CN108335820B - Stablize the magnetic powder core material and preparation method thereof of magnetic conductivity and low loss - Google Patents
Stablize the magnetic powder core material and preparation method thereof of magnetic conductivity and low loss Download PDFInfo
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- 239000006247 magnetic powder Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 122
- 239000000843 powder Substances 0.000 claims abstract description 104
- 239000002131 composite material Substances 0.000 claims abstract description 41
- 229910000859 α-Fe Inorganic materials 0.000 claims abstract description 39
- 229910052742 iron Inorganic materials 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000011258 core-shell material Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 5
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- NFCWKPUNMWPHLM-UHFFFAOYSA-N [Si].[B].[Fe] Chemical compound [Si].[B].[Fe] NFCWKPUNMWPHLM-UHFFFAOYSA-N 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 4
- 239000011863 silicon-based powder Substances 0.000 claims description 4
- 238000009689 gas atomisation Methods 0.000 claims description 3
- -1 iron aluminum silicon Chemical compound 0.000 claims description 3
- 239000003607 modifier Substances 0.000 claims description 3
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- MENXHHBNZPFGKB-UHFFFAOYSA-N [Fe].[Si].[B].[C] Chemical compound [Fe].[Si].[B].[C] MENXHHBNZPFGKB-UHFFFAOYSA-N 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims description 2
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- 230000005389 magnetism Effects 0.000 abstract description 11
- 238000012545 processing Methods 0.000 abstract description 5
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- 238000009692 water atomization Methods 0.000 description 6
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
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- 238000004519 manufacturing process Methods 0.000 description 4
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- 229910021529 ammonia Inorganic materials 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
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- 238000005303 weighing Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical group [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
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- PFRGGOIBYLYVKM-UHFFFAOYSA-N 15alpha-hydroxylup-20(29)-en-3-one Natural products CC(=C)C1CCC2(C)CC(O)C3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 PFRGGOIBYLYVKM-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- SOKRNBGSNZXYIO-UHFFFAOYSA-N Resinone Natural products CC(=C)C1CCC2(C)C(O)CC3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 SOKRNBGSNZXYIO-UHFFFAOYSA-N 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
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- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
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- 238000007599 discharging Methods 0.000 description 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
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Classifications
-
- 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
- H01F1/33—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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin
-
- 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
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- 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
-
- 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
-
- 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
-
- 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
- H01F1/20—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 in the form of particles, e.g. powder
- H01F1/22—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 in the form of particles, e.g. powder pressed, sintered, or bound together
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Soft Magnetic Materials (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to the magnetic powder core materials and preparation method of stablizing magnetic conductivity and low loss.Iron powder surface is modified first, iron/ferrite composite powder of core-shell structure is prepared by high-energy ball milling mode again, progress room temperature compacting in Alloy-steel mold is packed into after the composite powder is mixed with modified powder again, iron/ferrite soft magnetic composite magnetic powder core is obtained, subsequent heat treatment then is carried out to the powder core.Compared with prior art, the present invention prepares iron/ferrite cladding powder using ball grinding method, and technique time-consuming is short for this, is evenly coated, is easy to operate；Simultaneously, the present invention is using the ferrite of ferrimagnetism as insulating wrapped agent, reduce using namagnetic substance as covering bring magnetic dilution phenomenon, desired heat treatment temperature reacts when avoiding iron and ferrite hot processing and generates the unfavorable ingredient of magnetic, it ensure that powder core high saturation and magnetic intensity, high magnetic permeability, loss is reduced, the soft magnetism composite magnetic powder core of magnetic conductivity is obtained.
Description
Technical field
The present invention relates to a kind of soft magnetism composite magnetic powder cores, more particularly, to a kind of iron/iron oxygen of stable magnetic conductivity and low loss
Body soft magnetism composite magnetic powder core and preparation method thereof.
Background technique
Soft magnetic materials in high-power magnetic technique in development process, in order to improve working frequency, reduce electromagnetic consumable,
Reduce noise, new concept, new material, new construction continuously emerge.The period for updating replacement is shorter and shorter, and originally power frequency uses silicon
Steel, medium-high frequency have been broken using the situation of soft magnetic ferrite.Soft-magnetic composite material (including soft magnetic-powder core) is drawn soft simultaneously
Magnetic metal material and ferritic advantage, operating frequency range it is wider it is higher, soft magnet performance is excellent, cost is more reasonable, nearly ten
Develop into New raxa soft magnetic materials over year.
Preparing the most key process of soft-magnetic composite material is magnetic powder particles surface insulation treatment process, main at present
It is divided into following three classes: chemical surface treatment technique；Coated with Organic Matter treatment process: inorganic matter cladding processing.Chemical surface treatment
Technique primarily now uses inorganic acid or inorganic acid salt, such as phosphoric acid, phosphate, chromate, and it is blunt to carry out surface to powder particle
Change processing.Patent WO 1997030810 directlys adopt phosphoric acid solution and impregnates the method for metallic magnetic powder to realize cladding, the method
Coated insulating layer is uniform, and thickness is easily controllable, but this inorganic salts passivation layer non-refractory, and inorganic acid can be to environment
Cause considerable degree of pollution.In Coated with Organic Matter treatment process, Chinese patent CN1224899A disclose using epoxy resin,
The organic matters such as phenolic resin carry out insulating wrapped to FeSiAl powder core, and this technique can greatly improve Magnaglo surface
Resistivity is to reduce eddy-current loss.But since the heat resistance of organic coating material person's character is poor, this coating layer material system
Standby soft-magnetic composite material can only carry out hot-working when temperature is lower than 200 DEG C, and when the temperature is excessively high, organic coating layer material is
Start the fusing that softens, adjacent ferrous powder granules form effective contact, the resistivity of material is caused sharply to decline, to lose insulation
Effect, and magnetic property can be excessively greatly reduced in the organic matter coated.
Magnaglo method for coating more universal and applicable at present is the processing of inorganic matter cladding, Chinese patent
201310351622.4 realizing Al using sol-gel method2O3Cladding on Fe powder surface, but whole preparation process is more
Complexity, influence factor is more, is unfavorable for controlling product homogeneity, and time-consuming, and production efficiency is low, and nonmagnetic oxide coats
Reduce the magnetic conductivity of soft-magnetic composite material.Furthermore the method that Chinese patent 201010621275.9 uses discharge plasma sintering
It obtains soft magnetic ferrite and coats metallic magnetic powder, the insulating layer uniformity of this method cladding is not high, causes magnetic conductivity in high frequency
Under can be greatly reduced, and the production environment as needed for discharging plasma sintering equipment is more demanding, is only testing at present
It is carried out in room, is unfavorable for producing on a large scale.The development of high-grade, precision and advanced engineering technology does not require nothing more than soft magnetic materials with high magnetic conductance
Rate, small fissipation factor, it is often more important that high stability, the i.e. frequency stability of magnetic conductivity want high.Therefore, it studies and provides one
Kind simple process, easy to operate, at low cost, process flow is short, conducive to the metallic magnetic being mass produced and magnetic conductivity stability is good
Property powder and its preparation process, undoubtedly needed as this field.
Summary of the invention
The object of the invention is that existing chemical method cladding is overcome to prepare defect existing for soft-magnetic composite material and mention
For a kind of new magnetic powder core material of stabilization magnetic conductivity and low loss and preparation method thereof.
The present invention utilizes the change of iron powder surface polarity, keeps compatibility between iron powder and metal oxide more preferable, is being applicable in
Iron/ferrite soft magnetic composite magnetic powder core is prepared under the mechanical ball mill auxiliary of mass production, and metal oxide is existed
Iron powder surface is evenly coated, while adding the modified powder that partial size falls between, and is reduced porosity when compacting, is suppressed
The characteristic that the composite magnetic powder core arrived has high saturation and magnetic intensity, low-coercivity, low-loss, magnetic conductivity stable, to guarantee
The device stability of high-grade, precision and advanced field application.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of the magnetic powder core material of stable magnetic conductivity and low loss, by being grouped into iron/ferritic multiple
Room temperature compacting is heat-treated obtained again after conjunction powder modification, is included the following steps:
1) iron powder surface mechanical-chemical modification: being added basic modifier into iron powder first, and stirring guarantees iron powder table
The face agent that is modified is soaked, and iron powder surface polarity is changed, and activates particle surface, increases apparent activation energy；
2) ball milling is dry-mixed: modified iron powder and nanometer ferrite powder progress ball milling is dry-mixed, obtain core-shell structure
Iron/ferrite composite powder, for iron/ferrite composite powder using iron powder as core, external sheath has the ferrite shell of ferrimagnetism；
3) high temperature resistant binder and modified powder are added: iron/ferrite obtained by binder, modified powder and step 2) is multiple
Powder mixing is closed, and is stirred, guarantees that binder, modified powder are uniformly mixed with iron/ferrite composite powder and powder is dry, changes
Property powder be used for filling ferrous powder and ferrite powder particles gap；
4) room temperature compression moulding: the powder mixed according to step 3) is poured into alloy mold, is carried out room temperature compacting, is obtained
To iron/ferrite soft magnetic composite magnetic powder core；
5) subsequent heat treatment: iron/ferrite soft magnetic composite magnetic powder core of gained block in step 4) is protected in inert gas
Shield is lower to carry out vacuum heat treatment, obtains the magnetic powder core material for stablizing magnetic conductivity and low loss.
In an embodiment of the invention, iron powder described in step 1) is selected from water-atomized iron powder, gas atomization iron powder, goes back
One or more of former iron powder, iron silicon powder or iron aluminum silicon powder, the iron powder powder diameter are 30~100 microns.It is preferred that average
The gas atomization iron powder powder that partial size is 50 microns.
In an embodiment of the invention, the step 1) basic modifier selects ammonium hydroxide.
In an embodiment of the invention, it is preferable to use motor machine stirring rod is sufficiently stirred in step 1).
In an embodiment of the invention, the step 2) nanometer ferrite is selected from nano ferriferrous oxide, nanometer
One or more of manganese-zinc ferrite, nanometer nickel-zinc ferrite or nanometer copper zinc ferrite, the step 2) nanometer ferrite
Powder diameter is 10~50 nanometers.It is preferred that average grain diameter is the manganese-zinc ferrite powder of 30nm.
In an embodiment of the invention, in step 2), the quality of modified iron powder and nanometer ferrite powder
Proportion meets: soft magnetic powder shared mass percent in final product is 80%~98%, and remaining is ferrite powder, wherein soft
Magnetic powder includes iron powder and modified powder.It is preferred that mass percent shared by soft magnetic powder is 90%~96%.
In an embodiment of the invention, in step 2), milling parameters: ratio of grinding media to material is 10:1~30:1, is turned
Speed is 300r/min~200r/min, and Ball-milling Time is 1h~3h.It is preferred that ratio of grinding media to material=20:1, revolving speed 200r/min, ball milling
Time is 2h, wherein the commutation of every 30 minutes ball milling directions is primary and ball milling 1h suspends cooling in 20 minutes.
In an embodiment of the invention, in step 3), the binder selects epoxy modified silicone resin, institute
One or more of modified powder selection amorphous iron silicon boron, amorphous iron silicon boron carbon, amorphous iron silicochromium or amorphous matrix powder are stated,
The modified powder partial size is 10~30 microns.
In an embodiment of the invention, in step 3), the binder additional amount is that the iron/ferrite is compound
The 0.5-3% of powder quality, the modified powder additional amount are the iron/ferrite composite powder quality 2-10%.
In an embodiment of the invention, in step 3), the condition of stirring is sufficiently stirred under the conditions of 80 DEG C.
In an embodiment of the invention, in step 4), compression moulding is carried out in the case where 800-1000Mpa
's.
In an embodiment of the invention, in step 4), it is preferred to use circular ring shape Diamond dies are directly prepared
Annular powder core, avoids sintering into block and cuts ring again and generate machining stress, reduces process procedure.
In an embodiment of the invention, in step 5), the technique of vacuum heat treatment are as follows: sample is placed in vacuum tube
400-600 DEG C of heat preservation 60-120min, atmosphere are argon gas in formula furnace.It is preferred that heat treatment temperature is 450 DEG C, soaking time 1h.
The present invention prepares iron/ferrite cladding powder using ball grinding method, and technique time-consuming is short for this, is evenly coated, operates letter
It is single；Meanwhile the present invention reduces using the ferrite of ferrimagnetism as insulating wrapped agent using namagnetic substance as covering band
The magnetic dilution phenomenon come, desired heat treatment temperature react when avoiding iron and ferrite hot processing and generate the unfavorable ingredient of magnetic,
It ensure that powder core high saturation and magnetic intensity, high magnetic permeability, reduce loss, obtain the soft magnetism composite magnetic powder core of magnetic conductivity.
Compared with prior art, the present invention has the following advantages and beneficial effects:
1, cladding uses physical method, due to the two polarity on the contrary, shell powder guarantees automatically by stratum nucleare powder adsorption
The thickness of clad, and treatment process is without multi-chemistry is crossed, it will not generation environment pollution in production process；
2, modified powder of the granularity between micron order iron powder and nano-level iron oxide powder is added, is sufficient filling with
Particulate interspaces reduce porosity, improve magnetic conductivity while reducing block loss；
3, the present invention uses circular ring shape Diamond dies, directly prepares annular powder core, avoids and sinter block into again
It cuts ring and generates machining stress, reduce process procedure；
4, for working in the magnetic core under high magnetic flux density, amplitude permeability parameter is that reflection magnetic core is close in high magnetic flux
The important parameter of true magnetic characteristic under degree.The water-atomized iron powder of cladding nanometer ferrite powder is realized to shake as frequency changes
Width magnetic conductivity parameter change rate is maintained in ± 1% range, is shown under real operating environments, powder core prepared by the present invention
It can guarantee the stability of working frequency conversion.
Detailed description of the invention
Powder surface contrast scans electron microscope before and after Fig. 1 ball milling；
Cross-sectional scans electron microscope after the compacting of Fig. 2 high-performance soft magnetic composite powder room temperature；
The hysteresis loop of Fig. 3 high-performance soft magnetic composite powder；
The magnetic conductivity of Fig. 4 high-performance soft magnetism composite magnetic powder core changes with frequency；
Fig. 5 high-performance soft magnetic composite powder scanning electron microscope (SEM) photograph.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
The ammonia that can soak iron powder is added in beaker in the pure Fe powder of water atomization that the average grain diameter for weighing 47g is 75 μm
Water, glass bar stir 20min clockwise, then weigh the Fe that 3g partial size is 20nm3O4Powder is premixed in V-type batch mixer.
Dry type ball milling is carried out using planetary ball mill, the Fe/Fe for taking dry type ball milling to prepare3O4Core-shell structure cladding powder 4g, it is obtained
Cladding powder scanning electron microscope (SEM) photograph is as shown in Figure 1, comparison ball milling front and back powder surface topography, it is known that the pure Fe powder table of smooth water atomization
Face In-situ reaction under ball action obtains soft magnetic composite powder.Saturation induction using VSM equipment test composite powder is strong
Degree is as shown in figure 3, it can be seen that its saturation induction density is 207emu/g, than the saturation induction density of original iron powder
220emu/g only declines 5.9%, therefore 6% nanometer Fe3O4Addition influences powder original performance little.Powder is made in ball milling
The epoxy modified silicone resin of soft magnetic powder mass fraction 1% is added in end, amorphous iron silicon boron powder 1g is added, at 80 DEG C
Abundant mechanical stirring is carried out, then dried powder is put into progress room temperature compacting in circular ring type Alloy-steel mold, with adding for 5MPa/s
Rate compacting is pressed, pressure maintaining 3min under 800Mpa is obtained having a size of outer diameter 20mm, internal diameter 12mm, iron/tetra- oxidations three of height 3mm
Iron block composite material.By 450 DEG C of block progress, the vacuum heat treatment of 1h, vacuum degree≤10-3Pa.It is carried out using B-H analyzer
Magnetism testing, as shown in table 1 (Bmax=50mT), Effective permeability is with test frequency variation as schemed for obtained sample performance
Shown in 4.As shown in Figure 4, the Effective permeability of the powder core block changes smaller with frequency, is held essentially constant.Utilize MATS-
2010SD soft magnetism DC test system testing DC performance, obtaining sample maximum saturation magnetic induction density B s value is 1.71T, coercive
Power Hc is 6.44Oe, maximum permeability 223.
Table 1
| Frequency/kHz | 5 | 20 | 50 | 100 |
| Amplitude permeability | 94.64 | 93.88 | 93.52 | 92.38 |
| Magnetic loss (W/Kg) | 5.007 | 28.94 | 104.7 | 206 |
Embodiment 2
The ammonia that can soak iron powder is added in beaker in the pure Fe powder of water atomization that the average grain diameter for weighing 47g is 300 μm
Water, glass bar stir 20min clockwise, then weigh the Fe that 3g partial size is 20nm3O4Powder is premixed in V-type batch mixer.
Dry type ball milling is carried out using planetary ball mill, the Fe/Fe for taking dry type ball milling to prepare3O4Core-shell structure cladding powder 4g is added soft
The epoxy modified silicone resin of magnetic powder mass fraction 1% carries out abundant mechanical stirring at 80 DEG C, then dried powder is put
Enter progress room temperature compacting in circular ring type Alloy-steel mold, suppressed with the compression rate of 5MPa/s, pressure maintaining 3min under 800Mpa is obtained
Having a size of outer diameter 20mm, iron/ferroso-ferric oxide block composite material of internal diameter 12mm, height 3mm.Block is carried out 450 DEG C, 1h
Vacuum heat treatment, vacuum degree≤10-3Pa.Magnetism testing, obtained sample performance such as 2 institute of table are carried out using B-H analyzer
Show (Bmax=50mT), Effective permeability changes as shown in Figure 4 with test frequency.As shown in Figure 4, the powder core block has
It imitates magnetic conductivity and changes with frequency smaller, be held essentially constant, but magnetic conductivity is slightly below obtained by 75 μm of the pure Fe powder of water atomization
Composite magnetic powder core.Using MATS-2010SD soft magnetism DC test system testing DC performance, sample maximum saturation magnetic induction is obtained
Intensity Bs value is 1.44T, coercivity H 18.1Oe, maximum permeability 203.
Table 2
| Frequency/kHz | 5 | 20 | 50 | 100 |
| Amplitude permeability | 79.75 | 78.82 | 79.35 | 79.38 |
| Magnetic loss (W/Kg) | 7.084 | 43.67 | 178.5 | 325.1 |
Embodiment 3
The ammonia that can soak iron powder is added in beaker in the pure Fe powder of water atomization that the average grain diameter for weighing 47g is 75 μm
Water, glass bar stir 20min clockwise, then weigh the Mn that 3g partial size is 50nm0.6Zn0.4Fe2O4Powder, in V-type batch mixer into
Row premix.Dry type ball milling is carried out using planetary ball mill, Fig. 5 is by the Fe/Mn that obtains after high-energy ball milling0.6Zn0.4Fe2O4It is compound
The scanning electron microscope (SEM) photograph of powder, it can be seen that ball-milling technology is consistent for the oxide function and effect of heterogeneity or partial size, can
Obtain the soft magnetic composite powder that oxide on surface is evenly coated.The Fe/Mn for taking dry type ball milling to prepare0.6Zn0.4Fe2O4Core-shell structure
The epoxy modified silicone resin of soft magnetic powder mass fraction 1% is added in cladding powder 4g, and amorphous iron silicon boron powder is added
0.5g carries out abundant mechanical stirring at 80 DEG C, then dried powder is put into progress room temperature compacting in circular ring type Alloy-steel mold,
It is suppressed with the compression rate of 5MPa/s, pressure maintaining 3min under 800Mpa is obtained having a size of outer diameter 20mm, internal diameter 12mm, height 3mm's
Iron/manganese-zinc ferrite block composite material.By 550 DEG C of block progress, the vacuum heat treatment of 1h, vacuum degree≤10-3Pa.Use epoxy
Resin one fritter of cold edge is sintered block, and polishes to its surface, is swept using block section after scanning electron microscope shooting heat treatment
It is as shown in Figure 2 to retouch electron microscope, it is seen that the similar netted core-shell structure of honeycomb is obtained under the embodiment, core is straight iron powder, and shell is
Nanometer Mn0.6Zn0.4Fe2O4Powder.Magnetism testing, obtained sample performance (Bmax as shown in table 3 are carried out using B-H analyzer
=50mT), Effective permeability changes as shown in Figure 4 with test frequency.As shown in Figure 4, effective magnetic conductance of the powder core block
Rate is smaller with frequency variation, is held essentially constant, but magnetic conductivity is slightly below added to obtained by nano ferriferrous oxide powder
Composite magnetic powder core, composite magnetic powder core obtained by the pure Fe powder of water atomization higher than 75 μm.It is surveyed using MATS-2010SD soft magnetism direct current
Test system tests DC performance, obtains sample maximum saturation magnetic induction density B s value for 1.56T, coercivity H 8.35Oe, most
Big magnetic conductivity is 210.
Table 3
| Frequency/kHz | 5 | 20 | 50 | 100 |
| Amplitude permeability | 87.16 | 87.23 | 86.67 | 85.88 |
| Magnetic loss (W/Kg) | 7.498 | 34.39 | 114.3 | 269.3 |
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (9)
1. a kind of preparation method of the magnetic powder core material of stable magnetic conductivity and low loss, which is characterized in that by being grouped into iron/iron
The modified room temperature compacting of the composite powder of oxysome is heat-treated obtained again, includes the following steps:
1) iron powder surface mechanical-chemical modification: being added basic modifier into iron powder first, and stirring guarantees iron powder surface quilt
Modifying agent is soaked, and iron powder surface polarity is changed, and activates particle surface, increases apparent activation energy；
2) ball milling is dry-mixed: modified iron powder and nanometer ferrite powder progress ball milling is dry-mixed, obtain iron/iron of core-shell structure
Oxysome composite powder；
3) high temperature resistant binder and modified powder are added: by iron/ferrite composite powder obtained by binder, modified powder and step 2)
End mixing, and stir, guarantee that binder, modified powder are uniformly mixed with iron/ferrite composite powder and powder is dry；
4) room temperature compression moulding: the powder mixed according to step 3) is poured into alloy mold, is carried out room temperature compacting, is obtained
Iron/ferrite soft magnetic composite magnetic powder core；
5) subsequent heat treatment: gained iron/ferrite soft magnetic composite magnetic powder core in step 4) is carried out very under inert gas protection
Sky heat treatment, obtains the magnetic powder core material for stablizing magnetic conductivity and low loss；
In step 3), the binder selects epoxy modified silicone resin, and the modified powder selects amorphous iron silicon boron, amorphous
One or more of iron silicon boron carbon, amorphous iron silicochromium or amorphous matrix powder, the modified powder partial size are 10~30 microns.
2. the preparation method of the magnetic powder core material of stable magnetic conductivity and low loss according to claim 1, which is characterized in that step
1) iron powder described in is selected from one of water-atomized iron powder, gas atomization iron powder, reduced iron powder, iron silicon powder or iron aluminum silicon powder or several
Kind, the iron powder powder diameter is 30~100 microns.
3. the preparation method of the magnetic powder core material of stable magnetic conductivity and low loss according to claim 1, which is characterized in that step
2) nanometer ferrite is selected from nano ferriferrous oxide, Nanosized Mn-Zn Ferrite, nanometer nickel-zinc ferrite or Nanometer Copper zinc-iron
One or more of oxysome, step 2) the nanometer ferrite powder partial size are 10~50 nanometers.
4. the preparation method of the magnetic powder core material of stable magnetic conductivity and low loss according to claim 1, which is characterized in that step
2) in, milling parameters: ratio of grinding media to material be 10:1~30:1, revolving speed be 300r/min~200r/min, Ball-milling Time be 1h~
3h。
5. the preparation method of the magnetic powder core material of stable magnetic conductivity and low loss according to claim 1, which is characterized in that step
3) in, the binder additional amount is the iron/ferrite composite powder quality 0.5-3%, the modified powder additional amount
For the iron/ferrite composite powder quality 2-10%.
6. the preparation method of the magnetic powder core material of stable magnetic conductivity and low loss according to claim 1, which is characterized in that step
4) in, compression moulding is carried out in the case where 800-1000Mpa.
7. the preparation method of the magnetic powder core material of stable magnetic conductivity and low loss according to claim 1, which is characterized in that step
5) in, the technique of vacuum heat treatment are as follows: it is argon that sample, which is placed in 400-600 DEG C of heat preservation 60-120min, atmosphere in vacuum tube furnace,
Gas.
8. the preparation method of the magnetic powder core material of stable magnetic conductivity and low loss according to claim 1, which is characterized in that step
2) in, the quality proportioning of modified iron powder and nanometer ferrite powder meets: soft magnetic powder shared quality in final product
Percentage is 80%~98%, and remaining is ferrite powder, and wherein soft magnetic powder includes iron powder and modified powder.
9. using the magnetic powder core material for stablizing magnetic conductivity and low loss made from preparation method described in any one of claim 1-8.
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