CN109545494B - A kind of preparation method of iron silica magnetic particle core material - Google Patents
A kind of preparation method of iron silica magnetic particle core material Download PDFInfo
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- CN109545494B CN109545494B CN201811236795.0A CN201811236795A CN109545494B CN 109545494 B CN109545494 B CN 109545494B CN 201811236795 A CN201811236795 A CN 201811236795A CN 109545494 B CN109545494 B CN 109545494B
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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
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Abstract
The present invention relates to a kind of iron silica magnetic particle core material and preparation method thereof, which is by iron powder, a small amount of silicon powder, ultra-fine Fe3O4, Mn-Zn ferrite particle be uniformly mixed with suitable binder, annular material is prepared using novel powder metallurgy technology, after binder is removed high annealing be sintered, obtain high-densit, high performance soft magnetic materials.Based on iron powder, the nano-scale particle of addition can further promote magnetism of material under the premise of not influencing iron powder magnetic property the material.Compared with existing Related product, the present invention has many advantages, such as that processing is flexible, magnetic performance is high, product consistency is high.
Description
Technical field
The invention belongs to compound soft magnetic material technical fields, contain Fe more particularly, to one kind3O4Iron silica magnetic particle core material and
Preparation method.
Background technique
Soft-magnetic composite material (also known as powder core) is one kind using magnetic-particle as raw material, coats dielectric in particle surface
Powder is pressed by required shape, and the soft magnetic material as obtained from heat-treatment of annealing using powder metallurgical technique afterwards.Iron
Silica magnetic particle core is made of the alloy powder of 94%Fe and 6%Si.Saturation induction of the iron silica magnetic particle core with high Da 1.5T is strong
Degree, Effective permeability range 26~90, direct current biasing excellent are still up to 70% in 100Oe.
But the iron loss of iron silica magnetic particle core is higher than traditional Fe-Si-Al magnetic core (celestial Bei Hejin), this is because silicon is as one
Kind semiconductor element, resistivity are lower.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind to contain Fe3O4It is iron-based
Magnetic powder core material and preparation method.
In order to improve its resistivity, the present invention selects that magnetic property and the higher Fe of resistivity is added3O4As the make-up,
Fe3O4Price is more cheap, and cost performance is high.In order to improve its exchange stability and reduce magnetic loss, and Mn-Zn ferrite is added
Particle.
The present invention contains Fe3O4Iron-based magnetic powder core material processing performance it is good, magnetic property is high, production cost is low.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of iron silica magnetic particle core material, is composite material, including iron powder, and the surface coated silicon containing component of iron powder,
Fe3O4Particle and Mn-Zn ferrite particle, wherein
The weight percentage of iron powder is >=90wt%,
Fe3O4The weight percentage of particle is 3wt%-5wt%,
The weight percentage of Mn-Zn ferrite particle is 2wt%,
Due to ultra-fine Fe3O4Effect, silicone content is not higher than 5wt% in preferred composite material, to obtain optimal magnetism
It can matching.
The iron silica magnetic particle core material is core-shell structure, and iron powder is core, the silicon containing component, Fe3O4Particle and Mn-Zn iron
Oxysome particles coat forms shell outside iron powder.
Silicon containing component position pure silicon or siliceous iron-based component, ferrosilicon content is not less than in siliceous iron-based component
75wt%.
The iron powder is superfine spherical iron powder, and the iron powder has micro oxygen/nitride doping, wherein oxygen/nitrogen
Compound is no more than 1wt%.
The Fe3O4Particle is powder particle of the granularity less than 30 μm, the Fe3O4Particulate refractory is that ferrimagnetism is non-
Continuous nano-scale particle.
The present invention forms cladding in gained composite material, improves the magnetic property of material；Ultra-fine Fe3O4Resistivity is high, and has
Preferable magnetic property can preferably improve traditional iron silica magnetic particle core performance.
A kind of preparation method of iron silica magnetic particle core material, comprising the following steps:
(1) reduced iron powder and Nanosized Mn-Zn Ferrite Powders Prepared by Boiling particle, silicon containing component is dry-mixed uniform in vacuum glove box, it obtains
To mixed-powder, the mass ratio of reduced iron powder and Nanosized Mn-Zn Ferrite Powders Prepared by Boiling particle, silicon containing component is 19:0.4:0.6；
(2) mixed-powder obtained by step (1) and binder are kneaded on ball mill granulation, obtain soft-magnetic alloy powder,
The mass percent that binder accounts for mixed-powder obtained by step (1) is 10%；
(3) by soft-magnetic alloy powder and Fe3O4Particle be added vacuum glove box in uniform mixing, soft-magnetic alloy powder with
Fe3O4The mass ratio of particle is 10:1,
(4) after evenly mixing by soft-magnetic alloy powder obtained by step (3) and binder, in planetary ball mill prepared by ball milling
The mass ratio of soft magnetic powder, step (3) gained soft-magnetic alloy powder and binder is 22:5；
(5) magnetic powder coated is pressed into magnet ring using press；
(6) in vacuum heat treatment furnace, magnet ring is made annealing treatment, using argon gas as protective atmosphere, then with furnace
It is cooled to room temperature.
The binder is powdered, and with the sieve of 30 mesh.
The binder is zinc stearate.
In the step (1), mixing time 1h, mixing speed is 30r/min；
In the step (3), mixing time 1h, mixing speed is 30r/min；
In the step (4), in planetary ball mill, with the ratio of grinding media to material of 50:1, the revolving speed of 200rpm, argon atmosphere
Under the conditions of ball milling 2h；
In the step (5), pressing pressure 160kN, pressing time 5min；
In the step (6), powder core is made annealing treatment, using argon gas as protective atmosphere, heating rate 5K/
Min is heated to 1000 DEG C, keeps the temperature 2h, then furnace cooling to room temperature.
The present invention can uniformly coat Fe powder by mechanical ball mill technique, form the controllable core-shell structure magnetic powder of thickness.
In the present invention, different powder are subjected to Vacuum Mixture processing, guarantee to aoxidize in mixing process without Fe powder.Powder forming
It has to by compacting, degreasing sintered, the processes such as densification, heat treatment are intended to reach more preferably performance, also need certain lead
To the effect of filling process and field.Heat treatment process need to carry out under inert gas or inertia+protection of reducing atmosphere, generally
Effect is elimination stress.
With consistency, high, interior tissue is uniformly, D.C. magnetic biasing performance is good and power consumption is relatively low for prepared powder core
The characteristics of.
In preparation process of the present invention, need using reasonable lubricant assist formation, it, can be with according to the difference of process condition
Use targetedly lubricant.
It is extremely outstanding soft that feature of the present invention is that the high compactness iron silica magnetic particle core prepared using new technique is shown
Magnetic property.
Compared with prior art, the present invention has the following advantages and beneficial effects:
(1) the powder core density prepared is in 7g/cm3More than, consistency is up to 90% or more；
(2) Si, Fe being added3O4, Mn-Zn ferrite after appropriate proportioning, the soft magnet performance of Fe further improves；
(3) material price selected by inexpensively, lower production costs.
Detailed description of the invention
Fig. 1 is 1 gained magnet ring hysteresis graph of embodiment；
Fig. 2 is 1 gained magnet ring hysteresis data result of embodiment；
Fig. 3 is the xps map of 1 gained magnet ring of embodiment；
Fig. 4 is the CSONH composition analysis result one of 1 gained magnet ring of embodiment；
Fig. 5 is the CSONH composition analysis result two of 1 gained magnet ring of embodiment；
Fig. 6 is the CSONH composition analysis result three of 1 gained magnet ring of embodiment.
Specific embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
(1) raw material powder is reduced iron powder, binder zinc stearate is made it is powdered, and with the sieve of 30 mesh.
Reduced iron powder 19g and Nanosized Mn-Zn Ferrite Powders Prepared by Boiling particle 0.4g, nano silica fume 0.6g is dry-mixed uniform in vacuum glove box, it mixes
The material time is 1h, and mixing speed is 30r/min,
(2) mixed-powder obtained by step (1) and binder are kneaded on ball mill granulation, obtain soft-magnetic alloy powder,
The mass percent that binder accounts for mixed-powder obtained by step (1) is 10%, in planetary ball mill, with the ratio of grinding media to material of 50:1,
The revolving speed of 200rpm, ball milling 2h under the conditions of argon atmosphere；
(3) Fe is chosen3O4Powder, powder particle of the ball milling at granularity less than 30 μm；
(4) by soft-magnetic alloy powder obtained by step (2) and Fe3O4Uniform mixing in vacuum glove box is added, in 30r/min
1h is uniformly mixed under state；
(5) after evenly mixing by soft-magnetic alloy powder 22g obtained by step (4) and binder 5g, in planetary ball mill, with
The ratio of grinding media to material of 50:1, the revolving speed of 200rpm, ball milling 2h under the conditions of argon atmosphere prepare soft magnetic powder；
(6) magnetic powder coated is pressed into magnet ring, pressing pressure 160kN using press, the pressing time is
5min；
(7) in vacuum heat treatment furnace, powder core is made annealing treatment, using argon gas as protective atmosphere, heating speed
Rate is 5K/min, is heated to 1000 DEG C, keeps the temperature 2h, then furnace cooling to room temperature.
15 magnet rings are prepared altogether according to the above method, wherein the 5th performance is more prominent.Its performance is as follows:
Gained magnet ring density is 7.285g/cm3, when externally-applied magnetic field Hs takes 3000A/m, maximum permeability 25.92mH/
M, saturation induction density 1.949T, coercivity 22.4A/m, B-H loop are as shown in Figure 1.What Fig. 2 was shown is exactly these property
It is capable of measuring result.
Xps atlas analysis is done to it, as a result as shown in Figure 3.
CSONH constituent analysis is carried out to the sample, acquired results are as shown in Fig. 4, Fig. 5, Fig. 6.
In Fig. 4, Fig. 5, Fig. 6, sample mark indicates product prepared by the present embodiment with the 5 of sample ID.
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 (6)
1. a kind of preparation method of iron silica magnetic particle core material, which is characterized in that the iron silica magnetic particle core material is composite material, packet
Iron powder is included, and in the surface coated nano silica fume of iron powder, Fe3O4Particle and Nanosized Mn-Zn Ferrite Powders Prepared by Boiling particle,
The iron silica magnetic particle core material is prepared by the following method to obtain:
(1) reduced iron powder and Nanosized Mn-Zn Ferrite Powders Prepared by Boiling particle, nano silica fume is dry-mixed uniform in vacuum glove box, it is mixed
Close powder, reduced iron powder and Nanosized Mn-Zn Ferrite Powders Prepared by Boiling particle, nano silica fume mass ratio be 19:0.4:0.6；
(2) mixed-powder obtained by step (1) and binder are kneaded on ball mill granulation, obtain soft-magnetic alloy powder, bonded
The mass percent that agent accounts for mixed-powder obtained by step (1) is 10%；
(3) by soft-magnetic alloy powder and Fe3O4Uniform mixing, soft-magnetic alloy powder and Fe in vacuum glove box is added in particle3O4
The mass ratio of grain is 10:1；
(4) after evenly mixing by soft-magnetic alloy powder obtained by step (3) and binder, ball milling prepares soft magnetism in planetary ball mill
The mass ratio of powder, step (3) gained soft-magnetic alloy powder and binder is 22:5；
(5) soft magnetic powder obtained by step (4) is pressed into magnet ring using press；
(6) in vacuum heat treatment furnace, magnet ring is made annealing treatment, using argon gas as protective atmosphere, then furnace cooling
To room temperature.
2. a kind of preparation method of iron silica magnetic particle core material according to claim 1, which is characterized in that the iron silica magnetic particle core
Material is core-shell structure, and iron powder is core, the nano silica fume, Fe3O4Particle and Nanosized Mn-Zn Ferrite Powders Prepared by Boiling particles coat are in iron powder
Outside forms shell.
3. a kind of preparation method of iron silica magnetic particle core material according to claim 1, which is characterized in that the iron powder is ultra-fine
Spherical iron powder, and the iron powder has micro oxygen/nitride doping, and wherein oxygen/nitride is no more than 1wt%.
4. a kind of preparation method of iron silica magnetic particle core material according to claim 1, which is characterized in that the binder is powder
Last shape, and with the sieve of 30 mesh.
5. a kind of preparation method of iron silica magnetic particle core material according to claim 1, which is characterized in that the binder is hard
Resin acid zinc.
6. a kind of preparation method of iron silica magnetic particle core material according to claim 1, which is characterized in that in the step (1),
Mixing time is 1h, and mixing speed is 30r/min；
In the step (3), mixing time 1h, mixing speed is 30r/min；
In the step (4), in planetary ball mill, with the ratio of grinding media to material of 50:1, the revolving speed of 200rpm, argon atmosphere condition
Lower ball milling 2h；
In the step (5), pressing pressure 160kN, pressing time 5min；
In the step (6), powder core is made annealing treatment, using argon gas as protective atmosphere, heating rate is 5 K/
Min is heated to 1000 DEG C, keeps the temperature 2h, then furnace cooling to room temperature.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811236795.0A CN109545494B (en) | 2018-10-23 | 2018-10-23 | A kind of preparation method of iron silica magnetic particle core material |
| PCT/CN2019/112528 WO2020083281A1 (en) | 2018-10-23 | 2019-10-22 | Iron-silicon magnetic powder core material and preparation method therefor |
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| CN201811236795.0A CN109545494B (en) | 2018-10-23 | 2018-10-23 | A kind of preparation method of iron silica magnetic particle core material |
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| CN109545494B (en) * | 2018-10-23 | 2019-11-05 | 同济大学 | A kind of preparation method of iron silica magnetic particle core material |
| CN110098024A (en) * | 2019-05-13 | 2019-08-06 | 海安县巨力磁材有限责任公司 | A kind of anticorrosion magnetic material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1979698A (en) * | 2006-11-06 | 2007-06-13 | 南昌大学 | Method for making novel ferrite/iron-base composite material soft magnetic-powder core |
| JP2009185312A (en) * | 2008-02-04 | 2009-08-20 | Denso Corp | Composite soft magnetic material, dust core using the same, and their production method |
| CN101694800A (en) * | 2009-09-08 | 2010-04-14 | 清华大学 | Compound soft magnetic material with operational performances of high-frequency and large power and process for preparing same |
| CN104028762A (en) * | 2014-05-28 | 2014-09-10 | 浙江大学 | Preparation method of soft magnetic composite material |
| CN106409462A (en) * | 2016-09-07 | 2017-02-15 | 同济大学 | High-silicon-steel ferrite soft magnetic composite magnetic powder core and preparation method thereof |
| CN108057878A (en) * | 2017-12-19 | 2018-05-22 | 浙江大学 | A kind of preparation method of bivalve layer soft-magnetic composite material |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104550940B (en) * | 2013-10-29 | 2016-09-21 | 东睦新材料集团股份有限公司 | The method of a kind of soft magnetic ferrite cladding metallic magnetic powder and soft-magnetic composite material preparation method thereof |
| CN108335820B (en) * | 2018-02-23 | 2019-06-11 | 同济大学 | Stablize the magnetic powder core material and preparation method thereof of magnetic conductivity and low loss |
| CN109545494B (en) * | 2018-10-23 | 2019-11-05 | 同济大学 | A kind of preparation method of iron silica magnetic particle core material |
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2018
- 2018-10-23 CN CN201811236795.0A patent/CN109545494B/en active Active
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- 2019-10-22 WO PCT/CN2019/112528 patent/WO2020083281A1/en active Application Filing
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1979698A (en) * | 2006-11-06 | 2007-06-13 | 南昌大学 | Method for making novel ferrite/iron-base composite material soft magnetic-powder core |
| JP2009185312A (en) * | 2008-02-04 | 2009-08-20 | Denso Corp | Composite soft magnetic material, dust core using the same, and their production method |
| CN101694800A (en) * | 2009-09-08 | 2010-04-14 | 清华大学 | Compound soft magnetic material with operational performances of high-frequency and large power and process for preparing same |
| CN104028762A (en) * | 2014-05-28 | 2014-09-10 | 浙江大学 | Preparation method of soft magnetic composite material |
| CN106409462A (en) * | 2016-09-07 | 2017-02-15 | 同济大学 | High-silicon-steel ferrite soft magnetic composite magnetic powder core and preparation method thereof |
| CN108057878A (en) * | 2017-12-19 | 2018-05-22 | 浙江大学 | A kind of preparation method of bivalve layer soft-magnetic composite material |
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| CN109545494A (en) | 2019-03-29 |
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