CN108380875B - It is a kind of with highly thermally conductive tungsten-plating tungsten diamond composite and preparation method thereof - Google Patents
It is a kind of with highly thermally conductive tungsten-plating tungsten diamond composite and preparation method thereof Download PDFInfo
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- CN108380875B CN108380875B CN201810203246.7A CN201810203246A CN108380875B CN 108380875 B CN108380875 B CN 108380875B CN 201810203246 A CN201810203246 A CN 201810203246A CN 108380875 B CN108380875 B CN 108380875B
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 79
- 239000010937 tungsten Substances 0.000 title claims abstract description 79
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 62
- 239000010432 diamond Substances 0.000 title claims abstract description 62
- 238000007747 plating Methods 0.000 title claims abstract description 49
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011812 mixed powder Substances 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 2
- 239000004575 stone Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 20
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000004927 fusion Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 229910052722 tritium Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
-
- B22F1/0003—
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C26/00—Alloys containing diamond or cubic or wurtzitic boron nitride, fullerenes or carbon nanotubes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
-
- 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
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacturing & Machinery (AREA)
- Carbon And Carbon Compounds (AREA)
- Cooling Or The Like Of Semiconductors Or Solid State Devices (AREA)
- Ceramic Products (AREA)
Abstract
The invention discloses a kind of with highly thermally conductive tungsten-plating tungsten diamond composite and preparation method thereof, wherein by tungsten and plating tungsten diamond, hybrid process is made the tungsten-plating tungsten diamond composite by volume, wherein the mass fraction of plating tungsten diamond is 2%-15%.The present invention is doped using plating tungsten diamond particles, and the presence for plating tungsten layer is more advantageous to diffusion between tungsten and carbon during the sintering process, so that the combination between diamond and tungsten basal body interface is more preferable, to obtain better heating conduction.Under the harsh heat load environment of reactor, it is possible to reduce the damage for the damage bring PFM that material is subject to and plasma pollution etc. influence.
Description
Technical field
It is specifically a kind of with highly thermally conductive tungsten-the present invention relates to a kind of tungsten-based composite material and preparation method
Plate tungsten diamond composite and preparation method thereof.
Background technique
With the development of human society, the demand to the energy increasingly increases, fusion energy caused by light atom fusion reaction
It is likely to become the energy problem that the effective solution mankind face.Tokamak device (Tokamak) is most possible so far
The device of successful controllable thermonuclear fusion.But especially facing plasma material (PFM) subjects fusion in fusion facility
The neutron irradiation for reacting bring high H and He ionic flux and high-energy influences, while directly contacting with edge plasma,
A large amount of thermal energy, high energy particle, electromagnetic radiation release can make facing plasma material cause serious surface damage, calorifics and
Mechanical properties decrease, the service life of material will receive further influence.Therefore there are very high requirement, tungsten to the performance of material
Have the characteristics that high-melting-point (3410 DEG C), low physical sputtering rate, low tritium be detained, low swelling, it is considered to be it is most potential to be used as the
The candidate material of one wall.
However tungsten sill also faces many problems under real reaction heap environment, PFM will be exposed to stable state thermic load
Under the transient state thermic load of several types.These strong thermic loads may cause crackle, surface melting, evaporation, drop injection
And fatigue fracture, this may cause the damage of PFM and plasma pollution.So need material that there is high thermal conductivity, and one
As strengthen tungsten sill method be added into tungsten basal body the second phase (such as rare earth oxide and carbide) material is carried out it is strong
Change, but can not all improve the thermal conductivity of tungsten sill, the thermal conductivity of material can be reduced instead.Diamond has excellent due to itself
Different heating conduction, be doped into tungsten basal body can raising material by a relatively large margin thermal conductivity, reduce tungsten sill in height
Heat load environment under damage.
Summary of the invention
The present invention is intended to provide a kind of with highly thermally conductive tungsten-plating tungsten diamond composite and preparation method thereof.By
Tungsten-plating tungsten diamond composite thermal conductivity of sintering preparation is significantly improved compared with pure tungsten.
The present invention has highly thermally conductive tungsten-plating tungsten diamond composite, is mixed by volume by tungsten and plating tungsten diamond
Conjunction is processed into, wherein the mass fraction of plating tungsten diamond is 2%-15%.
The present invention has highly thermally conductive tungsten-plating tungsten diamond composite preparation method, includes the following steps:
Step 1: powder processed
Pure tungsten powder and plating tungsten diamond are uniformly mixed in 300 revs/min of mixed powder machine, obtain mixed powder;
In step 1, the purity of the pure tungsten powder is 99.9%, and granularity is 1.0-1.3 μm;Plate the average particle size of tungsten diamond
It is 300 μm, plates tungsten layer with a thickness of 200-300nm.
Step 2: sintering
The mixed powder that step 1 is obtained is put into graphite jig, then mold is put into discharge plasma sintering furnace, furnace
Chamber vacuumizes at room temperature, then heats to 1600 DEG C and keeps the temperature 3min, and room temperature is down to after heat preservation to get tungsten-plating tungsten is arrived
Diamond composite.
In step 2, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
Pressure, which is controlled, in step 2, in sintering process is no more than 50MPa.
The beneficial effects of the present invention are embodied in:
Diamond itself has high thermal conductivity (1500W/mK), the remote extraordinary highly heat-conductive material seen such as copper
Material conducts heat is greatly improved into Copper substrate by diamond doped already in the research of heat sink material in (400W/mK)
Performance, therefore the present invention is by the diamond doped heating conduction for improving material in tungsten (160W/mK).The present invention is using plating tungsten
Diamond particles are doped, and the presence for plating tungsten layer is more advantageous to diffusion between tungsten and carbon during the sintering process, so that Buddha's warrior attendant
Combination between stone and tungsten basal body interface is more preferable, to obtain better heating conduction.It, can under the harsh heat load environment of reactor
It is influenced with damage and the plasma pollution etc. that reduce the damage bring PFM that material is subject to.
Detailed description of the invention
Fig. 1 is the shape appearance figure for plating tungsten diamond particles, has plated one layer of tungsten on the surface of diamond particles as can be seen from Figure 1
Coating.
Fig. 2 is the fracture apperance figure after Composite Sintering, and plating tungsten diamond particles are in tungsten basal body after being sintered as can be seen from Figure 2
In be evenly distributed, the interface cohesion between tungsten basal body is preferable, without apparent hole and gap.
Fig. 3 is the linear sweep graph plated at tungsten diamond particles and tungsten basal body linkage interface, is sent out as can be seen from Figure 3 in interface
The phase counterdiffusion between wolfram element and carbon has been given birth to, W is formedXCXSubstance promotes the combination between interface.
Fig. 4 is the thermal coefficient of different quality containing composite material, plates the doping of tungsten diamond particles as can be seen from Figure 4
Improve the heating conduction of tungsten sill.
Specific embodiment
Embodiment 1:
There is highly thermally conductive tungsten-plating tungsten diamond composite in the present embodiment, be by tungsten and plating tungsten diamond by volume
It is made than hybrid process, wherein the mass fraction of plating tungsten diamond is 2%.The purity of pure tungsten powder is 99.9%, granularity 1.0-
1.3μm;The average particle size for plating tungsten diamond is 300 μm, and diamond particles are bought from Henan Huanghe Xuanfeng Co., Ltd., plating
Tungsten layer is completed in Guangdong University of Technology, with a thickness of 200-300nm.
In the present embodiment have highly thermally conductive tungsten-plating tungsten diamond composite the preparation method is as follows:
1, powder processed: pure tungsten powder and plating tungsten diamond being stirred 2 hours in 300 revs/min of mixed powder machine, are uniformly mixed,
Obtain mixed powder;
2, be sintered: the mixed powder that step 1 is obtained is put into graphite jig, then mold is put into discharge plasma sintering
In furnace, furnace chamber vacuumizes at room temperature, is warming up to 1600 DEG C through 16min with the heating rate of 100 DEG C/min, keeps the temperature 3min, then
Room temperature is dropped to the rate of temperature fall of 100 DEG C/min, control pressure is no more than 50MPa to get multiple to tungsten-plating tungsten diamond in sintering
Condensation material.
Diamond particles are evenly distributed in composite material after sintering, and material thermal conductivity reaches 173.1W/mK, higher than pure W's
160W/mK, also above homogenous quantities score without coating tungsten-diamond composite 164.3W/mK.
Embodiment 2:
There is highly thermally conductive tungsten-plating tungsten diamond composite in the present embodiment, be by tungsten and plating tungsten diamond by volume
It is made than hybrid process, wherein the mass fraction of plating tungsten diamond is 5%.The purity of pure tungsten powder is 99.9%, granularity 1.0-
1.3μm;The average particle size for plating tungsten diamond is 300 μm, and diamond particles are bought from Henan Huanghe Xuanfeng Co., Ltd., plating
Tungsten layer is completed in Guangdong University of Technology, with a thickness of 200-300nm.
In the present embodiment have highly thermally conductive tungsten-plating tungsten diamond composite the preparation method is as follows:
1, powder processed: pure tungsten powder and plating tungsten diamond being stirred 2 hours in 300 revs/min of mixed powder machine, are uniformly mixed,
Obtain mixed powder;
2, be sintered: the mixed powder that step 1 is obtained is put into graphite jig, then mold is put into discharge plasma sintering
In furnace, furnace chamber vacuumizes at room temperature, is warming up to 1600 DEG C through 16min with the heating rate of 100 DEG C/min, keeps the temperature 3min, then
Room temperature is dropped to the rate of temperature fall of 100 DEG C/min, control pressure is no more than 50MPa to get multiple to tungsten-plating tungsten diamond in sintering
Condensation material.
Diamond particles are evenly distributed in composite material after sintering, and material thermal conductivity reaches 222.8W/mK, higher than pure W's
160W/mK, also above homogenous quantities score without coating tungsten-diamond composite 169.3W/mK.
Embodiment 3:
There is highly thermally conductive tungsten-plating tungsten diamond composite in the present embodiment, be by tungsten and plating tungsten diamond by volume
It is made than hybrid process, wherein the mass fraction of plating tungsten diamond is 15%.The purity of pure tungsten powder is 99.9%, granularity 1.0-
1.3μm;The average particle size for plating tungsten diamond is 300 μm, and diamond particles are bought from Henan Huanghe Xuanfeng Co., Ltd., plating
Tungsten layer is completed in Guangdong University of Technology, with a thickness of 200-300nm.
In the present embodiment have highly thermally conductive tungsten-plating tungsten diamond composite the preparation method is as follows:
1, powder processed: pure tungsten powder and plating tungsten diamond being stirred 2 hours in 300 revs/min of mixed powder machine, are uniformly mixed,
Obtain mixed powder;
2, be sintered: the mixed powder that step 1 is obtained is put into graphite jig, then mold is put into discharge plasma sintering
In furnace, furnace chamber vacuumizes at room temperature, is warming up to 1600 DEG C through 16min with the heating rate of 100 DEG C/min, keeps the temperature 3min, then
Room temperature is dropped to the rate of temperature fall of 100 DEG C/min, control pressure is no more than 50MPa to get multiple to tungsten-plating tungsten diamond in sintering
Condensation material.
Diamond particles are evenly distributed in composite material after sintering, and material thermal conductivity reaches 241.5W/mK, higher than pure W's
160W/mK, also above homogenous quantities score without coating tungsten-diamond composite 166.7W/mK.
Claims (4)
1. a kind of with highly thermally conductive tungsten-plating tungsten diamond composite preparation method, it is characterised in that include the following steps:
Step 1: powder processed
Pure tungsten powder and plating tungsten diamond are uniformly mixed in 300 revs/min of mixed powder machine, obtain mixed powder, wherein
The mass fraction for plating tungsten diamond is 2%-15%;
Step 2: sintering
The mixed powder that step 1 is obtained is put into graphite jig, then mold is put into discharge plasma sintering furnace, and furnace chamber exists
It vacuumizes at room temperature, then heat to 1600 DEG C and keeps the temperature 3min, room temperature is down to after heat preservation to get tungsten-plating tungsten Buddha's warrior attendant is arrived
Stone composite material.
2. preparation method according to claim 1, it is characterised in that:
In step 1, the purity of the pure tungsten powder is 99.9%, and granularity is 1.0-1.3 μm;Plating tungsten diamond average particle size be
300 μm, tungsten layer is plated with a thickness of 200-300nm.
3. preparation method according to claim 1, it is characterised in that:
In step 2, heating rate is 100 DEG C/min, and rate of temperature fall is 100 DEG C/min.
4. preparation method according to claim 1, it is characterised in that:
Pressure, which is controlled, in step 2, in sintering process is no more than 50MPa.
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CN201810203246.7A CN108380875B (en) | 2018-03-13 | 2018-03-13 | It is a kind of with highly thermally conductive tungsten-plating tungsten diamond composite and preparation method thereof |
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CN109175354B (en) * | 2018-10-29 | 2020-09-04 | 合肥工业大学 | Preparation method of diamond/W-Cu composite material |
CN110846596B (en) * | 2019-12-12 | 2021-09-07 | 中国科学院合肥物质科学研究院 | Wf/W alloy-diamond composite material and preparation method thereof |
CN116005026B (en) * | 2022-10-28 | 2024-07-09 | 北京科技大学 | Method for preparing high-density tungsten/diamond composite material by low-temperature sintering |
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