CN104952583A - Preparing method of amorphous meal soft magnetic powder core - Google Patents
Preparing method of amorphous meal soft magnetic powder core Download PDFInfo
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Abstract
The invention discloses a preparing method of an amorphous meal soft magnetic powder core. The preparing method includes the steps of 1, embrittling an amorphous strip, and crushing the amorphous strip embrittled to obtain amorphous metal powder; 2, screening the amorphous metal powder, and performing particle size matching; 3, subjecting the matched amorphous metal powder to passivation; 4, subjecting the amorphous metal powder, passivated by phosphoric acid, to insulation coating; 5, adding binder, and granulating the amorphous metal powder coated; 6, subjecting the granulated amorphous metal powder to magnetic field orientation forming; 7, subjecting a magnetic core, subjected to orientation forming, to axial magnetic thermal treatment; and 8, cooling the magnetic core, subjected to axial magnetic thermal treatment, and performing spraying to obtain a product. The preparing method has the advantages that magnetic domain forms in the amorphous magnetic core, coercive force and loss are lowered, magnetic core loss is further reduced, magnetic conductivity is improved, soft magnetic property of the amorphous magnetic core is improved, and the cost is lowered.
Description
Technical field
The present invention relates to metal magnetic powder core and prepare correlative technology field, refer in particular to a kind of preparation method of amorphous metal soft-magnetic powder core.
Background technology
Metal magnetic powder core is the novel soft magnetic material of one after silicon steel, ferrite, amorphous band, is widely used in the middle of power electronic device.Traditional metal magnetic powder core mainly contains ferrocart core, iron sial, iron silicon, iron nickel molybdenum, iron nickel etc., but they have respective shortcoming, as poor in the superposition of iron sial poor performance, ferrocart core drain performance, iron nickel and iron nickel molybdenum have good performance, but the nickel containing higher proportion in the middle of its composition, need higher manufacturing cost, therefore develop that a kind of cost is lower, the powder core of function admirable is necessary.Amorphous powder core is a kind of Novel magnetic powder core developed on the basis of amorphous band, has the advantages such as high Bs, low-loss and higher temperature stability, by industry extensive concern.General amorphous powder core preparation technology, all obtain corresponding amorphous soft magnet powder core through techniques such as the broken powder process of band, grain size proportion, insulating wrapped, compressing and heat treatments, some patent is to this has been improvement, but magnetic property all can not get increasing substantially.
Chinese patent " a kind of preparation method of amorphous metal soft magnetic-powder core ", patent No. CN104190945A, describes a kind of technology of preparing of amorphous magnetic powder core, which employs isostatic pressed technology of preparing, improve the density of magnetic core, thus improve the magnetic permeability of magnetic core, there are some defects in this method, on the one hand before amorphous powder core heat treatment, because binding agent does not also solidify, magnetic core intensity is lower, and isostatic pressed process can make magnetic core rupture, and reduces rate of finished products; On the other hand, isostatic pressed process needs soft sheath, adds cost, is not suitable for batch production, limits use.
Chinese patent " a kind of heat treatment method of amorphous powder core ", patent No. CN103658642A, describe a kind of heat treatment technics of amorphous powder core, it adopts horizontal magnetic treatment, and vertical magnetic field is through magnet ring face, although this method has and certain falls loss effect, but it adopts larger magnetic field, intensity is 1000-3000Gs, needs very large magnetic field to drive magnetic domain orientation, cause heat treatment cost increase, magnetic core cost is increased; And the arrangement of magnetic is unordered in a jumble, horizontal magnetic effect is also not obvious.
Summary of the invention
There is above-mentioned deficiency to overcome in prior art in the present invention, provides a kind ofly reduce core loss and improve the preparation method of the amorphous metal soft-magnetic powder core of magnetic core magnetic performance.
To achieve these goals, the present invention is by the following technical solutions:
A preparation method for amorphous metal soft-magnetic powder core, comprises the steps:
(1) amorphous band is carried out embrittlement process, the amorphous band after embrittlement carries out break process, obtains amorphous metal powder;
(2) by amorphous metal powder sieving, grain size proportion is carried out;
(3) the amorphous metal powder after proportioning is carried out Passivation Treatment;
(4) the amorphous metal powder of phosphorus acid passivation is carried out insulating wrapped process;
(5) add binding agent, the amorphous metal powder after coated is carried out granulation process;
(6) by the amorphous metal powder after granulation, it is shaping to carry out magnetic field orientating;
(7) magnetic core after oriented moulding is carried out vertical magnetic heat treatment;
(8) carry out process of spraying paint after the magnetic core cooling after heat treatment, obtain product.
This preparation method indulges the methods such as magnetic heat treatment by preferred amorphous granularity of magnet powder proportioning, amorphous magnetic oriented moulding and amorphous powder core magnetic field, magnetic domain is formed in amorphous magnetic core inside, serve the effect reducing coercive force and loss, core loss can be reduced further, improve magnetic permeability, and improve magnetic core soft magnet performance, and reduce cost.
As preferably, in step (1), the composition of described amorphous band is Fe, Si, B, and its atomic percent is: Fe accounts for 76-80at%, and Si accounts for 7-10at%, and B accounts for 11-14at%; The thickness of described amorphous band is 20-30um.
As preferably, in step (1), described embrittlement process, its brittle temperature is 200-400 degree, and its brittle time is 10-200 minute; Described break process, is divided into two steps, and the first step is Mechanical Crushing, and second step is that airflow milling is broken.
As preferably, in step (2), described grain size proportion, its result is :+150 orders account for 5%-30%, and-150-+200 order accounts for 40%-70%, and-200-+300 order accounts for 10-30%.
As preferably, in step (3), described Passivation Treatment, the passivating solution adopted is triosephosphate solution, and wherein phosphorus acid content is the 0.1-3% of amorphous metal amount of powder, and content of acetone is the 2-10% of amorphous metal amount of powder.
As preferably, in step (4), described insulating wrapped process, the insulating wrapped agent adopted is kaolin, talcum powder, glass dust, B
2o
3, Al
2o
3, one or more in MgO, its granularity is-600 orders, and addition is the 0.1-2wt% of amorphous metal powder weight.
As preferably, in step (5), described binding agent is one or more in epoxy resin, phenolic resins, novolac epoxy resin, and addition is the 1-5wt% of amorphous metal powder weight, adopts acetone as diluent.
As preferably, in step (5), described granulation process, its granularity can pass through 60 eye mesh screens.
As preferably, in step (6), described magnetic field orientating is shaping, magnetic direction is horizontal direction, is parallel to the lower planes of magnet ring, and its magnetic field intensity adopted is 0.1-1T, what adopted is pulsed magnetic field, and adding the magnetic time is 5-20s, and briquetting pressure is 12-25T/cm
2, the dwell time is 2-10s.
As preferably, in step (6), described vertical magnetic heat treatment, magnet ring entirety is in horizontal magnetic field, and magnetic field levels is through magnet ring lower planes, and the magnetic field intensity of employing is 10-1000Gs; Heat treatment temperature is 400-550 degree, and temperature retention time is 10-200 minute, adopts nitrogen or inert gas, and adopt multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 degree/min.
The invention has the beneficial effects as follows: form magnetic domain in amorphous magnetic core inside, reduce coercive force and loss, core loss can be reduced further, improve magnetic permeability, and improve magnetic core soft magnet performance, and reduce costs.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:
By Fe
78si
9b
13amorphous band carries out embrittlement process, and brittle temperature is 200 degree, and brittle time is 200 minutes; First amorphous band after embrittlement carries out fragmentation with disintegrating machine, then adopts airflow milling to carry out fragmentation, obtains amorphous metal powder; By amorphous metal powder sieving, carry out grain size proportion ,+150 orders account for 5% ,-150-+200 order and account for 70% ,-200-+300 order and account for 25%; Amorphous powder after proportioning is carried out Passivation Treatment, and the passivator of employing is triosephosphate solution, and wherein phosphorus acid content is 0.1% of magnetic amount, and content of acetone is 2% of magnetic amount; The amorphous powder of phosphorus acid passivation is carried out insulating wrapped process, and covering is kaolin, talcum powder, glass dust, B
2o
3, Al
2o
3, one or more in MgO, granularity is-600 orders, and addition is the 0.1wt% of amorphous metal powder weight; Add one or more in epoxy resin, phenolic resins or novolac epoxy resin as binding agent, using acetone as diluent, addition is the 1wt% of amorphous metal powder weight, and the amorphous magnetic after coated is carried out granulation process, and granule size is-60 orders; By the amorphous magnetic after granulation, it is shaping to carry out magnetic field orientating, and magnetic direction is horizontal direction, is parallel to the lower planes of magnet ring, and magnetic field intensity is 1T, and adding the magnetic time is 5s, and briquetting pressure is 25T/cm
2, the dwell time is 2s, obtains blank; Magnetic core after oriented moulding is carried out vertical magnetic heat treatment; magnetic direction is horizontal through magnet ring lower planes; magnetic core entirety is in the middle of magnetic field; magnetic domain is formed in amorphous magnetic core inside; play the object reducing coercive force and loss; the magnetic field intensity adopted is 10Gs; heat treatment temperature is 400 degree, and temperature retention time is 200 minutes, protects with nitrogen or inert gas; avoid oxidation; worsen magnetic property, adopt multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 °/min; slowly to get rid of the inner glue of magnetic core, avoid cracking.Carry out process of spraying paint after magnetic core cooling after heat treatment, obtain final products, magnetic property is as shown in table 1.
Comparative example 1:
Process and condition identical with embodiment 1, do not add magnetic field in shaping and heat treatment process, the properties of product of acquisition are as shown in table 1.
Embodiment 2:
By Fe
79si
7b
14amorphous band carries out embrittlement process, and brittle temperature is 400 degree, and brittle time is 10 minutes; First amorphous band after embrittlement carries out fragmentation with disintegrating machine, then adopts airflow milling to carry out fragmentation, obtains amorphous metal powder; By amorphous metal powder sieving, carry out grain size proportion ,+150 orders account for 30% ,-150-+200 order and account for 40% ,-200-+300 order and account for 30%; Amorphous powder after proportioning is carried out Passivation Treatment, and the passivator of employing is triosephosphate solution, and wherein phosphorus acid content is 3% of magnetic amount, and content of acetone is 10% of magnetic amount; The amorphous powder of phosphorus acid passivation is carried out insulating wrapped process, and covering is kaolin, talcum powder, glass dust, B
2o
3, Al
2o
3, one or more in MgO, granularity is-600 orders, and addition is 2wt%; Add one or more in epoxy resin, phenolic resins or novolac epoxy resin as binding agent, using acetone as diluent, addition is the 1wt% of magnetic weight, and the amorphous magnetic after coated is carried out granulation process, and granule size is-60 orders; By the amorphous magnetic after granulation, it is shaping to carry out magnetic field orientating, and magnetic direction is horizontal direction, is parallel to the lower planes of magnet ring, and magnetic field intensity is 0.1T, and adding the magnetic time is 20s, and briquetting pressure is 12T/cm
2, the dwell time is 10s, obtains blank; Magnetic core after oriented moulding is carried out vertical magnetic heat treatment; magnetic direction is horizontal through magnet ring lower planes; magnetic core entirety is in the middle of magnetic field; magnetic domain is formed in amorphous magnetic core inside; play the object reducing coercive force and loss; the magnetic field intensity adopted is 1000Gs; heat treatment temperature is between 550 degree, and temperature retention time is 10 minutes, protects with nitrogen or inert gas; avoid oxidation; worsen magnetic property, adopt multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 °/min; slowly to get rid of the inner glue of magnetic core, avoid cracking.Carry out process of spraying paint after magnetic core cooling after heat treatment, obtain final products, magnetic property is as shown in table 1.
Comparative example 2:
Process and condition identical with embodiment 2, do not add magnetic field in shaping and heat treatment process, the properties of product of acquisition are as shown in table 1.
Embodiment 3:
By Fe
80si
9b
11amorphous band carries out embrittlement process, and brittle temperature is 350 degree, and brittle time is 30 minutes; First amorphous band after embrittlement carries out fragmentation with disintegrating machine, then adopts airflow milling to carry out fragmentation, obtains amorphous metal powder; By amorphous metal powder sieving, carry out grain size proportion ,+150 orders account for 10% ,-150-+200 order and account for 70% ,-200-+300 order and account for 20%; Amorphous powder after proportioning is carried out Passivation Treatment, and the passivator of employing is triosephosphate solution, and wherein phosphorus acid content is 0.8% of magnetic amount, and content of acetone is 8% of magnetic amount; The amorphous powder of phosphorus acid passivation is carried out insulating wrapped process, and covering is kaolin, talcum powder, glass dust, B
2o
3, Al
2o
3, one or more in MgO, granularity is-600 orders, and addition is 1.5wt%; Add one or more in epoxy resin, phenolic resins or novolac epoxy resin as binding agent, using acetone as diluent, addition is the 5wt% of magnetic weight, and the amorphous magnetic after coated is carried out granulation process, and granule size is-60 orders; By the amorphous magnetic after granulation, it is shaping to carry out magnetic field orientating, and magnetic direction is horizontal direction, is parallel to the lower planes of magnet ring, and magnetic field intensity is 1T, and adding the magnetic time is 5s, and briquetting pressure is 20T/cm
2, the dwell time is 5s, obtains blank; Magnetic core after oriented moulding is carried out vertical magnetic heat treatment; magnetic direction is horizontal through magnet ring lower planes; magnetic core entirety is in the middle of magnetic field; magnetic domain is formed in amorphous magnetic core inside; play the object reducing coercive force and loss; the magnetic field intensity adopted is 20Gs; heat treatment temperature is 450 degree, and temperature retention time is 30 minutes, protects with nitrogen or inert gas; avoid oxidation; worsen magnetic property, adopt multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 °/min; slowly to get rid of the inner glue of magnetic core, avoid cracking.Carry out process of spraying paint after magnetic core cooling after heat treatment, obtain final products, magnetic property is as shown in table 1.
Comparative example 3:
Process and condition identical with embodiment 3, do not add magnetic field in shaping and heat treatment process, the properties of product of acquisition are as shown in table 1.
Embodiment 4:
By Fe
76si
10b
14amorphous band carries out embrittlement process, and brittle temperature is 380 degree, and brittle time is 40 minutes; First amorphous band after embrittlement carries out fragmentation with disintegrating machine, then adopts airflow milling to carry out fragmentation, obtains amorphous metal powder; By amorphous metal powder sieving, carry out grain size proportion ,+150 orders account for 25% ,-150-+200 order and account for 55% ,-200-+300 order and account for 20%; Amorphous powder after proportioning is carried out Passivation Treatment, and the passivator of employing is triosephosphate solution, and wherein phosphorus acid content is 0.5% of magnetic amount, and content of acetone is 6% of magnetic amount; The amorphous powder of phosphorus acid passivation is carried out insulating wrapped process, and covering is kaolin, talcum powder, glass dust, B
2o
3, Al
2o
3, one or more in MgO, granularity is-600 orders, and addition is 1.2wt%; Add one or more in epoxy resin, phenolic resins or novolac epoxy resin as binding agent, using acetone as diluent, addition is the 2wt% of magnetic weight, and the amorphous magnetic after coated is carried out granulation process, and granule size is-60 orders; By the amorphous magnetic after granulation, it is shaping to carry out magnetic field orientating, and magnetic direction is horizontal direction, is parallel to the lower planes of magnet ring, and magnetic field intensity is 0.8T, and adding the magnetic time is 10s, and briquetting pressure is 22T/cm
2, the dwell time is 5s, obtains blank; Magnetic core after oriented moulding is carried out vertical magnetic heat treatment; magnetic direction is horizontal through magnet ring lower planes; magnetic core entirety is in the middle of magnetic field; magnetic domain is formed in amorphous magnetic core inside; play the object reducing coercive force and loss; the magnetic field intensity adopted is 200Gs; heat treatment temperature is 500 degree, and temperature retention time is 20 minutes, protects with nitrogen or inert gas; avoid oxidation; worsen magnetic property, adopt multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 °/min; slowly to get rid of the inner glue of magnetic core, avoid cracking.Carry out process of spraying paint after magnetic core cooling after heat treatment, obtain final products, magnetic property is as shown in table 1.
Comparative example 4:
Process and condition identical with embodiment 4, do not add magnetic field in shaping and heat treatment process, the properties of product of acquisition are as shown in table 1.
Table 1
| Magnetic permeability | Pcv(100kHz，100mT) | DC-Bias(1000e) | |
| Embodiment 1 | 60 | 680 | 68 |
| Embodiment 2 | 63 | 650 | 65 |
| Embodiment 3 | 62 | 670 | 66 |
| Embodiment 4 | 61 | 630 | 68 |
| Comparative example 1 | 55 | 870 | 65 |
| Comparative example 2 | 54 | 830 | 67 |
| Comparative example 3 | 56 | 860 | 68 |
| Comparative example 4 | 53 | 820 | 66 |
Claims (10)
1. a preparation method for amorphous metal soft-magnetic powder core, is characterized in that, comprises the steps:
(1) amorphous band is carried out embrittlement process, the amorphous band after embrittlement carries out break process, obtains amorphous metal powder;
(2) by amorphous metal powder sieving, grain size proportion is carried out;
(3) the amorphous metal powder after proportioning is carried out Passivation Treatment;
(4) the amorphous metal powder of phosphorus acid passivation is carried out insulating wrapped process;
(5) add binding agent, the amorphous metal powder after coated is carried out granulation process;
(6) by the amorphous metal powder after granulation, it is shaping to carry out magnetic field orientating;
(7) magnetic core after oriented moulding is carried out vertical magnetic heat treatment;
(8) carry out process of spraying paint after the magnetic core cooling after heat treatment, obtain product.
2. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1, is characterized in that, in step (1), the composition of described amorphous band is Fe, Si, B, its atomic percent is: Fe accounts for 76-80at%, and Si accounts for 7-10at%, and B accounts for 11-14at%; The thickness of described amorphous band is 20-30um.
3. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1 and 2, is characterized in that, in step (1), and described embrittlement process, its brittle temperature is 200-400 degree, and its brittle time is 10-200 minute; Described break process, is divided into two steps, and the first step is Mechanical Crushing, and second step is that airflow milling is broken.
4. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1, is characterized in that, in step (2), described grain size proportion, its result is :+150 orders account for 5%-30%, and-150-+200 order accounts for 40%-70%, and-200-+300 order accounts for 10-30%.
5. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1, it is characterized in that, in step (3), described Passivation Treatment, the passivating solution adopted is triosephosphate solution, wherein phosphorus acid content is the 0.1-3% of amorphous metal amount of powder, and content of acetone is the 2-10% of amorphous metal amount of powder.
6. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1, is characterized in that, in step (4), described insulating wrapped process, the insulating wrapped agent adopted is kaolin, talcum powder, glass dust, B
2o
3, Al
2o
3, one or more in MgO, its granularity is-600 orders, and addition is the 0.1-2wt% of amorphous metal powder weight.
7. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1, it is characterized in that, in step (5), described binding agent is one or more in epoxy resin, phenolic resins, novolac epoxy resin, addition is the 1-5wt% of amorphous metal powder weight, adopts acetone as diluent.
8. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1 or 7, is characterized in that, in step (5), described granulation process, its granularity can pass through 60 eye mesh screens.
9. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1, it is characterized in that, in step (6), described magnetic field orientating is shaping, and magnetic direction is horizontal direction, is parallel to the lower planes of magnet ring, its magnetic field intensity adopted is 0.1-1T, what adopted is pulsed magnetic field, and adding the magnetic time is 5-20s, and briquetting pressure is 12-25T/cm
2, the dwell time is 2-10s.
10. the preparation method of a kind of amorphous metal soft-magnetic powder core according to claim 1, is characterized in that, in step (6), described vertical magnetic heat treatment, magnet ring entirety is in horizontal magnetic field, and magnetic field levels is through magnet ring lower planes, and the magnetic field intensity of employing is 10-1000Gs; Heat treatment temperature is 400-550 degree, and temperature retention time is 10-200 minute, adopts nitrogen or inert gas, and adopt multistage temperature lift-down curve, less than 200 degree heating rates are less than 5 degree/min.
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| CN107610873A (en) * | 2017-10-31 | 2018-01-19 | 国网江苏省电力公司电力科学研究院 | A kind of preparation method of composite soft-magnetic powder core of the magnetic conductivity towards PFC inductance equal to 125 |
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| CN107578877A (en) * | 2017-06-29 | 2018-01-12 | 安泰科技股份有限公司 | A kind of iron based nano crystal powder core of magnetic permeability μ=90 and preparation method thereof |
| CN107653426A (en) * | 2017-09-12 | 2018-02-02 | 西北工业大学 | Ti is improved using magnetic field48Zr20Nb12Cu5Be15The method of mechanical property |
| CN107818854A (en) * | 2017-10-30 | 2018-03-20 | 东莞理工学院 | A kind of preparation method and application of iron-based non-crystalline soft magnetic-powder core |
| CN107610873A (en) * | 2017-10-31 | 2018-01-19 | 国网江苏省电力公司电力科学研究院 | A kind of preparation method of composite soft-magnetic powder core of the magnetic conductivity towards PFC inductance equal to 125 |
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| CN109604606A (en) * | 2018-11-30 | 2019-04-12 | 东莞理工学院 | A kind of longitudinally magnetic heat treatment method of iron-based non-crystalline soft magnetic-powder core |
| CN110571009A (en) * | 2019-08-27 | 2019-12-13 | 广东咏旺新材料科技有限公司 | Iron-based spheroidized micro-nano magnetic powder core and preparation method thereof |
| CN111029078A (en) * | 2019-09-18 | 2020-04-17 | 佛山市中研非晶科技股份有限公司 | Powder insulation coating method, finished product powder and finished product magnetic powder core preparation method |
| CN111383810A (en) * | 2019-10-25 | 2020-07-07 | 横店集团东磁股份有限公司 | Preparation method of amorphous alloy magnetic powder core |
| CN112908603A (en) * | 2021-01-21 | 2021-06-04 | 广东省科学院材料与加工研究所 | Iron-based amorphous magnetic powder core and preparation method thereof |
| CN112908603B (en) * | 2021-01-21 | 2023-09-26 | 广东省科学院材料与加工研究所 | Iron-based amorphous magnetic powder core and preparation method thereof |
| CN113380524A (en) * | 2021-05-21 | 2021-09-10 | 无锡蓝沛新材料科技股份有限公司 | Preparation method of integrally-formed inductor solidified by magnetic field |
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