CN101624662B - Method for preparing W-Cu alloy in microwave infiltration way - Google Patents
Method for preparing W-Cu alloy in microwave infiltration way Download PDFInfo
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- CN101624662B CN101624662B CN2009103041144A CN200910304114A CN101624662B CN 101624662 B CN101624662 B CN 101624662B CN 2009103041144 A CN2009103041144 A CN 2009103041144A CN 200910304114 A CN200910304114 A CN 200910304114A CN 101624662 B CN101624662 B CN 101624662B
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Abstract
The invention relates to a method for preparing W-Cu alloy in a microwave infiltration way, which comprises the following steps: 1. dispensing W powder and reduced Cu powder according to the weight percentage of W-3Cu, then ball-milling and mixing; 2. fetching the mixed powder and electrolytic copper powder according to design components, and respectively pressing the mixed powder under the pressure of 150-510MPa to form a cylindrical W framework and an infiltrated Cu pressed billet; 3. putting the pressed cylindrical W framework, the infiltrated Cu pressed billet and SiC slices into an alumina fiber heat-preserving sheath and then putting the sheath into an oven chamber of a microwave high-temperature oven, and vacuumizing the oven chamber to the vacuum degree within 100Pa by a vacuum pump; 4. injecting mixed protection gases of N2 and H2 into the oven chamber of the microwave oven, regulating the output power of the microwave high-temperature oven, heating to about 1350 DEG C at a temperature-rise speed of about 30 DEG C/min, preserving the heat, powering the microwave oven off and cooling to obtain the ideal alloy. The invention has simple process, convenient operation, short sintering period, low energy consumption and excellent performance of the obtained W-Cu alloy and can substitute for the prior process for preparing the W-Cu alloy in an infiltration way.
Description
Technical field
The invention discloses a kind of method of the W-Cu of preparation alloy.Be meant a kind of method of preparing W-Cu alloy in microwave infiltration way especially.
Background technology:
The W-Cu alloy is the pseudoalloy material that the copper by high-melting-point, high rigidity, low-expansion tungsten and high-ductility, high conduction, the capacity of heat transmission combines, and it has good anti-arc erosion, resistance fusion welding, fire-resistant oxidation resistant, intensity advantages of higher; Be widely used as at present in the industrial production such as electrical contact material, electronic package material, resistance welding, electrospark machining material, plasma spraying electrode materials and military project material.
Infiltration method is to prepare W-Cu alloy method commonly used on the industrial production, traditional technology normally in resistance furnace, take slowly heat-up rate (about 5-10 ℃/min) and measure such as medium temperature insulation, to avoid thermograde excessive and cause defectives such as alloy deformation, bubbling, the material relative density height that makes, over-all properties is good, but unique shortcoming is that the production technique cycle is long and complicated, the production cost height.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art and provide that a kind of technology is simple, easy to operate, the sintering period is short, energy consumption is low, the method for the preparing W-Cu alloy in microwave infiltration way of prepared W-Cu alloy property excellence.
The method of a kind of preparing W-Cu alloy in microwave infiltration way of the present invention comprises following processing step:
The first step: with purity greater than 99.9%, the W powder of 2 ~ 4 microns of mean particle sizes and purity greater than 99.7%, the reduction Cu powder of 20 ~ 50 microns of the mean particle sizes mass percent batching of pressing W-3Cu, ball milling mixes 5～7h;
Second step: add 0.5～1.5% stearic acid in the powder that combination drying is good and make binder, to improve its compactibility, press design mix, get powder mix and purity＞99.7%, the electrolytic copper powder that granularity is 60 ~ 90 microns is suppressed cylinder W skeleton and infiltration cu pressed compact respectively under the pressure of 150 ~ 510MPa;
The 3rd step: cylinder W skeleton, infiltration cu pressed compact and the boosting material SiC sheet that suppresses placed in the sapphire whisker insulation jacket, then, put into microwave high-temperature stove furnace chamber, and furnace chamber is evacuated in the vacuum tightness 100Pa with vacuum pump;
The 4th step: in micro-wave oven furnace chamber, feed N
2, H
2Hybrid protection gas is regulated microwave high-temperature stove output rating, is heated to 1300～1400 ℃ with the heat-up rate of 25～35 ℃/min, is incubated 15～25 minutes, closes microwave oven, promptly obtains the ideal alloy after the cooling.
Among the present invention, described ball milling mixes the employing planetary ball mill, and ball-milling medium is a dehydrated alcohol, and rotating speed is 100～200rpm, ratio of grinding media to material 2: 1.
Among the present invention, described boosting material SiC sheet addition is 100～140g.
Among the present invention, described N
2, H
2N in the hybrid protection gas
2, H
2The gas volume ratio is: N
2: H
2=(85～95): (5～15).
Among the present invention, described infiltration cu pressed compact is placed on cylinder W skeleton top integral body and places in the sapphire whisker insulation jacket.
Among the present invention, the Cu powder is an inductor in the described W-3Cu mixed powder.
The present invention is power owing to adopting above-mentioned processing method, utilizing microwave with the electromagnetic energy, is energy carrier, the inner features such as heat, volume heating of giving birth to the microwave, makes sintering process have characteristics such as heat-up rate is fast, sintering time weak point, energy utilization rate height.Studies have shown that microwave sintering can make that sintered article crystal grain is tiny, homogeneous microstructure, performance improve; And with short production cycle, save energy; Because microwave sintering is volume heating, overcome traditional sintering process and adopted resistance furnace slowly to heat up and medium temperature is incubated, excessive and cause defectives such as alloy deformation, bubbling to avoid thermograde; Simultaneously, in the microwave sintering process, add appropriate SiC and do the boosting material, both can promote being rapidly heated of sample, can make sample temperature more even again.Compared with prior art, the present invention has following advantage:
1. technology of the present invention is simple, energy expenditure is little, cost is lower.The alloy of employing microwave infiltration way method preparation only need can be finished whole sintering process in about 1 hour, and stove can take out in cold 1.5 hours.
2. the present invention adopts faster (30 ℃/min) heating of heat-up rates in the microwave high-temperature stove, the W-Cu alloy sample that sintering goes out is organized more even, microwave sintering has essential characteristics such as volume heating, non-thermal effect simultaneously, therefore, the W-Cu alloy phase of the present invention's preparation is more tiny than conventional infiltration method agglomerating alloy grain in resistance furnace, microstructure is more even, and performance all increases.
In sum, technology of the present invention is simple, easy to operate, the sintering period is short, energy consumption is low, prepared W-Cu alloy property excellence, and alternative existing infiltration method prepares the W-Cu alloy prior.
Embodiment:
Embodiment 1:
The first step: with purity greater than 99.9%, the W powder of 2 ~ 4 microns of mean particle sizes, purity greater than 99.7%, the reduction Cu powder of 20 ~ 50 microns of the mean particle sizes mass percent batching of pressing W-3Cu, adopt planetary ball mill in anhydrous ethanol medium with powder mixing 7h, rotating speed is 200rpm, ratio of grinding media to material 2: 1.
Second step: add 1.5% stearic acid in the powder that combination drying is good and make binder, to improve its compactibility.Take by weighing powder mix 10.2g and purity＞99.7% by the W-18Cu composition, the electrolytic copper powder 1.80g that granularity is 60 ~ 90 microns, suppressing diameter under 510MPa pressure respectively is cylinder W skeleton and the infiltration cu pressed compact of φ 18mm.
The 3rd step: cylinder W skeleton, infiltration cu pressed compact and the 140g boosting material SiC sheet that suppresses placed in the sapphire whisker insulation jacket, make the infiltration cu pressed compact be placed on cylinder W skeleton top, then, put into microwave high-temperature stove furnace chamber, and furnace chamber is evacuated in the vacuum tightness 100Pa with vacuum pump;
The 4th step: in micro-wave oven furnace chamber, feed N
2, H
2The gas volume ratio is: N
2: H
2=85: 15 N
2, H
2Hybrid protection gas is regulated microwave high-temperature stove output rating, is heated to 1400 ℃ with the heat-up rate of 35 ℃/min, is incubated 25 minutes, closes microwave oven, promptly obtains the ideal alloy after the cooling.
The alloy property parameter that cooling back obtains is: relative density reaches 97.7%, specific conductivity is 31.51%IACS, Brinell hardness (HB5) 214.
Embodiment 2:
The first step: with purity greater than 99.9%, the W powder of 2 ~ 4 microns of mean particle sizes, purity greater than 99.7%, the reduction Cu powder of 20 ~ 50 microns of the mean particle sizes mass percent batching of pressing W-3Cu, adopt planetary ball mill in anhydrous ethanol medium with powder mixing 6h, rotating speed is 150rpm, ratio of grinding media to material 2: 1.
Second step: add 1% stearic acid in the powder that combination drying is good and make binder, to improve its compactibility.Take by weighing powder mix 9.78g and purity＞99.7% by the W-20Cu composition, the electrolytic copper powder 2.02g that granularity is 60 ~ 90 microns, suppressing diameter under 460MPa pressure respectively is cylinder W skeleton and the infiltration cu pressed compact of φ 18mm.
The 3rd step: cylinder W skeleton, infiltration cu pressed compact and the 120g boosting material SiC sheet that suppresses placed in the sapphire whisker insulation jacket, make the infiltration cu pressed compact be placed on cylinder W skeleton top, then, put into microwave high-temperature stove furnace chamber, and furnace chamber is evacuated in the vacuum tightness 100Pa with vacuum pump;
The 4th step: in micro-wave oven furnace chamber, feed N
2, H
2The gas volume ratio is: N
2: H
2=90: 10 N
2, H
2Hybrid protection gas is regulated microwave high-temperature stove output rating, is heated to 1350 ℃ with the heat-up rate of 30 ℃/min, is incubated 20 minutes, closes microwave oven, promptly obtains the ideal alloy after the cooling.
The alloy property parameter that cooling back obtains is: relative density reaches 98.7%, specific conductivity is 32.15%IACS, Brinell hardness (HB5) 217.
Embodiment 3:
The first step: with purity greater than 99.9%, the W powder of 2 ~ 4 microns of mean particle sizes, purity greater than 99.7%, the reduction Cu powder of 20 ~ 50 microns of the mean particle sizes mass percent batching of pressing W-3Cu, adopt planetary ball mill in anhydrous ethanol medium with powder mixing 5h, rotating speed is 100rpm, ratio of grinding media to material 2: 1.
Second step: add 0.5% stearic acid in the powder that combination drying is good and make binder, to improve its compactibility.Take by weighing powder mix 8.82g and purity＞99.7% by the W-25Cu composition, the electrolytic copper powder 2.5g that granularity is 60 ~ 90 microns, compacting respectively under 150MPa pressure, diameter is cylinder W skeleton and the infiltration cu pressed compact of φ 18mm.
The 3rd step: cylinder W skeleton, infiltration cu pressed compact and the 100g boosting material SiC sheet that suppresses placed in the sapphire whisker insulation jacket, make the infiltration cu pressed compact be placed on cylinder W skeleton top, then, put into microwave high-temperature stove furnace chamber, and furnace chamber is evacuated in the vacuum tightness 100Pa with vacuum pump;
The 4th step: in micro-wave oven furnace chamber, feed N
2, H
2The gas volume ratio is: N
2: H
2=95: 5 N
2, H
2Hybrid protection gas is regulated microwave high-temperature stove output rating, is heated to 1300 ℃ with the heat-up rate of 25 ℃/min, is incubated 15 minutes, closes microwave oven, promptly obtains the ideal alloy after the cooling.
The alloy property parameter that cooling back obtains is: relative density reaches 98.7%, specific conductivity is 43.03%IACS, Brinell hardness (HB5) 196.
Claims (6)
1. the method for a preparing W-Cu alloy in microwave infiltration way comprises following processing step:
The first step: with purity greater than 99.9%, the W powder of 2 ~ 4 microns of mean particle sizes and purity greater than 99.7%, the reduction Cu powder of 20 ~ 50 microns of the mean particle sizes mass percent batching of pressing W-3Cu, ball milling mixes 5～7h;
Second step: add 0.5～1.5% stearic acid in the powder that combination drying is good and make binder, to improve its compactibility, press design mix, get powder mix and purity＞99.7%, the electrolytic copper powder that granularity is 60 ~ 90 microns is suppressed cylinder W skeleton and infiltration cu pressed compact respectively under the pressure of 150 ~ 510MPa;
The 3rd step: cylinder W skeleton, infiltration cu pressed compact and the boosting material SiC sheet that suppresses placed in the sapphire whisker insulation jacket, then, put into microwave high-temperature stove furnace chamber, and furnace chamber is evacuated in the vacuum tightness 100Pa with vacuum pump;
The 4th step: in micro-wave oven furnace chamber, feed N
2H
2Hybrid protection gas is regulated microwave high-temperature stove output rating, is heated to 1300～1400 ℃ with the heat-up rate of 25～35 ℃/min, is incubated 15～25 minutes, closes microwave oven, promptly obtains the ideal alloy after the cooling.
2. the method for a kind of preparing W-Cu alloy in microwave infiltration way according to claim 1 is characterized in that: described ball milling mixes and adopts planetary ball mill, and ball-milling medium is a dehydrated alcohol, and rotating speed is 100～200rpm, ratio of grinding media to material 2: 1.
3. the method for a kind of preparing W-Cu alloy in microwave infiltration way according to claim 1, it is characterized in that: described boosting material SiC sheet addition is 100～140g.
4. the method for a kind of preparing W-Cu alloy in microwave infiltration way according to claim 1 is characterized in that: described N
2H
2N in the hybrid protection gas
2H
2The gas volume ratio is: N
2: H
2=(85～95): (5～15).
5. the method for a kind of preparing W-Cu alloy in microwave infiltration way according to claim 1 is characterized in that: described infiltration cu pressed compact is placed on cylinder W skeleton top integral body and places in the sapphire whisker insulation jacket.
6. the method for a kind of preparing W-Cu alloy in microwave infiltration way according to claim 1, it is characterized in that: the Cu powder is an inductor in the described W-3Cu mixed powder.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103382534B (en) * | 2013-06-18 | 2016-03-09 | 武汉理工大学 | W-Cu-SiC ternary composite material and preparation method thereof |
| CN103526060B (en) * | 2013-10-09 | 2016-06-22 | 昆明理工大学 | A kind of fast preparation method of copper-tungsten |
| CN103882423B (en) * | 2013-12-25 | 2016-08-17 | 华侨大学 | A kind of method at Cu matrix surface microwave cladding CuW alloy |
| 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 |
| CN105568209B (en) * | 2016-03-04 | 2018-04-27 | 西安理工大学 | A kind of in-situ authigenic gradient WC strengthens the preparation method of CuW composite materials |
| CN110983210B (en) * | 2019-09-12 | 2021-05-28 | 全球能源互联网研究院有限公司 | Carbon fiber composite copper-tungsten alloy material and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483535A (en) * | 2003-06-30 | 2004-03-24 | 哈尔滨工业大学 | Method for preparing copper base electrode powder deformation compound material |
| CN1590571A (en) * | 2003-09-05 | 2005-03-09 | 上海材料研究所 | Tungsten copper functional composite material and its preparation technology |
| CN1728310A (en) * | 2005-06-15 | 2006-02-01 | 上海电器科学研究所（集团）有限公司 | Directional quick cooling method for manufacturing vacuum electrical contactor |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483535A (en) * | 2003-06-30 | 2004-03-24 | 哈尔滨工业大学 | Method for preparing copper base electrode powder deformation compound material |
| CN1590571A (en) * | 2003-09-05 | 2005-03-09 | 上海材料研究所 | Tungsten copper functional composite material and its preparation technology |
| CN1728310A (en) * | 2005-06-15 | 2006-02-01 | 上海电器科学研究所（集团）有限公司 | Directional quick cooling method for manufacturing vacuum electrical contactor |
Non-Patent Citations (2)
| Title |
|---|
| 宁超等.熔渗法制备的钨铜复合材料及其显微组织.《理化检验-物理分册》.2003,第39卷(第12期),第610、613页. * |
| 郭颖利等.W-Cu触头材料的微波烧结.《中南大学学报(自然科学版)》.2009,第40卷(第3期),第670-672页. * |
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