CN106373697A - Preparation method of FeSiAl/Mn-Zn ferrite composite magnetic powder core - Google Patents
Preparation method of FeSiAl/Mn-Zn ferrite composite magnetic powder core Download PDFInfo
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- CN106373697A CN106373697A CN201610866693.1A CN201610866693A CN106373697A CN 106373697 A CN106373697 A CN 106373697A CN 201610866693 A CN201610866693 A CN 201610866693A CN 106373697 A CN106373697 A CN 106373697A
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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
- H01F1/34—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 non-metallic substances, e.g. ferrites
- H01F1/36—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 non-metallic substances, e.g. ferrites in the form of particles
- H01F1/37—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 non-metallic substances, e.g. ferrites in the form of particles in a bonding agent
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F2003/023—Lubricant mixed with the metal powder
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
Abstract
The invention discloses a preparation method of an FeSiAl/Mn-Zn ferrite composite magnetic powder core. The method comprises the steps of carrying out in-situ synthesis on a ferric salt, a zinc salt and a manganese salt as raw materials and an NaOH solution as a precipitant through a chemical codeposition method on the surface of FeSiAl magnetic powder at 50-80 DEG C to form an Mn-Zn ferrite precursor and carrying out high-temperature roasting to obtain FeSiAl/Mn-Zn ferrite composite magnetic powder; and mixing the FeSiAl/Mn-Zn ferrite composite magnetic powder with epoxy resin and magnesium stearate evenly and then preparing the FeSiAl/Mn-Zn ferrite composite magnetic powder core through cold press molding. According to the method, a uniform and complete ferrite coating layer is formed on the surface of the FeSiAl magnetic powder, so that electric contact among metal magnetic powder particles is blocked; the resistivity of the composite magnetic powder core is improved; the eddy current loss of the composite magnetic powder core at a high frequency is effectively reduced; the prepared magnetic powder core is low in loss and high in magnetic conductivity; and the application field of the FeSiAl magnetic powder core is expanded.
Description
Technical field
The invention belongs to magnetic material and device preparing technical field, more particularly, to a kind of fesial/mn-zn ferrum
The preparation method of oxysome composite magnetic powder core.
Background technology
Powder core is a kind of soft magnetic materials being mixed compacting by magnetic material powder with dielectric.Due to its resistance
Rate is more much bigger than alloy, and therefore eddy-current loss is little, can use at higher frequencies.Again due to its saturation magnetization relatively
High it can also be used under higher power, these characteristics make powder core have other magnetic materials in many application scenarios to be difficult to compare
The advantage intended.Be widely used at present inductance filter in the products such as telecommunication, radar, TV and power supply, choking-winding and
Switching Power Supply iron core.
With the fast development of electronic technology, to the high frequency of electronic device, high power density, miniaturization and anti-electromagnetism
The requirement of interference becomes increasingly conspicuous, and the market demand increasingly increases.Fe-Si-Al magnetic core as a kind of NEW TYPE OF COMPOSITE electronic material, due to
It has a good high-gradient magnetism energy, the features such as good temperature stability, wide perseverance magnetic conduction and low-loss, low cost, quickly
Grow up, be widely used in the devices such as outputting inductance, line filter, power factor corrector.
The Fe-Si-Al magnetic core of early stage is relatively low due to operating frequency ratio, only requires that high pcrmeability requires simultaneously to low-loss
Not high.With the operating frequency more and more higher of Fe-Si-Al magnetic core application, how in the case of ensureing powder core high magnetic permeability,
Reducing core loss becomes outstanding problem.Therefore, the influence factor of research powder core pcrmeability and core loss just seems particularly
Important.Research with regard to metal magnetic powder core is mainly passed through to improve magnetic particle capability, is selected suitable insulating compound and magnetic powder both at home and abroad
Granularity, the adjustment method such as pressing parameter are improving the magnetic property of powder core.Going deep into it is considered to carry out from process aspect with research
Improve, such as the impact of pcrmeability to powder core of annealing temperature, briquetting pressure, granularity of magnet powder and magnetic powder heat treatment and drain performance
Increasingly receive publicity.Chinese patent cn201210443610.x discloses a kind of high magnetic flux density low core loss ferrum sial magnetic
The preparation technology of powder core, is walked by powder selection, pretreatment, Passivation Treatment, insulating wrapped process, compressing, heat treatment etc.
Suddenly obtain object, the product of preparation has higher pcrmeability and relatively low core loss, but step is relatively complicated.
Because insulating coating does not have magnetic, dilute magnetic, be unfavorable for the raising further of Fe-Si-Al magnetic core pcrmeability.
Content of the invention
The invention aims to overcoming non magnetic insulating barrier band in prior art fesial magnetic powder insulating wrapped technique
The deficiency of the magnetic dilution coming, provides a kind of preparation method of fesial/mn-zn ferrite composite magnetic powder core, with having Ferrimagnetic
Property ferrite make the insulating coating of Fe-Si-Al magnetic, it is to avoid non-in the fesial magnetic powder insulating wrapped technique commonly used at present
The magnetic dilution that magnetic insulating barrier brings, can fully ensure that uniformity and the integrity of insulating barrier.Prepared fesial/mn-zn
Ferrite composite magnetic powder core has higher pcrmeability and relatively low core loss and excellent combination property.
Another object of the present invention is to providing the fesial/mn-zn ferrite composite magnetic powder core of said method preparation.
It is still another object of the present invention to provide above-mentioned fesial/mn-zn ferrite composite magnetic powder core telecommunication, radar,
Inhale the application in ripple and electromagnetic shielding neck.
Above-mentioned purpose of the present invention is to be achieved by the following technical programs:
A kind of preparation method of fesial/mn-zn ferrite composite magnetic powder core, comprises the steps:
S1. fesial magnetic powder is placed in high energy ball mill and carries out ball milling, ratio of grinding media to material is 12:1, rotating speed is 35～50rpm,
Ball milling 40～60h, obtains flat fesial powder；
S2. press fe3+: zn2+: mn2+Molar ratio weighing iron salt, zinc salt and manganese salt, be dissolved in deionized water, agitated
After being completely dissolved, obtain fe-zn-mn mixing salt solution；
The fesial powder of the flattening s3. obtaining step s1, pours in deionized water, is heated to 50～80 DEG C, plus
Enter the fe-zn-mn mixing salt solution that step s2 obtains, instill the naoh solution of 2mol/l simultaneously, be stirred continuously, adjust solution
Ph value is 9～11, reacts 20～40min, obtains fesial/mn-zn ferrite presoma；
S4. it is washed with deionized fesial/mn-zn ferrite presoma, after 1～2h being dried at 100 DEG C；It is placed in horse
Not in 800～900 DEG C of roasting 1～2h in stove, obtain fesial/mn-zn ferrite composite magnetic powder；
S5. epoxy resin and magnesium stearate are mixed homogeneously with fesial/mn-zn ferrite composite magnetic powder, through being cold-pressed into
Type, and stress relief annealing 1～2h in an inert atmosphere, obtain fesial/mn-zn ferrite composite magnetic powder core.
Preferably, iron salt described in step s2 is fecl3Or fe (no3)3·9h2O, zinc salt is zncl2Or zn (no3)2·
6h2O, manganese salt is mncl2·4h2O or mn (no3)2.
Preferably, fe described in step s23+: zn2+: mn2+Mol ratio be 10:3:2.
Preferably, in the composite magnetic powder of fesial/mn-zn ferrite described in step s4, mn-zn ferrite is fesial magnetic
The 2～10% of silty amount.
Preferably, the pressure colded pressing described in step s5 is 1800～2200mpa, and the compression rate colded pressing is 1mm/min, protects
The pressure time is 3～8min.
Preferably, epoxy resin described in step s5: magnesium stearate: the mass ratio of fesial/mn-zn ferrite composite magnetic powder
It is respectively 1.5:1:97.5.
Preferably, the temperature of annealing described in step s5 is 600～720 DEG C.
Preferably, inert atmosphere described in step s5 is argon or nitrogen.
The fesial/mn-zn ferrite composite magnetic powder core of said method preparation and its in telecommunication, radar, inhale ripple and electromagnetism
Application in shielding neck is also within the scope of the present invention.
The present invention is to synthesize continuous, uniform ferrite on fesial magnetic powder surface to provide necessity using coprecipitation
Condition.Wherein, mn-zn ferrite is ferrimagnetic material and has higher resistivity, can be by controlling co-precipitation anti-
Answer temperature, response time, ph value, sintering temperature and the quality adjusting each reactant, to optimize fesial/ ferrite composite magnetic powder
In ferritic covering amount and form.The present invention passes through coprecipitation in fesial magnetic powder Surface coating ferrite, improves magnetic
Also improve its resistivity while conductance, mn-zn ferrite clad intensity is high and stable, abrasion-resistant it can be ensured that
During the compressing process of fesial powder core and use, the directly contact between barrier metal magnetic powder, is effectively reduced high frequency
Eddy-current loss ferrum, overcomes insulating barrier present in the fesial magnetic powder insulating coating method commonly used both at home and abroad at present in high temperature
The problems such as during easily decomposition, powder core are compressing, clad is easily crushed, discontinuous and thickness is difficult to control to.
Because powder core needs compression forming under very high pressure in preparation process, in the process inside powder core
In can produce the defects such as substantial amounts of internal stress, its presence can have a strong impact on the soft magnet performance of powder core.Generally briquetting pressure is bigger,
The internal stress that powder core sample interior produces is also bigger.Heat treatment is carried out to the powder core after compressing, can make inside it
The defect such as internal stress sufficiently discharged, not only can improve the comprehensive soft magnet performance of powder core, magnetic powder can also be improved
The mechanical strength of core.The effect of heat treatment of the present invention is to make that composite granule produces internal stress in compression molding and defect obtains very
Good elimination, the raising to Effective permeability plays a significant role.Composite magnetic powder core, through annealing heat-treats, releases it
Internal most internal stress, eliminates internal stress to neticdomain wall pinning, temperature is higher, the release of internal stress is more complete, this
The Effective permeability allowing for composite magnetic powder core increased.
Compared with prior art, the method have the advantages that
1. the present invention coats fesial magnetic powder using the magnetic ferrite of tool, solves the fesial magnetic powder commonly used at present
The dilution problem of non-magnetic phase magnetic present in insulating coating method, makes insulating barrier have high-temperature stability, powder core compressing
During clad is difficult to be crushed, continuous and thickness can control advantage, obtain the fesial powder core of high magnetic permeability.
2. fesial/mn-zn ferrite composite magnetic powder core of the present invention, after cold moudling, through the high temperature anneal, eliminates
The internal stress producing in preparation process, improves pcrmeability, obtains having that pcrmeability is high, high frequency eddy current losses are low
Fesial/mn-zn ferrite composite magnetic powder core.
3. the present invention adopts coprecipitation to prepare fesial/mn-zn ferrite composite powder, by adding bonding agent and lubrication
Agent is pressed into composite magnetic powder core, defines uniform and complete ferrite clad on fesial magnetic powder surface, thus blocks
Between metal magnetic granule, the electrical contact in compressing process and during using, improves the resistance of composite magnetic powder core
Rate, significantly reduces composite magnetic powder core eddy-current loss in high frequency, widens the application of fesial powder core.
Brief description
Fig. 1 is fesial powder and fesial/mn in embodiment 10.4zn0.6fe2o4The xrd figure of composite magnetic powder.
Fig. 2 is heat treatment temperature to fesial/mn0.4zn0.6fe2o4The impact of composite magnetic powder core power attenuation.
Fig. 3 is fesial/mn0.4zn0.6fe2o4The power attenuation of composite magnetic powder core is with the change of frequency.
Fig. 4 is fesial/mn0.4zn0.6fe2o4The stability of the pcrmeability of composite magnetic powder core.
Specific embodiment
Further illustrate present disclosure with reference to Figure of description and specific embodiment, but should not be construed as to this
The restriction of invention.If not specializing, the conventional handss that in embodiment, technological means used are well known to those skilled in the art
Section.Unless stated otherwise, the reagent that the present invention adopts, method and apparatus are the art conventional reagent, method and apparatus.
Embodiment 1
1. fesial magnetic powder is placed in ball mill and carries out high-energy ball milling, realize flattening.Ratio of grinding media to material is 12:1, ball milling
40h.
2. use coprecipitation in the Fe-Si-Al magnetic Surface coating mn-zn ferrite insulating barrier of flattening, coprecipitation reaction
Temperature is 60 DEG C, and the response time is 30min.
3. with fecl3、zncl2And mncl2·4h2O is Material synthesis mn-zn ferrite presoma, by mn0.4zn0.6fe2o4
Middle fe3+: zn2+: mn2+Mol ratio be 10:3:2 weigh raw material, be dissolved in deionized water, obtain fecl3-zncl2-mncl2
Mixing salt solution.
4. according to mn0.4zn0.6fe2o4The mass ratio of/fesial magnetic powder is 6%, weighs the fesial magnetic powder through flattening,
Pour in deionized water, be heated to 60 DEG C.It is slowly dropped into the fecl of respective amount toward in the fesial magnetic powder of heating3-zncl2-
mncl2Mixing salt solution, instills the naoh solution that concentration is 2mol/l simultaneously, is stirred continuously, the ph value adjusting solution is 10, instead
Answer 30min, obtain fesial/mn0.4zn0.6fe2o4Presoma.
5. it is washed with deionized fesial/mn0.4zn0.6fe2o4Presoma for several times, is placed in dry at 100 DEG C in drying baker
Dry 2h, by dried fesial/mn0.4zn0.6fe2o4Presoma is placed in Muffle furnace in 850 DEG C of roasting 2h, obtains fesial/
mn0.4zn0.6fe2o4Composite magnetic powder.
6. add the epoxy resin of 1.5wt.% and the magnesium stearate of 1wt.%, compression rate is 1mm/min, the dwell time
For 5min, cold pressing under 1800mpa, in AN 2h at 690 DEG C, obtain fesial/mn0.4zn0.6fe2o4Compound magnetic
Powder core.
After tested, fesial/mn under the test frequency of 100khz0.4zn0.6fe2o4The Effective permeability of composite magnetic powder core
For 78.4, it is lost as 48.2w/kg under 100khz, bm=300mt test condition.
Fig. 1 is fesial powder and fesial/mn in embodiment 10.4zn0.6fe2o4The xrd figure of composite magnetic powder.Wherein, (a)
For fesial powder, (b) is fesial/mn0.4zn0.6fe2o4Composite magnetic powder.Fesial and fesial/mn0.4zn0.6fe2o4Multiple
Close magnetic powder to compare, its diffraction peak intensity and position all no significant changes, are all in 2 θ=45 °, neighbouring presence 65.6 ° and 83 ° at
Stronger diffraction maximum, is compareed with pdf card, and its three strongest peak correspond to (200), (400) of fesial crystal, (422) crystal face respectively.
Xrd spectrum after former powder cladding is processed does not have significant difference, is not detected by the ferritic diffraction maximum of mn-zn.This is due to powder
The mn-zn film that surface is formed is very thin, and content is less.
Embodiment 2
1. fesial magnetic powder is placed in ball mill and carries out high-energy ball milling, realize flattening.Ratio of grinding media to material is 12:1, ball milling
40h.
2. use coprecipitation in the Fe-Si-Al magnetic Surface coating mn-zn ferrite insulating barrier of flattening, coprecipitation reaction
Temperature is 70 DEG C, and the response time is 30min.
3. with fecl3、zncl2And mncl2·4h2O is Material synthesis mn-zn ferrite presoma, by mn0.4zn0.6fe2o4
Middle fe3+: zn2+: mn2+Mol ratio be 10:3:2 weigh raw material, be dissolved in deionized water, obtain fecl3-zncl2-mncl2
Mixing salt solution.
4. according to mn0.4zn0.6fe2o4The mass ratio of/fesial magnetic powder is 6%, weighs the fesial magnetic powder through flattening,
Pour in deionized water, be heated to 70 DEG C.It is slowly dropped into the fecl of respective amount toward in the Fe-Si-Al magnetic of heating3-zncl2-
mncl2Mixing salt solution, instills the naoh solution that concentration is 2mol/l simultaneously, is stirred continuously, the ph value adjusting solution is 10, instead
Answer 30min, obtain fesial/mn0.4zn0.6fe2o4Presoma.
5. reaction is washed with deionized fesial/mn after terminating0.4zn0.6fe2o4Presoma for several times, is placed in drying baker
2h is dried at 100 DEG C.By dried fesial/mn0.4zn0.6fe2o4Presoma is placed in 850 DEG C of roasting 2h in Muffle furnace,
Obtain fesial/mn0.4zn0.6fe2o4Composite magnetic powder.
6. add the epoxy resin of 1.5wt.% and the magnesium stearate of 1wt.%, compression rate is 1mm/min, the dwell time
For 5min, cold pressing under 1800mpa, in AN 2h at 690 DEG C, obtain fesial/mn0.4zn0.6fe2o4Compound magnetic
Powder core.
After tested, under the test frequency of 100khz, the Effective permeability of ferrum sial composite magnetic powder core is 79.4,
It is lost as 46.8w/kg under 100khz, bm=300mt test condition.
Embodiment 3
1. Fe-Si-Al magnetic is placed in ball mill and carries out high-energy ball milling, ratio of grinding media to material is 12:1, ball milling 40h, obtains flat
Fe-Si-Al magnetic.
2. use coprecipitation in the Fe-Si-Al magnetic Surface coating mn-zn ferrite insulating barrier of flattening, coprecipitation reaction
Temperature is 80 DEG C, and the response time is 30min.
3. with fecl3、zncl2And mncl2·4h2O is Material synthesis mn-zn ferrite presoma, by mn0.4zn0.6fe2o4
Middle fe3+: zn2+: mn2+Mol ratio be 10:3:2 weigh raw material, be dissolved in deionized water, obtain fecl3-zncl2-mncl2
Mixing salt solution.
4. according to mn0.4zn0.6fe2o4The mass ratio of/fesial magnetic powder is 6%, weighs the fesial magnetic powder through flattening,
Pour in deionized water, be heated to 80 DEG C.It is slowly dropped into the fecl of respective amount toward in the Fe-Si-Al magnetic of heating3-zncl2-
mncl2Mixing salt solution, instills the naoh solution that concentration is 2mol/l simultaneously, is stirred continuously, the ph value adjusting solution is 10, instead
Answer 30min, obtain fesial/mn0.4zn0.6fe2o4Presoma.
5. reaction is washed with deionized fesial/mn after terminating0.4zn0.6fe2o4Presoma for several times, is placed in drying baker
2h is dried at 100 DEG C.By dried fesial/mn0.4zn0.6fe2o4Presoma is placed in 850 DEG C of roasting 2h in Muffle furnace,
Obtain fesial/mn0.4zn0.6fe2o4Composite magnetic powder.
6. add the epoxy resin of 1.5wt.% and the magnesium stearate of 1wt.%, compression rate is 1mm/min, the dwell time
For 5min, cold pressing under 1800mpa, in AN 2h at 690 DEG C, obtain fesial/mn0.4zn0.6fe2o4Compound magnetic
Powder core.
After tested, under 100khz, fesial/mn0.4zn0.6fe2o4The Effective permeability of composite magnetic powder core is 78.6,
It is lost under the conditions of 100khz, bm=300mt as 47.3w/kg.
Embodiment 4
1. Fe-Si-Al magnetic is placed in ball mill and carries out high-energy ball milling, realize flattening.Ratio of grinding media to material is 12:1, ball milling
40h.
2. use coprecipitation in the Fe-Si-Al magnetic Surface coating mn-zn ferrite insulating barrier of flattening, coprecipitation reaction
Temperature is 80 DEG C, and the response time is 30min.
3. with fecl3、zncl2And mncl2·4h2O is Material synthesis mn-zn ferrite presoma, by mn0.4zn0.6fe2o4
Middle fe3+: zn2+: mn2+Mol ratio be 10:3:2 weigh raw material, be dissolved in deionized water, obtain fecl3-zncl2-mncl2
Mixing salt solution.
4. according to mn0.4zn0.6fe2o4The mass ratio of/fesial magnetic powder is 2%, weighs the fesial magnetic powder through flattening,
Pour in deionized water, be heated to 80 DEG C.It is slowly dropped into the fecl of respective amount toward in the Fe-Si-Al magnetic of heating3-zncl2-
mncl2Mixing salt solution, instills the naoh solution that concentration is 2mol/l simultaneously, is stirred continuously, the ph value adjusting solution is 10, instead
Answer 30min, obtain fesial/mn0.4zn0.6fe2o4Presoma.
5. reaction is washed with deionized fesial/mn after terminating0.4zn0.6fe2o4Presoma for several times, is placed in drying baker
2h is dried at 100 DEG C.By dried fesial/mn0.4zn0.6fe2o4Presoma is placed in 850 DEG C of roasting 2h in Muffle furnace,
Obtain fesial/ ferrite composite magnetic powder.
6. add the epoxy resin of 1.5wt.% and the magnesium stearate of 1wt.%, compression rate is 1mm/min, the dwell time
For 5min, cold pressing under 1800mpa, in AN 2h at 690 DEG C, obtain fesial/mn0.4zn0.6fe2o4Compound magnetic
Powder core.
After tested, fesial/mn under the test frequency of 100khz0.4zn0.6fe2o4The Effective permeability of composite magnetic powder core
For 89.5, it is lost as 76.6w/kg under 100khz, bm=300mt test condition.
Embodiment 5
Different from embodiment 4 is, mn0.4zn0.6fe2o4The mass ratio of/fesial magnetic powder is 4%.
After tested, fesial/mn under the test frequency of 100khz0.4zn0.6fe2o4The Effective permeability of composite magnetic powder core
For 83.8, it is lost as 64.6w/kg under 100khz, bm=300mt test condition.
Embodiment 6
Different from embodiment 4 is, mn0.4zn0.6fe2o4The mass ratio of/fesial magnetic powder is 8%.
After tested, fesial/mn under the test frequency of 100khz0.4zn0.6fe2o4The Effective permeability of composite magnetic powder core
For 75.3, it is lost as 46.3w/kg under 100khz, bm=300mt test condition.
Embodiment 7
Different from embodiment 4 is, mn0.4zn0.6fe2o4The mass ratio of/fesial magnetic powder is 10%.
After tested, fesial/mn under the test frequency of 100khz0.4zn0.6fe2o4The Effective permeability of composite magnetic powder core
For 72.4, it is lost as 46.1w/kg under 100khz, bm=300mt test condition.
Fig. 2 is heat treatment temperature to fesial/mn0.4zn0.6fe2o4The impact of composite magnetic powder core power attenuation.Can from figure
Know, when heat treatment temperature is below 690 DEG C, with the rising of annealing temperature, the power attenuation of composite magnetic powder core declines, and reason is
The internal stress of the composite magnetic powder core that composite powder is prepared under the pressure of 1800mpa is very big, needs when discharging these internal stress
Very high heat treatment temperature.After annealing heat-treats, the internal stress of powder core is released, and coercivity declines, and therefore reduces compound
The magnetic hystersis loss of powder core is thus the power attenuation of composite magnetic powder core declines.It is preferably minimized 47.12w/kg when 690 DEG C.Simultaneously
Can see, when heat treatment temperature rises to 720 DEG C by 690 DEG C, the power attenuation of composite magnetic powder core increased on the contrary.One side
Face is because that, when heat treatment temperature is increased to certain value, the release of internal stress is basically completed, and annealing temperature continues to increase internally
The impact of stress is less and less.On the other hand, when heat treatment temperature is higher than 690 DEG C, the binding agent of powder core can decompose or carbon
Change, intergranular contact area increases and magnetic domain is pinned, therefore increases internal stress, so increased composite magnetic powder core
Power attenuation.
Fig. 3 is fesial/mn0.4zn0.6fe2o4The power consumption of composite magnetic powder core-frequency curve (bm: 300mt), can from figure
To find out, the power attenuation of composite magnetic powder core is gradually increased with the rising of frequency, and frequency is higher, and power attenuation is also got over
High.But when frequency is identical, the power attenuation of composite magnetic powder core is as the increase of covering amount and is gradually reduced, in high frequency
When decline and must become apparent from.Ferritic covering amount is more, and high-frequency loss is lower, but the Effective permeability of powder core also can reduce.
Covering amount is that the combination property of Fe-Si-Al magnetic core when 6% is optimal.
Fig. 4 is fesial/mn0.4zn0.6fe2o4The stability of powder core pcrmeability.It can be seen that being 1 in frequency
In the range of～1000khz, the Effective permeability of the composite magnetic powder core of different covering amounts reduces with the increase of frequency, but
Change is very little, shows preferable frequency stability.This is because the increasing of covering amount, in composite powder, ferritic content increases
Plus, so that the resistivity of powder core is improved, so that the Effective permeability of composite magnetic powder core obtains good frequency stability.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not subject to above-described embodiment
Limit, other any spirit without departing from the present invention and the change made under principle, modification, replacement, combine and simplify,
All should be equivalent substitute mode, be included within protection scope of the present invention.
Claims (10)
1. a kind of preparation method of fesial/mn-zn ferrite composite magnetic powder core is it is characterised in that comprise the steps:
S1. fesial magnetic powder is placed in high energy ball mill and carries out ball milling, ratio of grinding media to material is 12:1, rotating speed is 35～50rpm, ball milling
40～60h, obtains flat fesial powder；
S2. press fe3+: zn2+: mn2+Molar ratio weighing iron salt, zinc salt and manganese salt, be dissolved in deionized water, agitated completely
After dissolving, obtain fe-zn-mn mixing salt solution；
The fesial powder of the flattening s3. obtaining step s1, pours in deionized water, is heated to 50～80 DEG C, adds step
The fe-zn-mn mixing salt solution that rapid s2 obtains, instills the naoh solution of 2mol/l simultaneously, is stirred continuously, and adjusts the ph value of solution
For 9～11, reaction 20～40min, obtain fesial/mn-zn ferrite presoma；
S4. it is washed with deionized fesial/mn-zn ferrite presoma, after 1～2h being dried at 100 DEG C；It is placed in Muffle furnace
In in 800～900 DEG C of roasting 1～2h, obtain fesial/mn-zn ferrite composite magnetic powder；
S5. epoxy resin and magnesium stearate are mixed homogeneously with fesial/mn-zn ferrite composite magnetic powder, through cold moudling, and
Stress relief annealing 1～2h in an inert atmosphere, obtains fesial/mn-zn ferrite composite magnetic powder core.
2. the preparation method of fesial/mn-zn ferrite composite magnetic powder core according to claim 1 is it is characterised in that walk
Described in rapid s2, iron salt is fecl3Or fe (no3)3·9h2O, zinc salt is zncl2Or zn (no3)2·6h2O, manganese salt is mncl2·
4h2O or mn (no3)2.
3. the preparation method of fesial/mn-zn ferrite composite magnetic powder core according to claim 1 is it is characterised in that walk
Fe described in rapid s23+: zn2+: mn2+Mol ratio be 10:3:2.
4. the preparation method of fesial/mn-zn ferrite composite magnetic powder core according to claim 1 is it is characterised in that walk
In fesial/mn-zn ferrite composite magnetic powder described in rapid s4, mn-zn ferrite is the 2～10% of fesial magnetic powder quality.
5. the preparation method of fesial/mn-zn ferrite composite magnetic powder core according to claim 1 is it is characterised in that walk
The pressure colded pressing described in rapid s5 is 1800～2200mpa, and the compression rate colded pressing is 1mm/min, and the dwell time is 3～8min.
6. the preparation method of fesial/mn-zn ferrite composite magnetic powder core according to claim 1 is it is characterised in that walk
Epoxy resin described in rapid s5: magnesium stearate: the mass ratio of fesial/mn-zn ferrite composite magnetic powder is respectively 1.5:1:97.5.
7. the preparation method of fesial/mn-zn ferrite composite magnetic powder core according to claim 1 is it is characterised in that walk
Described in rapid s5, the temperature of annealing is 600～720 DEG C.
8. the preparation method of fesial/mn-zn ferrite composite magnetic powder core according to claim 1 is it is characterised in that walk
Inert atmosphere described in rapid s5 is argon or nitrogen.
9. a kind of fesial/mn-zn ferrite composite magnetic powder core according to the preparation of claim 1-8 any one methods described.
10. the fesial/mn-zn ferrite composite magnetic powder core described in claim 9 is in telecommunication, radar, suction ripple and electromagnetic shielding
Application in neck.
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| CN108242311A (en) * | 2017-12-18 | 2018-07-03 | 梅庆波 | A kind of preparation method of cladded type soft-magnetic powder core |
| CN109887698A (en) * | 2019-03-18 | 2019-06-14 | 电子科技大学 | A kind of composite magnetic powder core and preparation method thereof |
| CN110618151A (en) * | 2019-09-27 | 2019-12-27 | 南京宁智高新材料研究院有限公司 | Method for rapidly judging strength of magnetic permeability of FeSiAl material |
| CN112094114A (en) * | 2020-09-25 | 2020-12-18 | 麦格磁电科技（珠海）有限公司 | Manganese-zinc ferrite composite material and preparation method thereof |
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| CN114654823A (en) * | 2022-03-29 | 2022-06-24 | 重庆科技学院 | Mn-Zn ferrite-FeSiAl composite wave-absorbing material and preparation method thereof |
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| CN107414089B (en) * | 2017-07-20 | 2020-03-10 | 上海交通大学 | Iron-silicon-aluminum magnetic powder and preparation method thereof |
| CN108242311A (en) * | 2017-12-18 | 2018-07-03 | 梅庆波 | A kind of preparation method of cladded type soft-magnetic powder core |
| CN109887698A (en) * | 2019-03-18 | 2019-06-14 | 电子科技大学 | A kind of composite magnetic powder core and preparation method thereof |
| CN109887698B (en) * | 2019-03-18 | 2020-11-17 | 电子科技大学 | Composite magnetic powder core and preparation method thereof |
| CN110618151A (en) * | 2019-09-27 | 2019-12-27 | 南京宁智高新材料研究院有限公司 | Method for rapidly judging strength of magnetic permeability of FeSiAl material |
| CN112094114A (en) * | 2020-09-25 | 2020-12-18 | 麦格磁电科技（珠海）有限公司 | Manganese-zinc ferrite composite material and preparation method thereof |
| CN113658769A (en) * | 2021-08-30 | 2021-11-16 | 西安交通大学 | High-frequency high-Q-value FeSiAl @ MnZn ferrite soft magnetic composite magnetic powder core and preparation method thereof |
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