CN104525942B - Preparation method, slice component of soft magnetic metal composite and preparation method thereof - Google Patents
Preparation method, slice component of soft magnetic metal composite and preparation method thereof Download PDFInfo
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- CN104525942B CN104525942B CN201410809690.5A CN201410809690A CN104525942B CN 104525942 B CN104525942 B CN 104525942B CN 201410809690 A CN201410809690 A CN 201410809690A CN 104525942 B CN104525942 B CN 104525942B
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Abstract
The invention discloses a kind of preparation method, slice component of soft magnetic metal composite and preparation method thereof, the preparation method of the soft magnetic metal composite comprises the following steps：Material by wet type mixing is carried out to metal magnetic and insulating coating material, slurry is obtained；Slurry drying and sieving, obtain the powder of prescribed particle size；The powder is processed using thermal decomposition method in air atmosphere, the golden soft-magnetic composite material is obtained；The metal magnetic is iron silicon substrate magnetic or the Ni-based magnetic of iron, and the insulating coating material is MnO2、Mn(NO3)2Or MnCO3.It is well mixed by additive and metallicl magnetic material, then nanoscale clad is formed in metallicl magnetic material particle surface by being heat-treated generation chemical reaction, thus obtains that there is the soft magnetic metal composite of the pressure-resistant, high thermal stability of insulation high and preferable magnetic property.
Description
Technical field
The present invention relates to the preparing technical field of magnetic material, more particularly to a kind of preparation of soft magnetic metal composite
Method, and utilize the slice component of the material and preparation method thereof.
Background technology
High current has become one of industry development trend in electronic component industry, mainly uses iron in early time
Ferrite makes power inductor, but with the progress of material technology, appearance is started in the last few years and utilizes soft magnetic metal
Material make lamination or winding-type power inductor, research and develop high current large scale product process in, for product design into
This consideration, would have in face of two technical problems, and one is the soft magnetic metal that exploitation is suitable to vacuum or protective atmosphere sintering
Problem of materials, another is the sintering process problem of copper electrode.
Soft magnetic metal composite is a kind of soft magnetic materials mixed by ferromagnetic particle and dielectric.The magnetic
Material is the main raw material(s) of the products such as passive electronic component inductance and magnetic bead (including lamination or wire winding), in the type
Often relate to magnetic material and electrode material (silver or copper electrode material) burn problem altogether in electronic component, then will be right
Metallicl magnetic material proposes various requirement, for example, it is necessary to have after sintering under the vacuum or protective atmosphere environment high magnetic permeability,
Insulation high, high withstand voltage, high thermal stability etc., in order to reach above metallicl magnetic material technical requirements, it is necessary in ferromagnetic particle
The high megohmite insulant of the layer resistivity of Surface coating one.By the uniform insulating coating material of this layer, metallicl magnetic material is improved
High thermal stability, improve its resistance to pressure request of insulation under vacuum or protective atmosphere sintering condition.
And insulating wrapped is a most important link in soft-magnetic composite material preparation process, the direct shadow of quality of clad
Ring the magnetic property to soft-magnetic composite material.In general, insulating wrapped can be divided into two kinds of organic coating and inorganic coating, organic
It is resin-coated including thermosetting resin (epoxy resin, phenolic resin and silicones etc.) and thermoplastic resin (ethyl vinyl acetate second
Alkene polymer, polypropylene, PBT, PPS, nylon etc.), inorganic coating can be divided into inorganic phosphate cladding (zinc phosphoric acid, iron phosphoric acid
Salt and manganese phosphoric acid), metal oxide cladding (SiO2, MgO) and ferrite coating etc..Organic insulation agent has well to magnetic
Bond effect, therefore industrially apply more, but organic coating agent insulation effect is not good, while being unable to high-temperature heat treatment.Nothing
Phosphate coating heat treatment temperature in machine cladding is tended not to more than 600 degree, otherwise, can be there is insulating barrier and be decomposed asking for actual effect
Topic；Although ferrite coating can be heat-treated in high temperature, there is alloy under vacuum or protective atmosphere sintering condition
Insulated with material is pressure-resistant to can not meet the problems such as requiring.
Chinese patent 201310613702.2 discloses a kind of preparation method of iron silicon soft-magnetic composite material, and the technique is used
Add organic siliconresin to be bonded after phosphorus acid passivation, organic coating agent works well, but insulation resistance can and it is heat-resisting steady
The performances such as qualitative aspect do not reach the requirement of material.
Additionally, Chinese patent 201410246088.5 discloses a kind of preparation method of soft magnetic metal composite, select
The method that diethyl magnesium alkoxide passes through sol-gel, with aqua ammonia as hydrolyst formed gel, then by metal magnetic with
The gel mixes, the magnetic for being coated.Because metal magnetic mixes the method by stirring with gel, the dispersion of this method compared with
Difference, and nano particle is poor to the adhesion of magnetic, it is difficult to realize uniform cladding.And, the method prepares metallic composite
Also there is a problem of that mass is relatively difficult to achieve.
The disclosure of background above technology contents is only used for auxiliary and understands inventive concept of the invention and technical scheme, and it is not
Necessarily belong in the prior art of present patent application, the applying date of the above in present patent application is being shown without tangible proof
In the case of disclosed, above-mentioned background technology should not be taken to evaluate the novelty and creativeness of the application.
The content of the invention
It is above-mentioned existing to solve it is a primary object of the present invention to propose a kind of preparation method of soft magnetic metal composite
The performances such as the insulation resistance energy and heat-resistant stability of technology presence do not reach the technical problems such as requirement.
Therefore, the present invention proposes a kind of preparation method of soft magnetic metal composite, comprise the following steps：
Material by wet type mixing is carried out to metal magnetic and insulating coating material, slurry is obtained；Slurry drying and sieving, are made a reservation for
The powder of granularity；The powder is processed using thermal decomposition method in air atmosphere, the golden soft-magnetic composite material is obtained；The gold
Category magnetic is iron silicon substrate magnetic or the Ni-based magnetic of iron, and the insulating coating material is that the insulating coating material is MnO2、Mn
(NO3)2Or MnCO3。
Preferably, the present invention can also have following technical characteristic：
The amount of the insulating coating material is the 1wt%~6wt% of the metal magnetic.
The sieving is using screen clothes more than 30 mesh.
The thermal decomposition method treatment is carried out between 500~800 DEG C.
The material by wet type mixing is metal magnetic according to weight ratio:Zirconia ball:Absolute ethyl alcohol=(8~12):(4~6):1
Ratio carry out.
The present invention also proposes a kind of slice component, including magnetosphere and the interior electrode using Cu conductor integral sinterings
Layer, the soft magnetic metal composite that the magnetosphere is prepared by the preparation method of foregoing any described soft magnetic metal composite
Formed.
Preferably, the inner electrode layer is into coil structure.
The present invention is it is further proposed that a kind of preparation method of slice component, the slice component is as it was noted above, described
Preparation method comprises the following steps：Slurry is prepared and green compact sheetmolding, and the slurry is prepared using any described metal above
Soft magnetic metal composite prepared by the preparation method of soft-magnetic composite material is mixed with the common ball milling of organic solvent of adhesive is added
The method of material；Interior electrode fabrication, printing forms Cu inner wire figures in the green sheet；Lamination is suppressed, first by two or more
The green sheet stacking obtains stacked body, and the Cu inner wires figure of each adjacent green sheet is connected with each other shape in the stacked body
Into coil structure；Then the green sheet for being obtained with the green compact sheetmolding clamps the stacked body and integrally suppresses；Sintering, will be whole
Body compacting gained laminated body is sintered under being placed in more than 900 DEG C of vacuum or protective atmosphere；Grinding, is ground to gained sintered body
To expose the interior electrode；External electrode is manufactured, and is coated in the sintered body end face for exposing the interior electrode and is sintered Cu external electrodes.
Preferably, described adhesive is PVB adhesives, and the green compact sheetmolding uses doctor blade method.
The beneficial effect that the present invention is compared with the prior art includes：It is well mixed by additive and metallicl magnetic material,
Then nanoscale clad is formed in metallicl magnetic material particle surface by being heat-treated generation chemical reaction, is thus had
The soft magnetic metal composite of the height pressure-resistant, high thermal stability of insulation and preferable magnetic property.
Brief description of the drawings
Fig. 1 is the process chart of the specific embodiment of the invention one；
Fig. 2 is the slice component inner electrode layer structural representation of the specific embodiment of the invention two；
Fig. 3 is the structural representation of the slice component of the specific embodiment of the invention two (for convenience of understanding, using perspective
Method)；
Fig. 4 is the process chart of the specific embodiment of the invention three.
Specific embodiment
For ease of accurate understanding, the following is the accurate definition of the technical term that hereinafter will appear from：
" slice component " is also commonly referred to as " chip components and parts ", refers to the new mini component without lead or short leg
With reference to specific embodiment and compare accompanying drawing the present invention is described in further detail.It is emphasized that
What the description below was merely exemplary, rather than in order to limit the scope of the present invention and its application.
With reference to figure 1 below -4, the embodiment of non-limiting and nonexcludability, wherein identical reference table will be described
Show identical part, unless stated otherwise.
Embodiment one：
A kind of preparation method of soft magnetic metal composite, comprises the following steps：
Material by wet type mixing is carried out to metal magnetic and insulating coating material, slurry is obtained；Slurry drying and sieving, are made a reservation for
The powder of granularity；The powder is processed using thermal decomposition method in air atmosphere, the golden soft-magnetic composite material is obtained；The gold
Category magnetic is iron silicon substrate magnetic or the Ni-based magnetic of iron, and the insulating coating material is MnO2、Mn(NO3)2Or MnCO3。
Wherein, the amount of the insulating coating material is the 1wt%~6wt% of the metal magnetic.The sieving uses 30
Screen cloth more than mesh.The thermal decomposition method treatment is carried out between 500~800 DEG C.The material by wet type mixing is gold according to weight ratio
Category magnetic:Zirconia ball:Absolute ethyl alcohol=(8~12):(4~6):1 ratio is carried out.
It is well mixed by additive and metallicl magnetic material, then by being heat-treated generation chemical reaction in metal magnetic
Material granule surface forms nanoscale clad, thus obtains having insulation pressure-resistant, high thermal stability and preferable magnetic high
The soft magnetic metal composite of energy.
The following is to the present embodiment further citing description in detail, to be better understood from technical side of the invention
Case.
Example 1：
First, metal magnetic sieving:
Sieving treatment is carried out to metal magnetic with the screen cloth of 500 mesh, metal magnetic iron described in this example is silicochromium magnetic.
2nd, material by wet type mixing is carried out to metal magnetic and insulating coating material:
According to metal magnetic:Zirconia ball:Absolute ethyl alcohol=10:5:1 ratio is put into chamfering tank after weighing, Ran Houzai
Add the insulating coating material MnO of metal magnetic 4wt%2, batch mixing 18h on chamfering frame is put into after above chamfering tank is sealed, obtain
To slurry.
3rd, slurry drying:
Good slurry mixed above is poured into glass beaker, glass beaker is then placed in 45 degree of bands at angle of an inclination
Having in the whirligig of heater carries out Rotary drying, and the rotating speed of whirligig can be 100 revs/min, wherein heater
Temperature control in the range of 50-60 degree.
4th, powder sieving：
Dried metal magnetic crosses 30 eye mesh screens by more than, obtains the powder of prescribed particle size.
5th, the powder is processed using thermal decomposition method in air atmosphere：
Using air atmosphere, soft magnetic metal composite is placed in 30min is incubated in 700 DEG C of environment, finished product, i.e. gold
Category soft-magnetic composite material.
It is prepared by sintered body magnet ring:
Soft magnetic metal composite derived above is added the PVB adhesives of the 2wt% of powder, using dry-pressing formed work
Skill is made external diameter 8mm under the pressure of 1800MPa, interior through 5mm, the magnet ring of thickness 2.3mm or so, then under vacuum conditions,
Magnet ring is made the sintered body magnet ring of above example as insulation 2h in 900 degree of environment.
Example 2：
Difference with previous example 1 is that metal magnetic is iron nickel base alloy material in the step one, in the step 2
The metal magnetic of addition is the MnCO of 6wt%3, soft magnetic metal composite is placed in 550 DEG C of environment and is incubated in the step 5
120 minutes or so.
Equally, soft magnetic metal composite derived above is added the PVB adhesives of the 2wt% of powder, using dry-pressing
Moulding process is made external diameter 8mm under the pressure of 1800MPa, interior through 5mm, the magnet ring of thickness 2.3mm or so, then in vacuum ring
Under border, magnet ring is made the sintered body magnet ring of above example as insulation 2h in 900 degree of environment.
The test of the following performance is carried out to sintered body magnet ring sample prepared by above example 1 and example 2：
(1) initial permeability of the sintered body magnet ring under 1MHz
After the circle insulated copper wire of annular magnetic ring surface uniform winding 20, with Agilent equipment E4991+16192 test fixtures
Inductance value of the test magnet ring under 1MHz, material initial permeability is drawn by formula scales.
(2) magnet ring sample insulaion resistance
Using insulaion resistance on Agilent equipment meggers 4339B test sintered body magnet ring thickness directions, test condition is
100V/0.5mA。
(3) magnet ring sample is pressure-resistant
Using voltage endurance capability on same favour Hi-pot Tester TH-333 test sintered body magnet ring thickness directions, test condition is set
It is leakage current 0.5mA.
The data of test are as shown in table 1：
Table 1
| Sintered body magnet ring sample | μ/1MHz | Insulation/M Ω | Pressure-resistant/V |
| Example 1 | 40 | 2100 | 1100 |
| Example 2 | 67 | 1800 | 1200 |
Experimental result as shown in Table 1 is visible, and using the method for coating of the present embodiment, alloy material can be up to 900
Sintered more than degree, in vacuum or protective atmosphere, and the pressure-resistant performance of soft magnetic metal compound material insulation formed after sintering is high,
Clad uniformly (is mainly embodied, the pressure-resistant meeting of product is poor if uneven indirectly by pressure-resistant performance.), while being adapted to batch
Metaplasia is produced.Because of Mn2O3Insulating barrier has high resistivity, therefore coats Mn in alloy material surface2O3Insulating barrier can be carried significantly
The resistivity of high metal soft-magnetic composite material, and with magnetic conductivity higher.
Embodiment two：
A kind of slice component, including magnetosphere and the inner electrode layer using Cu conductor integral sinterings, the magnetic
Layer is formed by soft magnetic metal composite prepared by the preparation method of foregoing any described soft magnetic metal composite.It is preferred that
, the inner electrode layer is into coil structure.
The slice component to the embodiment by taking lamination sheet type power inductor as an example is described in further detail below.
As shown in Figures 2 and 3, it is the inner electrode layer and overall structure diagram of lamination sheet type power inductor, its
Including magnet 1 and coiled type electrode 3, the coiled type electrode 3 is printed on the Cu inner wire figures in green sheet by two or more
It is electrically connected by through hole 2 and is formed, the outer electrode 4 being electrically connected with interior electrode 3 is formed on the surface of magnet 1.
Embodiment three：
A kind of preparation method of slice component, the slice component are as it was noted above, as shown in figure 4, the preparation method
Comprise the following steps：Slurry is prepared and green compact sheetmolding, and the slurry is prepared and is combined using any described soft magnetic metal above
Soft magnetic metal composite and the method for the common ball mill mixing of organic solvent of addition adhesive prepared by the preparation method of material.
Interior electrode fabrication, i.e., printing forms Cu inner wire figures in the green sheet.
Lamination is suppressed, and the green sheet stacking after first two or more is printed obtains stacked body, each phase in the stacked body
The Cu inner wire figures of the adjacent green sheet are interconnected to form coil structure.Then obtained with the green compact sheetmolding
Green sheet clamps the stacked body and integrally suppresses, as laminated body.
Sintering, will integrally suppress under gained laminated body is placed in more than 900 DEG C of vacuum or protective atmosphere and sinter.During sintering
Between 2 hours or so, obtain the sintered body of built-in Cu coiled types electrode.
Grinding, i.e., be ground to expose the interior electrode to gained sintered body.
External electrode is manufactured, i.e., coated in the sintered body end face for exposing the interior electrode and sinter Cu external electrodes.
It is warm more than 900 DEG C in vacuum or protective atmosphere environment through the lamination sheet type power inductor obtained by above step
After degree sintering, that is, obtain low cost, the lamination sheet type power inductor of high current.Wherein, described adhesive is preferably glued using PVB
Mixture etc., the green compact sheetmolding can be using doctor blade method etc..
It would be recognized by those skilled in the art that it is possible that numerous accommodations are made to above description, so embodiment is only
For describing one or more particular implementations.
Although have been described above and describe being counted as example embodiment of the invention, it will be apparent to those skilled in the art that
It can be variously modified and replaced, without departing from spirit of the invention.Furthermore it is possible to make many modifications with by spy
Condition of pledging love is fitted to religious doctrine of the invention, without departing from invention described herein central concept.So, the present invention is unrestricted
May also include belonging to all embodiments of the scope of the invention and its be equal in specific embodiment disclosed here, but the present invention
Thing.
Claims (6)
1. a kind of preparation method of soft magnetic metal composite, it is characterised in that comprise the following steps：
Material by wet type mixing is carried out to metal magnetic and insulating coating material, slurry is obtained；
Slurry drying and sieving, obtain the powder of prescribed particle size；
The powder is processed using thermal decomposition method in air atmosphere, the thermal decomposition method treatment is entered between 500~800 DEG C
OK, nanoscale clad is formed on the metal magnetic surface by being heat-treated generation chemical reaction, obtains the soft magnetic metal
Composite；
The metal magnetic is iron silicon substrate magnetic or the Ni-based magnetic of iron, and the insulating coating material is MnO2、Mn(NO3)2Or
MnCO3；
The amount of the insulating coating material is the 1wt%~6wt% of the metal magnetic；
The material by wet type mixing is metal magnetic according to weight ratio:Zirconia ball:Absolute ethyl alcohol=(8~12):(4~6):1 ratio
Example is carried out.
2. the preparation method of soft magnetic metal composite as claimed in claim 1, it is characterised in that：The sieving uses 30 mesh
Screen cloth above.
3. a kind of slice component, it is characterised in that：Including magnetosphere and the inner electrode layer using Cu conductor integral sinterings,
Soft magnetic metal prepared by the preparation method of soft magnetic metal composite of the magnetosphere as described in claim any one of 1-2 is answered
Condensation material is formed.
4. slice component as claimed in claim 3, it is characterised in that：The inner electrode layer is into coil structure.
5. a kind of preparation method of slice component, it is characterised in that：The slice component as described in claim 3 or 4, the system
Comprise the following steps as method：
Slurry is prepared and green compact sheetmolding, and the slurry is prepared and is combined using the soft magnetic metal described in claim any one of 1-2
Soft magnetic metal composite and the method for the common ball mill mixing of organic solvent of addition adhesive prepared by the preparation method of material；
Interior electrode fabrication, printing forms Cu inner wire figures in the green sheet；
Lamination is suppressed, and green sheet stacking described in two or more first is obtained into stacked body, each adjacent green compact in the stacked body
The Cu inner wire figures of piece are interconnected to form coil structure；Then the green sheet for being obtained with the green compact sheetmolding clamps institute
Stacked body is stated integrally to suppress；
Sintering, overall compacting gained laminated body is placed under more than 900 DEG C of vacuum or protective atmosphere and is sintered；
Grinding, is ground to expose the interior electrode to gained sintered body；
External electrode is manufactured, and is coated in the sintered body end face for exposing the interior electrode and is sintered Cu external electrodes.
6. the preparation method of slice component as claimed in claim 5, it is characterised in that：Described adhesive is PVB adhesives, institute
State green compact sheetmolding and use doctor blade method.
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| CN109513933B (en) * | 2018-10-10 | 2021-04-27 | 麦格磁电科技（珠海）有限公司 | Preparation method of iron-based soft magnetic core with high temperature resistance and high surface resistance |
| CN109967734B (en) * | 2019-03-28 | 2021-02-19 | 深圳华络电子有限公司 | Soft magnetic alloy material and preparation method thereof |
| CN110202129A (en) * | 2019-07-02 | 2019-09-06 | 深圳市麦捷微电子科技股份有限公司 | A kind of metal soft magnetic powder thermostable rustproof type deactivation method |
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| CN101820569A (en) * | 2010-03-19 | 2010-09-01 | 张家港市玉同电子科技有限公司 | Formula of multilayer piezoelectric ceramic for loudspeaker drive and production method thereof |
| CN102311260A (en) * | 2011-08-08 | 2012-01-11 | 中国地质大学（北京） | Novel MnZn-doped ferrite material and preparation method thereof |
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| CN103426581A (en) * | 2012-05-15 | 2013-12-04 | 上海康顺磁性元件厂有限公司 | Manganese and zinc soft magnetic ferrite KP6B and method for manufacturing same |
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| CN1174443C (en) * | 2001-07-19 | 2004-11-03 | 清华同方股份有限公司 | Components and preparing process of VHF plate sensor material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101820569A (en) * | 2010-03-19 | 2010-09-01 | 张家港市玉同电子科技有限公司 | Formula of multilayer piezoelectric ceramic for loudspeaker drive and production method thereof |
| CN102311260A (en) * | 2011-08-08 | 2012-01-11 | 中国地质大学（北京） | Novel MnZn-doped ferrite material and preparation method thereof |
| CN102557604A (en) * | 2012-03-06 | 2012-07-11 | 深圳顺络电子股份有限公司 | NiCuZu ferrite material and preparation method thereof |
| CN103426581A (en) * | 2012-05-15 | 2013-12-04 | 上海康顺磁性元件厂有限公司 | Manganese and zinc soft magnetic ferrite KP6B and method for manufacturing same |
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