CN104347220A - Soft magnetic material composition and manufacturing method thereof, magnetic core, and coil type electronic component - Google Patents
Soft magnetic material composition and manufacturing method thereof, magnetic core, and coil type electronic component Download PDFInfo
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- CN104347220A CN104347220A CN201410369518.2A CN201410369518A CN104347220A CN 104347220 A CN104347220 A CN 104347220A CN 201410369518 A CN201410369518 A CN 201410369518A CN 104347220 A CN104347220 A CN 104347220A
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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
- H01F1/14—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 metals or alloys
- H01F1/20—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 metals or alloys in the form of particles, e.g. powder
- H01F1/22—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 metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—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 metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F27/00—Details of transformers or inductances, in general
- H01F27/24—Magnetic cores
- H01F27/255—Magnetic cores made from particles
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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
- H01F41/02—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 for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Abstract
The objective of the invention is to provide a soft magnetic material composition with excellent intensity, a manufacturing method thereof, a magnetic core, and a coil type electronic component. The soft magnetic material composition comprises a plurality of soft magnetic alloy particles and grain boundaries existing among the soft magnetic alloy particles. The soft magnetic material composition is characterized in that the soft magnetic alloy particles are composed of Fe-Si-M system soft magnetic alloy or Fe-Ni-Si-M system soft magnetic alloy, wherein M is selected from at least one of the group consisting of Cr, Al, Ti, Co and Ni, and glassy phases comprising Zn exist in the grain boundaries.
Description
Technical field
The present invention relates to soft-magnetic body composition and manufacture method, magnetic core and coil form electronic unit.
Background technology
Metallic magnetic gonosome its advantage compared with ferrite is to obtain high saturation magnetic flux density.As such a metallic magnetic elastomer material, as we all know there are the magnetic material employing non-retentive alloy etc.
Such non-retentive alloy expands the range of application as magnetic material, is thus expected to improve as mechanical strength when formed body.In patent documentation 1, propose the scheme that one employs the high magnetic material of the intensity of Fe-Si-M system soft-magnetic body alloy (wherein, M is the metallic element that is oxidized easier than iron).
But even if in the form proposed in patent documentation 1, intensity is still abundant not, also expects that mechanical strength improves further.Particularly in such magnetic material, the Si content existed in one side Fe-Si-M system soft-magnetic body alloy increases and more becomes high resistance high magnetic permeability, and mouldability gets over the problem worsened on the other hand.
Prior art document
Patent documentation
Patent documentation 1: Japan Patent No. 5082002 publications
Summary of the invention
Invent technical problem to be solved
The present invention studies in view of such present situation, its object is to provide a kind of soft-magnetic body composition and method processed, magnetic core and the coil form electronic unit with excellent in strength.
The means of technical solution problem
In order to achieve the above object, soft-magnetic body composition involved in the present invention, it is characterized in that: be the soft-magnetic body composition that there is multiple non-retentive alloy particle and be present in the crystal boundary between described non-retentive alloy particle, described non-retentive alloy particle is made up of Fe-Si-M system non-retentive alloy or Fe-Ni-Si-M system non-retentive alloy, described M is selected from least a kind in the middle of Cr, Al, Ti, Co and Ni, has the glassy phase comprising Zn at described crystal boundary.
In soft-magnetic body composition involved in the present invention, by having the glassy phase comprising Zn at the crystal boundary of non-retentive alloy particle, thus play excellent intensity.
Preferably, at described crystal boundary, Si is had further.
Preferably, at described crystal boundary, B is had further.
In addition, the manufacture method of soft-magnetic body composition involved in the present invention, is characterized in that: possess mixing soft-magnetic body alloy powder, sintered glass ceramics and jointing material and obtain the operation of mixture; By shaping for described mixture and obtain the operation of formed body; And heat the operation of described formed body.
Preferably, soft-magnetic body composition involved in the present invention obtained by the manufacture method of above-mentioned soft-magnetic body composition.
In addition, magnetic core involved in the present invention is made up of above-mentioned soft-magnetic body composition described in any one.
In addition, coil form electronic unit involved in the present invention has above-mentioned magnetic core.
As coil form electronic unit, be not particularly limited, the electronic units such as inductance component, EMC coil component, transistor component can be illustrated.Particularly suitably can be used in the dc-dc etc. of mobile phone etc.
Accompanying drawing explanation
Fig. 1 is the magnetic core involved by an embodiment of the invention.
Fig. 2 is the important part amplification sectional view of the magnetic core shown in Fig. 1.
Fig. 3 is the important part amplification sectional view of the magnetic core shown in Fig. 1, and is the schematic diagram of the existence representing the glassy phase comprising Zn.
Symbol description:
21 ... non-retentive alloy particle
30,31 ... crystal boundary
40 ... comprise the glassy phase of Zn
Embodiment
Below, based on execution mode shown in the drawings, the present invention is described.
The magnetic core of the coil form electronic component-use involved by present embodiment is by the shaping next shaping compressed-core of press-powder.Press-powder is shaping is carry out pressurizeing in mould by the material comprising soft magnetic alloy powder being filled in pressing machinery and with the pressure of regulation implementing compression forming and obtaining the method for formed body.
As the shape of the magnetic core involved by present embodiment, FT type, ET type, EI type, UU type, EE type, EER type, UI type, drum type, kettle type, cup type etc. can also be illustrated except the circular ring type shown in Fig. 1.By only coiling being wound in around this magnetic core by the regulation number of turns, thus just can obtain desired coil form electronic unit.
The soft-magnetic body composition of magnetic core involved by present embodiment of the coil form electronic component-use involved by present embodiment formed.
Soft magnetism composition involved by present embodiment, it is characterized in that: be the soft-magnetic body composition that there is multiple non-retentive alloy particle and be present in the crystal boundary between aforementioned non-retentive alloy particle, aforementioned non-retentive alloy particle is formed (wherein by Fe-Si-M system non-retentive alloy or Fe-Ni-Si-M system non-retentive alloy, aforementioned M is selected from least a kind in the middle of Cr, Al, Ti, Co and Ni), the glassy phase comprising Zn is had at aforementioned crystal boundary.
Soft-magnetic body composition involved according to the present embodiment, by meeting above-mentioned formation, thus can maintain magnetic characteristic (initial permeability μ i etc.) or resistivity well, and can improve intensity.
The crystal boundary 30 that soft-magnetic body composition involved by present embodiment has multiple non-retentive alloy particle 21 as shown in Figure 2 and is present between non-retentive alloy particle.
As shown in Figure 3, in the present embodiment, the glassy phase 40 comprising Zn is present in the crystal boundary 30 be formed between 2 particles or the crystal boundary 31 (triple point etc.) be present between more than 3 particles.Due to such existence comprising the glassy phase of Zn, the magnetic core involved by present embodiment plays excellent intensity.
When special soft-magnetic body composition involved by the glassy present embodiment being present in crystal boundary mutually comprising Zn, compared with when the glassy phase comprising Zn is not present in the soft-magnetic body composition of crystal boundary, the increase rate of intensity is preferably more than 3%, be more preferably more than 5%, more preferably more than 10%.
In the present embodiment, the glassy phase referred to mutually preferably primarily of amorphous glass and/or sintered glass ceramics formation.Be more preferably the phase formed primarily of sintered glass ceramics.Further, so glassy phase also can comprise the crystallization stemming from and form the composition of soft-magnetic body alloy or metal, oxide or the composite oxides of other compositions (adhesive or additive).
In addition, in the present embodiment, glassyly Zn is comprised mutually.So glassy mutually in, the existing forms of Zn is not particularly limited, such as, can be involved as the constitution element of above-mentioned amorphous glass and/or sintered glass ceramics, also can be scattered in as the oxide of the metal of Zn, Zn or the composite oxides etc. forming the composition of soft-magnetic body alloy and other compositions (adhesive and additive etc.) and Zn glassy mutually in and exist.
In addition, in the soft-magnetic body composition involved by present embodiment, preferably, boron (B) is had further at crystal boundary.More preferably, B is contained in the glassy phase comprising Zn.The existing forms of B is not particularly limited, such as, can be involved as the constitution element of above-mentioned amorphous glass and/or sintered glass ceramics, also can be scattered in as the oxide of B or the composite oxides etc. forming the composition of soft-magnetic body alloy and other compositions (adhesive and additive etc.) and B glassy mutually in and exist.
Further, in the soft-magnetic body composition involved by present embodiment, preferably, the concentration ratio non-retentive alloy granule interior of Zn and/or B in crystal boundary is high, and more preferably, Zn and/or B is not contained in non-retentive alloy granule interior in fact.
In addition, the mode that the glassy phase comprising Zn might not be necessary the surface integral covering non-retentive alloy particle exists, and also can be formed in the part on the surface of non-retentive alloy particle.
Further, in figure 3, for convenience's sake, represent the glassy phase 40 comprising Zn with graininess, but might not be necessary it is graininess, such as, also layeredly can be formed at the near interface of non-retentive alloy particle 21 with crystal boundary 30.
In the present embodiment, such as, as judging whether the glassy phase comprising Zn is present in the surface of non-retentive alloy particle and the not special restriction of method of crystal boundary, can be judged by mapping (mapping) image of resolving Zn.
Further, the differentiation of non-retentive alloy particle and crystal boundary can by using scanning transmission electron microscope (STEM) to observe magnetic core to carry out.Specifically, by STEM, photographed in the cross section of dielectric layer, and obtain bright field (BF) image.In this bright field image, using to be present between non-retentive alloy particle from non-retentive alloy particle and the region with the contrast different with this non-retentive alloy particle as crystal boundary.The judgement whether with different contrast can be estimated and be carried out, and also can be judged by the software etc. carrying out image procossing.
In addition, even if by determining observation station from the arbitrary section of magnetic core and carrying out EDS parsing or EPMA parsing, also can confirm that comprising the glassy of Zn is present in crystal boundary 30 mutually.In addition, resolve according to these, the CONCENTRATION DISTRIBUTION of the inside of alloying pellet or the various compositions on its surface can also be confirmed.In addition, resolve according to STEM, even if the phase being formed in the surface of alloying pellet is relevant to amorphous or crystalloid etc., also can specify.
Have again, in the soft-magnetic body composition involved by present embodiment, also can be judged by the method same with the situation of above-mentioned Zn whether various element is present in surface and the crystal boundary of non-retentive alloy particle about the element (B, Fe, Si, M etc.) beyond Zn.Further, about B, can resolve and judge whether various element is present in surface and the crystal boundary of non-retentive alloy particle by carrying out ICP parsing or EPMA.
In the soft-magnetic body composition involved by present embodiment, the content of zinc (Zn) is preferably 0.05 ~ 10.0 quality % relative to soft-magnetic body alloy 100 quality % with ZnO conversion, is more preferably 0.1 ~ 5.0 quality %.By meeting scope as described above, thus magnetic characteristic (particularly initial magnetic permeability mu i) or resistivity can be maintained well in the magnetic core involved by present embodiment, and improve mouldability (particularly rupture strength).
In the soft-magnetic body composition involved by present embodiment, the content of boron (B) relative to soft-magnetic body alloy 100 quality % with B
2o
3convert and be preferably 0.05 ~ 10.0 quality %, be more preferably 0.1 ~ 5.0 quality %.By meeting scope as described above, thus magnetic characteristic (particularly initial magnetic permeability mu i) or resistivity can be maintained well in the magnetic core involved by present embodiment, and improve mouldability (particularly rupture strength).
In the soft-magnetic body composition involved by present embodiment, when crystal boundary does not exist the glassy phase comprising Zn, there is the tendency that can not obtain enough intensity.In addition, the ratio of the glassy phase comprising Zn is had more to increase, the tendency that intensity more improves, but the tendency having that when too much magnetic characteristic (particularly initial magnetic permeability mu i) reduces.
Non-retentive alloy particle involved by present embodiment is made up of Fe-Si-M system non-retentive alloy or Fe-Ni-Si-M system non-retentive alloy.
Here, above-mentioned M is selected from least a kind in the middle of chromium (Cr), aluminium (Al), titanium (Ti), cobalt (Co) and nickel (Ni).
Especially in the present embodiment, non-retentive alloy particle is preferably Fe-Si-Cr system non-retentive alloy, Fe-Si-Al system non-retentive alloy or Fe-Ni-Si-Co system non-retentive alloy, Fe-Ni-Si-Co-M system non-retentive alloy, is more preferably Fe-Si-Cr system non-retentive alloy.
By using such non-retentive alloy particle, thus the soft-magnetic body composition involved by present embodiment can maintain magnetic characteristic (initial magnetic permeability mu i etc.) or resistivity and the mouldability that improves (particularly rupture strength) well.In addition, owing to can come shaping by lower shaping pressure when extrusion forming, therefore, it is possible to seek to alleviate the burden to mould further, can boost productivity.
When above-mentioned M is chromium (Cr), in Fe-Si-Cr system non-retentive alloy, preferably containing being scaled the silicon of 0.1 ~ 9 quality % with Si, being scaled the chromium of 0.1 ~ 15 quality % with Cr, surplus is made up of iron (Fe).More preferably, containing the silicon being preferably 1.4 ~ 9 quality %, being particularly preferably 4.5 ~ 8.5 quality % that converts with Si, in addition, containing the chromium being preferably 1.5 ~ 8 quality %, being particularly preferably 3 ~ 7 quality % that converts with Cr, preferred surplus is made up of iron (Fe).
When above-mentioned M is aluminium (Al), in Fe-Si-Al system non-retentive alloy, preferably, containing being scaled the silicon of 0.1 ~ 15 quality % with Si, being scaled the aluminium of 0.1 ~ 10 quality % with Al, surplus is made up of iron (Fe).
When above-mentioned M is cobalt (Co), in Fe-Ni-Si-Co system non-retentive alloy, preferably, containing be scaled with Si 0.1 ~ 3.0 quality % silicon, be scaled the nickel of 40.0 ~ 50.0 quality % with Ni, be scaled the cobalt of 0.1 ~ 5.0 quality % with Co, surplus is made up of iron (Fe).
The average crystallite particle diameter of the non-retentive alloy particle involved by present embodiment is preferably 30 ~ 60 μm.By making average crystallite particle diameter be above-mentioned scope, thus can easily realize the thin layer of magnetic core.
In the soft-magnetic body composition involved by present embodiment, on the surface (with the interface of crystal boundary 30) of non-retentive alloy particle 21, the oxide phase of the part comprising the composition forming non-retentive alloy particle can be formed with.
Such oxide is not particularly limited mutually, can be the oxide phase of the element comprised beyond oxygen and oxygen, also can be the composite oxides phase containing the element beyond two or more oxygen.In addition, as such oxide phase and composite oxides phase, the amorphous such as can enumerating the part comprising the composition forming non-retentive alloy particle is equal.
Further, in the present invention, oxide phase and composite oxides refer to the wide in range concept comprising amorphous phase, crystalline phase and their mixed phase mutually.
Here, when non-retentive alloy particle is Fe-Si-Cr system non-retentive alloy, above-mentioned oxide can be Si-Cr composite oxides phases many in the particle of Cr than non-retentive alloy particle 21 mutually.Si-Cr composite oxides are not particularly limited mutually, and the amorphous such as can enumerated containing Si and Cr is equal.
In addition, in the soft-magnetic body composition involved by present embodiment, above-mentioned oxide mutually can containing the glassy phase comprising Zn.As such oxide phase of glassy phase containing comprising Zn, such as, can enumerate amorphous fraction and the oxide phase that crystalline mixes or form the composition part chemical bond of non-retentive alloy particle with the composition such as Zn being contained in glassy phase and the composite oxides that formed are equal.
In addition, in the present embodiment, the mode that above-mentioned oxide is not necessarily necessary the surface integral covering non-retentive alloy particle is mutually formed, and also can be formed in a part for non-retentive alloy particle surface.In addition, the thickness of above-mentioned oxide phase can be uneven, and this composition also can be heterogeneous.
In addition, the surface of the non-retentive alloy particle involved by present embodiment, the presence or absence of above-mentioned oxide phase or its thickness can adjust according to the control of the heat treatment temperature and atmosphere gas etc. of the kind of the jointing material in the manufacture method of the alloy composition of non-retentive alloy particle, magnetic core described later (formed body) or its addition, other adding ingredients, formed body.
Further, in the soft-magnetic body composition involved by present embodiment, non-retentive alloy particle 21 directly can link via the non-retentive alloy particle 21 of above-mentioned oxide phase and phase neighbour.
Soft-magnetic body composition involved by present embodiment, except the constituent of above-mentioned soft-magnetic body alloying pellet, sometimes containing the composition such as carbon (C) and zinc (Zn).
Further, C is considered to stem from the organic compound ingredient used in the manufacture process of soft-magnetic body composition.In addition, Zn is considered to stem from the zinc stearate making an addition to mould when obtaining soft-magnetic body composition by press-powder is shaping in order to reduce the pulling out pressure of device.
The content of the carbon (C) in the soft-magnetic body composition involved by present embodiment is preferably less than 0.05 quality %, is more preferably 0.01 ~ 0.04 quality %.If the content of C is too much, then have the tendency of the enough intensity that can not obtain as magnetic core.
Further, in the soft-magnetic body composition involved by present embodiment, inevitable impurity can also be comprised except mentioned component.
In addition, as other execution mode, preferably, at the crystal boundary of soft-magnetic body composition, there is Si further.Thereby, it is possible to maintain high magnetic characteristic, and intensity can be improved further.Even also can obtain the enough intensity as magnetic core especially when shaping using lower briquetting pressure, thus also reduced the burden of mould, productivity ratio improves.
In the soft-magnetic body composition involved by present embodiment, Si is considered to be present in as the phase containing Si the crystal boundary 30 that is formed between 2 particles or is present in the crystal boundary 31 (triple point etc.) between the particle of more than 3.
By being present in crystal boundary mutually in this wise containing Si, even thus magnetic core involved by present embodiment also can obtain enough intensity as magnetic core when shaping using lower briquetting pressure.In addition, such effect can playing insulator by being present in crystal boundary containing Si.
Involved by present embodiment containing Si be mutually preferably Si oxide phase or Si composite oxides phase.As Si oxide phase and Si composite oxides phase, be not particularly limited, such as, can enumerate the amorphous phase containing Si, amorphous silicon, silicon dioxide, Si-M composite oxides etc.
In addition, in the soft-magnetic body composition involved by present embodiment, preferably, the surface (with the interface of crystal boundary 30) being present in non-retentive alloy particle 21 mutually further containing Si.
Such as, when non-retentive alloy particle is Fe-Si-Cr system non-retentive alloy, as containing Si be mutually preferably Si-Cr composite oxides phase.Si-Cr composite oxides are not particularly limited mutually, but many in the particle of Cr than non-retentive alloy particle 21.
Being made up of noncrystalline containing the mutually preferred of Si involved by present embodiment.Further, also can a part be made up of crystalline.
The thickness of the phase containing Si involved by present embodiment is preferably 0.01 ~ 0.2 μm, is more preferably 0.01 ~ 0.1 μm.
Further, the mode that the phase containing Si is not necessarily necessary the surface integral covering non-retentive alloy particle is formed, a part for non-retentive alloy particle surface also can be formed in.In addition, the thickness of the phase containing Si can be uneven, and this composition also can be heterogeneous.
The presence or absence of phase containing Si involved by present embodiment or its thickness can control according to the heat treatment temperature of the kind of the jointing material in magnetic core manufacture method described later or its addition, other adding ingredients, formed body and atmosphere gas etc.
Then, an example of the manufacture method of the magnetic core involved by present embodiment is described.
The magnetic core of present embodiment can make by the formed body comprising soft-magnetic body alloy powder and jointing material (adhering resin) is implemented heat treatment.Below, the preferred manufacture method with regard to the magnetic of present embodiment describes in detail.
Manufacture method involved by present embodiment preferably has: mixing soft-magnetic body alloy powder, lithium adding material and jointing material also obtain the operation of mixture; After making mixture dry and to obtain block dry body, form the operation of pelletizing by pulverizing this dry body; Mixture or pelletizing be shaped to the shape of the compressed-core that will make and obtain the operation of formed body; And by heating the formed body that obtains thus making jointing material harden and obtain the operation of compressed-core.
The magnetic core that manufacture method involved by present embodiment obtains can improve rupture strength especially.
Although obtain the reason of such effect and indefinite, the mechanism of the following stated can be thought.
In the operation of hot briquetting body, can think by making sintered glass ceramics be the condition of high temperature and occurring in the gap (grain boundary area) of non-retentive alloy particle softening, thus the combination between metallic particles become firm and the raising of the intensity of the magnetic core obtained.
As soft-magnetic body alloy powder, the soft-magnetic body alloy powder containing the alloying pellet be made up of Fe-Si-M system non-retentive alloy or Fe-Ni-Si-M system non-retentive alloy can be used.
The not special restriction of shape of soft magnetic alloy powder, but for until region, highfield still maintains the viewpoint of inductance, be preferably spherical or ellipsoid shaped.In the middle of these, for the viewpoint of intensity more increasing compressed-core, be preferably ellipsoid shaped.In addition, the average grain diameter of soft magnetic alloy powder is preferably 10 ~ 80 μm, is more preferably 30 ~ 60 μm.If average grain diameter is too small, then there is magnetic permeability step-down and the tendency declined as the magnetic characteristic of soft magnetic material, in addition, operation becomes difficult.On the other hand, if average grain diameter is excessive, then there is vortex flow loss and become large and the tendency of abnormal wear increase.
Soft magnetic alloy powder can be obtained by the method same with the modulator approach of known soft magnetic alloy powder.Now, aeroponics, water fog method, spining disk method etc. can be used to modulate.In the middle of these methods, in order to easily make the soft magnetic alloy powder with desired magnetic characteristic, preferred water fog method.
Sintered glass ceramics such as can enumerate pyrex and bismuth glass etc. as such sintered glass ceramics.
The addition of such sintered glass ceramics is preferably 0.1 ~ 10.0 mass parts relative to soft-magnetic body alloy powder 100 mass parts, is more preferably 0.1 ~ 5.0 mass parts.By meeting above-mentioned scope thus can effectively forming glassy phase at the crystal boundary of soft magnetism composition, and the intensity of magnetic core can be improved.
In addition, more preferably, above-mentioned sintered glass ceramics comprises Zn.By using such sintered glass ceramics, thus can effectively form at the crystal boundary of obtained soft magnetism composition the glassy phase comprising Zn, the intensity of magnetic core can be improved and improve magnetic characteristic (particularly initial magnetic permeability mu i).Zinc borosilicate glass and bismuth zinc glass etc. such as can be enumerated as such sintered glass ceramics comprising Zn.
In addition, the content of the Zn in above-mentioned sintered glass ceramics is preferably more than 10 % by mole, is more preferably 30 ~ 70 % by mole, more preferably 30 ~ 50 % by mole.
In addition, further preferably, above-mentioned sintered glass ceramics comprises boron (B).By using such sintered glass ceramics, thus the intensity of magnetic core can be improved and improve magnetic characteristic (particularly initial magnetic permeability mu i).As such sintered glass ceramics, such as, can enumerate pyrex and bismuth borate glass etc.
In addition, the content of the B in above-mentioned sintered glass ceramics is preferably more than 10 % by mole, is more preferably 15 ~ 30 % by mole.
As jointing material, known resin can be used, such as, can enumerate various organic polymer resin, silicone resin, phenolic resins, epoxy resin and waterglass etc.
Especially in the present embodiment, preferably use the jointing material comprising silicone resin as jointing material.By using silicone as jointing material, thus can effectively form phase containing Si at the crystal boundary of soft magnetism composition.Even the magnetic core be made up of such soft-magnetic body composition also can play enough intensity when shaping with lower briquetting pressure.
In the case, silicone resin can be used alone or combine to use with other jointing materials by jointing material.Further, be restricted to the viewpoint less than 0.05 quality % for the preferred content by the carbon (C) in soft-magnetic body composition, bond material preferably uses the jointing material formed primarily of silicone resin.If the content of the C in soft-magnetic body composition is too much, then the tendency that the intensity that there is the magnetic core obtained declines.
The addition of jointing material is different according to the magnetic characteristic of required magnetic core, preferably can add 1 ~ 10 weight portion relative to soft-magnetic body alloy powder 100 weight portion, is more preferably 3 ~ 9 weight portions relative to soft-magnetic body alloy powder 100 weight portion.If the addition of jointing material is too much, then there is magnetic permeability and to decline and loss becomes large tendency.On the other hand, if the addition of jointing material is very few, then there is the tendency being difficult to guarantee to insulate.
The addition of silicone resin is preferably 3 ~ 9 weight portions relative to soft-magnetic body alloy powder 100 weight portion.If the addition of silicone resin is very few, then has and be difficult to the phase formed containing Si and the tendency declined as the intensity of products formed at the crystal boundary of soft magnetism composition.
In addition, in aforementioned mixture or pelletizing, in the scope not hindering effect of the present invention, organic solvent can be added as required.
As organic solvent, as long as can dissolve jointing material, just there is no particular limitation, such as, can enumerate the various solvents such as toluene, isopropyl alcohol, acetone, methyl ethyl ketone, chloroform, ethyl acetate.
In addition, in aforementioned mixture or pelletizing, in the scope not hindering effect of the present invention, various additive, lubricant, plasticizer, thixotropic agent etc. can be added as required.
As lubricant, such as, can enumerate aluminum stearate, barium stearate, dolomol, calcium stearate, zinc stearate and strontium stearate etc.These lubricants can be used alone a kind or combinationally use two or more.In the middle of these lubricants, for the viewpoint that so-called resilience is little, preferably use zinc stearate as lubricant.
When making with lubricator, its addition is preferably 0.1 ~ 0.9 mass parts relative to soft-magnetic body alloy powder 100 weight portion, is more preferably 0.3 ~ 0.7 mass parts relative to soft-magnetic body alloy powder 100 weight portion.If lubricant is very few, then the demoulding of depositing after shaping can become difficulty and easily produce the tendency in shaping crack.On the other hand, if lubricant is too much, then can cause the decline of compact density, magnetic permeability reduces.
Particularly when using zinc stearate as lubricant, preferably adjust addition, the content making the zinc (Zn) in obtained soft-magnetic body composition is within the scope of 0.004 ~ 0.2 quality %.If the content of Zn is too much, then there is the tendency of the enough intensity that cannot obtain as magnetic core.
As the method obtaining mixture, be not particularly limited, mix soft-magnetic body alloy powder, jointing material and organic solvent by existing known method and obtain.Further, various adding material can be added as required.
The mixers such as such as pressure kneader, pulverizing mill, vibrating pulverizer, ball mill, V-Mixer can be used when mixing, or the comminutor such as fluidized granulation machine, rotation comminutor.
In addition, as the temperature and time of mixed processing, be preferably at room temperature about 1 ~ 30 minute.
As the method obtaining pelletizing, be not particularly limited, after drying composite, pulverized dried mixture obtain by existing known method.
As under the temperature and time of drying process is preferably about room temperature ~ 200 DEG C 5 ~ 60 minutes.
As required, lubricant can be added in pelletizing.Preferably 5 ~ 60 minutes are mixed add lubricant in pelletizing after.
As the method obtaining formed body, be not particularly limited, preferably, by existing known method, use the mould with the cavity of desired shape, mixture or pelletizing are filled in this cavity, and with the forming temperature of regulation and the briquetting pressure of regulation by this mixture compression forming.
Condition of molding in compression forming is not particularly limited, as long as suitably determine according to the shape and size of soft magnetic alloy powder, the shape of compressed-core, size and density etc.Such as, maximum pressure is generally about 100 ~ 1000MPa, and be preferably about 400 ~ 800MPa, the maximum pressure retention time is 0.5 second ~ about 1 minute.
If further, briquetting pressure is too low, then there is the tendency being difficult to seek by the shaping densification that brings and high magnetic permeability and being difficult to obtain enough mechanical strengths.On the other hand, if briquetting pressure time shaping is too high, then exist pressure apply effect there is saturated tendency and exist manufacturing cost increase and productivity ratio and economy can impaired tendency, in addition, there is mould and become easily deterioration and the tendency of durability reduction.
Forming temperature is not particularly limited, and is usually preferably about room temperature ~ 200 DEG C.Have again, the tendency that the density that there is forming temperature when improving shaping then formed body more rises, if but it is too high, the oxidation that then there is non-retentive alloy particle is promoted and the tendency of the performance degradation of the compressed-core obtained, in addition, manufacturing cost increase and productivity ratio and economy can be impaired.
As long as undertaken by known method shaping rear obtained formed body heat-treating methods, there is no particular limitation, generally speaking, preferably by using annealing furnace to carry out being heat-treated by shaping and formed body that is that be formed as arbitrary shape at an established temperature.
Treatment temperature during heat treatment is not particularly limited, and is usually preferably about 600 ~ 900 DEG C, is more preferably 700 ~ 850 DEG C.Treatment temperature during heat treatment is too high or too lowly all can there is the enough intensity that can not obtain as magnetic.
Heat treatment step preferably carries out under containing the atmosphere gas of aerobic.Here, containing the atmosphere gas of aerobic, there is no particular limitation, such as can enumerate atmospheric atmosphere gas (usually comprising the oxygen of 20.95%) or with the inert gas such as argon or nitrogen mix atmosphere gas etc.Preferably carry out under atmospheric atmosphere gas.By heat-treating under containing the atmosphere gas of aerobic, thus can effectively form phase containing Si at the crystal boundary of soft-magnetic body composition.
In addition, 5.50g/cm is preferably by its formed body density of the compressed-core obtained like this
3above.Formed body density is 5.50g/cm
3time above, exist and in the such various performances of high magnetic permeability, high strength, high magnetic core resistance, low core loss, all showed excellent tendency by the compressed-core of densification.
Above, be illustrated with regard to embodiments of the present invention, but the present invention is at all not limited to such execution mode, self-evident, as long as can implement with various form without departing from the spirit and scope of the present invention.
Such as, in the above-described embodiment, by carrying out mixture or pelletizing, press-powder is shaping manufactures magnetic core (compressed-core), but also can by said mixture being molded into flake and stackedly manufacturing magnetic core.In addition, extrusion molding shaping by wet type etc. formed body can also be obtained except dry formed.
In addition, in the above-described embodiment, formed containing the phase of Si at the crystal boundary of soft-magnetic body composition, therefore use silicone resin as jointing material, but also can substituted for silicon ketone resin and use silica gel or silica dioxide granule etc. containing Si composition as additive.
In addition, as required, also can by formed body glass coating or resin impregnated.Thus, the intensity of magnetic core can be improved further.
In addition, in the above-described embodiment, magnetic core involved by present embodiment is used as coil form electronic unit, but not special restriction, also can suitably use as the magnetic core of the various electronic units such as motor, Switching Power Supply, dc-dc, transformer, choking-winding.Especially the magnetic core as movement dc-dc is more suitable.
In addition, in the above-described embodiment, form magnetic core by soft-magnetic body composition involved in the present invention, but also can be made up of ferritic main body or other formed bodys of electronic unit soft-magnetic body composition involved in the present invention except magnetic core.
[embodiment]
Below, illustrate in greater detail the present invention by embodiment, but the present invention is not limited to these embodiments.
(embodiment 1)
about sample 1
[modulation of soft magnetic alloy powder]
First, the ingot casting of Fe monomer, Cr monomer and Si monomer, chunk (block) or pill (particle) is prepared.Then, become the Fe of 89.5 quality % with them, the mode of composition of Cr of the Si of 6.5 quality % and 4.0 quality % mixes, and be contained in the crucible be configured in water atomization plant.Then, in inert atmosphere gas, use and be arranged on the actuating coil of crucible outside, by high-frequency induction by more than crucible heating to 1600 DEG C, to dissolve and ingot casting, block or the particle mixed in crucible obtains and melt liquid.
Then, from be arranged on crucible nozzle ejection crucible in melt liquid, what meanwhile make the collision of high pressure (50MPa) current spray melts liquid and carries out quenching, produces the soft magnetic alloy powder (average grain diameter: 50 μm) be made up of Fe-Si-Cr system particle thus.
Carry out composition analysis by fluorescent x-ray analytic approach to obtained soft magnetic alloy powder, its result can confirm consistent with feed composition.
[making of compressed-core]
Add the silicone resin (eastern beautiful DOW CORNING organosilicon (company) system, trade name: SR2414LV) of 6 weight portions relative to obtained soft magnetic alloy powder 100 weight portion, these are at room temperature mixed 30 minutes by pressure kneader.Then, by mixture drying composite 20 minutes at 150 DEG C in atmosphere.In soft magnetic alloy powder after the drying relative to soft magnetic alloy powder 100 weight portion add 0.5 weight portion zinc stearate (day east change into system: Zinc Stearate) as lubricant, and mix 10 minutes by V-type blender.
Then, obtained mixture be molded into the square sample of 5mm × 5mm × 10mm and make formed body.Further, shaping pressure is 600MPa.By by the heat treated 60 minutes in an atmosphere at 750 DEG C of the formed body after pressurization, thus silicone resin is hardened and obtains compressed-core.
[various evaluation]
The observation > of < crystal boundary
First, compressed-core is cut off.Observed by scanning transmission electron microscope (STEM) with regard to this section, and carry out the differentiation of soft-magnetic body alloying pellet and crystal boundary.
<3 point bending strength test (rupture strength) >
To compressed-core sample, the regulation in accordance with JIS R1601 carries out 3 bending strength tests.3 bending strengths are maximum stress in bend (kg/mm when being placed in by test film on 2 fulcrums configuring at a certain distance and loading being put on 1 of the central authorities between fulcrum and fractureed
2).
< initial permeability (μ i) >
10 circle copper conductors are wound in compressed-core sample, use LCR tester (Hewlett-Packard's system, trade name: 4284A) to measure initial permeability μ i.As condition determination, mensuration frequency is 1MHz, and measuring temperature is 23 DEG C, and mensuration level is 0.4A/m.
about sample 2 ~ sample 7
Except value as shown in table 1 relative to soft magnetic alloy powder 100 weight portion in the making of compressed-core adds A like that, (commercially available zinc borosilicate sintered glass ceramics, average grain diameter is 1.5 μm to sample 2 ~ sample 7, and the coefficient of expansion is 63.0 × 10
-7, softening temperature is 590 DEG C, and crystallized temperature is 705 DEG C) beyond, make compressed-core sample with the method same with sample 1, and carry out same evaluation.Evaluation result represents in Table 1.
about sample 8 ~ sample 13
Sample 8 ~ sample 13 adds glass B (the commercially available zinc borosilicate sintered glass ceramics of Japan like that except value as shown in table 1 relative to soft magnetic alloy powder 100 weight portion in the manufacturing process of compressed-core, average grain diameter is 4.1 μm, and the coefficient of expansion is 57.0 × 10
-7, softening temperature is 661 DEG C, and crystallized temperature is 771 DEG C) outside, make compressed-core sample with the method same with sample 1, and carry out same evaluation.Evaluation result represents in Table 1.
about sample 14 ~ sample 19
Sample 14 ~ sample 19 except adding glass C (the bismuth sintered glass ceramics that Japan is commercially available relative to soft magnetic alloy powder 100 weight portion as become the value shown in table 1 in the manufacturing process of compressed-core, average grain diameter is 3.2 μm, and the coefficient of expansion is 67.8 × 10
-7, softening temperature is 578 DEG C, and crystallized temperature is 731 DEG C) beyond, make compressed-core sample with the method same with sample 1, and carry out same evaluation.Evaluation result represents in Table 1.
Further, each glass A ~ C composed as follows described in.Glass A comprises the B of 15 ~ 30 quality %
2o
3, the ZnO of 50 ~ 70 quality %, the SiO of 5 ~ 25 quality %
2, and other compositions.Glass B comprises the B of 15 ~ 30 quality %
2o
3, the ZnO of 50 ~ 70 quality %, the SiO of 5 ~ 25 quality %
2, and other compositions.Glass C comprises the Bi of 50 ~ 60 quality %
2o
3, 5 ~ 20 quality % B
2o
3, the ZnO of 10 ~ 20 quality %, the SiO of 1 ~ 10 quality %
2, and other compositions.
In addition, because rupture strength is different according to the formation metal of magnetic core or the kind of jointing material, therefore in the present embodiment with 11.7kg/mm
2be more than good.
[table 1]
The results verification that STEM observes and EDS resolves has the glassy phase comprising Zn at the crystal boundary of sample 2 ~ sample 19, there is not the glassy phase comprising Zn at the crystal boundary of sample 1.
As shown in table 1, confirm to have in the sample 2 ~ sample 19 of the glassy phase comprising Zn at crystal boundary, improve with the sample 1 phase specific strength that there is not the glassy phase comprising Zn.Confirm that its increase rate (increase rate relative to sample 1) is up to about 5 ~ 30%.
(embodiment 2)
about sample 21 ~ sample 26
Sample 21 ~ sample 26 is except using non-silicone-based resin (Nagase ChemteX Corporation system, trade name: DENATITE XNR 4338) as beyond tacky resin, make compressed-core sample with method same with sample 1, sample 2, sample 4, sample 7, sample 10 and sample 16 respectively, and carry out same evaluation.Evaluation result represents in table 2.
Further, due to rupture strength also can be different according to the kind forming the metal of magnetic core or jointing material, therefore in the present embodiment with 9.0kg/mm
2for well.
[table 2]
The results verification that STEM observes and EDS resolves has the glassy phase comprising Zn at the crystal boundary of sample 22 ~ sample 26, there is not the glassy phase comprising Zn at the crystal boundary of sample 21.
As shown in table 2, confirm to have in the sample 22 ~ sample 26 of the glassy phase comprising Zn at crystal boundary, compared with there is not the sample 21 of the glassy phase comprising Zn, intensity significantly improves.Particularly its increase rate (increase rate relative to sample 21) is up to about 5 ~ 30%.
Further, represented by table 2, do not observe Si in the crystal boundary essence of sample 22 ~ sample 26.By comparison sheet 2 and table 1, confirm by observing Si in crystal boundary essence thus rupture strength raising.In addition, in sample 2 ~ 19 and sample 22 ~ 26, be also observed at crystal boundary boron (B).Think this is because comprise boron (B) in glass A, B, C.
(embodiment 3)
about sample 31 ~ sample 36
Sample 31 ~ sample 36 except use by the Fe of 84.7 quality %, the Si of 9.7 quality % and 5.6 quality % Al form formed soft magnetic alloy powder as except soft magnetic alloy powder, make compressed-core sample with the method same with the sample 1 of embodiment 1, sample 2, sample 4, sample 7, sample 10 and sample 16, and carry out same evaluation.Evaluation result represents in table 3.
about sample 37 ~ sample 42
Sample 37 ~ sample 42 except use by Fe, the Ni of 44.0 quality % of 49.2 quality %, the Co of the Si of 2.3 quality % and 4.5 quality % form formed soft magnetic alloy powder as except soft magnetic alloy powder, make compressed-core sample with the method same with the sample 1 of embodiment 1, sample 2, sample 4, sample 7, sample 10 and sample 16, and carry out same evaluation.Evaluation result represents in table 3.
Further, due to rupture strength also can be different according to the kind forming the metal of magnetic core or jointing material, therefore, in the present embodiment, when the magnetic core be made up of Fe-Si-Al system non-retentive alloy, take rupture strength as 6.9kg/mm
2being more than good, when the magnetic core be made up of Fe-Ni-Si-Co system non-retentive alloy, take rupture strength as 11.0kg/mm
2be more than good.
[table 3]
The results verification that STEM observes and EDS resolves has at the crystal boundary of sample 32 ~ sample 36 and sample 38 ~ sample 42 the glassy phase comprising Zn, there is not at the crystal boundary of sample 31 and sample 37 the glassy phase comprising Zn.
As shown in table 3, in the sample 32 ~ sample 36 confirming to have at crystal boundary the glassy phase comprising Zn and sample 38 ~ sample 42, compared with the sample 31 that there is not the glassy phase comprising Zn and sample 37, intensity improves.
(embodiment 4)
In addition, confirm, when using Fe-Ni-Si-Cr non-retentive alloy, Fe-Ni-Si-Al non-retentive alloy, Fe-Si-Ti non-retentive alloy, Fe-Ni-Si-Ti non-retentive alloy, Fe-Si-Co non-retentive alloy, Fe-Si-Ni non-retentive alloy as alloy species, also to obtain the tendency same with embodiment 1 ~ 3.
From these results verifications, according to the present invention, even when the alloy species forming soft-magnetic body alloy composite changes, also can intensity be improved.
Claims (7)
1. a soft-magnetic body composition, is characterized in that:
The soft-magnetic body composition that there is multiple non-retentive alloy particle and be present in the crystal boundary between described non-retentive alloy particle,
Described non-retentive alloy particle is made up of Fe-Si-M system non-retentive alloy or Fe-Ni-Si-M system non-retentive alloy,
Described M is selected from least a kind in the middle of Cr, Al, Ti, Co and Ni,
At described crystal boundary, have the glassy phase comprising Zn.
2. soft-magnetic body composition as claimed in claim 1, is characterized in that:
At described crystal boundary, have Si further.
3. soft-magnetic body composition as claimed in claim 1 or 2, is characterized in that:
At described crystal boundary, have B further.
4. a manufacture method for soft-magnetic body composition, is characterized in that:
Possess:
Mixing soft-magnetic body alloy powder, sintered glass ceramics and jointing material and obtain the operation of mixture;
By shaping for described mixture and obtain the operation of formed body; And
Heat the operation of described formed body.
5. a soft-magnetic body composition, is characterized in that:
Obtained by manufacture method according to claim 4.
6. a magnetic core, is characterized in that:
Be made up of the soft-magnetic body composition described in any one in claims 1 to 3 and claim 5.
7. a coil form electronic unit, is characterized in that:
There is magnetic core according to claim 6.
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| JP2013157554A JP2015028985A (en) | 2013-07-30 | 2013-07-30 | Soft magnetic material composition, method for manufacturing the same, magnetic core, and coil type electronic component |
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| CN110880395A (en) * | 2018-09-05 | 2020-03-13 | Tdk株式会社 | Soft magnetic composition, magnetic core, and coil-type electronic component |
| CN112582125A (en) * | 2019-09-27 | 2021-03-30 | Tdk株式会社 | Soft magnetic alloy and electronic component |
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| CN111801752B (en) * | 2018-03-02 | 2024-03-19 | Tdk株式会社 | Magnetic core, method for manufacturing the same, and coil component |
| KR102155563B1 (en) * | 2018-11-23 | 2020-09-14 | 한국과학기술연구원 | Quenched powder core and methods for making same |
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| JP2010238914A (en) * | 2009-03-31 | 2010-10-21 | Mitsubishi Materials Corp | Method of producing high strength low loss composite soft magnetic material, and high strength low loss composite soft magnetic material |
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| CN1637962A (en) * | 2003-10-03 | 2005-07-13 | 松下电器产业株式会社 | Composite sintered magnetic material, its manufacturing method, and magnetic element using composite sintered magnetic material |
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| KR20150014860A (en) | 2015-02-09 |
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