CN110846596B - Wf/W alloy-diamond composite material and preparation method thereof - Google Patents
Wf/W alloy-diamond composite material and preparation method thereof Download PDFInfo
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- 239000010432 diamond Substances 0.000 title claims abstract description 102
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 102
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 36
- 239000010703 silicon Substances 0.000 claims abstract description 36
- 229910001080 W alloy Inorganic materials 0.000 claims abstract description 34
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 15
- 239000010937 tungsten Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 53
- 239000002245 particle Substances 0.000 claims description 48
- 239000000843 powder Substances 0.000 claims description 45
- 238000005245 sintering Methods 0.000 claims description 26
- 238000000498 ball milling Methods 0.000 claims description 21
- 238000005260 corrosion Methods 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 19
- 239000011863 silicon-based powder Substances 0.000 claims description 12
- 239000001110 calcium chloride Substances 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 7
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 5
- 238000005551 mechanical alloying Methods 0.000 claims description 5
- 238000005530 etching Methods 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 238000002490 spark plasma sintering Methods 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 238000002679 ablation Methods 0.000 abstract description 2
- 238000005275 alloying Methods 0.000 abstract description 2
- 238000005336 cracking Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000835 fiber Substances 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 229910026551 ZrC Inorganic materials 0.000 description 14
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 6
- 239000011247 coating layer Substances 0.000 description 5
- 230000007797 corrosion Effects 0.000 description 5
- 239000010431 corundum Substances 0.000 description 5
- 229910052593 corundum Inorganic materials 0.000 description 5
- 239000002270 dispersing agent Substances 0.000 description 5
- 230000004927 fusion Effects 0.000 description 5
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000011148 calcium chloride Nutrition 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008646 thermal stress Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/02—Pretreatment of the fibres or filaments
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C47/00—Making alloys containing metallic or non-metallic fibres or filaments
- C22C47/14—Making alloys containing metallic or non-metallic fibres or filaments by powder metallurgy, i.e. by processing mixtures of metal powder and fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C49/00—Alloys containing metallic or non-metallic fibres or filaments
- C22C49/02—Alloys containing metallic or non-metallic fibres or filaments characterised by the matrix material
- C22C49/10—Refractory metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses a WfAlloy/diamond composite material and preparation method thereof, WfThe raw material of the/W alloy-diamond composite material comprises WfW alloy and diamond coated with silicon film on surface, WfRepresenting a tungsten fiber. Invention Wfa/W alloy-diamond composite material prepared by adopting WfThe alloying and synergistic toughening of the matrix of the tungsten-based composite material can improve the ablation resistance and the cracking resistance of the composite material; by utilizing the property that the thermal conductivity of diamond is far higher than that of tungsten, the diamond is doped into the matrix of the composite material, so that the effect of improving the thermal conductivity can be achieved, and the aim of quickly transferring energy of the composite material is fulfilled.
Description
Technical Field
The invention relates to the field of materials, in particular to Wfa/W alloy-diamond composite material and a preparation method thereof.
Background
Tungsten is the most promising first wall material of a divertor in a fusion reactor due to the advantages of high melting point, low sputtering rate and the like. However, the main problem with pure tungsten is that the thermal conductivity is relatively low (-150W/m.K), above 20MW/m2Under the thermal load working condition, the divertor component has insufficient energy transfer capacity, the surface temperature is too high, the internal high temperature difference and high stress can be caused, and the tungsten target module can crack under the action of pulse thermal shock load.
Taking an international thermonuclear fusion experimental reactor (ITER) divertor tube-penetrating type tungsten target (W/Cu/CuCrZr) as an example, the tungsten target is subjected to 20MW/m2Thermal load conditionAnd the surface temperature of the module exceeds 2000 ℃, the temperature difference of about 1500 ℃ exists between the surface of the tungsten target and the heat sink copper pipe, and large thermal stress is generated, so that the risk that the divertor module is cracked possibly is caused. The steady-state heat load of the divertor of the Chinese fusion engineering experimental reactor (CFETR) under engineering design is higher and can reach 40MW/m2Therefore, the materials and the structure of the existing divertor can not meet the development requirements of the future fusion reactor. The development of high-heat-conductivity and high-toughness tungsten-based materials is one of the key points and trends of future fusion reactor divertor parts and material research and development.
Disclosure of Invention
The invention aims to solve the technical problem of providing the W with better heat conductivity and mechanical propertyfa/W alloy-diamond composite material and a preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme: wfThe material of the/W alloy-diamond composite material comprises WfW (W is a tungsten alloy in the Chinese language) and diamond coated with a silicon film on the surface, WfRepresenting a tungsten fiber.
Further, the W alloy is composed of a matrix component W and a dopant component including ZrC (a Chinese name of ZrC is zirconium carbide) and Y2O3(Y2O3Is named as yttrium oxide), ZrC and Y in W alloy2O3The mass fraction of (A) is 0-1%. In the process of implementing the invention, the inventor finds that the W alloy with the proportion is finally obtainedfThe thermal conductivity and toughness performance of the/W alloy-diamond composite material are better.
Further, WfThe diameter of (2) is 0 to 300 μm. In the course of carrying out the present invention, the inventors found that WfThe diameter of (A) is selected from 0 to 300 mu m, and the W obtained finallyfThe thermal conductivity and toughness performance of the/W alloy-diamond composite material are better.
Further, in the raw materials, W in the raw materialsfThe mass fraction of the diamond is 0-30%, the mass fraction of the diamond with the silicon film plated on the surface is 0-4%, and the balance is W alloy. In the process of implementing the invention, the inventor finds that the raw materials are adoptedThe W finally obtained by the proportioningfThe thermal conductivity and toughness performance of the/W alloy-diamond composite material are better.
The W isfThe preparation method of the/W alloy-diamond composite material comprises the following steps:
(1) preparation of W alloy
According to the composition of W alloy, respectively taking out the powder raw materials of each component, and then preparing W alloy powder in a mechanical alloying mode;
(2)Wfsurface treatment of
By using concentrated nitric acid solution to WfPerforming surface etching treatment, and cleaning to remove WfThe impurities on the surface are remained to obtain W subjected to surface corrosionf；
(3) Surface silicon plating treatment of diamond
Diamond particles, Si (Si is named as silicon in the Chinese language) powder and anhydrous CaCl2(CaCl2The Chinese name of calcium dichloride), and performing heat preservation treatment at high temperature to obtain diamond particles with silicon films plated on the surfaces;
the sequence of the steps (1), (2) and (3) is not limited;
(4) composite powder pressing and sintering
Respectively taking out the W subjected to surface corrosionfMixing the W alloy powder and the diamond particles with the silicon film plated on the surface uniformly, putting the mixture into a graphite die, and sintering by adopting a spark plasma sintering process to obtain Wfa/W alloy-diamond composite.
Further, in the step (1), mechanical alloying is realized by ball milling in a ball mill, the ball milling rotating speed is 200-400 r/min, and the ball milling time is 30-50 h. In carrying out the present invention, the inventors found that under such conditions, mechanical alloying of the W alloy can be sufficiently achieved.
Further, in the step (2), concentrated nitric acid is used for treating WfThe treatment time is 1-3 h. To be able to sufficiently etch away WfThe surface of the raw material is dirty and remains, thereby ensuring full contact with other raw materials.
Further, in the step (3), diamond particles and SiPowder and anhydrous CaCl2The mass ratio of the components is 1:1:4, the temperature of the heat preservation treatment at high temperature is 1100-1200 ℃, and the time is 30-60 min. In carrying out the present invention, the inventors have found that a silicon film having a uniform surface can be produced on the surface of the diamond particles by using this condition.
Further, in the step (4), the sintering treatment temperature is 1500-1800 ℃, the pressure is 20-60 MPa, and the time is 2-5 min. In the process of implementing the invention, the inventor finds that by adopting the condition, the raw materials can be fully combined to form the composite material with better thermal conductivity and toughness property.
The invention has the beneficial effects that:
invention Wfa/W alloy-diamond composite material prepared by adopting WfThe alloying and synergistic toughening of the matrix of the tungsten-based composite material can improve the ablation resistance and the cracking resistance of the composite material; the thermal conductivity of the diamond is far higher than that of tungsten, the diamond is doped into the matrix of the composite material, the effect of improving the thermal conductivity can be achieved, the aim of quickly transferring energy of the composite material is fulfilled, and the artificial diamond is mature in manufacturing process and low in cost.
According to the invention, the silicon film is plated on the surface of the diamond, so that a SiC layer with stable chemical property and higher thermal conductivity can be formed on the surface of the diamond through silicon elements, and the combination between the diamond and a tungsten substrate can be changed from mechanical inlaying into stable chemical metallurgical combination, thereby improving the wettability and the bonding force of the diamond and W and improving the thermal conductivity of the composite material.
Detailed Description
The invention is further described below with reference to the following examples:
the various starting materials used in the following examples are all commercially available products known in the art unless otherwise specified.
Example 1
WfPreparation of/W alloy-diamond composite material
(1) Taking W powder, ZrC powder and Y2O3Powder is evenly mixed to obtain a mixture I, wherein the mass fraction of W powder in the mixture I is 99 percent, and ZrC and Y are2O3The mass fraction of the mixture I is 0.5 percent, then the mixture I is put into a corundum ball milling tank, absolute ethyl alcohol is added as a dispersing agent, ball milling is carried out for 40 hours under the condition that the ball milling rotating speed is 300r/min, and the mixture I is mechanically alloyed to prepare W alloy powder;
(2) w is to befPutting into concentrated nitric acid solution with concentration of 68% to react with WfPerforming surface corrosion, and after 2h, ultrasonically cleaning by absolute ethyl alcohol to remove WfThe impurities on the surface are remained to obtain W subjected to surface corrosionf，WfHas an average diameter of 150 μm;
(3) taking diamond particles, Si powder and anhydrous CaCl2Uniformly mixing to obtain a mixture II, wherein diamond particles, Si powder and anhydrous CaCl are contained in the mixture II2The mass ratio of the mixture II to the diamond particles is 1:1:4, and then the mixture II is subjected to heat preservation at 1150 ℃ for 40min, so that silicon coating layers with uniform surfaces can be prepared on the surfaces of the diamond particles, and the diamond particles with silicon films plated on the surfaces are obtained;
(4) taking W subjected to surface corrosionfW alloy powder and diamond particles coated with silicon film on the surface, wherein W subjected to surface corrosionfThe mass fraction of the W alloy powder is 20 percent, the mass fraction of the diamond particles with the silicon film plated on the surface is 2 percent, the balance is W alloy powder, the mixture is uniformly mixed and then put into a graphite die for sintering, the sintering process adopts discharge plasma sintering, the sintering temperature is 1700 ℃, the heat preservation pressure is 50MPa, and the heat preservation time is 2min, thus obtaining the W alloy powderfa/W alloy-diamond composite.
Example 2
WfPreparation of/W alloy-diamond composite material
(1) Taking W powder, ZrC powder and Y2O3Powder is evenly mixed to obtain a mixture I, wherein the mass fraction of W powder in the mixture I is 99 percent, and ZrC and Y are2O3The mass fraction of the mixture I is 0.5 percent, then the mixture I is put into a corundum ball milling tank, absolute ethyl alcohol is added as a dispersing agent, ball milling is carried out for 40 hours under the condition that the ball milling rotating speed is 300r/min, and the mixture I is mechanically alloyed to prepare W alloy powder;
(2) w is to befPutting into concentrated nitric acid solution with concentration of 68% to react with WfPerforming surface corrosion, and after 2h, ultrasonically cleaning by absolute ethyl alcohol to remove WfThe impurities on the surface are remained to obtain W subjected to surface corrosionf，WfHas an average diameter of 150 μm;
(3) taking diamond particles, Si powder and anhydrous CaCl2Uniformly mixing to obtain a mixture II, wherein diamond particles, Si powder and anhydrous CaCl are contained in the mixture II2The mass ratio of the mixture II to the diamond particles is 1:1:4, and then the mixture II is subjected to heat preservation at 1150 ℃ for 40min, so that silicon coating layers with uniform surfaces can be prepared on the surfaces of the diamond particles, and the diamond particles with silicon films plated on the surfaces are obtained;
(4) taking W subjected to surface corrosionfW alloy powder and diamond particles coated with silicon film on the surface, wherein WfThe mass fraction of the diamond particles is 30 percent, the mass fraction of the diamond particles with the silicon film plated on the surface is 3 percent, the balance is W alloy, the diamond particles are uniformly mixed and then placed into a graphite die for sintering, the sintering process adopts discharge plasma for sintering, the sintering treatment temperature is 1800 ℃, the heat preservation pressure is 50MPa, and the heat preservation time is 2min, thus obtaining the W alloyfa/W alloy-diamond composite.
Example 3
WfPreparation of/W alloy-diamond composite material
(1) Taking W powder, ZrC powder and Y2O3Powder is evenly mixed to obtain a mixture I, wherein the mass fraction of the W powder in the mixture I is 98.9 percent, the mass fraction of the ZrC is 0.1 percent, and the mass fraction of the Y powder in the mixture I is2O3The mass fraction of the mixture I is 1 percent, then the mixture I is put into a corundum ball milling tank, absolute ethyl alcohol is added as a dispersing agent, ball milling is carried out for 50 hours under the condition that the ball milling rotating speed is 200r/min, and the mixture I is mechanically alloyed to prepare W alloy powder;
(2) w is to befPutting into concentrated nitric acid solution with concentration of 68% to react with WfPerforming surface corrosion, and after 3h, ultrasonically cleaning by absolute ethyl alcohol to remove WfThe impurities on the surface are remained to obtain W subjected to surface corrosionf，WfHas an average diameter of 300 μm;
(3) taking diamond particlesGranules, Si powder and anhydrous CaCl2Uniformly mixing to obtain a mixture II, wherein diamond particles, Si powder and anhydrous CaCl are contained in the mixture II2The mass ratio of the mixture II to the diamond particles is 1:1:4, and then the mixture II is subjected to heat preservation at the high temperature of 1100 ℃ for 60min, so that silicon coating layers with uniform surfaces can be prepared on the surfaces of the diamond particles, and the diamond particles with silicon films plated on the surfaces are obtained;
(4) taking W subjected to surface corrosionfW alloy powder and diamond particles coated with silicon film on the surface, wherein WfThe mass fraction of the diamond particles is 10 percent, the mass fraction of the diamond particles with the silicon film plated on the surface is 4 percent, the balance is W alloy, the diamond particles are uniformly mixed and then placed into a graphite die for sintering, the sintering process adopts discharge plasma for sintering, the sintering treatment temperature is 1500 ℃, the heat preservation pressure is 60MPa, and the heat preservation time is 4min, thus obtaining the W alloyfa/W alloy-diamond composite.
Example 4
WfPreparation of/W alloy-diamond composite material
(1) Taking W powder, ZrC powder and Y2O3Powder is evenly mixed to obtain a mixture I, wherein the mass fraction of the W powder in the mixture I is 98.9 percent, the mass fraction of the ZrC is 1 percent, and the mass fraction of the Y powder in the mixture I is2O3The mass fraction of the mixture I is 0.1 percent, then the mixture I is put into a corundum ball milling tank, absolute ethyl alcohol is added as a dispersing agent, ball milling is carried out for 30 hours under the condition that the ball milling rotating speed is 400r/min, and the mixture I is mechanically alloyed to prepare W alloy powder;
(2) w is to befPutting into concentrated nitric acid solution with concentration of 68% to react with WfPerforming surface corrosion, and after 1h, ultrasonically cleaning with absolute ethyl alcohol to remove WfThe impurities on the surface are remained to obtain W subjected to surface corrosionf，WfHas an average diameter of 30 μm;
(3) taking diamond particles, Si powder and anhydrous CaCl2Uniformly mixing to obtain a mixture II, wherein diamond particles, Si powder and anhydrous CaCl are contained in the mixture II2The mass ratio of the silicon-based alloy and the diamond particles is 1:1:4, then the mixture II is subjected to heat preservation at the high temperature of 1200 ℃ for 30min, and then the silicon coating layer with uniform surface can be prepared on the surfaces of the diamond particles to obtain the surface coatingDiamond particles having a silicon film;
(4) taking W subjected to surface corrosionfW alloy powder and diamond particles coated with silicon film on the surface, wherein WfThe mass fraction of the W is 5%, the mass fraction of the diamond particles with the silicon film plated on the surface is 1%, the balance is W alloy, the diamond particles are uniformly mixed and then placed into a graphite die for sintering, the sintering process adopts discharge plasma sintering, the sintering treatment temperature is 1600 ℃, the heat preservation pressure is 20MPa, and the heat preservation time is 5min, so that the W is obtainedfa/W alloy-diamond composite.
Example 5
WfPreparation of/W alloy-diamond composite material
(1) Taking W powder, ZrC powder and Y2O3Powder is evenly mixed to obtain a mixture I, wherein the mass fraction of the W powder in the mixture I is 98.8 percent, the mass fraction of the ZrC is 0.4 percent, and the mass fraction of the Y powder in the mixture I is2O3The mass fraction of the mixture I is 0.8 percent, then the mixture I is put into a corundum ball milling tank, absolute ethyl alcohol is added as a dispersing agent, ball milling is carried out for 35 hours under the condition that the ball milling rotating speed is 300r/min, and the mixture I is mechanically alloyed to prepare W alloy powder;
(2) w is to befPutting into concentrated nitric acid solution with concentration of 68% to react with WfPerforming surface corrosion, and after 2h, ultrasonically cleaning by absolute ethyl alcohol to remove WfThe impurities on the surface are remained to obtain W subjected to surface corrosionf，WfHas an average diameter of 100 μm;
(3) taking diamond particles, Si powder and anhydrous CaCl2Uniformly mixing to obtain a mixture II, wherein diamond particles, Si powder and anhydrous CaCl are contained in the mixture II2The mass ratio of the mixture II to the diamond particles is 1:1:4, and then the mixture II is subjected to heat preservation at the high temperature of 1100 ℃ for 50min, so that silicon coating layers with uniform surfaces can be prepared on the surfaces of the diamond particles, and the diamond particles with silicon films plated on the surfaces are obtained;
(4) taking W subjected to surface corrosionfW alloy powder and diamond particles coated with silicon film on the surface, wherein WfIs 15 percent, the mass fraction of the diamond particles with the silicon film plated on the surface is 0.5 percent, the balance is W alloy, and the components are mixedUniformly placing the mixture into a graphite mold for sintering, sintering by adopting discharge plasma in the sintering process, wherein the sintering treatment temperature is 1600 ℃, the heat preservation pressure is 40MPa, and the heat preservation time is 3min to obtain Wfa/W alloy-diamond composite.
Example 6
WfPerformance testing of/W alloy-diamond composite materials
According to ASTM E1461-13 Standard test method for thermal diffusivity by flash light, for WfThe room temperature thermal conductivity of the/W alloy-diamond composite material was tested, the obtained results are shown in Table 1, and the results show that W isfCompared with pure W (150W/m.K), the thermal conductivity of the/W alloy-diamond composite material is obviously improved, and the thermal conductivity of the composite material is obviously improved.
According to the national standard GB/T229-2007 method for testing charpy pendulum impact of metal materials, for WfThe ductile-to-brittle transition temperature (DBTT) of the/W alloy-diamond composite was tested and the results are shown in Table 1. The results show WfCompared with pure W, the DBTT of the/W alloy-diamond composite material is obviously reduced, and the toughness of the composite material is obviously improved.
TABLE 1WfPerformance test results of/W alloy-diamond composite material
It should be understood that the examples and embodiments described herein are for illustrative purposes only and are not intended to limit the scope of the present disclosure, and that various modifications or changes in light thereof will be suggested to persons skilled in the art and are to be included within the spirit and purview of this disclosure.
Claims (5)
1. Wfthe/W alloy-diamond composite material is characterized in that: the raw material comprises WfW alloy and diamond coated with silicon film on surface, WfIndicating tungsten fibresVitamin, WfThe diameter of (a) is 30-300 mu m; the W alloy consists of a matrix component W and a doping component, wherein the doping component comprises ZrC and Y2O3ZrC and Y in W alloy2O3The mass fraction of the components is 0.1-1%; in the raw materials, WfThe mass fraction of the diamond is 10-30%, the mass fraction of the diamond with the silicon film plated on the surface is 2-4%, and the balance is W alloy;
w isfthe/W alloy-diamond composite material comprises the following steps:
(1) preparation of W alloy
According to the composition of W alloy, respectively taking out the powder raw materials of each component, and then preparing W alloy powder in a mechanical alloying mode;
(2)Wfsurface treatment of
By using concentrated nitric acid solution to WfPerforming surface etching treatment, and cleaning to remove WfThe impurities on the surface are remained to obtain W subjected to surface corrosionf；
(3) Surface silicon plating treatment of diamond
Mixing diamond particles, Si powder and anhydrous CaCl2Mixing, and carrying out heat preservation treatment at high temperature to obtain diamond particles with silicon films plated on the surfaces;
the sequence of the steps (1), (2) and (3) is not limited;
(4) composite powder pressing and sintering
Respectively taking out the W subjected to surface corrosionfMixing the W alloy powder and the diamond particles with the silicon film plated on the surface uniformly, putting the mixture into a graphite die, and sintering by adopting a spark plasma sintering process to obtain Wfa/W alloy-diamond composite.
2. W according to claim 1fthe/W alloy-diamond composite material is characterized in that: in the step (1), mechanical alloying is realized by ball milling in a ball mill, the ball milling speed is 200-400 r/min, and the ball milling time is 30-50 h.
3. W according to claim 1 or 2fAlloy-diamondA composite material characterized by: in the step (2), concentrated nitric acid is used for treating WfThe treatment time is 1-3 h.
4. W according to claim 1 or 2fthe/W alloy-diamond composite material is characterized in that: in the step (3), the diamond particles, the Si powder and the anhydrous CaCl2The mass ratio of the components is 1:1:4, the temperature of the heat preservation treatment at high temperature is 1100-1200 ℃, and the time is 30-60 min.
5. W according to claim 1 or 2fthe/W alloy-diamond composite material is characterized in that: in the step (4), the sintering treatment temperature is 1500-1800 ℃, the pressure is 20-60 MPa, and the time is 2-5 min.
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