CN103526060B - A kind of fast preparation method of copper-tungsten - Google Patents
A kind of fast preparation method of copper-tungsten Download PDFInfo
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- CN103526060B CN103526060B CN201310463859.1A CN201310463859A CN103526060B CN 103526060 B CN103526060 B CN 103526060B CN 201310463859 A CN201310463859 A CN 201310463859A CN 103526060 B CN103526060 B CN 103526060B
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Abstract
The present invention relates to the fast preparation method of a kind of copper-tungsten, belong to PM technique, New Metallurgical Technique and Microwave Sintering Techniques field。Metal tungsten powder and copper powder are carried out ball mill mixing according to mass percent 95～70wt%:5～30% respectively, then briquet compacting is carried out, make W skeleton briquet, load mullite crucible, and it is covered with copper powder around W skeleton briquet, then crucible is placed in microwave frequency be 2400～2500MHz, power 3～5KW, vacuum less than 0.1KPa when, temperature is risen to 1100～1300 DEG C and is sintered 1～3 hour by the firing rate keeping 15～20 DEG C/min, and namely natural cooling obtains copper-tungsten。Copper-tungsten even tissue that this method prepares, compact structure, relative density is up to 98.7%。
Description
Technical field
The present invention relates to PM technique, New Metallurgical Technique and Microwave Sintering Techniques field, particularly to the fast preparation method of a kind of copper-tungsten。
Background technology
Namely copper-tungsten has the high-melting-point of W, high density, electrical erosion resistance, resistance fusion welding and higher elevated temperature strength, has again high conductance and thermal conductivity, plasticity and the workability of Cu。Owing to substantial amounts of arc energy can be absorbed when Cu evaporates under high arc temperature, reduce arc temperature, improve use condition and reduce galvanic action, therefore be widely used as the electrical contact material of High-Voltage Electrical Appliances, also serve as the electrode of electric machining, die material and other require the occasion of electrical and thermal conductivity performance and applied at elevated temperature。At present, it is generally adopted infiltration method and activating solution phase sintering method prepares W-Cu material。But owing to W and Cu is biphase immiscible, therefore, tradition infiltration W-Cu material structure segregation, thick and relative density is low, additionally, activating solution phase sintering can introduce the performance of foreign peoples's impurity effect material。Microwave Sintering Techniques is that the special wave band utilizing microwave to have couples with material and produces heat, make the method that the heating of material entirety realizes densification to sintering temperature, it has compared with conventional sintering technique that sintering temperature is low, sintering time is short, energy utilization rate and efficiency of heating surface advantages of higher, and the workpiece made has higher density, hardness and obdurability, excellent combination property。
Application number is " a kind of microwave infiltration way sinters the method preparing W-CU alloy " of 2009103041144; be be pressed into W skeleton after copper powder and tungsten powder ball milling being mixed, electrolytic copper powder makes infiltration cu pressed compact; it is collectively disposed in alumina fibre insulation jacket with auxiliary heating material SiC sheet, then sinters in microwave condition and hybrid protection gas atmosphere and obtain。Foregoing invention is to utilize the sintering that the condition of Microwave-assisted firing SiC sheet and atmosphere protection realizes alloy to prepare; compared with traditional preparation methods; microwave can quickly heat SiC sheet; and transfer heat to alloy pressed compact; one indirectly heat exchange pattern in heat transfer, the rate of heat addition and energy conversion efficiency with microwave directly heat compared with low。
Summary of the invention
For overcoming the deficiencies in the prior art, the present invention proposes the fast preparation method of a kind of copper-tungsten, the method utilizes microwave to directly heat copper powder to melting, and realize the Fast Sintering to metal pressed compact under vacuum, compared with traditional heating mode, the method is that the special wave band being had by microwave is coupled with the basic fine structure of material and produces heat, makes material entirety heat to fusion temperature, has that firing rate is fast, energy conversion rate advantages of higher。
The present invention prepares copper-tungsten in conjunction with microwave metal smelting powder, Microwave Sintering Techniques, PM technique and melting infiltration sintering method, is a kind of method quickly preparing copper-tungsten。Concrete steps include as follows:
(1) metal tungsten powder and copper powder are carried out ball mill mixing according to mass percent 95～70wt%:5～30% respectively；
(2) tungsten powder and the copper powder that are mixed by ball milling in step (1) carry out briquet compacting, make W skeleton briquet；
(3) W skeleton briquet is loaded mullite crucible, and around W skeleton briquet, it is covered with the copper powder that thickness is 2～5mm, be subsequently placed in microwave frequency be 2400～2500MHz, power 3～5KW, vacuum less than 0.1KPa when, temperature is risen to 1100～1300 DEG C and sinters 1～3 hour by the firing rate keeping 15～20 DEG C/min, and namely natural cooling obtains copper-tungsten。
The granularity of described metal tungsten powder and copper powder is respectively less than 200 orders, and purity is all higher than 99.8wt%。
Ball milling 10～40min when be 1～50:1, rotating speed being 100～300r/min according to ratio of grinding media to material during described ball mill mixing。
Stress control 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 big, otherwise then little。
The invention has the beneficial effects as follows:
(1) major embodiment is quickly prepared, because being adopt microwave sintering, it is possible to direct fusion copper powder, has firing rate fast, and the feature that the thermal efficiency is high, by regulating microwave power, it is possible to melt copper powder at 40 ~ 50min；
(2) mullite crucible adopted is wave transparent type pottery, it is possible to achieve microwave directly heats the purpose of copper powder, and after the absorbing materials such as non-heated silicon carbide plate, indirectly heats again through thermaltransmission mode；
(3) infiltration copper used in the present invention is copper powder, but not metallic copper briquet, copper powder is namely as inhaling ripple carrier, again as infiltration material, sintering process at alloy is also possible to prevent alloy surface oxidation, utilizes the method except preparing copper-tungsten, also can ooze in process for copper at other and apply；
(4) present invention sinters under vacuum condition, non-atmosphere protection, and technological process is simple, and alloy property is also comparatively excellent。
Accompanying drawing explanation
Fig. 1 is the fast preparation method process chart of copper-tungsten of the present invention；
Fig. 2 is that the present invention adds the copper-tungsten micro-organization chart of melting infiltration sintering after 8% copper powder；
Fig. 3 is that the present invention adds the copper-tungsten micro-organization chart of melting infiltration sintering after 20% copper powder。
Detailed description of the invention
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) according to mass percent 92wt%:8wt%, metal tungsten powder and copper powder being carried out ball mill mixing respectively, ball milling mixes
Ball milling 40min when be 50:1, rotating speed being 100r/min according to ratio of grinding media to material during material；The granularity of metal tungsten powder and copper powder is 10～20 μm, and purity is more than 99.8wt%。
(2) tungsten powder and the copper powder that are mixed by ball milling in step (1) carry out briquet compacting, and Stress control, at 30MPa, makes cylindrical W skeleton briquet；
(3) W skeleton briquet is loaded mullite crucible, and around W skeleton briquet, it is covered with the copper powder that thickness is 3mm, it is subsequently placed in microwave frequency when being 2400MHz, power 5KW, vacuum 0.08KPa, temperature is risen to 1200 DEG C and sinters 1.2 hours by the firing rate keeping 20 DEG C/min, namely natural cooling obtains copper-tungsten, being analyzed by sample, copper-tungsten Brinell hardness is 229, and relative density is 95.4%。Microscopic structure is as shown in Figure 2。
Embodiment two: the fast preparation method of the copper-tungsten of present embodiment is:
(2) according to mass percent 80wt%:20%, metal tungsten powder and copper powder being carried out ball mill mixing respectively, ball milling mixes
Ball milling 20min when be 30:1, rotating speed being 200r/min according to ratio of grinding media to material during material；The granularity of metal tungsten powder and copper powder is respectively less than 200 orders, and purity is all higher than 99.8wt%。
(2) tungsten powder and the copper powder that are mixed by ball milling in step (1) carry out briquet compacting, and Stress control, at 45MPa, makes W skeleton briquet；
(3) W skeleton briquet is loaded mullite crucible, and around W skeleton briquet, it is covered with the copper powder that thickness is 2mm, be subsequently placed in microwave frequency be 2500MHz, power 3KW, vacuum less than 0.1KPa when, temperature is risen to 1300 DEG C and sinters 1 hour by the firing rate keeping 15 DEG C/min, namely natural cooling obtains copper-tungsten, being analyzed by sample, copper-tungsten Bu Shi is 221, and relative density is 98.7%。Microscopic structure is as shown in Figure 3。
Embodiment three: the fast preparation method of the copper-tungsten of present embodiment is:
(1) according to mass percent 95wt%:5%, metal tungsten powder and copper powder being carried out ball mill mixing respectively, ball milling mixes
Ball milling 10min when be 1:1, rotating speed being 300r/min according to ratio of grinding media to material during material；The granularity of metal tungsten powder and copper powder is respectively less than 200 orders, and purity is all higher than 99.8wt%。
(2) tungsten powder and the copper powder that are mixed by ball milling in step (1) carry out briquet compacting, and Stress control, at 25MPa, makes W skeleton briquet；
(3) W skeleton briquet is loaded mullite crucible, and around W skeleton briquet, it is covered with the copper powder that thickness is 5mm, be subsequently placed in microwave frequency be 2450MHz, power 3.5KW, vacuum less than 0.1KPa when, temperature is risen to 1100 DEG C and sinters 3 hours by the firing rate keeping 18 DEG C/min, and namely natural cooling obtains copper-tungsten。
Embodiment four: the fast preparation method of the copper-tungsten of present embodiment is:
(1) according to mass percent 70wt%:30%, metal tungsten powder and copper powder being carried out ball mill mixing respectively, ball mixes
Ball milling 30min when be 20:1, rotating speed being 200r/min according to ratio of grinding media to material during material；The granularity of metal tungsten powder and copper powder is respectively less than 200 orders, and purity is all higher than 99.8wt%。
(2) tungsten powder and the copper powder that are mixed by ball milling in step (1) carry out briquet compacting, and Stress control, at 25MPa, makes W skeleton briquet；
(3) W skeleton briquet is loaded mullite crucible, and around W skeleton briquet, it is covered with the copper powder that thickness is 2.5mm, be subsequently placed in microwave frequency be 2500MHz, power 3.8KW, vacuum less than 0.1KPa when, temperature is risen to 1250 DEG C and sinters 3 hours by the firing rate keeping 17 DEG C/min, and namely natural cooling obtains copper-tungsten。
Above in association with accompanying drawing, 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 that those of ordinary skill in the art possess, it is also possible to make various change under the premise without departing from present inventive concept。
Claims (1)
1. the fast preparation method of a copper-tungsten, it is characterised in that concrete steps include:
(1) metal tungsten powder and copper powder are carried out ball mill mixing according to mass percent 95～70wt%:5～30wt% respectively；
(2) tungsten powder and the copper powder that are mixed by ball milling in step (1) carry out briquet compacting, make W skeleton briquet；
(3) W skeleton briquet is loaded mullite crucible, and around W skeleton briquet, it is covered with the copper powder that thickness is 2～5mm, be subsequently placed in microwave frequency be 2400～2500MHz, power 3～5KW, vacuum less than 0.1KPa when, temperature is risen to 1100～1300 DEG C and sinters 1～3 hour by the firing rate keeping 15～20 DEG C/min, and namely natural cooling obtains copper-tungsten；
The granularity of described metal tungsten powder and copper powder is respectively less than 200 orders, and purity is all higher than 99.8wt%；
Ball milling 10～40min when be 1～50:1, rotating speed being 100～300r/min according to ratio of grinding media to material during described ball mill mixing；
The Stress control during compacting of described briquet is at 25～45MPa。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107052342A (en) * | 2017-03-08 | 2017-08-18 | 宁波高新区远创科技有限公司 | A kind of preparation method of corrosion-resistant lightning protection inter space material |
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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 |
| CN105039876B (en) * | 2015-07-06 | 2017-05-03 | 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 |
| 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 |
| 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 |
| 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 |
| 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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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107052342A (en) * | 2017-03-08 | 2017-08-18 | 宁波高新区远创科技有限公司 | A kind of preparation method of corrosion-resistant lightning protection inter space material |
| CN107052342B (en) * | 2017-03-08 | 2019-01-11 | 宁波高新区远创科技有限公司 | A kind of preparation method of corrosion-resistant lightning protection inter space material |
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