CN113953510B - Method for preparing large-size tungsten fiber toughened tungsten Wf/W composite material - Google Patents
Method for preparing large-size tungsten fiber toughened tungsten Wf/W composite material Download PDFInfo
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- CN113953510B CN113953510B CN202111236657.4A CN202111236657A CN113953510B CN 113953510 B CN113953510 B CN 113953510B CN 202111236657 A CN202111236657 A CN 202111236657A CN 113953510 B CN113953510 B CN 113953510B
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- tungsten
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 58
- 239000010937 tungsten Substances 0.000 title claims abstract description 58
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 239000000835 fiber Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 6
- 239000011148 porous material Substances 0.000 claims abstract description 6
- 238000009826 distribution Methods 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 238000006073 displacement reaction Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 5
- 230000001681 protective effect Effects 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 6
- 238000005457 optimization Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 12
- 230000004927 fusion Effects 0.000 description 6
- 238000002490 spark plasma sintering Methods 0.000 description 6
- 230000001276 controlling effect Effects 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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
- 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
Abstract
The invention discloses a method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite material, which comprises the steps of mixing tungsten powder with tungsten fibers by adopting a roller-type powder mixer, then compacting by combining an SPS sintering technology, and realizing regulation and control of porosity and pore distribution in a Wf/W composite material sample by controlling mixing technological parameters and SPS sintering technological parameters and simultaneously realizing optimization of toughening effect by means of the cooperation of current guiding mediums. Through the mode, the method can effectively improve the brittleness of the tungsten material, realize effective toughening of the tungsten material, break through the large-size preparation technology of the Wf/W composite material and realize engineering application.
Description
Technical Field
The invention relates to the field of preparation of tungsten-based composite materials and performance improvement thereof, in particular to a method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite material.
Background
Today's society, the energy demand of human beings is increasing, and the development and utilization of new energy sources that are safe and pollution-free is becoming a focus of human beings. The nuclear fusion energy has the characteristics of no nuclear waste, no long-term radioactivity, greenness, high energy density and the like, and is widely paid attention to.
Nuclear fusion devices are bombarded with plasma-facing materials (PFMs) that are subject to energetic particle bombardment by fusion reactions, which is one of the key challenges in achieving controlled nuclear fusion. As the tungsten for the first wall has the characteristic of intrinsic brittleness, the tungsten can face the challenge of cracking and failure under the fusion working condition, and the brittle behavior of the tungsten is improved, so that the tungsten becomes a research hot spot. In addition, the first wall tungsten material is used in a future nuclear fusion device, and has certain requirements on the size, and the large-size preparation of the high-melting-point W material also becomes another challenge of W material engineering application. Therefore, improving toughness of the W material and realizing large-size preparation thereof are a breakthrough technology.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite material, which can obviously improve the brittleness behavior of the tungsten material at high temperature, realize effective toughening of the tungsten material, break through the large-size preparation technology of the Wf/W composite material and realize engineering application.
In order to solve the technical problems, the invention adopts the following technical scheme: the method for preparing the large-size tungsten fiber toughened tungsten Wf/W composite material comprises the steps of mixing tungsten powder with tungsten fibers by adopting a roller mixer, then densifying by combining an SPS sintering technology, and regulating and controlling the porosity and pore distribution in a large sample structure of the Wf/W composite material by controlling mixing technological parameters and SPS sintering technological parameters.
The beneficial effects of the invention are as follows: according to the invention, the current guiding medium is introduced on the basis of the electric plasma sintering technology, so that the sample material can be prepared with high efficiency and low cost, and the outstanding defect that large-size samples are difficult to synthesize by the traditional sintering methods such as hot pressing sintering, hot isostatic pressing sintering, solid phase reaction method and the like is effectively overcome.
The method disclosed by the invention relates to the use of a current guiding medium, and simultaneously, by controlling the preparation process, the self-design and regulation of material organization can be realized by means of the displacement change curve of the electrode, the porosity and the pore distribution of the Wf/W composite material are adjusted, and the composite material has higher toughness.
Drawings
FIG. 1 is a schematic diagram of the sintering principle of a method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite material;
FIG. 2 is an external dimension diagram of an alloy sample prepared by a method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite material;
FIG. 3 is a microstructure view of an alloy sample prepared by a method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making clear and defining the scope of the present invention.
Referring to fig. 1 and 2, an embodiment of the present invention includes:
the invention discloses a method for preparing a large-size tungsten fiber toughened tungsten (Wf/W) composite material, which can prepare a large-size tungsten and tungsten fiber composite material sample at a specific temperature and pressure, adopts an electric spark plasma sintering technology, adopts large SPS as equipment, synthesizes the tungsten and tungsten fiber composite material by the method, enhances the toughness of the material, and can make the size of the sample large. By laying a current guiding medium between the female die and the powder, the cavity forms a current surrounding layer, current is caused to pass through the upper pressure head, the sample and the lower pressure head, and the current effect is realized in the whole cavity; meanwhile, heat is concentrated on the pressure head, so that the heating effect of the pressure head is realized, the heat is transferred to the powder through the pressure head, the heat is concentrated on the powder, and the powder is sintered; wherein the current guiding medium can be tungsten foil or graphite paper sprayed with BN; on the basis of considering expansion of the graphite mold, the tungsten and tungsten fiber composite material sample and the volume of the electrode structure along with the temperature rise, the compact shrinkage degree of the sample can be accurately judged according to the displacement change curve of the electrode, and the accurate regulation and control of the sample pore is realized according to the actual compact shrinkage condition of the sample, wherein the regulation and control precision is +/-1%; as can be seen from fig. 3, the samples prepared by the present invention have uniform pore sizes and uniform distribution.
The invention prepares a large-size tungsten and tungsten fiber composite material sample, wherein W represents tungsten element, wf represents tungsten fiber, and the components thereof comprise the following components in percentage by mass:
w is 60wt%, wf is 40wt%, and the size is: 105mm 30mm, mass: 4500g.
The invention adopts a spark plasma sintering technology, and the tungsten and tungsten fiber samples with higher toughness and larger size are prepared by mixing the powder and then sintering the powder by using a large SPS device at a specific temperature and pressure. The method specifically comprises the following steps:
1) Taking tungsten powder and tungsten fiber (W: 60wt%, wf:40 wt%) of a certain mass, and mixing and ball milling for 24 hours by adopting a roller mixer;
2) Filling the powder after mixed ball milling into a graphite mold, filling tungsten foil and BN sprayed graphite paper in a female mold, and separating the powder from a pressing head by using carbon paper and tungsten foil;
3) Sintering the powder in the mold with a large SPS apparatus: the sintering temperature was 1500℃and the applied pressure was 30MPa.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related technical fields are included in the scope of the present invention.
Claims (2)
1. A method of preparing a large-size tungsten fiber toughened tungsten Wf/W composite, comprising:
step 1, under Ar protective atmosphere, weighing tungsten powder and tungsten fibers with the purity of 99.5% according to a certain mass ratio, and placing the tungsten powder and the tungsten fibers and a ball milling medium on a roller mixer for mixing, wherein the roller mixing time of the mixture is 24 hours, so as to obtain a mixture of tungsten and tungsten fibers;
step 2, filling the mixture obtained in the step 1 into a graphite mold paved with a current guiding medium, densifying the mixture under a vacuum condition by utilizing SPS technology, applying pressure of 30Mpa and sintering temperature of 1500 ℃ to prepare a large-size tungsten and tungsten fiber composite material sample;
forming a current surrounding layer by utilizing the coordination effect of a current guiding medium, so that current is promoted to pass through an upper pressure head, a sample and a lower pressure head, and the current effect is realized in the whole cavity; meanwhile, heat is concentrated on the pressure head, so that the heating effect of the pressure head is realized, the heat is transferred to the powder through the pressure head, the heat is concentrated on the powder, and the powder is sintered; the micro-structure porosity and pore distribution of the large-size Wf/W composite material sample are regulated and controlled, and the porosity regulation and control precision in the large-size Wf/W composite material sample tissue is controlled to be +/-1% by means of the displacement change curve of the electrode.
2. The method according to claim 1, characterized in that:
in step 1, the tungsten and tungsten fibers content in the mixture were 60wt% and 40wt%, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111236657.4A CN113953510B (en) | 2021-10-23 | 2021-10-23 | Method for preparing large-size tungsten fiber toughened tungsten Wf/W composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111236657.4A CN113953510B (en) | 2021-10-23 | 2021-10-23 | Method for preparing large-size tungsten fiber toughened tungsten Wf/W composite material |
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| Publication Number | Publication Date |
|---|---|
| CN113953510A CN113953510A (en) | 2022-01-21 |
| CN113953510B true CN113953510B (en) | 2023-12-29 |
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| CN202111236657.4A Active CN113953510B (en) | 2021-10-23 | 2021-10-23 | Method for preparing large-size tungsten fiber toughened tungsten Wf/W composite material |
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| CN114959518B (en) * | 2022-05-30 | 2023-01-31 | 合肥工业大学智能制造技术研究院 | Tungsten fiber and oxide nanoparticle synergistic toughening tungsten-based composite material and preparation method thereof |
Citations (7)
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|---|---|---|---|---|
| JP2000096180A (en) * | 1998-09-25 | 2000-04-04 | Toshiba Corp | Tungsten and molybdenum fiber reinforced composite, its production, and part for high temperature service using the composite |
| CN101117672A (en) * | 2007-09-18 | 2008-02-06 | 武汉理工大学 | Activated sintering preparation method of fine crystalline non-magnetic wolfram-copper alloy |
| RU2010140724A (en) * | 2010-10-06 | 2012-04-20 | ФЕДЕРАЛЬНОЕ ГОСУДАРСТВЕННОЕ УЧРЕЖДЕНИЕ РОССИЙСКИЙ НАУЧНЫЙ ЦЕНТР "Курчатовский институт" (RU) | METHOD FOR PRODUCING NANODISPERSED POWDERS IN MICROWAVE DISCHARGE PLASMA AND DEVICE FOR ITS IMPLEMENTATION |
| CN110438357A (en) * | 2019-09-17 | 2019-11-12 | 合肥工业大学 | A method of quickly preparing homogeneous texture tungsten alloy |
| CN110846596A (en) * | 2019-12-12 | 2020-02-28 | 中国科学院合肥物质科学研究院 | Wf/W alloy-diamond composite material and preparation method thereof |
| CN112030026A (en) * | 2020-08-31 | 2020-12-04 | 合肥工业大学 | Preparation method of high-hardness and high-density composite rare earth oxide doped tungsten-based composite material |
| CN113523273A (en) * | 2021-06-17 | 2021-10-22 | 北京科技大学 | Powder metallurgy method for rapidly preparing ultrafine crystal pure tungsten material under multi-field coupling |
-
2021
- 2021-10-23 CN CN202111236657.4A patent/CN113953510B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000096180A (en) * | 1998-09-25 | 2000-04-04 | Toshiba Corp | Tungsten and molybdenum fiber reinforced composite, its production, and part for high temperature service using the composite |
| CN101117672A (en) * | 2007-09-18 | 2008-02-06 | 武汉理工大学 | Activated sintering preparation method of fine crystalline non-magnetic wolfram-copper alloy |
| RU2010140724A (en) * | 2010-10-06 | 2012-04-20 | ФЕДЕРАЛЬНОЕ ГОСУДАРСТВЕННОЕ УЧРЕЖДЕНИЕ РОССИЙСКИЙ НАУЧНЫЙ ЦЕНТР "Курчатовский институт" (RU) | METHOD FOR PRODUCING NANODISPERSED POWDERS IN MICROWAVE DISCHARGE PLASMA AND DEVICE FOR ITS IMPLEMENTATION |
| CN110438357A (en) * | 2019-09-17 | 2019-11-12 | 合肥工业大学 | A method of quickly preparing homogeneous texture tungsten alloy |
| CN110846596A (en) * | 2019-12-12 | 2020-02-28 | 中国科学院合肥物质科学研究院 | Wf/W alloy-diamond composite material and preparation method thereof |
| CN112030026A (en) * | 2020-08-31 | 2020-12-04 | 合肥工业大学 | Preparation method of high-hardness and high-density composite rare earth oxide doped tungsten-based composite material |
| CN113523273A (en) * | 2021-06-17 | 2021-10-22 | 北京科技大学 | Powder metallurgy method for rapidly preparing ultrafine crystal pure tungsten material under multi-field coupling |
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| CN113953510A (en) | 2022-01-21 |
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