CN104465004A - 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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- CN104465004A CN104465004A CN201410684479.5A CN201410684479A CN104465004A CN 104465004 A CN104465004 A CN 104465004A CN 201410684479 A CN201410684479 A CN 201410684479A CN 104465004 A CN104465004 A CN 104465004A
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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, particularly relate to a kind of alkalescence technique of giving a protective coating to metal objects and prepare the method for high saturation magnetic flux density soft-magnetic composite material.
Background technology
Soft-magnetic composite material is a kind of soft magnetic material adopting powder metallurgical technique to manufacture, the advantage that its special magnetic property makes it have other material in many application scenarios to hardly match, and this material has become the important component part of soft magnetic material so far.Soft-magnetic composite material production history is long, but real formation industrialization is from the 1980s, and along with fast development and the extensive use of inversion transformation technique, along with the demand of EMC, soft-magnetic composite material is widely used; Enter 21st century, along with the requirements at the higher level of the high frequency of inverter circuit, high power density and EMC, add the further intensification of people to the understanding of soft-magnetic composite material, the industrialized development speed of soft-magnetic composite material has exceeded other any soft magnetic material.
Ferrocart core can not be saturated under high magnetizing field, has good DC stacked stability.And it produces technique simply, price is minimum in all kinds of metal soft magnetic powder core.General when instructions for use can be met, preferentially can select ferrocart core.At present in all kinds of metal soft magnetic powder core, be use the most universal, the one that consumption is maximum.
The preparation technology of traditional soft-magnetic composite material is the phosphide forming iron with phosphorus acid passivation, and then add binding agent, compressing, annealing or unannealed, obtains soft magnetic-powder core at a lower temperature.Because the phosphide of iron can decompose at a higher temperature, cause decreasing insulating, therefore annealing temperature is lower, the internal stress produced when making to suppress can not be eliminated completely, therefore be unfavorable for reducing magnetic hysteresis loss, therefore, occur in recent years different carrying out coated preparation process for magnetic powder core with oxide, as Mitsubishi has invented a kind of vapour deposition method at iron powder Surface coating one deck MgO insulating barrier, in addition, in recent years, also there is the report preparing the coated powder core of oxide with sol-gal process, the powder core utilizing above method to prepare can be annealed at a higher temperature, therefore be conducive to eliminating compressing internal stress, but insulating barrier prepared by this several method is all non-magnetic phase, therefore magnetic can be caused to dilute, the saturation induction density of powder core is caused to decline.
Summary of the invention
The object of the invention is for above-mentioned phenomenon, provide a kind of alkalescence technique of giving a protective coating to metal objects to prepare the method for high saturation magnetic flux density soft-magnetic composite material.Magnetic surface oxidation is made to generate the uniform Fe of one deck by alkalescence technique of giving a protective coating to metal objects
3o
4insulating barrier, due to Fe
3o
4be a kind of alloy of ferrimagnetism, effectively can fall the dilution of low-alloyed magnetic, be conducive to putting forward heavy alloyed magnetic permeability and saturation flux density.Simultaneously alkalescence is given a protective coating to metal objects, and to carry out insulating wrapped be a kind of reaction in-situ process to technique, the Fe therefore prepared
3o
4be directly react generation with the Fe on magnetic surface, therefore there is higher conjugation, and easily generate the insulating protective layer of one deck densification.
A kind of alkalescence is given a protective coating to metal objects, and to prepare the method step of high saturation magnetic flux density soft-magnetic composite material as follows for technique:
1) insulating wrapped of magnetic: get NaOH, NaNO
3, NaNO
2be dissolved in H
2be configured to alkalescence in O to give a protective coating to metal objects liquid, control NaOH, NaNO
3, NaNO
2concentration be respectively 0.4 ~ 0.7 g/ml, 0.06 ~ 0.15 g/ml, 0.02 ~ 0.05 g/ml, the liquid that the alkalescence prepared given a protective coating to metal objects heating is boiled, add magnetic, and ensure that the concentration of magnetic is less than 0.75 g/ml, continue heating and keep boil condition 5 ~ 35 min, make magnetic Surface coating one layer insulating, then filter, drying, obtains soft-magnetic alloy powder;
2) add binding agent: poured in coated good soft-magnetic alloy powder by the binding agent of magnetic mass percent 0.5%-2%, heat and be stirred well to mixture drying, mix;
3) compressing: the alloy powder after above-mentioned mixing is added the zinc stearate of magnetic mass percent 0.25%, 0.25% barium stearate as lubricant, become magnetic core at the pressure of 400 ~ 2000 MPa;
4) heat treatment: 400 ~ 700 under the protection of inert gas
oheat treatment 0.5 ~ 2 h at the temperature of C, to eliminate the internal stress that compacting produces, obtains soft-magnetic composite material.
Described binding agent is silicones, melmac, phenolic resins, epoxy resin, silicone resin, glass powder with low melting point, SiO
2in one or more.
Described magnetic is iron powder or iron silica flour.
The soft-magnetic composite material utilizing the method to prepare is due to the surface coated one deck Fe of magnetic
3o
4for ferrimagnetic material, too large loss can not be caused to the saturation flux density of soft-magnetic composite material, the saturation flux density of soft-magnetic composite material can be improved further, in addition, give a protective coating to metal objects technique and the method such as evaporation, sol-gal process of alkalescence is compared, technique is simple, and preparation cost is low, is more conducive to realizing large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the magnetic hysteresis loop of ferrocart core prepared by technique and traditional phosphorus acid passivation technique of giving a protective coating to metal objects by alkalescence.
Embodiment
Soft-magnetic composite material of the present invention magnetic is carried out alkalescence to give a protective coating to metal objects process at iron powder Surface Creation one deck Fe
3o
4as 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: get NaOH, NaNO
3, NaNO
2be dissolved in H
2be configured to alkalescence in O to give a protective coating to metal objects liquid, control NaOH, NaNO
3, NaNO
2concentration be respectively 0.4 ~ 0.7 g/ml, 0.06 ~ 0.15 g/ml, 0.02 ~ 0.05 g/ml, the liquid that the alkalescence prepared given a protective coating to metal objects heating is boiled, add magnetic, and ensure that the concentration of magnetic is less than 0.75 g/ml, continue heating and keep boil condition 5 ~ 35 min, make magnetic Surface coating one layer insulating, then filter, drying, obtains soft-magnetic alloy powder;
2) add binding agent: poured in coated good soft-magnetic alloy powder by the binding agent of magnetic mass percent 0.5%-2%, heat and be stirred well to mixture drying, mix;
3) compressing: the alloy powder after above-mentioned mixing is added the zinc stearate of magnetic mass percent 0.25%, 0.25% barium stearate as lubricant, become magnetic core at the pressure of 400 ~ 2000 MPa;
4) heat treatment: 400 ~ 700 under the protection of inert gas
oheat treatment 0.5 ~ 2 h at the 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 NaNO
3and 3 g NaNO
2be dissolved in 100 ml H
2in O, stir, be heated to boiling, then add 60g Fe powder, continue heating and make solution keep fluidized state 10 min, then filter, with absolute ethyl alcohol cyclic washing 3 times, 80
ostir under C condition until the iron powder obtained is dry.
The iron powder obtained is added in the ethylene glycol solution of 2wt% silicones and 10wt%, 80
ostir until powder for drying under C condition, then add the zinc stearate of 0.25wt% and the barium stearate of 0.25wt%, under the condition of 800 MPa, be pressed into fine and close annular, to loop sample 450
oanneal under C condition 1 h, makes soft-magnetic composite material.
After testing, the saturation flux density of magnetically soft alloy is 1.6 T, and magnetic permeability is 83.Fig. 1 is the magnetic hysteresis loop of ferrocart core prepared by technique and traditional phosphorus acid passivation technique of giving a protective coating to metal objects by alkalescence.As can be seen from Figure 1, the ferrocart core adopting alkaline technique of giving a protective coating to metal objects to prepare has higher saturation flux density and magnetic permeability.
Embodiment 2:
By 40 g NaOH, 6 g NaNO
3and 5 g NaNO
2be dissolved in 100 ml H
2in O, stir, be heated to boiling, then add 75gFe powder, continue heating and make solution keep fluidized state 5 min, then filter, with absolute ethyl alcohol cyclic washing 3 times, 80
ostir under C condition until the iron powder obtained is dry.
The iron powder obtained is added in the acetone soln of 0.5wt% epoxy resin and 10wt%, 80
ostir until powder for drying under C condition, then add the zinc stearate of 0.25wt% and the barium stearate of 0.25wt%, under the condition of 400 MPa, be pressed into fine and close annular, to loop sample 400
oanneal under C condition 2 h, makes soft-magnetic composite material.
After testing, the saturation flux density of magnetically soft alloy is 1.5 T, and magnetic permeability is 78.
Embodiment 3:
By 70 g NaOH, 15 g NaNO
3and 2 g NaNO
2be dissolved in 100 ml H
2in O, stir, be heated to boiling, then add 50 g iron silica flours, continue heating and make solution keep fluidized state 35 min, then filter, with absolute ethyl alcohol cyclic washing 3 times, 80
ostir under C condition until the iron powder obtained is dry.
The iron powder obtained is added 1wt% phenolic resins, 1wt%SiO
2with the acetone soln of 10wt%, 80
ostir until powder for drying under C condition, then add the zinc stearate of 0.25wt% and the barium stearate of 0.25wt%, under the condition of 2000 MPa, be pressed into fine and close annular, to loop sample 700
oanneal under C condition 0.5 h, makes soft-magnetic composite material.
After testing, the saturation flux density of magnetically soft alloy is 1.6 T, and magnetic permeability is 95.
Claims (3)
1. 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 characterized in that its step is as follows:
1) insulating wrapped of magnetic: get NaOH, NaNO
3, NaNO
2be dissolved in H
2be configured to alkalescence in O to give a protective coating to metal objects liquid, control NaOH, NaNO
3, NaNO
2concentration be respectively 0.4 ~ 0.7 g/ml, 0.06 ~ 0.15 g/ml, 0.02 ~ 0.05 g/ml, the liquid that the alkalescence prepared given a protective coating to metal objects heating is boiled, add magnetic, and ensure that the concentration of magnetic is less than 0.75 g/ml, continue heating and keep boil condition 5 ~ 35 min, make magnetic Surface coating one layer insulating, then filter, drying, obtains soft-magnetic alloy powder;
2) add binding agent: poured in coated good soft-magnetic alloy powder by the binding agent of magnetic mass percent 0.5%-2%, heat and be stirred well to mixture drying, mix;
3) compressing: the alloy powder after above-mentioned mixing is added the zinc stearate of magnetic mass percent 0.25%, 0.25% barium stearate as lubricant, become magnetic core at the pressure of 400 ~ 2000 MPa;
4) heat treatment: 400 ~ 700 under the protection of inert gas
oheat treatment 0.5 ~ 2 h at the temperature of C, to eliminate the internal stress that compacting produces, obtains soft-magnetic composite material.
2. method according to claim 1, is characterized in that described binding agent is silicones, melmac, phenolic resins, epoxy resin, silicone resin, glass powder with low melting point, SiO
2in one or more.
3. method according to claim 1, is characterized in that described magnetic is iron powder or iron silica flour.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106782982A (en) * | 2016-12-31 | 2017-05-31 | 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 |
| CN110295362A (en) * | 2019-07-10 | 2019-10-01 | 湖南三泰新材料股份有限公司 | A kind of online alkalinity of hot-rolled reinforced bar is given a protective coating to metal objects method |
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| CN110295362A (en) * | 2019-07-10 | 2019-10-01 | 湖南三泰新材料股份有限公司 | A kind of online alkalinity of hot-rolled reinforced bar is given a protective coating to metal objects 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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