CN103981389B - A kind of method that low-temperature sintering W skeleton prepares tungsten-copper alloy - Google Patents
A kind of method that low-temperature sintering W skeleton prepares tungsten-copper alloy Download PDFInfo
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Abstract
The invention discloses a kind of method that low-temperature sintering W skeleton prepares tungsten-copper alloy, the tungsten powder that to adopt purity be 99.9%, granularity is 1 ~ 7 μm, and account for powder gross mass percentage ratio 5% ~ 20% used, granularity is the WO of 1 ~ 15 μmxPowder, drying and screening after wet grinding Homogeneous phase mixing. Mixed powder obtains pressed compact by isostatic pressing, after sintering obtains W skeleton, copper amount is oozed in calculating, by purity > the fine copper plate of 99.5% is cut into the copper sheet equivalently-sized with skeleton surface and is placed on W skeleton, putting in tube furnace, be warming up to 1200 ~ 1400 DEG C and carry out oozing copper under the atmosphere of hydrogen, the copper of gained tungsten-copper alloy is 15wt% ~ 40wt%, surplus is tungsten, and have more than 98% high-compactness, be suitable for electrical contact and electrode material, electronic package material, high temperature transpiration material etc.
Description
Technical field
The present invention relates to the preparation of tungsten-copper composite material, specifically provide a kind of method that low-temperature sintering W skeleton prepares tungsten-copper alloy.
Background technology
Tungsten-copper alloy be the copper Binder Phase of a kind of tungsten particle by body-centered cubic structure and face-centred cubic structure form neither mutually solid solution be also formed without a kind of composite of intermetallic compound, be commonly called pseudo-alloy or pseudo-alloy. It combines tungsten and the respective characteristic of copper, such as high elevated temperature strength, high electrical and thermal conductivity, good electrical erosion resistance, higher hardness, low thermal coefficient of expansion and certain plasticity etc., and by the change of its proportion of composing, can control and performance of adjust them each corresponding machinery and physics. Additionally, the advantage that tungsten-copper composite material has tungsten, copper concurrently, it is possible to meet the instructions for use of many zone material. As: the resistance fusion welding of tungsten can be good with corrosion resistance, and conducting electricity very well of copper, in combination with for vacuum circuit breaker, it is possible to meets vacuum circuit breaker Large Copacity and cut-offs requirement; The linear expansion coefficient of tungsten is little, the good heat conductivity of copper, tungsten-copper composite material is used as the heat dissipation element in large scale integrated circuit and microwave device, it is possible to effectively reduces because of the not enough stress problem caused with difference of linear expansion of dispelling the heat, extends the service life of electronic component. Therefore, it can be widely applied to the field of each industrial departments, particularly some high-tech such as space flight, electronics, machinery, electrical equipment.
It is the POROUS TUNGSTEN skeleton first prepared and have certain density and intensity that infiltration method prepares Tungsten-copper Composites, then oozes the copper relatively low with fusing point, utilizes capillarity to make copper be packed in W skeleton, thus forming the tungsten-copper composite material of densification. One of infiltration method key preparing tungsten-copper composite material be prepare even structure, good to the wettability of copper, impurity content is few, have the W skeleton of some interconnected pores. In order to make W skeleton possess network structure, generally adopt W skeleton high temperature pre-burning connection, it is that tungsten powder is first pressed into green compact that relative density is relatively low at lower pressures, then sinters through the long period at the temperature of about 2000 DEG C, obtains the W skeleton of required relative density.The weak point of this technique is that sintering temperature is high, and sintering time is long, and closed pore is more, and the tungsten-copper composite material relative density after infiltration is relatively low, and energy consumption is big, and the requirement of equipment is high, and technique is difficult to control. Due to the wettability of tungsten is poor almost without dissolubility and copper between tungsten and copper, when adopting the tungsten-copper alloy that infiltration method prepares high copper content, gained W skeleton intensity is all relatively low with alloy consistency. And in tungsten, add the active elements such as Fe, Co, Ni, although W skeleton sintering can be improved, but conduction and the heat conductivility of Tungsten-copper Composites can be substantially reduced.
Summary of the invention
The method of the tungsten-copper alloy of the technical problem to be solved be in that to provide a kind of low-temperature sintering W skeleton to prepare copper to be 15wt% ~ 40wt%, surplus be tungsten, it can obtain the high-compactness of more than 98%, is suitable for electrical contact and electrode material, electronic package material, high temperature transpiration material etc.
For solving above-mentioned technical problem, the technical solution of the present invention is:
A kind of method that low-temperature sintering W skeleton prepares tungsten-copper alloy, its preparation process is as follows:
Tungsten powder adds and accounts for (tungsten powder+WO used2) WO of powder gross mass percentage ratio 5% ~ 20%xPowder, wet grinding Homogeneous phase mixing 6 ~ 8 hours;
After mixed powder drying and screening, isostatic pressing under the pressure of 150 ~ 200MPa, obtain pressed compact;
Pressed compact is placed in tube furnace, within 2 ~ 2.5 hours, is sintered 1300 ~ 1500 DEG C of insulations under dry hydrogen gas shielded, obtains W skeleton;
Measure the sintering mass M of back skeleton, volume V, the then actual density of skeleton, calculate its porosity, and then calculate ooze copper amount, wherein ρWFor the solid density of tungsten, ρCuSolid density for copper;
Calculate, according to above-mentioned formula, copper amount of oozing needed for skeleton, and to ooze 1.1 ~ 1.2 times of copper amount, fine copper plate is cut into the copper sheet equivalently-sized with skeleton surface;
Copper sheet is placed on W skeleton, puts in tube furnace, under the atmosphere of hydrogen, be warming up to 1200 ~ 1400 DEG C carry out oozing copper, insulation within 1 ~ 2 hour, namely obtain the mass percent of copper be 15% ~ 40%, surplus be the tungsten-copper alloy of tungsten.
Tungsten powder purity used is 99.9%, granularity is 1 ~ 7 μm; WO usedxPowder Particle Size is 1 ~ 15 μm.
Copper coin purity used > 99.5%.
After adopting such scheme, account for tungsten powder+WO owing to the present invention adds in tungsten powderxPowder gross mass percentage ratio is the WO of 5% ~ 20%xPowder, can reach to be formed at a lower temperature the purpose of some strength back bone network, compares with active elements such as adding Fe, Co, Ni, and the impurity content of this technique is relatively fewer.
In sum, the present invention has the following advantages:
(1) present invention is adopted to prepare tungsten-copper alloy, it is not necessary to adding any activator, it may be achieved low-temperature sintering W skeleton, after oozing copper, alloy consistency is up to more than 98%.
(2) adopting the present invention to prepare tungsten-copper alloy, technique is simple, and cost is low, and applicable industrialization produces continuously.
(3) WOxCan as pore forming material to improve the copper content of tungsten-copper composite material, the porosity of skeleton can pass through WOxAddition be adjusted.
Accompanying drawing explanation
Fig. 1 is the copper mass percentage ratio of the present invention is 25, and surplus is the section SEM of the tungsten-copper alloy of tungsten;
Fig. 2 is the copper mass percentage ratio of the present invention is 30, and surplus is the section SEM of the tungsten-copper alloy of tungsten;
Fig. 3 is the copper mass percentage ratio of the present invention is 35, and surplus is the section SEM of the tungsten-copper alloy of tungsten.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment 1: copper mass percentage ratio is 25, surplus is the preparation of the tungsten-copper alloy of tungsten
The tungsten powder that to adopt purity be 99.9%, granularity is 2 μm, and account for powder used (tungsten powder+WO2) gross mass 5wt.%, granularity be the WO of 11.22 μmxPowder, loads in ball grinding cylinder, and adds a small amount of sintered carbide ball and ethanol, mix 6 hours to mix homogeneously, and dried 80 orders of mixed powder sieve.Mixed powder isostatic pressing rear mold under the pressure of 160MPa is molded, is placed in hydrogen furnace by the pressed compact obtained and is sintered, sintering temperature 1400 DEG C, is incubated 2 hours, obtains W skeleton. After cooling feeding, measuring W skeleton porosity λ is 57.5%, and then copper amount is oozed in calculating. Actual copper amount of oozing adopts 1.1 times of amount of calculation, by purity > the fine copper plate of 99.5% is cut into the copper sheet equivalently-sized with skeleton surface and is placed on W skeleton, and put into and hydrogen furnace is warming up to 1350 DEG C carries out oozing copper, after insulation 1h, after cooling down, namely obtain tungsten-copper alloy.
Product is carried out correlated performance detection: copper content 25.4%, in permission content 25% ± 2% scope; Density 14.781g/cm3, relative density 98.36%, hardness HRB95.9, bending strength 843MPa. It will be seen from figure 1 that define extraordinary copper mesh structure, each tungsten particle periphery fills full copper, and even structure is fine and close.
Above testing result shows, obtain to be copper mass percentage ratio be 25%, surplus is the tungsten-copper alloy of tungsten, and while ensureing the high copper content of 25wt.%, consistency >=98%, there is superior performance.
Embodiment 2: copper mass percentage ratio is 30, surplus is the preparation of the tungsten-copper alloy of tungsten
The tungsten powder that to adopt purity be 99.9%, granularity is 2 μm, and account for powder used (tungsten powder+WO2) gross mass 10wt.%, granularity be the WO of 11.22 μmxPowder, loads in ball grinding cylinder, and adds a small amount of sintered carbide ball and ethanol, mix 6 hours to mix homogeneously, and dried 80 orders of mixed powder sieve. Mixed powder isostatic pressing rear mold under the pressure of 160MPa is molded, is placed in hydrogen furnace by the pressed compact obtained and is sintered, sintering temperature 1400 DEG C, is incubated 2 hours, obtains W skeleton. After cooling feeding, measuring W skeleton porosity λ is 50.54%, and then copper amount is oozed in calculating. Actual copper amount of oozing adopts 1.1 times of amount of calculation, by purity > the fine copper plate of 99.5% is cut into the copper sheet equivalently-sized with skeleton surface and is placed on W skeleton, and put into and hydrogen furnace is warming up to 1350 DEG C carries out oozing copper, after insulation 2h, after cooling down, namely obtain tungsten-copper alloy.
Product is carried out correlated performance detection: copper content 29.3%, in permission content 30% ± 2% scope; Density 14.208g/cm3, relative density 98.65%, hardness HRB92.5, bending strength 837MPa. Figure it is seen that define extraordinary copper mesh structure, each tungsten particle periphery fills full copper, and even structure is fine and close.
Above testing result shows, obtain to be copper mass percentage ratio be 30%, surplus is the tungsten-copper alloy of tungsten, and while protecting the high copper content of 30wt.%, consistency >=98%, there is superior performance.
Embodiment 3: copper mass percentage ratio is 35, surplus is the preparation of the tungsten-copper alloy of tungsten
The tungsten powder that to adopt purity be 99.9%, granularity is 2 μm, and account for powder used (tungsten powder+WO2) gross mass 15wt.%, granularity be the WO of 11.22 μmxPowder, loads in ball grinding cylinder, and adds a small amount of sintered carbide ball and ethanol, mix 6 hours to mix homogeneously, and dried 80 orders of mixed powder sieve. Mixed powder isostatic pressing rear mold under the pressure of 160MPa is molded, is placed in hydrogen furnace by the pressed compact obtained and is sintered, sintering temperature 1400 DEG C, is incubated 2 hours, obtains W skeleton. After cooling feeding, measuring W skeleton porosity λ is 46.63%, and then copper amount is oozed in calculating. Actual copper amount of oozing adopts 1.1 times of amount of calculation, by purity > the fine copper plate of 99.5% is cut into the copper sheet equivalently-sized with skeleton surface and is placed on W skeleton, and put into and hydrogen furnace is warming up to 1350 DEG C carries out oozing copper, after insulation 1.5h, after cooling down, namely obtain tungsten-copper alloy.
Product is carried out correlated performance detection: copper content 33.0%, in permission content 35% ± 2% scope; Density 13.764g/cm3, relative density 98.55%, hardness HRB90.4, bending strength 693MPa. From figure 3, it can be seen that define extraordinary copper mesh structure, each tungsten particle periphery fills full copper, and even structure is fine and close.
Above testing result shows, obtain to be copper mass percentage ratio be 35%, surplus is the tungsten-copper alloy of tungsten, and while ensureing the high copper content of 35wt.%, consistency >=98%, there is superior performance.
The above, be only presently preferred embodiments of the present invention, is not used for limiting scope of the invention process. Therefore the change that claim under this invention and description are done in every case or modification, all should belong within the scope that patent of the present invention contains.
Claims (3)
1. the method that a low-temperature sintering W skeleton prepares tungsten-copper alloy, it is characterised in that its preparation process is as follows:
Tungsten powder adds and accounts for tungsten powder+WO usedxThe WO of powder gross mass percentage ratio 5%～20%xPowder, wet grinding Homogeneous phase mixing 6～8 hours;
After mixed powder drying and screening, isostatic pressing under the pressure of 150～200MPa, obtain pressed compact;
Pressed compact is placed in tube furnace, within 2～2.5 hours, is sintered 1300～1500 DEG C of insulations under dry hydrogen gas shielded, obtains W skeleton;
Measure the sintering mass M of back skeleton, volume V, the then actual density of skeletonCalculate its porosityAnd then calculate ooze copper amount m=λ × V × ρCu, wherein ρWFor the solid density of tungsten, ρCuSolid density for copper;
Calculate, according to above-mentioned formula, copper amount of oozing needed for skeleton, and to ooze 1.1～1.2 times of copper amount, fine copper plate is cut into the copper sheet equivalently-sized with skeleton surface;
Copper sheet is placed on W skeleton, puts in tube furnace, under the atmosphere of hydrogen, be warming up to 1200～1400 DEG C carry out oozing copper, insulation within 1～2 hour, namely obtain the mass percent of copper be 15%～40%, surplus be the tungsten-copper alloy of tungsten.
2. the method that a kind of low-temperature sintering W skeleton according to claim 1 prepares tungsten-copper alloy, it is characterised in that: tungsten powder purity used is 99.9%, granularity is 1～7 μm; WO usedxPowder Particle Size is 1～15 μm.
3. the method that a kind of low-temperature sintering W skeleton according to claim 1 prepares tungsten-copper alloy, it is characterised in that: copper coin purity used > 99.5%.
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| CN104213009A (en) * | 2014-08-29 | 2014-12-17 | 浙江立泰复合材料有限公司 | Method for cladding copper on surface of infiltration sintered tungsten-copper composite material |
| CN104384518B (en) * | 2014-10-27 | 2016-05-04 | 浙江立泰复合材料有限公司 | The method of copper is covered on a kind of tungsten carbide carbon/carbon-copper composite material surface |
| CN104362015B (en) * | 2014-11-28 | 2017-05-10 | 桂林电器科学研究院有限公司 | Preparation method of copper-tungsten contact material |
| CN108213762B (en) * | 2018-01-17 | 2020-03-31 | 宁国市顺鑫金属制品有限公司 | Welding head for high-hardness spot welding machine and preparation method thereof |
| CN108436079A (en) * | 2018-03-15 | 2018-08-24 | 北京矿冶科技集团有限公司 | A kind of preparation method of hole even porous tungsten |
| CN108620592B (en) * | 2018-05-03 | 2019-11-19 | 朱绘嘉 | A method of preparing tungsten copper capillary |
| CN111230103A (en) * | 2018-11-29 | 2020-06-05 | 西安西电高压开关有限责任公司 | Preparation method of tungsten-copper alloy wear-resistant electrode |
| CN109609792A (en) * | 2018-12-17 | 2019-04-12 | 河源市凯源硬质合金有限公司 | A method of preparing tungsten-copper alloy |
| CN110480008B (en) * | 2019-09-03 | 2021-10-15 | 北京工业大学 | Three-dimensional communicated tungsten-based composite material prepared by laser 3D printing and preparation method thereof |
| CN110976889A (en) * | 2019-12-30 | 2020-04-10 | 西安理工大学 | Preparation method of high-W-content W-Cu composite material |
| CN111363941B (en) * | 2020-03-27 | 2021-06-29 | 陕西理工大学 | Polygonal microstructure tungsten alloy material and preparation method and application thereof |
| CN114160787A (en) * | 2021-12-07 | 2022-03-11 | 沈阳金昌蓝宇新材料股份有限公司 | Manufacturing method of non-shrinkage tungsten framework |
| CN114570915B (en) * | 2022-03-08 | 2024-03-19 | 厦门欧斯拓科技有限公司 | Preparation method of rare earth composite material |
| CN114959333B (en) * | 2022-05-31 | 2022-11-11 | 河源市凯源硬质合金股份有限公司 | Tungsten-copper alloy and preparation method thereof |
| CN115976434A (en) * | 2022-12-30 | 2023-04-18 | 湖南金博碳素股份有限公司 | Carbon-tungsten-copper composite material, preparation method and application thereof, and electrode |
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