CN106531388B - A kind of preparation method of composite magnetic powder and composite magnetic powder core - Google Patents
A kind of preparation method of composite magnetic powder and composite magnetic powder core Download PDFInfo
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- CN106531388B CN106531388B CN201610972526.5A CN201610972526A CN106531388B CN 106531388 B CN106531388 B CN 106531388B CN 201610972526 A CN201610972526 A CN 201610972526A CN 106531388 B CN106531388 B CN 106531388B
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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
- H01F1/33—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
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Abstract
The invention belongs to field of magnetic material preparation more particularly to the preparation methods of a kind of composite magnetic powder and composite magnetic powder core, method includes the following steps: a), using melt-quenching method preparing sendust strip;In preparation process, magnetic field is applied directional when getting rid of band;Sendust strip obtained is crushed, sendust fragment is obtained;B), by the sendust fragment and ferrite powder mixing and ball milling, composite magnetic powder is obtained;C), binder, lubricant and the composite magnetic powder are successively mixed and is suppressed, obtain composite magnetic powder core.The experimental results showed that Effective permeability of the powder core made of method provided by the present invention under the test frequency of 100kHz is higher than 40, the loss at 100kHz, Bm=300mT test condition is lower than 83W/kg.
Description
Technical field
The invention belongs to field of magnetic material preparation more particularly to the preparation sides of a kind of composite magnetic powder and composite magnetic powder core
Method.
Background technique
Iron-silicon-aluminum soft magnet alloy, also known as Sendust alloy, chemical composition 5.4wt.%Al, 9.6
Wt.%Si, remaining is Fe (85wt.%).Sendust is highly brittle, it is easy to be broken into powder, be typically prepared into
Powder core uses.
Compared with iron silicon core and ferrocart core, Fe-Si-Al magnetic core high-frequency loss is lower, and saturation magnetic strength with higher
Intensity and magnetic conductivity are answered, it is cheap, it is advantageously implemented miniaturization.In addition, the magnetostriction coefficient λ of sendustsIt is close
In zero, be conducive to eliminate the audible frequencies noise generated when filter inductor work.Due to spies such as low-loss, low costs
Point and the unrivaled comprehensive performance of other powder cores, Fe-Si-Al magnetic core get up by fast development, in outputting inductance, line
It is widely used in the devices such as path filter, power factor corrector.
The Fe-Si-Al magnetic core working frequency of early stage is relatively low, only requires high magnetic conductivity and requires loss not high.
As the use working frequency of Fe-Si-Al magnetic core is higher and higher, high-frequency loss is big, how to guarantee powder core high magnetic permeability
In the case of, reducing magnetic core high-frequency loss becomes outstanding problem.Therefore the influence factor of powder core magnetic conductivity and core loss is studied
Just it is particularly important.Mainly pass through that improve magnetic particle capability, selection suitable exhausted about the research of metal magnetic powder core both at home and abroad
Edge agent and granularity of magnet powder adjust the methods of pressing parameter to improve the magnetic property of powder core.With going deep into for research, consider from work
It is improved in terms of skill, as the magnetic conductivity of powder core and the influence of loss are got in briquetting pressure, insulating wrapped technique and heat treatment
More to attract attention.One of most critical process is exactly the insulating wrapped technique of powder in Fe-Si-Al magnetic core production process.Pass through
Insulating wrapped can obstruct the electrical contact between magnetic powder, so as to increase the resistivity of magnetic powder, reduce high-frequency loss.
The insulating wrapped technique that common Fe-Si-Al magnetic core preparation method uses both at home and abroad at present, what is used is non magnetic exhausted
Edge layer dilutes magnetism, causes magnetic conductivity low;Insulating layer unstable (pyrolytic) and low (the powder core compression moulding process of intensity
Middle clad is easy to be crushed) lead to high-frequency loss height.In addition, currently used Fe-Si-Al magnetic flatness is not good enough, it is unfavorable
In further increase magnetic conductivity and reduce high-frequency loss.
Summary of the invention
In view of this, the purpose of the present invention is to provide the preparation method of a kind of composite magnetic powder and composite magnetic powder core, by this
Powder core magnetic conductivity with higher and lower high-frequency loss made from the method provided are provided.
The present invention provides a kind of preparation methods of composite magnetic powder, comprising the following steps:
A), sendust strip is prepared using melt-quenching method;In preparation process, magnetic field is applied directional when getting rid of band;It will
Sendust strip obtained is crushed, and sendust fragment is obtained;
B), by the sendust fragment and ferrite powder mixing and ball milling, composite magnetic powder is obtained.
Preferably, the magnetic field strength of the directional magnetic field is 500~2000Oe.
Preferably, it gets rid of band and applies directional magnetic field always in the process.
Preferably, the sendust strip with a thickness of 5~50 μm.
Preferably, the partial size of the ferrite powder is 10nm~2 μm.
Preferably, the mass ratio of the sendust fragment and ferrite powder is 100:(2~20).
Preferably, the ball material mass ratio in the mechanical milling process is (10~15): 1.
Preferably, the ball radius that the ball milling uses is 3~15mm.
The present invention provides a kind of preparation methods of composite magnetic powder core, comprising the following steps:
Binder, lubricant and the composite magnetic powder being prepared according to above-mentioned technical proposal the method are successively mixed
And compacting, obtain composite magnetic powder core.
Preferably, the pressure of the compacting is 1500~2000MPa;The time of the compacting is 3~8min.
Compared with prior art, the present invention provides the preparation method of a kind of composite magnetic powder and composite magnetic powder core, the present invention
The preparation method of the composite magnetic powder core of offer is the following steps are included: a), using melt-quenching method prepare sendust strip;System
During standby, magnetic field is applied directional when getting rid of band;Sendust strip obtained is crushed, it is broken to obtain sendust
Piece;B), by the sendust fragment and ferrite powder mixing and ball milling, composite magnetic powder is obtained;C), by binder, lubrication
Agent and the composite magnetic powder are successively mixed and are suppressed, and composite magnetic powder core is obtained.The present invention is preparing sendust first
The band that gets rid of when strip applies directional magnetic field in the process, improves the saturation magnetization of sendust strip in this way
And magnetic conductivity.Sendust fragment and ferrite powder ball milling are obtained by broken later, by means of the effect of being rolled when ball milling, is made
Ferrite powder is uniformly embedded into sendust fractal surfaces, forms ferrite insulating coating.The present invention passes through ball milling
Mode mixed ferrite powder and sendust fragment are not only able to that ferrite is made uniformly, to be firmly coated on the conjunction of iron sial
Golden fractal surfaces, and can be realized as ferrite powder foot couple sendust in the lower situation of the dosage of ferrite powder
The complete cladding on surface reduces ferritic influence of the introducing for magnetic powder magnetic conductivity, make the magnetic conductivity of magnetic powder maintain compared with
High level, while ball milling can also further realize the flattening of magnetic powder, to further increase magnetic conductivity and the reduction of magnetic powder
The high-frequency loss for the powder core being made from it.Powder core made of composite magnetic powder provided by the present invention have high magnetic conductivity and
Low high-frequency loss, has a extensive future, and cannot be only used for telecommunication, radar, applies also for inhaling and involves electromagnetic shielding field.It is real
Test the result shows that, Effective permeability of the powder core made of method provided by the present invention under the test frequency of 100kHz is higher than
40, the loss at 100kHz, Bm=300mT test condition is lower than 83W/kg.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the Effective permeability of the composite magnetic powder core for the different ratio that the embodiment of the present invention 6 provides;
Fig. 2 is the loss of the composite magnetic powder core for the different ratio that the embodiment of the present invention 6 provides;
Fig. 3 is the Effective permeability of the composite magnetic powder core for the different annealing temperature that the embodiment of the present invention 12 provides;
Fig. 4 is the loss of the composite magnetic powder core for the different annealing temperature that the embodiment of the present invention 12 provides.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of preparation methods of composite magnetic powder, comprising the following steps:
A), sendust strip is prepared using melt-quenching method;In preparation process, magnetic field is applied directional when getting rid of band;It will
Sendust strip obtained is crushed, and sendust fragment is obtained;
B), by the sendust fragment and ferrite powder mixing and ball milling, composite magnetic powder is obtained.
In preparation method provided by the invention, sendust strip is prepared first.The present invention uses melt-quenching method
Sendust strip is prepared, applies directional magnetic field always during getting rid of band.In the present invention, the magnetic field of the directional magnetic field
Intensity is preferably 500~2000Oe, more preferably 1000~1200Oe.It in the present invention, can be by adjusting copper during getting rid of band
Roller revolving speed controls the thickness of strip, and copper roller revolving speed is faster, and thickness is thinner, and copper roller revolving speed is preferably 30~80m/s.The present invention couple
The equipment for preparing sendust strip is not particularly limited, induction type fast melt-quenching preferably well known to those skilled in the art
Equipment.After preparation, sendust strip is obtained.In the present invention, the sendust strip is by Si, Al and Fe group
At, wherein content of the Si in alloy thin band is preferably 9.3~9.7wt%, more preferably 9.6wt%;Al in alloy thin band
In content be preferably 5.2~5.6wt%, more preferably 5.4wt%;Surplus is Fe.In the present invention, the sendust
The thickness of strip is preferably 5~50 μm, more preferably 5~30 μm, most preferably 5~15 μm.After obtaining sendust strip,
Sendust strip obtained is crushed, sendust fragment is obtained.
After obtaining sendust fragment, by the sendust fragment and ferrite powder mixing and ball milling.Wherein, iron
Ferrite powder is preferably manganese-zinc ferrite powder, chemical general formula MnxZn1-xFe2O4, 0 < x < 1.Provided by the invention one
In a embodiment, the chemical general formula of the manganese-zinc ferrite powder is Mn0.4Zn0.6Fe2O4.In the present invention, the ferrite powder
The partial size at end is preferably 10nm~2 μm.The source of the ferrite powder is not particularly limited in the present invention, and chemistry can be used altogether
Heavy method is prepared, and by taking manganese-zinc ferrite powder as an example, can be prepared in accordance with the following methods:
(1), molysite, zinc salt, manganese salt and water mixing, obtain mixing salt solution;
(2), the pH value that the mixing salt solution is adjusted with water soluble alkali, is reacted, and manganese-zinc ferrite presoma is obtained;
(3), the manganese-zinc ferrite presoma is roasted, and obtains manganese-zinc ferrite powder.
In the above-mentioned method for preparing manganese-zinc ferrite powder provided by the invention, first by molysite, zinc salt, manganese salt and water
Mixing, wherein the molysite is the soluble salt or its hydrate of iron, including but not limited to FeCl3、Fe(NO3)3And Fe2(SO4)3
One of or it is a variety of;The zinc salt is the soluble salt or its hydrate of zinc, including but not limited to ZnCl2、Zn(NO3)2With
ZnSO4One of or it is a variety of;The manganese salt is the soluble salt or its hydrate of manganese, including but not limited to MnCl2、MnCl2·
4H2O、Mn(NO3)2And MnSO4One of or it is a variety of.After molysite, zinc salt and manganese salt are completely dissolved in water, salt-mixture is obtained
Solution.
After obtaining mixing salt solution, the pH value of the mixing salt solution is adjusted to alkalinity with water soluble alkali.Wherein, described can
Dissolubility alkali is preferably NaOH or its aqueous solution, and the concentration of the NaOH aqueous solution is preferably 1~2mol/L.In the present invention, excellent
It recruits and saves the pH value of the mixing salt solution to 9~13, more preferably 10~11.In the present invention, it is preferred to existing by the mixing
The temperature of liquor is heated to 50~90 DEG C, adjusts its pH value again after more preferably 70~80 DEG C.After pH is adjusted, salt-mixture
It reacts between each ion in solution, obtains solid sediment, the solid sediment is manganese-zinc ferrite presoma.
In the present invention, the time of the reaction is preferably 10~60min, more preferably 30~40min.
After obtaining manganese-zinc ferrite presoma, the manganese-zinc ferrite presoma is roasted.Wherein, the roasting
Temperature is preferably 800~900 DEG C, and more preferably 850~870 DEG C;The time of the roasting is preferably 1~5h, more preferably 2~
3h.After roasting, manganese-zinc ferrite powder is obtained.In the present invention, the manganese-zinc ferrite presoma is preferably being roasted
Before burning, is first washed and dried.The temperature of the drying is preferably 90~100 DEG C;The time of the drying is preferably 1~
2h。
In the present invention, during ferrite powder and sendust fragment carry out ball milling, the sendust
The mass ratio of fragment and ferrite powder is preferably 10:(2~20), more preferably 100:2,100:4,100:6,100:10 or
100:20.In the present invention, the ball material mass ratio in the mechanical milling process is preferably (10~15): 1, more preferably (12~
13): 1.In the present invention, the abrading-ball that the ball milling uses is preferably steel ball;The steel ball size is preferably 3~15mm, more excellent
It is selected as 5~10mm;In one embodiment provided by the invention, the abrading-ball includes the steel ball that diameter is 5mm and diameter is
The steel ball of 10mm, the number for the steel ball that the steel ball and diameter that diameter is 5mm are 10mm is than being preferably (3~10): 1, more preferably
5:1.In the present invention, the revolving speed of the ball milling is preferably 30~80rpm, more preferably 50~60rpm;The time of the ball milling
Preferably 20~60h, more preferably 30~40h.After ball milling, composite magnetic powder is obtained.
The present invention applies directional magnetic field during getting rid of band when preparing sendust strip first, in this way
It can be improved the saturation magnetization and magnetic conductivity of sendust strip.Later by broken sendust strip and iron oxygen
Body powder ball milling is uniformly embedded into ferrite powder in sendust fractal surfaces, is formed by means of the effect of rolling when ball milling
Ferrite insulating coating.The present invention mixed ferrite powder and sendust fragment by way of ball milling are not only able to make
Ferrite uniformly, is firmly coated on sendust fractal surfaces, and in the lower situation of the dosage of ferrite powder
The complete cladding that can be realized as ferrite powder foot couple sendust surface reduces ferritic introducing for magnetic powder magnetic conductance
The influence of rate makes the magnetic conductivity of magnetic powder maintain higher level, while ball milling can also realize the flattening of magnetic powder, thus into one
The high-frequency loss for the powder core that step improves the magnetic conductivity of magnetic powder and reduction is made from it.With answering for method provided by the invention preparation
Closing magnetic powder is that powder core made of raw material has high magnetic conductivity and low high-frequency loss, has a extensive future, cannot be only used for
Telecommunication, radar apply also for inhaling and involve electromagnetic shielding field.The experimental results showed that with made from method provided by the invention
Composite magnetic powder is that Effective permeability of the composite magnetic powder core under the test frequency of 100kHz made of raw material is higher than 40,
Loss under 100kHz, Bm=300mT test condition is lower than 83W/kg.
The present invention also provides the composite magnetic powders that one kind is prepared according to the method described above, which includes iron sial
Alloy magnetic powder and the ferrite powder for being coated on the Fe-Si-Al magnetic surface, the composite magnetic powder are with higher in flat
Magnetic conductivity, higher saturation magnetization and lower high-frequency loss, have a extensive future.
The present invention also provides a kind of preparation methods of composite magnetic powder core, comprising the following steps:
Binder, lubricant and the composite magnetic powder being prepared according to above-mentioned technical proposal the method are successively mixed
And compacting, obtain composite magnetic powder core.
In the preparation method of composite magnetic powder core provided by the invention, first by binder, lubricant and the compound magnetic
Powder is mixed.Wherein, the binder is preferably epoxy resin;The mass ratio of the binder and composite magnetic powder is preferably (1
~2): 100, more preferably 1.5:100.The lubricant is preferably magnesium stearate;The quality of the lubricant and composite magnetic powder
Than preferably (0.5~2): 100, more preferably (1~1.5): 100.After mixing, suppressed.Wherein, the compacting
Pressure is preferably 1500~2000MPa, more preferably 1700~1800MPa;The time of the compacting is preferably 3~8min.Pressure
After system, composite magnetic powder core is obtained.In the present invention, it is preferred to be made annealing treatment to obtained composite magnetic powder core, to eliminate
Its internal stress improves magnetic conductivity.Wherein, the temperature of the annealing is preferably 600~700 DEG C, more preferably 650~
690℃;The soaking time of the annealing is preferably 1~2h.
There is high magnetic conductivity and low high-frequency loss, application using composite magnetic powder core made from method provided by the invention
It has a extensive future, cannot be only used for telecommunication, radar, apply also for inhaling and involve electromagnetic shielding field.The experimental results showed that the present invention
Effective permeability of the composite magnetic powder core of offer under the test frequency of 100kHz is higher than 40, surveys in 100kHz, Bm=300mT
Loss under the conditions of examination is lower than 83W/kg.
Overall merit technical solution provided by the invention, has the advantage that
1) sendust strip is produced using induction type fast melt-quenching equipment, gets rid of band and apply directional magnetic field in the process, makes
Easy axis is orientated along external magnetic field, improves the saturation magnetization and magnetic conductivity of sendust strip obtained;
2), mixed ferrite powder and sendust fragment by the way of ball milling, by means of the effect of being rolled when ball milling,
It is uniformly embedded into ferrite powder in sendust fractal surfaces, forms uniform, firm ferrite insulating coating;It avoids
Insulating layer unstable (pyrolytic) that Fe-Si-Al magnetic easily occurs during insulating wrapped, the low (compression moulding of intensity
Clad is easy to be crushed in journey), discontinuous and thickness the problems such as being difficult to control;
3), mixed ferrite powder and sendust fragment by the way of ball milling, can be in the dosage of ferrite powder
The complete cladding that can be realized as ferrite powder foot couple sendust surface in lower situation, reduces ferritic introducing
Influence for magnetic powder magnetic conductivity makes the magnetic conductivity of magnetic powder maintain higher level, provides to obtain the powder core of high magnetic permeability
Technical guarantee;
4), by carrying out ball milling to sendust fragment, flattening magnetic powder can be obtained, to further increase magnetic powder
Magnetic conductivity and the high-frequency loss for reducing the powder core being made from it;
5) ferrite powder preferably, is prepared using chemical coprecipitation, reaction speed is fast, and yield is high;
6), the composite magnetic powder core preferably obtained to compacting makes annealing treatment, to eliminate the internal stress of powder core, further
Improve the magnetic conductivity of powder core.
For the sake of becoming apparent from, it is described in detail below by following embodiment.
Embodiment 1
(1) the standard analysis sendust band with a thickness of 5~15 μm is prepared in induction type fast melt-quenching equipment
(5.4wt%Al, 9.6wt%Si, remaining Fe), during preparing alloy strip, copper roller revolving speed when getting rid of band is 60m/s, gets rid of band
Apply the directional magnetic field of 1000Oe always in the process.It after obtaining sendust band, is crushed in stainless cylinder of steel, obtains iron
Silico-aluminum fragment.
(2) with FeCl3、ZnCl2And MnCl2·4H2O is raw material, by Mn0.4Zn0.6Fe2O4Middle Fe3+、Zn2+、Mn2+Mole
Than n [Fe3+]:n[Zn2+]:n[Mn2+]=10:3:2 weighs the raw material of needs respectively, appropriate amount of deionized water is added, being stirred continuously makes
Feed particles dissolution completely, obtains Fe-Zn-Mn mixing salt solution, is heated to 80 DEG C, while instilling the NaOH that concentration is 2mol/L
Solution is stirred continuously, and the pH value for adjusting solution is 10, is reacted 30min, is synthesized manganese-zinc ferrite presoma;It uses after reaction
Deionized water washs ferrite presoma for several times, is placed in drying box at 100 DEG C dry 1h.Iron after drying is supported into body forerunner
Body is placed in Muffle furnace the manganese-zinc ferrite powder for obtaining that partial size is 10nm~2 μm in 850 DEG C of roasting 2h.
(3) sendust fragment is placed in the stainless steel jar mill of ball mill, by manganese-zinc ferrite powder and iron silicon
The mass ratio of aluminium alloy fragment is 2%, and the manganese-zinc ferrite powder of corrresponding quality is put into stainless steel jar mill and iron sial
Alloy fragment carries out ball milling;For the abrading-ball that ball milling uses for the steel ball of diameter 10mm and 5mm, the number ratio of big ball and bead is 1:5;
Ball material mass ratio when ball milling is 12:1, after drum's speed of rotation 50rpm, ball milling 30h, obtains iron sial/compound magnetic of ferrite
Powder.
(4) epoxy resin and composite magnetic powder quality of composite magnetic powder quality 1.5wt% are added in obtained composite magnetic powder
The magnesium stearate of 1wt.% is cold-pressed 5min at 1800Mpa later, obtains composite magnetic powder core blank.
(5) by composite magnetic powder core blank at 600 DEG C in annealing in nitrogen 2h, obtain composite magnetic powder core product.
Embodiment 2~5
Referring to the preparation method of embodiment 1, it is sequentially adjusted in the mass ratio of manganese-zinc ferrite powder Yu sendust fragment
It is 4%, 6%, 10%, 20%, composite magnetic powder core product is prepared.
Comparative example 1
Referring to the preparation method of embodiment 1, the mass ratio for adjusting manganese-zinc ferrite powder and sendust fragment is 0,
Composite magnetic powder core product is prepared.
Embodiment 6
Composite magnetic powder core product made from testing example 1~5 and comparative example 1 is distinguished under the test frequency of 100kHz
Effective permeability, as a result as shown in Figure 1, Fig. 1 is effective magnetic of the composite magnetic powder core for the different ratio that the embodiment of the present invention 6 provides
Conductance, as seen in Figure 1, the Effective permeability of powder core made from the method provided using Examples 1 to 5 are higher than 40.
Composite magnetic powder made from testing example 1~5 and comparative example 1 is distinguished at 100kHz, Bm=300mT test condition
The loss (Core loss) of core product, as a result as shown in Fig. 2, Fig. 2 is answering for the different ratio that the embodiment of the present invention 6 provides
The loss of powder core is closed, as seen in Figure 2, the loss using powder core made from the method that Examples 1 to 5 provides is lower than
83W/kg。
Embodiment 7
(1) the standard analysis sendust band with a thickness of 5~15 μm is prepared in induction type fast melt-quenching equipment
(5.4wt%Al, 9.6wt%Si, remaining Fe), during preparing alloy strip, copper roller revolving speed when getting rid of band is 60m/s, gets rid of band
Apply the directional magnetic field of 1000Oe always in the process.It after obtaining sendust band, is crushed in stainless cylinder of steel, obtains iron
Silico-aluminum fragment.
(2) with FeCl3、ZnCl2And MnCl2·4H2O is raw material, by Mn0.4Zn0.6Fe2O4Middle Fe3+、Zn2+、Mn2+Mole
Than n [Fe3+]:n[Zn2+]:n[Mn2+]=10:3:2 weighs the raw material of needs respectively, appropriate amount of deionized water is added, being stirred continuously makes
Feed particles dissolution completely, obtains Fe-Zn-Mn mixing salt solution, is heated to 80 DEG C, while instilling the NaOH that concentration is 2mol/L
Solution is stirred continuously, and the pH value for adjusting solution is 10, is reacted 30min, is synthesized manganese-zinc ferrite presoma;It uses after reaction
Deionized water washs ferrite presoma for several times, is placed in drying box at 100 DEG C dry 1h.Iron after drying is supported into body forerunner
Body is placed in Muffle furnace the manganese-zinc ferrite powder for obtaining that partial size is 10nm~2 μm in 850 DEG C of roasting 2h.
(3) sendust fragment is placed in the stainless steel jar mill of ball mill, by manganese-zinc ferrite powder and iron silicon
The mass ratio of aluminium alloy fragment is 6%, and the manganese-zinc ferrite powder of corrresponding quality is put into stainless steel jar mill and iron sial
Alloy fragment carries out ball milling;For the abrading-ball that ball milling uses for the steel ball of diameter 10mm and 5mm, the number ratio of big ball and bead is 1:5;
Ball material mass ratio when ball milling is 12:1, drum's speed of rotation 50rpm, ball milling 30h, after ball milling, obtains iron sial/iron oxygen
Bluk recombination magnetic powder.
(4) epoxy resin and composite magnetic powder quality of composite magnetic powder quality 1.5wt% are added in obtained composite magnetic powder
The magnesium stearate of 1wt.% is cold-pressed 5min at 1800Mpa later, obtains composite magnetic powder core blank.
(5) by composite magnetic powder core blank at 600 DEG C in annealing in nitrogen 1h, obtain composite magnetic powder core product.
Embodiment 8~11
Referring to the preparation method of embodiment 7, the temperature for being sequentially adjusted in composite magnetic powder core blank anneal is 630 DEG C, 660 DEG C,
690 DEG C, 720 DEG C, are prepared composite magnetic powder core product.
Embodiment 12
Effective magnetic conductance of composite magnetic powder core product made from testing example 7~11 is distinguished under the test frequency of 100kHz
Rate, as a result as shown in figure 3, Fig. 3 is effective magnetic conductance of the composite magnetic powder core for the different annealing temperature that the embodiment of the present invention 12 provides
Rate, as seen in Figure 3, the Effective permeability of powder core made from the method provided using embodiment 7~11 are higher than 60.
Composite magnetic powder core product made from testing example 7~11 is distinguished at 100kHz, Bm=300mT test condition
Loss (Core loss), as a result as shown in figure 4, Fig. 4 be the embodiment of the present invention 12 provide different annealing temperature compound magnetic
The loss of powder core, as seen in Figure 4, the loss using powder core made from the method that embodiment 7~11 provides are lower than
68W/kg。
Comparative example 2
Referring to the preparation method of embodiment 1, magnetic field, manganese-zinc ferrite powder are not only applied directional during getting rid of band
Mass ratio with sendust fragment is 6%, and composite magnetic powder core product is prepared, at 690 DEG C after annealing in nitrogen 1h,
Detect Effective permeability and loss.Effective permeability is only 51.2 under the test frequency of 100kHz.In 100kHz, Bm=
Loss is 71W/kg under 300mT test condition.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of composite magnetic powder, comprising the following steps:
A), sendust strip is prepared using melt-quenching method;In preparation process, magnetic field is applied directional when getting rid of band;It will be made
Sendust strip be crushed, obtain sendust fragment;
B), by the sendust fragment and ferrite powder according to mass ratio 100:(2~20) mixing and ball milling, it obtains compound
Magnetic powder;
The composite magnetic powder includes sendust fragment and coats the ferrite powder of the sendust fractal surfaces completely
End.
2. preparation method according to claim 1, which is characterized in that the magnetic field strength of the directional magnetic field be 500~
2000Oe。
3. preparation method according to claim 2, which is characterized in that get rid of band and apply directional magnetic field always in the process.
4. preparation method according to claim 1, which is characterized in that the sendust strip with a thickness of 5~50 μ
m。
5. preparation method according to claim 1, which is characterized in that the partial size of the ferrite powder is 10nm~2 μm.
6. preparation method according to claim 1, which is characterized in that the ball material mass ratio in the mechanical milling process is (10
~15): 1.
7. preparation method according to claim 1, which is characterized in that the ball radius that the ball milling uses is 3~15mm.
8. a kind of preparation method of composite magnetic powder core, comprising the following steps:
It binder, lubricant and is successively mixed according to the composite magnetic powder that any one of claim 1~7 the method is prepared
It closes and suppresses, obtain composite magnetic powder core.
9. preparation method according to claim 8, which is characterized in that the pressure of the compacting is 1500~2000MPa;Institute
The time for stating compacting is 3~8min.
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CN107598160B (en) * | 2017-09-05 | 2020-01-14 | 山东非金属材料研究所 | Iron-silicon-aluminum/ferrite composite wave absorbing agent and preparation method thereof |
CN108039260A (en) * | 2017-10-26 | 2018-05-15 | 中国兵器科学研究院宁波分院 | A kind of preparation method of 60 iron silica magnetic particle core materials of μ |
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CN109192432A (en) * | 2018-08-31 | 2019-01-11 | 周晓东 | A kind of preparation method of compound structure type soft magnetic materials |
CN111584222B (en) * | 2019-02-18 | 2021-11-30 | 深圳市麦捷微电子科技股份有限公司 | Method for manufacturing laminated chip type power inductor |
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CN113345703B (en) * | 2021-04-19 | 2022-11-29 | 马鞍山市鑫洋永磁有限责任公司 | Preparation method of composite magnetic powder |
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