CN107275033A - A kind of magnetically soft alloy material and preparation method thereof - Google Patents
A kind of magnetically soft alloy material and preparation method thereof Download PDFInfo
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- CN107275033A CN107275033A CN201710370561.4A CN201710370561A CN107275033A CN 107275033 A CN107275033 A CN 107275033A CN 201710370561 A CN201710370561 A CN 201710370561A CN 107275033 A CN107275033 A CN 107275033A
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0207—Using a mixture of prealloyed powders or a master alloy
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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
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Abstract
The present invention provides a kind of preparation method of high insulation low-loss magnetically soft alloy material, and its method comprises the following steps：FeSiAl powder and FeSiCr powder are chosen, the particle of the FeSiAl powder is thicker than the particle of FeSiCr powder；By FeSiAl powder and FeSiCr powder by ball milling mixing, orthosilicic acid solution continuation ball milling mixing is added into mixed powder, processing is then dried；Dried mixed-powder is heat-treated under air；Mixed-powder after heat treatment is subjected to ball mill grinding, the progress of powder after ball mill grinding is sieved；Powder after screening and pure water, phosphate dihydrogen aluminum solution, copper monoxide powder, dispersant slurrying are spray-dried to form second particle powder again；The second particle powder is pressed into magnetic core；Magnetic core curing molding under air.The method of the present invention can prepare higher insulation and low-loss magnetically soft alloy material, realize higher magnetic conductivity.
Description
Technical field
The present invention relates to that the present invention relates to magnetically soft alloy material correlative technology field, and in particular to a kind of high insulation low-loss is soft
Permalloy material and preparation method thereof.
Background technology
The great advantage of magnetically soft alloy is that have higher saturation flux density (Bs), with the good spy of DC superposition characteristic
Point.But the insulaion resistance of magnetically soft alloy material is relatively low, loss is high.
As device is for minimizing the requirement more and more higher with efficiency, magnetically soft alloy material performance is proposed higher
It is required that.Power inductor is used in high frequency, and especially in 500kHz and used above, one side magnetically soft alloy is often due to electricity
Resistance rate is relatively low, and insulation and pressure-resistant performance are relatively low, and magnetic core heating is larger, the penalty of device is caused, on the other hand with device
Transmittability lifting, transmission electric current incrementally increases, requires to improve for the Bs of material, general soft magnetic ferrite without
Method meets the requirement of device.In addition, the magnetic conductivity of soft magnetic alloy powder core is typically relatively low, to obtain higher inductance value, device is past
It is past to need to increase the number of turns of coiling, so that cause copper loss to increase, the penalty of device, thus improve the initial permeability of material
It is necessary.For the miniaturization and high energy efficiency, the requirement of low heating of correspondence power inductance, corresponding higher insulation is developed and low-loss
Magnetically soft alloy material is very necessary.
The manufacture method of some related magnetically soft alloy materials is had at home, there are some to use coarse granule material in the prior art
The Monosized powder of material and pass through Passivation Treatment, the electromagnetic performance of material can be remarkably decreased；Although also certain methods are using two kinds
Particle size powders are mixed, but employ substantial amounts of nonmagnetic substance as composite, also can significantly reduce the electromagnetism of material
Performance, so needing one kind to prepare higher insulation and low-loss magnetically soft alloy material and method.
The content of the invention
The present invention in order to solve not preparing in the prior art it is higher insulation and low-loss magnetically soft alloy material and method
The problem of there is provided a kind of high insulation low-loss magnetically soft alloy material and preparation method thereof.
In order to solve the above problems, the technical solution adopted by the present invention is as described below：
A kind of preparation method of high insulation low-loss magnetically soft alloy material, comprises the following steps：
S1：Choose FeSiAl powder and FeSiCr powder, particle of the particle than FeSiCr powder of the FeSiAl powder
Slightly；
S2：By FeSiAl powder and FeSiCr powder by ball milling mixing, orthosilicic acid is added into mixed powder molten
Liquid continues ball milling mixing, and processing is then dried；
S3：Dried mixed-powder is heat-treated under air；
S4：Mixed-powder after heat treatment is subjected to ball mill grinding, the powder after ball mill grinding is sieved；
S5：By the powder after screening and pure water, phosphate dihydrogen aluminum solution, copper monoxide powder, dispersant slurrying again
Spray drying forms second particle powder；
S6：The second particle powder is pressed into magnetic core；
S7：Magnetic core curing molding under air.
Preferably, in the step S1 FeSiAl powder median D50 >=20 μm, the median of FeSiCr powder
D50≤10μm。
Preferably, the mass percent of the FeSiAl powder of ball milling mixing is 18wt%-30wt% in the step S2：
FeSiCr powder qualities percentage is 70wt%-82wt%.
Preferably, it is powder gross mass after mixing to add quality in the step S2 into mixed powder
0.5wt%-3wt%, concentration is 1%-5% orthosilicic acid solution.
Preferably, the temperature being heat-treated in the step S3 is 600 DEG C -800 DEG C, and the time is 2-4 hours.
Preferably, in the step S4 ball mill grinding time 1-3 hour, screening choose the following powder of 400 mesh.
Preferably, the step of preparing second particle powder in the step S5 includes：
S51：By the powder after screening and pure water, phosphate dihydrogen aluminum solution, copper monoxide powder, dispersant, wherein
The addition of the phosphate dihydrogen aluminum solution is the 1wt%-4wt% of powder weight, and the copper monoxide powder addition is
0.05wt%-0.3wt%；
S52：After mixture ball milling 10-30 minutes in step S51, agitator tank is placed into 120 DEG C of -150 DEG C of constant temperature
Lower stirring 12-16 hours, is made slurry；
S53：Slurry is made second particle powder is formed in 200 DEG C of spray tower by centrifugal spraying granulator.
Preferably, pressure when magnetic core is suppressed in the step S6 is 600MPa-1200MPa.
Preferably, the temperature that magnetic core solidifies in the step S7 is 350 DEG C -450 DEG C, and constant temperature time is 120-150 points
Clock.
A kind of high insulation low-loss magnetically soft alloy material, is prepared from using as above any methods described.
Beneficial effects of the present invention are：A kind of high insulation low-loss magnetically soft alloy material and preparation method thereof is provided, passed through
Using being heat-treated after coarse grained FeSiAl powder and the mixing of fine grain FeSiCr powder, make the Cr and Al of two kinds of powder in sky
Under gas formed Cr-Al labyrinth metallic glass layer, be finally pressed into magnetic core and under air curing molding prepare compared with
Height insulation and low-loss magnetically soft alloy material, realize higher magnetic conductivity, its insulation impedance 50V voltages assign 1G Ω with
On, loss is 520mW/cm3 or so under the conditions of 100kHz/100mT, just corresponds to the FeSiCr materials of identical magnetic conductivity
The 40% of loss.
Embodiment
The present invention is described in detail below by specific embodiment, for a better understanding of the present invention, but it is following
Embodiment is not intended to limit the scope of the invention.In addition, it is necessary to which the diagram provided in explanation, following embodiments is only with signal side
Formula illustrates the basic conception of the present invention.
Embodiment 1
A kind of high insulation low-loss magnetically soft alloy material is prepared according to method provided by the present invention, comprised the following steps that：
(1) particle diameter D50=23um coarse granule FeSiAl powder and particle diameter D50=8um fine grained FeSiCr powder are chosen
End；
(2) by two kinds of powder according to coarse grained FeSiAl powder=18wt%, fine grain FeSiCr powder=
82wt% ratio is sufficiently mixed by ball milling, and the 1.6wt% that quality is two kinds of powder gross masses is added to mixed powder
Concentration carries out ball milling mixing again for 3% orthosilicic acid solution, and 60 minutes are toasted to powder drying at 120 DEG C after the completion of mixing；
(3) dried mixed-powder is heat-treated, heat treatment condition is to be incubated 4 hours under 600 DEG C of air；
(4) powder after heat treatment is subjected to ball mill grinding, the ball mill grinding time is 1 hour, by the powder after ball mill grinding
End carries out screening process using 400 mesh mesh screens, and chooses the following powder of 400 mesh；
(5) by the powder after screening and pure water, phosphate dihydrogen aluminum solution, copper monoxide powder, dispersant ball milling 10
After~30 minutes, place into 140 DEG C of constant temperature of agitator tank and stir 14 hours, obtained slurry is being passed through into centrifugal spraying granulator again
Second particle powder is formed in 200 DEG C of spray tower；The mass ratio of powder and pure water is 1 after wherein sieving:1, di(2-ethylhexyl)phosphate
The addition of hydrogen aluminum solutions is the 3wt% of powder quality after screening, and copper monoxide powder addition is powder quality after screening
0.05wt%；
(6) second particle powder is pressed into magnetic core under 800MPa pressure；
(7) magnetic core 120 minutes curing moldings of constant temperature under 450 DEG C of air.
Composite magnet ring after heat treatment is tested and evaluated respectively, uses CH333 Hi-pot Tester test samples
Insulation impedance；With the power attenuation of SY-8218 type B-H analyzer test samples, 1 the results are shown in Table.
Embodiment 2
Another high insulation low-loss magnetically soft alloy material is prepared according to method provided by the present invention, specific steps are such as
Under：
(1) particle diameter D50=30um coarse granule FeSiAl powder and particle diameter D50=10um fine grained FeSiCr are chosen
Powder；
(2) by two kinds of powder according to coarse granule FeSiAl powder=26wt%, fine grained FeSiCr powder=74wt%'s
Ratio is sufficiently mixed by ball milling, and adding the 0.5wt% concentration that quality is powder gross mass after mixing to mixed powder is
5% orthosilicic acid solution ball milling mixing again, toasts at 120 DEG C 60 minutes after mixing and dries to powder；
(3) dried powder is heat-treated, heat treatment condition is to be incubated 2 hours under 720 DEG C of air；
(4) by the powder ball mill grinding after heat treatment, the ball mill grinding time is 3 hours, and powder after ball mill grinding is used
400 mesh mesh screens carry out screening process, and choose the following powder of 400 mesh；
(5) by the powder after screening and pure water, phosphate dihydrogen aluminum solution, copper monoxide powder, dispersant ball milling 10
After~30 minutes, place into 150 DEG C of constant temperature of agitator tank and stir 12 hours, obtained slurry is existed by centrifugal spraying granulator
Second particle powder is formed in 150 DEG C of spray tower；The mass ratio of powder and pure water after wherein sieving is 1:1, di(2-ethylhexyl)phosphate
The addition of hydrogen aluminum solutions is the 1.2wt% of powder quality after screening, and copper monoxide powder addition is powder quality after screening
0.3wt%；
(6) powder is pressed into magnetic core under 600MPa pressure；
(7) magnetic core 150 minutes curing moldings of constant temperature under 350 DEG C of air.
Composite magnet ring after heat treatment is tested and evaluated respectively.Use CH333 Hi-pot Tester test samples
Insulation impedance；With the power attenuation of SY-8218 type B-H analyzer test samples, 1 the results are shown in Table.
Embodiment 3
Another height insulation low-loss magnetically soft alloy material is prepared according to method provided by the present invention, specific steps are such as
Under：
(1) particle diameter D50=20um coarse granule FeSiAl powder and particle diameter D50=5um fine grained FeSiCr powder are chosen
End；
(2) by two kinds of powder according to coarse granule=30wt%, coarse granule=70wt% ratio is sufficiently mixed by ball milling
Afterwards, 3wt% of the quality for powder gross mass after mixing is added to mixed powder, concentration is 1% orthosilicic acid solution ball milling
Mixing, 60 minutes are toasted to powder drying after the completion of mixing at 120 DEG C；
(3) dried powder is heat-treated, heat treatment condition is to be incubated 3 hours under 800 DEG C of air；
(4) by the powder ball mill grinding after heat treatment, the ball mill grinding time is 2 hours, and powder after ball mill grinding is used
400 mesh mesh screens carry out screening process, and choose the following powder of 400 mesh；
(5) by the powder after screening and pure water, phosphate dihydrogen aluminum solution, copper monoxide powder, dispersant 10 minutes
Afterwards, place into 120 DEG C of constant temperature of agitator tank to stir 16 hours, by obtained slurry in the spray by centrifugal spray granulation at 250 DEG C
Second particle is formed in mist tower；Wherein the mass ratio of powder and pure water is 1:1, the addition of phosphate dihydrogen aluminum solution is screening
The 4wt% of powder quality afterwards, copper monoxide powder addition is powder quality 0.18wt% after screening；
(6) powder is pressed into magnetic core under 1200MPa pressure；
(7) magnetic core 130 minutes curing moldings of constant temperature under 400 DEG C of air.
Composite magnet ring after heat treatment is tested and evaluated respectively.Use CH333 Hi-pot Tester test samples
Insulation impedance；With the power attenuation of SY-8218 type B-H analyzer test samples, 1 the results are shown in Table.
Comparative example 1
Particle diameter D50=10um fine grained FeSiCr powder is chosen, 2.9wt% epoxy resin granulation is added into powder
Afterwards, then under 800MPa magnetic core is pressed into, magnetic core is incubated 2 hours obtained magnetic cores at 160 DEG C.Composite magnetic after heat treatment
Core is tested and evaluated respectively.Use the insulation impedance of CH333 Hi-pot Tester test samples；Analyzed with SY-8218 types B-H
The power attenuation of instrument test sample, the results are shown in Table 1.
The embodiment 1-3 of table 1 and the Comparative result of contrast 1
| Embodiment | Insulation impedance | Q values | It is lost (100kHz/100mT) |
| 1 | 2.6GΩ | 42 | 607mw/cm3 |
| 2 | 1.7GΩ | 44 | 585mw/cm3 |
| 3 | 3.1GΩ | 48 | 521mw/cm3 |
| Comparative example 1 | 0.39GΩ | 43 | 1422mw/cm3 |
From table 1, the high insulation low-loss magnetically soft alloy material prepared using method provided by the present invention, insulation resistance
Resist and assign more than 1G Ω in 50V voltages, loss is 520mW/cm3 or so under the conditions of 100kHz/100mT, is just corresponded to identical
The 40% of the loss of the FeSiCr materials of magnetic conductivity, the excellent other magnetically soft alloy material with prior art of performance.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to assert
The specific implementation of the present invention is confined to these explanations.For those skilled in the art, do not taking off
On the premise of from present inventive concept, some equivalent substitutes or obvious modification can also be made, and performance or purposes are identical, all should
When being considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high insulation low-loss magnetically soft alloy material, it is characterised in that comprise the following steps：
S1：FeSiAl powder and FeSiCr powder are chosen, the particle of the FeSiAl powder is thicker than the particle of FeSiCr powder；
S2：By FeSiAl powder and FeSiCr powder by ball milling mixing, into mixed powder add orthosilicic acid solution after
Continuous ball milling mixing, is then dried processing；
S3：Dried mixed-powder is heat-treated under air；
S4：Mixed-powder after heat treatment is subjected to ball mill grinding, the powder after ball mill grinding is sieved；
S5：Powder after screening is sprayed again with pure water, phosphate dihydrogen aluminum solution, copper monoxide powder, dispersant slurrying
Drying forms second particle powder；
S6：The second particle powder is pressed into magnetic core；
S7：Magnetic core curing molding under air.
2. the preparation method of high insulation low-loss magnetically soft alloy material as claimed in claim 1, it is characterised in that the step
Median D50 >=20 μm of FeSiAl powder in S1, median D50≤10 μm of FeSiCr powder.
3. the preparation method of high insulation low-loss magnetically soft alloy material as claimed in claim 1, it is characterised in that the step
The mass percent of the FeSiAl powder of ball milling mixing is 18wt%-30wt% in S2：FeSiCr powder quality percentages are
70wt%-82wt%.
4. the preparation method of high insulation low-loss magnetically soft alloy material as claimed in claim 1, it is characterised in that the step
0.5wt%-3wt% of the quality for powder gross mass after mixing is added in S2 into mixed powder, concentration is 1%-5%'s
Orthosilicic acid solution.
5. the preparation method of high insulation low-loss magnetically soft alloy material as claimed in claim 1, it is characterised in that the step
The temperature being heat-treated in S3 is 600 DEG C -800 DEG C, and the time is 2-4 hours.
6. the preparation method of high insulation low-loss magnetically soft alloy material as claimed in claim 1, it is characterised in that the step
The following powder of 400 mesh is chosen in time 1-3 hour of ball mill grinding in S4, screening.
7. the preparation method of high insulation low-loss magnetically soft alloy material as claimed in claim 1, it is characterised in that the step
The step of second particle powder is prepared in S5 includes：
S51：By the powder after screening and pure water, phosphate dihydrogen aluminum solution, copper monoxide powder, dispersant, wherein described
The addition of phosphate dihydrogen aluminum solution is the 1wt%-4wt% of powder weight, and the copper monoxide powder addition is
0.05wt%-0.3wt%；
S52：After mixture ball milling 10-30 minutes in step S51, place into agitator tank and stirred under 120 DEG C of -150 DEG C of constant temperature
Mix 12-16 hours, slurry is made；
S53：Slurry is made second particle powder is formed in 200 DEG C of spray tower by centrifugal spraying granulator.
8. the preparation method of high insulation low-loss magnetically soft alloy material as claimed in claim 1, it is characterised in that the step
Pressure when magnetic core is suppressed in S6 is 600MPa-1200MPa.
9. the preparation method of high insulation low-loss magnetically soft alloy material as claimed in claim 1, it is characterised in that the step
The temperature that magnetic core solidifies in S7 is 350 DEG C -450 DEG C, and constant temperature time is 120-150 minutes.
10. a kind of high insulation low-loss magnetically soft alloy material, it is characterised in that using such as any methods describeds of claim 1-9
It is prepared from.
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| CN108831731A (en) * | 2018-06-27 | 2018-11-16 | 四川东阁科技有限公司 | A kind of powder core resistant to high temperature |
| CN109273231A (en) * | 2018-08-28 | 2019-01-25 | 江西尚朋电子科技有限公司 | A kind of preparation method of soft magnetism electronic material |
| CN109967734A (en) * | 2019-03-28 | 2019-07-05 | 深圳顺络电子股份有限公司 | A kind of magnetically soft alloy material and preparation method thereof |
| CN114121477A (en) * | 2022-01-25 | 2022-03-01 | 广东力王高新科技股份有限公司 | Integrally-formed transformer, manufacturing method thereof and electronic equipment |
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