CN113953510A - 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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- CN113953510A CN113953510A CN202111236657.4A CN202111236657A CN113953510A CN 113953510 A CN113953510 A CN 113953510A CN 202111236657 A CN202111236657 A CN 202111236657A CN 113953510 A CN113953510 A CN 113953510A
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 52
- 239000010937 tungsten Substances 0.000 title claims abstract description 52
- 239000000835 fiber Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 238000005245 sintering Methods 0.000 claims abstract description 16
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 10
- 239000011148 porous material Substances 0.000 claims abstract description 6
- 238000009826 distribution Methods 0.000 claims abstract description 4
- 230000000694 effects Effects 0.000 claims abstract description 3
- 238000002490 spark plasma sintering Methods 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 5
- 239000011812 mixed powder Substances 0.000 claims 1
- 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 8
- 238000000280 densification Methods 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract 1
- 230000004927 fusion Effects 0.000 description 6
- 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
- 230000008859 change Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 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
- 238000010438 heat treatment 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 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
Images
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
-
- 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 and tungsten fibers by using a drum-type powder mixer, then carrying out densification by combining with an SPS sintering technology, and realizing regulation and control of the porosity and pore distribution in a Wf/W composite material sample by controlling mixing technological parameters and SPS sintering technological parameters and simultaneously by means of the cooperation of a current guide medium so as to realize optimization of toughening effect. 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
In the modern society, the energy demand of human beings is increasing day by day, and the development and the utilization of safe, pollution-free novel energy become the 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 concerned.
Nuclear fusion devices are subject to bombardment by high energy particles produced by the fusion reaction, using plasma-oriented materials (PFMs), which is one of the key challenges in achieving controlled nuclear fusion. Tungsten used as the first wall has the characteristic of intrinsic brittleness, faces the challenge of cracking failure under the fusion working condition, improves the brittleness behavior of W, and becomes a hot point of research. In addition, the first wall tungsten material is used in future nuclear fusion devices, and has certain requirements on the size, and the large-size preparation of the high-melting-point W material also becomes another challenge for the engineering application of the W material. Therefore, improving the toughness of W materials and realizing large-scale 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 brittle 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 technical scheme that: the method for preparing the large-size tungsten fiber toughened tungsten Wf/W composite material is characterized by mixing tungsten powder and tungsten fibers by using a drum mixer, then performing densification by combining an SPS sintering technology, and controlling the porosity and pore distribution in a large sample tissue of the Wf/W composite material by controlling the mixing technological parameters and the SPS sintering technological parameters.
The invention has the beneficial effects that: the invention introduces the current guide medium on the basis of the electric plasma sintering technology, can realize the preparation of sample materials with high efficiency and low cost, and effectively overcomes the prominent defect that the traditional sintering methods such as hot pressing sintering, hot isostatic pressing sintering, solid phase reaction method and the like are difficult to synthesize large-size samples.
The method adopted by the invention relates to the use of a current guide medium, and meanwhile, by controlling the preparation process, the material tissue can be independently designed and regulated by means of the displacement change curve of the electrode, the porosity and 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 a sintering principle of a method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite material according to the invention;
FIG. 2 is a plot of the physical dimensions of alloy samples prepared by a method for preparing large-size tungsten fiber toughened tungsten Wf/W composites;
FIG. 3 is a microstructure diagram of an alloy sample prepared by a method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite material.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention easier to understand by those skilled in the art, and thus will clearly and clearly define the scope of the invention.
Referring to fig. 1 and 2, an embodiment of the present invention includes:
the invention relates to a method for preparing a large-size tungsten fiber toughened tungsten (Wf/W) composite material, which can realize the preparation of a large-size tungsten and tungsten fiber composite material sample under specific temperature and pressure by adopting an electric spark plasma sintering technology and using large-size SPS equipment. A current guide medium is laid between the female die and the powder, so that a current surrounding layer is formed in the cavity, the current is promoted to pass through the upper pressure head, the sample and the lower pressure head, and the current action is realized in the whole cavity; meanwhile, heat is concentrated on the pressure head to realize the heating effect on the pressure head, the heat is transferred to the powder through the pressure head, the heat is concentrated on the powder, and the powder is sintered; the current guiding medium can be tungsten foil and graphite paper sprayed with BN; on the basis of considering that the graphite mold, the tungsten and tungsten fiber composite material sample and the volume of the electrode structure expand 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 pores are 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 sample prepared by the present invention has uniform pore size and uniform distribution.
The invention prepares a large-size tungsten and tungsten fiber composite material sample, wherein W represents a tungsten element, Wf represents a tungsten fiber, and the sample comprises the following components in percentage by mass:
60 wt% of W, 40 wt% of Wf, and the sizes of W and Wf are as follows: 105mm by 30mm, mass: 4500 g.
The invention adopts a spark plasma sintering technology, and tungsten fiber samples with higher toughness and larger size are prepared by a sintering process at specific temperature and pressure by using large-scale SPS equipment. The method specifically comprises the following steps:
1) taking tungsten powder and tungsten fibers (W:60 wt%, Wf:40 wt%) with certain mass, and mixing and ball-milling for 24 hours by using a drum mixer;
2) filling the mixed and ball-milled powder into a graphite die, filling tungsten foil and graphite paper sprayed with BN in a female die, and separating the powder from a pressure head by using carbon paper and the tungsten foil;
3) sintering the powder in the mould with a large SPS apparatus: the sintering temperature was 1500 ℃ and the applied pressure was 30 MPa.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (6)
1. A method for preparing a large-size tungsten fiber toughened tungsten Wf/W composite material is characterized by comprising the following steps:
mixing the W powder and the W fiber by a roller type powder mixer;
the SPS technology is used for densifying the mixed powder;
the porosity and pore distribution of the microstructure of a large-size Wf/W composite material sample are regulated and controlled by controlling the mixing process parameters and the SPS sintering process parameters and utilizing the cooperation effect of a current guide medium.
2. The method according to claim 1, characterized by comprising the steps of:
step 1: weighing tungsten powder and tungsten fibers with the purity of 99.5 percent according to a certain mass ratio under the Ar protective atmosphere, placing the tungsten powder and the tungsten fibers together with a ball-milling medium on a drum mixer for mixing, and regulating and controlling the mixing time to obtain a mixture of the tungsten and the tungsten fibers;
step 2: and (2) filling the mixture obtained in the step (1) into a graphite mold paved with a current guide medium, densifying the mixture under a vacuum condition by using an SPS (spark plasma sintering) technology, and preparing a large-size tungsten and tungsten fiber composite material sample by controlling applied pressure and sintering temperature.
3. The method of claim 1, wherein:
the regulation and control precision of the porosity in the tissue of the large-size Wf/W composite material sample is +/-1%.
4. The method of claim 2, wherein:
in the step 1, the content of tungsten and tungsten fiber in the mixture is respectively 60 wt% and 40 wt%.
5. The method of claim 2, wherein:
in step 1, the drum-type mixing time of the mixture is 24 hours.
6. The method of claim 2, wherein:
in step 2, the applied pressure is 30MPa, and the sintering temperature is 1500 ℃.
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 |
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| 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 |
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| CN113953510A true CN113953510A (en) | 2022-01-21 |
| CN113953510B CN113953510B (en) | 2023-12-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114959518A (en) * | 2022-05-30 | 2022-08-30 | 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)
| 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 |
-
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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114959518A (en) * | 2022-05-30 | 2022-08-30 | 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 |
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| CN113953510B (en) | 2023-12-29 |
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