m 3 /h;
Step 3, at H 2 Under protection, pressure infiltration copper
Step 3.1, weighing a proper amount of pure copper block (T2 copper);
calculating the mass M of the actual infiltrated pure copper block 2 =1.2*8.9*(k 1 *V 1 +k 2 *V 2 +k 3 *V 3 )=6.37g;
Step 3.2, wrapping the periphery and the bottom surface of the porous gradient tungsten framework by graphite paper, then filling the graphite paper into a graphite crucible, filling high-purity alumina corundum sand around the graphite crucible, lightly tamping the alumina corundum sand to make the alumina corundum sand slightly higher than the top surface of the tungsten framework, then placing a pure copper block on the upper end surface of the exposed tungsten framework, covering a graphite cover, and placing the tungsten framework in a high-temperature atmosphere protection furnace to pressurize and infiltrate copper to obtain a sample;
wherein, the process of copper infiltration under pressure in the high-temperature atmosphere protection furnace comprises the following steps: heating to 1300 ℃, and then preserving heat for 90min; h is led in during the heating process 2 The flux of the protective atmosphere is 1-3L/h, so that the oxidation of a sample can be prevented, and the infiltration process of copper can be promoted; the grain diameter of the high-purity alumina corundum sand is 80-100 meshes;
step 3.3, removing floating copper on the surface of the sample by mechanical processing to obtain a tungsten copper composite material which changes along the gradient; as shown in fig. 1, it can be seen from fig. 1 that the tungsten volume fraction changes from the side contacting the armature to the side far from the armature, and that the tungsten content is high on the side near the armature, the ablation resistance is good, the copper content is high on the side far from the armature, and the conductivity is good, so that both the ablation resistance and the conductivity of the tungsten-copper composite material in the invention are improved.
Step 4, placing the tungsten-copper composite material which changes along the gradient on a hot rolling mill for rolling treatment; annealing is carried out once for each rolling time to obtain a tungsten-copper gradient composite material;
wherein the rolling treatment comprises two rolling steps and two annealing steps;
the temperature of the first rolling is 800 ℃, the rolling reduction is 20%, the heat preservation time is 20min, and the unit rolling pressure is 500MPa; the temperature of the second rolling is 450 ℃, the rolling reduction is 10%, the heat preservation time is 20min, and the unit rolling pressure is 350MPa; annealing for 2h at 300 ℃ after the first rolling; annealing at 200 ℃ for 2h after the second rolling.
Claims (6)
1. The method for preparing the tungsten-copper gradient composite material is characterized by comprising the following steps of:
step 1, designing a porous tungsten skeleton model with gradient porosity distribution;
step 2,3D printing a porous gradient tungsten skeleton;
step 3, at H 2 Pressurizing and infiltrating 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 framework by graphite paper, then filling the wrapped periphery with high-purity alumina corundum sand into a graphite crucible, lightly tamping the wrapped periphery and the lightly tamped periphery to be slightly higher than the top surface of the tungsten framework, then placing the pure copper block on the upper end surface of the exposed tungsten framework, covering a graphite cover, and placing the exposed tungsten framework in a high-temperature atmosphere protection furnace to pressurize and infiltrate copper to obtain a sample;
step 3.3, removing floating copper on the surface of the sample by mechanical processing to obtain a tungsten-copper composite material changing along the gradient;
step 4, placing the tungsten-copper composite material along the gradient change on a hot rolling mill for rolling treatment; annealing is carried out once for each rolling time, and then the tungsten-copper gradient composite material is obtained;
the porous tungsten skeleton model comprises three gradient layers, wherein the porosities of the three gradient layers sequentially increase from the side contacted with the armature to the side far away from the armature, and k is respectively 1 、k 2 And k 3 The volumes of the three gradient layers are V respectively 1 、V 2 And V 3 ;
The k is 1 =65%,k 2 =80%,k 3 =95%;
In the step 4, the rolling treatment comprises two rolling steps and two annealing steps;
the temperature of the first rolling is 800-830 ℃, the rolling reduction is 20-30%, the heat preservation time is 15-30 min, and the unit rolling pressure is 500MPa; the temperature of the second rolling is 450-500 ℃, the rolling reduction is 10-15%, the heat preservation time is 15-30 min, and the unit rolling pressure is 350MPa;
the annealing temperature after the first rolling is 300 ℃, and the heat preservation is carried out for 2 hours; the annealing temperature after the second rolling is 200 ℃, and the heat preservation is carried out for 2 hours.
2. The method of preparing a tungsten copper gradient composite according to claim 1, wherein the porous tungsten skeleton model has a shape of a square, an regular octahedron or a hexagonal prism.
3. The method for preparing the tungsten-copper gradient composite material according to claim 1, wherein the step 2 is specifically:
step 2.1, placing tungsten powder in a powder loading bin of a laser selective melting device, inputting a porous tungsten skeleton model, starting a printing device, selecting checkerboard scanning, forming layer by layer, and continuously introducing inert gas in the printing process to obtain a porous gradient tungsten skeleton;
and 2.2, pickling the porous gradient tungsten skeleton for 1-3 min, removing greasy dirt 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.
4. A method of preparing a tungsten copper gradient composite material according to claim 3, wherein the printing parameters of the laser selective melting apparatus are: the diameter of the light spot is 45-100 mu m, the scanning interval is 60 mu m, the scanning speed is 550-650 mm/s, the thickness of the powder spreading layer is 25 mu m, the laser power is 70-100W, and the laser energy is 80-130J/mm 3 。
5. A method for preparing a tungsten copper gradient composite material according to claim 3, wherein the inert gas has a gas flow rate of 1 to 3m 3 /h; the acid washing solution is as follows: HF. HNO (HNO) 3 And H is 2 Mixing solution of O with the volume ratio of 8:1:21; the ultrasonic frequency is not less than 1MHz, and the ultrasonic temperature is room temperature.
6. The method for preparing the tungsten-copper gradient composite material according to claim 1, wherein the process of pressure infiltration of copper by the high-temperature atmosphere protection furnace is as follows: heating to 1300 ℃, and then preserving heat for 90min; h is led in during the heating process 2 The flux is 1-3L/h when the protective atmosphere is used.
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