CN104550940B - The method of a kind of soft magnetic ferrite cladding metallic magnetic powder and soft-magnetic composite material preparation method thereof - Google Patents
The method of a kind of soft magnetic ferrite cladding metallic magnetic powder and soft-magnetic composite material preparation method thereof Download PDFInfo
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Abstract
A kind of soft magnetic ferrite cladding metallic magnetic powder method, the method is to be mixed with a small amount of micron or submicron soft magnetic ferrite by metallic magnetic powder, with after form clad through microwave high-temperature heat treatment.The invention also discloses the method using above-mentioned cladding powder to prepare soft magnetic metal composite, cladding powder is carried out Coated with Organic Matter, add lubricant, compressing, finally make annealing treatment and i.e. obtain soft-magnetic composite material.The present invention takes full advantage of soft magnetic ferrites and has the feature of magnetic, high resistivity and heat-resisting quantity, it is the compound of two kinds of soft magnetic materials, namagnetic substance is few compared with other kinds of soft-magnetic composite material, and has higher heat treatment temperature, thus has preferable comprehensive magnetic energy.Using the soft-magnetic composite material prepared by the present invention to have high pcrmeability and low loss concurrently, frequency stability is good, and magnetic loss is little in high frequency, and preparation technology operation simple and environmentally-friendly, easy, low cost, is suitable for industrial mass, large-scale production.
Description
Technical field
The invention belongs to powder metallurgy and technical field of magnetic materials, particularly to a kind of micron or submicron soft magnetic ferrite
The method of cladding metallic magnetic powder, and use this cladding powder to the method preparing soft-magnetic composite material.
Background technology
Soft magnetic materials is a kind of important electronic material, at aspects such as power industry, telecommunications engineering and high frequency radio technology
All there is important application.Metal soft magnetic material has the advantages that magnetic induction is high, but its resistivity is low, and medium-high frequency is lost
Excessive.Ferrite soft magnetic belongs to nonmetal ferrimagnetism soft magnetic materials, and resistivity is high (as NiZn ferrite resistivity is
107～1010Ω m), saturation magnetization is lower than metal, and cheap.Along with electrical equipment miniaturization, high energy
Change, multifunction, in order to prepare the powder core material that efficiency is higher, volume is less, weight is lighter, develop novel
Soft-magnetic composite material becomes focus, and an urgent demand provides a kind of high-effect soft-magnetic composite material with very high resistivity.
Soft-magnetic composite material in early days is to use metallic magnetic powder and Organic substance mixing to be coated with.Such as United States Patent (USP) US
Patent 874908 just reports employing ferrum-resin compounded and makes soft magnetic materials.In recent years, with ultra-fine even nano metal
Oxide is (such as Al2O3、TiO2、SiO2、MgO2Deng) obtain commonly used as inorganic matter clad.European patent
EP434669 is reported in the powder of 10-300 μm the cladding one layer alkali metal oxide less than 10 μm.Middle promulgated by the State Council
Bright patent 200610040493.7 reports a kind of employing Nano-meter SiO_22The preparation method of coating carbonyl iron powder.
But, use metal-oxide as insulating coating, although to improve the performance of material.But the oxidation used
Thing or Organic substance are namagnetic substance, and insulating barrier increases the air gap of magnet, thus reduces the effective rate of utilization of magnet.
Then, someone uses the soft magnetic ferrite with high resistivity as clad, replaces namagnetic substance with magnetisable material
To reduce the loss of magnet and to improve pcrmeability.Patent US2002/0088505 applied for such as the David Earl Gay of the U.S.
A1 etc. use the MgFe that granule is tiny2O4Cladding iron powder granule, gained is removed as insulating barrier with thermoplastic polypropylene acid fat
Soft-magnetic composite material has more preferable pcrmeability and resistivity.Patent 201010297482.3 report uses control oxidizing process to exist
One layer of Fe of Fe powder Surface Creation3O4Shell is to improve resistivity.Document (Yang Hongchuan, Yu Dunbo, Li Shipeng, Hu Quanxia,
The sintering process of the complex sintered soft magnetic materials of Yan Wenlong, Li Kuo society .MnZn-FeNi and performance study. rare metal,
2011,35(1): 28-34) use with equigranular with patent 200710063843.6, patent 201110046386.6
Fe-Ni system alloy and soft magnetic ferrite particles carry out being mixed and made into sintering soft-magnetic composite material.And patent
200610124964.2 is to use to be combined with equigranular soft magnetic ferrite and iron-based soft magnetic to make the soft magnetism of cladding and be combined
Material.But this biggest with ferrite consumption in equigranular two kinds of powder, it is unfavorable for that magnet obtains high magnetic conductance
Rate.
To this end, progressively replace original coarse grain powder to be coated with iron-based powder with nanoscale ferrite powder become research
New direction.Document (Shen Wu, Aizhi Sun, Wenhuan Xu, Qian Zhang, Fuqiang Zhai, Philip Logan, Alex
A.Volinsky.Journal of Magnetism and Magnetic Materials, 2012,324 (22): 3899-3905) and patent
CN103151134.A uses sol-gel process at one layer of nano-crystalline MnZn ferrite of Fe powder Surface coating, this Magnetic Materials
The clad of matter can obtain more higher pcrmeability than namagnetic substance clad.Document (Zhiyong Zhong, QiWang,
Longxu Tao,Lichuan Jin,Xiaoli Tang,Feiming Bai,and Huaiwu Zhang.Permeability Dispersion and
Magnetic Loss of Fe/NixZn1-xFe2O4 Soft Magnetic Composites.IEEE Transactions on Magnetics,
2012,48 (11): 3622-3625) chemical coprecipitation method is used to be made for Fe/ (NiZn) Fe equally2O4The soft magnetism of nanometer cladding is multiple
Condensation material.For obtaining high mechanical property, Chinese invention patent 201010621275.9 uses metal Fe or alloy powder
It is combined with Ni nanoparticle Zn ferrite powder, uses discharge plasma sintering (SPS) technology to carry out solidifying magnet.This
Method can improve the mechanical property of magnet, but the shortcoming of SPS technology is preparation cost height, it is difficult to batch preparation.With
One common issue of upper employing nanometer ferrite powder is, nanometer powder preparation and difficulties in dispersion, the change stayed after preparation
Learn liquid difficult treatment, and preparation cost is high, limits large batch of application.
In order to improve soft magnetic metal and the suitability of ferrite soft magnetic composite material, low cost further, the present invention uses
Micron or submicron soft magnetic ferrite are as raw material, after being mixed homogeneously with soft magnetic ferrite by metallic magnetic powder, at microwave
In Chang, powder metallurgy heat treatment is formed clad, owing to ferrite soft magnetic has higher dielectric constant, thus have
Stronger Microwave Absorption Properties, and microwave heating has a selectivity feature, thus when Fe powder is not the most heated ferrite
Just it is provided with the highest temperature, thus promotes micron or submicron soft magnetic ferrite to be bonded to shape on metallic magnetic powder surface
Become strong bonded, form clad, it is ensured that the soft-magnetic composite material made has highly stable magnetic property.Further,
Owing to the ferrite powder of micron or submicron is readily available, as being raw material by each metal-oxide formed, use micro-
Ripple synthesis (patent 201210580954.5) or the synthesis of common china-clay method, the material after synthesis is through coarse crushing, at certain ball
The ball grinder of material ratio can be milled to required micron or submicron ferrite soft magnetic powder size.Thus reduce metal
Problem with preparation difficulty, environmental protection and the cost of ferrite soft magnetic composite material so that this soft-magnetic composite material is conducive to work
Industry metaplasia is produced.
Summary of the invention
First technical problem to be solved by this invention is to provide the soft magnetic ferrite cladding gold of a kind of micron or submicron
The method belonging to Magnaglo, the method technique is simple to operation, and equipment is simple, the uniform and thin densification of clad prepared.
Second technical problem to be solved by this invention is to provide the preparation method of a kind of soft-magnetic composite material, uses above-mentioned
Micron or submicron ferrite cladding metallic magnetic powder be raw material, by the cladding of organic solution, add lubricant,
The techniques such as shaping, annealing and be prepared as.Prepared soft-magnetic composite material has good insulating, stable performance, system
The features such as standby technique is simple, are suitable for large-scale production.
The present invention solves the technical scheme that above-mentioned first technical problem used: a kind of soft magnetic ferrite cladding metallic magnetic
The method of property powder, it is characterised in that comprise the following steps:
1) batch mixing: by micron-sized for 92-99wt% metallic magnetic powder and 1-8wt% micron or the ferrite of submicron order
Soft magnetic powder mixes 30-120min in mixing machine and obtains mixed-powder, and batch mixing rotating speed is 80-150r/min；
2) heat treatment: above-mentioned mixed-powder is formed clad through microwave high-temperature heat treatment.Owing to ferrite soft magnetic has
There is higher dielectric constant, thus there is stronger Microwave Absorption Properties, and microwave heating has selectivity feature, thus
When Fe powder is not the most heated, ferrite is just provided with the highest temperature, thus promotes ultra-fine soft magnetic ferrite to be bonded to gold
Belong to and on Magnaglo surface, form strong bonded, form clad.
As preferably, the metallic magnetic powder in described step 1) be by pure Fe, Fe-Si, Fe-Si-Al, Fe-Ni,
One or more compositions in Fe-Ni-Mo or Fe-Co, the particle mean size of metallic magnetic powder is 10～150 μm.
As preferably, the ferroxcube magnetic powder in described step 1) is by Ni-Zn, Mn-Zn, Mg-Zn, Li-Zn
Or in Cu-Zn soft magnetic ferrite one or more composition, the particle mean size of described ferroxcube magnetic powder be 0.5～
2μm。
As improvement, described step 2) microwave high-temperature process of thermal treatment be: mixed-powder is placed in industrial microwave oven
Middle 700-900 DEG C of insulation 30-120min, atmosphere is argon or nitrogen.
The present invention solves the technical scheme that above-mentioned second technical problem used: the preparation side of a kind of soft-magnetic composite material
Method, it is characterised in that comprise the following steps:
1) cladding powder is obtained according to above-mentioned method；
2) Coated with Organic Matter: first add whiting end 0.3-1.2wt% coupling agent and carry out mixing cladding, then add 0.5-1.5wt% silicon
Mixed with resin is coated with, and above-mentioned percentage ratio is on the basis of cladding powder weight, then the material mixed is put into drying baker
In 145～155 DEG C be dried 1.5～2.5h, after cooling material through solve broken mistake 90～110 mesh sieve；
3) it is subsequently added that to account for the mix lubricant of compound weight 0.3-1.5% uniform；
4) by compressing for step 3) mixed material, then through 145～155 DEG C, insulation 1.5～2.5h is dried；
5) finally pressed compact is carried out heat treatment of annealing, i.e. obtain required soft-magnetic composite material.
As preferably, the lubricant of described step 3) is in KP-11, stearic acid, zinc stearate or lithium stearate
Plant or several mixing.
As improvement, the compressing technique of described step 4) is: be pressed into annular under 600-1200MPa pressure
Or U-shaped.
Improving, the annealing treating process of described step 5) is: temperature 600-900 DEG C again, is incubated 30-120min, atmosphere
For hydrogen, cracked ammonium, argon or nitrogen.
Compared with prior art, it is an advantage of the current invention that: select soft magnetic ferrite to be coated with, ferrite raw material used
Convenient sources, processes technique simple, and covered effect is good；Prepared soft-magnetic composite material, takes full advantage of ferroxcube
Magnetic material has magnetic, high resistivity and the feature of heat-resisting quantity, is the compound of two kinds of soft magnetic materials, namagnetic substance
Few compared with other kinds of soft-magnetic composite material, and there is higher heat treatment temperature, thus there is preferable comprehensive magnetic energy.
Using the soft-magnetic composite material prepared by the present invention to have high pcrmeability and low loss concurrently, frequency stability is good, at high frequency
Lower magnetic loss is little, and preparation technology is simple and environmentally-friendly, easily operate, low cost, be particularly suitable for industrial mass,
Large-scale production.
Accompanying drawing explanation
Fig. 1 is the preparation technology flow chart of the soft-magnetic composite material of the present invention；
Fig. 2 is the SEM photograph of straight iron powder；
Fig. 3 is the SEM photograph of Ni0.5Zn0.5Fe2O4 powder；
Fig. 4 is the SEM photograph of the Magnaglo after heat treatment；
Fig. 5 is the SEM photograph of soft-magnetic composite material pressed compact；
Fig. 6 is the SME photo after soft-magnetic composite material annealing.
Detailed description of the invention
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1:
The 96wt% water atomization pure Fe powder that mean diameter is 41 μm that will act as soft-magnetic composite material with 4wt% granularity is
The Ni of 1.0 μm0.5Zn0.5Fe2O4Mix homogeneously, subsequently by compound at industrial high temperature microwave oven (2.45GHz, 6kW)
In under argon atmosphere 800 DEG C be incubated 30min.By in heat treated compound add 0.3% silane coupled
Agent carries out mix homogeneously, then 1.0% silicones is added mix homogeneously.The material mixed is put in drying baker 150
DEG C dry 2h, after cooling, material is through solving broken mistake 100 mesh sieve.Gained powder adds the KP-11 lubricant of 0.6% content to be mixed
Close uniformly, with after be pressed into ф 21 × ф 12 × 5 ring through 800MPa pressure, then through 150 DEG C, insulation 120min is dried.
The sample 700 DEG C of heat treatments in the sintering furnace of cracked ammonium atmosphere that will obtain, are incubated 60min.Last at BH tester
On sample is carried out magnetism testing, gained sample performance is shown in Table 1 (Bmax=20mT).
Table 1
| Frequency/kHz | 5 | 20 | 50 | 100 |
| Pcrmeability | 69.31 | 69.64 | 69.02 | 68.84 |
| Magnetic loss (kW/m3) | 1.61 | 11.68 | 46.45 | 93.76 |
Embodiment 2:
The 98wt% water atomization pure Fe powder that mean diameter is 41 μm that will act as soft-magnetic composite material with 2wt% granularity is
The Ni of 1.2 μm0.5Zn0.5Fe2O4Mix homogeneously, subsequently by compound microwave oven in argon atmosphere at 900 DEG C
Insulation 30min.The silane coupler adding 0.4% in heat treated compound is carried out mix homogeneously, then by 1.3%
Silicones adds mix homogeneously.The material mixed is put into 150 DEG C of dry 2h in drying baker, and after cooling, material is broken through solving
Cross 100 mesh sieves.The KP-11 mix lubricant that gained powder adds 0.5% content is uniform, with after through 1000MPa pressure
It is pressed into ф 21 × ф 12 × 5 ring, then through 150 DEG C, insulation 120min is dried.By the sample that obtains in cracked ammonium atmosphere
800 DEG C of heat treatments in sintering furnace, are incubated 60min.Finally sample is carried out magnetism testing, institute on BH tester
Obtain sample performance and be shown in Table 2 (Bmax=20mT).
Table 2
| Frequency/kHz | 5 | 20 | 50 | 100 |
| Pcrmeability | 71.54 | 71.83 | 70.92 | 70.24 |
| Magnetic loss (kW/m3) | 1.75 | 13.62 | 49.69 | 94.15 |
Embodiment 3:
The pure Fe powder of the water atomization that mean diameter is 96wt%41 μm that will act as soft-magnetic composite material is 1.1 μ with granularity
The ultra-fine Mn of 4wt% of m0.5Zn0.5Fe2O4Mix homogeneously, subsequently by compound microwave oven in argon atmosphere
800 DEG C of insulation 30min.The silane coupler adding 0.3% in heat treated compound is carried out mix homogeneously, then will
1% silicones adds mix homogeneously.The material mixed is put into 150 DEG C of dry 2h in drying baker, material warp after cooling
Solve broken mistake 100 mesh sieve.The KP-11 mix lubricant that gained powder adds 0.6% content is uniform, with after through 800MPa
Pressure is pressed into ф 21 × ф 12 × 5 ring, then through 150 DEG C, insulation 120min is dried.The sample obtained is being decomposed ammonia
700 DEG C of heat treatments in the sintering furnace of atmosphere, are incubated 60min.Finally on BH tester, sample is carried out magnetism testing,
Gained sample performance is shown in Table 3 (Bmax=20mT).
Table 3
| Frequency/kHz | 5 | 20 | 50 | 100 |
| Pcrmeability | 71.46 | 71.88 | 70.64 | 70.08 |
| Magnetic loss (kW/m3) | 1.71 | 12.35 | 48.67 | 96.92 |
Embodiment 4:
The 97wt% water atomization pure Fe powder that mean diameter is 41 μm that will act as soft-magnetic composite material is 1.3 μ with granularity
The ultra-fine Mn of 3wt% of m0.5Zn0.5Fe2O4Mix homogeneously, subsequently by compound microwave oven in argon atmosphere
900 DEG C of insulation 30min.The silane coupler adding 0.4% in heat treated compound is carried out mix homogeneously, then will
1.3% silicones adds mix homogeneously.The material mixed is put into 150 DEG C of dry 2h in drying baker, material warp after cooling
Solve broken mistake 100 mesh sieve.The KP-11 mix lubricant that gained powder adds 0.5% content is uniform, with after through 1000MPa
Pressure is pressed into ф 21 × ф 12 × 5 ring, then through 150 DEG C, insulation 120min is dried.The sample obtained is being decomposed ammonia
800 DEG C of heat treatments in the sintering furnace of atmosphere, are incubated 60min.Finally on BH tester, sample is carried out magnetism testing,
Gained sample performance is shown in Table 4 (Bmax=20mT).
Table 4
| Frequency/kHz | 5 | 20 | 50 | 100 |
| Pcrmeability | 73.54 | 73.61 | 72.87 | 72.03 |
| Magnetic loss (kW/m3) | 1.82 | 14.43 | 52.68 | 104.24 |
Claims (7)
1. the preparation method of a soft-magnetic composite material, it is characterised in that comprise the following steps:
1) cladding powder is prepared according to the following steps；
(1) batch mixing: by micron-sized for 92-99wt% metallic magnetic powder and 1-8wt% micron or the soft magnet of submicron order
Ferrite powder mixes 30-120min in mixing machine and obtains mixed-powder, and batch mixing rotating speed is 80-150r/min；
(2) heat treatment: above-mentioned mixed-powder is formed clad through microwave high-temperature heat treatment；
2) Coated with Organic Matter: first add 0.3-1.2wt% coupling agent and carry out mixing cladding, then it is mixed to add 0.5-1.5wt% silicones
Closing cladding, above-mentioned percentage ratio is on the basis of cladding powder weight, is then put in drying baker by the material mixed
145～155 DEG C are dried 1.5～2.5h, and after cooling, material is through solving broken mistake 90～110 mesh sieve；
3) it is subsequently added that to account for the mix lubricant of gained powder weight 0.3-1.5% uniform；
4) by step 3) mixed material is compressing, then through 145～155 DEG C, insulation 1.5～2.5h is dried；
5) finally pressed compact is carried out heat treatment of annealing, i.e. obtain required soft-magnetic composite material.
Preparation method the most according to claim 1, it is characterised in that: described step 3) lubricant be KP-11,
One or more mixing in stearic acid, zinc stearate or lithium stearate.
Preparation method the most according to claim 1, it is characterised in that: described step 4) compressing technique
For: under 600-1200MPa pressure, it is pressed into annular or U-shaped.
Preparation method the most according to claim 1, it is characterised in that: described step 5) annealing treating process be:
Temperature 600-900 DEG C, is incubated 30-120min, and atmosphere is hydrogen, cracked ammonium, argon or nitrogen.
Preparation method the most according to claim 1, it is characterised in that: described step 1) metal magnetic in batch mixing
Powder is made up of one or more in pure Fe, Fe-Si, Fe-Si-Al, Fe-Ni, Fe-Ni-Mo or Fe-Co, gold
The particle mean size belonging to Magnaglo is 10～150 μm.
Preparation method the most according to claim 1, it is characterised in that: described step 1) soft magnet oxygen in batch mixing
Body powder is made up of one or more in Ni-Zn, Mn-Zn, Mg-Zn, Li-Zn or Cu-Zn soft magnetic ferrite,
The particle mean size of described soft magnetic ferrite powder is 0.5～2 μm.
Preparation method the most according to claim 1, it is characterised in that: described step 1) microwave in heat treatment is high
Temperature process of thermal treatment is: mixed-powder is placed in 700-900 DEG C of insulation 30-120min in industrial microwave oven, and atmosphere is argon
Gas or nitrogen.
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