CN109461558A - A kind of low-loss Fe-Si-Al magnetic core compound coating method - Google Patents
A kind of low-loss Fe-Si-Al magnetic core compound coating method Download PDFInfo
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- CN109461558A CN109461558A CN201811415827.3A CN201811415827A CN109461558A CN 109461558 A CN109461558 A CN 109461558A CN 201811415827 A CN201811415827 A CN 201811415827A CN 109461558 A CN109461558 A CN 109461558A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/147—Alloys characterised by their composition
- H01F1/14766—Fe-Si based alloys
- H01F1/14791—Fe-Si-Al based alloys, e.g. Sendust
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Abstract
The present invention provides a kind of compound coating method of low-loss Fe-Si-Al magnetic core, is related to soft magnetic materials and powder field of surface treatment, is the improvement to FeSiAl soft-magnetic powder core manufacturing process.A kind of compound coating method of low-loss Fe-Si-Al magnetic core is the following steps are included: select powder, phosphoric acid cladding, MnZn ferrite cladding, compression moulding, annealing, spraying.The process costs are low, easy to operate, greatly improve powder covered effect, using phosphoric acid-MnZn ferrite compound coating technique, it can avoid the saturation magnetization for causing powder core using non magnetic covering and magnetic conductivity decline, in the case where guaranteeing high magnetic permeability, low-loss high performance Fe SiAl powder core can be prepared.
Description
Technical field
The present invention relates to soft magnetic materials and powder field of surface treatment, more particularly to a kind of low-loss Fe-Si-Al magnetic core
Compound coating method.
Background technique
As electronic component tends to high frequency, miniaturization, filming, high power, to the performance indicator of soft magnetic materials
It puts forward higher requirements.In soft magnetic materials, FeSiAl powder core has low-loss, low cost, high saturated magnetic induction etc.
Advantage, in switching mode power supply transformer magnetic core, power corrector, high frequency power filter, uninterruptible power supply, energy storage filter inductor
In be used widely.
It can significantly be mentioned by improving the techniques such as iron sial powder pre-treating, insulating wrapped, compression moulding and heat treatment
Rise the magnetic property of powder core.Fe-Si-Al magnetic core carries out surface insulation and coats the contact that can effectively obstruct between powder particle, from
And increase resistivity, it reduces the eddy-current loss of powder core, improve the superposition performance and quality factor of powder core.In traditional iron silicon
It in aluminium insulating wrapped, is handled by phosphoric acid, forms the phosphate phosphating coat of one or more of slightly solubilities in particle surface, or pass through
Addition inorganic insulation agent and binder make to separate between iron sial powder particle, to reach reduction eddy-current loss, improve magnetic powder
The magnetic property of core.But the namagnetic substance of traditional cladding process addition will be greatly reduced the saturation magnetization and magnetic conductance of powder core
Rate deteriorates the magnetic property of powder core.To obtain high magnetic permeability, low-loss high-performance iron silicon-aluminum soft magnet powder core, it is badly in need of improving
The cladding and preparation process of Fe-Si-Al magnetic core.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention provides a kind of compound coating side of low-loss Fe-Si-Al magnetic core
Method.Using phosphoric acid-MnZn ferrite compound coating technique, it can make that there is better insulating properties between iron sial powder particle, warp
650 DEG C~800 DEG C high annealings can make Fe-Si-Al magnetic core obtain better magnetic property.
Specifically, the present invention provides a kind of compound coating method of low-loss Fe-Si-Al magnetic core comprising following steps:
S1, it selects powder: FeSiAl powder being prepared using high energy ball mill, by FeSiAl powder under protective atmosphere, through 800 DEG C
~900 DEG C of 1~5h of high annealing；
S2, phosphoric acid cladding: phosphoric acid is diluted with 75-95 DEG C of deionized water；Phosphoric acid dilution is added in powder, tentatively
It is surface-treated, the additive amount of phosphoric acid is 0.2-1.0wt%, is stirred continuously, and the reaction time is 10-25 minutes, later by powder
End is heated to 90-150 DEG C, stirring to drying；
S3, MnZn ferrite cladding: MnZn ferrite powder and FeSiAl powder are mixed in proportion, and bonding is added
Agent, the additive amount of binder are 0.10-0.50wt%, are uniformly mixed；Mixed-powder is heated to 90-150 DEG C, is stirred to dry
It is dry；
S4, addition release agent: the release agent for accounting for powder weight 0.8%-1.2% is added, is uniformly mixed；
S5, compression moulding: by press by the powder pressing forming after having coated, powder core is obtained；
S6, annealing: under protective atmosphere, powder core being placed in 650 DEG C~800 DEG C furnaces and is annealed, and keeps the temperature 60min
~90min, 10 DEG C/min of heating rate, furnace cooling after annealing；
S7, spraying: magnetic powder wicking surface is sprayed with epoxy resins insulation powder.
Preferably, the protective atmosphere is argon gas, nitrogen or hydrogen.
Preferably, the composition and mass percent of FeSiAl powder are as follows: Si:9.8%, Al:5.6%, surplus Fe, powder
Last granularity be 2%+150 mesh, 75% -150~+400 mesh and -23% 400 mesh.
Preferably, binder is silane coupling agent, organic siliconresin, silica solution, one in sodium silicate solution in step S3
Kind is a variety of.
Preferably, the release agent in step S4 is one or more of zinc stearate or micro mist wax.
Preferably, phosphoric acid is diluted with 80 DEG C of deionized water in step S2.
Preferably, the ratio of MnZn ferrite powder and FeSiAl powder is 1:(24-34 in step S3).
Compared with prior art, the invention has the following advantages:
1, manufacture craft of the present invention is simple, is not necessarily to complex device, under protective atmosphere, FeSiAl powder is through 800 DEG C~900
DEG C 1~5h of high annealing, eliminates the internal stress generated by ball milling, and by high temperature, can obviously reduce carbon in powder, oxygen and other
The content of impurity improves powder purity, and reduce impurity influences caused by powder core magnetic property；
2, the present invention uses phosphoric acid-MnZn ferrite compound coating technique, can effectively completely cut off iron sial powder particle, increases
Big powder resistivity can avoid the saturation magnetic that non magnetic covering causes powder core by adding magnetisable material MnZn ferrite
Change intensity and magnetic conductivity decline.
3, the present invention can effectively improve subsequent heat treatment temperature using high-temperature agglomerants such as silane coupling agent, sodium metasilicate,
Discharge the magnetic property of powder core；
4, Fe-Si-Al magnetic core magnetic conductivity produced by the present invention is up to 135 or more, there is good superposition performance and lower
Power loss.
Specific embodiment
Illustrate exemplary embodiment of the present invention, feature and aspect below with reference to specific embodiment.
Specifically, the present invention provides a kind of compound coating method of low-loss Fe-Si-Al magnetic core comprising following steps:
S1, it selects powder: FeSiAl powder being prepared using high energy ball mill, by FeSiAl powder under protective atmosphere, through 800 DEG C
~900 DEG C of 1~5h of high annealing.
S2, phosphoric acid cladding: phosphoric acid is diluted with 75-95 DEG C of deionized water；Phosphoric acid dilution is added in powder, tentatively
It is surface-treated, the additive amount of phosphoric acid is 0.2-1.0wt%, is stirred continuously, and the reaction time is 10-25 minutes, later by powder
End is heated to 90-150 DEG C, stirring to drying.
S3, MnZn ferrite cladding: MnZn ferrite powder and FeSiAl powder are mixed in a certain ratio uniformly, are added
Binder, the additive amount of binder are 0.10-0.50wt%, are uniformly mixed；Mixed-powder is heated to 90-150 DEG C, stirring is extremely
It is dry.
Wherein, the ratio of MnZn ferrite powder and FeSiAl powder is 1:(24-34 in step S3).
S4, demoulding: being added the release agent for accounting for powder weight 0.8%-1.2%, is uniformly mixed.
S5, compression moulding: by the powder pressing forming after having coated, powder core is obtained.
S6, annealing: under protective atmosphere, powder core being placed in 650 DEG C~800 DEG C furnaces and is annealed, and keeps the temperature 60min
~90min, 10 DEG C/min of heating rate, furnace cooling after annealing.
S7, spraying: magnetic powder wicking surface is sprayed with epoxy resins insulation powder.
Preferably, the protective atmosphere is argon gas, nitrogen or hydrogen.
Preferably, the composition and mass percent of FeSiAl powder are as follows: Si:9.8%, Al:5.6%, surplus Fe, powder
2%+150 mesh, 75% -150~+400 mesh and -23% 400 mesh that last granularity is.
Preferably, binder is silane coupling agent, organic siliconresin, silica solution, one in sodium silicate solution in step S3
Kind is a variety of.
Preferably, the release agent in step S4 is one or more of zinc stearate or micro mist wax.
Embodiment 1
FeSiAl powder, ingredient are as follows: Si:9.8%, Al:5.6%, surplus Fe are prepared using high energy ball mill；After ball milling
Powder under a nitrogen atmosphere, 800 DEG C of high annealing 2h are crushed after annealing with pulverizer；300g powder is taken with the sieve sieve of 100 mesh
End, it is desirable that grain size proportion are as follows:+150 mesh: 2%, -150~+400 mesh: 75%, -400 mesh: 23%.
It adds phosphoric acid in powder.Phosphoric acid additive amount is 0.9g, the 0.3% of powder weight is accounted for, using preceding with powder weight
80 DEG C of deionized water of amount 2% is diluted；Stirring 15 minutes, until end of reaction.Powder is heated to 120 DEG C, not
Disconnected stirring is dry to powder.
The MnZn ferrite powder of 200 mesh is added in the powder coated to phosphoric acid, additive amount 12g accounts for powder weight
4%, it is uniformly mixed；1.8g sodium metasilicate is added into mixed powder, the additive amount of sodium metasilicate accounts for the 0.60% of powder weight, before use
It is diluted with deionized water；The mixed-powder that MnZn ferrite and sodium metasilicate is added is stirred evenly, and is reacted 10 minutes；It will mixing
Powder is heated to 90 DEG C and is stirred continuously, until dry；
Powder to be mixed is cooled to room temperature, and 0.8% zinc stearate release agent is added, and is uniformly mixed with sieve, and pressure is made
Powder processed.
By compound coating powder pressing forming.Pressure is 17.5t/cm2, magnet ring blank dimension are as follows: outer diameter: 26.90mm, interior
Diameter: 14.70mm, height: 11.20mm.
Powder core is placed in nitrogen heat treatment, 750 DEG C keep the temperature 45 minutes.
Powder core is heated to 200 DEG C, magnetic powder wicking surface is uniformly sprayed by epoxy resin powder using electrostatic painting process
Sample 1 is made in end.
Embodiment 2
FeSiAl powder, ingredient are as follows: Si:9.8%, Al:5.6%, surplus Fe are prepared using high energy ball mill；After ball milling
Powder under a nitrogen atmosphere, 850 DEG C of high annealing 2h are crushed after annealing with pulverizer；300g powder is taken with the sieve sieve of 100 mesh
End, it is desirable that grain size proportion are as follows:+150 mesh: 2.8%, -150~+400 mesh: 74%, -400 mesh: 23.2%.
It adds phosphoric acid in powder.Phosphoric acid additive amount is 2.4g, the 0.8% of powder weight is accounted for, using preceding with powder weight
80 DEG C of deionized water of amount 2% is diluted.Stirring 15 minutes, until end of reaction.Powder is heated to 90 DEG C, and constantly
Stirring is dry to powder.
The MnZn ferrite powder of 200 mesh is added in the powder coated to phosphoric acid, additive amount 10.5g accounts for powder weight
3.5%, be uniformly mixed；1.8g sodium metasilicate is added into mixed powder, the additive amount of sodium metasilicate accounts for the 0.60% of powder weight, makes
It is diluted with preceding with deionized water；The mixed-powder that MnZn ferrite and sodium metasilicate is added is stirred evenly, and is reacted 10 minutes；It will
Mixed powder is heated to 90 DEG C and is stirred continuously, until dry；
Powder to be mixed is cooled to room temperature, and 0.7% zinc stearate release agent is added, and is uniformly mixed with sieve, and pressure is made
Powder processed.
By compound coating powder pressing forming, pressure 17.5t/cm2, magnet ring blank dimension are as follows: outer diameter: 26.90mm, it is interior
Diameter: 14.70mm, height: 11.20mm.
Powder core is placed in nitrogen heat treatment, 750 DEG C keep the temperature 45 minutes.
Powder core is heated to 200 DEG C, magnetic powder wicking surface is uniformly sprayed by epoxy resin powder using electrostatic painting process
Sample 2 is made in end.
Embodiment 3
FeSiAl powder is prepared using high energy ball mill, ingredient are as follows: Si:9.8%, Al:5.6%, surplus Fe；After ball milling
Powder under a nitrogen atmosphere, 880 DEG C of high annealing 3h are crushed after annealing with pulverizer；300g powder is taken with the sieve sieve of 100 mesh
End, it is desirable that grain size proportion are as follows:+150 mesh: 2.8%, -150~+400 mesh: 74%, -400 mesh: 23.2%.
It adds phosphoric acid in powder.Phosphoric acid additive amount is 3g, accounts for the 1.00% of powder weight, uses powder weight before use
2% 80 DEG C of deionized water is diluted.Stirring 15 minutes, until end of reaction.Powder is heated to 90 DEG C, and is constantly stirred
It mixes dry to powder.
The MnZn ferrite powder of 200 mesh is added in the powder coated to phosphoric acid, additive amount 9g accounts for powder weight
3.00%, it is uniformly mixed；0.51g silane coupling agent is added into mixed powder, the additive amount of silane coupling agent accounts for powder weight
0.17%, it is diluted using preceding with deionized water；The mixed-powder that MnZn ferrite and sodium metasilicate is added is stirred evenly, and is reacted
10 minutes；Mixed powder is heated to 90 DEG C and is stirred continuously, until dry.
Powder to be mixed is cooled to room temperature, and 1.00% zinc stearate release agent is added, and is uniformly mixed with sieve, and pressure is made
Powder processed.
By the powder pressing forming of compound coating, pressure 17.5t/cm2, magnet ring blank dimension are as follows: outer diameter: 26.90mm,
Internal diameter: 14.70mm, height: 11.20mm.
Powder core is placed in nitrogen heat treatment, 800 DEG C keep the temperature 45 minutes.
Powder core is heated to 200 DEG C, magnetic powder wicking surface is uniformly sprayed by epoxy resin powder using electrostatic painting process
Sample 3 is made in end.
The magnetic performance that sample is made in the present invention is as shown in table 1.
The magnetic property of 1 powder core of table
The present invention prepares Fe-Si-Al magnetic core using compound coating technique, obtains excellent magnetic property.Pass through phosphoric acid-
MnZn ferrite compound coating technique can significantly increase the resistivity of powder, reduce powder core power loss；MnZn ferrite packet
It covers, can avoid saturation magnetization and magnetic conductivity decline that non magnetic covering causes powder core；The high temperature of powder core blank
Annealing can be released effectively the internal stress that compacting generates, and improve the performance indicator of powder core.
Compared with prior art, the invention has the following advantages:
1, manufacture craft of the present invention is simple, is not necessarily to complex device, under protective atmosphere, FeSiAl powder is through 800 DEG C~900
DEG C 1~5h of high annealing, eliminates the internal stress generated by ball milling, and by high temperature, can obviously reduce carbon in powder, oxygen and other
The content of impurity improves powder purity, and reduce impurity influences caused by powder core magnetic property；
2, the present invention uses phosphoric acid-MnZn ferrite compound coating technique, can effectively completely cut off iron sial powder particle, increases
Big powder resistivity can avoid the saturation magnetic that non magnetic covering causes powder core by adding magnetisable material MnZn ferrite
Change intensity and magnetic conductivity decline.
3, the present invention can effectively improve subsequent heat treatment temperature using high-temperature agglomerants such as silane coupling agent, sodium metasilicate,
Discharge the magnetic property of powder core；
4, Fe-Si-Al magnetic core magnetic conductivity produced by the present invention is up to 135 or more, there is good superposition performance and lower
Power loss.
Finally, it should be noted that above-described embodiments are merely to illustrate the technical scheme, rather than to it
Limitation；Although the present invention is described in detail referring to the foregoing embodiments, those skilled in the art should understand that:
It can still modify to technical solution documented by previous embodiment, or to part of or all technical features into
Row equivalent replacement；And these modifications or substitutions, it does not separate the essence of the corresponding technical solution various embodiments of the present invention technical side
The range of case.
Claims (7)
1. a kind of compound coating method of low-loss Fe-Si-Al magnetic core, it is characterised in that: itself the following steps are included:
S1, select powder: using high energy ball mill prepare FeSiAl powder, by FeSiAl powder under protective atmosphere, through 800 DEG C~
900 DEG C of 1~5h of high annealing；
S2, phosphoric acid cladding: phosphoric acid is diluted with 75-95 DEG C of deionized water, phosphoric acid dilution is added in FeSiAl powder, just
Step is surface-treated, and the additive amount of phosphoric acid is 0.2-1.0wt%, is stirred continuously, and the reaction time is 10-25 minutes, later will
FeSiAl powder is heated to 90-150 DEG C, stirring to drying；
S3, MnZn ferrite cladding: MnZn ferrite powder and FeSiAl powder are mixed in proportion, and binder is added,
The additive amount of binder is 0.10-0.50wt%, is uniformly mixed；Mixed-powder is heated to 90-150 DEG C, stirring to drying；
S4, addition release agent: the release agent for accounting for powder weight 0.8%-1.2% is added, is uniformly mixed；
S5, compression moulding: by press by the powder pressing forming after having coated, powder core is obtained；
S6, annealing: under protective atmosphere, powder core being placed in 650 DEG C~800 DEG C furnaces and is annealed, and heat preservation 60min~
90min, 10 DEG C/min of heating rate, furnace cooling after annealing；
S7, spraying: magnetic powder wicking surface is sprayed with epoxy resins insulation powder.
2. the compound coating method of low-loss Fe-Si-Al magnetic core according to claim 1, it is characterised in that: the protection
Atmosphere is argon gas, nitrogen or hydrogen.
3. the compound coating method of low-loss Fe-Si-Al magnetic core according to claim 1, it is characterised in that: FeSiAl powder
End composition and mass percent are as follows: Si:9.8%, Al:5.6%, surplus Fe, powder size be 2%+150 mesh,
- the 150 of 75%~+400 mesh and -23% 400 mesh.
4. the compound coating method of low-loss Fe-Si-Al magnetic core according to claim 1, it is characterised in that: in step S3
Binder is one of silane coupling agent, organic siliconresin, silica solution, sodium silicate solution or a variety of.
5. the compound coating method of low-loss Fe-Si-Al magnetic core according to claim 1, it is characterised in that: in step S4
Release agent be one or more of zinc stearate or micro mist wax.
6. the compound coating method of low-loss Fe-Si-Al magnetic core according to claim 1, it is characterised in that: in step S2
Phosphoric acid is diluted with 80 DEG C of deionized waters.
7. the compound coating method of low-loss Fe-Si-Al magnetic core according to claim 1, it is characterised in that:
The ratio of MnZn ferrite powder and FeSiAl powder is 1:(24-34 in step S3).
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| CN113380487A (en) * | 2021-05-25 | 2021-09-10 | 合泰盟方电子（深圳）股份有限公司 | Magnetic core powder for integrally formed inductor and preparation method thereof |
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| CN113658768A (en) * | 2021-08-27 | 2021-11-16 | 西安交通大学 | FeSiAl/MnZn ferrite soft magnetic composite magnetic powder core with stable magnetic conductivity and low loss and preparation method thereof |
| CN113674979A (en) * | 2021-07-06 | 2021-11-19 | 浙江东睦科达磁电有限公司 | Preparation method and material of metal soft magnetic core applied to ultrahigh frequency |
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