CN103981389A - Method for preparing tungsten-copper alloy by low-temperature sintering of tungsten skeleton - Google Patents
Method for preparing tungsten-copper alloy by low-temperature sintering of tungsten skeleton Download PDFInfo
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Abstract
The invention discloses a method for preparing tungsten-copper alloy by low-temperature sintering of a tungsten skeleton. The method comprises the steps of carrying out wet grinding on tungsten powder of which the purity is 99.9% and the particle size is 1-7 mum and WOx powder which accounts for 5%-20% of the total mass of the powder and of which the particle size is 1-15 mum, uniformly mixing, drying and sieving, carrying out isostatic pressing on the mixed powder to obtain a green compact, sintering the green compact to obtain the tungsten skeleton, calculating the copper infiltration amount, cutting a copper plate of which the purity is greater than 99.5% into copper sheets with the same surface size as that of the tungsten skeleton, placing the copper sheets on the tungsten skeleton, feeding into a tubular furnace, heating to 1200-1400 DEG C under hydrogen atmosphere and carrying out copper infiltration. The content of copper in the tungsten-copper alloy is 15wt%-40wt%, and the balance is tungsten; the tungsten-copper alloy has more than 98% of density and the tungsten-copper alloy is suitable for being used as an electrical contact and electrode material, an electronic packaging material, a high-temperature sweating materials and the like.
Description
Technical field
The present invention relates to the preparation of tungsten-copper composite material, provide especially a kind of low-temperature sintering W skeleton to prepare the method for 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 do not form a kind of matrix material of intermetallic compound yet, be commonly called pseudo-alloy or pseudoalloy.It combines tungsten and copper characteristic separately, as high hot strength, high electrical and thermal conductivity, good electrical erosion resistance, higher hardness, low thermal expansivity and certain plasticity etc., and can pass through the change of its proportion of composing, control and the performance of each corresponding machinery of adjusting them and physics.In addition, tungsten-copper composite material has the advantage of tungsten, copper concurrently, can meet the service requirements of many fields material.As the resistance fusion welding of: tungsten can and corrosion resistance good, the conducting electricity very well of copper, both,, in conjunction with being used for vacuum interrupter, can meet the large capacity of vacuum interrupter and cut-off requirement; The linear expansivity of tungsten is little, the good heat conductivity of copper, tungsten-copper composite material, as the heat dissipation element in large-scale integrated circuit and microwave device, can effectively reduce because of the stress problem not enough and that difference of linear expansion causes of dispelling the heat, and extends the work-ing life of electronic component.Therefore, it can be widely used in the field of each industrial sectors, particularly some hi-techs such as space flight, electronics, machinery, electrical equipment.
It is first to prepare the POROUS TUNGSTEN skeleton with certain density and intensity that infiltration method is prepared Tungsten-copper Composites, then oozes with the relatively low copper of fusing point, utilizes capillary action that copper is packed in W skeleton, thereby forms fine and close tungsten-copper composite material.It is preparation even structure that infiltration method is prepared one of key of tungsten-copper composite material, to the wettability of copper is good, foreign matter content is few, there is the W skeleton of some amount open pore.In order to make W skeleton possess network structure, conventionally adopt W skeleton High Temperature Pre sintering process, it is first tungsten powder to be pressed under lower pressure to the green compact that relative density is lower, then at the temperature of 2000 ℃ of left and right through long period sintering, obtain 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 lower, and energy consumption is large, to equipment require highly, technique is restive.Owing to almost having between tungsten and copper, solubleness and copper are not poor to the wettability of tungsten, and while adopting infiltration method to prepare the tungsten-copper alloy of high copper content, gained W skeleton intensity and alloy density are all lower.And in tungsten, add the activating elements such as Fe, Co, Ni, although can improve W skeleton sintering, can greatly reduce conduction and the heat conductivility of Tungsten-copper Composites.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of low-temperature sintering W skeleton to prepare the method that copper is 15wt% ~ 40wt%, the surplus tungsten-copper alloy that is tungsten, the high-compactness that it can obtain more than 98%, is suitable for electrical contact and electrode materials, electronic package material, high temperature transpiring material etc.
For solving the problems of the technologies described above, technical solution of the present invention is:
Low-temperature sintering W skeleton is prepared a method for tungsten-copper alloy, and its preparation process is as follows:
In tungsten powder, add and account for (tungsten powder+WO used
2) WO of powder total mass per-cent 5% ~ 20%
xpowder, wet-milling evenly mixes 6 ~ 8 hours;
After powder mix drying and screening, isostatic pressing under the pressure of 150 ~ 200MPa, obtains pressed compact;
Pressed compact is placed in to tube furnace, under dry hydrogen shield, 1300 ~ 1500 ℃ of insulations, within 2 ~ 2.5 hours, carries out sintering, obtain W skeleton;
Measure mass M, the volume V of sintering back skeleton, the actual density of skeleton
, calculate its porosity
, and then calculate the copper amount of oozing
, ρ wherein
wtheoretical density, ρ for tungsten
cutheoretical density for copper;
According to above-mentioned formula, calculate the required copper amount of oozing of skeleton, and to ooze 1.1 ~ 1.2 times of copper amount, fine copper plate is cut into the copper sheet measure-alike with skeleton surface;
Copper sheet is placed on W skeleton, puts into tube furnace, under the atmosphere of hydrogen, be warming up to 1200 ~ 1400 ℃ and ooze copper, the tungsten-copper alloy that the mass percent that insulation obtains copper for 1 ~ 2 hour is 15% ~ 40%, surplus is tungsten.
Tungsten powder purity used is 99.9%, granularity is 1 ~ 7 μ m; WO used
xpowder Particle Size is 1 ~ 15 μ m.
Copper coin purity >99.5% used.
Adopt after such scheme, because the present invention adds in tungsten powder, account for tungsten powder+WO
xthe WO that powder total mass per-cent is 5% ~ 20%
xpowder, can reach the object that forms at a lower temperature some strength back bone network, with activating elements such as adding Fe, Co, Ni, compares, and the foreign matter content of this technique is relatively less.
In sum, the present invention has the following advantages:
(1) adopt the present invention to prepare tungsten-copper alloy, without adding any activator, can realize low-temperature sintering W skeleton, ooze copper after alloy density can reach more than 98%.
(2) adopt the present invention to prepare tungsten-copper alloy, technique is simple, and cost is low, and applicable industrialization is produced continuously.
(3) WO
xcan be used as pore-creating material to improve the copper content of tungsten-copper composite material, the porosity of skeleton can be passed through WO
xaddition regulate.
Accompanying drawing explanation
Fig. 1 is that copper mass per-cent of the present invention is 25, the section SEM of the tungsten-copper alloy that surplus is tungsten;
Fig. 2 is that copper mass per-cent of the present invention is 30, the section SEM of the tungsten-copper alloy that surplus is tungsten;
Fig. 3 is that copper mass per-cent of the present invention is 35, the section SEM of the tungsten-copper alloy that surplus is tungsten.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
embodiment 1:copper mass per-cent is 25, the preparation of the tungsten-copper alloy that surplus is tungsten
Adopt that purity is 99.9%, granularity is the tungsten powder of 2 μ m, and accounts for powder (tungsten powder+WO used
2) total mass 5wt.%, granularity be the WO of 11.22 μ m
xpowder, packs in ball grinding cylinder, and adds a small amount of sintered carbide ball and alcohol, mixes 6 hours to mixing, and after powder mix is dry, 80 orders sieve.Powder mix isostatic pressing rear mold under the pressure of 160MPa is molded, the pressed compact obtaining is placed in to hydrogen furnace and carries out sintering, and 1400 ℃ of sintering temperatures, are incubated 2 hours, obtain W skeleton.After cooling feeding, measuring W skeleton porosity λ is 57.5%, and then calculates the copper amount of oozing.Actual 1.1 times of oozing copper amount employing calculated amount, the fine copper plate of purity >99.5% is cut into the copper sheet measure-alike with skeleton surface to be placed on W skeleton, put into hydrogen furnace and be warming up to 1350 ℃ and ooze copper, after insulation 1h, after cooling down, obtain tungsten-copper alloy.
Product is carried out to correlated performance detection: copper content 25.4%, in allowing content 25% ± 2% scope; Density 14.781g/cm
3, relative density 98.36%, hardness HRB95.9, bending strength 843MPa.As can be seen from Figure 1, formed extraordinary copper mesh structure, each tungsten particle is filled full copper around, and even structure is fine and close.
Above detected result shows, what obtain is the tungsten-copper alloy that copper mass per-cent is 25%, surplus is tungsten, and when guaranteeing the high copper content of 25wt.%, density >=98%, has superior performance.
embodiment 2:copper mass per-cent is 30, the preparation of the tungsten-copper alloy that surplus is tungsten
Adopt that purity is 99.9%, granularity is the tungsten powder of 2 μ m, and accounts for powder (tungsten powder+WO used
2) total mass 10wt.%, granularity be the WO of 11.22 μ m
xpowder, packs in ball grinding cylinder, and adds a small amount of sintered carbide ball and alcohol, mixes 6 hours to mixing, and after powder mix is dry, 80 orders sieve.Powder mix isostatic pressing rear mold under the pressure of 160MPa is molded, the pressed compact obtaining is placed in to hydrogen furnace and carries out sintering, and 1400 ℃ of sintering temperatures, are incubated 2 hours, obtain W skeleton.After cooling feeding, measuring W skeleton porosity λ is 50.54%, and then calculates the copper amount of oozing.Actual 1.1 times of oozing copper amount employing calculated amount, the fine copper plate of purity >99.5% is cut into the copper sheet measure-alike with skeleton surface to be placed on W skeleton, put into hydrogen furnace and be warming up to 1350 ℃ and ooze copper, after insulation 2h, after cooling down, obtain tungsten-copper alloy.
Product is carried out to correlated performance detection: copper content 29.3%, in allowing content 30% ± 2% scope; Density 14.208 g/cm
3, relative density 98.65%, hardness HRB92.5, bending strength 837MPa.As can be seen from Figure 2, formed extraordinary copper mesh structure, each tungsten particle is filled full copper around, and even structure is fine and close.
Above detected result shows, what obtain is the tungsten-copper alloy that copper mass per-cent is 30%, surplus is tungsten, and when protecting the high copper content of 30wt.%, density >=98%, has superior performance.
embodiment 3:copper mass per-cent is 35, the preparation of the tungsten-copper alloy that surplus is tungsten
Adopt that purity is 99.9%, granularity is the tungsten powder of 2 μ m, and accounts for powder (tungsten powder+WO used
2) total mass 15wt.%, granularity be the WO of 11.22 μ m
xpowder, packs in ball grinding cylinder, and adds a small amount of sintered carbide ball and alcohol, mixes 6 hours to mixing, and after powder mix is dry, 80 orders sieve.Powder mix isostatic pressing rear mold under the pressure of 160MPa is molded, the pressed compact obtaining is placed in to hydrogen furnace and carries out sintering, and 1400 ℃ of sintering temperatures, are incubated 2 hours, obtain W skeleton.After cooling feeding, measuring W skeleton porosity λ is 46.63%, and then calculates the copper amount of oozing.Actual 1.1 times of oozing copper amount employing calculated amount, the fine copper plate of purity >99.5% is cut into the copper sheet measure-alike with skeleton surface to be placed on W skeleton, put into hydrogen furnace and be warming up to 1350 ℃ and ooze copper, after insulation 1.5h, after cooling down, obtain tungsten-copper alloy.
Product is carried out to correlated performance detection: copper content 33.0%, in allowing content 35% ± 2% scope; Density 13.764 g/cm
3, relative density 98.55%, hardness HRB90.4, bending strength 693MPa.As can be seen from Figure 3, formed extraordinary copper mesh structure, each tungsten particle is filled full copper around, and even structure is fine and close.
Above detected result shows, what obtain is the tungsten-copper alloy that copper mass per-cent is 35%, surplus is tungsten, and when guaranteeing the high copper content of 35wt.%, density >=98%, has superior performance.
The above, be only preferred embodiment of the present invention, is not used for limiting scope of the invention process.Therefore variation or the modification in every case done according to claim of the present invention and specification sheets, within all should belonging to the scope that patent of the present invention contains.
Claims (3)
1. low-temperature sintering W skeleton is prepared a method for tungsten-copper alloy, it is characterized in that its preparation process is as follows:
In tungsten powder, add and account for tungsten powder+WO used
xthe WO of powder total mass per-cent 5% ~ 20%
xpowder, wet-milling evenly mixes 6 ~ 8 hours;
After powder mix drying and screening, isostatic pressing under the pressure of 150 ~ 200MPa, obtains pressed compact;
Pressed compact is placed in to tube furnace, under dry hydrogen shield, 1300 ~ 1500 ℃ of insulations, within 2 ~ 2.5 hours, carries out sintering, obtain W skeleton;
Measure mass M, the volume V of sintering back skeleton, the actual density of skeleton
, calculate its porosity
, and then calculate the copper amount of oozing
, ρ wherein
wtheoretical density, ρ for tungsten
cutheoretical density for copper;
According to above-mentioned formula, calculate the required copper amount of oozing of skeleton, and to ooze 1.1 ~ 1.2 times of copper amount, fine copper plate is cut into the copper sheet measure-alike with skeleton surface;
Copper sheet is placed on W skeleton, puts into tube furnace, under the atmosphere of hydrogen, be warming up to 1200 ~ 1400 ℃ and ooze copper, the tungsten-copper alloy that the mass percent that insulation obtains copper for 1 ~ 2 hour is 15% ~ 40%, surplus is tungsten.
2. a kind of low-temperature sintering W skeleton according to claim 1 is prepared the method for tungsten-copper alloy, it is characterized in that: tungsten powder purity used is 99.9%, granularity is 1 ~ 7 μ m; WO used
xpowder Particle Size is 1 ~ 15 μ m.
3. a kind of low-temperature sintering W skeleton according to claim 1 is prepared the method for tungsten-copper alloy, it is characterized in that: copper coin purity >99.5% used.
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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 |
| CN104362015A (en) * | 2014-11-28 | 2015-02-18 | 桂林电器科学研究院有限公司 | Preparation method of copper-tungsten contact material |
| CN104384518A (en) * | 2014-10-27 | 2015-03-04 | 浙江立泰复合材料有限公司 | Method for coating copper on surface of tungsten copper carbide alloy composite material |
| CN108213762A (en) * | 2018-01-17 | 2018-06-29 | 宁国市顺鑫金属制品有限公司 | A kind of high rigidity mash welder soldering tip 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 |
| CN108620592A (en) * | 2018-05-03 | 2018-10-09 | 朱绘嘉 | A method of preparing tungsten copper capillary |
| 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 |
| CN110480008A (en) * | 2019-09-03 | 2019-11-22 | 北京工业大学 | It is a kind of to prepare three-dimensional communication tungsten-based composite material and method using laser 3D printing |
| CN110976889A (en) * | 2019-12-30 | 2020-04-10 | 西安理工大学 | Preparation method of high-W-content W-Cu composite material |
| 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 |
| CN111363941A (en) * | 2020-03-27 | 2020-07-03 | 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 |
| CN114570915A (en) * | 2022-03-08 | 2022-06-03 | 厦门欧斯拓科技有限公司 | Preparation method of rare earth composite material |
| CN114959333A (en) * | 2022-05-31 | 2022-08-30 | 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 |
| CN116426782A (en) * | 2023-03-15 | 2023-07-14 | 西安斯瑞先进铜合金科技有限公司 | Preparation method of tungsten copper material with high tungsten content |
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| CN104384518A (en) * | 2014-10-27 | 2015-03-04 | 浙江立泰复合材料有限公司 | Method for coating copper on surface of tungsten copper carbide alloy composite material |
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| CN108620592A (en) * | 2018-05-03 | 2018-10-09 | 朱绘嘉 | A method of preparing tungsten copper capillary |
| 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 |
| CN110480008A (en) * | 2019-09-03 | 2019-11-22 | 北京工业大学 | It is a kind of to prepare three-dimensional communication tungsten-based composite material and method using laser 3D printing |
| CN110976889A (en) * | 2019-12-30 | 2020-04-10 | 西安理工大学 | Preparation method of high-W-content W-Cu composite material |
| CN111363941A (en) * | 2020-03-27 | 2020-07-03 | 陕西理工大学 | Polygonal microstructure tungsten alloy material and preparation method and application thereof |
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