CN104217834A - Soft magnetic powder compound, core and electric reactor - Google Patents

Soft magnetic powder compound, core and electric reactor Download PDF

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Publication number
CN104217834A
CN104217834A CN201410241756.5A CN201410241756A CN104217834A CN 104217834 A CN104217834 A CN 104217834A CN 201410241756 A CN201410241756 A CN 201410241756A CN 104217834 A CN104217834 A CN 104217834A
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soft magnetic
magnetic powder
weight
phosphoric acid
powder
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CN104217834B (en
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大岛泰雄
纲川昌明
赤岩功太
田村泰治
中津良
二宫亨和
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Tamura Corp
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Tamura Corp
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Priority claimed from JP2013116921A external-priority patent/JP6346412B2/en
Priority claimed from JP2013161678A external-priority patent/JP6339776B2/en
Priority claimed from JP2013246721A external-priority patent/JP6042792B2/en
Application filed by Tamura Corp filed Critical Tamura Corp
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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
    • 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
    • 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

Abstract

The invention provides a low-noise electric reactor, soft magnetic compound for the low-noise electric reactor and a core capable of improving hardness of an insulation layer of soft magnetic powder and effectively preventing noise. The soft magnetic powder is mixed with condensed phosphoric acid metal compounds with 0.25 wt% to 2.0 wt%, so a wrapped layer made from the condensed phosphoric acid metal compounds is formed on the periphery of the soft magnetic powder; and preferentially, condensed aluminum phosphate, especially trimerization aluminum phosphate is chosen.

Description

Soft magnetic powder composition, core, reactor
Technical field
The present invention relates to the manufacture method of lower-noise reactor and high strength reactor, the soft magnetic powder composition being suitable for this lower-noise reactor and high strength reactor, core and core.
Background technology
Employ choke in the control power supplies such as OA equipment, solar power system, automobile, uninterrupted power supply, as its core, use FERRITE CORE or compressed-core.Among those, there is the little shortcoming of saturation flux density in FERRITE CORE.On the other hand, the compressed-core of shaping for metal dust making had the saturation flux density higher than soft magnetic ferrite, so direct current overlapping features is excellent.
In view of the raising requirement such as energy exchange efficiency and low heat release, compressed-core needs to have the little magnetic characteristic of energy loss in the magnetic characteristic and change in magnetic flux density that can obtain larger magnetic flux density under less externally-applied magnetic field.
When compressed-core is used for AC magnetic field, produce the energy loss being referred to as iron loss (Pc).As shown in Equation 1, this iron loss can be expressed as magnetic hysteresis loss (Ph) and eddy current loss (Pe) sum, and what mainly become problem is magnetic hysteresis loss and eddy current loss.
Magnetic hysteresis loss is directly proportional to operating frequency, and square being directly proportional of eddy current loss and operating frequency.Therefore, play a leading role at low-frequency region magnetic hysteresis loss, play a leading role in the eddy current loss of high-frequency region.Require that compressed-core has the magnetic characteristic of the generation reducing this iron loss.
Pc=Ph+Pe, Ph=Kh × f, Pe=Ke × f 2formula 1
Kh: the coefficient of hysteresis, Ke: eddy current loss coefficient, f: frequency
In order to reduce the magnetic hysteresis loss of compressed-core, making the movement of magnetic wall become easily, can be realized by the coercive force reducing soft magnetic powder particle for this reason.By reducing this coercive force, the raising of initial permeability and the minimizing of magnetic hysteresis loss can be realized.
On the other hand, as shown in Equation 2, the ratio resistance of eddy current loss and core is inversely proportional to.
Ke=k1 (Bm 2t 2)/ρ ... formula 2
K1: coefficient, Bm: magnetic flux density, t: particle diameter (being thickness when sheet material), ρ: ratio resistance
The compressed-core having carried out high density shaping has high magnetic flux density, can play excellent magnetic characteristic.
In addition, choke is employed in order to make the output waveform of Switching Power Supply etc. level and smooth.Along with high performance and the multifunction of various electronic equipment, the core for the choke used wherein also requires that characteristic variations is little when big current.Specifically, need a kind of to there is excellent direct current overlapping features and the core of low loss property.As this core, employed FERRITE CORE, compressed-core in the past.Wherein, the compressed-core made by the powder of noncrystalline non-retentive alloy (amorphous non-retentive alloy) have direct current overlapping features excellent, lose few characteristic.
In order to use these noncrystalline soft magnetic powders to make compressed-core, noncrystalline soft magnetic powder being mixed with low-melting glass and adhesion resin etc., by after its mixture compression forming under normal temperature or high temperature, obtained formed body being heat-treated.In addition, low-melting glass has the high problem of cost, thus replaces low-melting glass, proposes and use aluminium dihydrogen phosphate as insulating coating to realize the improvement of insulation property as shown in patent documentation 3; Attempt using the phosphate or phosphate cpd that contain aluminium to obtain high-insulativity and magnetic flux density as shown in patent documentation 4.But these prior aries are all conceived to improve insulation property, are not improve core intensity or low noise turns to object.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 6-176914 publication
Patent documentation 2: Japanese Unexamined Patent Publication 2008-192897 publication
Patent documentation 3: Japanese Unexamined Patent Publication 2003-272911 publication
Patent documentation 4: Japanese Unexamined Patent Publication 2005-113258 publication
Summary of the invention
The problem that invention will solve
Solar power systems etc. mostly are the situation of component configuration in indoor, there is the problems such as noise, as the material of the compressed-core of the reactor wherein used, the less Fe-6.5Si alloy powder, FeSiAl alloy (sendust) etc. of magnetostriction is suitable.But, even if use these materials, if the intensity of the insulating barrier of compressed-core is insufficient, the large problem of noise also can be there is.That is, even if reduce the magnetostriction of powder core, make vibrate powder by the excitation field in driving, thus also can produce noise.Therefore, need to improve the dhering strength of insulating barrier and powder, improve the hardness of insulating barrier to reduce vibrate powder.
As this low noise technology, describe in patent documentation 1 and the average hardness of sendust powder core brought up to more than Hv350 or compression failure load is brought up to 6.0 tons/cm 2above (more than 600MPa).In the prior art, as the means improving magnetic core hardness, the addition of the waterglass mixed in sendust powder is made to be 1 % by weight ~ 3 % by weight (wt%).
But the technology of patent documentation 1 prevents the crackle in Magnaglo from producing the noise caused, and do not prevent the noise under flawless generation state.That is, the noise in the reactor such as choke is not only occur when crackle produces, even if in flawless situation, the powder forming magnetic core vibrates because of excitation field, thus also can produce noise.The vibration that this magnetic core powder causes to utilize the method for adding this patent documentation 1 of waterglass in magnetic core powder to prevent.Particularly, as recorded in patent documentation 1, also there is following problems: if improve hardness and increase the addition of waterglass, then the magnetic characteristic of obtained reactor reduces.
In addition, form forming magnetic core is ring-type by the reactors such as choke, thus, be average hardness is 6.0 tons/cm at more than Hv350 or compression failure load only by making the hardness of formed body 2above, then noise suppression is insufficient.
On the other hand, as low noise technology, describe in patent documentation 2 by FeSi alloy to be mixed the technology improving duty factor with pure iron.But, though improve duty factor, to reduce empty wall effective, but can occur to lose the problem increased by adding pure iron.That is, although can use in the big current reactor purposes that frequency is low, lose in the solar power generation purposes that frequency ratio is higher high, cannot use.In addition, even if reduce empty wall, suppress the effect of the vibrate powder formed by excitation field also little.
In addition, the aluminium dihydrogen phosphate used in the technical scheme of patent documentation 3 is by Al 2o 33P 2o 56H 2the water miscible superphosphate that the rational formula of O represents, it is by showing sclerosis associativity with the reaction of aggregate or the dehydrating condensation caused by heating and the crystalline transition caused by high-temperature heating etc.On the other hand, its moisture absorption is very high, also demonstrates violent reaction with the steam of surrounding at normal temperatures, therefore operating difficulties.In addition, exist and make the problems such as formed body density reduction because of the expansion caused by moisture absorption, not easily volume production.In addition, if the hardness of soft magnetic powder is high, during compression forming, powder Anchoring Effect is each other weak, can produce the problem of the reduction of formed body intensity, core breakage.
The technical scheme recorded in patent documentation 4 is mixed by phosphate cpd metallizing thing and adds in soft magnetic powder, produces chemical conversion reaction, thus can improve the adaptation of the chemical composition coating of metal powder surface on the surface of soft magnetic powder; But then, if suitably can not control the mixing of phosphate cpd metallizing thing, the chemical conversion reaction on soft magnetic powder surface is insufficient, cannot obtain the effect at initial stage.In addition, remaining at phosphate or phosphate cpd Free Phosphoric Acid unreacted, so remaining free phosphoric acid also exists and causes powder to have hygroscopic problem.
The present invention proposes in order to the problem solving above-mentioned prior art.The object of the present invention is to provide the lower-noise reactor that a kind of hardness, effectively restraint speckle that can improve the insulating barrier of soft magnetic powder occurs; High strength reactor; Soft magnetic powder composition; Core; And the manufacture method of core.
In addition, the object of the present invention is to provide that mechanical strength is high, the core of the compressed-core of excellent in magnetic characteristics and manufacture method thereof.In addition, the soft magnetic powder composition used to obtain this excellent core is provided also to be an object of the present invention.
For solving the scheme of problem
In order to achieve the above object, the feature of soft magnetic powder composition of the present invention is, soft magnetic powder is mixed with the condensed phosphoric acid metallic compound relative to described soft magnetic powder being 0.25 % by weight ~ 2.0 % by weight, around this soft magnetic powder, defines the coating of described condensed phosphoric acid metallic compound.
In addition, following formation can also be had.
(1) described condensed phosphoric acid metallic compound is preferably condensation of aluminum phosphate.
(2) as condensation of aluminum phosphate, single component or the mixture of both of aluminium triphosphate or aluminium metaphosphate is preferably used.
(3) in condensed phosphoric acid metallic compound, alkaline matter can be added as hardening accelerator.As this alkaline matter, Al can be used 2o 3, SiO 2, MgO, Mg (OH) 2, CaO, Ca (OH) 2, asbestos, talcum, at least one in flying dust.In addition, hardening accelerator preferably with the addition of 10 % by weight ~ 30 % by weight relative to condensed phosphoric acid metallic compound.
Employ above-mentioned soft magnetic powder composition core or employ surface the core of soft magnetic powder that covers by silicon dioxide layer be also one of mode of the present invention, wherein, this silicon dioxide layer comprise relative to soft magnetic powder be 0.25 % by weight ~ 2.0 % by weight condensed phosphoric acid metallic compound.Employ the lower-noise reactor of any one core in them, high strength reactor, these cores manufacture method be also one of mode of the present invention.
In addition, the feature of soft magnetic powder composition of the present invention is, is mixed by soft magnetic powder, further mix insulation micro mist with the condensed phosphoric acid metallic compound relative to described soft magnetic powder being 0.20 % by weight ~ 0.80 % by weight.The coating comprising described condensed phosphoric acid metallic compound is defined around this soft magnetic powder.
In addition, following formation can also be had.
(1) described insulation micro mist is preferably relative to described soft magnetic powder mixing 0.1 % by weight ~ 0.6 % by weight.As this insulation micro mist, Al can be used 2o 3.
(2) described condensed phosphoric acid metallic compound is preferably condensation of aluminum phosphate.
(3) as condensation of aluminum phosphate, single component or the mixture of both of aluminium triphosphate or aluminium metaphosphate is preferably used.
(4) alkaline matter can be added as hardening accelerator in condensed phosphoric acid metallic compound.As this alkaline matter, Al can be used 2o 3, SiO 2, MgO, Mg (OH) 2, CaO, Ca (OH) 2, asbestos, talcum, at least one in flying dust.In addition, hardening accelerator preferably adds 10 % by weight ~ 30 % by weight relative to condensed phosphoric acid metallic compound.
Employ above-mentioned soft magnetic powder composition core or employ surface the core of soft magnetic powder that covers by silicon dioxide layer be also one of mode of the present invention, wherein, this silicon dioxide layer comprise relative to soft magnetic powder be 0.20 % by weight ~ 0.75 % by weight condensed phosphoric acid metallic compound.Employ the lower-noise reactor of any one core in them, high strength reactor, these cores manufacture method be also one of mode of the present invention.
In addition, the feature of soft magnetic powder composition of the present invention is, in noncrystalline soft magnetic powder, mix its condensed phosphoric acid metallic compound of 0.25 % by weight ~ 2.0 % by weight, around noncrystalline soft magnetic powder, define the coating of described condensed phosphoric acid metallic compound.Except condensed phosphoric acid metallic compound, low-melting glass can also be added as reinforcing material.
As described noncrystalline soft magnetic powder, preferably by powder that the 2nd soft magnetic powder that the 1st soft magnetic powder and the noncrystalline less than described 1st soft magnetic powder by average grain diameter are formed is obtained by mixing.As condensed phosphoric acid metallic compound, heated phosphoric aluminum dihydrogen can be used to make its dehydration and the aluminium triphosphate obtained or aluminium metaphosphate.
In described condensed phosphoric acid metallic compound, Al can also be added 2o 3, SiO 2, MgO, Mg (OH) 2, CaO, Ca (OH) 2, asbestos, talcum, at least one in flying dust is as its hardening accelerator.
The manufacture method of core and such core that above-mentioned amorphous soft magnetic powder composition is shaped to given shape is also one of mode of the present invention.Employ the lower-noise reactor of any one core in them, high strength reactor, these cores manufacture method be also one of mode of the present invention.
The effect of invention
According to the present invention, a kind of lower-noise reactor can be provided, it is by improving the hardness of insulating barrier of soft magnetic powder, can provide the vibration that suppresses powder and the low-noise reactor that occurs of restraint speckle effectively, the manufacture method of high strength reactor, soft magnetic powder composition, core and core.
In addition, according to the present invention, for amorphous composite powder that two or more noncrystalline soft magnetic powders different for average grain diameter is mixed, the metallic compound of heated phosphoric is used to make the condensed phosphoric acid metallic compound of its dehydrating condensation as binding agent, thus the noncrystalline soft magnetic powder composition of no hygroscopicity, processing ease under normal temperature can be obtained.
Compared with low-melting glass, the cost of condensed phosphoric acid metallic compound is especially low, has the advantage that the cost competitiveness of product is high.Condensed phosphoric acid metallic compound is generally also used as rust inhibitor, can suppress getting rusty of compressed-core, and the phenomenon that magnetic hysteresis loss is worsened as low-melting glass can not occur.
Accompanying drawing explanation
Fig. 1 is the chart that the addition of condensed phosphoric acid metallic compound and the relation of noise are shown.
Fig. 2 is the chart of the relation of the addition of the condensed phosphoric acid metallic compound illustrated when making soft magnetic powder be Fe-Si-Al alloy powder and the noise level of carrier frequency periphery.
Fig. 3 is the chart of the relation of the addition of the condensed phosphoric acid metallic compound illustrated when making soft magnetic powder be Fe-6.5%Si alloy powder and the noise level of carrier frequency periphery.
Fig. 4 is the chart that the addition of condensed phosphoric acid metallic compound and the relation of noise are shown.
Fig. 5 illustrates to make the addition of insulation micro mist constant and the chart that changes the value of noise when comprising the addition of magnesian condensed phosphoric acid metallic compound.
Fig. 6 is the chart of value of noise when illustrating that the addition making to comprise magnesian condensed phosphoric acid metallic compound is constant and change the addition of insulation micro mist.
Fig. 7 is the chart that the addition relative to the condensed phosphoric acid metallic compound of soft magnetic powder and the relation of the radial crushing strength (radial crushing strength) of compressed-core obtained are shown.
Fig. 8 is the SEM image of the example that the 1st noncrystalline soft magnetic powder is shown, (a) illustrates the noncrystalline soft magnetic powder with main face, and (b) illustrates the noncrystalline soft magnetic powder without main face.
Fig. 9 is the SEM image of the example that the 2nd noncrystalline soft magnetic powder is shown, (a) illustrates that circularity (degree of circularity) is the water atomized powders of 0.962, and (b) illustrates that circularity is the water atomized powders of 0.965.
Figure 10 is the chart that the addition relative to the condensed phosphoric acid metallic compound of noncrystalline soft magnetic powder and the relation of the radial crushing strength of compressed-core obtained are shown.
Figure 11 is the chart that the addition relative to the condensed phosphoric acid metallic compound of noncrystalline soft magnetic powder and the relation of the magnetic permeability μ a of compressed-core obtained are shown.
Figure 12 is the chart that the addition relative to the condensed phosphoric acid metallic compound of noncrystalline soft magnetic powder and the relation of the loss Pcv of compressed-core obtained are shown.
Figure 13 is the chart that the addition relative to the condensed phosphoric acid metallic compound of the 1st noncrystalline soft magnetic powder and the 2nd noncrystalline soft magnetic powder and the relation of the radial crushing strength of the compressed-core obtained are shown.
Embodiment
1) execution mode 1
(1) soft magnetic powder
As soft magnetic powder, ferro-silicon-aluminium (Fe-Si-Al alloy) powder, Fe-Si alloyed powder, straight iron powder etc. can be used.
In addition, as soft magnetic powder, FeBPN (N is the element of more than a kind of being selected from Cu, Ag, Au, Pt, Pd) can be used.Soft magnetic powder can use by the soft magnetic powder manufactured by water atomization, gas atomization, water gas atomization, particularly preferably by soft magnetic powder that water atomization obtains.Reason is water atomization quenching when being atomized, and is therefore difficult to crystallization.
The average grain diameter of soft magnetic powder is preferably 20 μm ~ 100 μm.The powder hardness (in order to conjugate the pressure required for 10%) of soft magnetic powder is preferably more than 100MPa.Such as, the powder hardness of the powder hardness of amorphous alloy to be the powder hardness of 700MPa, Fe-6.5%Si alloy be 390MPa, Fe-Si-Al alloy is 100MPa, and thus these alloys are suitable for the present invention.But, be the straight iron powder of about 30MPa for powder hardness, also can be suitable for the present invention.
(2) condensed phosphoric acid metallic compound
As condensed phosphoric acid metallic compound, condensed phosphoric acid slaine is suitable, and condensation of aluminum phosphate is suitable especially.Wherein, heated phosphoric aluminum dihydrogen makes its dehydration and the aluminium triphosphate, aluminium metaphosphate or their mixture that obtain are suitable.Aluminium dihydrogen tripolyphosphate is suitable especially.If its average grain diameter is 1.5 μm ~ 6.0 μm, more preferably.In addition, condensed phosphoric acid calcium, condensed phosphoric acid magnesium etc. also have same effect.0.5 % by weight ~ 2.0 % by weight is preferably relative to the addition of the condensed phosphoric acid metallic compound of soft magnetic powder.By choosing this scope, the insulating barrier around soft magnetic powder can be made hardening, the dhering strength of soft magnetic powder and insulating barrier can be improved simultaneously.Therefore, it is possible to suppress the vibration of powder, low noise effect can be obtained.If addition is less than 0.5 % by weight, then cannot obtain noise suppression effect; If more than 2.0 % by weight, then magnetic permeability reduces, thus ripple current becomes large, and vibration becomes large, and noise increases.
(3) hardening accelerator
Alkaline matter can be added as its hardening accelerator in condensed phosphoric acid metallic compound.As alkaline matter, Al can be enumerated 2o 3, SiO 2, MgO, Mg (OH) 2, CaO, Ca (OH) 2, asbestos, talcum, at least one in flying dust.From the aspect obtaining low noise effect, particularly preferably add Al 2o 3, its particle diameter can be made further to be 7nm ~ 500nm.Also can similarly obtain low noise effect when adding MgO, its particle diameter can be made further to be 0.2 μm ~ 1 μm.Hardening accelerator preferably relative to condensed phosphoric acid metallic compound be its 10 % by weight ~ 30 % by weight.This is because when being less than 10 % by weight, the effect as curing agent is little; When more than 30 % by weight, the epithelium of the condensed phosphoric acid metallic compound on soft magnetic powder surface can be hindered to be formed.
(4) caking property insulating resin
Caking property insulating resin adds in the mixture of soft magnetic powder and condensed phosphoric acid metallic compound.As caking property insulating resin, use following resin: when at normal temperatures the mixture of soft magnetic powder and condensed phosphoric acid metallic compound being pressurizeed, can obtain with the formed body of the state of densification to a certain degree, and, only otherwise the viscosity that excessive power then has the degree that can maintain given shape is applied to its formed body.
Exemplarily, silicone-based resin, wax (wax) etc. can be enumerated.As the resin of silicone-based, preferable methyl phenyl system silicone resin.For the addition of methylbenzene base system silicone resin, be 0.75 % by weight ~ 2.0 % by weight relative to soft magnetic powder be appropriate.If be less than this addition, then the undercapacity of formed body, can break.If more than this addition, then can there is the problem that density reduces the magnetic characteristic that peakflux density reduces, magnetic hysteresis loss increase the causes reduction caused.
As other adhesion resin, acrylic copolymer resin (EAA) emulsion (emulsion) can be used.The addition of mixed acrylic copolymer resin (EAA) emulsion is 0.5 % by weight ~ 2.0 % by weight relative to alloy powder, and the baking temperature in this situation and drying time are 80 DEG C ~ 150 DEG C, 2 hours.Also can replace acrylic copolymer resin (EAA) emulsion and use PVA (polyvinyl alcohol) aqueous solution (12% aqueous solution).The addition of PVA (polyvinyl alcohol) aqueous solution (12% aqueous solution) is 0.5 % by weight ~ 3.0 % by weight relative to soft magnetic powder is appropriate.
In addition, also can use the aqueous solution (12% aqueous solution) of PVB (polyvinyl butyral resin), can also be dissolved in dimethylbenzene, butanols equal solvent and use.Now identical with PVA relative to the addition of soft magnetic powder.
(5) lubrification resin
As lubrification resin, stearic acid and the wax such as slaine and ethylene bis stearamide thereof can be used.By mixing them, powder slickness each other can be improved, therefore, it is possible to density, raising compact density when improving mixing.In addition, the punching press reduction of upper punch when can prevent shaping, mould produce with the longitudinal grin contacting the core wall caused of powder.The addition of lubrification resin is preferably 0.1 % by weight ~ 1.0 about % by weight relative to soft magnetic powder, is generally about 0.5 % by weight.
(6) manufacture method
The manufacture method of the core of present embodiment has following each operation.
A the 1st mixed processes that soft magnetic powder mixes with condensed phosphoric acid metallic compound by ().
B () is for the 2nd mixed processes of the mixture mixing caking property insulating resin obtained in the 1st mixed processes.
The c extrusion forming operation of mixture extrusion forming that () will obtain in the 2nd mixed processes.
D heat treatment step that () is heat-treated the formed body obtained in extrusion forming operation.
Below, each operation is described in detail.
(a) the 1st mixed processes
In 1st mixed processes, the soft magnetic powder being such as 20 μm ~ 100 μm to average grain diameter adds its condensed phosphoric acid metallic compound of 0.5 % by weight ~ 2.0 % by weight and mixes.Such as use V-Mixer that described mixture is mixed 2 hours.The opportunity of adding condensed phosphoric acid metallic compound may not be this operation, can also add mixing in the 2nd mixed processes of the adhesion resin of following (b) together with lubricant.But, when mixing condensed phosphoric acid metallic compound in front operation, effectively can carry out epithelium formation on soft magnetic powder surface.
(b) the 2nd mixed processes
For the mixture of soft magnetic powder and condensed phosphoric acid metallic compound, add the caking property insulating resin of 0.75 % by weight ~ 2.0 % by weight and the lubrification resin of 0.1 % by weight ~ 1.0 % by weight relative to soft magnetic powder, and mix further.The mixing of condensed phosphoric acid metallic compound of described (a) with can carry out the adhesion resin of (b) and mixing of lubrification resin simultaneously.
In the mixed processes of caking property insulating resin, silane coupler can also be added.When using silane coupler, the component of caking property insulating resin can be reduced.As the kind of the good silane coupler of adaptability, the silane coupler of amino system can be used, particularly preferably γ aminopropyltriethoxy silane.0.25 % by weight ~ 1.0 % by weight is preferably relative to the addition of the silane coupler of caking property insulating resin.By adding the silane coupler of this scope in caking property insulating resin, the standard deviation of the density of shaping compressed-core, magnetic characteristic, strength characteristics can be improved.
(c) extrusion forming operation
In extrusion forming operation, the mixture through the 2nd mixed processes is filled in mould, carries out extrusion forming.In this situation, mold temperature is preferably normal temperature, also can be the scope of less than 80 DEG C.That is, normal temperature herein refers to the scope of 5 DEG C ~ 35 DEG C, also can be the scope of 5 DEG C ~ 80 DEG C.Briquetting pressure is such as 900MPa ~ 1700MPa.
(d) heat treatment step
Heat treatment for formed body is carried out with specified temp in particular atmosphere according to the kind of soft magnetic powder.Heating-up temperature is more than 500 DEG C, and heated hold time is 2 hours ~ 4 hours.When soft magnetic powder is Fe-Si-Al alloy powder, heat-treating atmosphere is nitrogen atmosphere or air atmosphere.Because the noise of made reactor is low, therefore particularly preferably air atmosphere.When soft magnetic powder is Fe-Si alloy powder, straight iron powder, the reducing atmospheres such as preferred nitrogen atmosphere, 10% ~ 30% hydrogen.In addition, if heat treatment temperature is too high, then can cause insulation breakdown, eddy current loss increases.Therefore, from the aspect suppressing iron loss to increase, when Fe-Si-Al alloy powder and Fe-Si alloy powder, preferably 600 DEG C ~ 750 DEG C, particularly Fe-Si-Al alloy powder more preferably 600 DEG C ~ 725 DEG C.When straight iron powder, preferably 500 DEG C ~ 650 DEG C.By choosing these temperature ranges, the noise reduction of made reactor.
In the 2nd mixed processes, interpolation comprises the caking property insulating resin of silicon, by heat treatment step, this caking property insulating resin is changed to silicon dioxide layer.That is, the state that the silicon dioxide layer that soft magnetic powder becomes involved condensed phosphoric acid metallic compound by heat treatment step covers.Such as, when also added silane coupler as caking property insulating resin except methylbenzene base system silicone resin, their are oxidized and form silicon dioxide layer.By forming silicon dioxide layer, the hardness of the layer around soft magnetic powder improves, and comprise condensed phosphoric acid metallic compound, thus the hardness of this silicon dioxide layer improves further simultaneously, thus can obtain low noise effect.When except also comprising hardening accelerator in the external silicon dioxide layer of condensed phosphoric acid metallic compound, low noise effect can be obtained further.
Soft magnetic powder of the present invention may not only in compressed-core.Such as, by by soft magnetic powder of the present invention and specific resin injection is shaping or transfer molding, also core can be formed.In this situation, be preferably 55 % by weight ~ 95 % by weight relative to the filling rate of the soft magnetic powder of resin.As resin, the resin of the excellent size stability after preferably shaping, such as, if thermosetting resin then preferred epoxy or phenolic resins; If thermoplastic resin is preferred, polyethers sulfone then.When the filling rate of soft magnetic powder is low, there is the problem that magnetic property reduces.On the other hand, when carrying out height filling with more than 95 % by weight, the loading of binding agent reduces, and the intensity of core reduces, and cannot suppress the vibrate powder of soft magnetic powder, noise can increase.
2) execution mode 2
Use soft magnetic powder, hardening accelerator, adhesion resin, the lubrification resin same with execution mode 1.
Condensed phosphoric acid metallic compound uses the material same with execution mode 1.The addition of the condensed phosphoric acid metallic compound relative to soft magnetic powder in present embodiment is preferably 0.20 % by weight ~ 0.80 % by weight.
In present embodiment, by adding insulation micro mist further, soft magnetic powder bonding each other can be prevented, and the insulating barrier around soft magnetic powder can be made hardening, the vibration of soft magnetic powder can be suppressed, can noise suppression effect be obtained.From the aspect of noise suppression effect, the average grain diameter of insulation micro mist is preferably 7nm ~ 1 μm.Be more preferably 7nm ~ 500nm.As insulation micro mist, alumina powder (Al can be used 2o 3), SiO 2, MgO etc.In addition, the hardness of insulation micro mist is higher, then can obtain more excellent low noise effect.Insulation micro mist preferably use Mohs' hardness be more than 7 insulation micro mist.Such as, can use Mohs' hardness be 7.0 SiO 2, Mohs' hardness is the Al of 9.0 2o 3.But, even if the MgO that use Mohs' hardness is 4.0 also can obtain the effect of low noise.
Manufacture method is identical with execution mode 1.In present embodiment, there is the mixed processes of mix insulation micro mist.The operation of mix insulation micro mist can be carried out together with the 1st mixed processes soft magnetic powder and condensed phosphoric acid metallic compound mixed.In addition, for the mixture obtained in the 1st mixed processes, can in the 2nd mixed processes of mixing caking property insulating resin mix insulation micro mist.In addition, following powder heat treatment step can be had before the 1st mixed processes: insulation micro mist is added to soft magnetic powder and mixes, its mixed powder is heat-treated.
The mixture comprising soft magnetic powder and condensed phosphoric acid metallic compound is shaped to given shape, its formed body is heat-treated, make compressed-core thus.Except condensed phosphoric acid metallic compound, can comprise in the insulating barrier formed around soft magnetic powder insulation micro mist or hardening accelerator or both.The thickness of insulating barrier is about 20nm ~ 50nm.
3) execution mode 3
Use soft magnetic powder, hardening accelerator, adhesion resin, the lubrification resin same with execution mode 1.
Condensed phosphoric acid metallic compound uses the material same with execution mode 1.The addition of the condensed phosphoric acid metallic compound relative to soft magnetic powder in present embodiment is preferably 0.25 % by weight ~ 2.0 % by weight.When addition is more than 0.25 % by weight, the effect that the intensity that can obtain made core increases; When addition is more than 2.0 % by weight, the density of core reduces, and intensity also reduces.
Manufacture method is same with execution mode 1.In present embodiment, the heat treated operation for formed body is carried out in the non-reducing atmosphere such as air atmosphere.As non-reducing atmosphere, can also be in the inert gas atmospheres such as 100% nitrogen except in air.Such as, also with the temperature of 350 DEG C, formed body can be heated 2 hours in an atmosphere, be converted to nitrogen atmosphere afterwards, 470 DEG C of heating 2 hours.
When noncrystalline soft magnetic alloy powder, heat treatment temperature is preferably 400 DEG C ~ 440 DEG C, and heating time is 2 hours ~ 4 hours.Keep such temperature and the reason of heating time to be, the state be in below the crystallization temperature of soft magnetic powder can be guaranteed, and, radial crushing strength required when compressed-core being shaped to ring-type.On the other hand, if heat treatment temperature is too high, then the crystallization of soft magnetic powder carries out, and magnetic permeability reduces, and iron loss (magnetic hysteresis) increases.Therefore, in order to suppress iron loss to increase, the temperature keeping 400 DEG C ~ 440 DEG C is effective.In addition, when sendust alloy or Fe-Si alloy, preferably heat-treat with the temperature of 600 DEG C ~ 750 DEG C.
4) execution mode 4
(1) noncrystalline soft magnetic powder
The core of present embodiment by mixing condensed phosphoric acid metallic compound aftershaping for specific shape and obtaining in noncrystalline soft magnetic powder.In this situation, as noncrystalline soft magnetic powder, can be used alone by comminuted powder or by the powder manufactured by water atomization, gas atomization, water gas atomization or be used in combination of two or more.That is, the invention is characterized in, use condensed phosphoric acid metallic compound to replace the low-melting glass be used for as binding agent in known noncrystalline soft magnetic powder.
Particularly, as noncrystalline soft magnetic powder, the composite magnetic powder that 1st noncrystalline soft magnetic powder and the 2nd noncrystalline soft magnetic powder are obtained by mixing by preferred use, described 1st noncrystalline soft magnetic powder has specific average grain diameter, and described 2nd noncrystalline soft magnetic powder is made up of the noncrystalline that average grain diameter is less than the average grain diameter of described 1st noncrystalline soft magnetic powder.
1st noncrystalline soft magnetic powder preferably uses comminuted powder.2nd noncrystalline soft magnetic powder can use by the noncrystalline soft magnetic powder manufactured by water atomization, gas atomization, water gas atomization, particularly preferably by noncrystalline soft magnetic powder that water atomization obtains.Reason is water atomization quenching when being atomized, and is therefore difficult to crystallization.
The core of present embodiment is that the 1st noncrystalline soft magnetic powder and the 2nd noncrystalline soft magnetic powder mix according to the mixed proportion of 80:20 to 40:60.Such as, when making 80 % by weight to be the 1st noncrystalline soft magnetic powder in composite magnetic powder, remaining 20 % by weight is the 2nd noncrystalline soft magnetic powder.By mixing in this scope, the density of compressed-core improves, and can be formed and have 5.70g/cm 3the compressed-core of above density, can increase magnetic permeability.
(2) the 1st noncrystalline soft magnetic powders
As the 1st noncrystalline soft magnetic powder, the comminuted powder of Fe base amorphous can be used.This comminuted powder is such as by the powder of 25 μm of thick strip pulverizing.As the 1st noncrystalline soft magnetic powder, the powder that such as Si composition is 6.7%, B component is 2.5%, Cr composition is 2.5%, C composition is 0.75%, residual components is Fe can be used.In addition, as noncrystalline soft magnetic powder, FeBPN (N is the element of more than a kind of being selected from Cu, Ag, Au, Pt, Pd) can be used.The crystallization start temperature of the 1st noncrystalline soft magnetic powder is like this generally about 470 DEG C.
1st noncrystalline soft magnetic powder preferably uses average grain diameter to be the powder of the scope of 30 μm ~ 100 μm.If average grain diameter is greater than this scope, then eddy current loss increases; If average grain diameter is less than this scope, then density reduces the magnetic hysteresis loss caused increases.
As shown in the SEM image of (a) of Fig. 8, comminuted powder at least has 1 main face.That is, not there is the shape of continuous surface as spherical, but be the shape of such as hemisphere or tabular and so on.Such as when thinking that comminuted powder is hemisphere, main face refers to the face of the circle forming this hemisphere.In addition, such as, when thinking that comminuted powder is highly low cuboid, main face refers to two rectangular maximum and relative among the face forming this cuboid.
On the other hand, the powder shown in (b) of Fig. 8 is the shape of subglobular, does not have main face.The circularity of the comminuted powder of (b) of Fig. 8 is 0.980, and as shown in the Examples, the direct current overlapping features without the comminuted powder in main face is poor, therefore cannot use.
The shape in main face is not defined as rectangle, comprises the various shapes such as square or circular, and may not be homogeneous.When comminuted powder has multiple main face, the area in each main face can be different, among the face forming comminuted powder according to the large order of area using plural as main face.In addition, main face may not be relative abreast, can be adjacent three, also can be angularly relative.
The end in main face is the shape with circle.Shape with circle is that finger ends has curve form, there is not the angle with summit.Curve form is not limited to the shape of the arc of positive round, then can be understood as curve form as long as no angle.
The circularity of main of comminuted powder is preferably less than 0.98.For reference, if use regular polygon that circularity is described, then the circularity of dodecagon is 0.9885, and the circularity of octagon is 0.9737.Therefore, the circularity in main of the comminuted powder of present embodiment is 0.980, the intermediate degree of dodecagon and octagon is referred to.But the shape in main face is not defined as regular polygon.
In addition, the circularity of such as equilateral triangle is 0.7776, and preferably main face at least has the circularity of equilateral triangle degree.This is because if circularity is below this, then the easy end in main face produces rib (edge).
(3) the 2nd noncrystalline soft magnetic powders
2nd noncrystalline soft magnetic powder uses the noncrystalline soft magnetic powder that average grain diameter is less than the 1st noncrystalline soft magnetic powder.As the 2nd noncrystalline soft magnetic powder, the alloy atomization powder of Fe system (Fe-Si-B etc.) can be used.The crystallization start temperature of the 2nd noncrystalline soft magnetic powder is like this generally about 450 DEG C.
As shown in Figure 9, the shape of powder can be used to be spherical, that its average grain diameter is the scope of 5 μm ~ 30 μm powder, to be preferably the powder of scope of 5 μm ~ 20 μm, the powder of the scope of more preferably 8 μm ~ 15 μm.If average grain diameter is greater than this scope, when being atomized, cooling rate does not catch up with and causes crystallization, likely produces circularity and reduces, loses spherical problem.In addition, if average grain diameter is less than this scope, the gap (clearance) (about 10 μm) of mould can be entered when shaping, be engaged (bite).
The circularity of the 2nd noncrystalline soft magnetic powder is preferably more than 0.962.For reference, if use regular polygon that circularity is described, then orthohexagonal circularity is 0.9523, and the circularity of octagon is 0.9737.Therefore, when the circularity of the 2nd powder of present embodiment is 0.962, refer to the intermediate degree of regular hexagon and octagon, close to round shape.Wherein, the 2nd noncrystalline soft magnetic powder is the compound shapes such as circle or ellipse, roughly divides into and belongs to spherical shape.As the 2nd above-mentioned noncrystalline soft magnetic powder, the powder of (a) of Fig. 9 or (b) of Fig. 9 can be used, but be not limited to these.
As noncrystalline soft magnetic powder, except Fe-Si-B alloy, the amorphous powder of the various known non-retentive alloy such as Fe-Si-B system alloy, Fe-Cr-P system alloy, Fe-Zr-B system alloy, sendust system alloy, Co-Fe-Si-B system alloy having added the elements such as Nb, Cu, C wherein can also be used alone or as a mixture.
In present embodiment, the average grain diameter of each powder and circularity are the value that the mean value using following apparatus to get 3000 obtains, and by powder dispersion on glass substrate, with microscope photographing powder photo, are automatically measured by image for each.
Exabyte: Malvern
Device name: morphologi G3S
(4) condensed phosphoric acid metallic compound
As condensed phosphoric acid metallic compound, the aluminium triphosphate that heated phosphoric aluminum dihydrogen makes its dehydration and obtains, aluminium metaphosphate etc. are suitable.In addition, condensed phosphoric acid calcium, condensed phosphoric acid magnesium etc. also have same effect.
0.25 % by weight ~ 2.0 % by weight is preferably relative to the addition of the condensed phosphoric acid metallic compound of composite magnetic powder.When addition is more than 0.25 % by weight, the effect that the intensity that can obtain made core increases; When addition is more than 2.0 % by weight, the density of core reduces, and intensity also reduces.
(5) hardening accelerator
Al can also be added in condensed phosphoric acid metallic compound 2o 3, SiO 2, MgO, Mg (OH) 2, CaO, Ca (OH) 2, asbestos, talcum, at least one in flying dust is as hardening accelerator.Hardening accelerator relative to condensed phosphoric acid metallic compound be preferably its 10 % by weight ~ 30 % by weight.This is because, for less than 10% time, the effect as curing agent is little; When more than 30 % by weight, the epithelium of the condensed phosphoric acid metallic compound on noncrystalline soft magnetic powder surface can be hindered to be formed.
(6) adhesion resin
At least one of softening point than the 1st and in the low glass powder of the crystallization temperature of the 2nd noncrystalline soft magnetic powder and lubrification resin is mixed with in composite magnetic powder.Adhesion resin adds in the mixed powder of composite magnetic powder and condensed phosphoric acid metallic compound.As adhesion resin, use following resin: when at normal temperatures the mixture of composite magnetic powder and condensed phosphoric acid metallic compound being pressurizeed, can obtain with the formed body of the state of densification to a certain degree, and, only otherwise the viscosity that excessive power then has the degree that can maintain given shape is applied to its formed body.
Exemplarily, silicone-based resin, wax etc. can be enumerated.As the resin of silicone-based, preferable methyl phenyl system silicone resin.For the addition of methylbenzene base system silicone resin, be 0.75 % by weight ~ 2.0 % by weight relative to composite magnetic powder be appropriate.If be less than this addition, then the undercapacity of formed body, can break.If more than this addition, then can there is the problem that density reduces the magnetic characteristic that peakflux density reduces, magnetic hysteresis loss increase the causes reduction caused.
As other adhesion resin, acrylic copolymer resin (EAA) emulsion can be used.The addition of mixed acrylic copolymer resin (EAA) emulsion is 0.5 % by weight ~ 2.0 % by weight relative to composite magnetic powder, and the baking temperature in this situation and drying time are 80 DEG C ~ 150 DEG C, 2 hours.Also can replace acrylic copolymer resin (EAA) emulsion and use PVA (polyvinyl alcohol) aqueous solution (12% aqueous solution).The addition of PVA (polyvinyl alcohol) aqueous solution (12% aqueous solution) is 0.5 % by weight ~ 3.0 % by weight relative to composite magnetic powder is appropriate.In addition, also can use the aqueous solution (12% aqueous solution) of PVB (polyvinyl butyral resin), can also be dissolved in dimethylbenzene, butanols equal solvent and use.Now identical with PVA relative to the addition of soft magnetic powder.
(7) lubrification resin
As lubrification resin, stearic acid and the wax such as slaine and ethylene bis stearamide thereof can be used.Specifically, be ethylene bis stearamide, lithium stearate, dolomol etc.By mixing them, powder slickness each other can be improved, therefore, it is possible to density, raising compact density when improving mixing.In addition, the punching press reduction of upper punch when can prevent shaping, mould produce with the longitudinal grin contacting the core wall caused of powder.
The addition of lubrification resin is preferably 0.1 % by weight ~ 1.0 about % by weight relative to composite magnetic powder, is generally about 0.5 % by weight.If be less than this addition, sufficient effect cannot be obtained; If more than this addition, then can there is the problem that density reduces the magnetic characteristic that peakflux density reduces, magnetic hysteresis loss increase the causes reduction caused.
(8) glass
Glass can be mixed in composite magnetic powder as powder.As glass, use the low-melting glass of bismuth system or phosphoric acid system.In addition, preferably use transition temperature and softening point than the 1st and glass that the crystallization start temperature at 2-in-1 bronze end is low.By using softening point lower than the glass of crystallization start temperature, even if when being heated to the temperature of Glass Transition, the magnetic characteristic that also can prevent the crystallization of alloy powder from causing reduces.
As glass, use the glass with mobility of transition temperature and lower than the crystallization start temperature of alloy powder about about 50 DEG C of softening point.By making the difference of transition temperature and softening point and heat treatment temperature large, the viscosity of glass reduces, mobility increases, between alloy powder, be thus easy to flowing.Thereby, it is possible to raising mechanical strength.
Representatively glass, can enumerate the glass (Bi of bismuth system 2o 3b 2o 3).The combined amount of glass sets according to desired magnetic permeability.But if few relative to the combined amount of the glass of composite magnetic powder, then coated (coating) between alloy powder is insufficient, therefore eddy current loss increases.If the combined amount of glass is many, then reduce relevant with the magnetic permeability of alloy powder, alloy powder condenses each other simultaneously, cannot guarantee sufficient magnetic characteristic.The combined amount of glass is such as selected from the scope of 0.75 % by weight ~ 1.5 about % by weight of alloy powder.
The average grain diameter of glass powder is preferably 0.5 μm ~ 3.0 μm.If the average grain diameter of glass powder is less than 0.5 μm, then glass powder is too small relative to alloy powder.Therefore, be difficult to fully prevent alloy powder contact each other, be difficult to the generation fully preventing, suppress eddy current.In addition, if the average grain diameter of glass powder is greater than 3.0 μm, then glass powder is excessive relative to alloy powder, therefore produces gap each other at alloy powder, and magnetic permeability and density reduce.In addition, be difficult to fully prevent alloy powder contact each other, be difficult to the generation fully preventing, suppress eddy current.
(9) action effect
The action effect with the core of the present embodiment of above-mentioned formation is as described below.
(9-1) for the composite magnetic powder that the noncrystalline varied in size soft magnetic powder is mixed, add condensed phosphoric acid metallic compound more cheap compared with low-melting glass and that moisture absorption is few, simple to operate, thus the excellent compressed-core of radial crushing strength, magnetic permeability μ a and loss Pcv can be obtained.In addition, radial crushing strength excellent described compressed-core winding coil is used and the reactor that obtains has the effect of low noise.
(9-2) in the 1st noncrystalline soft magnetic powder, use the noncrystalline soft magnetic powder at least with two main faces, thus adjacent powder forming surface contact.When face contacts, can resistance be reduced compared with point cantact, thus can improve direct current overlapping features.
(9-3) end of main of the 1st noncrystalline soft magnetic powder is the shape with circle, therefore, it is possible to do not destroy the epithelium of insulating resin and improve insulation property.When there being rib, the space produced between adjacent powder diminishes, and when end is the shape with circle, can expand the space corresponding to this part.Therefore, the 2nd noncrystalline soft magnetic powder enters its spatial portion, thus can improve the density of compressed-core.
(9-4) as the 2nd noncrystalline soft magnetic powder, employ the powder that average grain diameter is less than the 1st noncrystalline soft magnetic powder, therefore the 2nd noncrystalline soft magnetic powder enters above-mentioned gap, can improve the density of compressed-core.Therefore, it is possible to improve formed body intensity further.Thus, by making the density of compressed-core be 5.70g/cm 3above, magnetic permeability can be improved.
Even if (9-5) adhesion resin is at high temperature heat-treated, insulating properties is not deteriorated yet, and the magnetic hysteresis loss that oxidation etc. causes can not increase.In addition, when using methylbenzene base system silicone sticker, powder adhesion strength each other can be increased, therefore, it is possible to improve formed body intensity further.In addition, by carrying out the heat treatment of compressed-core in an atmosphere, densification can be formed and firmly silicon dioxide film.By heat-treating in an atmosphere, methyl can not be made to remain, therefore, it is possible to improve mechanical strength as carbon because of thermal decomposition.
(9-6) when using stearic slaine as lubrification resin, the thermal decomposition rate (temperature) of methyl can be improved by catalytic effect according to the kind of metal, therefore, even if also firmly silicon dioxide layer can be formed from lower temperature.
(9-7) by adding low-melting glass, the mouldability of formed body can be made enough excellent, can compact density be improved simultaneously.
(10) manufacture method
The manufacture method of the core of present embodiment comprises following each operation.
The operation of (a) mixing composite magnetic powder and condensed phosphoric acid metallic compound.
B () adds the operation of adhesion resin for the mixture obtained in mixed processes.
C () is pressurizeed to the mixture that have passed through adhesion resin interpolation operation and makes the molding procedure of formed body.
D heat treatment step that the formed body obtained by molding procedure heats by ().
Below, each operation is described in detail.
The mixed processes of (a) condensed phosphoric acid metallic compound
In mixed processes, such as, for the composite magnetic powder that the 1st noncrystalline soft magnetic powder and the 2nd noncrystalline soft magnetic powder are mixed to get with the mixed proportion of 75:25 to 50:50, add its condensed phosphoric acid metallic compound of 0.25 % by weight ~ 2.0 % by weight.Thereafter, such as use V-Mixer that these mixtures are mixed 2 hours.In this situation, can to the glass powder of composite magnetic powder mixing specified quantitative.
The opportunity of adding condensed phosphoric acid metallic compound may not be this operation, can also add mixing in the interpolation operation of the adhesion resin of (b) together with lubricant.But, when mixing condensed phosphoric acid metallic compound in front operation, effectively can carry out epithelium formation at composite magnetic powder surface.
The interpolation operation of (b) adhesion resin
For the mixture of composite magnetic powder and condensed phosphoric acid metallic compound, add the adhesion resin of 0.75 % by weight ~ 2.0 % by weight and the lubrification resin of 0.1 % by weight ~ 1.0 % by weight relative to composite magnetic powder, and mix further.The mixing of condensed phosphoric acid metallic compound of described (a) with also can carry out the adhesion resin of (b) and mixing of lubrification resin simultaneously.Be mixed with relative to composite magnetic powder be 0.75 % by weight ~ 1.5 % by weight glass powder and relative to composite magnetic powder be 0.3 % by weight lubrification resin at least one.
Silane coupler can also be added in the interpolation operation of adhesion resin.When using silane coupler, the component of adhesion resin can be reduced.As the kind of the good silane coupler of adaptability, the silane coupler of amino system can be used, particularly preferably γ aminopropyltriethoxy silane.0.25 % by weight ~ 1.0 % by weight is preferably relative to the addition of the silane coupler of adhesion resin.By adding the silane coupler of this scope in adhesion resin, the standard deviation of the density of shaping compressed-core, magnetic characteristic, strength characteristics can be improved.
(c) molding procedure
In molding procedure, the mixture being added with adhesion resin is filled in mould, carries out extrusion forming.In this situation, mold temperature is preferably normal temperature, also can be the scope of less than 80 DEG C.That is, normal temperature herein refers to the scope of 5 DEG C ~ 35 DEG C, also can be the scope of 5 DEG C ~ 80 DEG C.Briquetting pressure is such as 1300MPa ~ 1700MPa.
(d) heat treatment step
Heat treatment for formed body is carried out in the non-reducing atmosphere such as air atmosphere.As non-reducing atmosphere, can also be in the inert gas atmospheres such as 100% nitrogen except in air.Such as, also with the temperature of 350 DEG C, formed body can be heated 2 hours in an atmosphere, be converted to nitrogen atmosphere afterwards, 470 DEG C of heating 2 hours.Particularly, when adding low-melting glass, by the heat treatment in non-reducing atmosphere, can realize following function: can not lose the oxygen in glass, can keep the character of glass originally, the surrounding of alloy powder carries out coated.
When noncrystalline soft magnetic powder, heat treatment temperature is preferably 400 DEG C ~ 440 DEG C, and heating time is 2 hours ~ 4 hours.Keep such temperature and the reason of heating time to be, the state be in below the crystallization temperature of noncrystalline soft magnetic powder can be guaranteed, and, radial crushing strength required when compressed-core being shaped to ring-type.On the other hand, if heat treatment temperature is too high, then the crystallization of noncrystalline soft magnetic powder carries out, and magnetic permeability reduces, and iron loss (magnetic hysteresis) increases.Therefore, in order to suppress iron loss to increase, the temperature keeping 400 DEG C ~ 440 DEG C is effective.In addition, when sendust alloy or Fe-Si alloy, preferably heat-treat with the temperature of 600 DEG C ~ 750 DEG C.
Composite magnetic powder of the present invention may not only in compressed-core.Such as, by by composite magnetic powder of the present invention and specific resin injection is shaping or transfer molding, core can also be formed.In this situation, be preferably 55 % by weight ~ 95 % by weight relative to the filling rate of the soft magnetic metal powder of resin.As resin, the resin of the excellent size stability after preferably shaping, such as, if thermosetting resin then preferred epoxy or phenolic resins; If thermoplastic resin is preferred, polyethers sulfone then.When the filling rate of soft magnetic metal powder is low, there is the problem that magnetic property reduces.On the other hand, when carrying out height filling with more than 95 % by weight, the loading of binding agent reduces, and the intensity of core reduces.
Embodiment
1. example I
Below, with reference to table 1 ~ table 3, Fig. 1 ~ Fig. 4, embodiments of the invention I is described.
(1) project is measured
Mensuration project is magnetic permeability, iron loss and noise.To the sample of each compressed-core made, implement 42 circle kinkings with the copper cash of φ 2.6mm, make reactor.Calculate magnetic permeability and the iron loss of this reactor under the following conditions, under the following conditions the noise produced by reactor is measured.
< magnetic permeability and iron loss >
The condition determination of magnetic permeability and iron loss is frequency 100kHz, peakflux density Bm=50mT.Magnetic permeability is amplitude permeability when setting peakflux density Bm when iron loss Pcv measures.For iron loss, the BH analyzer of magnetism measuring equipment (rock amounts to and surveys Co., Ltd.: SY-8232) is used as to calculate.In this calculating, for the frequency curve of iron loss, utilize least square method to calculate the coefficient of hysteresis, eddy current loss coefficient by following (1) ~ (3) formula, thus carry out.
Pcv＝Kh×f+Ke×f 2…(1)
Ph＝Kh×f…(2)
Pe＝Ke×f 2…(3)
Pcv: iron loss
Kh: the coefficient of hysteresis
Ke: eddy current loss coefficient
F: frequency
Ph: magnetic hysteresis loss
Pe: eddy current loss
< noise level measurement >
About noise level measurement, its determinator is shown below, measures environment, assay method etc.
[noise evaluation device and software]
(1) determinator sound level meter (SOUND LEBEL METER) NL-31 ... RION Co., Ltd. manufactures
(2) environment silencer box (dark noise is 25dB) KM-1 is measured ... Co., Ltd. ACO manufactures
(3) power amplifier (sound source) high-speed power amplifier/bipolar power supply (HIGH SPEED POWER AMPLIFIER/BIPOLAR POWER SUPPLY) 4025 ... NF ELECTRONIC INSTRUMENTS society manufactures
(4) oscillator 80MHz function/Arbitrary Waveform Generator (Function/Arbitrary Waveform Generator) 33250A ... Agilent Technologies Co., Ltd. manufactures
(5) interpretation software SA-01CATSYSSA Ver3.5 ... RION Co., Ltd. manufactures
[assay method]
(1) solar power generation power governor is connected
(2) microphone distance: range determination sample 10mm
(3) be arranged in silencer box by working sample, the distance of the microphone of noise level measurement is set to distance sample 10mm.
(2) manufacture method of sample
Use (a) Fe-Si-Al alloy powder, (b) Fe-6.5%Si alloy powder, (c) pure iron powder as soft magnetic powder respectively, utilize following manufacture method to make the sample of compressed-core.Their manufacture method and result thereof are shown below successively.
(a) Fe-Si-Al alloy powder
It is the powder of the Fe-Si-Al alloy powder (average grain diameter 40 μm) of 100MPa for hardness, add and be mixed with the aluminium dihydrogen tripolyphosphate (average grain diameter 2.3 μm) 0 ~ 2.5 % by weight of 25 % by weight magnesium oxide as hardening accelerator, and mix, further hybrid lubricant 0.3 % by weight.Then, for this mixture mixed silanes coupling agent 1.0 % by weight, methylbenzene base system silicone resin 1.0 % by weight, the heat drying of 2 hours is carried out at 150 DEG C, further hybrid lubricant 0.3 % by weight.
At room temperature with the pressure of 1000MPa, extrusion forming is carried out to it, make the ring-type formed body of external diameter 77.8mm, internal diameter 49.2mm, height 30.0mm, heat-treated with 2 hours retention times in 700 DEG C in an atmosphere, make compressed-core.
For these samples, as shown in above-mentioned " (1) measure project ", make reactor and carried out magnetic permeability, the calculating of iron loss and noise level measurement.The results are shown in table 1 and Fig. 1.It should be noted that, in table 1 ~ table 3, μ a represents magnetic permeability, and Pcv represents iron loss.Noise Max value is the peak value under carrier frequency.
[table 1]
Fig. 1 is the chart that the addition of condensed phosphoric acid metallic compound and the relation of noise are shown.From table 1 and Fig. 1, the addition of condensed phosphoric acid metallic compound is preferably 0.5 % by weight ~ 2.0 % by weight.When addition is less than 0.5 % by weight, addition is few, and the hardness of the insulating barrier of compressed-core cannot fully improve.Therefore, the vibrate powder that excitation field causes cannot be suppressed, sufficient noise suppression effect cannot be obtained.
On the other hand, known: when the addition of condensed phosphoric acid metallic compound is more than 0.5 % by weight, noise Max value reduces, and becomes low noise.The reason becoming low noise is the hardness raising of the insulating barrier of compressed-core.In addition, the dhering strength of soft magnetic powder and insulating barrier improves, and can suppress vibrate powder.When addition is more than 2.0 % by weight, noise Max value increases.Its reason is, reduces, the reduction of the L value of reactor owing to resulting from the magnetic permeability that density reduces.Thus, ripple current increases, and change in magnetic flux density increases, and thus vibrate powder increases, and noise increases.In addition, as shown in comparative example 2, when the addition of condensed phosphoric acid metallic compound is more than 2.0 % by weight, magnetic permeability or iron loss equimagnetic characteristic degradation, performance when making reactor product is insufficient, impracticable.Therefore, from the aspect of low noise effect and high strength and good magnetic characteristic, the addition of condensed phosphoric acid metallic compound is preferably 0.5 % by weight ~ 2.0 % by weight.
It should be noted that, refer to the noise level of which kind of degree about low noise, the level required by the difference of the environment for use of reactor is different.Generally speaking, the noise of level that can not feel unpleasant when using reactor is below 42dB, when by cell locations such as solar power systems in indoor, sometimes require lower noise level.In the present embodiment, even if in this case, by making the addition of condensed phosphoric acid metallic compound be 0.5 % by weight ~ 2.0 % by weight, low noise effect can be realized.
Fig. 2 shows the relation of the addition of condensed phosphoric acid metallic compound and the noise level of carrier frequency periphery.Embodiment 1,4 shown in Fig. 2 and comparative example 1 all have peak value (noise Max value) near frequency 19.0kHz.The noise Max value of embodiment 1 and embodiment 4 all reduces than comparative example 1, can confirm noise suppression effect.It should be noted that, the noise level La of the longitudinal axis of Fig. 2 measures to each sample the mean value obtained for 3 times respectively.
(b) Fe-6.5%Si alloy powder
It is the powder of the Fe-6.5%Si alloy powder (average grain diameter 20 μm) of 390MPa for hardness, add and be mixed with the aluminium dihydrogen tripolyphosphate (average grain diameter 2.3 μm) 0 ~ 2.5 % by weight of 25 % by weight magnesium oxide as hardening accelerator, and mix.Next, for this mixed powder mixed silanes coupling agent 0.5 % by weight, methylbenzene base system silicone resin 1.8 % by weight, carry out the heat drying of 2 hours at 150 DEG C, mixing 0.6 % by weight zinc stearate is as lubricant further.
At room temperature with the pressure of 1000MPa, extrusion forming is carried out to it, make the ring-type formed body of external diameter 77.8mm, internal diameter 49.2mm, height 30.0mm, heat-treated with 2 hours retention times in 700 DEG C in nitrogen atmosphere, make compressed-core.
For these samples, as shown in above-mentioned " (1) measure project ", make reactor and carried out magnetic permeability, the calculating of iron loss and noise level measurement.The results are shown in table 2, Fig. 1 and Fig. 3.
[table 2]
From table 2 and Fig. 1, the addition of condensed phosphoric acid metallic compound is preferably the scope of 0.5 % by weight ~ 2.0 % by weight.Its reason is identical with the reason of above-mentioned (a).It should be noted that, although comparative example 4 noise Max value compared with embodiment 5 is low, noise suppression effect good, magnetic permeability, iron loss equimagnetic characteristic degradation, impracticable when making reactor product.
Fig. 3 shows the relation of the addition of condensed phosphoric acid metallic compound and the noise level of carrier frequency periphery.Embodiment 6 shown in Fig. 3 and comparative example 3 all have peak value (noise Max value) near frequency 19.0kHz.Noise Max value minimizing compared with comparative example 3 of embodiment 6, also can confirm noise level on the whole simultaneously and reduce under its week side frequency.It should be noted that, the noise level La of the longitudinal axis of Fig. 3 measures to each sample the mean value obtained for 3 times respectively.
(c) pure iron (Fe) powder
It is the powder of the pure iron powder (average grain diameter 43 μm) of 30MPa for hardness, add and be mixed with the aluminium dihydrogen tripolyphosphate (average grain diameter 2.3 μm) 0 ~ 2.5 % by weight of 25 % by weight magnesium oxide as hardening accelerator, and mix.Next, for this mixed powder mixed silanes coupling agent 0.5 % by weight, methylbenzene base system silicone resin 1.4 % by weight, carry out the heat drying of 2 hours at 175 DEG C, mixing 0.5 % by weight zinc stearate is as lubricant further.
At room temperature with the pressure of 900MPa, extrusion forming is carried out to it, make the ring-type formed body of external diameter 77.8mm, internal diameter 49.2mm, height 30.0mm, heat-treated with 2 hours retention times in 550 DEG C in nitrogen atmosphere, make compressed-core.
For these samples, as shown in above-mentioned " (1) measure project ", make reactor and carried out magnetic permeability, the calculating of iron loss and noise level measurement.The results are shown in table 3.
[table 3]
As shown in Table 3, when pure iron powder, also the addition of condensed phosphoric acid metallic compound is preferably the scope of 0.5 % by weight ~ 2.0 % by weight in the same manner as the Fe-Si-Al alloy powder of above-mentioned (a) and (b), Fe-6.5%Si alloy powder.Its reason is identical with the reason of (b) with above-mentioned (a).When particularly addition is 0.5 % by weight ~ 1.0 % by weight, low noise Be very effective, and magnetic permeability, iron loss magnetic characteristic also good.Because the hardness of soft magnetic powder also contributes to noise decrease, thus wish its powder hardness be more than 100MPa (such as, Fe-Si-Al alloy powder, Fe-6.5%Si alloy powder), even if do not meet the pure iron powder of this numerical value, also can confirm by adding condensed phosphoric acid metallic compound and obtain noise suppression effect.When using pure iron powder as soft magnetic powder, such as, be suitable for the unit such as solar power system being arranged at outdoor situation.
2. example II
Below, with reference to table 4, Fig. 5 ~ Fig. 6, embodiments of the invention II is described.
The calculating of mensuration project, magnetic permeability and iron loss, noise level measurement method utilize the method same with example I to carry out.About determinator, the device same with example I is also used to measure.
The manufacture method of sample
Use Fe-Si-Al alloy powder as soft magnetic powder, utilize following manufacture method to make the sample of compressed-core.Their manufacture method and result thereof are shown below successively.
It is the powder of the Fe-Si-Al alloy powder (average grain diameter 40 μm) of 100MPa for hardness, add and be mixed with the aluminium dihydrogen tripolyphosphate (average grain diameter 2.3 μm) 0 ~ 1.0 % by weight of 25 % by weight magnesium oxide as hardening accelerator, and mix, add Al 2o 3(average grain diameter 0.05 μm, Mohs' hardness 9.0, Bi Biao Mian Plot 100m 2/ g) 0 ~ 0.8 % by weight conduct insulation micro mist, further hybrid lubricant 0.3 % by weight.Then, for this mixture mixed silanes coupling agent 1.0 % by weight, methylbenzene base system silicone resin 1.0 % by weight, the heat drying of 2 hours is carried out at 150 DEG C, further hybrid lubricant 0.3 % by weight.
At room temperature with the pressure of 1000MPa, extrusion forming is carried out to it, make the ring-type formed body of external diameter 77.8mm, internal diameter 49.2mm, height 30.0mm, heat-treated with 2 hours retention times in 700 DEG C in an atmosphere, make compressed-core.
For these samples, as shown in above-mentioned " (1) measure project ", make reactor and carried out magnetic permeability, the calculating of iron loss and noise level measurement.The results are shown in table 4 and Fig. 5 ~ 6.It should be noted that, in table 4, μ a represents magnetic permeability, and Pcv represents iron loss.Noise Max value is the peak value under carrier frequency.
[table 4]
Fig. 5 is chart interpolation 0.1 % by weight insulation micro mist being shown and changing the value of noise when comprising the addition of magnesian condensed phosphoric acid metallic compound.From table 4 and Fig. 5, the addition of condensed phosphoric acid metallic compound is preferably 0.20 % by weight ~ 0.80 % by weight.When addition is less than 0.20 % by weight, addition is few, and the hardness of the insulating barrier of compressed-core cannot fully improve.Therefore, the vibrate powder that excitation field causes cannot be suppressed, sufficient noise suppression effect cannot be obtained.
On the other hand, known: when the addition of condensed phosphoric acid metallic compound is more than 0.20 % by weight, noise Max value reduces, and becomes low noise.The reason becoming low noise is the hardness raising of the insulating barrier of compressed-core.In addition, the dhering strength of soft magnetic powder and insulating barrier improves, and can suppress vibrate powder.When addition is more than 0.80 % by weight, noise Max value increases.Its reason is, reduces, the reduction of the L value of reactor owing to resulting from the magnetic permeability that density reduces.Thus, ripple current increases, and change in magnetic flux density increases, and thus vibrate powder increases, and noise increases.In addition, as shown in comparative example 104, when the addition of condensed phosphoric acid metallic compound is more than 0.80 % by weight, magnetic permeability or iron loss equimagnetic characteristic degradation, performance when making reactor product is insufficient, impracticable.Therefore, from the aspect of low noise effect and high strength and good magnetic characteristic, the addition of condensed phosphoric acid metallic compound is preferably 0.20 % by weight ~ 0.80 % by weight relative to soft magnetic powder.Although also can obtain sufficient characteristic value with above-mentioned addition, the addition of condensed phosphoric acid metallic compound is more preferably 0.20 % by weight ~ 0.50 % by weight.
Fig. 6 illustrates to add to be mixed with 25 % by weight magnesian aluminium dihydrogen tripolyphosphates 0.25 % by weight and the Al changed as insulation micro mist 2o 3addition time the chart of value of noise.From table 4 and Fig. 6, the addition of insulation micro mist is preferably 0.1 % by weight ~ 0.6 % by weight relative to soft magnetic powder.When addition is less than 0.1 % by weight, addition is few, and the hardness of the insulating barrier of compressed-core cannot fully improve.Therefore, the vibrate powder that excitation field causes cannot be suppressed, sufficient noise suppression effect cannot be obtained.
On the other hand, known: when the addition of insulation micro mist is more than 0.1 % by weight, noise Max value reduces, and becomes low noise.The reason becoming low noise is the hardness raising of the insulating barrier of compressed-core.In addition, the dhering strength of soft magnetic powder and insulating barrier improves, and can suppress vibrate powder.When addition is more than 0.6 % by weight, noise Max value increases.Its reason is, reduces, the reduction of the L value of reactor owing to resulting from the magnetic permeability that density reduces.Thus, ripple current increases, and change in magnetic flux density increases, and thus vibrate powder increases, and noise increases.In addition, as shown in comparative example 107, when the addition of insulation micro mist is more than 0.6 % by weight, magnetic permeability or iron loss equimagnetic characteristic degradation, performance when making reactor product is insufficient, impracticable.Therefore, from the aspect of low noise effect and high strength and good magnetic characteristic, the addition of insulation micro mist is preferably 0.1 % by weight ~ 0.6 % by weight relative to soft magnetic powder.
3. EXAMPLE III
Below, with reference to table 5 ~ table 9 and Fig. 7, embodiments of the invention III is described.
(1) project is measured
As mensuration project, following method is utilized to determine magnetic permeability and iron loss.For magnetic permeability, 1 kinking (10 circle) is implemented to each compressed-core made, uses impedance analyzer, thus calculate magnetic permeability by inductometer when 100kHz, 0.5V.
For iron loss, 1 kinking (15 circle) and 2 kinkings (3 circle) are implemented to each compressed-core, be used as the BH analyzer of magnetism measuring equipment (rock amounts to and surveys Co., Ltd.: SY-8232), under the condition of frequency 100kHz, peakflux density Bm=0.05T, calculate iron loss.In this calculating, for the frequency curve of iron loss, utilize least square method to calculate the coefficient of hysteresis, eddy current loss coefficient by above-mentioned (1) ~ (3) formula, thus carry out.About intensity, according to JIS2507, radial crushing strength is measured.
(2) manufacture method of sample
The sample used in following making Property comparison.
Hardness be 700MPa, average grain diameter is in the noncrystalline soft magnetic alloy powder of 50 μm, relative to aluminium dihydrogen tripolyphosphate mixing 0 ~ 4% condensed phosphoric acid metallic compound, this condensed phosphoric acid metallic compound mixture has 25 % by weight as the magnesium oxide of its hardening accelerator, for this mixed-powder mixed methyl phenyl system silicone resin 2.0 % by weight, the heat drying of 2 hours is carried out at 180 DEG C, further mixing 0.3 % by weight lithium stearate, as lubricant, makes prilling powder.
Be made into formed body with the pressure of 1500MPa at normal temperatures, in air atmosphere, carry out the heat treatment of 120 minutes with the temperature of 410 DEG C, make compressed-core.
(3) measurement result
The radial crushing strength of made compressed-core is shown in table 5 and Fig. 7.
[table 5]
From table 5 and Fig. 7, when the addition of condensed phosphoric acid metallic compound and its curing agent is more than 0.25 % by weight, intensity increases, can obtain effect; If addition is more than 2.0 % by weight, then density reduction, intensity also reduce.In addition, this compressed-core of increasing of working strength the reactor of the coil that reeled has the effect of low noise.
(4) Fe-6.5Si alloy powder
For hardness be 390MPa, average grain diameter is the Fe-6.5Si alloy powder of 20 μm, mixing aluminium dihydrogen tripolyphosphate+magnesium oxide 0.5 % by weight, for this mixed-powder mixed methyl phenyl system silicone resin 1.8 % by weight, carry out the heat drying of 2 hours at 180 DEG C, mixing 0.6 quality % zinc stearate is as lubricant further.
At room temperature with the pressure of 1500MPa, extrusion forming is carried out to it, make the ring-type formed body of external diameter 16mm, internal diameter 8mm, height 5mm.In addition, at nitrogen atmosphere (N 2) in 700 DEG C, the heat treatment of 120 minutes is carried out to this formed body, make compressed-core.
[table 6]
From this embodiment, by adding aluminium dihydrogen tripolyphosphate and the magnesium oxide as hardening accelerator, intensity increases.In addition, this compressed-core of increasing of working strength the reactor of the coil that reeled has the effect of low noise.
(5) pure iron and sendust
As soft magnetic powder, the pure iron that use hardness is 30MPa and the sendust that hardness is 100MPa, make compressed-core under condition similar to the above.The relation of their content of binder and three-point bending strength and iron loss is shown in table 7.
[table 7]
From the No.A1 ~ A3 of table 7, effect cannot be obtained when hardness is the pure iron of 30MPa.When hardness is the sendust of 100MPa, as B2, low-melting glass powder makes magnetic hysteresis loss increase.From B3, B4, when adding aluminium dihydrogen tripolyphosphate in sendust, intensity is high.Compared with C2, C3, in sendust, with the addition of aluminium dihydrogen tripolyphosphate and increase as the intensity of the magnesian product of its curing agent.In addition, this compressed-core of increasing of working strength the reactor of the coil that reeled has the effect of low noise.
4. EXAMPLE IV
Below, be described with reference to table 8 ~ table 12 and Fig. 8 ~ 13 couple embodiments of the invention IV.
(1) project is measured
As mensuration project, following method is utilized to determine magnetic permeability and iron loss.1 kinking (15 circle) and 2 kinkings (3 circle) are implemented to each compressed-core, be used as the BH analyzer of magnetism measuring equipment (rock amounts to and surveys Co., Ltd.: SY-8232), under the condition of frequency 100kHz, peakflux density Bm=0.05T, measure iron loss and amplitude permeability.If excitation field is now set to Hm, then can obtain the peak swing magnetic permeability of μ=Bm/Hm.In the calculating of iron loss, for the frequency curve of iron loss, utilize least square method to calculate the coefficient of hysteresis, eddy current loss coefficient by above-mentioned (1) ~ (3) formula, thus carry out.About intensity, according to JIS2507, radial crushing strength is measured.
(2) manufacture method of core
The sample used in following making Property comparison.
For the composite magnetic powder that the amorphous alloy powder utilizing water atomization to make shown in (b) of the Fe base amorphous comminuted powder shown in (a) of Fig. 8 and Fig. 8 is mixed according to the ratio of 60:40, lithium stearate 0.3 % by weight, aluminium dihydrogen tripolyphosphate as the magnesium oxide 25 % by weight of hardening accelerator is mixed with using the addition of table 1, for this mixed-powder mixed silanes coupling agent 0.05 % by weight, methylbenzene base system silicone resin 2.0 % by weight, carry out the heat drying of 2 hours at 150 DEG C.
Make it be the sieve of 350 μm by sieve aperture, mixing 0.3 % by weight lithium stearate is as lubricant.At room temperature with the pressure of 1500MPa, extrusion forming is carried out to it, make the ring-type powder compact of external diameter 16mm, internal diameter 8mm, height 5mm, in oxygen atmosphere (air), implement the heat treatment of 120 minutes in 410 DEG C, make the core of embodiment 11 ~ the 16 and comparative example 13,14 formed by compressed-core.
As comparative example 11, making and with the addition of 1.5 % by weight average grain diameters is that the bismuth system low-melting glass of 1.1 μm is as the core of Strength enhancing materials; As comparative example 2, make the core not adding reinforcing material completely.
(3) measurement result
The radial crushing strength of made core is shown in table 8 and Figure 10.
[table 8]
From table 8 and Figure 10, when the addition of condensed phosphoric acid metallic compound and its curing agent is more than 0.25 % by weight, intensity increases, and can obtain effect; If addition is more than 2.0 % by weight, then density reduction, intensity also reduce.Because manufactured core needs to reel the operation of coil in operation thereafter, thus need the radial crushing strength of more than 10MPa, the core that the scope 0.25 % by weight ~ 2.0 % by weight with the addition of the embodiment 11 ~ 16 of aluminium dihydrogen tripolyphosphate all possesses sufficient radial crushing strength in practicality.Particularly, with do not add reinforcing material comparative example 12 or separately using low-melting glass compared with the comparative example 11,12 of reinforcing material, can be confirmed that by these data the radial crushing strength of the core of embodiment 11 ~ 16 is especially excellent.In addition, the excellent described compressed-core of radial crushing strength is used and the reactor of the coil that reeled has the effect of low noise.
About magnetic permeability μ a, as shown in table 8 and Figure 11, the core that scope 0.25 % by weight ~ 2.0 % by weight with the addition of the embodiment 11 ~ 16 of aluminium dihydrogen tripolyphosphate with use low-melting glass as reinforcing material comparative example 11 compared with, very excellent as embodiment 11 ~ 13, or almost equal performance is demonstrated as embodiment 14 ~ 16.
About loss Pcv, as shown in table 8 and Figure 12, the core that scope 0.25 % by weight ~ 2.0 % by weight with the addition of the embodiment 11 ~ 16 of aluminium dihydrogen tripolyphosphate with use low-melting glass as reinforcing material comparative example 11 compared with, very excellent as embodiment 14 ~ 16, or almost equal performance is demonstrated as embodiment 11 ~ 13.
If consider these all conditions, about the addition of aluminium dihydrogen tripolyphosphate, when being 1.5 % by weight ~ 2.0 % by weight in the scope of 0.25 % by weight ~ 2.0 % by weight, radial crushing strength, magnetic permeability μ a are all excellent compared with the reinforcing material of low-melting glass with loss Pcv, are preferred scopes.
(4) other composite magnetic powder
For the composite magnetic powder that the amorphous alloy powder utilizing water atomization to make shown in (a) of the Fe base amorphous aqueous vapor body atomized powder shown in (b) of Fig. 8 and Fig. 9 is mixed according to the ratio of 70:30, lithium stearate 0.3 % by weight, aluminium dihydrogen tripolyphosphate as the magnesium oxide 25 % by weight of hardening accelerator is mixed with using the addition of table 9, for this mixed-powder mixed silanes coupling agent 0.05 % by weight, methylbenzene base system silicone resin 2.0 % by weight, carry out the heat drying of 2 hours at 150 DEG C.
Make it be the sieve of 350 μm by sieve aperture, mixing 0.3 % by weight lithium stearate is as lubricant.At room temperature with the pressure of 1500MPa, extrusion forming is carried out to it, make the ring-type powder compact of external diameter 16mm, internal diameter 8mm, height 5mm, in oxygen atmosphere (air), implement the heat treatment of 120 minutes in 410 DEG C, make the core of the embodiment 17 formed by compressed-core.
As comparative example 15, making and with the addition of 1.5 % by weight average grain diameters is that the bismuth system low-melting glass of 1.1 μm is as the core of Strength enhancing materials.
[table 9]
From this embodiment, with the addition of aluminium dihydrogen tripolyphosphate and as in the magnesian embodiment 17 of hardening accelerator, with use low-melting glass as the comparative example 15 of reinforcing material core compared with, intensity improves.But if compared with the addition of the embodiment 14 of 1.5 % by weight aluminium dihydrogen tripolyphosphates, the intensity of the comminuted powder of embodiment 14 is stronger, Pcv is also lower in loss.As mentioned above, this compressed-core is used and the reactor of the coil that reeled has the effect of low noise.
(5) opportunity is mixed
As comparative example 16, for the composite magnetic powder that the amorphous alloy powder utilizing water atomization to make shown in (b) of the Fe amorphous comminuted powder shown in (a) of Fig. 8 and Fig. 9 is mixed according to the ratio of 60:40, mix 0.3 % by weight lithium stearate, for this mixed-powder mixed silanes coupling agent 0.05 % by weight, methylbenzene base system silicone resin 2.0 % by weight, carry out the heat drying of 2 hours at 150 DEG C.
Make it be the sieve of 350 μm by sieve aperture, mixing aluminium dihydrogen tripolyphosphate, is mixed with the lithium stearate 0.3 % by weight as lubricant, the magnesium oxide 25 % by weight as hardening accelerator in this aluminium dihydrogen tripolyphosphate.
At room temperature with the pressure of 1500MPa, extrusion forming is carried out to it, make the ring-type powder compact of external diameter 16mm, internal diameter 8mm, height 5mm, in oxygen atmosphere (air), implement the heat treatment of 120 minutes in 410 DEG C, make the core of compressed-core.
[table 10]
As shown in Table 10, if compare with the comparative example 16 being mixed with aluminium dihydrogen tripolyphosphate after mixing silicone resin the embodiment 14 being mixed with aluminium dihydrogen tripolyphosphate prior to silicone resin, when rear mixing aluminium dihydrogen tripolyphosphate, loss Pcv and radial crushing strength cannot give play to large effect.
The mixed ratio of (6) the 1st noncrystalline soft magnetic powders and the 2nd noncrystalline soft magnetic powder
Utilize the method same with above-described embodiment, as shown in table 11 such change the 1st noncrystalline soft magnetic powder and the 2nd noncrystalline soft magnetic powder circularity and containing proportional, and determine its characteristic.In table 11, A refers to: make the 1st noncrystalline soft magnetic powder be comminuted powder, make the 2nd noncrystalline soft magnetic powder be the powder utilizing water atomization to obtain, according to 80:20 to 40:60 5 phasic changes its containing proportional, each ratio is added to the aluminium dihydrogen tripolyphosphate of 1.5 % by weight.
B refers to: make the 1st noncrystalline soft magnetic powder be comminuted powder, the 2nd noncrystalline soft magnetic powder is made to be the powder utilizing water atomization to obtain, according to the 50:50 of 70:30 3 phasic changes its containing proportional, each ratio is added to the aluminium dihydrogen tripolyphosphate of 2.0 % by weight.
C refers to: make the 1st noncrystalline soft magnetic powder be the powder utilizing water gas atomization to obtain, the 2nd noncrystalline soft magnetic powder is made to be the powder utilizing water atomization to obtain, making it contain proportional is 70:30, it is added to the aluminium dihydrogen tripolyphosphate of 1.5 % by weight.
[table 11]
From the chart of table 11 and Figure 13, when the combination of comminuted powder with the powder that utilizes water atomization to obtain, no matter aluminium dihydrogen tripolyphosphate is any one in 1.5 % by weight or 2.0 % by weight, when the 1st noncrystalline soft magnetic powder and the 2nd noncrystalline soft magnetic powder containing proportional be 70:30 to 60:40, radial crushing strength is excellent all especially.In addition, with use low-melting glass as reinforcing material comparative example 15 compared with, the radial crushing strength of embodiment 18 ~ 26 is also all especially excellent.
(7) low-melting glass+aluminium dihydrogen tripolyphosphate
When utilizing same with above-described embodiment method manufacture core, using being used alone the comparative example 15 of low-melting glass as intensity enhancing parts, be used alone aluminium dihydrogen tripolyphosphate as the embodiment 20 during intensity enhancing parts and low-melting glass and aluminium dihydrogen tripolyphosphate are combinationally used comparing of embodiment 27,28 be shown in table 12.
[table 12]
From this table 12, compared with the embodiment 27,28 low-melting glass and aluminium dihydrogen tripolyphosphate combinationally used and the embodiment 20 being used alone aluminium dihydrogen tripolyphosphate, its radial crushing strength especially increases.As mentioned above, the excellent described compressed-core of radial crushing strength is used and the reactor of the coil that reeled has the effect of low noise.

Claims (25)

1. a soft magnetic powder composition, it is characterized in that, soft magnetic powder is mixed with the condensed phosphoric acid metallic compound relative to described soft magnetic powder being 0.50 % by weight ~ 2.0 % by weight, around this soft magnetic powder, defines the coating of described condensed phosphoric acid metallic compound.
2. soft magnetic powder composition as claimed in claim 1, it is characterized in that, described condensed phosphoric acid metallic compound is condensation of aluminum phosphate.
3. soft magnetic powder composition as claimed in claim 2, it is characterized in that, described condensation of aluminum phosphate is the single component of aluminium triphosphate or aluminium metaphosphate or the mixture of aluminium triphosphate and aluminium metaphosphate.
4. the soft magnetic powder composition according to any one of claims 1 to 3, is characterized in that, in described condensed phosphoric acid metallic compound, be added with alkaline matter as hardening accelerator,
Described alkaline matter is Al 2o 3, SiO 2, MgO, Mg (OH) 2, CaO, Ca (OH) 2, asbestos, talcum, at least one in flying dust.
5. soft magnetic powder composition as claimed in claim 4, it is characterized in that, described hardening accelerator with the addition of 10 % by weight ~ 30 % by weight relative to described condensed phosphoric acid metallic compound.
6. a core, it is for by the soft magnetic powder composition according to any one of the claims 1 ~ 5 shaping and form.
7. a core, it is soft magnetic powder is shaping and core that is that form, it is characterized in that, the surface of described soft magnetic powder cover by silicon dioxide layer, described silicon dioxide layer comprise relative to described soft magnetic powder be 0.5 % by weight ~ 2.0 % by weight condensed phosphoric acid metallic compound.
8. a lower-noise reactor, is characterized in that, it is formed the claims 6 or core according to claim 7 winding coil.
9. a soft magnetic powder composition, it is characterized in that, soft magnetic powder is mixed with the condensed phosphoric acid metallic compound relative to described soft magnetic powder being 0.25 % by weight ~ 2.0 % by weight, around this soft magnetic powder, defines the coating of described condensed phosphoric acid metallic compound.
10. soft magnetic powder composition as claimed in claim 9, it is characterized in that, the powder hardness of described soft magnetic powder is more than 100MPa.
11., as claim 9 or soft magnetic powder composition according to claim 10, is characterized in that, described condensed phosphoric acid metallic compound is condensation of aluminum phosphate.
12. soft magnetic powder composition as claimed in claim 11, is characterized in that, described condensation of aluminum phosphate is the single component of aluminium triphosphate or aluminium metaphosphate or the mixture of aluminium triphosphate and aluminium metaphosphate.
13. 1 kinds of soft magnetic powder composition, it is characterized in that, soft magnetic powder is mixed with the condensed phosphoric acid metallic compound relative to described soft magnetic powder being 0.20 % by weight ~ 0.80 % by weight, further mix insulation micro mist, defines the coating comprising described condensed phosphoric acid metallic compound around this soft magnetic powder.
14. soft magnetic powder composition as claimed in claim 13, is characterized in that, described insulation micro mist is 0.1 % by weight ~ 0.6 % by weight relative to described soft magnetic powder.
15., as claim 13 or soft magnetic powder composition according to claim 14, is characterized in that, described insulation micro mist is Al 2o 3.
16. soft magnetic powder composition according to any one of claim 13 ~ 15, it is characterized in that, described condensed phosphoric acid metallic compound is condensation of aluminum phosphate.
17. soft magnetic powder composition as claimed in claim 16, is characterized in that, described condensation of aluminum phosphate is the single component of aluminium triphosphate or aluminium metaphosphate or the mixture of aluminium triphosphate and aluminium metaphosphate.
18. 1 kinds of soft magnetic powder composition, it is characterized in that, relative to the condensed phosphoric acid metallic compound of described noncrystalline soft magnetic powder mixing 0.25 % by weight ~ 2.0 % by weight in noncrystalline soft magnetic powder, around described noncrystalline soft magnetic powder, define the coating of described condensed phosphoric acid metallic compound.
19. soft magnetic powder composition as claimed in claim 18, it is characterized in that, described noncrystalline soft magnetic powder is the composite magnetic powder the 1st noncrystalline soft magnetic powder and the 2nd noncrystalline soft magnetic powder are obtained by mixing, described 1st noncrystalline soft magnetic powder has specific average grain diameter, and described 2nd noncrystalline soft magnetic powder is made up of the noncrystalline that average grain diameter is less than the average grain diameter of described 1st noncrystalline soft magnetic powder.
20., as claim 18 or soft magnetic powder composition according to claim 19, is characterized in that, described 1st noncrystalline soft magnetic powder is comminuted powder, and described 2nd noncrystalline soft magnetic powder is the soft magnetic powder utilizing atomization to obtain.
21. soft magnetic powder composition according to any one of claim 18 ~ 20, it is characterized in that, described condensed phosphoric acid metallic compound is condensation of aluminum phosphate.
22. soft magnetic powder composition as claimed in claim 21, is characterized in that, described condensation of aluminum phosphate is the single component of aluminium triphosphate or aluminium metaphosphate or the mixture of aluminium triphosphate and aluminium metaphosphate.
23. soft magnetic powder composition according to any one of claim 18 ~ 22, is characterized in that, in described condensed phosphoric acid metallic compound, be added with alkaline matter as hardening accelerator,
Described alkaline matter is Al 2o 3, SiO 2, MgO, Mg (OH) 2, CaO, Ca (OH) 2, asbestos, talcum, at least one in flying dust.
24. soft magnetic powder composition according to any one of claim 18 ~ 23, is characterized in that, except described condensed phosphoric acid metallic compound, also added low-melting glass as reinforcing material.
25. 1 kinds of cores, it is for by the soft magnetic powder composition according to any one of the claims 18 ~ 24 shaping and form.
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