CN112620631A - Method for preparing Mo-Cu alloy by field-assisted activation sintering - Google Patents
Method for preparing Mo-Cu alloy by field-assisted activation sintering Download PDFInfo
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- CN112620631A CN112620631A CN202011314911.3A CN202011314911A CN112620631A CN 112620631 A CN112620631 A CN 112620631A CN 202011314911 A CN202011314911 A CN 202011314911A CN 112620631 A CN112620631 A CN 112620631A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/04—Alloys based on tungsten or molybdenum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
The invention discloses a method for preparing a Mo-Cu alloy by field-assisted activation sintering, and belongs to the technical field of refractory metal processing. The method comprises the steps of carrying out wet grinding and vacuum drying on molybdenum powder and copper powder according to a certain component ratio to obtain Mo-Cu mixed powder, then putting the Mo-Cu mixed powder into a die to be pressed into a pressed compact, then putting the pressed compact into sintering equipment, and carrying out rapid sintering at a lower temperature by using a specific sintering process to obtain the Mo-Cu alloy. The invention provides a method for preparing Mo-Cu alloy by field-assisted activated sintering, aiming at the problems in the preparation of Mo-Cu alloy in the prior art, which can conveniently and effectively control the sintering process and can quickly obtain a Mo-Cu composite material with fine and compact crystal grains at a lower temperature. The invention utilizes the comprehensive action of three physical fields of an electric field, a thermal field and a force field to carry out activation sintering, so that the compact can quickly finish the densification process at a lower temperature, the preparation process is easy to control, and the sintering process does not need to add an activation element, thereby improving the product quality.
Description
Technical Field
The invention belongs to the technical field of refractory metal processing, and particularly relates to a method for preparing a Mo-Cu alloy by field-assisted activation sintering.
Background
Mo-Cu alloys are typically pseudoalloys composed of Mo and Cu elements that are neither in solid solution with each other nor form intermetallic compounds. The Mo-Cu alloy has the characteristics of high strength, high hardness, low expansion coefficient and the like of Mo, and also has the characteristics of high electric conductivity, heat conductivity and the like of Cu, and is applied to the fields of electric contacts, electrode materials, electronic packaging, thermal deposition materials, military equipment, aerospace, high-temperature gas part parts and the like of various high-voltage electric switches. It is noted that Mo-Cu alloys have less good heat resistance than W-Cu alloys with similar functions and properties, but are lighter and easier to process. Therefore, the Mo — Cu alloy is more advantageous in applications such as substrates, connectors, and heat dissipation elements, which require lightweight electronic packaging materials and heat sink materials.
The melting points of Mo and Cu are greatly different, wherein the melting point of Mo is up to 2622 ℃, and the melting point of Cu is 1083 ℃. The Mo-Cu alloy prepared by adopting a smelting method is difficult to prepare, and the prepared material has the problems of coarse grains, uneven microstructure distribution and the like, so that the advantages of the material are difficult to fully exert. At present, Mo-Cu alloy is generally prepared by a powder metallurgy method, and the commonly used method comprises a high-temperature liquid phase sintering method, an activation sintering method, an infiltration method, a discharge plasma sintering method and the like.
Yangchen et al (Yangchen, Qigong, Van Guangning, Yang zang Xin, Zhang Yabin, the influence of sintering temperature on the structure and performance of molybdenum-copper alloy) at the university of Liaoning industry, Mo-Cu alloy is prepared at 1550-1650 ℃ by a high-temperature liquid phase sintering method in the China molybdenum industry, 2020, 44 (2): 52-57. But the high-temperature liquid phase sintering temperature is high, the time is long, the energy consumption in the preparation process is large, and the cost is high; in addition, the crystal grains of the material are easy to grow in the high-temperature liquid phase sintering process, and the liquid phase copper is easy to seep out to cause the occurrence of holes in the material, thereby influencing the microstructure and the performance of the alloy.
In the activation sintering, a trace amount of an activating element such as Ni, Co, Fe or the like is usually added to a Mo-Cu mixture to enhance the sintering effect. The Mo-Cu alloy with different Ni contents in the activated element is prepared by heat preservation of 185-189 (2006, 11) through an activated sintering method at 1250 ℃ for 0.5-3 h. However, the introduction of the activating element may reduce the electric and thermal conductivity of the Mo-Cu alloy, thereby limiting the application range of the material.
The Mo-Cu alloy is prepared by sintering Zhao tiger and other people (Zhao tiger, Yangqili, Zhuang Fei, Liuren Zhi, Mo-Cu alloy infiltration process influence factor research in Mo industry of Jintu, 2019, 43 (2): 52-55.) for 60-120 minutes at the temperature of 1200-1350 ℃ by an infiltration method. However, because the sintering temperature of the infiltration method is higher, Mo crystal grains are easy to grow up, and the structure and the performance of the material are influenced; in addition, Cu not only can cause segregation in the infiltration process to influence the uniformity of the microstructure of the material, but also is easy to seep out of the framework, so that additional machining is needed, and the production cost is increased.
Guo Shi Bai et al (a method for rapidly preparing molybdenum-copper alloy, application publication No. CN 101942591A) at the university of Hunan science and technology prepares Mo-Cu alloy by using Spark Plasma Sintering (SPS). The sintering process comprises the following steps: the Mo-Cu mixed powder is loaded in a graphite die and then is put in a discharge plasma sintering device for sintering to obtain the Mo-Cu alloy, the sintering process is that the temperature is increased to 900-1300 ℃ at the speed of 100 ℃/min, the sintering pressure is 50MPa, the temperature is kept for 5min at the temperature, and then the Mo-Cu alloy is obtained by cooling along with the furnace. However, in this technique, a Mo — Cu mixed powder is generally charged into a graphite die and sintered in a spark plasma sintering apparatus, and not only is the amount of consumption of the die large, but also since an electric field is applied to both the powder and the die, that is, the electric field is only partially applied to the green compact, the accelerating action of the electric field on the sintering densification is not exhibited well.
In summary, the main preparation method of the current Mo-Cu alloy has the defects of high sintering temperature, long sintering time, serious grain growth and the like, or the performance of the Mo-Cu alloy is reduced due to the addition of the activating element; or the defects of complicated production process, high production cost and the like or the defects of high mold consumption and the like exist, so that the popularization and the application of the Mo-Cu alloy are limited to a certain extent.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method for preparing a Mo-Cu alloy by field-assisted activated sintering. The green compact is directly and rapidly heated by high current, and certain pressure is applied to two ends of a sample in the sintering process to realize field-assisted activated sintering. The Mo-Cu powder compact generates high Joule heat under the action of large current, and the temperature is rapidly increased to realize sintering; in addition, the high current can also induce a field emission effect, and can provide more energy for the diffusion and migration of atoms, thereby being beneficial to promoting the sintering densification of the material. Therefore, the Mo-Cu powder pressed compact is activated and sintered under the comprehensive action of three physical fields, namely an electric field, a thermal field and a force field, so that sintering densification can be realized at a lower temperature in a shorter time, and the Mo-Cu alloy with uniform and dense tissue distribution is obtained.
In order to achieve the above object, the present invention comprises the following steps.
1. Firstly, 65-95 wt% of Mo and 5-35 wt% of Cu powder are put into a stainless steel ball milling tank in a high-energy planetary ball mill to be subjected to wet milling and mixing uniformly (the ball milling rotation speed is 100-200 r/min, and the ball milling time is 4-12 hours), and then the powder is dried in a vacuum drying oven to obtain Mo-Cu mixed powder.
2. The Mo-Cu powder which is subjected to ball milling and uniform mixing is pressed into a pressed compact with the relative density of 65-75% in a die, then the pressed compact is placed in sintering equipment, and the electric field, the thermal field and the force field directly act on a green body to rapidly realize sintering densification under the conditions that the output voltage is 3-10V and the output current is 20000-50000A. At vacuum degree higher than 10-1And under the condition of Pa, heating to 750-900 ℃ at the heating rate of 10-75 ℃/s, applying 5-20 MPa pressure to two ends of the sample, preserving heat for 3-10 min, and then cutting off the power and cooling to obtain the Mo-Cu alloy.
According to the method for preparing the Mo-Cu alloy by field-assisted activated sintering, the granularity of the selected Mo powder is 3-15 mu m, and the granularity of the Cu powder is 1-15 mu m.
Compared with the prior art, the invention has the following positive effects.
1. The invention carries out activation sintering under the comprehensive action of three physical fields of an electric field, a thermal field and a force field, can accelerate element diffusion in a powder compact, is beneficial to densification of a sintered body, and further realizes the purpose of obtaining a dense Mo-Cu alloy under a lower temperature condition.
2. The Mo-Cu alloy is prepared by field-assisted activated sintering, so that the production process is simplified, the preparation period is greatly shortened, the energy consumption is reduced, the production cost is further saved, and the working condition of the preparation environment can be improved. Therefore, the energy consumption is low, the period is short, the efficiency is high, and the requirement of green production is met.
3. Because the Mo-Cu alloy sintered by the method has low sintering temperature and short sintering time, the grain growth of the sintered body can be effectively controlled, and an ultra-fine grain structure of about 0.1-3 mu m can be obtained, which is beneficial to improving the performance of the Mo-Cu alloy.
4. The method is simple and reliable, and is easy to adjust and control.
The technical solution of the present invention is further described in detail with reference to the accompanying drawings and embodiments.
Drawings
FIG. 1 is a microstructure diagram of a Mo-Cu alloy prepared in example 4 of the present invention.
FIG. 2 is a microstructure diagram of a Mo-Cu alloy prepared in example 6 of the present invention.
FIG. 3 is a microstructure diagram of a Mo-Cu alloy prepared in example 7 of the present invention.
Detailed Description
The following examples are given by way of illustration and description of the present invention and are not to be construed as limiting the scope of the invention, which is intended to be covered by the claims appended hereto.
The specific implementation steps of the invention are as follows.
Examples 1 to 16.
1. The preparation method comprises the following steps of respectively mixing molybdenum powder with the particle size of 3-15 mu m and copper powder with the particle size of 1-15 mu m according to the mass percentage listed in the table, putting the mixture into a high-energy planetary ball mill for wet grinding, and then performing vacuum drying to obtain Mo-Cu mixed powder.
2. And filling the Mo-Cu mixed powder into a die, and pressing into a pressed compact with a certain shape.
3. Placing the pressed blank in sintering equipment, and in an electric field with the output voltage of 3-10V and the output current of 20000-50000A, the vacuum degree is higher than 10-1And (2) under the condition of Pa, directly electrifying the pressed blank for rapid heating, heating the pressed blank to 750-900 ℃ at the heating rate of 10-75 ℃/s, applying 5-20 MPa pressure to two ends of the sample, preserving heat for 3-10 min, and then powering off to obtain the Mo-Cu alloy.
4. The shape of the blank is kept intact in the sintering process, and the densification degree of the obtained Mo-Cu alloy is high; the Mo-Cu alloys obtained by sintering the inventive examples 4, 6 and 7 were observed and photographed by a scanning electron microscope, and the photographs are shown in FIGS. 1, 2 and 3, respectively. As can be seen from the figure, the Mo-Cu alloy sintered by the method of the invention is more compact and the tissue structure distribution is more uniform, which shows that the Mo-Cu alloy with uniformly distributed and compact microstructure can be obtained by the field-assisted activated sintering method adopted by the invention.
Table 1 formulation and process conditions for each example of Mo-Cu alloys.
Claims (5)
1. A method for preparing Mo-Cu alloy by field-assisted activation sintering is characterized by comprising the following steps: the method comprises the steps of mixing molybdenum powder with the particle size of 3-15 microns and copper powder with the particle size of 1-15 microns according to a certain mass percentage, putting the mixture into a high-energy planetary ball mill for wet grinding and vacuum drying to obtain Mo-Cu mixed powder, pressing the Mo-Cu mixed powder into a pressed blank in a mold, putting the pressed blank into sintering equipment, and putting the pressed blank into the sintering equipment under the condition that the vacuum degree is higher than 10-1Under the condition of Pa, directly and rapidly heating the pressed blank by high current, heating the pressed blank to 750-900 ℃ at a certain heating rate, applying certain pressure to two ends of the sample, preserving heat, and finally, cutting off the power, cooling and taking out a sintered body to obtain the Mo-Cu alloy; the Mo-Cu powder compact of the invention is activated and sintered under the comprehensive action of three physical fields of an electric field, a thermal field and a force field, so thatWhile achieving sintering densification at lower temperatures and in a shorter time.
2. The method for preparing the Mo-Cu alloy by the field-assisted activated sintering according to claim 1, wherein the Mo-Cu alloy is prepared by the following steps: the sintering temperature of the method is 750-900 ℃.
3. The method for preparing the Mo-Cu alloy by the field-assisted activated sintering according to claim 1, wherein the Mo-Cu alloy is prepared by the following steps: the method controls the sintering temperature rise speed of the pressed compact to be 10-75 ℃/s.
4. The method for preparing the Mo-Cu alloy by the field-assisted activated sintering according to claim 1, wherein the Mo-Cu alloy is prepared by the following steps: the pressure applied by the method is 5-20 MPa.
5. The method for preparing the Mo-Cu alloy by the field-assisted activated sintering according to claim 1, wherein the Mo-Cu alloy is prepared by the following steps: the sintering heat preservation time of the method is 3-10 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113523273A (en) * | 2021-06-17 | 2021-10-22 | 北京科技大学 | Powder metallurgy method for rapidly preparing ultrafine crystal pure tungsten material under multi-field coupling |
| CN114850473A (en) * | 2022-04-13 | 2022-08-05 | 金堆城钼业股份有限公司 | Molybdenum and molybdenum alloy material sintering method and application thereof |
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| CN101942591A (en) * | 2010-07-31 | 2011-01-12 | 湖南科技大学 | Method for fast preparing molybdenum-copper alloy |
| CN104762498A (en) * | 2015-04-14 | 2015-07-08 | 中国工程物理研究院材料研究所 | Hot isostatic pressing preparation method of high-density molybdenum-copper alloy |
| CN107937748A (en) * | 2017-10-20 | 2018-04-20 | 四川大学 | A kind of method that tungsten molybdenum copper composite material is prepared with high current electrical resistance sintering |
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2020
- 2020-11-20 CN CN202011314911.3A patent/CN112620631A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59222555A (en) * | 1983-06-02 | 1984-12-14 | Nissan Motor Co Ltd | Wear-resistant sintered alloy |
| CN101942591A (en) * | 2010-07-31 | 2011-01-12 | 湖南科技大学 | Method for fast preparing molybdenum-copper alloy |
| CN104762498A (en) * | 2015-04-14 | 2015-07-08 | 中国工程物理研究院材料研究所 | Hot isostatic pressing preparation method of high-density molybdenum-copper alloy |
| CN107937748A (en) * | 2017-10-20 | 2018-04-20 | 四川大学 | A kind of method that tungsten molybdenum copper composite material is prepared with high current electrical resistance sintering |
Non-Patent Citations (1)
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| 刘艳芳，冯可芹，周虹伶，柯思璇: "烧结温度对大电流电场烧结制备W-Mo-Cu合金的影响", 《材料工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113523273A (en) * | 2021-06-17 | 2021-10-22 | 北京科技大学 | Powder metallurgy method for rapidly preparing ultrafine crystal pure tungsten material under multi-field coupling |
| CN113523273B (en) * | 2021-06-17 | 2022-10-21 | 北京科技大学 | Powder metallurgy method for rapidly preparing ultrafine crystal pure tungsten material under multi-field coupling |
| CN114850473A (en) * | 2022-04-13 | 2022-08-05 | 金堆城钼业股份有限公司 | Molybdenum and molybdenum alloy material sintering method and application thereof |
| CN114850473B (en) * | 2022-04-13 | 2024-02-02 | 金堆城钼业股份有限公司 | Sintering method and application of molybdenum and molybdenum alloy material |
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Application publication date: 20210409 |