CN103943321B - Magnetic core and coil-type electronic element - Google Patents
Magnetic core and coil-type electronic element Download PDFInfo
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- CN103943321B CN103943321B CN201310641723.5A CN201310641723A CN103943321B CN 103943321 B CN103943321 B CN 103943321B CN 201310641723 A CN201310641723 A CN 201310641723A CN 103943321 B CN103943321 B CN 103943321B
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Abstract
The present invention aims to provide a magnetic core has excellent strength and a coil-type electronic element. The magnetic core has a core part formed by a soft magnetic body composition, and at least part of a covering layer formed on the surface of the core part; the soft magnetic body composition has a plurality of soft magnetic alloy particles, and a crystal boundary disposed among the soft magnetic alloy particles; the soft magnetic alloy particles are Fe-Si-Al series alloy particles or Fe-Si-Cr series alloy particles; and the crystal boundary is provided with a Si-containing layer.
Description
Technical field
The present invention relates to magnetic core and coil form electronic unit.
Background technology
Metallic magnetic gonosome compared with ferrite haves the advantages that high saturation flux density can be obtained.As so
Metallic magnetic gonosome, it is known to Fe-Si-Al systems alloy or Fe-Si-Cr systems alloy etc..
In patent document 1, it is proposed that possess low cost and have both the coil of the magnetic of high permeability and magnetic flux density
Type electronic unit.
As such coil form electronic unit, inductance component, EMC coil components, transformer part etc. can be enumerated,
In recent years, as the magnetic core of these electronic units, it is widely used and is made up of Fe-Si-Al systems alloy or Fe-Si-Cr systems alloy
Metallic magnetic gonosome.
Especially, using such metallic magnetic gonosome being made up of Fe-Si-Al systems alloy or Fe-Si-Cr systems alloy as can
In the case of realizing that the magnetic core of the coil form electronic unit of the miniaturization installed to the face on circuit substrate carrys out use, it is desirable to make
For the high intensity of magnetic core.
Prior art literature
Patent document
Patent document 1：Japanese Unexamined Patent Publication 2011-249774 publications
The content of the invention
The present invention its object is to provide the magnetic core with excellent intensity and coil form in view of such actual state
Electronic unit.
In order to achieve the above object, magnetic core involved in the present invention, it is characterised in that with by soft-magnetic body composition structure
Into core and be formed in the core surface at least one of coating, the soft-magnetic body composition has
Multiple non-retentive alloy particles and it is present in the intergranular crystal boundary of the non-retentive alloy, the non-retentive alloy particle is
Fe-Si-Al systems alloying pellet or Fe-Si-Cr systems alloying pellet, in the crystal boundary, there are the layer containing Si.
In magnetic core involved in the present invention, the crystal boundary of the soft-magnetic body composition in non-retentive alloy particle of core is constituted
With the layer containing Si, additionally, at least a portion on the surface of core is formed with coating, thus, it is possible to play as magnetic core
Excellent intensity.
Preferably, it is characterised in that the layer containing Si is Si oxide skin(coating)s or Si composite oxide layers.
Preferably, it is characterised in that the layer containing Si is also present in the surface of the non-retentive alloy particle.
Preferably, it is characterised in that the layer containing Si for being present in the surface of the non-retentive alloy particle is multiple for Si-Cr
Close oxide skin(coating).
Additionally, coil electronic unit involved in the present invention has above-mentioned magnetic core.As coil form electronic unit without spy
Other restriction, can illustrate the electronic unit of inductance component, EMC coil components, transformer part etc..Especially, it is adaptable to
The coil form electronic unit of the miniaturization to the face installation on circuit substrate can be realized.
Description of the drawings
Fig. 1 is the summary sectional view of the magnetic core involved by an embodiment of the invention.
Fig. 2 is the outline section of the drum apparatus that the manufacture of the magnetic core involved by an embodiment of the invention is used
Figure.
Fig. 3 is the sectional view for having wound the magnetic core after coil.
Fig. 4 is the major part amplification sectional view of the core shown in Fig. 1.
Fig. 5 is the major part amplification sectional view for representing the core for carrying out observation station when EDS is parsed.
Fig. 6 is the result that EDS parsings are carried out in the observation station shown in Fig. 5.Fig. 6（a）It is involved by embodiments of the invention
And sample 1 and 2 analysis result, Fig. 6（b）It is the analysis result of the sample 3 and 4 involved by comparative example of the invention.Further,
The longitudinal axis is strength ratio, and transverse axis is depth.
Specific embodiment
Hereinafter, based on the embodiment shown in the drawings explanation present invention.
Magnetic core
The shape of magnetic core involved in the present invention, in addition to the drum type shown in Fig. 1, can also illustrate FT types, ET types, EI
Type, UU types, EE types, EER types, UI types, ring-like, kettle type, cup type etc..In the present embodiment, as shown in figure 1, magnet 1 has drum
Core shape, with the surface entirety in core 2 structure of coating 10 is formed with.
Core
Core 2 has the core 4 of cylinder or corner post shape and is formed on two along the axial direction of the core 4
A pair of flanges portion 5 of side.The external diameter of flange part 5 is bigger than the external diameter of core 4, is formed with by flange part 5 in the periphery of core 4
The recess 6 of encirclement.Furthermore, by the way that coiling 30 is made into coil component wound on the recess 6.
The size of core 2 has no particular limits, and in the present embodiment, the external diameter of core 4 is 0.6～1.2mm, is rolled up
The axial width of core 4 is 0.3～1.0mm, and the external diameter of flange part 5 is 2.0～3.0mm, the thickness of flange part 5 is 0.2～
0.3mm, the depth from the outer surface of the outer surface to core 4 of flange part 5 is 0.5～1.0mm.Further, flange part 5
Shape than circular, can also be quadrangle, octagon etc..
Soft-magnetic body composition of the core 2 involved by present embodiment is constituted.
Soft-magnetic body composition involved by present embodiment, it is characterised in that with multiple non-retentive alloy particles, with
And be present in the intergranular crystal boundary of the non-retentive alloy, the non-retentive alloy particle be Fe-Si-Al systems alloying pellet or
Fe-Si-Cr systems alloying pellet, in the crystal boundary, there are the layer containing Si.
Soft-magnetic body composition involved by present embodiment by meeting above-mentioned composition, such that it is able to obtain excellent magnetic
Characteristic, even and if can also obtain the enough intensity as magnetic core in the case of than relatively low shaping pressing formation.Separately
Outward, in press molding, can be by than relatively low shaping pressing formation, it is thus possible to seek the burden to mould further under
Drop, it is possible to increase productivity.
Soft-magnetic body composition involved by present embodiment, as shown in figure 4, have multiple non-retentive alloy particles 21,
And it is present in the intergranular crystal boundary 30 of non-retentive alloy.
The layer containing Si involved by present embodiment is present in and is formed in 2 intergranular crystal boundaries 30 or is present in 3
Crystal boundary 31 between particle above（Three phase point etc.）.By the presence of such layer containing Si, involved by present embodiment
Even if magnetic core in the case of with than relatively low shaping pressing formation, it is also possible to obtain the enough intensity as magnetic core.Additionally,
Such layer containing Si plays a part of insulator by being present in crystal boundary.
The layer containing Si involved by present embodiment is preferably Si oxide skin(coating)s or Si composite oxide layers.
Further, in the present invention, oxide skin(coating) and composite oxide layer are comprising amorphous layer（amorphous
layer）, crystallizing layer and their mixed layer wide concept.
As the Si oxide skin(coating)s or Si composite oxide layers involved by present embodiment, there is no particular limitation, Ke Yiju
Go out such as amorphous layer containing Si, non-crystalline silicon（amorphous silicon）, silica, Si-Cr composite oxides etc..
The layer containing Si involved by present embodiment is preferably also present in the surface of non-retentive alloy particle.This is present in
The layer containing Si on the surface of non-retentive alloy particle is preferably Si-Cr composite oxide layers.Si-Cr composite oxide layers do not have
It is special to limit, amorphous layer containing Si and Cr etc. can be enumerated.
The layer containing Si involved by present embodiment is preferably made up of noncrystalline.Further, a part can also be by crystallizing
Quality structure into.
The thickness of the layer containing Si involved by present embodiment is preferably 0.01～0.2 μm, and more preferably 0.01～0.1
μm。
Further, the layer containing Si is not necessarily required to all modes to cover the surface of non-retentive alloy particle formed,
The part on the surface of non-retentive alloy particle can be formed in.In addition, the thickness of the layer containing Si can be uneven, should
Composition may not be homogeneous.
The presence or absence of layer containing Si involved by present embodiment or its thickness can be by the systems of magnetic core described below
Make species in method, with reference to material or its addition, other adding ingredients, the heat treatment temperature of formed body and atmosphere gas etc.
To control.
In the present embodiment, as judge the layer containing Si whether there is in the surface of non-retentive alloy particle and crystal boundary
Method, have no particular limits, for example can be parsed to judge by the mapping graph picture to Si.Following presentation is specific
Method.
First, by using scanning infiltration type electron microscope（STEM）To observe magnetic core, non-retentive alloy particle is differentiated
And crystal boundary.Specifically, the section of dielectric layer is photographed by STEM, obtains bright-field（BF）Picture.By the bright-field
It is present between non-retentive alloy particle and non-retentive alloy particle as in and with different with the non-retentive alloy particle right
Than degree region as crystal boundary.Whether have the judgement of different contrasts can be with visually carrying out, it is also possible to by carrying out
Software of image procossing etc. is judging.
Further, for the other elements of Cr etc., it is also possible to mapping graph picture is made and observed of same method.
The average crystallite grain diameter of the non-retentive alloy particle involved by present embodiment is preferably 30～60 μm.Pass through
Average crystallite grain diameter is set to into above-mentioned scope, the thin layer of magnetic core can be easily realized.
Non-retentive alloy particle involved by present embodiment is Fe-Si-Al systems alloying pellet or Fe-Si-Cr systems alloy
Particle.
Above-mentioned composition is met by non-retentive alloy particle, the soft-magnetic body composition involved by present embodiment can be obtained
To excellent magnetic characteristic, even and if also can obtain as the enough of magnetic core in the case of than relatively low shaping pressing formation
Intensity.In addition, in press molding, can be by than relatively low shaping pressing formation, it is thus possible to seek the burden to mould
Further decline, it is possible to increase productivity.In addition, above-mentioned composition is met by non-retentive alloy particle, easily at interface 30
Form the layer containing Si.
There is no particular limitation for the composition of Fe-Si-Al systems alloying pellet, preferably comprises and is scaled 0.5～10.5 matter by Al
The aluminium of amount %（Al）, be scaled by Si the silicon of 4.5～14.5 mass %（Si）, surplus is by iron（Fe）Constitute.
Surplus can only by iron in non-retentive alloy particle（Fe）Constitute.
There is no particular limitation for the composition of Fe-Si-Cr systems alloying pellet, preferably comprises and is scaled 1.5～8 mass % by Cr
Chromium（Cr）, be scaled by Si the silicon of 1.4～9 mass %（Si）, surplus is by iron（Fe）Constitute.
Chromium in non-retentive alloy particle（Cr）Amount press Cr conversion be preferably 1.5～8 mass %, more preferably 3～
7 mass %.If the amount of Cr is very few, there is intensity and magnetic characteristic downward trend；If excessive, there is intensity decline
Trend.
Silicon in non-retentive alloy particle（Si）Amount press Si conversion be preferably 1.4～9 mass %, more preferably 4.5
～8.5 mass %.The amount of Si is too little or too much, there is intensity and magnetic characteristic downward trend.
Surplus can only by iron in non-retentive alloy particle（Fe）Constitute.
Soft-magnetic body composition involved by present embodiment in addition to the constituent of above-mentioned non-retentive alloy particle,
Sometimes carbon is also included（C）And zinc（Zn）Deng composition.
Further, C is considered as to come from the organic compound ingredient used in the manufacture process of soft-magnetic body composition.
In addition, Zn be considered as come from by press-powder shaping obtain soft-magnetic body composition when in order to reduce the pressure release of device and in mould
The zinc stearate of addition.
In soft-magnetic body composition involved by present embodiment, carbon（C）Amount be preferably smaller than 0.05 mass %,
More preferably 0.01～0.04 mass %.If the amount of C is excessive, presence cannot becoming as the enough intensity of magnetic core
Gesture.
In soft-magnetic body composition involved by present embodiment, zinc（Zn）Amount be preferably 0.004～0.2 matter
Amount %, more preferably 0.01～0.2 mass %.The amount of Zn is excessive or vice versa very few, and existing cannot be used as the foot of magnetic core
The trend of enough intensity.
Further, in the soft-magnetic body composition involved by present embodiment, in addition to mentioned component, can also contain
Inevitable impurity.
In addition, the thermal coefficient of expansion of core 2 changes according to the composition of soft-magnetic body composition, about 9 × 10-6/℃
～10 × 10-6/ DEG C or so.
Coating
As the material of coating 10, as long as the material of the thermal coefficient of expansion below the thermal coefficient of expansion with core 2
Just have no particular limits, for example, can illustrate glass composition, SiO2、B2O3、ZrO2Deng.Further, coating 10 can be by more
Plant material to constitute, it is possible to have the lit-par-lit structure being made up of multilayer.
In the present embodiment, coating 10 is preferably made up of glass composition.As glass composition, as long as with non-
The state of crystalloid is formed in the composition on the surface of core 2 or just no special as the composition of sintered glass ceramics formation
Limit, for example, can illustrate Si-B systems glass（Pyrex）, alkali-free glass, lead system glass etc..
The composition of composition of the thermal coefficient of expansion of glass composition according to contained by glass composition or containing for each composition
Amount etc. and change.Therefore, in the way of the thermal coefficient of expansion of glass composition is necessary below the thermal coefficient of expansion to become core 2
The composition being properly set to point or amount.
As long as coating 10 is capped just without special limit with the degree that can obtain the improvement of power loss
It is fixed, at least a portion on the surface of core 2 can be formed in, relative to the surface area of core 2, it is formed with the ratio of coating
（Coverage rate）Preferably 50～100%, more preferably 90～100%.Coverage rate is higher, then as the breach for preventing core 2 etc.
The effect of protective layer is also bigger.
Further, in FIG, the situation that coverage rate is 100% is represented.In addition, in core 2, if being wound with coiling etc.
Part（It is in the present embodiment recess 6）Coating 10 is formed about, has then been readily obtained more preferable effect.
As long as the thickness of coating 10 can obtain the thickness of the degree of the improvement of power loss just without special
Restriction, preferably greater than 0 μm and less than 50 μm, more preferably more than 5 μm and less than 25 μm.If being formed with coating 10, electricity
Power loss be improved, if but coating is blocked up, due to the contribution of the improvement to power loss it is little, manufacturing cost increase and
It is not preferred.If in addition, coating has the thickness of a certain degree, the function of the protective layer as core can be played.Therefore,
The thickness of coating 10 is preferably in above-mentioned scope.
If additionally, coating 10 has insulating properties, even if core 2 is electric conductivity, it is also possible to guarantee and wound
The insulation of coiling.
Then, the magnetic core for illustrating to be made up of glass composition as the coating 10 of the magnetic core involved by present embodiment
One example of manufacture method.
Manufacture method involved by present embodiment preferably has：By soft-magnetic body alloy powder with mixed with reference to material
To obtain the operation of mixture；Be dried mixture and after obtaining the hirudo leech of bulk, by the way that the hirudo leech are crushed come shape
Into the operation of pelletizing；Mixture or pelletizing are configured to into the shape of the compressed-core to be made to obtain the work of formed body
Sequence；By the way that resulting formed body is heated made that the operation of core 2 is hardened and obtained with reference to material；In resulting core
2 form the operation for burning till front coating；And be heat-treated and formed coating to being formed with the core 2 for burning till front coating
10 and obtain the operation of magnetic core.
The compressed-core that manufacture method by involved by present embodiment is obtained is soft by involved by above-mentioned present embodiment
Magnetic composition is constituted.
As soft-magnetic body alloy powder, it is possible to use Fe-Si-Al systems alloying pellet or Fe-Si-Cr systems alloying pellet.
The shape of soft magnetic alloy powder has no particular limits, excellent for viewpoint of the inductance up to highfield domain is maintained
Elect spherical or ellipsoid shaped as.In the middle of these, for the viewpoint of the further intensity of increase compressed-core, preferably ellipsoid
Shape.In addition, the average grain diameter of soft magnetic alloy powder is preferably 10～80 μm, more preferably 30～60 μm.If average grain diameter mistake
It is little, then there is permeability step-down and as the magnetic characteristic downward trend of soft magnetic material, in addition, operation becomes difficult.On the other hand, if
Average grain diameter is excessive, then have vortex flow to become trend that is big and losing increase extremely.
Soft magnetic alloy powder can be obtained by the method same with the modulator approach of known soft magnetic alloy powder.
At this point it is possible to be modulated using gas atomization, water atomization, rotating disk method.In the middle of these, have to easily make
The soft magnetic alloy powder of desired magnetic characteristic, preferably water atomization.
As material is combined, using the combination material comprising silicone resin.By using silicone resin as material is combined, in soft magnetism
The crystal boundary of elastomeric composition is formed effectively with the layer containing Si.Even if the magnetic core being made up of such soft-magnetic body composition exists
In the case of than relatively low shaping pressing formation, it may have enough intensity.
Further, in the range of the effect of the without prejudice to present invention material can also be combined comprising others.As other knots
Material is closed, for example various organic polymer resins, phenolic resin, epoxy resin and waterglass etc. can be enumerated.
Silicone resin is can be used alone with reference to material, or combines to use silicone resin with reference to material with others.Further,
For preferably by the carbon in soft-magnetic body composition（C）Amount be limited to less than the viewpoint of 0.05 mass %, it is preferred with reference to material
Mainly use silicone resin.If the amount of the C in soft-magnetic body composition is excessive, the intensity of the magnetic core obtained by having declines
Trend.
It is different according to the characteristic of required magnetic core with reference to the addition of material, but preferably with respect to the soft of 100 weight portions
Magnetic alloy powder, can add 1～10 weight portion, and the more preferably soft-magnetic body alloy powder relative to 100 weight portions is 3
～9 weight portions.If the addition with reference to material is excessive, there is permeability to decline and lose the big trend of change.On the other hand, if with reference to
The addition of material is very few, then have the trend for being difficult to ensure that insulation.
The addition of silicone resin is 3～9 weight portions preferably with respect to the soft-magnetic body alloy powder of 100 weight portions.If
The addition of silicone resin is very few, then the crystal boundary in soft magnetism composition is difficult to form the layer containing Si, has as formed products
Intensity downward trend.
In addition, in the mixture or pelletizing, can add as needed in the range of the effect of the without prejudice to present invention
Plus organic solvent.
As organic solvent, as long as just there is no particular limitation for the solvent that can dissolve with reference to material, can enumerate for example
The various solvents of toluene, isopropanol, acetone, methyl ethyl ketone, chloroform, ethyl acetate etc..
In addition, in the mixture or pelletizing, as needed can be with the range of the effect of the without prejudice to present invention
Addition various additives, lubricant, plasticizer, thixotropic agent etc..
As lubricant, can enumerate for example aluminum stearate, barium stearate, magnesium stearate, calcium stearate, zinc stearate,
And strontium stearate etc..They can be used alone or combine two or more to use.In the middle of these, for so-called resilience
Little such viewpoint, preferably uses zinc stearate as lubricant.
In the case of using lubricant, its addition is preferably with respect to the soft-magnetic body alloy powder of 100 weight portions
0.1～0.9 weight portion, more preferably the soft-magnetic body alloy powder relative to 100 weight portions are 0.3～0.7 weight portion.If lubrication
Agent is very few, then have the demoulding after shaping to become trend that is difficult and easily producing shaping crackle.On the other hand, if lubricant mistake
It is many, then cause the decline of shaping density, permeability reduces.
Especially, using zinc stearate as lubricant in the case of, the soft-magnetic body combination obtained by preferred adjustment
In thing, zinc（Zn）Amount be in the range of 0.004～0.2 mass %, addition.If the amount of Zn is excessive, have
Cannot be used as the trend of the enough intensity of magnetic core.
As the method for obtaining mixture, there is no particular limitation, by existing known method, by soft-magnetic body alloy
Powder, mixed to obtain with organic solvent with reference to material.Further, various addition materials can be added as needed.
In mixing, it is, for example possible to use pressure kneader, agitating ball mill, vibrating mill, ball mill, V mixers etc.
Mixer or fluidized granulation machine, rotate the comminutor of comminutor etc..
In addition, as the temperature and time of mixed processing, there is no particular limitation, preferably 1～30 minute left side at room temperature
It is right.
As the method for obtaining pelletizing, there is no particular limitation, by existing known method, after mixture is dried,
Dried mixture is broken into pieces to obtain.
It is preferably lower 5～60 minutes in room temperature～200 DEG C or so as the temperature and time of dried process.
As needed, lubricant can be added in pelletizing.In pelletizing add lubricant after, preferably mixing 5～
60 minutes.
As the method for obtaining formed body, there is no particular limitation, preferably by existing known method, using with institute
The shaping dies of the cavity of desired shape, filling mixture or pelletizing in the cavity, with the forming temperature of regulation and rule
Fixed forming pressure is by the mixture compression molding.
There is no particular limitation for the molding condition of compression molding, can according to the shape and size of soft magnetic alloy powder or
The shape of compressed-core, size and density etc. are suitably determining.For example, generally, maximum pressure is 100～1000MPa or so,
Preferably 400～800MPa or so, the time for remaining maximum pressure is 0.5 second～1 minute or so.
In the manufacture method involved by present embodiment, by including silicone-based resin with reference to material, can be by shaping pressure
Power is decreased to above-mentioned maximum pressure.Even if additionally, in the case where so forming pressure is reduced, due in the soft magnetism for constituting magnetic core
The crystal boundary of elastomeric composition is formed with the layer containing Si, therefore magnetic core also becomes the magnetic core with enough intensity.As a result, energy
Enough reduce manufacturing cost, it is possible to increase productivity and economy.
If further, forming pressure is too low, having and being difficult to seek the densification and high permeability and difficulty obtained by shaping
To obtain the trend of enough mechanical strengths.On the other hand, if shaping when shaping presses through height, pressure applies effect saturation
Trend, and have manufacturing cost to increase and the impaired trend of productivity and economy, in addition, have shaping dies easily deterioration and
Durability downward trend.
There is no particular limitation for forming temperature, generally, it is preferred to be room temperature～200 DEG C or so.Further, when having more lifting shaping
Forming temperature, then the higher trend of the density of formed body, but have the oxidation and institute for promoting non-retentive alloy particle if too high
The trend of the performance degradation of the compressed-core for obtaining, in addition, manufacturing cost increases and productivity and economy can be damaged.
Formed body resulting after shaping is carried out into heat-treating methods, can be carried out by known method, do not had
It is special to limit, it is however generally that, preferably using annealing furnace will be configured at an established temperature arbitrary shape by shaping
Formed body carry out heat treatment to carry out.
There is no particular limitation for treatment temperature during heat treatment, generally, it is preferred to be 600～900 DEG C or so, more preferably
700～850 DEG C.Treatment temperature during heat treatment is too high or too low, and have cannot be used as the trend of the enough intensity of magnetic core.
Heat treatment step is preferably carried out under oxygen-containing atmosphere gas.Here, there is no particular limitation for oxygen-containing atmosphere gas, Ke Yiju
Go out atmospheric atmosphere gas（Generally comprise 20.95% oxygen）Or with the mixing atmosphere gas of the inactive gas of argon or nitrogen etc. etc., it is excellent
Under electing atmospheric atmosphere gas as.By being heat-treated under oxygen-containing atmosphere gas, can effectively in the crystalline substance of soft-magnetic body composition
Boundary forms the layer containing Si.
In addition, the preferred shaping density of core obtained by so is 5.50g/cm3More than.It is 5.50g/cm in shaping density3
During the above, there are compressed-core various property as high permeability, high intensity, high core resistance, low core loss of densification
Excellent trend can be gone up.
For following resulting core 2, using the drum apparatus shown in Fig. 2, on the surface of core 2, formed by glass
Coating 10a before the heat treatment of the compositions such as composition, binder resin.
Drum apparatus 20 shown in Fig. 2 have cylindric or corner post shape cylinder sleeve 20a, and drum container 22 is in its shaft core week
Enclosing can be along arrow A direction（Or its rightabout）Rotatably it is accommodated in the hollow inside of drum apparatus 20.
In cylinder sleeve 20a, inlet tube 23 and outlet 24 are respectively formed with.Drying gas enters cylinder from inlet tube 23
The inside of set 20a, from outlet 24 air inside cylinder sleeve can be discharged.
In the shaft core position of the inside of drum container 22, nozzle 25 is axially configured with, can be from nozzle 25 towards storage
There is the spraying slurry 26 of multiple cores 2 of the inside of drum container 22.Drum container 22 rotates along arrow A directions, thus core 2
Exist with the state shown in Fig. 2, stirred by the rotation of drum container 22.
Nozzle 25 can spray slurry 26 towards the set of core 2.Further, can freely change from nozzle 25
The spray direction of slurry.In addition, in cylinder sleeve 20a, being connected with the discharge pipe for omitting diagram, unnecessary slurry 26 can be discharged.
In the wall of drum container 22, the outside multiple holes with inside of connection are formed with, are stored in the lower section of cylinder sleeve 20a
Slurry 26 invades the inside of drum container 22, core 2 can be immersed in into the slurry 26.In addition, in drying gas from entering
When mouth pipe 23 is passed to outlet 24 by cylinder sleeve 20a, the inside of drum container 22 is also passed to.
Coating 10a before in order to form heat treatment, first, the drum container 22 multiple cores 2 being accommodated in shown in Fig. 2
Inside.Then, rotate drum container 22, while the set of stirring core 2, while from the spraying slurry 26 of nozzle 25, being formed
Coating 10a before heat treatment.
Slurry 26 is comprising by glass powder, binder resin and solvent obtained from the above-mentioned glass composition of crushing.
In addition can also be comprising other additives.Glass composition can will constitute the non-of oxide, the halide of said composition etc.
The raw material of oxide etc. mixes, melts, rapidly cools down and become noncrystalline.In addition, as glass composition, it is also possible to using knot
Crystallized glass.In the present embodiment, using Si-B systems glass as glass powder.The average grain diameter of glass powder（Intermediate value is straight
Footpath）There is no particular limitation, preferably less than more than 0.1 μm 10 μm of scope.
The binder resin that slurry 26 is included is preferably polyvinyl alcohol（PVA）, polyvinyl alcohol resin become gonosome or they
Mixture.By doing so it is possible, the coating 10a before the heat treatment for being formed is excellent with the close attachment of core 2.
Solvent preferably comprises water.Solvent can only be water, preferably logical when the surface of glass powder and the big contact angle of water
After being mixed into ethanol, isopropanol according to a certain percentage（IPA）, isobutanol（IBA）Deng water miscible alcohol suppressing glass powder
Cohesion is settled.
What the slurry 26 for spraying to core 2 formed the surface that covers each core 2 burns till front coating 10a.Now, it is unnecessary
Slurry 26 is discharged by omitting the discharge pipe of diagram.Process time from the spraying slurry 26 of nozzle 25 is without special limit
It is fixed, for example, 30～180 minutes or so.In addition, although the temperature of the slurry 26 during injection depends on the composition of solvent but preferably
For less than more than 40 DEG C 100 DEG C.In the case of using low-boiling solvent, temperature is preferably reduced in the range of said temperature.
Then, slurry 26 is sprayed while while the dried process of the coating 10a before being heat-treated.At drying
In reason, drying gas is flowed into the inside of cylinder sleeve 20a from inlet tube 23, and is discharged from outlet 24.The dried process
The drying gas for being used is, for example, 50～100 DEG C of air.After spray treatment, it is also possible to carry out such as 5～30 minutes again
Dried process.
After dried process, the core 2 of the coating 10a being formed with before heat treatment takes out from drum container 22, carries out heat soft
Change is processed.Softening point of glass powder that heat treatment condition is included according to the coating 10a before heat treatment etc. is determining.Specifically
For, heat treatment temperature is preferably 600～800 DEG C, and heat treatment time is 5～120 minutes.
Heat treatment step is preferably carried out under oxygen-containing atmosphere gas.Here, there is no particular limitation for oxygen-containing atmosphere gas, Ke Yiju
Go out atmospheric atmosphere gas（Generally comprise 20.95% oxygen）Or with the mixing atmosphere gas of the inactive gas of argon or nitrogen etc. etc..It is excellent
Under being selected in atmospheric atmosphere gas.
After heat treatment, the coating 10 of vitrifying is formed with the surface of core 2, obtains the ferrite core shown in Fig. 1
1.Further, in the present embodiment, vitrifying is defined as becoming with same with crystalline phase in continuous amorphous individual film
The rigid state of degree.
Thereafter, as shown in figure 3, the end face of a flange part 5 in each core 2, by printing, transfer, dipping, sputtering,
Plating method etc. is forming a pair of terminal electrode 32 being made up of silver, titanium, nickel, chromium, copper etc..Even if the core 2 of terminal electrode 32 is to lead
Electrical, also due to there is coating 10 and insulated.
Thereafter, by coiling 30 around core 4, by the two ends of the coiling respectively by being thermally compressed, utilizing super
Welding, welding of sound wave or laser etc. etc. and be connected to terminal electrode 32, complete involved by an embodiment of the invention
Coil component.
In the magnetic core involved by present embodiment, the excellent intensity as magnetic core can be played.In addition, especially through
Coating is constituted by glass composition, coating can be readily formed on the surface of core.In addition, by the surface shape in core
Into by being made up of the coating that constitutes glass, it is possible to increase as the intensity of magnetic core.In addition, being insulating properties in glass composition
In the case of, even if core is electric conductivity, it is also possible to guarantee the insulating properties with the coiling of winding etc..
More than, embodiments of the present invention are illustrated, but the present invention is not limited to completely such embodiment,
It is self-evident, can implement in a wide variety of ways in the range of the purport without departing from the present invention.
For example, in the above-described embodiment, magnetic core is manufactured by carrying out press-powder shaping to mixture or pelletizing（Pressure
Powder magnetic core）, but it is also possible to said mixture is carried out into laminar shaping and is laminated to manufacture magnetic core.In addition, except duse process
In addition, it is also possible to which formed body is obtained by wet-formed, extrusion shaping etc..
In the above-described embodiment, in order to form the layer containing Si in the crystal boundary of soft-magnetic body composition, using silicone
Resin is used as combining material, but it is also possible to substitute silicone resin and using the Si of silica gel or silica dioxide granule etc. contain composition as
Additive.
In addition, in the above-described embodiment, to burning till after core form the coating before heat treatment, and carried out
It is heat-treated and forms coating, but it is also possible to while carries out the heat treatment burnt till with coating of core.By doing so it is possible, can
Simplify operation.
Further, while carry out core burn till with coating heat treatment when heat treatment condition can be single with core
Firing condition is identical, it is also possible to identical with the heat treatment condition of coating.
Additionally, as needed, resin dipping can be carried out to formed body.Thereby, it is possible to the intensity for further improving magnetic core.
In addition, in the above-described embodiment, using the magnetic core involved by present embodiment as coil form electronic unit,
But have no particular limits, it is also possible to function properly as motor, Switching Power Supply, dc-dc, transformer, choke coil etc.
Various electronic units magnetic core.
[embodiment]
Hereinafter, invention is illustrated in greater detail by embodiment, but the present invention is not limited to these embodiments.
（Embodiment 1）
With regard to sample 1
[modulation of soft magnetic alloy powder]
First, ingot bar, the chunk of Fe simple substance, Cr simple substance and Si simple substance are prepared（Block）Or pill（Particle）.Then by them
It is to be mixed in the way of 88.5 mass %, Cr are 5 mass % and composition that Si is 6.5 mass % to become Fe, is accommodated in and is configured in
Crucible in water atomization plant.Then, in torpescence atmosphere gas, using the actuating coil being arranged on outside crucible, by height
Crucible is heated to more than 1600 DEG C by frequency induction, and by the ingot bar in crucible, chunk or pill liquation is melted and be obtained by mixing.
Then, from the liquation being arranged in the nozzle of crucible ejection crucible, at the same time, by making high pressure（50MPa）Water
Stream collides sprayed liquation and is rapidly cooled down, and makes the soft magnetic alloy powder being made up of Fe-Si-Cr systems particle（It is flat
Equal particle diameter：50μm）.
By fluorescent x-ary analysis resulting soft magnetic alloy powder is carried out composition analysis as a result, it is possible to really
Recognize consistent with the composition for preparing.
[making of core]
Relative to the soft magnetic alloy powder obtained by 100 weight portions, add the silicone resin of 6 weight portions（Dong Lidao
It is healthy and free from worry（Strain）System：SR2414LV）, they are mixed at room temperature 30 minutes by pressure kneader.Then, by mixture in air
In at 150 DEG C be dried 20 minutes.In Magnaglo after the drying, add these soft magnetisms conjunctions relative to 100 weight portions
Bronze end is the zinc stearate of 0.5 weight portion（Day east chemical conversion system：zinc stearate）It is mixed by V mixers as lubricant
Close 10 minutes.
Then, resulting mixture is configured to the angular sample of 5mm × 5mm × 10mm, formed body is made.Further,
Shaping pressure is 600MPa.Formed body after by pressurization carries out in an atmosphere heat treatment 60 minutes at 750 DEG C, makes silicone tree
Fat is hardened, and obtains magnetic core sample.
[various evaluations]
<The Si of crystal boundary contains the confirmation of layer>
First, compressed-core is cut off.For the section, by scanning infiltration type electron microscope（STEM）Seen
Examine, carry out the differentiation of soft-magnetic body alloying pellet and crystal boundary.
Then, as shown in figure 5, in optional observation station, using the EDS devices for being attached to STEM, carrying out EDS point
Analysis.The result of EDS parsings is represented in Fig. 6 as skeleton diagram.Further, the longitudinal axis of Fig. 6 is by the characteristic X-ray obtained by measurement
Strength ratio.
<3 bending strength tests（Intensity）>
For compressed-core sample, in accordance with the regulation of JIS R1601,3 bending strength tests are carried out.
3 bending strengths are placed in test film on 2 fulcrums for configuring at a certain distance, central 1 point between fulcrum
Maximum stress in bend when applying loading and fractureing（kg/mm2）.
Additionally, from the result of resulting maximum stress in bend, by following formula carrying for the intensity that coating is formed is calculated
High rate.
The increase rate of intensity（%）
=100×（There is the sample-intectate sample of coating）/（Intectate sample）
In the present embodiment, it is good by increase rate more than 24%.As a result represent in table 1.
With regard to sample 2
Style 2 is except the coating before the formed body being similarly obtained with sample 1 forms heat treatment by following method
In addition, magnetic core sample is made with the method same with sample 1, carries out same evaluation.Result is represented in table 1 and Fig. 6.
First, the powder for forming the glass composition of coating is prepared.Using Si-B systems glass as glass combination
Thing.Si-B systems glass, the raw material for constituting the oxide of glass ingredient etc. is mixed and is melted, and followed by rapidly cools down
Make.
Further, the thermal coefficient of expansion of the Si-B systems glass composition used as coating is 6 × 10-6/℃.Core and glass
The thermal coefficient of expansion of glass composition is measured by TMA.
Then, the slurry used to form coating is made.First, by the weight of regulation than the glass obtained by mixing
The powder and PVA of glass composition.Additionally, by the weight of regulation than the solid composition obtained by mixing（Glass powder and PVA's is mixed
Compound）With solvent, mixed with ball mill and prepared slurry.It is molten with ethanol using water is mixed with by 8 ︰ 2 as solvent
Agent.Binder resin is 10 weight % relative to the amount of the glass powder in slurry.
Then, formed body is put in the drum container of drum apparatus, it is on the surface of formed body all, by using on
The spray treatment of the slurry stated and formed heat treatment before coating.In addition, with injection simultaneously, entering at 70 DEG C of warm air temperature
Row dried process.
Thereafter, the formed body of the coating being formed with before heat treatment is taken out from drum container, by the formed body at 750 DEG C
Heat treatment 1 hour, the coating for obtaining vitrifying is formed in all magnetic core sample in surface of formed body.
The thickness of coating is 3～25 μm or so.Further, the size before and after the thickness of coating is formed by coating is calculated
Go out.
In addition, coverage rate is 98～100% or so.Further, coverage rate is by for 20 samples are by visually observing,
For the incomplete sample of the formation of coating, measure area coverage to calculate.
With regard to sample 3
Sample 3 is except using non-silicone-based resin（The rapids chemical conversion of length（Strain）System：DENATITE XNR4338）As bonding tree
Beyond fat, magnetic core sample is made with the method same with sample 1, carry out same evaluation.As a result represent in table 1 and Fig. 6.
With regard to sample 4
Sample 4 is except using non-silicone-based resin（The rapids chemical conversion of length（Strain）System：DENATITE XNR4338）As bonding tree
Beyond fat, magnetic core sample is made with the method same with sample 2, carry out same evaluation.As a result represent in table 1 and Fig. 6.
[table 1]
In sample 1 and 2, STEM observations and EDS parsings are as a result, it is possible to confirm constituting the soft-magnetic body combination of core
The crystal boundary of thing is formed with the layer containing Si.
Confirm the big difference of such sample 1 and 2, and the covering that is made up of glass whether is formed on the surface of core
Layer is relevant, and in the sample 2 of coating is formed with, compared with the sample 1 for not forming coating, the increase rate of intensity is more than 24%.
On the other hand, the result of STEM observations and EDS parsings, it is thus identified that in the crystalline substance of the soft-magnetic body composition for constituting core
Boundary is not formed in the sample 3 and 4 of the layer containing Si, is compared with 2 with sample 1, and intensity is low.
Even if additionally, being formed with the situation of coating on the surface of core（Sample 4）Under, also confirm sample 2 so
Intensity drastically raising.
From these results, it is thus identified that in magnetic core involved in the present invention, by constituting the soft-magnetic body combination of core
There is the layer with Si in the crystal boundary of thing, so as to the increase rate of the intensity when the surface of core forms coating increases.
Especially, the result of EDS parsings, in sample 1 and 2, confirms comprising Si in the crystal boundary of soft-magnetic body composition
Amorphous layer.Additionally, in particle surface, it is thus identified that the amorphous layer comprising Si and Cr（With reference to Fig. 6（a））.On the other hand, exist
In sample 3 and 4, the layer containing Si is not observed in the crystal boundary of soft-magnetic body composition（With reference to Fig. 6（b））.Such difference
It is considered as the difference of the increase rate of intensity of the impact when the surface of core forms coating.
Further, the thickness of the layer containing Si of the observation station of sample 1 and 2 is for about respectively 0.1 μm or so.
（Embodiment 2）
With regard to sample 5～8
Sample 5 is except using being that 85 mass %, Al are 5.5 mass % and Si is that 9.5 mass % constitute the soft magnetism for constituting by Fe
Property alloy powder as soft magnetic alloy powder beyond, make compressed-core sample with the method same with sample 1, carry out same
Evaluation.The results are shown in table 1.
Sample 6 is except using being that 85 mass %, Al are 5.5 mass % and Si is that 9.5 mass % constitute the soft magnetism for constituting by Fe
Property alloy powder as soft magnetic alloy powder beyond, make compressed-core sample with the method same with sample 2, carry out same
Evaluation.The results are shown in table 1.
In addition, sample 7 is except using being that 85 mass %, Al are 5.5 mass % and Si is that constituting for 9.5 mass % is constituted by Fe
Soft magnetic alloy powder as soft magnetic alloy powder beyond, make compressed-core sample with the method same with sample 3, enter
The same evaluation of row.The results are shown in table 1.
In addition, sample 8 is except using being that 85 mass %, Al are 5.5 mass % and Si is that constituting for 9.5 mass % is constituted by Fe
Soft magnetic alloy powder as soft magnetic alloy powder beyond, make compressed-core sample with the method same with sample 4, enter
The same evaluation of row.The results are shown in table 1.
As shown in table 1, in sample 5 and 6, it is thus identified that form the layer containing Si in crystal boundary.Therefore, in the surface shape of core
Into in the sample 6 for having coating, compared with the sample 5 for not forming coating, it is thus identified that the raising of the intensity more than 24%.
On the other hand, in sample 7 and 8, the layer containing Si is not formed in crystal boundary, even if be formed with the surface of core covering
The situation of cap rock（Sample 8）Under, the also raising of the intensity to as sample 6 drastically unconfirmed.
Industrial applicability
Magnetic core involved in the present invention is made up of core the soft-magnetic body composition in crystal boundary with the layer containing Si,
Coating is formed with the surface of the core, so as to play excellent intensity.Especially, in the feelings for making core be press-powder formed body
Under condition, even if can also obtain the magnetic core with enough intensity than relatively low shaping pressure, it is thus possible to reduce the bad of mould
Change, productive raising can be sought.And, by using the magnetic core of such manufacture, it is possible to reduce coil form electronic unit
Manufacturing cost.
The explanation of symbol
1 ... magnetic core
2 ... cores
10 ... coatings
Coating before 10a ... heat treatments
20 ... drum apparatus
21,22 ... non-retentive alloy particles
30,31 ... crystal boundaries
Claims (3)
1. a kind of magnetic core, it is characterised in that
It is to cover with the core being made up of soft-magnetic body composition and at least one of of surface for being formed in the core
The magnetic core of cap rock,
The soft-magnetic body composition has multiple non-retentive alloy particles and to be present in the non-retentive alloy intergranular
Crystal boundary,
The non-retentive alloy particle is Fe-Si-Cr systems alloying pellet,
In the crystal boundary, the layer containing Si is there are,
The thickness of the layer containing Si is 0.01～0.2 μm,
The layer containing Si is also present in the surface of the non-retentive alloy particle,
The layer containing Si for being present in the surface of the non-retentive alloy particle is Si-Cr composite oxide layers,
The Si-Cr composite oxide layers are the amorphous layers containing Si and Cr,
The coating is made up of glass composition,
The thickness of the coating is 3～25 μm.
2. magnetic core as claimed in claim 1, it is characterised in that
The layer containing Si is Si oxide skin(coating)s or Si composite oxide layers.
3. a kind of coil form electronic unit, it is characterised in that
With the magnetic core described in claim 1 or 2.
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| JP2013010481A JP2014143286A (en) | 2013-01-23 | 2013-01-23 | Soft magnetic material composition, method for producing the same, magnetic core, and coil type electronic component |
| JP2013-010481 | 2013-01-23 | ||
| JP2013-010845 | 2013-01-24 | ||
| JP2013010845A JP6382487B2 (en) | 2013-01-24 | 2013-01-24 | Magnetic core and coil type electronic components |
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| JP7128445B2 (en) * | 2018-09-05 | 2022-08-31 | Tdk株式会社 | Soft magnetic compositions, cores, and coil-type electronic components |
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| JP4010296B2 (en) * | 2003-11-20 | 2007-11-21 | 株式会社デンソー | Method for producing soft magnetic powder material |
| JP4548035B2 (en) * | 2004-08-05 | 2010-09-22 | 株式会社デンソー | Method for producing soft magnetic material |
| EP2055797A4 (en) * | 2006-08-23 | 2014-12-17 | Japan Science & Tech Agency | Iron-based alloy and process for producing the same |
| JP4845800B2 (en) * | 2007-04-26 | 2011-12-28 | 東邦亜鉛株式会社 | Wire wound inductor and manufacturing method thereof |
| JP2009117651A (en) * | 2007-11-07 | 2009-05-28 | Mitsubishi Materials Pmg Corp | High-strength soft-magnetic composite material obtained by compaction/burning, and method of manufacturing the same |
| JP5195669B2 (en) * | 2009-06-29 | 2013-05-08 | Ｔｄｋ株式会社 | Ferrite core and electronic components |
| JP4906972B1 (en) * | 2011-04-27 | 2012-03-28 | 太陽誘電株式会社 | Magnetic material and coil component using the same |
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