CN110125421A - A kind of preparation method of sheet CuFe alloy powder - Google Patents
A kind of preparation method of sheet CuFe alloy powder Download PDFInfo
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- CN110125421A CN110125421A CN201910322942.4A CN201910322942A CN110125421A CN 110125421 A CN110125421 A CN 110125421A CN 201910322942 A CN201910322942 A CN 201910322942A CN 110125421 A CN110125421 A CN 110125421A
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/068—Flake-like particles
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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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
- B22F2009/0848—Melting process before atomisation
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Abstract
The invention discloses a kind of preparation methods of sheet CuFe alloy powder, comprising the following steps: (1) ingredient takes electrolytic copper plate according to proportion and CuFe master alloy is raw material；(2) melting raw material is fitted into heating heating refining in the crucible in vacuum induction melting furnace；(3) it is atomized, the aluminium alloy of fusing is subjected to aerosolization processing；(4) wet ball grinding carries out flaky process to the alloy powder after atomization by mechanical ball mill；(5) powder is dried, and the powder after wet ball grinding is carried out drying post-processing and obtains sheet CuFe alloy powder.Two kinds of metal powders in sheet CuFe alloy powder that the present invention is prepared by way of atomizing humidifying performance method ball milling are uniformly mixed, it is easy to be sintered, and radius-thickness ratio is big, the interlaced bond strength for being conducive to improve coating between particle, suitable for preparing electrocondution slurry, industrial coating and electromagnetic wave shield film.
Description
Technical field
The invention belongs to field of alloy preparation technology, and in particular to a kind of preparation method of sheet CuFe alloy powder.
Background technique
In sintered metal product, copper powder and iron powder are the maximum two kinds of powder of dosage, the system of prior powder metallurgy product
Standby is to be used in mixed way copper powder, iron powder, and the two mixing is uneven and the two fusion temperature difference is larger, and sintering temperature is difficult to really
The features such as determining, the quality and performance for leading to manufactured goods are by serious influence；The production method of another copper iron compound powder is
Using diffusion method, copper powder and iron powder are mixed in a certain ratio uniformly, certain temperature is then heated to, copper powder is made to be coated on iron powder
Particle surface, due to this method be it is a kind of in a manner of physics copper clad on ferrous powder granules surface, there is also much not
Foot place.
In view of the above problems, we prepare copper-iron alloy powder by melting+atomization method, thoroughly solve two kinds
Powder mixes non-uniform problem and is difficult to the problem of being sintered, but in the practical application of powder, as conductive coating, brush plating are thin
Film etc., usually using the alloy powder of sheet.Sheet alloy powder has biggish radius-thickness ratio, and less amount can be used and obtain
Biggish masked area is obtained, and the interlaced bond strength etc. for being conducive to improve coating between particle.However the prior art
The application effect of the CuFe alloy powder of preparation is not ideal as expected, especially need to be improved in terms of electromagnetic shielding.
Summary of the invention
For the above technical problems, the present invention provides a kind of preparation method of sheet CuFe alloy powder.
The technical solution of the present invention is as follows: a kind of preparation method of sheet CuFe alloy powder, comprising the following steps:
(1) ingredient: taking electrolytic copper plate according to proportion and CuFe master alloy is raw material, for use；
(2) melting: the good raw material of said ratio is fitted into the crucible in vacuum induction melting furnace, when vacuum degree is extracted into р
When=2Pa-4Pa, gradient promotion heating power to 60KW-70KW is kept, and after raw material in crucible reaches uniformly up and down, drop adds
Thermal power is filled with protective gas to 10KW-20KW, boosts to 0.06Mpa-0.08Mpa, stops inflation, and power per liter to 70KW ±
5KW refines 1min-2min；
(3) it is atomized: the aluminium alloy of fusing being subjected to aerosolization processing, aerosolization pressure is 0.5MPa-10MPa, flow velocity control
System is in 4L/min-20L/min；
(4) flaky process, the alloy powder wet ball grinding: are carried out to the alloy powder after atomization by mechanical ball mill
Be 10:1 with the ratio of grinding media to material of ball-milling medium, Ball-milling Time 2h-12h, cooling time 2h-12h；
(5) powder is dried: the powder after wet ball grinding being carried out drying post-processing and obtains sheet CuFe alloy powder.
Further, the percentage composition of Fe element is 5%-30% in the CuFe master alloy.
Further, the gradient promotes the specific steps of heating power are as follows: first stage, heating power rise to 20KW-
30KW keeps the temperature 5min-10min；Second stage, heating power rise to 40KW-50KW, keep the temperature 5min-10min；Phase III adds
Thermal power rises to 60KW-70KW, keeps, and drops heating power to 10KW-20KW after raw material in crucible reaches uniformly up and down.
Further, the crucible is seriously affected using oxidation zirconium crucible containing the carbon in carbon crucible (such as graphite crucible)
The melting of copper-iron alloy.
Further, the protective gas is the argon gas of 99.9% or more purity.
Further, the ball-milling medium is that ethyl alcohol, soluble conductive macromolecular, graphene dispersing solution are according to mass ratio
7:2:1 composition.Ethyl alcohol reduces ball milling resistance as lubricant；Soluble conductive macromolecular can be embedded into mechanical milling process
In lamella sprills, the electric conductivity of sheet CuFe alloy powder can be improved, help to absorb microwave so as to improve electromagnetic screen
Performance is covered, the graphene in the graphene dispersing solution has porosity characteristic and low reflection characteristic, can equally be conducive to improve
Electromagnetic shielding performance.
Further, the soluble conductive macromolecular is Soluble Polypyrrole, soluble polyaniline, soluble poly thiophene
Any one or a few in pheno combines.
Further, the specific steps of the drying post-processing include:
(51) alloy powder after wet ball grinding is placed in vacuum drying box and is dried；
(52) using the alloy powder after the processing drying of electric field discharge processes, the positive ion bombardment alloy powder of ionization is utilized
Its surface irregularity degree is improved, and then improves wave-absorbing effect in surface；
(53) screening finally obtains varigrained sheet CuFe alloy powder.
Further, the method for the electric field discharge processes processing are as follows: the alloy powder after drying is laid in mold,
Using the one side for carrying alloy powder as field-transmitting cathode, the one side not contacted with alloy powder is as anode, discharge electric field
Intensity be 2 × 103-1×104Volt/cm, discharge time 10-30s.
Sheet CuFe alloy powder prepared by the present invention can be applied to electrocondution slurry, industrial coating and electromagnetic wave shield film
Preparation.
Compared with prior art, the invention has the benefit that the present invention is prepared by way of atomizing humidifying performance method ball milling
Sheet CuFe alloy powder in two kinds of metal powders be uniformly mixed, be easy to be sintered, and radius-thickness ratio is big, phase between particle
Mutually it is interleaved with the bond strength for being conducive to improve coating, soluble conductive macromolecular, the graphene dispersing solution being added in mechanical milling process
The electric conductivity that can be improved sheet CuFe alloy powder helps to absorb microwave so as to improve electromagnetic shielding performance, therefore special
Electrocondution slurry, industrial coating and electromagnetic wave shield film Shi Heyongyu not prepared.
Detailed description of the invention
Fig. 1 is sheet CuFe alloy powder pattern and X100 metallographic structure schematic diagram prepared by the embodiment of the present invention 2；
Fig. 2 is sheet CuFe alloy powder pattern and X500 metallographic structure schematic diagram prepared by the embodiment of the present invention 2.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
Embodiment 1
A kind of preparation method of sheet CuFe alloy powder, comprising the following steps:
(1) ingredient: taking the CuFe master alloy that the percentage composition of electrolytic copper plate and Fe element is 5% according to proportion is raw material,
For use；
(2) melting: the good raw material of said ratio is fitted into the crucible in vacuum induction melting furnace, wherein zirconium oxide earthenware
Crucible seriously affects the melting of copper-iron alloy containing the carbon in carbon crucible (such as graphite crucible).When vacuum degree is extracted into р=2Pa, add
Thermal power rises to 20KW, keeps the temperature 5min；Second stage, heating power rise to 40KW, keep the temperature 5min；Phase III heating power liter
It to 60KW, keeps, drops heating power to 10KW after raw material in crucible reaches uniformly up and down.It is filled with the argon of 99.9% or more purity
Gas boosts to 0.06Mpa, stops inflation, and power per liter to 70KW refines 1min；
(3) it is atomized: the aluminium alloy of fusing being subjected to aerosolization processing, aerosolization pressure is 0.5MPa, and flow control is in 4L/
min；
(4) flaky process, the alloy powder wet ball grinding: are carried out to the alloy powder after atomization by mechanical ball mill
Be 10:1 with the ratio of grinding media to material of ball-milling medium, Ball-milling Time 2h, cooling time 2h；The ball-milling medium is ethyl alcohol, solubility is led
Electric macromolecule (Soluble Polypyrrole), graphene dispersing solution are 7:2:1 composition according to mass ratio.Ethyl alcohol is reduced as lubricant
Ball milling resistance；Soluble conductive macromolecular can be embedded into lamella sprills in mechanical milling process, can be improved sheet
The electric conductivity of CuFe alloy powder helps to absorb microwave so as to improve electromagnetic shielding performance, in the graphene dispersing solution
Graphene has porosity characteristic and low reflection characteristic, can equally be conducive to improve electromagnetic shielding performance.
(5) powder is dried: the powder after wet ball grinding being carried out drying post-processing and obtains sheet CuFe alloy powder.
Embodiment 2
A kind of preparation method of sheet CuFe alloy powder, comprising the following steps:
(1) ingredient: taking the CuFe master alloy that the percentage composition of electrolytic copper plate and Fe element is 10% according to proportion is raw material,
For use；
(2) melting: the good raw material of said ratio is fitted into the crucible in vacuum induction melting furnace, wherein zirconium oxide earthenware
Crucible seriously affects the melting of copper-iron alloy containing the carbon in carbon crucible (such as graphite crucible).When vacuum degree is extracted into р=3Pa, add
Thermal power rises to 25KW, keeps the temperature 8min；Second stage, heating power rise to 45KW, keep the temperature 8min；Phase III heating power liter
It to 65KW, keeps, drops heating power to 15KW after raw material in crucible reaches uniformly up and down.It is filled with the argon of 99.9% or more purity
Gas boosts to 0.07Mpa, stops inflation, and power per liter to 75KW refines 2min；
(3) it is atomized: the aluminium alloy of fusing being subjected to aerosolization processing, aerosolization pressure is 5.5MPa, and flow control exists
12L/min；
(4) flaky process, the alloy powder wet ball grinding: are carried out to the alloy powder after atomization by mechanical ball mill
Be 10:1 with the ratio of grinding media to material of ball-milling medium, Ball-milling Time 7h, cooling time 7h；The ball-milling medium is ethyl alcohol, solubility is led
Electric macromolecule (soluble polyaniline), graphene dispersing solution are 7:2:1 composition according to mass ratio.Ethyl alcohol is reduced as lubricant
Ball milling resistance；Soluble conductive macromolecular can be embedded into lamella sprills in mechanical milling process, can be improved sheet
The electric conductivity of CuFe alloy powder helps to absorb microwave so as to improve electromagnetic shielding performance, in the graphene dispersing solution
Graphene has porosity characteristic and low reflection characteristic, can equally be conducive to improve electromagnetic shielding performance.
(5) powder is dried: the powder after wet ball grinding being carried out drying post-processing and obtains sheet CuFe alloy powder.
Embodiment 3
A kind of preparation method of sheet CuFe alloy powder, comprising the following steps:
(1) ingredient: taking the CuFe master alloy that the percentage composition of electrolytic copper plate and Fe element is 30% according to proportion is raw material,
For use；
(2) melting: the good raw material of said ratio is fitted into the crucible in vacuum induction melting furnace, wherein zirconium oxide earthenware
Crucible seriously affects the melting of copper-iron alloy containing the carbon in carbon crucible (such as graphite crucible).When vacuum degree is extracted into р=4Pa, add
Thermal power rises to 30KW, keeps the temperature 10min；Second stage, heating power rise to 50KW, keep the temperature 10min；Phase III heating power
70KW is risen to, is kept, drops heating power to 20KW after raw material in crucible reaches uniformly up and down.It is filled with 99.9% or more purity
Argon gas boosts to 0.08Mpa, stops inflation, and power per liter to 73KW refines 2min；
(3) it is atomized: the aluminium alloy of fusing being subjected to aerosolization processing, aerosolization pressure is 10MPa, and flow control is in 20L/
min；
(4) flaky process, the alloy powder wet ball grinding: are carried out to the alloy powder after atomization by mechanical ball mill
Be 10:1 with the ratio of grinding media to material of ball-milling medium, Ball-milling Time 12h, cooling time 12h；The ball-milling medium is ethyl alcohol, solubility
Conducting polymer (soluble polythiophene), graphene dispersing solution are 7:2:1 composition according to mass ratio.Ethyl alcohol is as lubricant, drop
Low ball grinds resistance；Soluble conductive macromolecular can be embedded into lamella sprills in mechanical milling process, can be improved sheet
The electric conductivity of CuFe alloy powder helps to absorb microwave so as to improve electromagnetic shielding performance, in the graphene dispersing solution
Graphene has porosity characteristic and low reflection characteristic, can equally be conducive to improve electromagnetic shielding performance.
(5) powder is dried: the powder after wet ball grinding being carried out drying post-processing and obtains sheet CuFe alloy powder.
Embodiment 4
The present embodiment and implementation 2 are essentially identical, the difference is that:
(5) powder is dried: the powder after wet ball grinding being placed in vacuum drying box and is dried, at electric field discharge processes
Alloy powder after reason drying, the method for the electric field discharge processes processing are as follows: the alloy powder after drying is laid in mold
It is interior, with a thickness of 1mm, using the one side for carrying alloy powder as field-transmitting cathode, the one side conduct that is not contacted with alloy powder
Anode, the intensity of discharge electric field are 2 × 103Volt/cm, discharge time 20s；Utilize the positive ion bombardment alloy powder table of ionization
Its surface irregularity degree is improved, and then improves wave-absorbing effect in face.Screening finally obtains varigrained sheet CuFe alloyed powder
End.
Embodiment 5
The present embodiment and implementation 2 are essentially identical, the difference is that:
(6) powder is dried: the powder after wet ball grinding being placed in vacuum drying box and is dried, at electric field discharge processes
Alloy powder after reason drying, the method for the electric field discharge processes processing are as follows: the alloy powder after drying is laid in mold
It is interior, with a thickness of 2mm, using the one side for carrying alloy powder as field-transmitting cathode, the one side conduct that is not contacted with alloy powder
Anode, the intensity of discharge electric field are 1 × 104Volt/cm, discharge time 30s；Utilize the positive ion bombardment alloy powder table of ionization
Its surface irregularity degree is improved, and then improves wave-absorbing effect in face.Screening finally obtains varigrained sheet CuFe alloyed powder
End.
Embodiment 6
The present embodiment and implementation 2 are essentially identical, the difference is that: the ball-milling medium is ethyl alcohol.
Experimental example
1, it chooses the sheet CuFe alloy powder prepared in embodiment 4 and carries out metallographic detection, testing result such as Fig. 1 and figure
Shown in 2, it can be seen that sheet is presented in CuFe metal powder pattern by Fig. 1-2, and radius-thickness ratio is big, interlaced between particle and table
Face more out-of-flatness.
2, the electromagnetic wave shield film being prepared into using the sheet CuFe alloy powder prepared in embodiment 1-6 and comparison
Example 1 (electromagnetic wave shield film that common sheet CuFe alloy powder is prepared into), and test and assess to its shield effectiveness, shielding effect
Energy (SE) is measured using the coaxial method of testing that National Bureau of Standards (NBS) recommends, and electromagnetic wave bands are 200MHz to 10GHz frequency
Rate range.Evaluating result is as shown in table 1:
Table 1: by the shield effectiveness of electromagnetic wave shield film prepared by embodiment 1-5 and 1 ultimate constituent of comparative example
| Shield effectiveness (dB) | |
| Embodiment 1 | 37-42 |
| Embodiment 2 | 40-45 |
| Embodiment 3 | 38-44 |
| Embodiment 4 | 44-50 |
| Embodiment 5 | 42-46 |
| Embodiment 6 | 35-37 |
| Comparative example 1 | 20-30 |
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment or equivalent replacement of some of the technical features；And
These are modified or replaceed, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (9)
1. a kind of preparation method of sheet CuFe alloy powder, which comprises the following steps:
(1) ingredient: taking electrolytic copper plate according to proportion and CuFe master alloy is raw material, for use；
(2) melting: the good raw material of said ratio is fitted into the crucible in vacuum induction melting furnace, when vacuum degree be extracted into р=
When 2Pa-4Pa, gradient promotes heating power to 60KW-70KW, keeps, after raw material in crucible reaches uniformly up and down, drops heating
Power is filled with protective gas to 10KW-20KW, boosts to 0.06Mpa-0.08Mpa, stops inflation, and power per liter to 70KW ±
5KW refines 1min-2min；
(3) it is atomized: the aluminium alloy of fusing being subjected to aerosolization processing, aerosolization pressure is 0.5MPa-10MPa, and flow control exists
4L/min-20L/min；
(4) flaky process, the alloy powder and ball wet ball grinding: are carried out to the alloy powder after atomization by mechanical ball mill
The ratio of grinding media to material of grinding media be 10:1, Ball-milling Time 2h-12h, cooling time 2h-12h；
(5) powder is dried: the powder after wet ball grinding being carried out drying post-processing and obtains sheet CuFe alloy powder.
2. a kind of preparation method of sheet CuFe alloy powder as described in claim 1, which is characterized in that the CuFe is female
The percentage composition of Fe element is 5%-30% in alloy.
3. a kind of preparation method of sheet CuFe alloy powder as described in claim 1, which is characterized in that the crucible is adopted
With oxidation zirconium crucible.
4. a kind of preparation method of sheet CuFe alloy powder as described in claim 1, which is characterized in that the protection gas
Body is the argon gas of 99.9% or more purity.
5. a kind of preparation method of sheet CuFe alloy powder as described in claim 1, which is characterized in that the ball milling is situated between
Matter be ethyl alcohol, soluble conductive macromolecular, graphene dispersing solution according to mass ratio be 7:2:1 composition.
6. a kind of preparation method of sheet CuFe alloy powder as described in claim 1, which is characterized in that the ball milling is situated between
Matter be ethyl alcohol, soluble conductive macromolecular, graphene dispersing solution according to mass ratio be 7:2:1 composition.
7. a kind of preparation method of sheet CuFe alloy powder as claimed in claim 6, which is characterized in that the solubility
Conducting polymer is Soluble Polypyrrole, any one or a few in soluble polyaniline, soluble polythiophene combines.
8. a kind of preparation method of sheet CuFe alloy powder as described in claim 1, which is characterized in that after the drying
The specific steps of processing include:
(51) alloy powder after wet ball grinding is placed in vacuum drying box and is dried；
(52) using the alloy powder after the processing drying of electric field discharge processes, the positive ion bombardment alloy powder table of ionization is utilized
Its surface irregularity degree is improved in face；
(53) screening finally obtains varigrained sheet CuFe alloy powder.
9. a kind of preparation method of sheet CuFe alloy powder as described in claim 1-8 any one, which is characterized in that
The sheet CuFe alloy powder can be applied to the preparation of electrocondution slurry, industrial coating and electromagnetic wave shield film.
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| CN111687424A (en) * | 2020-05-19 | 2020-09-22 | 陕西斯瑞新材料股份有限公司 | Preparation method and application of copper-iron alloy powder |
| CN111822710A (en) * | 2020-09-14 | 2020-10-27 | 陕西斯瑞新材料股份有限公司 | Preparation method of SLM (Selective laser melting) type 3D printing CuFe alloy |
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