CN104465004B - Method for manufacturing high-saturation-flux-density soft magnetic composite material according to alkaline bluing technique - Google Patents
Method for manufacturing high-saturation-flux-density soft magnetic composite material according to alkaline bluing technique Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title abstract description 5
- 239000006247 magnetic powder Substances 0.000 claims abstract description 29
- 230000004907 flux Effects 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims description 22
- 239000002184 metal Substances 0.000 claims description 20
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000011253 protective coating Substances 0.000 claims description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 229910045601 alloy Inorganic materials 0.000 claims description 7
- 239000000956 alloy Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229910001004 magnetic alloy Inorganic materials 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 235000013312 flour Nutrition 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000000314 lubricant Substances 0.000 claims description 3
- 229910052756 noble gas Inorganic materials 0.000 claims description 3
- 150000002835 noble gases Chemical class 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 2
- 238000002844 melting Methods 0.000 claims description 2
- 229920002050 silicone resin Polymers 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims 1
- LCDFWRDNEPDQBV-UHFFFAOYSA-N formaldehyde;phenol;urea Chemical compound O=C.NC(N)=O.OC1=CC=CC=C1 LCDFWRDNEPDQBV-UHFFFAOYSA-N 0.000 claims 1
- 239000000696 magnetic material Substances 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 abstract 8
- 238000005253 cladding Methods 0.000 abstract 4
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- 230000005294 ferromagnetic effect Effects 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 10
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- 239000010410 layer Substances 0.000 description 7
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000000137 annealing Methods 0.000 description 3
- 229960000935 dehydrated alcohol Drugs 0.000 description 3
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- 238000002161 passivation Methods 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
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- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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- 208000037516 chromosome inversion disease Diseases 0.000 description 1
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- 238000000280 densification Methods 0.000 description 1
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- 239000012895 dilution Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
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- 239000002902 ferrimagnetic material Substances 0.000 description 1
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- -1 melmac Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
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- Powder Metallurgy (AREA)
- Soft Magnetic Materials (AREA)
Abstract
The invention discloses a method for manufacturing a high-saturation-flux-density soft magnetic composite material according to the alkaline bluing technique. The method for manufacturing the high-saturation-flux-density soft magnetic composite material according to the alkaline bluing technique comprises the steps that the surface of magnetic powder is oxidized according to the alkaline bluing technique, so that a layer of uniform Fe3O4 insulating layer is generated, and then the novel soft magnetic composite material is manufactured through bonding, press-forming and heat treatment. The method for manufacturing the high-saturation-flux-density soft magnetic composite material according to the alkaline bluing technique has the advantages that Fe3O4 prepared according to the alkaline bluing technique grows on the surface of the magnetic powder in an in-situ mode, in this way, the degree of binding of the insulating cladding layer and the magnetic powder is high, and uniform and compact cladding is achieved; due to the fact that Fe3O4 has high specific resistance, the insulating effect is good; on the other hand, the ferromagnetic Fe3O4 is taken as the insulating cladding layer, in this way, magnetic attenuation caused when non-magnetic materials are taken as cladding agents in the prior art is avoided, and higher magnetic conductivity and higher magnetic flux density can be achieved; according to the alkaline bluing technique, operation is easy, cost is low, and industrial production can be achieved easily.
Description
Technical field
The present invention relates to field of magnetic material, more particularly, to a kind of alkalescence technique of giving a protective coating to metal objects prepares high saturation magnetic flux density soft magnetism
The method of composite.
Background technology
Soft-magnetic composite material is a kind of soft magnetic materials being manufactured using powder metallurgical technique, and its special magnetic property makes it
In many application scenarios, there is the advantage that other materials hardly match, this material has become as the important set of soft magnetic materials so far
Become part.Soft-magnetic composite material production history is long, but really forming industrialization is from the 1980s, with
The fast development of inversion transformation technique and extensive application, along with the demand of emc, soft-magnetic composite material is widely used；Enter
Enter 21st century, with the requirements at the higher level of the high frequency of inverter circuit, high power density and emc, add that people are multiple to soft magnetism
The intensification further of the understanding of condensation material, the industrialized development speed of soft-magnetic composite material has exceeded other any soft magnetic materials.
Ferrocart core can not be saturated under high magnetizing field, has good DC stacked stability.And it produces work
Skill is simple, and price is minimum in all kinds of metal soft magnetic powder core.Typically in the case of meeting use requirement, can preferentially select
Use ferrocart core.At present in all kinds of metal soft magnetic powder core, it is to use to popularize most, the maximum one kind of consumption.
The preparation technology of traditional soft-magnetic composite material is to form the phosphide of ferrum with phosphorus acid passivation, then adds bonding
Agent, compressing, annealing or unannealed, obtains soft magnetic-powder core at a lower temperature.Because the phosphide of ferrum is in higher temperature
Degree is lower to be decomposed, and lead to decreasing insulating, therefore annealing temperature relatively low so that the internal stress producing when suppressing can not be complete
Eliminate, be therefore unfavorable for reducing magnetic hystersis loss, therefore, occur in that the different powder cores being coated with oxide in recent years
Preparation method, such as Mitsubishi has invented a kind of vapour deposition method in one layer of mgo insulating barrier of iron powder Surface coating, in addition, in recent years,
Also occur in that and prepare, with sol-gal process, the report that oxide coats powder core, the powder core using above method preparation can be
Anneal at a temperature of higher, be thus advantageous to eliminate compressing internal stress, but the insulating barrier of this several method preparation is all
Non-magnetic phase, therefore can cause magnetic to dilute, lead to the saturation induction density of powder core to decline.
Content of the invention
The purpose of the present invention is for above-mentioned phenomenon, provides a kind of alkalescence technique of giving a protective coating to metal objects to prepare high saturation magnetic flux density soft magnetism
The method of composite.By alkalescence give a protective coating to metal objects technique make magnetic powder surface oxidation generate one layer of uniform fe3o4Insulating barrier, due to
fe3o4It is a kind of alloy of ferrimagnetism, can effectively drop low-alloyed magnetic dilution, be conducive to putting forward heavy alloyed pcrmeability and saturation
Magnetic flux density.Alkalescence is given a protective coating to metal objects simultaneously, and to carry out insulating wrapped be a kind of reaction in-situ process to technique, the fe therefore preparing3o4It is and magnetic
The fe direct reaction on powder surface produces, and therefore has higher conjugation, and easily generates one layer of fine and close insulating protective layer.
A kind of alkalescence give a protective coating to metal objects technique prepare high saturation magnetic flux density soft-magnetic composite material method and step as follows:
1) insulating wrapped of magnetic powder: take naoh, nano3、nano2It is dissolved in h2It is configured to alkalescence in o to give a protective coating to metal objects liquid, control
naoh、nano3、nano2Concentration be respectively 0.4 ~ 0.7 g/ml, 0.06 ~ 0.15 g/ml, 0.02 ~ 0.05 g/ml, will prepare
Good alkalescence is given a protective coating to metal objects liquid heated and boiled, adds magnetic powder, and ensures that the concentration of magnetic powder is less than 0.75 g/ml, continues heating holding and boils
Boiling state 5 ~ 35 min, so that magnetic powder Surface coating one layer insulating, then filters, and is dried, obtains soft-magnetic alloy powder；
2) add binding agent: the binding agent of magnetic powder mass percent 0.5% -2% is poured into the soft-magnetic alloy powder having coated
In end, heat and be stirred well to mixture drying, mix homogeneously；
3) compressing: the alloy powder after above-mentioned mix homogeneously to be added the stearic acid of magnetic powder mass percent 0.25%
Zinc, 0.25% barium stearate, as lubricant, depress to magnetic core in the pressure of 400 ~ 2000 mpa；
4) heat treatment: 400 ~ 700 under the protection of noble gasesoHeat treatment 0.5 ~ 2 h at a temperature of c, to eliminate
The internal stress that compacting produces, obtains soft-magnetic composite material.
Described binding agent is silicones, melmac, phenolic resin, epoxy resin, silicone resin, low melting point glass
Glass powder, sio2One or more of.
Described magnetic powder is iron powder or ferrum silica flour.
Using the method preparation soft-magnetic composite material due to the surface coated one layer of fe of magnetic powder3o4For ferrimagnetic material,
Too big loss will not be caused to the saturation flux density of soft-magnetic composite material, the full of soft-magnetic composite material can be improved further
And magnetic flux density, in addition, alkalescence is given a protective coating to metal objects, technique and the methods such as evaporation, sol-gal process are compared, process is simple, and preparation cost is low,
It is more beneficial for realizing large-scale industrial production.
Brief description
Fig. 1 is the hysteresis curve of the ferrocart core with alkaline give a protective coating to metal objects technique and the preparation of traditional phosphorus acid passivation technique.
Specific embodiment
The soft-magnetic composite material of the present invention is magnetic powder to be carried out alkalescence give a protective coating to metal objects process in one layer of fe of iron powder Surface Creation3o4Make
For insulating barrier, then add binding agent, compressing after annealing makes soft-magnetic composite material.
The step of soft-magnetic composite material preparation method is as follows:
1) insulating wrapped of magnetic powder: take naoh, nano3、nano2It is dissolved in h2It is configured to alkalescence in o to give a protective coating to metal objects liquid, control
naoh、nano3、nano2Concentration be respectively 0.4 ~ 0.7 g/ml, 0.06 ~ 0.15 g/ml, 0.02 ~ 0.05 g/ml, will prepare
Good alkalescence is given a protective coating to metal objects liquid heated and boiled, adds magnetic powder, and ensures that the concentration of magnetic powder is less than 0.75 g/ml, continues heating holding and boils
Boiling state 5 ~ 35 min, so that magnetic powder Surface coating one layer insulating, then filters, and is dried, obtains soft-magnetic alloy powder；
2) add binding agent: the binding agent of magnetic powder mass percent 0.5% -2% is poured into the soft-magnetic alloy powder having coated
In end, heat and be stirred well to mixture drying, mix homogeneously；
3) compressing: the alloy powder after above-mentioned mix homogeneously to be added the stearic acid of magnetic powder mass percent 0.25%
Zinc, 0.25% barium stearate, as lubricant, depress to magnetic core in the pressure of 400 ~ 2000 mpa；
4) heat treatment: 400 ~ 700 under the protection of noble gasesoHeat treatment 0.5 ~ 2 h at a temperature of c, to eliminate
The internal stress that compacting produces, obtains soft-magnetic composite material.
Below in conjunction with example, the present invention is described in further detail:
Embodiment 1:
By 50 g naoh, 10 g nano3And 3 g nano2It is dissolved in 100 ml h2In o, stir, be heated to seething with excitement,
It is subsequently adding 60g fe powder, continuing heating makes solution keep fluidized state 10 min, then filters, uses dehydrated alcohol cyclic washing
3 times, 80oStirring under the conditions of c is until the iron powder obtaining is dried.
The iron powder obtaining is added in the ethylene glycol solution that 2wt% silicones are with 10wt%, 80oUnder the conditions of c stirring until
Powder is dried, and is subsequently adding the zinc stearate of 0.25wt% and the barium stearate of 0.25wt%, is pressed under conditions of 800 mpa
Fine and close annular, to loop sample 450oAnneal under the conditions of c 1 h, makes soft-magnetic composite material.
After testing, the saturation flux density of magnetically soft alloy is 1.6 t, and pcrmeability is 83.Fig. 1 be with alkalescence give a protective coating to metal objects technique and
The hysteresis curve of traditional ferrocart core of phosphorus acid passivation technique preparation.From figure 1 it appears that using alkalescence give a protective coating to metal objects technique preparation
Ferrocart core there is higher saturation flux density and pcrmeability.
Embodiment 2:
By 40 g naoh, 6 g nano3And 5 g nano2It is dissolved in 100 ml h2In o, stir, be heated to seething with excitement,
It is subsequently adding 75gfe powder, continuing heating makes solution keep fluidized state 5 min, then filters, with dehydrated alcohol cyclic washing 3
Secondary, 80oStirring under the conditions of c is until the iron powder obtaining is dried.
The iron powder obtaining is added in the acetone soln that 0.5wt% epoxy resin is with 10wt%, 80oStir straight under the conditions of c
It is dried to powder, is subsequently adding the zinc stearate of 0.25wt% and the barium stearate of 0.25wt%, suppress under conditions of 400 mpa
Become fine and close annular, to loop sample 400oAnneal under the conditions of c 2 h, makes soft-magnetic composite material.
After testing, the saturation flux density of magnetically soft alloy is 1.5 t, and pcrmeability is 78.
Embodiment 3:
By 70 g naoh, 15 g nano3And 2 g nano2It is dissolved in 100 ml h2In o, stir, be heated to seething with excitement,
It is subsequently adding 50 g ferrum silica flours, continuing heating makes solution keep fluidized state 35 min, then filters, with dehydrated alcohol repeatedly
Washing 3 times, 80oStirring under the conditions of c is until the iron powder obtaining is dried.
The iron powder obtaining is added 1wt% phenolic resin, 1wt%sio2In the acetone soln of 10wt%, 80oUnder the conditions of c
Stirring, until powder is dried, is subsequently adding the zinc stearate of 0.25wt% and the barium stearate of 0.25wt%, in the bar of 2000 mpa
It is pressed into the annular of densification, to loop sample 700 under partoAnneal under the conditions of c 0.5 h, makes soft-magnetic composite material.
After testing, the saturation flux density of magnetically soft alloy is 1.6 t, and pcrmeability is 95.
Claims (3)
1. a kind of alkalescence technique of giving a protective coating to metal objects prepares the method for high saturation magnetic flux density soft-magnetic composite material it is characterised in that its step
As follows:
1) insulating wrapped of magnetic powder: take naoh, nano3、nano2It is dissolved in h2Be configured to alkalescence in o to give a protective coating to metal objects liquid, control naoh,
nano3、nano2Concentration be respectively 0.4 ~ 0.7 g/ml, 0.06 ~ 0.15 g/ml, 0.02 ~ 0.05 g/ml, by the alkali preparing
Property give a protective coating to metal objects liquid heated and boiled, add magnetic powder, and ensure that the concentration of magnetic powder is less than 0.75 g/ml, continues heating and keeps boil condition 5
~ 35 min, so that magnetic powder Surface coating one layer insulating, then filter, and are dried, obtain soft-magnetic alloy powder；
2) add binding agent: the binding agent of magnetic powder mass percent 0.5% -2% is poured into the soft-magnetic alloy powder having coated
In, heat and be stirred well to mixture drying, mix homogeneously；
3) compressing: by after above-mentioned mix homogeneously alloy powder add magnetic powder mass percent 0.25% zinc stearate,
0.25% barium stearate, as lubricant, depresses to magnetic core in the pressure of 400 ~ 2000 mpa；
4) heat treatment: 400 ~ 700 under the protection of noble gasesoHeat treatment 0.5 ~ 2 h at a temperature of c, to eliminate compacting
The internal stress producing, obtains soft-magnetic composite material.
2. method according to claim 1 is it is characterised in that described binding agent is silicones, melmac, phenol
Urea formaldehyde, epoxy resin, silicone resin, glass powder with low melting point, sio2One or more of.
3. method according to claim 1 is it is characterised in that described magnetic powder is iron powder or ferrum silica flour.
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| CN106782982B (en) * | 2016-12-31 | 2019-02-01 | 浙江工业大学 | A kind of soft-magnetic composite material and preparation method thereof |
| CN109727745A (en) * | 2018-12-17 | 2019-05-07 | 北京康普锡威科技有限公司 | Iron-based soft magnetic composite material and preparation method |
| CN110295362B (en) * | 2019-07-10 | 2021-05-18 | 湖南三泰新材料股份有限公司 | Online alkaline bluing method for hot-rolled steel bars |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1282291A (en) * | 1997-12-16 | 2001-01-31 | 材料革新公司 | Ferromagnetic powder for low core loss, well-bonded parts |
| CN101896632A (en) * | 2007-12-13 | 2010-11-24 | 杜费里特有限责任公司 | Method for producing corrosion-resistant surfaces of nitrated or nitrocarburated steel components |
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| DE19945592A1 (en) * | 1999-09-23 | 2001-04-12 | Bosch Gmbh Robert | Soft magnetic material and process for its production |
| JP3748425B2 (en) * | 2002-09-04 | 2006-02-22 | パーカー熱処理工業株式会社 | Salt bath nitriding method for metal members with enhanced corrosion resistance |
| CN102212815B (en) * | 2011-06-20 | 2015-01-28 | 南昌大学 | Method for preparing ferroferric oxide coating on surface of iron-based amorphous strip by using high-temperature oxidation method |
| CN104028762B (en) * | 2014-05-28 | 2016-08-24 | 浙江大学 | A kind of preparation method of soft-magnetic composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1282291A (en) * | 1997-12-16 | 2001-01-31 | 材料革新公司 | Ferromagnetic powder for low core loss, well-bonded parts |
| CN101896632A (en) * | 2007-12-13 | 2010-11-24 | 杜费里特有限责任公司 | Method for producing corrosion-resistant surfaces of nitrated or nitrocarburated steel components |
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