CN112635189B - Production method of high-yield iron-nickel magnetic powder core - Google Patents
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- CN112635189B CN112635189B CN202011474893.5A CN202011474893A CN112635189B CN 112635189 B CN112635189 B CN 112635189B CN 202011474893 A CN202011474893 A CN 202011474893A CN 112635189 B CN112635189 B CN 112635189B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Abstract
The invention discloses a production method of a high-yield iron-nickel magnetic powder core, which comprises a) sieving the iron-nickel magnetic powder core with a particle size range of +200 to-325 meshesThe water atomized iron-nickel powder and the gas atomized iron-nickel powder are uniformly mixed to form mixed iron-nickel powder, and the mass fraction of the water atomized iron-nickel powder is 5-30%; b) Adding an insulating coating agent accounting for 0.1-0.5% of the weight of the mixed iron-nickel powder for passivation treatment, and fully and uniformly mixing; c) Adding a binder which is 0.5 to 2 percent of the weight of the mixed iron-nickel powder, fully mixing uniformly and drying; d) Adding a lubricant which accounts for 0.2 to 1 percent of the weight of the mixed iron-nickel powder to prepare powder suitable for molding; e) Placing the powder in a special die for molding to obtain an iron-nickel annular green body; f) Heat treatment of the green body in an atmosphere of N 2 And/or H 2 Under the protection, the temperature is 700-800 ℃, and a product after heat treatment is obtained. The invention has the advantages of high yield, insensitivity to heat treatment atmosphere, good sphericity of gas atomized powder, less powder impurities, low oxygen content, high relative molding density and the like.
Description
Technical Field
The invention relates to the technical field of metal soft magnetic materials, in particular to a production method of a high-yield iron-nickel magnetic powder core.
Background
At present, the method for producing the magnetic powder core of iron and nickel (wherein the Ni content is 45-55 percent, and the rest is Fe) by using iron and nickel powder mainly comprises the following steps:
the first method is to use water as medium to disperse liquid iron-nickel material into small particles by water cooling, then to further crush the small particles by ball milling or crushing process, then to screen them and to obtain iron-nickel powder with required mesh ratio, to passivate, insulate and cover by chemical method, finally to add lubricant to obtain corresponding iron-nickel powder, to form ring-shaped or other-shaped magnetic powder core by compression molding, to obtain semi-finished product of iron-nickel magnetic powder core under heat treatment of certain temperature and time, to coat the surface of the product with powder or liquid paint to obtain finished product of iron-nickel magnetic powder core. The iron-nickel magnetic powder core prepared by the method can be made into a relatively complex shape, the blank strength is good, the heat treatment yield is high, and the defects of large loss and low superposition performance of the magnetic powder core made of iron-nickel powder by a crushing method are overcome.
The second method is to use water atomized iron-nickel powder to produce iron-nickel magnetic powder core, mainly using water as medium, atomizing and cooling liquid iron-nickel material, sieving, obtaining iron-nickel powder with required mesh, then carrying out chemical passivation, insulation and coating, finally adding lubricant to obtain corresponding iron-nickel powder, carrying out compression molding on magnetic powder core with certain size and ring shape or other shapes, preparing semi-finished iron-nickel magnetic powder core under heat treatment of certain temperature and time, and finally coating the surface of the product with powder or liquid paint to obtain finished iron-nickel magnetic powder core. The iron-nickel magnetic powder core prepared by the method can be made into a relatively complex shape, the blank strength is good, the heat treatment yield is high, and the defects are that the magnetic powder core made of iron-nickel powder by a water atomization method has large loss and low superposition performance.
The third method is to use gas atomization iron-nickel powder to produce iron-nickel magnetic powder core. With the maturity of the existing atomization powder preparation process, using liquid N 2 The gasified iron-nickel powder is sprayed and cooled with medium to produce iron-nickel powder, which is then screened and proportioned to obtain iron-nickel powder with required mesh number, and then passivated, insulated and coated by chemical method, finally added with lubricant to produce corresponding iron-nickel powder, and then pressed into ring-shaped or other-shaped magnetic powder core with certain size, and heat treated at certain temperature and time to produce semi-finished iron-nickel magnetic powder core, and finally the surface of the product is coated with powder or liquid paint to obtain the finished iron-nickel magnetic powder core. The iron-nickel magnetic powder core prepared by the method has low loss and high superposition performance, but the powder is spherical or spheroidal and is difficult to form during forming and pressing, the shape of the prepared magnetic powder core product is simple, the strength of a blank is poor, and the heat treatment yield is not high.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a method for preparing iron-nickel powder by mixing iron-nickel powder with different properties, comprehensively utilizing the advantages of the three iron-nickel powder and overcoming the defects of the three iron-nickel powder, so that the prepared product has good green strength, keeps higher stacking property and lower product loss, and has the characteristics of more loose atmosphere and temperature change range in heat treatment.
The technical scheme adopted by the invention is as follows: the production method of the iron-nickel magnetic powder core with high yield comprises the following steps:
a) Uniformly mixing water atomized iron-nickel powder with the granularity range of +200 to-325 meshes and gas atomized iron-nickel powder in a mixer to form mixed iron-nickel powder, wherein the mass fraction of the water atomized iron-nickel powder in the mixed iron-nickel powder is 5-30%;
b) Adding an insulating coating agent accounting for 0.1-0.5 percent of the weight of the mixed iron-nickel powder for passivation treatment, fully and uniformly mixing, and generating a layer of oxide on the surface of the iron-nickel powder;
c) Adding a binder accounting for 0.5-2% of the weight of the mixed iron-nickel powder, fully and uniformly mixing, and drying the mixed iron-nickel powder through natural air drying for 24 hours or drying for 2-4 hours;
d) Adding a lubricant which accounts for 0.2 to 1 percent of the weight of the mixed iron-nickel powder to prepare powder suitable for forming;
e) Placing the powder treated in the step d) into a special die for molding, wherein the pressure is 1.9-2.3 GPa, and preparing an iron-nickel annular green body;
f) Heat treating the green body in an atmosphere of N 2 And/or H 2 Under the protection, the temperature is 700-800 ℃, and the product is taken out for about 4 hours from the temperature rise to the temperature reduction, so that the product after heat treatment is obtained. In the heat treatment of green bodies, O is to be prevented 2 Thus requiring a shielding gas, pure H 2 Is the best because of H 2 Having a reducing action, followed by H 2 And N 2 Mixed gas (industrial by NH) 3 Decomposed to) again is N 2 N used in industry 2 Usually liquid nitrogen or N obtained by air separation, the cost of liquid nitrogen is high, the cost of nitrogen prepared by air separation is low, but the purity of the nitrogen is lower than that of liquid nitrogen, and the invention can prepare N by air separation 2 And carrying out green body heat treatment in the atmosphere.
Preferably, step f) is followed by:
g) And (3) soaking the heat-treated product in an impregnation liquid for 10 minutes, washing the surface impregnation liquid, standing for 24 hours, and then curing and heating in an oven at the temperature of not more than 230 ℃ to obtain the reinforced iron-nickel product.
Preferably, step g) is followed by:
h) And chamfering the reinforced iron-nickel product, wherein C is 0.5-1.5, and removing sharp corner edges.
Preferably, step h) is followed by:
i) Coating epoxy resin on the surface of the product to obtain a finished product of the iron-nickel magnetic powder core.
Preferably, the insulating coating agent comprises phosphoric acid, the phosphoric acid needs to be diluted by alcohol or acetone, and the dilution ratio is the mass of the phosphoric acid: the mass =1 of alcohol or acetone.
Preferably, the binder is one or more of kaolin or a water glass solution, i.e. an aqueous sodium silicate solution.
Preferably, the lubricant is one or more of stearic acid, graphite or molybdenum disulphide.
The invention has the beneficial effects that:
(1) The invention adopts the method of combining the water atomized powder and the gas atomized powder, thereby not only keeping the forming performance of the water atomized powder.
(2) Insensitivity to heat treatment atmosphere, compared with gas atomization, only in high-purity liquid N 2 Or H 2 Under the atmosphere of (2), the invention can separate N prepared by air 2 And/or H 2 Is operated under an atmosphere of (c). That is, the invention reduces the requirement of the green body on the protective atmosphere in the heat treatment process, and can separate the N from the air with the maximum oxygen content of 50PPM 2 The temperature is changed within 700-800 ℃ without obvious performance difference (mainly referring to Q value or loss change).
(3) The invention uses water atomization iron nickel powder, which is added to be evenly mixed with gas atomization iron nickel powder, and can strengthen the combination between the two powders during molding, so that the green compact has higher density and increased strength, and the invention also has the characteristics of good sphericity, less powder impurities, low oxygen content (the superposition and loss characteristics can be obviously improved), high molding relative density and great improvement in molding.
(4) The invention improves the yield of the original pure gas atomization iron-nickel production from about 70% to about 90%.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below, but the embodiments of the present invention are not limited thereto.
Example 1:
a) Uniformly mixing water atomized iron-nickel powder with the granularity range of +200 to-325 meshes and gas atomized iron-nickel powder in a mixer to form mixed iron-nickel powder, wherein the mass fraction of the water atomized iron-nickel powder in the mixed iron-nickel powder is 5%; the particle size ratio is as follows: 5% of +200 meshes, 45% of-200- +325 meshes and 50% of-325 meshes.
b) Adding an insulating coating agent accounting for 0.2 percent of the weight of the mixed iron-nickel powder for passivation treatment, and fully and uniformly mixing, wherein the insulating coating agent is phosphoric acid diluted by alcohol.
c) Adding a binder accounting for 1.5 percent of the weight of the mixed iron-nickel powder, fully and uniformly mixing, and drying for 4 hours; wherein the binder is kaolin.
d) Adding a lubricant accounting for 0.5 percent of the weight of the mixed iron-nickel powder to prepare powder suitable for molding; wherein the lubricant is graphite.
e) Placing the powder treated in the step d) into a special mould for forming, wherein the pressure is 2.1GPa, and preparing an iron-nickel annular green body;
f) Heat treating the green body in an atmosphere of N 2 And H 2 Under the protection of the mixed gas, the temperature is 780 ℃, and a product after heat treatment is obtained.
g) And (3) soaking the heat-treated product in the soaking solution for 10 minutes, washing the soaking solution on the surface, standing for 24 hours, and curing and heating in an oven at the temperature of not more than 230 ℃ to obtain the reinforced iron-nickel product.
h) And chamfering the reinforced iron-nickel product, wherein C is 0.5-1.5, and removing sharp corner edges.
i) Coating epoxy resin on the surface of the product to obtain a finished product of the iron-nickel magnetic powder core.
Table 1 shows the test data of the finished product of the iron-nickel magnetic powder core of this example, wherein 3 products were randomly selected from each batch of products for testing, and the iron-nickel annular green compact of this example is a typical 106 product, and has an outer diameter of 26.92mm, an inner diameter of 14.73mm and a height of 11.18mm.
TABLE 1
Example 2
a) Uniformly mixing water atomized iron-nickel powder with the granularity range of +200 to-325 meshes and gas atomized iron-nickel powder in a mixer to form mixed iron-nickel powder, wherein the mass fraction of the water atomized iron-nickel powder in the mixed iron-nickel powder is 10%; the particle size ratio is as follows: the content of +200 meshes is 2.5%, the content of-200 to +325 meshes is 40%, and the content of-325 meshes is 57.5%.
b) Adding an insulating coating agent accounting for 0.5 percent of the weight of the mixed iron-nickel powder for passivation treatment, and fully and uniformly mixing, wherein the insulating coating agent is phosphoric acid diluted by acetone.
c) Adding a binder accounting for 0.5 percent of the weight of the mixed iron-nickel powder, fully and uniformly mixing, and drying for 4 hours; wherein the binder is kaolin.
d) Adding a lubricant which accounts for 0.5 percent of the weight of the mixed iron-nickel powder to prepare powder suitable for forming; wherein the lubricant is stearic acid.
e) Placing the powder treated in the step d) into a special mould for forming, wherein the pressure is 2.1GPa, and preparing an iron-nickel annular green body;
f) Heat treating the green body in an atmosphere of N 2 Under the protection of (2), the temperature is 700 ℃, and a product after heat treatment is obtained.
g) And (3) soaking the heat-treated product in an impregnation liquid for 10 minutes, washing the surface impregnation liquid, standing for 24 hours, and then curing and heating in an oven at the temperature of not more than 230 ℃ to obtain the reinforced iron-nickel product.
h) And chamfering the reinforced iron-nickel product, wherein C is 0.5-1.5, and removing sharp corner edges.
i) Coating epoxy resin on the surface of the product to obtain a finished product of the iron-nickel magnetic powder core.
Table 2 shows the test data of the finished product of the iron-nickel magnetic powder core of this example, wherein 3 products were randomly selected from each batch of products for testing, and the iron-nickel annular green compact of this example is a typical 106 product, and has an outer diameter of 26.92mm, an inner diameter of 14.73mm and a height of 11.18mm.
TABLE 2
Example 3
a) Uniformly mixing water atomized iron-nickel powder with the granularity range of +200 to-325 meshes and gas atomized iron-nickel powder in a mixer to form mixed iron-nickel powder, wherein the mass fraction of the water atomized iron-nickel powder in the mixed iron-nickel powder is 15%; the particle size ratio is as follows: 5% of +200 meshes, 45% of-200- +325 meshes and 50% of-325 meshes.
b) Adding an insulating coating agent accounting for 0.1 percent of the weight of the mixed iron-nickel powder for passivation treatment, and fully and uniformly mixing, wherein the insulating coating agent is phosphoric acid diluted by alcohol.
c) Adding a binder accounting for 2 percent of the weight of the mixed iron-nickel powder, fully and uniformly mixing, and carrying out drying treatment for 4 hours; wherein the binder is water glass solution.
d) Adding a lubricant accounting for 0.5 percent of the weight of the mixed iron-nickel powder to prepare powder suitable for molding; wherein the lubricant is molybdenum disulfide.
e) Placing the powder treated in the step d) in a special mould for forming under the pressure of 2.1GPa to obtain an iron-nickel annular green body;
f) Heat treatment of the green body in an atmosphere of N 2 And H 2 Under the protection of the mixed gas, the temperature is 750 ℃, and a product after heat treatment is obtained.
g) And (3) soaking the heat-treated product in an impregnation liquid for 10 minutes, washing the surface impregnation liquid, standing for 24 hours, and then curing and heating in an oven at the temperature of not more than 230 ℃ to obtain the reinforced iron-nickel product.
h) And chamfering the reinforced iron-nickel product, wherein C is 0.5-1.5, and removing sharp corner edges.
i) Coating epoxy resin on the surface of the product to obtain a finished product of the iron-nickel magnetic powder core.
Table 3 shows the test data of the finished product of the iron-nickel magnetic powder core of this embodiment, 3 products are randomly selected from each batch of products for testing, and the annular iron-nickel green compact of this embodiment is a typical 106 product, with an outer diameter of 26.92mm, an inner diameter of 14.73mm, and a height of 11.18mm.
TABLE 3
Example 4
a) Uniformly mixing water atomized iron-nickel powder with the granularity range of +200 to-325 meshes and gas atomized iron-nickel powder in a mixer to form mixed iron-nickel powder, wherein the mass fraction of the water atomized iron-nickel powder in the mixed iron-nickel powder is 20%; the particle size ratio is as follows: the +200 meshes account for 2.5%, the-200- +325 meshes account for 40%, and the-325 meshes account for 57.5%.
b) Adding an insulating coating agent accounting for 0.2 percent of the weight of the mixed iron-nickel powder for passivation treatment, and fully and uniformly mixing, wherein the insulating coating agent is phosphoric acid diluted by alcohol.
c) Adding a binder accounting for 1.5 percent of the weight of the mixed iron-nickel powder, fully and uniformly mixing, and drying for 4 hours; wherein the binder is water glass solution.
d) Adding a lubricant which accounts for 0.5 percent of the weight of the mixed iron-nickel powder to prepare powder suitable for forming; wherein the lubricant is molybdenum disulfide.
e) Placing the powder treated in the step d) into a special mould for forming, wherein the pressure is 2.1GPa, and preparing an iron-nickel annular green body;
f) Heat treatment of the green body in an atmosphere H 2 Under the protection of (2), the temperature is 800 ℃, and a product after heat treatment is obtained.
g) And (3) soaking the heat-treated product in the soaking solution for 10 minutes, washing the soaking solution on the surface, standing for 24 hours, and curing and heating in an oven at the temperature of not more than 230 ℃ to obtain the reinforced iron-nickel product.
h) And chamfering the reinforced iron-nickel product, wherein C is 0.5-1.5, and removing sharp corner edges.
i) Coating epoxy resin on the surface of the product to obtain a finished product of the iron-nickel magnetic powder core.
Table 4 shows the test data of the finished product of the iron-nickel magnetic powder core of this example, wherein 3 products were randomly selected from each batch of products for testing, and the iron-nickel annular green compact of this example is a typical 106 product, and has an outer diameter of 26.92mm, an inner diameter of 14.73mm and a height of 11.18mm.
TABLE 4
Example 5
a) Uniformly mixing water atomized iron-nickel powder with the granularity range of +200 to-325 meshes and gas atomized iron-nickel powder in a mixer to form mixed iron-nickel powder, wherein the mass fraction of the water atomized iron-nickel powder in the mixed iron-nickel powder is 30%; the particle size ratio is as follows: 5% of +200 meshes, 40% of-200- +325 meshes and 50% of-325 meshes.
b) Adding an insulating coating agent accounting for 0.5 percent of the weight of the mixed iron-nickel powder for passivation treatment, and fully and uniformly mixing, wherein the insulating coating agent is phosphoric acid diluted by acetone.
c) Adding a binder accounting for 0.5 percent of the weight of the mixed iron-nickel powder, fully and uniformly mixing, and drying for 4 hours; wherein the binder is water glass solution.
d) Adding a lubricant accounting for 0.5 percent of the weight of the mixed iron-nickel powder to prepare powder suitable for molding; wherein the lubricant is graphite.
e) Placing the powder treated in the step d) into a special mould for forming, wherein the pressure is 2.1GPa, and preparing an iron-nickel annular green body;
f) Heat treatment of the green body in an atmosphere of N 2 The temperature is 720 ℃ under the protection of (3), and a product after heat treatment is obtained.
g) And (3) soaking the heat-treated product in an impregnation liquid for 10 minutes, washing the surface impregnation liquid, standing for 24 hours, and then curing and heating in an oven at the temperature of not more than 230 ℃ to obtain the reinforced iron-nickel product.
h) And chamfering the reinforced iron-nickel product, wherein C is 0.5-1.5, and removing sharp corner edges.
i) Coating epoxy resin on the surface of the product to obtain a finished product of the iron-nickel magnetic powder core.
Table 5 shows the test data of the finished product of the iron-nickel magnetic powder core of this example, wherein 3 products were randomly selected from each batch of products for testing, and the iron-nickel annular green compact of this example is a typical 106 product, and has an outer diameter of 26.92mm, an inner diameter of 14.73mm and a height of 11.18mm.
TABLE 5
In the invention, the specific parameters of the test conditions of the 100 oersted superposition proportion, the 50KHz/100mT loss mw/cm3, the 100KHz/1V Q value, the 100KHz/1KHz inductance proportion and the technical indexes of the finished product rate are as follows:
| item | Technical index | Test conditions |
| 100 oersted superposition ratio | ≥37％ | 100kHz,1.0V,26Ts,Φ0.8mm，I DC ＝20A |
| Loss of power | 350mw/cm 3 max | 50KHz/100mT |
| Inductance ratio of 100KHz/1KHz | >96％ | 100kHz，1.0Vrms，26Ts，Φ0.8mm |
| Q value | ≥25 | 100kHz，1.0V，26Ts，Φ0.8mm |
The above examples are only intended to illustrate the technical solution of the present invention, and not to limit it; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (7)
1. The production method of the iron-nickel magnetic powder core with high yield is characterized by comprising the following steps:
a) Uniformly mixing water atomized iron-nickel powder with the granularity range of +200 to-325 meshes with gas atomized iron-nickel powder to form mixed iron-nickel powder, wherein the mass fraction of the water atomized iron-nickel powder in the mixed iron-nickel powder is 5-30%;
b) Adding an insulating coating agent accounting for 0.1-0.2% of the weight of the mixed iron-nickel powder for passivation treatment, and fully and uniformly mixing;
c) Adding a binder which is 0.5 to 2 percent of the weight of the mixed iron-nickel powder, fully and uniformly mixing, and drying;
d) Adding a lubricant which accounts for 0.2 to 1 percent of the weight of the mixed iron-nickel powder to prepare powder suitable for forming;
e) Placing the powder treated in the step d) into a special die for molding, wherein the pressure is 1.9-2.3 GPa, and preparing an iron-nickel annular green body;
f) Heat treatment of the green body in an atmosphere of N 2 And/or H 2 Under protection, the temperature is 700-80 DEG CObtaining a product after heat treatment at 0 ℃; said N is 2 And/or H 2 Is high-purity liquid N 2 And/or H 2 Or N obtained by air separation 2 And/or H 2 And N obtained by air separation at an oxygen content of up to 50PPM 2 Heat treatment is carried out.
2. The method for producing high-yield iron-nickel magnetic powder cores according to claim 1, further comprising, after step f):
g) Immersing the heat-treated product in the immersion liquid for a certain period of time, washing the immersion liquid on the surface, standing, and curing and heating in a drying oven at the temperature of not more than 230 ℃ to obtain the strengthened iron-nickel product.
3. The method for producing high-yield iron-nickel magnetic powder cores according to claim 2, further comprising, after step g):
h) And chamfering the reinforced iron-nickel product, wherein C is 0.5-1.5, and removing sharp corner edges.
4. The method for producing high-yield Fe-Ni magnetic powder core as claimed in claim 3, further comprising, after step h):
i) Coating epoxy resin on the surface of the product to obtain a finished product of the iron-nickel magnetic powder core.
5. The method for producing a high-yield iron-nickel magnetic powder core according to any one of claims 1 to 4, wherein the insulating coating agent comprises phosphoric acid, and the phosphoric acid needs to be diluted by alcohol or acetone in a proportion of the mass of the phosphoric acid: the mass of alcohol or acetone =1 to 5.
6. The method for producing a high-yield iron-nickel magnetic powder core according to any one of claims 1 to 4, wherein the binder is one or more of kaolin or an aqueous solution of water glass.
7. The method for producing a high-yield Fe-Ni magnetic powder core as claimed in any one of claims 1 to 4, wherein the lubricant is one or more of stearic acid, graphite or molybdenum disulfide.
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