CN103526060A - Rapid preparation method of copper-tungsten alloy - Google Patents
Rapid preparation method of copper-tungsten alloy Download PDFInfo
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- CN103526060A CN103526060A CN201310463859.1A CN201310463859A CN103526060A CN 103526060 A CN103526060 A CN 103526060A CN 201310463859 A CN201310463859 A CN 201310463859A CN 103526060 A CN103526060 A CN 103526060A
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- copper
- tungsten
- briquet
- powder
- skeleton
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- SBYXRAKIOMOBFF-UHFFFAOYSA-N copper tungsten Chemical compound [Cu].[W] SBYXRAKIOMOBFF-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910001080 W alloy Inorganic materials 0.000 title abstract 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000005245 sintering Methods 0.000 claims abstract description 22
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000000498 ball milling Methods 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 9
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052863 mullite Inorganic materials 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 238000000227 grinding Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 abstract description 17
- 238000005516 engineering process Methods 0.000 abstract description 8
- 238000009768 microwave sintering Methods 0.000 abstract description 5
- 238000004663 powder metallurgy Methods 0.000 abstract description 3
- 238000003825 pressing Methods 0.000 abstract description 2
- 230000008595 infiltration Effects 0.000 description 9
- 238000001764 infiltration Methods 0.000 description 9
- 239000010949 copper Substances 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 4
- 230000004927 fusion Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 229910000714 At alloy Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052594 sapphire Inorganic materials 0.000 description 1
- 239000010980 sapphire Substances 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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Abstract
The invention relates to a rapid preparation method of a copper-tungsten alloy, and belongs to the fields of a powder metallurgy technology, a metallurgical new technology and a microwave sintering technology. The method comprises the following steps: carrying out ball milling mixing of metallic tungsten powder and copper powder according to a proportion ratio of 95-70wt%:5-30wt%, carrying out briquet pressing to prepare a tungsten skeleton briquet, filling into a mullite crucible, distributing the copper powder surrounding the tungsten skeleton briquet, putting the crucible under conditions comprising a microwave frequency of 2400-2500MHz, a power of 3-5KW and a degree of vacuum of below 0.1KPa, sintering for 1-3h by heating to 1100-1300DEG C at a heating speed of 15-20DEG C/min, and naturally cooling to obtain the copper-tungsten alloy. The copper-tungsten alloy prepared through the method has a uniform structure and a compact structure, and has a relative density reaching 98.7%.
Description
Technical field
The present invention relates to powder metallurgy technology, metallurgical new technology and Microwave Sintering Techniques field, particularly a kind of fast preparation method of copper-tungsten.
Background technology
Copper-tungsten has high-melting-point, high-density, electrical erosion resistance, resistance fusion welding and the higher hot strength of W, and the height electricity again with Cu is led and thermal conductivity, plasticity and workability.While evaporating under high arc temperature due to Cu, can absorb a large amount of arc energies, reduce arc temperature, improve working conditions and reduce galvanic action, therefore be widely used as the electrical contact material of High-Voltage Electrical Appliances, also as the electrode of electromachining, die material and other, require the occasion of electrical and thermal conductivity performance and applied at elevated temperature.At present, generally adopt infiltration method and activation solution phase sintering legal system for W-Cu material.But due to W and Cu two-phase immiscible, therefore, the segregation of traditional infiltration W-Cu material structure, thick and relative density is low, in addition, activation solution phase sintering can be introduced the performance of foreign peoples's impurity effect material.Microwave Sintering Techniques is to utilize special wave band and the material that microwave has be coupled and produce heat, make material monolithic be heated to sintering temperature and realize the method for densification, its compare with normal sintering technology have that sintering temperature is low, sintering time is short, energy utilization rate and heating efficiency advantages of higher, and the workpiece of making has higher density, hardness and obdurability, excellent combination property.
Application number is 2009103041144 " a kind of microwave infiltration way sintering is prepared the method for W-CU alloy "; be after copper powder and tungsten powder ball milling are mixed, be pressed into W skeleton, electrolytic copper powder is made infiltration cu pressed compact; jointly be placed in sapphire whisker insulation jacket with boosting material SiC sheet, then in microwave condition and hybrid protection gas atmosphere, sintering obtains.Foregoing invention is to utilize the condition of Microwave-assisted firing SiC sheet and atmosphere protection to realize the sintering preparation of alloy; compare with traditional preparation method; microwave can rapid heating SiC sheet; and transfer heat to alloy pressed compact; aspect heat transfer, be a kind of indirectly heat exchange pattern, heating rate is compared low with effciency of energy transfer with microwave direct heating.
Summary of the invention
For overcoming the deficiencies in the prior art, the present invention proposes a kind of fast preparation method of copper-tungsten, the method utilizes microwave direct heating copper powder to fusing, and under vacuum condition, realize the Fast Sintering to metal pressed compact, compare with traditional heating mode, the method is that the basic fine structure coupling of the special wave band that has by microwave and material produces heat, makes material monolithic be heated to temperature of fusion, have rate of heating soon, energy conversion rate advantages of higher.
The present invention prepares copper-tungsten in conjunction with microwave metal smelting powder, Microwave Sintering Techniques, powder metallurgy technology and melting infiltration sintering method, is a kind of method of preparing fast copper-tungsten.Concrete steps comprise as follows:
(1) metal tungsten powder and copper powder are carried out to ball mill mixing according to mass percent 95～70wt%:5～30% respectively;
(2) tungsten powder and the copper powder that ball milling in step (1) are mixed carry out briquet compacting, make W skeleton briquet;
(3) pack W skeleton briquet into mullite crucible, and be covered with at W skeleton briquet the copper powder that thickness is 2～5mm around, then being placed in microwave frequency is that 2400～2500MHz, power 3～5KW, vacuum tightness are less than under the condition of 0.1KPa, keep the rate of heating of 15～20 ℃/min that temperature is risen to 1100～1300 ℃ of sintering 1～3 hour, naturally cooling obtains copper-tungsten.
The granularity of described metal tungsten powder and copper powder is all less than 200 orders, and purity is all greater than 99.8wt%.
During described ball mill mixing, according to ratio of grinding media to material, be ball milling 10～40min under 1～50:1, the rotating speed condition that is 100～300r/min.
Pressure-controlling during described compacting briquet is at 25～45MPa, and pressure is controlled according to the content of copper powder in pressed compact, and when mixed copper powder content is low, pressing pressure is large, otherwise little.
The invention has the beneficial effects as follows:
(1) major embodiment is prepared fast, because be to adopt microwave sintering, can direct fusion copper powder, and there is rate of heating fast, the feature that thermo-efficiency is high, by regulating microwave power, can be at 40 ~ 50min deposite metal copper powder;
(2) mullite crucible adopting is wave transparent type pottery, can realize the object of microwave direct heating copper powder, but not after the absorbing materials such as heating silicon carbide plate, then by thermaltransmission mode indirect heating;
(3) infiltration copper used in the present invention is copper powder, but not metallic copper briquet, copper powder is as inhaling ripple carrier, again as infiltration material, sintering process at alloy also can prevent alloy surface oxidation, utilizes the method except preparing copper-tungsten, also can ooze in process for copper and apply at other;
(4) the present invention is sintering under vacuum condition, non-atmosphere protection, and technical process is simple, and alloy property is also comparatively excellent.
Accompanying drawing explanation
Fig. 1 is the fast preparation method process flow sheet of copper-tungsten of the present invention;
Fig. 2 is the copper-tungsten micro-organization chart that the present invention adds melting infiltration sintering after 8% copper powder;
Fig. 3 is the copper-tungsten micro-organization chart that the present invention adds melting infiltration sintering after 20% copper powder.
Embodiment
Below in conjunction with the drawings and specific embodiments, the invention will be further described.
Embodiment one: the fast preparation method of the copper-tungsten of present embodiment is:
(1) metal tungsten powder and copper powder are carried out to ball mill mixing according to mass percent 92wt%:8wt% respectively, ball milling is mixed
During material, according to ratio of grinding media to material, be ball milling 40min under 50:1, the rotating speed condition that is 100r/min; The granularity of metal tungsten powder and copper powder is 10～20 μ m, and purity is greater than 99.8wt%.
(2) tungsten powder and the copper powder that ball milling in step (1) are mixed carry out briquet compacting, and pressure-controlling, at 30MPa, is made cylindrical W skeleton briquet;
(3) pack W skeleton briquet into mullite crucible, and be covered with at W skeleton briquet the copper powder that thickness is 3mm around, then being placed in microwave frequency is under the condition of 2400MHz, power 5KW, vacuum tightness 0.08KPa, keep the rate of heating of 20 ℃/min that temperature is risen to 1200 ℃ of sintering 1.2 hours, naturally cooling obtains copper-tungsten, sample is analyzed, and copper-tungsten Brinell hardness is 229, and relative density is 95.4%.Microstructure as shown in Figure 2.
Embodiment two: the fast preparation method of the copper-tungsten of present embodiment is:
(2) metal tungsten powder and copper powder are carried out to ball mill mixing according to mass percent 80wt%:20% respectively, ball milling is mixed
During material, according to ratio of grinding media to material, be ball milling 20min under 30:1, the rotating speed condition that is 200r/min; The granularity of metal tungsten powder and copper powder is all less than 200 orders, and purity is all greater than 99.8wt%.
(2) tungsten powder and the copper powder that ball milling in step (1) are mixed carry out briquet compacting, and pressure-controlling, at 45MPa, is made W skeleton briquet;
(3) pack W skeleton briquet into mullite crucible, and be covered with at W skeleton briquet the copper powder that thickness is 2mm around, then being placed in microwave frequency is that 2500MHz, power 3KW, vacuum tightness are less than under the condition of 0.1KPa, keep the rate of heating of 15 ℃/min that temperature is risen to 1300 ℃ of sintering 1 hour, naturally cooling obtains copper-tungsten, sample is analyzed, and copper-tungsten Bu Shi is 221, and relative density is 98.7%.Microstructure as shown in Figure 3.
Embodiment three: the fast preparation method of the copper-tungsten of present embodiment is:
(1) metal tungsten powder and copper powder are carried out to ball mill mixing according to mass percent 95wt%:5% respectively, ball milling is mixed
During material, according to ratio of grinding media to material, be ball milling 10min under 1:1, the rotating speed condition that is 300r/min; The granularity of metal tungsten powder and copper powder is all less than 200 orders, and purity is all greater than 99.8wt%.
(2) tungsten powder and the copper powder that ball milling in step (1) are mixed carry out briquet compacting, and pressure-controlling, at 25MPa, is made W skeleton briquet;
(3) pack W skeleton briquet into mullite crucible, and be covered with at W skeleton briquet the copper powder that thickness is 5mm around, then being placed in microwave frequency is that 2450MHz, power 3.5KW, vacuum tightness are less than under the condition of 0.1KPa, keep the rate of heating of 18 ℃/min that temperature is risen to 1100 ℃ of sintering 3 hours, naturally cooling obtains copper-tungsten.
Embodiment four: the fast preparation method of the copper-tungsten of present embodiment is:
(1) metal tungsten powder and copper powder are carried out to ball mill mixing according to mass percent 70wt%:30% respectively, ball is mixed
During material, according to ratio of grinding media to material, be ball milling 30min under 20:1, the rotating speed condition that is 200r/min; The granularity of metal tungsten powder and copper powder is all less than 200 orders, and purity is all greater than 99.8wt%.
(2) tungsten powder and the copper powder that ball milling in step (1) are mixed carry out briquet compacting, and pressure-controlling, at 25MPa, is made W skeleton briquet;
(3) pack W skeleton briquet into mullite crucible, and be covered with at W skeleton briquet the copper powder that thickness is 2.5mm around, then being placed in microwave frequency is that 2500MHz, power 3.8KW, vacuum tightness are less than under the condition of 0.1KPa, keep the rate of heating of 17 ℃/min that temperature is risen to 1250 ℃ of sintering 3 hours, naturally cooling obtains copper-tungsten.
Below by reference to the accompanying drawings the specific embodiment of the present invention is explained in detail, but the present invention is not limited to above-mentioned embodiment, in the ken possessing those of ordinary skills, can also under the prerequisite that does not depart from aim of the present invention, make various variations.
Claims (4)
1. a fast preparation method for copper-tungsten, is characterized in that concrete steps comprise:
(1) metal tungsten powder and copper powder are carried out to ball mill mixing according to mass percent 95～70wt%:5～30% respectively;
(2) tungsten powder and the copper powder that ball milling in step (1) are mixed carry out briquet compacting, make W skeleton briquet;
(3) pack W skeleton briquet into mullite crucible, and be covered with at W skeleton briquet the copper powder that thickness is 2～5mm around, then being placed in microwave frequency is that 2400～2500MHz, power 3～5KW, vacuum tightness are less than under the condition of 0.1KPa, keep the rate of heating of 15～20 ℃/min that temperature is risen to 1100～1300 ℃ of sintering 1～3 hour, naturally cooling obtains copper-tungsten.
2. the fast preparation method of copper-tungsten according to claim 1, is characterized in that: the granularity of described metal tungsten powder and copper powder is all less than 200 orders, and purity is all greater than 99.8wt%.
3. the fast preparation method of copper-tungsten according to claim 1, is characterized in that: during described ball mill mixing, according to ratio of grinding media to material, be ball milling 10～40min under 1～50:1, the rotating speed condition that is 100～300r/min.
4. the fast preparation method of copper-tungsten according to claim 1, is characterized in that: pressure-controlling during described compacting briquet is at 25～45MPa.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN105039876A (en) * | 2015-07-06 | 2015-11-11 | 西安理工大学 | Preparation method for W-Cu composite materials of fiber and particle hybrid structure |
| CN105057873A (en) * | 2015-07-20 | 2015-11-18 | 沈阳金昌蓝宇新材料股份有限公司 | Method for preparing CuW/Cu/CuCrZr integrated contact through electron beam welding |
| CN105215566A (en) * | 2015-09-14 | 2016-01-06 | 泰州市华诚钨钼制品有限公司 | A kind of electrode tungsten copper rod |
| CN106282714A (en) * | 2016-09-23 | 2017-01-04 | 西安理工大学 | A kind of preparation method of self-lubricating copper tungsten material |
| CN107326241A (en) * | 2017-07-10 | 2017-11-07 | 四川大学 | A kind of method that tungsten molybdenum copper composite material is prepared with discharge plasma sintering |
| CN109852861A (en) * | 2019-02-28 | 2019-06-07 | 北京工业大学 | A kind of low-temperature rapid preparation method of the nanocrystalline tungsten copper matrix composite material of high-compactness |
| CN111020334A (en) * | 2020-01-08 | 2020-04-17 | 郑州航空工业管理学院 | Preparation method of high-densification tungsten-copper refractory alloy |
| CN111451492A (en) * | 2020-03-23 | 2020-07-28 | 陕西斯瑞新材料股份有限公司 | Method for preparing CuW90 material by using spherical tungsten powder |
| CN112063877A (en) * | 2020-09-25 | 2020-12-11 | 江西省科学院应用物理研究所 | Preparation method of copper-tungsten alloy |
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| CN101624662A (en) * | 2009-07-08 | 2010-01-13 | 中南大学 | Method for preparing W-Cu alloy in microwave infiltration way |
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Patent Citations (2)
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| US6183689B1 (en) * | 1997-11-25 | 2001-02-06 | Penn State Research Foundation | Process for sintering powder metal components |
| CN101624662A (en) * | 2009-07-08 | 2010-01-13 | 中南大学 | Method for preparing W-Cu alloy in microwave infiltration way |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN105039876A (en) * | 2015-07-06 | 2015-11-11 | 西安理工大学 | Preparation method for W-Cu composite materials of fiber and particle hybrid structure |
| CN105057873A (en) * | 2015-07-20 | 2015-11-18 | 沈阳金昌蓝宇新材料股份有限公司 | Method for preparing CuW/Cu/CuCrZr integrated contact through electron beam welding |
| CN105215566A (en) * | 2015-09-14 | 2016-01-06 | 泰州市华诚钨钼制品有限公司 | A kind of electrode tungsten copper rod |
| CN106282714A (en) * | 2016-09-23 | 2017-01-04 | 西安理工大学 | A kind of preparation method of self-lubricating copper tungsten material |
| CN107326241A (en) * | 2017-07-10 | 2017-11-07 | 四川大学 | A kind of method that tungsten molybdenum copper composite material is prepared with discharge plasma sintering |
| CN107326241B (en) * | 2017-07-10 | 2019-01-15 | 四川大学 | A method of tungsten molybdenum copper composite material is prepared with discharge plasma sintering |
| CN109852861A (en) * | 2019-02-28 | 2019-06-07 | 北京工业大学 | A kind of low-temperature rapid preparation method of the nanocrystalline tungsten copper matrix composite material of high-compactness |
| CN109852861B (en) * | 2019-02-28 | 2020-07-03 | 北京工业大学 | Low-temperature rapid preparation method of high-density nanocrystalline tungsten-copper-based bulk composite material |
| CN111020334A (en) * | 2020-01-08 | 2020-04-17 | 郑州航空工业管理学院 | Preparation method of high-densification tungsten-copper refractory alloy |
| CN111020334B (en) * | 2020-01-08 | 2020-10-20 | 郑州航空工业管理学院 | Preparation method of high-densification tungsten-copper refractory alloy |
| CN111451492A (en) * | 2020-03-23 | 2020-07-28 | 陕西斯瑞新材料股份有限公司 | Method for preparing CuW90 material by using spherical tungsten powder |
| CN111451492B (en) * | 2020-03-23 | 2021-09-07 | 陕西斯瑞新材料股份有限公司 | Method for preparing CuW90 material by using spherical tungsten powder |
| CN112063877A (en) * | 2020-09-25 | 2020-12-11 | 江西省科学院应用物理研究所 | Preparation method of copper-tungsten alloy |
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