阅读说明：本技术 钨铜合金的制备方法及制备设备 (Preparation method and preparation equipment of tungsten-copper alloy ) 是由 李世杰 罗学萍 赖奇 程玉玲 张磊 游世建 于 2021-08-03 设计创作，主要内容包括：本发明提供了一种钨铜合金的制备方法,将电子束熔炼炉抽真空,利用电子枪组件向铜原料发射电子束,使铜液化并蒸发,形成铜蒸气；利用电子枪组件向钨原料发射电子束,使钨液化并蒸发,形成钨蒸气；钨蒸气与铜蒸气混合,得到铜钨混合蒸气,经过快速冷却降温后,铜钨混合蒸气凝固成为铜钨合金。还提供了一种钨铜合金的制备设备,包括电子束熔炼炉,所述电子束熔炼炉的顶部设置有电子枪组件,底部设置有原料放置机构,侧壁设置有进料机构,所述进料机构的出料端与原料放置机构相连。电子束熔炼本身具有提纯、精炼的作用,因此本发明的铜原料和钨原料可以是低成本的回收料,成本比只使用粉末冶金降低15％以上。(The invention provides a preparation method of tungsten-copper alloy, which comprises the steps of vacuumizing an electron beam smelting furnace, emitting electron beams to a copper raw material by using an electron gun assembly, liquefying and evaporating copper to form copper vapor; an electron gun assembly is utilized to emit electron beams to a tungsten raw material, so that tungsten is liquefied and evaporated to form tungsten vapor; and mixing the tungsten vapor and the copper vapor to obtain copper-tungsten mixed vapor, and solidifying the copper-tungsten mixed vapor into copper-tungsten alloy after rapid cooling. The preparation equipment of the tungsten-copper alloy comprises an electron beam melting furnace, wherein an electron gun assembly is arranged at the top of the electron beam melting furnace, a raw material placing mechanism is arranged at the bottom of the electron beam melting furnace, a feeding mechanism is arranged on the side wall of the electron beam melting furnace, and the discharging end of the feeding mechanism is connected with the raw material placing mechanism. The electron beam melting has the functions of purification and refining, so the copper raw material and the tungsten raw material can be recycled materials with low cost, and the cost is reduced by more than 15 percent compared with the cost only using powder metallurgy.)

1. The preparation method of the tungsten-copper alloy is characterized in that an electron beam melting furnace (1) is vacuumized, an electron gun assembly (2) is utilized to emit electron beams to a copper raw material, so that copper is liquefied and evaporated to form copper vapor; an electron gun component (2) is used for emitting electron beams to the tungsten raw material, so that tungsten is liquefied and evaporated to form tungsten vapor; and mixing the tungsten vapor and the copper vapor to obtain copper-tungsten mixed vapor, rapidly cooling the copper-tungsten mixed vapor to be lower than the melting point of copper, and solidifying the copper-tungsten mixed vapor into copper-tungsten alloy.

2. The method of producing a tungsten-copper alloy according to claim 1, wherein the copper raw material and the tungsten raw material are simultaneously charged into an electron beam melting furnace (1) with a space therebetween, and electron beams are emitted to the copper raw material and the tungsten raw material, respectively, by two sets of electron gun assemblies (2), so that the copper and the tungsten are simultaneously liquefied and vaporized to produce copper vapor and tungsten vapor.

3. The method for producing a tungsten-copper alloy according to claim 1 or 2, characterized in that: the upper portion of the inner cavity of the electron beam melting furnace (1) is provided with a horizontal substrate (3), the lower surface of the substrate (3) is provided with a heat insulation layer (4), a wavy cooling pipe (5) is arranged inside the substrate (3), when the copper-tungsten mixed steam moves to the upper portion of the substrate (3), a cooling medium is introduced into the cooling pipe (5), the copper-tungsten mixed steam above the substrate (3) is rapidly cooled to a melting point lower than copper, and the copper-tungsten mixed steam is solidified and attached to the upper surface of the substrate (3).

4. The method for producing a tungsten-copper alloy according to claim 1 or 2, characterized in that: the copper raw material and the tungsten raw material are in a cake shape, the electron beam of the electron gun assembly (2) scans the copper raw material and the tungsten raw material annularly, the scanning speed of the copper raw material is 5min-20min per revolution, and the scanning speed of the tungsten raw material is 10min-20min per revolution.

5. The method for producing a tungsten-copper alloy according to claim 1, wherein: the power of the electron gun assembly (2) for emitting electron beams to the copper raw material is 10kw-30kw, and the power of the electron gun assembly (2) for emitting electron beams to the tungsten raw material is 30kw-140 kw.

6. The method for producing a tungsten-copper alloy according to claim 1, wherein: after the copper raw material and the tungsten raw material are completely evaporated, the electron gun assembly (2) continuously emits electron beams for more than 1 hour, and then the copper-tungsten mixed vapor is cooled.

7. The apparatus for preparing tungsten-copper alloy according to any one of claims 1 to 6, comprising an electron beam melting furnace (1), wherein the electron beam melting furnace (1) is provided with an electron gun assembly (2) at the top, a raw material placing mechanism (6) at the bottom, and a feeding mechanism (7) at the side wall, and the discharge end of the feeding mechanism (7) is connected with the raw material placing mechanism (6).

8. The apparatus for producing a tungsten-copper alloy as claimed in claim 7, wherein: the electron gun assembly (2), the raw material placing mechanism (6) and the feeding mechanism (7) are two, and each raw material placing mechanism (6) is located below one electron gun assembly (2).

9. The apparatus for producing a tungsten-copper alloy as claimed in claim 7 or 8, wherein: a horizontal substrate (3) is arranged on the upper portion of an inner cavity of the electron beam melting furnace (1), a heat insulation layer (4) is arranged on the lower surface of the substrate (3), and a wavy cooling pipe (5) is arranged inside the substrate (3).

Technical Field

The invention relates to the technical field of tungsten-copper alloy preparation, in particular to a preparation method and preparation equipment of a tungsten-copper alloy.

Background

The tungsten-copper alloy is an alloy consisting of tungsten and copper, and the copper content of the common tungsten-copper alloy is 10-50%. The tungsten-copper alloy has good electrical and thermal conductivity, good high-temperature strength and certain plasticity. At very high temperatures, such as above 3000 ℃, copper in the alloy is liquefied and evaporated, a large amount of heat is absorbed, and the surface temperature of the material is reduced. Such materials are also known as metallic sweating materials. Because the melting points of tungsten and copper are different, the preparation efficiency is low and the cost is high. The existing preparation method comprises a powder metallurgy method, an injection molding method, a copper oxide method and a tungsten and molybdenum skeleton infiltration method. Particularly, due to the fact that the wettability of molybdenum copper is poorer than that of tungsten copper, when molybdenum copper with low copper content is prepared, the density of the infiltrated material is low, so that the air tightness, the electrical conductivity and the thermal conductivity of the material cannot meet the requirements, and the application of the material is limited. The technological process of preparing tungsten-copper alloy by powder metallurgy method includes powdering, mixing, press forming, sintering, infiltration and cold working. The process is complicated, the production efficiency is low, and the batch production is difficult.

The patent with the application number of 200610136919.9 provides a method for preparing a tungsten-copper alloy with 25-40 wt% of copper and the balance of tungsten and high copper content, wherein 5-20 wt% of copper powder with the purity of more than or equal to 99.5% and the granularity of 15-20 microns and tungsten powder with the same mass percentage as tungsten in the tungsten-copper alloy, the purity of more than or equal to 99% and the granularity of 3-6 microns are uniformly mixed and then are molded, a green compact with the porosity lambda controlled at 35 +/-2% is pre-sintered to obtain a tungsten-copper alloy framework, the copper infiltration amount is calculated, the copper powder with the purity of more than or equal to 99.5% and the granularity of less than 76 microns is molded into a copper sheet with the same size as the surface of the framework and is placed on the tungsten-copper alloy framework, the copper sheet is placed in a graphite crucible, and the copper infiltration is carried out by heating after aluminum oxide is adopted for filling; the obtained tungsten-copper alloy with high copper content has high compactness of more than 98 percent and excellent conductivity, and is suitable for electrical contacts and electrode materials, electronic packaging materials, high-temperature sweating materials and the like. However, the method has the defects of long process flow, large porosity of the tungsten-copper alloy framework, difficult adjustment of the content of copper and tungsten and still waiting for improvement of electric and heat conductivity. In addition, the production cost thereof is still high.

Disclosure of Invention

The invention aims to provide a preparation method and preparation equipment of a tungsten-copper alloy with lower cost.

The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the tungsten-copper alloy comprises the steps of vacuumizing an electron beam smelting furnace, emitting electron beams to a copper raw material by using an electron gun assembly, liquefying and evaporating copper to form copper vapor; an electron gun assembly is utilized to emit electron beams to a tungsten raw material, so that tungsten is liquefied and evaporated to form tungsten vapor; and mixing the tungsten vapor and the copper vapor to obtain copper-tungsten mixed vapor, and solidifying the copper-tungsten mixed vapor into copper-tungsten alloy after rapid cooling.

And further, putting the copper raw material and the tungsten raw material into an electron beam melting furnace at the same time, wherein a space is reserved between the copper raw material and the tungsten raw material, and two groups of electron gun assemblies are utilized to respectively emit electron beams to the copper raw material and the tungsten raw material, so that the copper and the tungsten are simultaneously liquefied and evaporated to generate copper vapor and tungsten vapor.

And furthermore, a horizontal substrate is arranged at the upper part of the inner cavity of the electron beam melting furnace, a heat insulation layer is arranged on the lower surface of the substrate, a wavy cooling pipe is arranged in the substrate, when the copper-tungsten mixed steam moves to the upper part of the substrate, a cooling medium is introduced into the cooling pipe, and the copper-tungsten mixed steam above the substrate is rapidly cooled to be lower than the melting point of copper, so that the copper-tungsten mixed steam is solidified and attached to the upper surface of the substrate.

Furthermore, the copper raw material and the tungsten raw material are in a cake shape, the electron beam of the electron gun assembly carries out annular scanning on the copper raw material and the tungsten raw material, the scanning speed of the copper raw material is 5min-20min per revolution, and the scanning speed of the tungsten raw material is 10min-20min per revolution.

Further, the power of an electron gun assembly for emitting an electron beam to the copper raw material is 10kw to 30kw, and the power of an electron gun assembly for emitting an electron beam to the tungsten raw material is 30kw to 140 kw.

Further, after the copper raw material and the tungsten raw material are completely evaporated, the electron gun assembly continues to emit electron beams for more than 1 hour, and then the copper-tungsten mixed vapor is cooled.

The tungsten-copper alloy preparation equipment used for the tungsten-copper alloy preparation method comprises an electron beam melting furnace, wherein an electron gun assembly is arranged at the top of the electron beam melting furnace, a raw material placing mechanism is arranged at the bottom of the electron beam melting furnace, a feeding mechanism is arranged on the side wall of the electron beam melting furnace, and the discharging end of the feeding mechanism is connected with the raw material placing mechanism.

Furthermore, the number of the electron gun assemblies, the number of the raw material placing mechanisms and the number of the feeding mechanisms are two, and each raw material placing mechanism is located below one electron gun assembly.

Furthermore, a horizontal base plate is arranged at the upper part of an inner cavity of the electron beam melting furnace, a heat insulation layer is arranged on the lower surface of the base plate, and a wavy cooling pipe is arranged in the base plate.

The invention has the beneficial effects that: 1. the electron beam melting has the functions of purification and refining, so the copper raw material and the tungsten raw material can be recycled materials with low cost, and the cost is reduced by more than 15 percent compared with the cost only using powder metallurgy. 2. The process is simple, the whole process can be carried out in an electron beam smelting furnace, the electron beam smelting furnace is a common device in the field of metallurgy at present, the process parameters such as smelting temperature and the like can be accurately controlled, and the quality of copper-tungsten alloy can be ensured. 3. The proportion of copper and tungsten can be adjusted, and the copper-tungsten alloy with high tungsten content can be prepared.

Drawings

FIG. 1 is a schematic diagram of a first embodiment;

FIG. 2 is a schematic view of the second embodiment;

FIG. 3 is a schematic top view of a substrate;

FIG. 4 is a schematic cross-sectional view of a substrate;

reference numerals: 1-electron beam smelting furnace; 2-an electron gun assembly; 3-a substrate; 4, a heat insulation layer; 5-a cooling pipe; 6, a raw material placing mechanism; 7-feeding mechanism.

Detailed Description

The invention is further illustrated with reference to the following figures and examples.

Example one

As shown in fig. 1, the apparatus for preparing tungsten-copper alloy comprises an electron beam melting furnace 1, wherein an electron gun assembly 2 is arranged at the top of the electron beam melting furnace 1, a raw material placing mechanism 6 is arranged at the bottom of the electron beam melting furnace, a feeding mechanism 7 is arranged on the side wall of the electron beam melting furnace, and the discharging end of the feeding mechanism 7 is connected with the raw material placing mechanism 6.

The electron gun assembly 2 comprises an electron gun and a rotating seat for mounting the electron gun, wherein the electron gun is a cold cathode electron gun, the maximum power is 600kw, the melting temperature can reach 10000 ℃, and the rotating seat can rotate in a certain range, so that the electron gun can perform annular scanning. The raw material placing mechanism 6 is used for placing raw materials, and can adopt a crucible, and the position of the crucible corresponds to the position of an electron gun, so that the electron beam of the electron gun can reach the raw materials on the crucible. The feeding mechanism 7 is used for feeding the raw material into the raw material placing mechanism 6, and the feeding mechanism 7 can specifically adopt an existing roller type feeder.

The raw materials for preparing the tungsten-copper alloy comprise a copper raw material and a tungsten raw material, the copper raw material and the tungsten raw material are preferably in a round cake shape, and during preparation, the copper raw material is firstly conveyed to a raw material placing mechanism 6 through a feeding mechanism 7. Then vacuumizing the electron beam melting furnace 1, specifically, performing first vacuumizing on the electron beam melting furnace, keeping the vacuum degree for 30min-1h after the vacuum degree reaches 2pa, and performing second vacuumizing to make the vacuum degree reach 5 multiplied by 10^-2pa. The copper-tungsten alloy can be prevented from being polluted by elements in the air through vacuumizing.

After vacuumizing, electron beams are emitted to the copper raw material by using the electron gun assembly 2, the power of the electron gun assembly 2 is 10-30 kw, so that copper is liquefied and evaporated to form copper vapor, and the internal space of the electron beam melting furnace 1 is filled with the copper vapor. After copper in the copper raw material is completely evaporated, the tungsten raw material is conveyed to the raw material placing mechanism 6 by the re-feeding mechanism 7, electron beams are emitted to the tungsten raw material by the electron gun assembly 2, the power of the electron gun assembly 2 is increased to 30kw-140kw, tungsten is liquefied and evaporated, and tungsten vapor is formed. When melting tungsten, the temperature of the copper vapor is further increased by the electron beam until it approaches the temperature of the tungsten vapor. And mixing the generated tungsten vapor with the copper vapor to obtain copper-tungsten mixed vapor, and rapidly cooling the copper-tungsten mixed vapor to be lower than the melting point of copper to solidify the copper-tungsten mixed vapor into copper-tungsten alloy. Because the solidifying point of copper is far lower than the solidifying point of tungsten, in order to ensure that copper and tungsten in the copper-tungsten alloy are uniformly distributed, the mixed vapor of copper and tungsten is rapidly cooled, so that the temperature of the mixed vapor of copper and tungsten is reduced to be below the melting point of copper in a short time, and the copper and tungsten are simultaneously condensed and solidified into a solid alloy.

In order to uniformly heat, liquefy and evaporate the copper raw material and the tungsten raw material, the copper raw material and the tungsten raw material are in a cake shape, the electron beam of the electron gun assembly 2 carries out annular scanning on the copper raw material and the tungsten raw material, the scanning speed of the copper raw material is 5min-20min per revolution, and the scanning speed of the tungsten raw material is 10min-20min per revolution.

In order to facilitate the control of the condensation and solidification of the copper-tungsten mixed vapor, as shown in fig. 1, 3 and 4, a horizontal substrate 3 is arranged at the upper part of the inner cavity of the electron beam melting furnace 1, the substrate 3 is made of high-temperature-resistant materials, the two substrates 3 are respectively arranged on two inner side walls of the electron beam melting furnace 1, the electron gun assembly 2 is positioned above the substrate 3, and a space is reserved between the two substrates 3, so that an electron beam emitted by the electron gun assembly 2 can reach a raw material below through the space. By adopting the position layout of the electron gun assembly 2 and the substrate 3, when the copper-tungsten mixed vapor moves above the substrate 3, the electron beam of the electron gun assembly 2 can continuously heat the copper-tungsten mixed vapor above the substrate 3, so that the temperature of the copper-tungsten mixed vapor is kept higher than the boiling point of tungsten.

The wavy cooling pipe 5 is arranged in the substrate 3, and a cooling medium can be introduced into the cooling pipe 5, wherein the cooling medium can be air, water or oil and the like and is used for cooling the copper-tungsten mixed vapor above the substrate 3. The lower surface of the substrate 3 is provided with a heat insulation layer 4, the heat insulation layer 4 is made of high-temperature-resistant heat insulation materials, and the cooling medium in the cooling pipe 5 is prevented from cooling the copper-tungsten mixed steam below the substrate 3. When the copper-tungsten mixed vapor moves to the position above the substrate 3, a cooling medium is introduced into the cooling pipe 5, and the copper-tungsten mixed vapor above the substrate 3 is rapidly cooled to a temperature lower than the melting point of copper, so that the copper-tungsten mixed vapor is solidified and attached to the upper surface of the substrate 3. Under the action of a cooling medium, the temperature of the upper surface of the substrate 3 and the space nearby the upper surface of the substrate 3 is very low, the mixed copper-tungsten vapor is gas and does irregular movement, when the mixed copper-tungsten vapor moves to the upper surface of the substrate 3 and the space nearby the upper surface of the substrate, the temperature drops suddenly, so that the mixed copper-tungsten vapor is condensed, liquefied and falls on the upper surface of the substrate 3 under the action of gravity to form a copper-tungsten alloy layer, after the gas nearby the upper surface of the substrate 3 is solidified, the gas pressure is reduced, the mixed copper-tungsten vapor at other parts can fill the space nearby the upper surface of the substrate 3 and is continuously condensed and solidified, and therefore the mixed copper-tungsten vapor is orderly and slowly cooled, and finally a copper-tungsten alloy block can be obtained on the upper surface of the substrate 3. By adopting the cooling mode, most of the mixed vapor of copper and tungsten can be attached to the upper surface of the substrate 3, only a small amount of mixed vapor of copper and tungsten is attached to the inner wall of the electron beam melting furnace 1, and the copper and tungsten material on the inner wall of the electron beam melting furnace 1 can be recovered after multiple times of melting preparation. The cooling temperature of the copper-tungsten mixed vapor can be controlled by controlling the flow and the temperature of the cooling medium, preferably, the cooling temperature is controlled to be about 800-1000 ℃, and after most of the copper-tungsten mixed vapor is condensed and solidified, the copper-tungsten alloy is cooled to room temperature by a natural cooling mode, so that impurity elements such as gasified hydrogen and oxygen can be prevented from entering the copper-tungsten alloy again when the copper raw material and the tungsten raw material are smelted, and the purity of the copper-tungsten alloy is improved.

In order to ensure that the components of the obtained copper-tungsten alloy are uniformly distributed, the electron gun assembly 2 continues to emit electron beams for more than 1 hour after tungsten in the tungsten raw material is completely evaporated, so that the temperature of copper vapor is uniform and equal to that of tungsten vapor, the copper vapor and the tungsten vapor are uniformly mixed, and then the copper-tungsten mixed vapor is cooled by adopting the mode.

Example two

As shown in fig. 2, the apparatus for preparing tungsten-copper alloy comprises an electron beam melting furnace 1, wherein 2 electron gun assemblies 2 are arranged at the top of the electron beam melting furnace 1, 2 raw material placing mechanisms 6 are arranged at the bottom of the electron beam melting furnace, 2 feeding mechanisms 7 are arranged on the side wall of the electron beam melting furnace, the discharge end of each feeding mechanism 7 is connected with one raw material placing mechanism 6, and each raw material placing mechanism 6 is located below one electron gun assembly 2. The structure and function of the electron gun assembly 2, the raw material placing mechanism 6 and the feeding mechanism 7 are the same as those of the first embodiment.

When preparing copper-tungsten alloy, putting copper raw materials and tungsten raw materials into two raw material placing mechanisms 6 of an electron beam smelting furnace 1 at the same time, wherein a certain distance is reserved between the two raw material placing mechanisms 6, so that a certain distance is reserved between the copper raw materials and the tungsten raw materials, and two groups of electron gun assemblies 2 are utilized to respectively emit electron beams to the copper raw materials and the tungsten raw materials, so that copper and tungsten are liquefied and evaporated at the same time, copper vapor and tungsten vapor are generated, and the electron beam smelting furnace 1 is filled with the copper vapor and the tungsten vapor and mixed into copper-tungsten mixed vapor. And after the copper raw material and the tungsten raw material are completely liquefied and evaporated, quickly cooling the temperature of the copper-tungsten mixed vapor to be below the melting point of copper, so that the copper-tungsten mixed vapor is condensed and solidified to obtain the copper-tungsten alloy.

In order to enable the copper-tungsten mixed steam to be condensed and solidified orderly and controllably, a horizontal base plate 3 is arranged at the upper part of an inner cavity of the electron beam melting furnace 1, a heat insulation layer 4 is arranged on the lower surface of the base plate 3, and a wavy cooling pipe 5 is arranged inside the base plate 3. Specifically, the cooling process is the same as in the first embodiment.

The copper raw material and the tungsten raw material are in a cake shape, the electron beam of the electron gun assembly 2 scans the copper raw material and the tungsten raw material annularly, the scanning speed of the copper raw material is 5min-20min per revolution, and the scanning speed of the tungsten raw material is 10min-20min per revolution, so that the copper raw material and the tungsten raw material are guaranteed to be smelted uniformly.

In order to ensure that the components of the obtained copper-tungsten alloy are uniformly distributed, the electron gun assembly 2 continues to emit electron beams for more than 1 hour after tungsten in the copper raw material and the tungsten raw material is completely evaporated, so that the temperature of the copper vapor is uniform and equal to that of the tungsten vapor, and the copper vapor and the tungsten vapor are uniformly mixed.

The copper raw material and the tungsten raw material can adopt cheap reclaimed materials, the cost is reduced by more than 15 percent compared with that of the method only using powder metallurgy, after the electron beam melting, the defects of pores and the like in the raw materials do not influence the quality of the copper-tungsten alloy, low-melting-point impurity elements such as hydrogen, oxygen, nitrogen and the like in the raw materials are gasified, and the low-melting-point impurity elements cannot enter the copper-tungsten alloy in the subsequent condensation and solidification process of the copper-tungsten mixed steam, so that the purity of the copper-tungsten alloy is ensured. In addition, the invention has simple process, can complete the whole preparation process in the electron beam melting furnace 1, and the electron beam melting furnace 1 is the existing common metallurgical equipment, has accurate and controllable process parameters, and ensures the quality of the copper-tungsten alloy. The tungsten content in the copper-tungsten alloy can be controlled by adjusting the proportion of the copper raw material and the tungsten raw material, so that the copper-tungsten alloy with high tungsten content can be prepared.

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.