CN103959405A - Composite soft magnetic material and production method therefor - Google Patents
Composite soft magnetic material and production method therefor Download PDFInfo
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- CN103959405A CN103959405A CN201280059179.7A CN201280059179A CN103959405A CN 103959405 A CN103959405 A CN 103959405A CN 201280059179 A CN201280059179 A CN 201280059179A CN 103959405 A CN103959405 A CN 103959405A
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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
- H01F1/26—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 by macromolecular organic substances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
- H01F1/20—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder
- H01F1/22—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together
- H01F1/24—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys in the form of particles, e.g. powder pressed, sintered, or bound together the particles being insulated
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- 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
- H01F1/33—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 mixtures of metallic and non-metallic particles; metallic particles having oxide skin
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Abstract
Provided are a composite soft magnetic material, having favorable DC bias characteristics and high specific resistance, and a production method therefor. An inorganic insulative powder (3) and a coated powder obtained by coating a soft magnetic powder (1) that is coated with an insulative film (4) with a silicone resin (2) are uniformly mixed, and the resultant mixture is molded and fired. By uniformly mixing the inorganic insulative powder (3) and the coated powder obtained by coating the soft magnetic powder that is coated with the insulative film (4) with the silicone resin (2), rupture of the insulative film due to the inorganic insulative material when molding pressed powder is prevented. By uniformly dispersing the inorganic insulative material while high specific resistance is maintained, the gap between molded soft magnetic powder particles is uniformly maintained. As a result, a composite soft magnetic material is provided having high specific resistance and favorable DC bias characteristics.
Description
Technical field
The present invention relates to have again soft-magnetic composite material and the manufacture method thereof of good DC superposition characteristic in keeping high specific resistance.
Background technology
As the iron core of reactor etc., from just using lamination silicon sheet core, ferrite iron core and dust core in the past.In lamination silicon steel sheet, in order to prevent that eddy current from needing the magnetic silicon steel sheet attenuation as far as possible of lamination.But the sheet of magnetic silicon steel sheet is limited, in addition, also have for sheet so that cause manufacturing cost increase problem.In addition, ferrite iron core and dust core, because saturation flux density is little, therefore, can produce inductance and decline, and bring in order to avoid these problem maximizing in large current applications.
From such background, turn to the material for being used as alternative layer stack silicon sheet core, ferrite iron core and dust core, and there is the dielectric film of minute quantity, and with the soft-magnetic composite material of the method manufacturing of press-powder moulding to high-density.This soft-magnetic composite material its eddy current loss compared with lamination silicon steel sheet is little, and declines also littlely strengthening inductance when externally-applied magnetic field, and has expeditiously good DC superposition characteristic.In addition, compare with dust core with ferrite iron core and also have advantages of and can under large current conditions, use.
Manufacturing when this soft-magnetic composite material, in order to obtain good magnetic force, therefore, how dielectric film is formed on and between soft magnetic powder particle, becomes a problem.In the past, by a small amount of high more soft silicone resin of compressibility that adds, and then with after the coated soft magnetic powder particle of silicone resin, reshaping and burning till, thus be manufactured on the soft-magnetic composite material that forms dielectric film between soft magnetic powder particle.In addition, a kind of method (patent documentation 1) of manufacture is also disclosed,, mix soft magnetic powder and inorganic insulation powder, then by reshaping after coated this mixed-powder of silicone resin with burn till, thereby produce at the soft-magnetic composite material also aspect high frequency and high magnetic flux density with excellent magnetic force property.
But, need like that boosting of large electric current at the reactor to be mounted on electric automobile and compound power vehicle etc. etc., the DC superposition characteristic of soft-magnetic composite material in the past can not meet above-mentioned needs mostly, therefore, the soft-magnetic composite material of further demand DC superposition characteristic excellence.Have again, conventionally need to arrange and adjust space in order to improve DC superposition characteristic, for import space the shape of mould become complicated, and operation and parts also increase, and have had again the problem that causes manufacturing cost to increase.Further, the problem that also has the loss causing due to the leakage flux in space to increase.
In addition, in the time manufacturing soft-magnetic composite material, in order further to improve the insulating properties between soft magnetic powder particle, also have the situation with the coated soft magnetic material of insulation tunicle in advance that uses.In this situation, in the time that silicone resin is hard, owing to forming sufficient gap between soft magnetic powder particle, obtain thus good DC superposition characteristic, but can cause silicone resin breakage in the time of moulding, and then cause until the defect of the insulation tunicle of coated soft magnetic material, thereby decline and soft magnetic characteristic worsens than resistance, finally cause loss to increase.On the other hand, in the time using soft silicone resin, although can obtain good soft magnetic characteristic by high specific resistance, be difficult to remain on equably the gap between soft magnetic powder particle in the time of moulding, its result, has the problem that causes DC superposition characteristic to worsen.
Patent documentation 1 TOHKEMY 2010-2454460 communique
Summary of the invention
, the object of the invention is to for this reason, a kind of soft-magnetic composite material and preparation method thereof is provided, it can realize void-free design by addressing the above problem, thereby can not increase cost, and has high specific resistance and good DC superposition characteristic.
A kind of soft-magnetic composite material of scheme 1, it is characterized in that, by mixing equably cladding powder and inorganic insulation powder, and this mixture is carried out moulding and burns till and obtain, this cladding powder is by having been obtained by the coated soft magnetic powder of insulation tunicle with silicone resin is coated; And in the time that the total amount of described silicone resin and described inorganic insulation powder is X quality %, in section is observed, to a soft magnetic powder particle, carry out the mensuration by the thickness of the thick part of the segregation of the insulating barrier of silicone resin and inorganic insulation powder constituent in two positions, and (μ is m) below 5 times of X according to said method 20 above particles to be measured to the average segregation thickness D averaging again and obtain.
A kind of soft-magnetic composite material of scheme 2, it is characterized in that, in scheme 1, described soft magnetic powder is the straight iron powder of average grain diameter 10～100 μ m, the average grain diameter of described inorganic insulation powder is below 1 μ m, and the total amount of described silicone resin and described inorganic insulation powder is 0.3～2 quality % with respect to described soft magnetic powder.
A kind of soft-magnetic composite material of scheme 3, it is characterized in that, in scheme 2, in the total amount of described silicone resin and described inorganic insulation powder, the relatively described soft magnetic powder of the amount of described silicone resin is 0.15～1.2 quality %, and the relatively described soft magnetic powder of the amount of described inorganic insulation powder is 0.1～1 quality %.
A kind of soft-magnetic composite material of scheme 4, is characterized in that, in arbitrary scheme of scheme 1～3, described insulation tunicle is iron phosphate membrane or magnesium oxide films.
The manufacture method of a kind of soft-magnetic composite material of scheme 5, it is characterized in that, thereby by obtaining cladding powder by the coated soft magnetic powder of insulation tunicle with silicone resin is coated, then mix equably described cladding powder and inorganic insulation powder, and this mixture is carried out moulding and burnt till.
According to the present invention, due to by mixing equably cladding powder and inorganic insulation powder, this cladding powder is by by being obtained by the coated soft magnetic powder of insulation tunicle with silicone resin is coated, thereby can evenly not be attached to the outside of the silicone resin of coated soft magnetic powder aggegation inorganic insulation powder, and make the thickness segregation-free of the insulating barrier after moulding and evenly, and the gap between soft magnetic powder particle is maintained at constant, therefore, provided the soft-magnetic composite material with high specific resistance and good DC superposition characteristic.In addition, soft-magnetic composite material of the present invention is owing to having high specific resistance value and can suppress eddy current loss, therefore, even also can use in large-scale reactor.In addition, owing to thering is good DC superposition characteristic, therefore do not need to arrange space, so do not increase manufacturing cost.Further, even in the case of using in advance by the coated soft magnetic material of insulation tunicle and soft silicone resin, also can make inorganic insulation powder be dispersed between the particle of soft magnetic powder, in the time of moulding, keep equably the gap between the particle of soft magnetic powder, thereby the soft-magnetic composite material with good DC superposition characteristic is provided.
Brief description of the drawings
The schematic diagram that Fig. 1 is the cladding powder that obtains with the coated soft magnetic powder of silicone resin.
Fig. 2 represents the silicone resin between soft magnetic powder after moulding and the schematic diagram of inorganic insulation powder.
Fig. 3 is the curve chart that represents DC superposition characteristic.
Fig. 4 is the schematic diagram of cladding powder.
Fig. 5 is the curve chart that represents DC superposition characteristic.
Fig. 6 is the bar chart that represents density.
Fig. 7 represents than the bar chart of resistance.
Fig. 8 is the bar chart that represents maximum relative permeability.
Fig. 9 is the microphotograph of section.
Figure 10 is the schematic diagram that represents the mensuration part of coated thickness.
Embodiment
Soft-magnetic composite material of the present invention is for by mixing equably cladding powder and inorganic insulation powder, and this mixture is carried out moulding and burnt till and the soft-magnetic composite material that obtains.This cladding powder is by being obtained by the coated soft magnetic powder of insulation tunicle with silicone resin is coated.In addition, the manufacture method of soft-magnetic composite material of the present invention, for by mixing equably cladding powder and inorganic insulation powder, and the manufacture method that this mixture is carried out moulding and burnt till.This cladding powder is by being obtained by the coated soft magnetic powder of insulation tunicle with silicone resin is coated.
The present invention is by mixing equably cladding powder and inorganic insulation powder, this cladding powder is by being obtained by the coated soft magnetic powder of insulation tunicle with silicone resin is coated, as shown in Figure 1, inorganic insulation powder 3 is attached to the outside of the silicone resin 2 of coated soft magnetic powder 1.Still, the 4 insulation tunicles for coated soft magnetic powder 1.Like this, by mix inorganic insulation powder after being coated soft magnetic powder with silicone resin, therefore, it is good that the dispersiveness of inorganic insulation powder becomes.Its result, as shown in Figure 2, the silicone resin after moulding and inorganic insulation powder are between soft magnetic powder, and because the gap between soft magnetic powder particle is maintained at constant, therefore, obtained the soft-magnetic composite material with high specific resistance value and good DC superposition characteristic.
The schematic of having mixed the cladding powder of inorganic insulation powder in the operation different from the present invention is shown in Fig. 4.
(a) of Fig. 4 is for mixing the cladding powder of the inorganic insulation powder in the present invention.
To this, initially, mix soft magnetic powder and inorganic insulation powder, and then the soft magnetic powder of inorganic insulation powder has been adhered in acquisition, for silicone resin being mixed and is coated on the cladding powder obtaining in these soft magnetic powders, as shown in Fig. 4 (b), inorganic insulation powder is attached to the outside of soft magnetic powder, and silicone resin is covered by its outside.
But in fact, in the mixed processes of silicone resin, the inorganic insulation powder that has been attached to soft magnetic powder separates and then is dispersed in silicone resin with the surperficial of soft magnetic powder, because the inorganic insulation powder having disperseed is in the drying process aggegation of silicone resin, as shown in Fig. 4 (b), can be coated equably.Due to this aggegation, inorganic insulation powder and silicone resin can not spread all over the surface of soft magnetic powder fully, and then cause coating film in uneven thickness, or local attenuation and then cause declining than resistance, thereby can not fully remain on the gap between soft magnetic powder particle, cause DC superposition characteristic to worsen.
In addition, initially, mix inorganic insulation powder and silicone resin and obtain the silicone resin that disperses inorganic insulation powder, for soft magnetic powder being mixed with these silicone resins and cladding powder coated and that obtain, in the mode shown in Fig. 4 (c), the mixture of silicone resin and inorganic insulation powder is covered by the outside of soft magnetic powder.
But, due to the inorganic insulation powder aggegation in the drying process of silicone resin being dispersed in silicone resin,, as shown in Fig. 4 (c), can not be coated equably actually.Due to this aggegation, inorganic insulation powder and silicone resin can not spread over the surface of soft magnetic powder fully, and then cause coating film thickness to become inhomogeneous, or local attenuation and then decline than resistance, or can not fully remain on the gap between soft magnetic powder particle, and then cause DC superposition characteristic to worsen.
On the other hand, if according to the present invention of Fig. 4 (a), soft magnetic powder particle is owing to mixing inorganic insulation powder after being coated equably by silicone resin, and then be attached to the surface of cladding powder, therefore, the aggegation of inorganic insulation powder particle can not occur, thereby coating film thickness becomes evenly and can possess high specific resistance.In addition, soft-magnetic composite material is owing to can possessing equably the gap between soft magnetic powder particle, thereby can obtain good DC superposition characteristic.
In addition, soft-magnetic composite material of the present invention is owing to having high specific resistance value and can suppress eddy current loss, even therefore also can use in large-scale reactor.In addition, owing to thering is good DC superposition characteristic, therefore do not need to arrange space, and do not increase manufacturing cost yet.Soft-magnetic composite material of the present invention, except reactor, also can utilize in fields such as transformer, choke iron core, acoustic filter, Switching Power Supply, DC/DC transducer, magnetic cartridge iron core, adjuster and motor iron cores.
At this, be used in soft magnetic powder of the present invention, it is preferably the straight iron powder that average grain diameter is 10～100 μ m.As soft magnetic powder, be the straight iron powder of 10～100 μ m by using average grain diameter, can in common manufacturing equipment, manufacture soft-magnetic composite material, and can obtain the soft-magnetic composite material with good DC superposition characteristic.
Be used in the average grain diameter of inorganic insulation powder of the present invention, it is preferably below 1 μ m.Once owing to exceeding 1 μ m, the gap between soft magnetic powder particle becomes large, and then inductance becomes too low, therefore not by preferably.
In addition, the total amount of silicone resin and inorganic insulation powder, its preferably relative soft magnetic powder is 0.3～2 quality %.If less than 0.3 quality %, because DC superposition characteristic in high galvanic areas worsens, therefore not by preferably.On the other hand, if exceed 2 quality %, due to constrictive deterioration and then cause the density of obtained soft-magnetic composite material to decline, its result, causes can not get high magnetic flux density, therefore not by preferably.
The amount of the silicone resin in the total amount of silicone resin and inorganic insulation powder, its preferably relative soft magnetic powder is 0.15～1.2 quality %.If less than 0.15 quality %, thickness attenuation and can not keep insulation, and then decline than resistance, therefore not by preferably.On the other hand, if exceed 1.2 quality %, due to constrictive deterioration and then cause the density of obtained soft-magnetic composite material to decline, can not get high magnetic flux density, therefore not by preferably.
In addition, the amount of the inorganic insulation powder in total amount, its preferably relative soft magnetic powder is 0.1～1.0 quality %.If less than 0.1 quality %, inorganic insulation powder can not spread over the surface integral of soft magnetic powder, and then can not remain on the gap between soft magnetic powder particle, DC superposition characteristic worsens, therefore not by preferably.On the other hand, if exceed 1.0 quality %, due to constrictive deterioration so that cause obtained soft-magnetic composite material density decline, not only can not get high magnetic flux density, and owing to there being the trickle inorganic insulation powder of volume between soft magnetic powder particle, cause mouldability to decline, formed body intensity declines, therefore not by preferably.
In addition, the insulation tunicle of coated soft magnetic powder its be preferably iron phosphate membrane or magnesium oxide films.This is because of by easily being obtained by the soft magnetic powder of iron phosphate membrane or the coated straight iron powder of magnesium oxide films etc., and cheap.
In addition, for burning till, it is preferably at 500 DEG C and carries out above.By firing temperature being made as more than 500 DEG C, can eliminate significantly the distortion after moulding.
In addition, as silicone resin, for example can use, methyl is silicone resin and toluene base system silicone resin.As inorganic insulation powder, for example can use silicon dioxide (tripoli, SiO
2), aluminium oxide (alumina, Al
2o
3) and magnesium oxide (magnesia, MgO).
The tissue of soft-magnetic composite material of the present invention, it is preferably the even thickness of the insulating barrier by silicone resin and inorganic insulation powder constituent between soft magnetic powder particle.
Its state, in section is observed, carries out the mensuration of the thickness of the thick part of segregation in two positions to a soft magnetic powder particle, and according to said method 20 above particles are measured, and then can differentiate by the average segregation thickness D having calculated.Be uniform state for the thickness of insulating barrier, the average segregation thickness D between soft magnetic powder particle is little, and its perfect condition is identical with the thickness of insulating barrier.On the other hand, for the thickness of insulating barrier, it is inhomogeneous state, silicone resin and inorganic insulation powder concentrate on the part of triple point etc., this structure segregation part thickening and average segregation thickness D become large, and the silicone resin of the insulating barrier between soft magnetic powder particle and inorganic insulation powder, owing to being taken by force to segregation part, the therefore thickness attenuation of insulating barrier.
Though average segregation thickness D increases and decreases with the variation of the interpolation total amount X quality % of silicone resin and inorganic insulation powder, if 5 times of X are roughly uniform state with next.
But, once average segregation thickness D exceedes 5 times of X, the segregation part thickening of insulating barrier.On the other hand, due to too attenuation of the insulating barrier between soft magnetic powder particle, insulation becomes not exclusively, and declines than resistance, or gap between soft magnetic powder particle can not fully form and cause DC superposition characteristic to worsen.
Therefore, (μ m) is preferably below 5 times of total amount X quality % of silicone resin and inorganic insulation powder to average segregation thickness D, and it is more preferably below 4 times.
Below, the specific embodiment of soft-magnetic composite material of the present invention and manufacture method thereof is illustrated.Have, the present invention is not limited to described execution mode again, also can carry out various distortion and implement.
Embodiment 1
As soft magnetic powder, it uses the water atomization straight iron powder that is implemented Phosphate coating processing (Japanese Hoeganaes Corp. manufactures S110i) of average grain diameter approximately 50 μ m.As silicone resin, use toluene base system (chemical company of SHIN-ETSU HANTOTAI manufactures KR resin).In addition, as inorganic insulation powder, use specific area is 170～180m
2the hydrophobic SiO 2 powder (the Japanese AEROSIL manufacture R974 of company) that/g, average grain diameter are about 12nm.
First, mixing equably soft magnetic powder is the silicone resin of 0.7 quality % (having removed the amount of the solute of solvent) with relative soft magnetic powder, and at 50 DEG C, carry out while stirring 5 hours dry, and then obtained the cladding powder with the coated soft magnetic powder of silicone resin.
Next, mixing equably this cladding powder is the inorganic insulation powder of 0.5 quality % with relative soft magnetic powder.At this moment powder, as shown in Figure 1, inorganic insulation powder 3 is attached to the outside of the silicone resin 2 of coated soft magnetic powder 1.Further, adding relative soft magnetic powder is the powder used in metallurgy wax base lubricant of 0.8 quality %, and by this mixture with briquetting pressure 8t/cm
2after moulding, then in the nitrogen environment of 620 DEG C, carry out burn till (embodiment A) of 30 minutes.Or mixing equably this cladding powder is the inorganic insulation powder of 1.0 quality % with relative soft magnetic powder.Further, adding relative soft magnetic powder is the powder used in metallurgy wax base lubricant of 0.8 quality %, and by this mixture with briquetting pressure 8t/cm
2after moulding, then in the nitrogen environment of 620 DEG C, carry out burn till (Embodiment B) of 30 minutes.In addition, as a comparative example, except not mixing inorganic insulation powder, other is with above-mentioned same, then burns till that (comparative example a).
By above operation, prepare respectively the annular sample of φ 35 × φ 25 × 5mm, and implement coiling (coil number N=50 circle), and by using LCR instrument (Agilent company manufactures 4248A) to measure the inductance that exchanges 10kHz in the D.C. magnetic field of 0～20kA/m, thereby evaluate DC superposition characteristic.The results are shown in Fig. 3.Embodiment A, B both, even also all low than the rate of descent of the inductance of comparative example a in wide area magnetic field range.Therefore, be confirmed to be and there is good DC superposition characteristic.
In addition, implement coiling (primary coil is counted N1=50 circle, secondary wire number of turns N2=50 circle), and while measuring the core loss (Pc) in 100mT, 10kHz, it is 21.4W/kg.In addition, under similarity condition, magnetic hysteresis loss (Ph) is 17.1W/kg, and eddy current loss (Pe) is 3.6W/kg.
Embodiment 2
On mixing the opportunity of inorganic insulation powder, it gives the density of sample, inquires into than the impact of resistance and magnetic permeability.Raw material uses raw material similarly to Example 1, its condition except clearly recording similarly to Example 1.
(1) Embodiment C
First, mixing equably soft magnetic powder is the silicone resin of 0.7 quality % with relative soft magnetic powder, and is dried while stirring, and then has obtained being coated with silicone resin the cladding powder of soft magnetic powder.
Next, mixing equably this cladding powder is the inorganic insulation powder of 0.5 quality % with relative soft magnetic powder.At this moment powder, as shown in Fig. 4 (a), inorganic insulation powder is attached to the outside of the silicone resin of coated soft magnetic powder.
Further, add the lubricant that relative soft magnetic powder is 0.8 quality %, and by this mixture with briquetting pressure 8t/cm
2or 12t/cm
2after moulding, then in the nitrogen environment of 620 DEG C, carry out 30 minutes burn till.
By above operation, preparation respectively
annular sample, and implement coiling (coil number N=50 circle), and by using LCR instrument to measure inductance, measure DC superposition characteristic.In addition, in measuring the density of sample, use BH tracer to measure maximum relative permeability.
In addition, prepare respectively the bar-shaped sample of 60 × 10 × 5mm, and measure and compare resistance value with four-terminal method.
(2) comparative example b
First, mixing equably soft magnetic powder is the inorganic insulation powder of 0.5 quality % with relative soft magnetic powder, and then has obtained adhering to the soft magnetic powder of inorganic insulation powder.
Next, mixing the soft magnetic powder that has adhered to inorganic insulation powder is equably the silicone resin of 0.7 quality % with relative soft magnetic powder, and be dried while stirring, and then obtained being coated with silicone resin the cladding powder of the soft magnetic powder that has adhered to inorganic insulation powder.At this moment powder, as shown in Fig. 4 (b), inorganic insulation powder is attached to the outside of soft magnetic powder, and silicone resin is covered by the outside of inorganic insulation powder.
Further, add the lubricant that relative soft magnetic powder is 0.8 quality %, and by this mixture with briquetting pressure 8t/cm
2or 12t/cm
2after moulding, then in the nitrogen environment of 620 DEG C, carry out 30 minutes burn till.
By above operation, preparation respectively
annular sample, and implement coiling (coil number N=50 circle), and by using LCR instrument to measure inductance, thereby measure DC superposition characteristic.In addition, in measuring the density of sample, use BH tracer to measure maximum relative permeability.
In addition, prepare respectively the bar-shaped sample of 60 × 10 × 5mm, and measure and compare resistance value with four-terminal method.
(3) comparative example c
Mix equably soft magnetic powder, soft magnetic powder is that the silicone resin of 0.7 quality % is the inorganic insulation powder of 0.5 quality % with relative soft magnetic powder relatively.And be dried while stirring, and then obtained the cladding powder with the coated soft magnetic powder of mixture of silicone resin and inorganic insulation powder.At this moment powder, as shown in Fig. 4 (c), the mixture of silicone resin and inorganic insulation powder is covered by the outside of soft magnetic powder.
And, add the lubricant that relative soft magnetic powder is 0.8 quality %, and by this mixture with briquetting pressure 8t/cm
2or 12t/cm
2after moulding, then in the nitrogen environment of 620 DEG C, carry out 30 minutes burn till.
By above operation, preparation respectively
annular sample, and implement coiling (coil number N=50 circle), and by using LCR instrument to measure inductance, thereby measure DC superposition characteristic.In addition, in measuring the density of sample, use BH tracer to measure maximum relative permeability.
In addition, prepare respectively the bar-shaped sample of 60 × 10 × 5mm, and measure and compare resistance value with four-terminal method.
(4) result
The results are shown in Fig. 5～8.Embodiment C confirms, and in wide area magnetic field range, the rate of descent of its inductance is low compared with comparative example b, c, and has good DC superposition characteristic.About density, between Embodiment C and more routine b, c, find no significant difference.About than resistance, compared with comparative example b, c, in Embodiment C, obtain significant high value.About maximum relative permeability, compared with comparative example b, c, in Embodiment C, obtain significant low value.In addition, in Embodiment C, not because briquetting pressure makes to change than resistance and maximum relative permeability.
By more than, below thing be identified,, mix equably the cladding powder that obtains with the coated soft magnetic powder of silicone resin and, inorganic insulation powder, and by by this mixture moulding with burn till, and then can obtain pressing with moulding the soft-magnetic composite material of irrelevant excellent.
Embodiment 3
About the sample of having prepared in the Embodiment C of embodiment 2 and comparative example b, by microscope, its section is observed.The results are shown in Fig. 9.The photo that (a) of Fig. 9 is Embodiment C, (b) of Fig. 9 is the photo of comparative example b.
In Fig. 9 of comparative example b (b), the common bad part (in figure, arrow part) having because the aggegation of inorganic insulation powder causes between soft magnetic powder particle.
Think because this inorganic insulation powder is assembled and segregation locally, so, inorganic insulation powder and silicone resin can not spread between soft magnetic powder particle fully, therefore, the thickness of insulating barrier becomes inhomogeneous, and then locality attenuation declines than resistance, or can not protect fully gap between soft magnetic powder particle, and then cause DC superposition characteristic to worsen.
On the other hand, in Fig. 9 of embodiments of the invention C (a), because the bad part of the aggegation by inorganic insulation powder is few, think thus, due in the present invention, inorganic insulation powder and silicone resin spread between soft magnetic powder particle fully, thereby the thickness of insulating barrier becomes evenly, and then possess high specific resistance, and, by can possess fully gap between soft magnetic powder particle, thereby obtain good DC superposition characteristic.
In addition, in order to evaluate the uniformity of thickness of the insulating barrier by silicone resin and inorganic insulation powder constituent between the soft magnetic powder particle of soft-magnetic composite material, measured average segregation thickness.
Assay method, as shown in figure 10, in section is observed, to a soft magnetic powder particle in two positions, carry out the thickness measurement by the thick part of the segregation of the insulating barrier of silicone resin and inorganic insulation powder constituent, and after the same method 20 particles are measured, and then calculated mean value.; in the insulating barrier by silicone resin and inorganic insulation powder constituent; to a soft magnetic powder particle; and the particle of soft magnetic powder arbitrarily of adjacency between in the gap that forms; measure the size of maximal clearance and the size in the 2nd large gap; and according to said method 20 particles are measured, and then calculate mean value.Its result is illustrated in table 1.
The average segregation thickness of Embodiment C is 3.8 μ m, and its value than 7.8 μ m of the average segregation thickness of comparative example b is little.Hence one can see that, and the segregation of the insulating barrier of Embodiment C between soft magnetic powder particle is little, therefore, is confirmed to be the thickness of insulating barrier for even.
[table 1]
Embodiment 4
Use various soft magnetic materials, silicone resin (silicone resin) and inorganic insulation powder, and the use level of these materials and firing temperature are changed, and then prepare soft-magnetic composite material and its performance is evaluated.The results are shown in table.In addition, in the observation of the section tissue of each soft-magnetic composite material, a soft magnetic powder particle is carried out to the mensuration by the thickness of the thick part of the segregation of the insulating barrier of silicone resin and inorganic insulation powder constituent in two positions, and according to said method 20 above particles are measured, and then (μ m) to have obtained average segregation thickness D.; in the insulating barrier by silicone resin and inorganic insulation powder constituent; to a soft magnetic powder particle; and the particle of soft magnetic powder arbitrarily of adjacency between in the gap that forms; measure the size of maximal clearance and the size in the 2nd large gap; and (μ m) according to said method 20 particles to be measured, and then obtained average segregation thickness D.Further, obtained the ratio of the average segregation thickness D of the total amount X quality % of relative silicone resin and inorganic insulation powder, i.e. D/X.The results are shown in table.Have, the preparation of soft-magnetic composite material, except the condition shown in following table, carries out under the condition same with described embodiment 1 again.As characteristic value, use than the inductance L of resistance and high magnetic area (10kA/m), and compare as the rate of descent that DC superposition characteristic applies the inductance L of 0～5.3kA/m.
[table 2]
[table 3]
As soft magnetic material, use by iron phosphate membrane or the coated material of magnesium oxide (MgO) film.As silicone resin, use the material (C in table) of material (A in table), the material (B in table) of soft (hardness 5.0MHv) of methyl system and the hard (hardness 8.9MHv) of the alkyl of methyl system of soft (the hardness 3.9MHv) of toluene base system.As inorganic insulation powder, use silicon dioxide (SiO
2), aluminium oxide (Al
2o
3) and magnesium oxide (MgO).
The average grain diameter of soft magnetic powder is 10～100 μ m, and the average grain diameter of inorganic insulation powder is below 1 μ m.The relative soft magnetic powder of total amount (interpolation total amount) of silicone resin and inorganic insulation powder is 0.3～2 quality %, and the relative soft magnetic powder of the amount of silicone resin is 0.15～1.2 quality %, the relative soft magnetic powder of amount of inorganic insulation powder is 0.1～1 quality %.The interpolation of inorganic insulation powder is after with the coated soft magnetic powder of silicone resin, and, while burning till under condition (Embodiment C～R), obtained good characteristic value more than 500 DEG C.In addition, relatively having shown the average segregation thickness D and the ratio D/X that adds total amount X quality % of the soft-magnetic composite material (Embodiment C～R) of superperformance, is all below 5.
Have again, about than resistance, because the reactor at magnetic circuit section 1 limit 50mm is decided to be (eddy current loss of intergranular)/(eddy current loss of entirety) 5%, need the ratio resistance value of 2 Ω m, so, next being judged as well of situation more than 2 Ω m.About inductance L, its value in high magnetic area (10kA/m) in the case of than the dust core of market sale high more than 10%, be judged as good.In addition, about inductance rate of descent (L rate of descent), its in the time the magnetic field of implementing coiling (coil number N=50 circle) and logical upper 10A electric current being added to the annular sample of φ 35X φ 25X5mm (magnetic field 5.3kA/m), if compared with before additional the situation of inductance rate of descent below 30% next be judged as good.Once inductance rate of descent exceedes 30%, need in design machining gap or increase parts, therefore, be not preferred.
Symbol description
1-soft magnetic powder, 2-silicone resin, 3-inorganic insulation powder, the 4-tunicle that insulate.
Claims (5)
1. a soft-magnetic composite material, it is characterized in that, by mixing equably cladding powder and inorganic insulation powder, and gained mixture is carried out moulding and burns till and obtain, this cladding powder is by having been obtained by the coated soft magnetic powder of insulation tunicle with silicone resin is coated; And in the time that the total amount of described silicone resin and described inorganic insulation powder is X quality %, in section is observed, to a soft magnetic powder particle, carry out the mensuration by the thickness of the thick part of the segregation of the insulating barrier of silicone resin and inorganic insulation powder constituent in two positions, and according to said method to 20 above particles, to measure the average segregation thickness D that averages again and obtain be X below 5 times, wherein, the unit of average segregation thickness D is μ m.
2. soft-magnetic composite material as claimed in claim 1, is characterized in that,
Described soft magnetic powder is the straight iron powder of average grain diameter 10～100 μ m, and the average grain diameter of described inorganic insulation powder is below 1 μ m, and the total amount of described silicone resin and described inorganic insulation powder is 0.3～2 quality % with respect to described soft magnetic powder.
3. soft-magnetic composite material as claimed in claim 2, is characterized in that,
In the total amount of described silicone resin and described inorganic insulation powder, the relatively described soft magnetic powder of the amount of described silicone resin is 0.15～1.2 quality %, and the relatively described soft magnetic powder of the amount of described inorganic insulation powder is 0.1～1 quality %.
4. the soft-magnetic composite material as described in any one of claim 1～3, is characterized in that,
Described insulation tunicle is iron phosphate membrane or magnesium oxide films.
5. a manufacture method for soft-magnetic composite material, is characterized in that,
Thereby by obtaining cladding powder by the coated soft magnetic powder of insulation tunicle with silicone resin is coated, then mix equably cladding powder and inorganic insulation powder, and gained mixture is carried out moulding and burnt till.
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| PCT/JP2012/084158 WO2013100143A1 (en) | 2011-12-28 | 2012-12-28 | Composite soft magnetic material and production method therefor |
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