CN105039876B - Preparation method for W-Cu composite materials of fiber and particle hybrid structure - Google Patents

Preparation method for W-Cu composite materials of fiber and particle hybrid structure Download PDF

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CN105039876B
CN105039876B CN201510390722.7A CN201510390722A CN105039876B CN 105039876 B CN105039876 B CN 105039876B CN 201510390722 A CN201510390722 A CN 201510390722A CN 105039876 B CN105039876 B CN 105039876B
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powder
fiber
tailings
hot pressing
preparation
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CN105039876A (en
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梁淑华
李阳
张乔
李向阳
李玉春
邹军涛
卓龙超
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Xian University of Technology
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Xian University of Technology
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Abstract

The invention provides a preparation method for W-Cu composite materials of a fiber and particle hyrid structure. Particularly, W powder and Cu powder hyrid evenly and a W fiber net obtained after acid pickling are laid in a cold pressing mold in a layered mode and then subjected to pre-pressing and pressure maintenance to obtain a composite material green body; then the green body is put in to a mold capable of being pressurized and subjected to hot pressing in an atmosphere protection hot pressing furnace; and finally, the composite material green body obtained after hot pressing is subjected to copper cementation in a high-temperature atmosphere sintering furnace, so that the W-Cu composite materials of the fiber and particle hyrid structure are obtained. The two-dimensional W fiber net is added in the preparation process of a W-Cu pseudo alloy W framework. The two-dimensional W fiber net and the W-Cu pseudo alloy W framework form metallurgical bonding through processing of an interface of fibers and the W framework and reasonable technological parameters, the W fiber net has a function like reinforcing ribs for the W framework, and therefore the high-temperature strength of the composite materials is obviously improved.

Description

A kind of preparation method of fiber and confusion structure Cu tailings
Technical field
The invention belongs to technical field of composite preparation, is related to a kind of fiber and confusion structure Cu tailings Preparation method.
Background technology
To adapt to the requirement of the continuous development of electricity market, the high-tension switch gear of China towards high voltage, Large Copacity, The direction of miniaturization is developed.New chopper capacity constantly will increase, and the space of arc-chutes then constantly reduces, so that Obtain the load undertaken in arcing contact unit area constantly to increase;Meanwhile, in order to reduce maintenance cost, to the life requirements of contact but It is increasingly longer, it is desirable to contact material not only has excellent arc ablation resistance performance, and there should be excellent high temperature strong Degree.In traditional technique, the space of the elevated temperature strength and arc ablation resistance characteristic of collaboration raising contact material is very limited, such as strong Change sintering, addition third element of W skeleton etc., although contact material arc ablation resistance characteristic can be improved, but in many frequencys After cut-offfing, as powder is random sintering, it is difficult to accomplish complete continuous framing structure, cause the strong of W skeleton after ablation Degree is inadequate, so as to increase ablation and abrasion.
The content of the invention
It is an object of the invention to provide the preparation method of a kind of fiber and confusion structure Cu tailings, by Add fiber reinforcement in copper-tungsten and mutually form fiber and confusion structure, realize that multiphase is strengthened so as to improve copper tungsten composite wood The elevated temperature strength of material.
The technical solution adopted in the present invention is, the preparation side of a kind of fiber and confusion structure Cu tailings Method, specifically implements according to the following steps:
Step 1, prepares composite green compact:
By the tungsten fiber net of the W powder and Cu powder of mix homogeneously and pickling in the cold stamping die place Min layers cloth, which is carried out Pre-stamped, pressurize, obtains composite green compact;
Step 2, hot pressing:
The green compact that step 1 is obtained are mounted in can be in pressurizing mold, and in atmosphere protection hot pressing furnace leading to hydrogen carries out hot pressing;
Step 3, infiltration:
Composite blank Jing after step 2 hot pressing in micro-computer controlled high-temperature hydrogen atmosphere sintering furnace is carried out oozing copper, Fiber and confusion structure Cu tailings are obtained.
The characteristics of of the invention, also resides in,
In step 1, W powder and Cu powder are respectively W powder 70%~90%, Cu powder 10%~30%, above group by mass percentage Mass percent sum is divided to be 100%.
Mix in step 1, specially:By W powder and Cu powder with 0.5~1:1 ratio of grinding media to material 400r/ in drum mixer Mix 6~8h under min rotating speeds.
Pickling in step 1, is tungsten fiber net to be cleaned with HF, removes the oxide-film on its surface.
In step 1, tungsten fiber net is formed by the tungsten fiber braiding of 40~60 μm of string diameter, and its specification is 30~100 mesh.
Pre-stamped in step 1 to require to be spaced 1~3mm for tungsten fiber net after compacting, precompressed pressing pressure is 200~400MPa, Dwell time is 30~90s.
Hot compression parameterses in step 2, specially:It is heated to after 920~970 DEG C with the firing rate of 15~25 DEG C/min, it is right Composite green compact carry out hot pressing under the pressure of 5~30MPa and are incubated 10~60min.
Infiltration parameter in step 3, specially:Heated with the firing rate of 15~25 DEG C/min, when temperature reaches When 1300~1350 DEG C, furnace cooling after 30~120min of insulation.
The invention has the beneficial effects as follows, the present invention adds two-dimentional tungsten fiber in the preparation process of copper tungsten pseudo-alloy W skeleton Net, by making both form metallurgical binding, Ran Houli with the process at W skeleton interface and the rational technological parameter of control fiber W skeleton and fiber are organically combined with follow-up infiltration process for copper, make fleece that similar reinforcement is played to W skeleton Effect so that the elevated temperature strength of composite is significantly improved.
Description of the drawings
Fig. 1 is the structural representation that the present invention prepares Cu tailings;
Fig. 2 is the interface micro-organization chart that the embodiment of the present invention 3 prepares fiber and W skeleton in Cu tailings;
Fig. 3 is the embodiment of the present invention 3 Cu tailings for preparing and the Cu tailings for being not added with fleece High temperature compressive stress-strain curve.
In figure, 1. tungsten fiber net, 2. tungsten copper mixed-powder.
Specific embodiment
The present invention is described in detail with reference to the accompanying drawings and detailed description.
The preparation method of a kind of fiber of the present invention and confusion structure Cu tailings, it is specifically real according to the following steps Apply:
Step 1, prepares composite green compact:
Weigh W powder 70%~90% by mass percentage respectively, Cu powder 10%~30%, above constituent mass percentage ratio it With for 100%, by W powder and Cu powder with 0.5~1:1 ratio of grinding media to material mixes 6~8h in drum mixer under 400r/min rotating speeds;
Mixed composite powder is sieved after the removal of impurity with the tungsten fiber net of pickling the place Min layers cloth in the cold stamping die, 1~3mm is spaced according to tungsten fiber net after compacting, pre-stamped, formation after 30~90s of pressurize is carried out to which under 200~400MPa Composite green compact.
Tungsten fiber net is formed by the tungsten fiber braiding of 40~60 μm of string diameter, and its specification is 30~100 mesh;Before place Min layers cloth Pickling is carried out to tungsten fiber net with HF, the oxide-film on its surface is removed.
Step 2, hot pressing:
The green compact that step 1 is obtained are mounted in can be in pressurizing mold, and in atmosphere protection hot pressing furnace leading to hydrogen carries out hot pressing:With After the firing rate of 15~25 DEG C/min is heated to 920~970 DEG C, composite green compact are carried out under the pressure of 5~30MPa Hot pressing is simultaneously incubated 10~60min.
Step 3, infiltration:
Composite blank Jing after step 2 hot pressing in micro-computer controlled high-temperature hydrogen atmosphere sintering furnace is carried out oozing copper: Heated with the firing rate of 15~25 DEG C/min, when temperature reaches 1300~1350 DEG C, insulation 30~120min after with Stove is cooled down, that is, obtain fiber and confusion structure Cu tailings, and its structure is as shown in Figure 1.
The preparation method of fiber of the present invention and confusion structure Cu tailings, in the system of copper tungsten pseudo-alloy W skeleton Two-dimentional tungsten fiber net is added during standby, both shapes are made by the process to fiber and W skeleton interface and rational technological parameter Into metallurgical binding, tungsten fiber net is made to play a part of similar reinforcement to W skeleton, so that its elevated temperature strength is significantly improved.
Embodiment 1
Step 1, prepares composite green compact:
Weigh W powder 70%, Cu powder 30% by mass percentage respectively, above constituent mass percentage ratio sum is 100%, will W powder and Cu powder are with 0.5:1 ratio of grinding media to material mixes 6h under 400r/min rotating speeds in drum mixer;
Mixed composite powder is sieved after the removal of impurity with the tungsten fiber net of pickling the place Min layers cloth in the cold stamping die, According to tungsten fiber net interval 2mm after compacting, and pre-stamped, formation composite green compact after pressurize 90s are carried out to its 200MPa.
Tungsten fiber net is formed by the tungsten fiber braiding of 60 μm of string diameter, and its specification is 100 mesh;With HF to tungsten before place Min layers cloth Fleece carries out pickling, removes the oxide-film on its surface.
Step 2, hot pressing:
The green compact that step 1 is obtained are mounted in can be in pressurizing mold, and in atmosphere protection hot pressing furnace leading to hydrogen carries out hot pressing:With After the firing rate of 15 DEG C/min is heated to 920 DEG C, composite green compact is carried out under the pressure of 5MPa with hot pressing and is incubated 60min。
Step 3, infiltration:
Composite blank Jing after step 2 hot pressing in micro-computer controlled high-temperature hydrogen atmosphere sintering furnace is carried out oozing copper: Heated with the firing rate of 15 DEG C/min, when temperature reaches 1300 DEG C, furnace cooling after insulation 120min obtains fibre Dimension and confusion structure Cu tailings.
Embodiment 2
Step 1, prepares composite green compact:
Weigh W powder 90%, Cu powder 10% by mass percentage respectively, above constituent mass percentage ratio sum is 100%, will W powder and Cu powder are with 0.7:1 ratio of grinding media to material mixes 7h under 400r/min rotating speeds in drum mixer;
Mixed composite powder is sieved after the removal of impurity with the tungsten fiber net of pickling the place Min layers cloth in the cold stamping die, According to tungsten fiber net interval 3mm after compacting, and pre-stamped, formation composite life after pressurize 30s is carried out to which under 400MPa Base.
Tungsten fiber net is formed by the tungsten fiber braiding of 40 μm of string diameter, and its specification is 30 mesh;With HF to tungsten before place Min layers cloth Fleece carries out pickling, removes the oxide-film on its surface.
Step 2, hot pressing:
The green compact that step 1 is obtained are mounted in can be in pressurizing mold, and in atmosphere protection hot pressing furnace leading to hydrogen carries out hot pressing:With After the firing rate of 20 DEG C/min is heated to 950 DEG C, composite green compact is carried out under the pressure of 15MPa with hot pressing and is incubated 40min。
Step 3, infiltration:
Composite blank Jing after step 2 hot pressing in micro-computer controlled high-temperature hydrogen atmosphere sintering furnace is carried out oozing copper: Heated with the firing rate of 20 DEG C/min, when temperature reaches 1320 DEG C, furnace cooling after insulation 90min obtains fibre Dimension and confusion structure Cu tailings.
Embodiment 3
Step 1, prepares composite green compact:
Weigh W powder 85%, Cu powder 15% by mass percentage respectively, above constituent mass percentage ratio sum is 100%, will W powder and Cu powder are with 1:1 ratio of grinding media to material mixes 8h under 400r/min rotating speeds in drum mixer;
Mixed composite powder is sieved after the removal of impurity with the tungsten fiber net of pickling the place Min layers cloth in the cold stamping die, According to tungsten fiber net interval 1mm after compacting, and pre-stamped, precompression 340MPa is carried out to which, after pressurize 60s, form composite Green compact.
Tungsten fiber net is formed by the tungsten fiber braiding of 40 μm of string diameter, and its specification is 30 mesh;With HF to tungsten before place Min layers cloth Fleece carries out pickling, removes the oxide-film on its surface.
Step 2, hot pressing:
The green compact that step 1 is obtained are mounted in can be in pressurizing mold, and in atmosphere protection hot pressing furnace leading to hydrogen carries out hot pressing:With After the firing rate of 25 DEG C/min is heated to 970 DEG C, composite green compact is carried out under the pressure of 30MPa with hot pressing and is incubated 10min。
Step 3, infiltration:
Composite blank Jing after step 2 hot pressing in micro-computer controlled high-temperature hydrogen atmosphere sintering furnace is carried out oozing copper: Heated with the firing rate of 25 DEG C/min, when temperature reaches 1350 DEG C, furnace cooling after insulation 30min obtains fibre Dimension and confusion structure Cu tailings.
Define between fiber that embodiment 3 is prepared and the fiber and granule of confusion structure Cu tailings Metallurgical binding, its microstructure are shown in Fig. 2.Fiber prepared by embodiment 3 and confusion structure Cu tailings with do not add Plus the Cu tailings of fleece are prepared as high temperature compressive sample respectively, note during processing so that tungsten fiber net is perpendicular to resistance to compression The radial direction of coupon.High temperature crush test is carried out respectively to which, its result is as shown in figure 3, wherein a figures are to be not added with fleece Cu tailings high temperature compressive stress-strain curve, b figures be the present invention in embodiment 3 prepare fiber and confusion Structure Cu tailings high temperature compressive stress-strain curve.As seen from Figure 3, for commaterial, with temperature Raise, the yield strength of material is constantly reduced;And at the same temperature, fiber is bent with confusion structure Cu tailings Take strength ratio and be not added with the Cu tailings of fleece and significantly improve.

Claims (6)

1. the preparation method of a kind of fiber and confusion structure Cu tailings, it is characterised in that it is concrete according to the following steps Implement:
Step 1, prepares composite green compact:
By the tungsten fiber net of the W powder and Cu powder of mix homogeneously and pickling in the cold stamping die place Min layers cloth, precompressed is carried out to which System, pressurize, obtain composite green compact;
The W powder and Cu powder are respectively W powder 70%~90%, Cu powder 10%~30%, above constituent mass by mass percentage Percentage ratio sum is 100%;The tungsten fiber net is formed by the tungsten fiber braiding of 40~60 μm of string diameter, its specification is 30~ 100 mesh;
Step 2, hot pressing:
The green compact that step 1 is obtained are mounted in can be in pressurizing mold, and in atmosphere protection hot pressing furnace leading to hydrogen carries out hot pressing;
Step 3, infiltration:
Composite blank Jing after step 2 hot pressing in micro-computer controlled high-temperature hydrogen atmosphere sintering furnace is carried out oozing copper, is obtained final product To fiber and confusion structure Cu tailings.
2. the preparation method of a kind of fiber according to claim 1 and confusion structure Cu tailings, its feature It is to mix described in step 1, specially:By W powder and Cu powder with 0.5~1:1 ratio of grinding media to material 400r/ in drum mixer Mix 6~8h under min rotating speeds.
3. the preparation method of a kind of fiber according to claim 1 and confusion structure Cu tailings, its feature It is, pickling described in step 1 to be tungsten fiber net to be cleaned with HF, remove the oxide-film on its surface.
4. the preparation method of a kind of fiber according to claim 1 and confusion structure Cu tailings, its feature It is that pre-stamped described in step 1 to require to be spaced 1~3mm for tungsten fiber net after compacting, precompressed pressing pressure is 200~400MPa, Dwell time is 30~90s.
5. the preparation method of a kind of fiber according to claim 1 and confusion structure Cu tailings, its feature It is, hot compression parameterses described in step 2, specially:It is heated to after 920~970 DEG C with the firing rate of 15~25 DEG C/min, it is right Composite green compact carry out hot pressing under the pressure of 5~30MPa and are incubated 10~60min.
6. the preparation method of a kind of fiber according to claim 1 and confusion structure Cu tailings, its feature It is, infiltration parameter described in step 3, specially:Heated with the firing rate of 15~25 DEG C/min, when temperature reaches When 1300~1350 DEG C, furnace cooling after 30~120min of insulation.
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CN107740006B (en) * 2017-09-19 2020-01-03 上海工程技术大学 Cu/W composite material with anisotropic performance and preparation method thereof
CN109440024B (en) * 2018-12-21 2019-10-01 攀枝花学院 Tungsten fiber/copper-based composite plate preparation method
CN110343978A (en) * 2019-07-08 2019-10-18 西安理工大学 The short tungsten fiber Reinforced Cu W composite material and preparation method of random distribution
CN110565033B (en) * 2019-09-30 2021-06-25 北京科技大学 Preparation method of tungsten-rhenium wire reinforced tungsten-copper alloy for high temperature
CN111893406B (en) * 2020-06-23 2021-12-17 西安理工大学 Composite material wire drawing die and preparation method thereof
CN113564499B (en) * 2021-07-29 2023-03-14 安徽工业大学科技园有限公司 Continuous tungsten fiber and zirconium carbide composite reinforced tungsten-copper material, preparation method and application thereof
CN115612948B (en) * 2022-10-31 2023-10-03 合肥工业大学智能制造技术研究院 Tungsten-copper alloy reinforced by high-strength high-heat-conductivity tungsten fiber and low-cost preparation method thereof

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JPH02125853A (en) * 1988-11-04 1990-05-14 Toshiba Corp Formation of coating layer of refractory metal, tungsten fiber coated with coating layer of refractory metal, and tungsten fiber-reinforced super alloy body
CN100503851C (en) * 2007-05-18 2009-06-24 西安建筑科技大学 Method for preparing tungsten copper or tungsten silver composite material
CN101386948B (en) * 2008-10-31 2010-09-29 于洋 Rolled tungsten-copper alloy material preparation method
CN102061431B (en) * 2010-12-17 2013-04-03 上海工程技术大学 Tungsten-copper composite material and preparation method thereof
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