CN104124021A - Soft magnetic body composition, magnetic core, coil-type electronic component, and manufacturing method of molded body - Google Patents
Soft magnetic body composition, magnetic core, coil-type electronic component, and manufacturing method of molded body Download PDFInfo
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- CN104124021A CN104124021A CN201410171562.2A CN201410171562A CN104124021A CN 104124021 A CN104124021 A CN 104124021A CN 201410171562 A CN201410171562 A CN 201410171562A CN 104124021 A CN104124021 A CN 104124021A
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Abstract
The present invention aims to provide a soft magnetic body composition and a manufacturing method thereof, by which molded products have enough strength and load to a mould during molding can be reduced, and a coil-type electronic component. 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 composed of Fe-Si-Cr alloy or Fe-Si-Al alloy. At least triple points of the crystal boundary have carrier particles (42), and the peripheries of the carrier particles (42) have Si phases.
Description
Technical field
The present invention relates to the manufacture method of soft-magnetic body composition, magnetic core, coil form electronic unit and formed body.
Background technology
Metallic magnetic gonosome is compared with ferrite magnetic body and is had advantages of and can obtain high saturation magnetic flux density.As such metallic magnetic gonosome, known have Fe-Si-Al to be associated gold or Fe-Si-Cr is associated gold etc.These metal magnetic styles are used (patent documentation 1 etc.) as the studied element body as electronic unit or magnetic core etc.
, the more miniaturization of electronic unit, the requirement of slimming improve in recent years.The miniaturization of electronic equipment, the requirement of slimming uprise, and make together therewith the magnetic core miniaturization that electronic unit uses, the requirement of slimming also improve.Yet, being accompanied by the miniaturization of magnetic core, the mechanical strength of the magnetic core particularly deficiency of rupture strength becomes technical problem increasingly.
Prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2000-30925 communique
Summary of the invention
Invent technical problem to be solved
The present invention is in view of such actual conditions, and its object is to provide a kind of manufacture method that can improve soft-magnetic body composition, magnetic core, coil form electronic unit and the formed body of the intensity of products formed.
The means of technical solution problem
The result that the soft-magnetic body composition that the inventor etc. just can improve the intensity of products formed is concentrated one's attention on research, discovery is by making to have at least triple point that is present in the crystal boundary of non-retentive alloy particle containing the carrier granular of Si phase on surface, thereby there is excellent magnetic characteristic, can improve the intensity (particularly rupture strength) of products formed, to such an extent as to complete the present invention.
; soft-magnetic body composition involved in the present invention; it is characterized in that: there are a plurality of non-retentive alloy particles and be present in the crystal boundary between described non-retentive alloy particle; described non-retentive alloy particle is associated gold or Fe-Si-Al by Fe-Si-Cr and is associated gold institute and is formed; at least triple point at described crystal boundary has carrier granular, in the surrounding of described carrier granular, has the phase containing Si.
Preferably, in the situation that make the average particulate diameter of described non-retentive alloy particle, be the 1st particle diameter d1, the 1st particle diameter d1 is preferably 5～50 μ m, more preferably 10～30 μ m.In addition, in the situation that make the average particulate diameter of described carrier granular, be the 2nd particle diameter d2, described the 2nd particle diameter d2 is preferably 0.05～2.0 μ m, more preferably 0.1～2.0 μ m.In the situation that in such scope, effect of the present invention is large.
In addition, the crystal boundary beyond described triple point, also can have described containing Si phase.
In addition, described can be the amorphous phase that contains Si containing Si mutually.
Magnetic core involved in the present invention is consisted of the soft-magnetic body composition described in above-mentioned any one.
Have, coil form electronic unit involved in the present invention has the element body consisting of the soft-magnetic body composition described in above-mentioned any one again.
In addition, the manufacture method of formed body involved in the present invention, it is characterized in that: be the method for manufacturing the formed body comprise the soft-magnetic body composition described in above-mentioned any one, after the surface of described carrier granular forms the coating that comprises Si, after soft magnetic alloy powder is mixed with the binding material that comprises silicone resin, obtain formed body, described formed body is implemented to heat treatment.
In addition, the manufacture method of formed body can have the operation of described formed body being carried out to vitreous coating.
Accompanying drawing explanation
Fig. 1 is the related magnetic cores of an embodiment of the invention.
Fig. 2 be the magnetic core shown in Fig. 1 want portion's amplification sectional view.
Fig. 3 is the amplification sectional view of the triple point shown in Fig. 2.
Fig. 4 is the amplification sectional view of the carrier granular shown in Fig. 3.
Fig. 5 carries out the skeleton diagram of the result of EDS parsing on the observation station V shown in Fig. 2.Have, the longitudinal axis is strength ratio again, and transverse axis is the degree of depth.
Symbol description:
21 ... non-retentive alloy particle
22 ... surface
30 ... crystal boundary
31 ... triple point
41 ... carrier granular
42 ... carrier granular main body
43 ... coating.
Embodiment
Below, based on execution mode explanation the present invention shown in the drawings.
The related coil form electronic component-use magnetic core of present embodiment is by press-powder moulding, to be carried out the compressed-core of moulding.Press-powder moulding is containing the material of soft magnetic alloy powder, with the exert pressure stipulated and implement the method that compression forming obtains formed body by filling bag in the mould of pressing machinery.
As the shape of the related magnetic core of present embodiment, except ring-like shown in Fig. 1, can also illustration FT type, ET type, EI type, UU type, EE type, EER type, UI type, drum type, crucible type, cup type etc.By just in time coiling being wound in to the surrounding of this magnetic core and can obtaining desired coil form electronic unit with the regulation number of turns.
The related coil form electronic component-use magnetic core of present embodiment is consisted of the related soft-magnetic body composition of present embodiment.
The related soft-magnetic body composition of present embodiment has the crystal boundary 30 of a plurality of non-retentive alloy particles 21 and soft-magnetic body composition as shown in Figure 2.
In the present embodiment, non-retentive alloy particle 21 is associated gold institute by Fe-Si-Cr and is formed.In the situation that non-retentive alloy particle 21 is golden for Fe-Si-Cr is associated, preferably contain with Cr be scaled 0.1～15 quality % chromium, with Si, be scaled the silicon of 0.1～9 quality %, surplus consists of iron.Preferably, more preferably contain with Cr be scaled 1.5～8 quality % particularly preferably 3～7 quality % chromium, with Si, be scaled the particularly preferably Si of 4.5～8.5 quality % of 1.4～9 quality %, surplus consists of iron.
By non-retentive alloy particle 21, meet above-mentioned composition, thereby the related soft-magnetic body composition of present embodiment obtains gratifying sintered density and excellent magnetic characteristic (initial permeability μ i etc.) and can obtain high rupture strength.In addition, owing to can carrying out moulding by lower briquetting pressure when the extrusion forming, therefore can seek, to further the alleviating of the burden of mould, can enhance productivity.In addition, by non-retentive alloy particle 21, meet above-mentioned composition, thereby be easily formed with the phase containing Si at crystal boundary 30.
In the related soft-magnetic body composition of present embodiment, except the constituent of above-mentioned non-retentive alloy particle 21, also comprise the compositions such as carbon and zinc.
Have, carbon is considered to come from the organic compound ingredient using in the manufacture process of soft-magnetic body composition again.In addition, zinc is considered to come from the zinc stearate that is added on mould when obtaining soft-magnetic body composition by press-powder moulding in order to reduce extracting of device to press.
The content of the carbon in the related soft-magnetic body composition of present embodiment is preferably less than 0.05 quality %, more preferably 0.01～0.04 quality %.
The content of the zinc in the related soft-magnetic body composition of present embodiment is preferably 0.004～0.2 quality %, more preferably 0.01～0.2 quality %.
Have again, in the related soft-magnetic body composition of present embodiment, except the above composition, can also comprise inevitable impurity.
In the present embodiment, as shown in Figures 2 and 3, non-retentive alloy particle 21 be formed with each other crystal boundary 30, crystal boundary 30 has and is present in more than 3 triple point between non-retentive alloy particle 21 31 on cross section, at triple point 31 at least, has carrier granular 41.As shown in Figure 4, carrier granular 41 has carrier granular main body 42 and is formed on its coating 43 around.
In the present embodiment, confirm in coating 43, to comprise containing Si phase.In addition, in the present embodiment, the crystal boundary 30 beyond triple point 31 also can comprise containing Si phase.Be present in mainly forming by having carrier granular 41 mutually containing Si of triple point 31, but the crystal boundary 30 beyond triple point 31 comprise mutually can be by the wanting thereby be imported into different from carrier granular 41 as described later containing Si.Have again, the kind containing Si phase that is present in the crystal boundary 30 beyond triple point 31 can be be present in carrier granular 42 surrounding coating 43 containing the mutually identical kind of Si, can be also different kinds.
There is no particular limitation for the kind of carrier granular main body 42, for example, can enumerate ceramic particle or metallic particles.Especially be preferably selected from one kind or two or more in the middle of aluminium oxide, zirconia, chromium.When especially particularly aluminium oxide is due to heat treatment, do not react with non-retentive alloy particle 21 and stable and preferably.
As containing Si phase, for example, can enumerate Si oxide phase or Si composite oxides phase.Oxide phase or composite oxides refer to the wide in range concept that comprises amorphous phase, crystalline phase and their mixing phase mutually.Particularly, as Si oxide phase and Si composite oxides phase, be not particularly limited, for example, can enumerate the amorphous phase, amorphous silicon phase, silicon dioxide phase, the Si-Cr composite oxides that comprise Si and equate.What present embodiment was related is preferably containing Si the amorphous phase that comprises Si mutually.Have again, also can a part be formed by crystalline.Containing Si, by being present in crystal boundary, bring into play the function of insulator.
In addition, coating 43 preferably forms to cover all modes in surface of carrier granular main body 42, but all modes in surface that might not be necessary to cover carrier granular main body 42 form, and can be formed on a surperficial part for carrier granular main body 42.In addition, the thickness of coating 43 can be inhomogeneous, and the composition of coating 43 also can heterogeneity.The thickness of coating 43 is preferably 0.005～0.2 μ m.
Non-retentive alloy particle 21 involved in the present invention and the average particulate diameter of carrier granular main body 42 are not particularly limited, but be the 1st particle diameter d1 at the average particulate diameter that makes non-retentive alloy particle 21, the average particulate diameter of carrier granular 42 is in the situation of the 2nd particle diameter d2, the 1st particle diameter d1 is preferably 5～50 μ m, more preferably 10～30 μ m; The 2nd particle diameter d2 is preferably 0.05～2.0 μ m, more preferably 0.1～2.0 μ m.In addition, d2/d1 is preferably d2/d1≤0.003.By becoming such scope, thereby sintered density improves and rupture strength also improves.
In the present embodiment, preferably at crystal boundary 30, having the phase containing Si, there is the tendency of the combination grow of 21 of particles in the little position of thickness t 1 of this crystal boundary 30, and the tendency that exists intensity to improve.Therefore, different from triple point 31, the crystal boundary 30 beyond the triple point is preferably the thickness of the degree that carrier granular 41 do not enter.
In the present embodiment, on the surface 22 of non-retentive alloy particle 21 (with the interface of crystal boundary 30), can be formed with as shown in Figure 3 the Si-Cr composite oxides phase that Cr is inner more than particle 21.There is no particular limitation mutually for Si-Cr composite oxides, for example, can enumerate the amorphous that contains Si and Cr and equate.
Have again, be formed on surperficial all modes that surface 22 Si-Cr composite oxides might not be necessary to cover non-retentive alloy particle 21 mutually and form, can form to cover the modes of non-retentive alloy particle 21 surface parts.
Be present in crystal boundary 30 beyond triple point 31 containing Si phase have or not or the heat treatment temperature of kind that its thickness can be by the binding material in the manufacture method of magnetic core described later (formed body) or its addition, other adding ingredients, formed body and atmosphere gas etc. are controlled.
In the present embodiment, the method that whether is present in mutually crystal boundary 30 and coating 43 containing Si as judgement is not particularly limited, for example, can judge by resolving mapping (mapping) image of Si.Below represent concrete method.
First, by using scanning transmission electron microscope (STEM) to observe magnetic core, distinguish non-retentive alloy particle 21 and carrier granular 42 and crystal boundary 30.Particularly, by STEM, take the arbitrary section of magnetic core, obtain bright field (BF) image.In this bright field image using be present between non-retentive alloy particle 21 and non-retentive alloy particle 21 and the region with the contrast not identical with this non-retentive alloy particle 21 as crystal boundary 30.In addition, will be present in the grain shape part of crystal boundary 30 or triple point 31 and the crystal boundary 30 of contrast and periphery or the discrepant part of triple point 31 as carrier granular 42.The judgement whether with different contrasts can be undertaken by visual, also can be judged by software that carries out image processing etc.
Have again, with regard to other elements such as Cr, Al, also can make map image and observe with same method.
In addition, by determining measuring point from the arbitrary section of magnetic core and carrying out EDS parsing or EPMA resolves, thereby can confirm to contain the phase containing Si in the coating 43 of surrounding that is present in crystal boundary 30, carrier granular 42.In addition about containing Si, be that amorphous or crystalline etc. also can be resolved to specify by EDS mutually.
An example of the magnetic core manufacture method that present embodiment is related then, is described.
The magnetic core of present embodiment can by comprising soft magnetic alloy powder, binding material (adhesive resin), the formed body with the carrier granular of coating implements heat treatment and makes.Preferred manufacture method with regard to the magnetic core of present embodiment elaborates below.
First, in the related manufacture method of present embodiment, prepare to have the carrier granular 41 of coating 43.For the surface in carrier granular main body 42 forms coating 43, for example carrier granular main body 42 be impregnated in the solution that is used to form coating 43.As dipping method, be not particularly limited, such as using the methods such as coating, mixing, spraying (spraying), dip-coating.
Raw material as coating is not particularly limited, and can use solution such as the methyl that comprises Si is class silicone resin, methylbenzene base system silicone resin and their sex change body etc.
After making solution be attached to the periphery of carrier granular main body 42 and being dried, at room temperature～300 ℃, heat-treat, coating is pre-fixed in carrier granular main body 42 around., so resulting carrier granular, soft magnetic alloy powder and adhesive mixed, obtain mixture thereafter.Mixture be dried and obtain block dry body after, by pulverize this dry body, form pelletizing thereafter., mixture or pelletizing be shaped to the shape of the compressed-core that will make, obtain formed body, obtained formed body is heated, make thus binder material hardens, obtain compressed-core thereafter.
By the prepared compressed-core of the related manufacture method of present embodiment, by the related soft-magnetic body composition of above-mentioned present embodiment, formed.
The shape of soft magnetic alloy powder has no particular limits, but from until region, highfield still maintains the viewpoint of inductance, is preferably spherical or ellipsoid shaped.In the middle of these, the viewpoint from the intensity of further increase compressed-core, is preferably ellipsoid shaped.In addition, the average particulate diameter of soft magnetic alloy powder is preferably 5～50 μ m.If average particulate diameter is too small, there is magnetic permeability step-down and as the tendency that the magnetic characteristic of soft magnetic material declines, in addition, process and become difficult.On the other hand, if average particulate diameter is excessive, exist vortex flow loss to become the tendency that large and abnormal loss increases.
Soft magnetic alloy powder can be same by the modulator approach with known soft magnetic alloy powder method obtain.Now, can modulate with gas atomization, water atomization and rotating disk method etc.In the middle of these, water atomization due to easily make have desired magnetic characteristic soft magnetic alloy powder and preferably.
As binding material, use the binding material that comprises silicone resin.By using silicone resin as binding material, thereby be effectively formed with the phase containing Si at the crystal boundary of soft-magnetic body composition.Even if the magnetic core consisting of such soft-magnetic body composition also has enough intensity in the situation that compress into row moulding with lower shaping.
Have again, in the scope that does not hinder effect of the present invention, can contain other binding materials.As other binding materials, such as enumerating various organic polymer resins, phenolic resins, epoxy resin and waterglass etc.
Binding material can be used separately silicone resin, or can combine to use with other binding materials.Have again, from preferably the carbon content soft-magnetic body composition being limited in to the viewpoint less than 0.05 quality %, the main silicone resin that preferably uses of binding material.If the carbon content in soft-magnetic body composition is crossed the tendency of the intensity decline that has at most resulting magnetic core.
The addition of binding material according to the characteristic of necessary magnetic core and difference preferably can be added 1～10 weight portion with respect to soft magnetic alloy powder 100 weight portions, more preferably adds 3～9 weight portions with respect to soft magnetic alloy powder 100 weight portions.If crossing, the addition of binding material exist at most magnetic permeability decline and loss to become large tendency.On the other hand, if crossing, the addition of binding agent there is at least the tendency that is difficult to guarantee insulation.
The addition of silicone resin is preferably 3～9 weight portions with respect to soft magnetic alloy powder 100 weight portions.If crossing at least, the addition of silicone resin there is the crystal boundary that is difficult to mutually be formed on soft-magnetic body composition containing Si, and the tendency declining as the intensity of products formed.
As carrier granular, use ceramic particle metallic particles.Wherein, be preferably selected from one kind or two or more in aluminium oxide, zirconia, chromium, particularly preferably aluminium oxide.
In addition, in aforementioned mixture or pelletizing, in not hindering the scope of effect of the present invention, can add organic solvent as required.
As organic solvent, as long as just can dissolve binding material and be not particularly limited, such as enumerating the various solvents such as toluene, isopropyl alcohol, acetone, methyl ethyl ketone, chloroform, ethyl acetate.
In addition, in aforementioned mixture or pelletizing, in not hindering the scope of effect of the present invention, can add various additives, lubricant, plasticizer, thixotropic agent etc. as required.
As lubricant, such as enumerating aluminum stearate, barium stearate, dolomol, calcium stearate, zinc stearate and strontium stearate etc.These can be used singly or in combination of two or more kinds to use.In the middle of these, from the little viewpoint of so-called resilience (springback), preferably use zinc stearate as lubricant.
In the situation that making with lubricator, its addition is preferably 0.1～0.9 weight portion with respect to soft magnetic alloy powder 100 weight portions, with respect to soft magnetic alloy powder 100 weight portions, is more preferably 0.3～0.7 weight portion.
Especially in the situation that using zinc stearate as lubricant, the zinc content of preferably take in resulting soft-magnetic body composition is adjusted addition as the mode of the scope of 0.004～0.2 quality %.
The operation that obtains formed body that present embodiment is related consists of following operation: the operation that obtains the mixture that comprises soft magnetic alloy powder, binding material, carrier granular; Pulverizing makes the dry body that mixture is dried and obtains the operation of pelletizing; To pelletizing moulding and obtain the operation of formed body.When mixing, such as using mixer or the fluidized granulation machines such as pressurization kneader, mixer (ア タ ラ イ タ), oscillating mill, ball mill, V-type blender, rotate the comminutors such as comminutor.
In addition, as the temperature and time of mixed processing, be not particularly limited, preferably at room temperature about 1～30 minute.
As the method that obtains pelletizing, be not particularly limited, after can being dried mixture by existing known method, pulverize dried mixture and obtain pelletizing.As the method that obtains formed body, be not particularly limited, preferably by existing known method, use the mould of the cavity with desired shape, filling mixture or pelletizing in this cavity, implement compression forming with the briquetting pressure of the forming temperature stipulated and regulation to this mixture.
There is no particular limitation for condition of molding in compression forming process, as long as do suitably to determine according to the shape of the shape and size of soft magnetic alloy powder, compressed-core, size and density etc.For example, maximum pressure is 100～1000MPa left and right conventionally, is preferably 400～800MPa left and right, and the time that remains on maximum pressure is about 0.5 second～1 minute.
In the related manufacture method of present embodiment, can comprise silicone-based resin by binding material and make briquetting pressure be reduced to above-mentioned maximum pressure.In addition,, even in the situation that reducing briquetting pressure like this, the crystal boundary that forms the soft-magnetic body composition of magnetic core also can form containing Si phase, thereby magnetic core becomes the magnetic core with sufficient intensity.Its result, can reduce manufacturing cost, and can enhance productivity and economy.
Have again, if briquetting pressure is too low, be difficult to densification and the high magnetic permeability seeking to be brought by moulding, and have the tendency that is difficult to obtain enough mechanical strengths.In addition, if briquetting pressure during moulding is too high, exist pressure to apply the tendency that effect is saturated, and have the tendency that manufacturing cost increase and production efficiency and economy can be impaired, in addition, have the mould tendency that easily deteriorated and durability declines.
There is no particular limitation for forming temperature, is conventionally preferably ℃ left and right, room temperature～200.Have again, the tendency that forming temperature while improving moulding more can exist the density of formed body to rise, if forming temperature is too high, promote the oxidation of non-retentive alloy particle, there is the tendency of the performance degradation of resulting compressed-core, in addition, manufacturing cost increase and production efficiency and economy are impaired.
As long as the formed body obtaining after moulding is carried out to heat-treating methods by known method, there is no particular limitation, generally speaking, preferably by heat-treating to carry out to be formed as the formed body of arbitrary shape through moulding with annealing furnace and under set point of temperature.
There is no particular limitation for treatment temperature during heat treatment, is conventionally preferably 600～900 ℃ of left and right, more preferably 700～850 ℃.
Heat treatment step is preferably carrying out containing under oxygen atmosphere gas.At this, there is no particular limitation containing oxygen atmosphere gas, for example, can enumerate atmospheric atmosphere condition (conventionally containing 20.95% oxygen), or with the inert gas such as argon and nitrogen mix atmosphere gas etc.Be preferably under atmospheric atmosphere gas.By heat-treating containing under oxygen atmosphere gas, can effectively form at the crystal boundary of soft-magnetic body composition the phase containing Si.
In addition, the compact density of such obtained compressed-core is preferably 5.70g/cm
3above.Compact density by densification to 5.70g/cm
3in the such various performances of high magnetic permeability, high strength, high magnetic resistance, low core loss, all there is excellent tendency in above compressed-core.
Have, the present invention is not limited to above-mentioned execution mode, self-evident again, in the scope that does not depart from aim of the present invention, can implement with various forms.
For example, in the above-described embodiment, non-retentive alloy particle 21 is associated gold by Fe-Si-Cr and forms, but also can be associated gold by Fe-Si-Al in the present invention, forms.In the situation that non-retentive alloy particle 21 is golden for Fe-Si-Al is associated, preferably contain the aluminium that is scaled 0.1～10 quality % with Al, with Si, be scaled the silicon of 0.1～15 quality %, surplus consists of iron.Can envision in this case and in the surface 22 shown in Fig. 3, be formed with Si-Al composite oxides phase.There is no particular limitation mutually for Si-Al composite oxides, for example, can enumerate the amorphous that contains Si and Al and equate.
The 2nd particle diameter d2 of carrier granular main body 42 that in addition, can be with the 1st particle diameter d1 of the non-retentive alloy particle 21 after burning till and after burning till becomes that the mode of desired value is suitably adjusted the average particulate diameter of the soft magnetic alloy powder before burning till, the average particulate diameter, firing condition etc. of the carrier granular of coating before forming before burning till.
In addition, in the above-described embodiment, as non-retentive alloy particle, use a kind of non-retentive alloy particle 21, but also can use multiple particle.For example, as non-retentive alloy particle, except aforesaid non-retentive alloy particle 21, can also comprise the auxiliary soft magnetic particles of holding in contrast less average grain diameter.The average grain diameter of auxiliary soft magnetic particles is for example 4～15 μ m.By comprising so auxiliary soft magnetic particles, can improve the overlapping characteristic of direct current of coil.
The composition of auxiliary non-retentive alloy particle can be with main non-retentive alloy Particle Phase with can be not identical yet.In addition, the content of auxiliary non-retentive alloy particle is in the situation that to make main non-retentive alloy particle 21 be that 100 mass parts are preferably below 2 mass parts.
In addition, in the above-described embodiment, by mixture or the moulding of pelletizing enforcement press-powder are manufactured to magnetic core (compressed-core), but also can be by said mixture being carried out to laminar moulding the stacked magnetic core of manufacturing.In addition, except dry formed, can also obtain formed body by wet type moulding, extrusion molding etc.
In the above-described embodiment, for crystal boundary at soft-magnetic body composition forms containing Si phase and uses silicone resin as binding material, but also can substituted for silicon ketone resin and use silica gel or silica dioxide granule etc. containing Si composition as additive.
Other also can carry out vitreous coating to formed body as required.Thus, can further improve the intensity of magnetic core.
In addition, in the above-described embodiment, the related magnetic core of present embodiment uses as coil form electronic unit, but not special restriction, and the magnetic core that also can be used as the various electronic units such as motor, Switching Power Supply, DC-DC converter, transformer, choking-winding suitably uses.Have again, in the above-described embodiment, by soft-magnetic body composition involved in the present invention, form magnetic core, but except magnetic core, also can be formed by soft-magnetic body composition involved in the present invention element body or other formed bodys of electronic unit.
[embodiment]
Below, by embodiment, illustrate in greater detail the present invention, but the present invention is not limited to these embodiment.
(embodiment 1)
about sample 2～8
[modulation of soft magnetic alloy powder]
First, prepare ingot casting, chunk (piece) or the ball material (particle) of Fe simple substance, Cr simple substance and Si simple substance.Then, take becomes Fe as 88.5 quality %, Cr as 5 quality % and Si mixes as the mode of the composition of 6.5 quality %, and is contained in the crucible being configured in water atomization plant.Then, in inert atmosphere gas, use the actuating coil be arranged on crucible outside by high-frequency induction by more than crucible heating to 1600 ℃, melting the ingot casting, chunk or the ball material that mix in crucible obtain fused solution.
Then, with from being arranged on fused solution in the nozzle ejection crucible of crucible simultaneously, the fused solution that makes high pressure (50MPa) current collide ejection carries out quenching, produces thus by Fe-Si-Cr and is associated the soft magnetic alloy powder (average particulate diameter is 30 μ m) that gold grain forms.
By fluorescent x-ary analysis, obtained soft magnetic alloy powder is carried out to composition analysis, its result can be confirmed consistent with feed composition.
[having the making of the carrier granular of coating around]
First, according to each sample and the AES-12 particle (alumina particle) of different average particulate diameters is prepared as carrier granular.Then,, as the raw material of coating, prepare poly-alkylsiloxane TSR127B (Mai Tu new high-tech material Japanese firm system).Then the TSR127B that, mixes 12 mass parts (solid part 6 mass parts) with respect to AES-21 particle 100 mass parts.Then, at 80 ℃, carry out pre-hardening., with the Filter paper filtering of #120, remove thick particle, make the carrier granular that has the coating that comprises poly-alkylsiloxane around thereafter.
[making of compressed-core]
With respect to obtained soft magnetic alloy powder 100 weight portions add around have carrier granular 0.5 weight portion (test piece number (Test pc No.) 2～7) of the coating that comprises poly-alkylsiloxane and silicone resin (eastern beautiful DOW CORNING organosilicon (company) system: SR2414LV) 6 weight portions, these are at room temperature mixed 30 minutes by pressurization kneader.Then, by mixture in air at 150 ℃ drying composite 20 minutes.In dried soft magnetic alloy powder, with respect to soft magnetic alloy powder 100 weight portions, add zinc stearate (Nitto Kasei Co., Ltd's system: Zinc Stearate) as lubricant, and mixed 10 minutes by V-type blender of 0.5 weight portion.
Then, obtained mixture be molded into the square sample of 5mm * 5mm * 10mm and make formed body.Have, moulding is pressed as 600MPa again.By by the formed body after pressurization at 745 ℃ in atmosphere heat treated 30 minutes, thereby silicone resin is hardened and obtains compressed-core.
[various evaluation]
<STEM observes and EDS resolves >
First, cut off compressed-core.With regard to this section, by scanning transmission electron microscope (STEM), observed.Thus, carry out distinguishing of non-retentive alloy particle, carrier granular and crystal boundary.Confirm thus having or not of carrier granular on triple point.Then, by image analysis, measure the average particulate diameter d1 of non-retentive alloy particle and the average particulate diameter d2 of carrier granular.Then, optional observation station V as shown in Figure 2, carries out EDS analysis with the EDS device that is attached to STEM.EDS analysis result is represented as skeleton diagram in Fig. 5.Fig. 5 is the skeleton diagram of the situation of carrier-free particle in observation station.Have, the longitudinal axis of Fig. 5 is by the strength ratio of measuring the characteristic X-ray obtaining again.In addition, by changing observation station, in observation station, there is the EDS of the situation of carrier granular to resolve, thereby confirm that the coating comprising containing Si phase is present in carrier granular around.
< three-point bending strength test (rupture strength) >
Compressed-core sample is carried out to three-point bending strength test according to the regulation of JIS R1601.Three-point bending strength is that test film is placed at a certain distance on 2 fulcrums of configuration, and 1, the central authorities between fulcrum add loading and maximum stress in bend (kg/mm while fractureing
2).In embodiment 1, with 14.0kg/mm
2be more than good.The results are shown in table 1.
< initial permeability (μ i) >
The 10 circle copper conductors of reeling on compressed-core sample, are used LCR measuring instrument (4284A of Hewlett-Packard) to measure initial permeability μ i.As condition determination, mensuration frequency is 1MHz, and measuring temperature is 23 ℃, and mensuration level is 0.4A/m.In embodiment 1, the μ i under 1MHz be take more than 40 as good.The results are shown in table 1.
< sintered density Ds>
Sintered density Ds passes through to measure size and the quality of compressed-core sample, and calculates quality W/ volume V and try to achieve (unit: g/cm
3).In embodiment 1, with 5.70g/cm
3for well.The results are shown in table 1.
[table 1]
The confirmation of STEM observed result, the soft-magnetic body composition of sample 2～8 is the non-retentive alloy particles of the average particulate diameter d1 shown in table 1.In addition, can confirm to have the carrier granular of the average particulate diameter d2 shown in table 1 on the crystal boundary triple point of sample 2～8.Have, EDS analysis result shows to confirm that the crystal boundary at sample 2～8 is formed with the phase containing Si again.Have again, confirm that the coating (thickness is 0.005～0.2 μ m) comprising containing Si phase is present in carrier granular around.
Have again, STEM observed result, the crystal boundary at soft-magnetic body composition in sample 2～8 is confirmed the amorphous phase that comprises Si.In addition, at the particle surface of soft-magnetic body composition, confirm the amorphous layer that comprises Si and Cr.
In the sample 2～8 that comprises carrier granular, obtain all equal gratifying soft-magnetic body compositions of rupture strength, initial permeability, sintered density.
about sample 11
Except making the average particulate diameter of soft magnetic alloy powder, be 10 μ m, to make compressed-core sample with the same method of sample 5, carry out same evaluation.The results are shown in table 1.
STEM observes and EDS resolves result and sample 2～8 are same.In addition, in sample 11, obtain all equal gratifying soft-magnetic body compositions of rupture strength, initial permeability, sintered density.
(comparative example 1)
about sample 1
In sample 1, except not comprising carrier granular, all with the method making compressed-core sample same with sample 4, carry out same evaluation.The results are shown in table 1.
The result that STEM observes and EDS resolves is all same with sample 4 except not there is not carrier granular.But the soft-magnetic body composition obtaining can not get enough rupture strengths.
about sample 21
Except with respect to soft magnetic alloy powder 100 weight portions, add 0.5 weight portion AES-12 substitute around have coating carrier granular and as the carrier granular without coating around, method making compressed-core sample with same with sample 4, carries out same evaluation.The results are shown in table 1.
STEM observed result and sample 2～8 are same.EDS analysis result is also that to be present in carrier granular same with sample 2～8 around except confirming to comprise coating containing Si phase.
The soft-magnetic body composition obtaining, its rupture strength and sample 1 equal extent, can not get enough rupture strengths.In addition, sintered density and initial permeability decline.
(embodiment 2, comparative example 2)
about sample 31,32
Sample 31,32 forms formed soft magnetic alloy powder as soft magnetic alloy powder except using by the Si of the Fe of 85 quality %, the Al of 5.5 quality % and 9.5 quality %, to make compressed-core sample with sample 1 and the same method of sample 4, carry out same evaluation.The results are shown in table 2.
[table 2]
STEM observed result can be confirmed to have carrier granular on the crystal boundary triple point of sample 32.In addition, EDS analysis result can be confirmed to be formed with the phase containing Si at the crystal boundary of sample 31,32.In addition, confirm that the coating comprising containing Si phase is present in carrier granular around.
In addition, STEM observed result, in sample 31,32, confirms at the crystal boundary of soft-magnetic body composition the amorphous phase that comprises Si.In addition, at the particle surface of soft-magnetic body composition, confirm the amorphous layer that comprises Si and Al.
Use around has containing the sample 32 of the carrier granular of Si phase and compares with the sample 31 that does not use carrier granular and can confirm that rupture strength improves.
Claims (9)
1. a soft-magnetic body composition, is characterized in that:
There are a plurality of non-retentive alloy particles and be present in the intergranular crystal boundary of described non-retentive alloy,
Described non-retentive alloy particle is associated gold or Fe-Si-Al by Fe-Si-Cr and is associated gold institute and is formed,
At least triple point at described crystal boundary has carrier granular, in the surrounding of described carrier granular, has the phase containing Si.
2. soft-magnetic body composition as claimed in claim 1, is characterized in that:
In the situation that make the average particulate diameter of described non-retentive alloy particle, be the 1st particle diameter d1, the 1st particle diameter d1 is 5～50 μ m.
3. soft-magnetic body composition as claimed in claim 1 or 2, is characterized in that:
In the situation that make the average particulate diameter of described carrier granular, be the 2nd particle diameter d2, described the 2nd particle diameter d2 is 0.1～2.0 μ m.
4. soft-magnetic body composition as claimed in claim 1 or 2, is characterized in that:
Crystal boundary beyond described triple point also has the phase containing Si.
5. soft-magnetic body composition as claimed in claim 1 or 2, is characterized in that:
The described Si that contains comprises the amorphous phase that contains Si mutually.
6. a magnetic core, is characterized in that:
By the soft-magnetic body composition described in any one in claim 1～5, formed.
7. a coil form electronic unit, is characterized in that:
There is the element body being formed by the soft-magnetic body composition described in any one in claim 1～5.
8. a manufacture method for formed body, is characterized in that:
The method of manufacturing the formed body comprise the soft-magnetic body composition described in any one in claim 1～5,
Surface at described carrier granular forms after the coating that comprises Si, obtains formed body after soft magnetic alloy powder is mixed with the binding material that comprises silicone resin, and described formed body is heat-treated.
9. the manufacture method of formed body as claimed in claim 8, is characterized in that:
Also there is the operation of described formed body being carried out to vitreous coating.
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| JP2013092892A JP2014216495A (en) | 2013-04-25 | 2013-04-25 | Soft magnetic material composition, magnetic core, coil type electronic component, and process of manufacturing compact |
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