CN107671299A - A kind of method that vacuum aerosolization prepares Cu Cr alloy powders - Google Patents
A kind of method that vacuum aerosolization prepares Cu Cr alloy powders Download PDFInfo
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- CN107671299A CN107671299A CN201710759506.4A CN201710759506A CN107671299A CN 107671299 A CN107671299 A CN 107671299A CN 201710759506 A CN201710759506 A CN 201710759506A CN 107671299 A CN107671299 A CN 107671299A
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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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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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
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0844—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid in controlled atmosphere
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Abstract
The method that a kind of vacuum aerosolization disclosed by the invention prepares Cu Cr alloy powders, comprises the following steps, step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state；Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas, heating graphite crucible obtains aluminium alloy, and insulation makes the degree of superheat of aluminium alloy reach 50~250 DEG C, and preparation starts to be atomized；Step 3：Regulation atomizing pressure is 4~6MPa, the aluminium alloy obtained in step 2 is sprayed into spray chamber by graphite nozzle, atomization is broken to obtain Cu Cr alloy powders.Powder oxygen content produced by the present invention is less than 0.08%, and gained powder is atomized much smaller than normal atmospheric；In vacuum aerosolization, the fine powder recovery rate less than 50 μm can reach more than 60%.
Description
Technical field
The invention belongs to the preparation method technical field of copper alloy powder, and in particular to a kind of vacuum aerosolization prepares Cu-
The method of Cr alloy powders.
Background technology
Cu-Cr alloys have good combination property, and because its is excellent as a kind of high strength and high conductivity Cu alloy material
Mechanical characteristic and receive significant attention, it is one of current important integrated circuit frame material.Mainly pass through founding at present
Method and mechanical alloying method prepare Cu-Cr alloys, and the Cu-Cr alloy grains prepared by both approaches are thick, and composition be present
Segregation.And Cr size depends on the diameter of Cr powder in alloy prepared by powder metallurgic method, thus this method be difficult to obtain it is ultra-fine
The Cu-Cr alloys of Cr phases.Therefore, the original metal powder of particle diameter fine uniform is only made, can just prepare comprehensive
The excellent Cu-Cr alloys of energy.But metal powder granulates diameter made from existing electrolysis, mechanical crushing method it is more thick and
High energy consumption.And serious and in irregular shape, synthesis after compacting is aoxidized by Cu-Cr alloy powders made from traditional atomization
Performance is unsatisfactory.
The content of the invention
It is an object of the invention to provide a kind of method that vacuum aerosolization prepares Cu-Cr alloy powders, solve existing
Atomization made from Cu-Cr alloy powders oxidation it is serious and in irregular shape the problem of.
The technical solution adopted in the present invention is：A kind of method that vacuum aerosolization prepares Cu-Cr alloy powders, including with
Lower step,
Step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state；
Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas,
Heating graphite crucible obtains aluminium alloy, and insulation makes the degree of superheat of aluminium alloy reach 50~250 DEG C, and preparation starts to be atomized；
Step 3：Regulation atomizing pressure is 4~6MPa, and the aluminium alloy obtained in step 2 is sprayed into by graphite nozzle and is atomized
Room, atomization is broken to obtain Cu-Cr alloy powders.
The features of the present invention also resides in,
Pressure when atomizing furnace is evacuated to vacuum state in step 1 is 5x10-3~7x10-3Pa。
Step 2 heats to obtain aluminium alloy by high-frequency induction equipment.
The atomizing pressure adjusted in step 3 is 5MPa.
A diameter of 4mm of graphite nozzle in step 3.
The beneficial effects of the invention are as follows：The method that a kind of vacuum aerosolization of the present invention prepares Cu-Cr alloy powders, due to
Vacuum atomizing process is to carry out under an inert atmosphere, has effectively completely cut off contact of the aluminium alloy with oxygen, has avoided the oxidation of powder, because
Cu-Cr alloy powder oxygen content obtained by this vacuum aerosolization is very low；Meanwhile under the chilling effect of atomization, Cr is in Cu
Supersaturated solid solution is formed, by subsequent heat treatment Cr can be made to be separated out in the form of tiny particle, while keeps what is quickly solidified
Original small grains tissue, improve the intensity of alloy powder, and electric conductivity is restored.Powder oxygen content produced by the present invention
Less than 0.08%, gained powder is atomized much smaller than normal atmospheric；In vacuum aerosolization, the fine powder recovery rate less than 50 μm can reach
To more than 60%.
Brief description of the drawings
Fig. 1 is Cu-Cr alloy powder shape appearance figures made from atomization under atmospheric conditions；
Fig. 2 is that a kind of vacuum aerosolization of the present invention prepares different embodiments in the methods of Cu-Cr alloy powders and is prepared into
The Cu-Cr alloy powder shape appearance figures arrived.
Embodiment
Below in conjunction with the accompanying drawings and embodiment the present invention is described in detail.
The invention provides a kind of method that vacuum aerosolization prepares Cu-Cr alloy powders, comprise the following steps,
Step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state, pressure 5x10-3~7x10- 3Pa；
Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas,
Graphite crucible is heated by high-frequency induction equipment and obtains aluminium alloy, insulation makes the degree of superheat of aluminium alloy reach 50~250 DEG C, prepares
Start to be atomized；
Step 3：Regulation atomizing pressure is 4~6MPa, and the aluminium alloy obtained in step 2 is sprayed into by graphite nozzle and is atomized
Room, a diameter of 4mm of graphite nozzle, atomization is broken to obtain Cu-Cr alloy powders.
In the present invention based on principle be, by using the vacuum atomizing stove in routine techniques, mainly to there is vacuum acquirement survey
Amount and inflation system, induction smelting system, atomization chilling system, automatically controlled and water circulation system etc..Working chamber passes through with spray chamber
Graphite nozzle connects, and ceramic blocked shot is pressed on above nozzle during melting, rises ceramic bar during atomization, aluminium alloy is entered by nozzle
Spray chamber starts to be atomized.Pressure regulation system is provided between gas cylinder and atomizer, atomizer is internally provided with small structure, gives
The high pressure nitrogen of pressure acts on aluminium alloy into spray chamber by atomizer aperture as high pressure draught, is atomized aluminium alloy.
Embodiment 1
Step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state, pressure 5x10-3Pa；
Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas,
Graphite crucible is heated by high-frequency induction equipment and obtains aluminium alloy, insulation makes the degree of superheat of aluminium alloy reach 50 DEG C, prepares to start
Atomization；
Step 3：Regulation atomizing pressure is 4MPa, and the aluminium alloy obtained in step 2 is sprayed into spray chamber by graphite nozzle,
Atomization is broken to obtain Cu-Cr alloy powders, wherein, atomization opens air bleeding valve after carrying out 3s, it is ensured that atomization room pressure will not mistake
Height, closing air bleeding valve after the completion of aluminium alloy atomization prevents the oxidation of alloy powder, after the completion of measure alloy powder oxygen content and be less than
0.08%, wherein spherical powder recovery rate of the particle diameter less than 50 μm is 48%, and 50~150 μm of spherical powder recovery rates are 42%, its
He is the spherical powder more than 150 μm and minimal amount of special-shaped powder.
Embodiment 2
Step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state, pressure 5x10-3Pa；
Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas,
Graphite crucible is heated by high-frequency induction equipment and obtains aluminium alloy, insulation makes the degree of superheat of aluminium alloy reach 150 DEG C, prepares to start
Atomization；
Step 3：Regulation atomizing pressure is 5MPa, and the aluminium alloy obtained in step 2 is sprayed into spray chamber by graphite nozzle,
Atomization is broken to obtain Cu-Cr alloy powders, wherein, atomization opens air bleeding valve after carrying out 3s, it is ensured that atomization room pressure will not mistake
Height, closing air bleeding valve after the completion of aluminium alloy atomization prevents the oxidation of alloy powder, after the completion of measure alloy powder oxygen content and be less than
0.08%, wherein spherical powder recovery rate of the particle diameter less than 50 μm is 60.2%, and 50~150 μm of spherical powder recovery rates are 28%,
Other are the spherical powder more than 150 μm and minimal amount of special-shaped powder
Embodiment 3
Step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state, pressure 6x10-3Pa；
Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas,
Graphite crucible is heated by high-frequency induction equipment and obtains aluminium alloy, insulation makes the degree of superheat of aluminium alloy reach 150 DEG C, prepares to start
Atomization；
Step 3：Regulation atomizing pressure is 6MPa, and the aluminium alloy obtained in step 2 is sprayed into spray chamber by graphite nozzle,
Atomization is broken to obtain Cu-Cr alloy powders, wherein, atomization opens air bleeding valve after carrying out 3s, it is ensured that atomization room pressure will not mistake
Height, closing air bleeding valve after the completion of aluminium alloy atomization prevents the oxidation of alloy powder, after the completion of measure alloy powder oxygen content and be less than
0.09%, wherein spherical powder recovery rate of the particle diameter less than 50 μm is 55%, and 50~150 μm of spherical powder recovery rates are 32%, its
He is the spherical powder more than 150 μm and minimal amount of special-shaped powder
Embodiment 4
Step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state, pressure 6x10-3Pa；
Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas,
Graphite crucible is heated by high-frequency induction equipment and obtains aluminium alloy, insulation makes the degree of superheat of aluminium alloy reach 250 DEG C, prepares to start
Atomization；
Step 3：Regulation atomizing pressure is 5MPa, and the aluminium alloy obtained in step 2 is sprayed into spray chamber by graphite nozzle,
Atomization is broken to obtain Cu-Cr alloy powders, wherein, atomization opens air bleeding valve after carrying out 3s, it is ensured that atomization room pressure will not mistake
Height, closing air bleeding valve after the completion of aluminium alloy atomization prevents the oxidation of alloy powder, after the completion of measure alloy powder oxygen content and be less than
0.08%, wherein spherical powder recovery rate of the particle diameter less than 50 μm is 48%, and 50~150 μm of spherical powder recovery rates are 26%, its
He is the spherical powder more than 150 μm and minimal amount of special-shaped powder.
Embodiment 5
Step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state, pressure 7x10-3Pa；
Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas,
Graphite crucible is heated by high-frequency induction equipment and obtains aluminium alloy, insulation makes the degree of superheat of aluminium alloy reach 250 DEG C, prepares to start
Atomization；
Step 3：Regulation atomizing pressure is 6MPa, and the aluminium alloy obtained in step 2 is sprayed into spray chamber by graphite nozzle,
Atomization is broken to obtain Cu-Cr alloy powders, wherein, atomization opens air bleeding valve after carrying out 3s, it is ensured that atomization room pressure will not mistake
Height, closing air bleeding valve after the completion of aluminium alloy atomization prevents the oxidation of alloy powder, after the completion of measure alloy powder oxygen content and be less than
0.08%, wherein spherical powder recovery rate of the particle diameter less than 50 μm is 38%, and 50~150 μm of spherical powder recovery rates are 50%, its
He is the spherical powder more than 150 μm and minimal amount of special-shaped powder
Interpretation of result
Cu-Cr alloy powders obtained by big aerosolization as shown in Figure 1, wherein in the presence of a large amount of powder in irregular shape
Particle；A, b, c, d, e are followed successively by the Cu-Cr alloy powder shape appearance figures being prepared in embodiment 1-5 in Fig. 2, it can be seen that adopt
The Cu-Cr alloy powders microscopic appearance prepared with the present invention program is mainly the spherical of rule, there is very much minimal amount of club shaped structure,
Powder surface is smooth, and sphericity is high, and fine powder recovery rate is higher.
Claims (5)
1. a kind of method that vacuum aerosolization prepares Cu-Cr alloy powders, it is characterised in that comprise the following steps,
Step 1：Working chamber in vacuum atomizing stove and spray chamber are evacuated to vacuum state；
Step 2：Cu and Cr are put into the graphite crucible in working chamber, and N is filled with to working chamber2As protective gas, stone is heated
Black crucible obtains aluminium alloy, and insulation makes the degree of superheat of aluminium alloy reach 50~250 DEG C, and preparation starts to be atomized；
Step 3：Regulation atomizing pressure is 4~6MPa, and the aluminium alloy obtained in step 2 is sprayed into spray chamber by graphite nozzle,
Atomization is broken to obtain Cu-Cr alloy powders.
2. the method that a kind of vacuum aerosolization as claimed in claim 1 prepares Cu-Cr alloy powders, it is characterised in that described
Pressure when atomizing furnace is evacuated to vacuum state in step 1 is 5x10-3~7x10-3Pa。
3. the method that a kind of vacuum aerosolization as claimed in claim 1 prepares Cu-Cr alloy powders, it is characterised in that described
Step 2 heats to obtain aluminium alloy by high-frequency induction equipment.
4. the method that a kind of vacuum aerosolization as claimed in claim 1 prepares Cu-Cr alloy powders, it is characterised in that described
The atomizing pressure adjusted in step 3 is 5MPa.
5. the method that a kind of vacuum aerosolization as claimed in claim 1 prepares Cu-Cr alloy powders, it is characterised in that described
A diameter of 4mm of graphite nozzle in step 3.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109351982A (en) * | 2018-11-21 | 2019-02-19 | 陕西斯瑞新材料股份有限公司 | A kind of continuous production chromiumcopper milling method |
| CN110153438A (en) * | 2019-06-22 | 2019-08-23 | 陕西斯瑞新材料股份有限公司 | A kind of chromiumcopper powder by atomization technique of free-falling formula nozzle |
| CN110814356A (en) * | 2019-11-25 | 2020-02-21 | 西安和光明宸科技有限公司 | Preparation method of conductive nano copper powder |
| CN111014703A (en) * | 2019-12-26 | 2020-04-17 | 中天上材增材制造有限公司 | Preparation method of nickel-based alloy powder for laser cladding |
| CN111421135A (en) * | 2020-04-23 | 2020-07-17 | 西安理工大学 | Preparation method of copper-tin prealloying powder with ultrahigh tin content and controllable particle size |
| CN113134614A (en) * | 2021-04-22 | 2021-07-20 | 昆明冶金研究院有限公司 | Copper powder for low-oxygen spherical injection molding and preparation method thereof |
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| CN102423805A (en) * | 2011-11-23 | 2012-04-25 | 西安理工大学 | Preparation method of CuCr alloy powder with low chromium content |
| CN102728843A (en) * | 2012-07-12 | 2012-10-17 | 陕西斯瑞工业有限责任公司 | Preparation method for copper-chromium alloy powder and preparation method for copper-chromium contacts |
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| JPS61163223A (en) * | 1985-01-14 | 1986-07-23 | Sumitomo Electric Ind Ltd | Manufacture of copper-chromium alloy product |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109351982A (en) * | 2018-11-21 | 2019-02-19 | 陕西斯瑞新材料股份有限公司 | A kind of continuous production chromiumcopper milling method |
| CN109351982B (en) * | 2018-11-21 | 2021-12-03 | 陕西斯瑞新材料股份有限公司 | Powder making method for continuously producing copper-chromium alloy |
| CN110153438A (en) * | 2019-06-22 | 2019-08-23 | 陕西斯瑞新材料股份有限公司 | A kind of chromiumcopper powder by atomization technique of free-falling formula nozzle |
| CN110814356A (en) * | 2019-11-25 | 2020-02-21 | 西安和光明宸科技有限公司 | Preparation method of conductive nano copper powder |
| CN111014703A (en) * | 2019-12-26 | 2020-04-17 | 中天上材增材制造有限公司 | Preparation method of nickel-based alloy powder for laser cladding |
| CN111421135A (en) * | 2020-04-23 | 2020-07-17 | 西安理工大学 | Preparation method of copper-tin prealloying powder with ultrahigh tin content and controllable particle size |
| CN113134614A (en) * | 2021-04-22 | 2021-07-20 | 昆明冶金研究院有限公司 | Copper powder for low-oxygen spherical injection molding and preparation method thereof |
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Application publication date: 20180209 |