CN109887698A - A kind of composite magnetic powder core and preparation method thereof - Google Patents
A kind of composite magnetic powder core and preparation method thereof Download PDFInfo
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Abstract
A kind of composite magnetic powder core and preparation method thereof, is related to the preparation method of metal soft magnetic powder core.The composite magnetic powder core includes FeSiCr magnetic powder and Ni nanoparticle Zn ferrite covering, wherein FeSiCr magnetic powder is Fe80~90Si0.1~10Cr5~10, 5 μm~20 μm of partial size；NiZn ferrite is NixZn1‑xFe2O4, partial size 100nm~1 μm, 0.2≤x≤0.4；NiZn ferrite covering is 3wt%~5wt% of FeSiCr magnetic powder quality.The present invention uses NiZn ferrite for raw material, Ni nanoparticle Zn ferrite is prepared as covering through crushing ball mill, and insulating wrapped process is completed in acetone soln, NiZn ferrite powder is set to be evenly coated at FeSiCr magnetic powder surface, to prepare the composite magnetic powder core of a kind of high resistivity, high magnetic flux density, high Effective permeability, low-power consumption.
Description
Technical field
The present invention relates to a kind of preparation methods of metal soft magnetic powder core, and in particular to a kind of FeSiCr/ Ni nanoparticle Zn iron oxygen
The preparation method of bluk recombination powder core.
Background technique
Due to the high frequency of electronic device applications environment, high DC stacked, high current and high power density demand, tradition
Core material such as soft magnetic ferrite, metal soft magnetic material etc. is no longer applicable in.Soft magnetic ferrite although electricity with higher
Resistance rate, but since it belongs to ferrimagnetic material, magnetic flux density only has the 1/3~1/2 of metal soft magnetic material；Metal soft magnetic material
Magnetic flux density with higher, but its resistivity is extremely low, meets difficulty in frequency applications.Metal soft magnetic powder core refers to by iron
A kind of metallic composite of Magnaglo and the repressed molding of dielectric and formation.Since it combines soft magnetic metallic material
And the advantages of soft magnetic ferrite, operating frequency range it is wider it is higher, soft magnet performance is excellent, cost is relatively low, become domestic in recent years
The new hot spot of outer investigation of materials.
Preparing the most key process of soft magnetism composite magnetic powder core is magnetic powder particles surface insulation cladding process, main at present
It is divided into following three classes: chemical surface treatment technique；Coated with Organic Matter treatment process；Inorganic matter coats treatment process.Chemical table
Surface treatment technique mainly uses inorganic acid salt, such as phosphoric acid, phosphate, carries out surface passivating treatment to metal magnetic.Patent CN
107424706 A directly adopt phosphoric acid solution and impregnate the method for silicon-steel magnetic powder to realize cladding, the composite magnetic powder core of preparation
Magnetic induction density B at 50Hz, 5000A/m5000>=500mT, the loss at 25 DEG C, 20kHz, 100mT are 30~50W/
kg.The coated insulating layer of the method is uniform, and thickness is easily controllable, but this inorganic salts passivation layer non-refractory, and inorganic acid
Considerable degree of pollution can be caused to environment.In Coated with Organic Matter treatment process, 105225783 A of Chinese patent CN is disclosed
Insulating wrapped is carried out to powder core using resulting epoxy modified silicone resin after the reaction such as epoxy resin, organic siliconresin,
The composite magnetic powder core magnetic permeability μ of preparationeIt is 60 ± 8%, the loss at 25 DEG C, 50kHz, 100mT is 450mW/cm3Left and right.This
Kind technique can greatly improve the resistivity on Magnaglo surface to reduce eddy-current loss.But it is resistance to due to organic coating material
Hot property is poor, and the soft-magnetic composite material of this coating layer material preparation can only carry out hot-working when temperature is lower than 500 DEG C, when
When the temperature is excessively high, organic coating layer material starts the fusing that softens, and adjacent ferrous powder granules form effective contact, lead to the electricity of material
Resistance rate sharply declines, to lose insulating effect, and excessive namagnetic substance is added can make powder core soft magnet performance substantially
Degree decline.Magnaglo method for coating more universal at present is the processing of inorganic matter cladding, 108335820 A of Chinese patent CN
The cladding on Fe powder surface, the composite magnetic powder core Effective permeability μ of preparation are completed using MnZn ferrite and iron powder mixing and ball millingeMost
It can reach 223 greatly, saturation induction density Bs=1.71T, but whole preparation process is complex, and it is equal to be unfavorable for control product
One property, furthermore MnZn ferrite resistivity is far below NiZn ferrite, coats the composite magnetic powder core of preparation with MnZn ferrite
Resistivity is relatively low.106356177 A of Chinese patent CN prepares Nano-MnZn Ferrite to FeSiAl magnetic powder using hydro-thermal method
It is coated, the composite magnetic powder core Effective permeability μ of preparationeReach 76.4, the loss at 100kHz, 300mT, 25 DEG C is
56.5W/kg, although the FeSiAl composite magnetic powder core magnetic conductivity of this method preparation is higher, this method preparation process is multiple
It is miscellaneous, it is difficult to realize volume production.Therefore, the powder core that a kind of preparation process is simple, cost is relatively low, composite magnetic powder core electromagnetic performance is excellent
Preparation method becomes needing for this field.
Summary of the invention
Present invention is generally directed to when prior art preparation composite magnetic powder core, the covering and method for coating of selection cause multiple
The Effective permeability and saturation magnetization sharp fall of powder core are closed, resistivity promotes the problems such as amplitude is little, provides one
The novel method for coating that kind preparation process is simple, at low cost, composite magnetic powder core is had excellent performance.The present invention use NiZn ferrite for
Raw material prepares Ni nanoparticle Zn ferrite as covering through crushing ball milling, and insulating wrapped process is completed in acetone soln,
NiZn ferrite powder is set to be uniformly coated on FeSiCr magnetic powder surface, so that it is strong to prepare a kind of high resistivity, high magnetic
The FeSiCr/ Ni nanoparticle Zn ferrite composite magnetic powder core of degree, high Effective permeability, low-power consumption.
The technical problem to be solved by the invention is to provide a kind of preparation processes high resistivity simple, at low cost, Gao Ci
Induction, high Effective permeability, the FeSiCr/ Ni nanoparticle Zn ferrite composite magnetic powder core material of low-power consumption and preparation side
Method.Comparative example 1 and 2 is set forth uncoated FeSiCr powder core and has coated 4wt% Nano-meter SiO_22Composite magnetic powder core,
Coat Nano-meter SiO_22Although composite magnetic powder core resistivity afterwards is higher, since it is namagnetic substance, lead to composite magnetic powder
The saturation magnetization M of coresWith Effective permeability μeSharp fall.And the Ni nanoparticle Zn ferrite cladding that the present invention develops
Composite magnetic powder core material, compared to uncoated pure FeSiCr magnetic powder, Effective permeability only declines 16%, saturation magnetization Ms
Only decline 8%, resistivity improves three orders of magnitude, and loss declines 25% at 25 DEG C of 3MHz 10mT.Composite magnetic powder of the present invention
Core material has Effective permeability μe=55 ± 10%, saturation magnetization MsP is lost in: >=1.4T (25 DEG C)L(500kHz
10mT) :≤47kW/m3P is lost in (25 DEG C)L(1MHz 10mT) :≤97kW/m3P is lost in (25 DEG C)L(3MHz 10mT) :≤
671kW/m3(25 DEG C), electricalresistivityρ > 103Ω m, density dm> 6.85g/cm3Etc. characteristics.
The technical solution adopted by the invention is as follows:
A kind of composite magnetic powder core, which is characterized in that including FeSiCr magnetic powder and Ni nanoparticle Zn ferrite covering, wherein
The FeSiCr powder structure formula is Fe80~90Si0.1~10Cr5~10, partial size is 5 μm~20 μm；The NiZn ferrite structure formula
For NixZn1-xFe2O4, partial size is 100nm~1 μm, 0.2≤x≤0.4；The NiZn ferrite covering is FeSiCr magnetic powder matter
3wt%~5wt% of amount.
A kind of preparation method of composite magnetic powder core, specifically includes the following steps:
The cleaning of step 1, FeSiCr magnetic powder:
Deionized water is respectively adopted, acetone cleans FeSiCr magnetic powder, to remove the impurity and greasy dirt on magnetic powder surface；
The preparation of step 2, Ni nanoparticle Zn ferrite covering:
Use traditional solid sintering technology preparation structure formula for NixZn1-xFe2O4NiZn ferrite, 0.2≤x≤0.4,
It crushes, ball milling, obtains the powder that partial size is 100nm~200nm, as ferrite covering；
Step 3, insulating wrapped:
The magnetic powder after step 1 cleaning is infiltrated using acetone, wherein acetone account for the 10wt% of magnetic powder quality~
15wt%；Then, the Ni nanoparticle Zn iron oxygen that the step 2 for the 3wt%~5wt% for accounting for FeSiCr magnetic powder quality obtains is added thereto
Body covering, account for FeSiCr magnetic powder quality 1wt%~3wt% W-6C binder, be stirred continuously, dry, sieving；
Step 4, compression moulding:
By the powder after step 3 sieving using hydraulic press compression moulding under the pressure of 1GPa~20GPa, the pressing time is
10s obtains the Both ring sam having a size of Ф 12.0mm × Ф 8.0mm × h mm (h is thickness of sample)；
Step 5, annealing:
The Both ring sam that step 4 is obtained is placed in tube furnace, at a temperature of 600 DEG C~1000 DEG C, under air atmosphere, is moved back
0.5~2h of fire to in-furnace temperature cooled to room temperature, takes out after the completion, the composite magnetic powder core can be obtained；
Step 6, test:
The composite magnetic powder core that step 5 is obtained carries out electromagnetic performance test: where Effective permeabilityIn formula, L is the inductance of powder core, LeFor the effective magnetic circuit length of powder core, when N is test on magnet ring
Coil turn, AeFor the effective sectional area of powder core；Test condition is f=1kHz, and U=0.5V, number of turns is 10 circles.It is multiple
The power consumption of powder core is closed using the rugged SY-8232 B-H analyzer test of rock, test condition are as follows: 500kHz 10mT, 1MHz 10mT,
3MHz 10mT, test temperature are 25 DEG C.The saturation magnetization of composite magnetic powder core uses vibrating specimen magnetometer VSM
(Vibrating Sample Magnetometer) test.
Compared with prior art, the invention has the benefit that
1, the present invention uses NiZn ferrite for raw material, grinds Ni nanoparticle Zn ferrite obtained as covering through crushing ball
FeSiCr magnetic powder is coated, compared to micron NiZn ferrite, Ni nanoparticle Zn ferrite specific surface area is bigger, can effectively coat
FeSiCr magnetic powder surface avoids the direct contact between FeSiCr magnetic powder particle.Meanwhile selected NiZn ferrite is iron deficiency
Formula, conductive mechanism are p-type, and the ferritic resistivity of NiZn may be up to 106Ω·m。
2, Fig. 1 and Fig. 2 gives the EDS map of the composite magnetic powder core different location of Ni nanoparticle Zn ferrite cladding, can be with
Find out that Ni nanoparticle Zn ferrite forms one layer of uniform and thin clad between magnetic powder particle.It, will according to brick-wall model theory
FeSiCr magnetic powder and NiZn ferrite clad are seen as series equivalent circuit, and the NiZn ferrite as clad has very high
Resistivity effectively hinders the electron transfer campaign between FeSiCr magnetic powder particle, to considerably increase composite magnetic powder core
Resistivity reduces eddy-current loss of the composite magnetic powder core in high frequency；Simultaneously according to dynamic magnetization theory, in the effect of external magnetic field
Under, composite magnetic powder core be magnetized rotate in magnetic domain in magnetized state, composite magnetic powder core, position occurs for domain wall between magnetic domain
It moves.It is excellent that NiZn ferrite as soft magnetic materials has that initial permeability is high, saturation induction density is high and eddy-current loss is low etc.
FeSiCr magnetic powder particle can be effectively reduced using the composite magnetic powder core after NiZn ferrite cladding during dynamic magnetization in point
Between demagnetizing field, reduce magnetization resistance, to make composite magnetic powder core Effective permeability with higher and saturation magnetization；?
In alternating magnetic field, composite magnetic powder core can also generate energy loss, and magnetic loss is by eddy-current loss, magnetic hystersis loss and residual loss three
It is grouped as.There is high resistivity and Effective permeability using the composite magnetic powder core after NiZn ferrite cladding, it is possible to have
Effect reduces the eddy-current loss and magnetic hystersis loss of composite magnetic powder core.
Detailed description of the invention
Fig. 1 is the EDS map of FeSiCr magnetic powder particle in the composite magnetic powder core that embodiment 3 obtains；
Fig. 2 is EDS map between FeSiCr magnetic powder particle in the composite magnetic powder core that embodiment 3 obtains；
Fig. 3 is the SEM spectrum for the composite magnetic powder core that embodiment 3 obtains.
Specific embodiment
With reference to the accompanying drawings and examples, technical solution of the present invention is described in detail.
Embodiment
A kind of preparation method of composite magnetic powder core, specifically includes the following steps:
The cleaning of step 1, FeSiCr magnetic powder:
Deionized water, acetone is respectively adopted, and to FeSiCr magnetic powder, (group is divided into Fe85Si6.8Cr8.2) cleaned, to remove magnetic
The impurity and greasy dirt on powder surface；
The preparation of step 2, Ni nanoparticle Zn ferrite covering:
Use traditional solid sintering technology preparation structure formula for NixZn1-xFe2O4NiZn ferrite, 0.2≤x≤0.4,
It crushes, ball milling, obtains the powder that partial size is 100nm~200nm, as ferrite covering；
Step 3, insulating wrapped:
Magnetic powder after taking 100g step 1 to clean, infiltrates magnetic powder using 15g acetone；Then, it is added thereto and accounts for magnetic
The W- of the Ni nanoparticle Zn ferrite covering that the step 2 of 3wt%~5wt% of silty amount obtains and the 2wt% for accounting for magnetic powder quality
6C binder, is stirred continuously, and 40 meshes are crossed in drying；
The component of Examples 1 to 3 and comparative example 1,2 is as follows:
Step 4, compression moulding:
Powder after step 3 sieving is used into hydraulic press compression moulding under the pressure of 20GPa, pressing time 10s is obtained
To the Both ring sam having a size of Ф 12.0mm × Ф 8.0mm × h 3.0mm (h is thickness of sample)；
Step 5, annealing:
The Both ring sam that step 4 is obtained is placed in tube furnace, and at a temperature of 700 DEG C, under air atmosphere, anneal 1h, complete
Cheng Hou takes out to in-furnace temperature cooled to room temperature, the composite magnetic powder core can be obtained；
Step 6, test:
The composite magnetic powder core that step 5 is obtained carries out electromagnetic performance test: where Effective permeabilityIn formula, L is the inductance of powder core, LeFor the effective magnetic circuit length of powder core, when N is test on magnet ring
Coil turn, AeFor the effective sectional area of powder core；Test condition is f=1kHz, and U=0.5V, number of turns is 10 circles.It is multiple
The power consumption of powder core is closed using the rugged SY-8232B-H analyzer test of rock, test condition are as follows: 500kHz 10mT, 1MHz 10mT,
3MHz 10mT, test temperature are 25 DEG C.The saturation magnetization of composite magnetic powder core uses vibrating specimen magnetometer VSM
(Vibrating Sample Magnetometer) test.
Examples 1 to 3 and comparative example 1,2 test result is as follows table:
Fig. 1 is the EDS map inside the composite magnetic powder core throwing face FeSiCr magnetic powder particle that embodiment 3 obtains；It can by Fig. 1
Know only have tri- kinds of elements of Fe, Si, Cr to occur inside FeSiCr magnetic powder particle, show that NiZn ferrite does not enter into
Inside FeSiCr magnetic powder particle.
Fig. 2 is the EDS map between the composite magnetic powder core throwing face FeSiCr magnetic powder particle that embodiment 3 obtains；As shown in Figure 2,
There is the appearance of Ni and Zn element in FeSiCr magnetic powder particle gap, shows that the NiZn ferrite as covering is uniformly coated on
FeSiCr magnetic powder particle surface.
Fig. 3 is the SEM spectrum for the composite magnetic powder core that embodiment 3 obtains；From the figure 3, it may be seen that the composite magnetic powder core after annealing is tight
It is real fine and close, and FeSiCr magnetic powder particle surface has coated one layer of uniform and thin ferrite particle, shows the method for the present invention energy
It is uniformly coated on covering in magnetic powder particle.
Claims (2)
1. a kind of composite magnetic powder core, which is characterized in that including FeSiCr magnetic powder and Ni nanoparticle Zn ferrite covering, wherein institute
Stating FeSiCr powder structure formula is Fe80~90Si0.1~10Cr5~10, partial size is 5 μm~20 μm；The NiZn ferrite structure formula is
NixZn1-xFe2O4, partial size is 100nm~1 μm, 0.2≤x≤0.4；The NiZn ferrite covering is FeSiCr magnetic powder quality
3wt%~5wt%.
2. a kind of preparation method of composite magnetic powder core, specifically includes the following steps:
The cleaning of step 1, FeSiCr magnetic powder:
Deionized water is respectively adopted, acetone cleans FeSiCr magnetic powder, to remove the impurity and greasy dirt on magnetic powder surface；
The preparation of step 2, Ni nanoparticle Zn ferrite covering:
Use solid sintering technology preparation structure formula for NixZn1-xFe2O4NiZn ferrite, 0.2≤x≤0.4, crush, ball milling,
Obtain the powder that partial size is 100nm~200nm, as ferrite covering；
Step 3, insulating wrapped:
The magnetic powder after step 1 cleaning is infiltrated using acetone, wherein acetone accounts for 10wt%~15wt% of magnetic powder quality；
Then, the Ni nanoparticle Zn ferrite cladding that the step 2 for the 3wt%~5wt% for accounting for FeSiCr magnetic powder quality obtains is added thereto
Agent, account for FeSiCr magnetic powder quality 1wt%~3wt% binder, be stirred continuously, dry, sieving；
Step 4, compression moulding:
Powder after step 3 sieving is used into hydraulic press compression moulding under the pressure of 1GPa~20GPa, obtains sample；
Step 5, annealing:
The sample that step 4 is obtained is placed in tube furnace, and under 600 DEG C~1000 DEG C temperature, air atmospheres, anneal 0.5~2h,
After the completion, it to in-furnace temperature cooled to room temperature, takes out, the composite magnetic powder core can be obtained.
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Cited By (4)
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| CN111986866A (en) * | 2020-08-24 | 2020-11-24 | 天津大学 | High-frequency low-magnetic-loss power type soft magnetic composite material and preparation method thereof |
| WO2021103466A1 (en) * | 2019-11-28 | 2021-06-03 | 中国计量大学 | Method for preparing soft magnetic composite material with high magnetic conductivity and low loss, and magnet ring thereof |
| CN113066627A (en) * | 2021-02-26 | 2021-07-02 | 广东省科学院材料与加工研究所 | Composite magnetic powder core and preparation method thereof |
| CN113345703A (en) * | 2021-04-19 | 2021-09-03 | 马鞍山市鑫洋永磁有限责任公司 | Preparation method of composite magnetic powder |
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