CN103894597B - The manufacture method of the prilling powder with magnetic powder as raw material - Google Patents
The manufacture method of the prilling powder with magnetic powder as raw material Download PDFInfo
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- CN103894597B CN103894597B CN201310522829.3A CN201310522829A CN103894597B CN 103894597 B CN103894597 B CN 103894597B CN 201310522829 A CN201310522829 A CN 201310522829A CN 103894597 B CN103894597 B CN 103894597B
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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
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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
- H01F1/147—Alloys characterised by their composition
- H01F1/153—Amorphous metallic alloys, e.g. glassy metals
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Abstract
The present invention is to provide a kind of mesh screen can be used to realize stable pulverizing, thus manufacture the method for the granules with homogeneous particle diameter and the granules (Magnaglo) prepared by the method efficiently, and employ the electronic component of this Magnaglo as purpose.The invention provides the manufacture method of a kind of granules, including: mictomagnetism powder, resin, low boiling solvent, high boiling point solvent are to manufacture the mixture manufacturing step of pulp-like mixture；Heating pulp-like mixture makes the evaporation of low boiling solvent to manufacture the first drying steps of unguentum shape mixture；With mesh screen by unguentum shape mixture pulverizing also granulate to obtain the granulate step of particle；And heat up particles makes high boiling point solvent evaporate with the second drying steps obtaining magnetic particle.
Description
Technical field
The present invention, relates to the manufacture method of the metal magnetic particles of the material as compressed-core.More
In detail, relate to be mainly used in the metal magnetic grain that the electronic machine such as inductance, reactor manufactures
The manufacture method of son.
Background technology
In recent years, along with household electrical appliances and the energy-saving of electronic machine and miniaturization, for being used for this magnetic
Core, while requiring it to have high-output power, also requires that it has high power converter efficiency and little
Type.Although size is little, in order to obtain high-output power and the magnetic core of high power converter efficiency, it is known that
Improving clock frequency is more effective means.Even if therefore special demands are a kind of at high frequency region, magnetic flux
Density and pcrmeability are the highest, the material powder that iron loss is relatively low.
Up to now, the soft magnetic powder always using the mixture of ferrum and silicon is used as this magnetic core.
Typically, compressed-core, is by pressurizeing the soft magnetic powder with silicon system resin involucra
Molding, and obtained powder compact is carried out high-temperature heat treatment, makes the resin involucra degeneration of above-mentioned silicon system be
SiOx system insulator and prepared.The magnetic characteristic of the compressed-core of such gained and mechanical property, generally
Depend on as the composition of soft magnetic powder, shape, condition of molding and the heat setting out material and use
Treatment conditions etc..Accordingly, with respect to for the material of compressed-core and its manufacture method, go out up to now
Having showed various motion, such as JP 2007-12744 publication is (hereinafter referred to as " existing skill
Art 1 ") described in invention.
It addition, employ the granules of the least magnetic powder that particle diameter is 3～5 μm, it is logical
Cross and comprise (1) by magnetic powder and the manufacturing step of mixed with resin form slurry, (2) by heating, allowed
The drying steps of machine solvent volatilization and (3), by magnetic powder and the mixture of resin, are pulverized with mesh screen
And then the granulate step of granulate prepares.
On the other hand, the when of using the lamination type ceramic electron element of multilayer ceramic capacitor etc., make
With ceramic size (ceramic slurry), electric conductivity unguentum, pottery unguentum (ceramic paste)
Technology, by No. 4714996 publications of Japanese Patent No. (hereinafter referred to as " prior art 2 ") institute
Open.Here, above-mentioned ceramic size is used to ceramic green sheet forming.It addition, above-mentioned pottery
It is partially coated with electric conductivity unguentum on the principal plane of porcelain green compact thin plate, and is formed with inner conductor circuit
Element film.Further, pottery unguentum produces owing to being coated with above-mentioned electric conductivity unguentum to fill,
Difference in height between principal plane and the inner wire component thin film of ceramic green thin plate.
Further, pottery unguentum includes the 2nd ceramic powders and the 2nd resinous principle, and by carrying out the 1st
Secondary dispersion steps and the 2nd dispersion steps and be made.In the 1st dispersion steps, to low boiling
1 mixture formed by the organic solvent of point and the 2nd ceramic powders carries out dispersion process.Secondly, exist
In 2nd dispersion steps, in the 1st step, added the 2nd organic in scattered mixture
Agent, then carry out dispersion process.Ceramic powders used herein above is magnetic ceramics powder.
Prior art literature:
Patent documentation:
Patent documentation 1: Japanese Patent Laid-Open 2007-12744 publication
Patent documentation 2: No. 4714996 publications of Japanese Patent No.
Summary of the invention
Technical problem
As it has been described above, along with the miniaturization of the electronic component employing Magnaglo, the magnetic used
The particle diameter of powder also becomes less, but, it is well known that the particle diameter of Magnaglo is the least,
The adhesion of each particle is the strongest.
If using above-mentioned manufacture method, the mixture of magnetic and resin after the drying step can
Firmly it is coagulated together.Therefore, even if by obtained dried object by mesh screen, also can produce down
State problem, i.e. particle diameter becomes irregular, it is impossible to the granules obtaining uniform particle size is (following, the most also
It is referred to as " prilling powder ").
Above-mentioned conventional example 1 is outstanding technology from the point of view of following viewpoint.That is, owing to being
In 1 dispersion steps, do not add organic bond, be therefore possible to dispersion at a low viscosity
Process, it is thus possible to improve the dispersibility of ceramic powders included in pottery unguentum, and powder fully
The coagulated state of broken ceramic powders., the problem about particle size distribution it is not taken into account.
On the other hand, winding is arranged in punch die, then by prilling powder uneven for above-mentioned particle diameter
Putting into and carry out pressure forming to if manufacturing magnetics, the mobility of prilling powder can be no good, from
And cause the bad quality of products formed.And, the prilling powder that particle diameter is little enters drift and the punching of punch die
If space between mould, punch die likely weares and teares.Accordingly, there exist following problems.That is, if
If the prilling powder that use particle diameter is uneven, production efficiency can reduce.Therefore, for making efficiently
The method making the prilling powder with uniform particle size, also exists the highest social need.
Solution
The present inventor studies the most with keen determination, finally completes the present invention.
That is, the 1st form of the present invention is the manufacture method of a kind of granules, including: by Magnaglo,
Resin, low boiling solvent and high boiling point solvent are mixed together to manufacture the mixing of pulp-like mixture
Thing manufacturing step；Heat above-mentioned pulp-like mixture, make above-mentioned low boiling solvent be evaporated and manufacture
1st drying steps of unguentum shape mixture；With mesh screen, above-mentioned unguentum shape mixture is pulverized and granulate,
Thus obtain the granulate step of particle；And heat above-mentioned particle, make the evaporation of above-mentioned high boiling point solvent
Obtain the 2nd drying steps of magnetic particle.
Here, above-mentioned Magnaglo is preferably from carbonyl iron dust, noncrystalline iron powder, silicon steel, permalloy
And in the group of ferrum alusil alloy selected any one.It addition, the preferred hardening temperature of above-mentioned resin exists
The resin of more than 150 DEG C.Further, above-mentioned high boiling point solvent is preferably the 10～60 of above-mentioned amount of resin
Weight %, below preferably 10～45 weight %(, also can be referred to as " wt% ").
Above-mentioned resin preferably from by epoxy resin, phenolic resin, silicones, unsaturated polyester resin and
The group that amide resin is formed selects.
The organic solvent of the above-mentioned preferred boiling point of low boiling solvent less than 90 DEG C, above-mentioned low boiling solvent is preferred
The group being made up of butanone, acetone, toluene, ethyl acetate, benzene, methanol, ethanol and isopropanol
In any one.
The above-mentioned preferred boiling point of high boiling point solvent organic solvent in the range of 110～200 DEG C, above-mentioned height
Boiling point solvent preferably by butyl cellosolve, isobutyrone, terpineol, amylalcohol, isoamyl alcohol, two
Any one in the group that toluene and n-butyl acetate are formed.
It addition, heating-up temperature is preferably 50～60 DEG C in above-mentioned 1st drying steps, the above-mentioned 2nd
In drying steps, heating-up temperature is preferably 110～130 DEG C.Mesh screen used in above-mentioned granulate step is excellent
2～5 times of big mesh screens in the particle footpath of a diameter of above-mentioned granules of network selection eye.
In pulp-like mixture, the gross weight of relative slurry, the magnetic of 80～95 weight % is preferably used
Powder, 4～15 weight % low boiling solvent, 0.2～1.5 weight % high boiling point solvent and 1.5～
The resin of 3.5 weight %.
2nd form of the present invention is the granules manufactured by above-mentioned any means.It addition,
3rd form of the present invention is the use of the inductance of above-mentioned prepared granules.Here, it is preferred that above-mentioned electricity
Feel after assembled winding, make it harden under conditions of 150～200 DEG C.
Invention beneficial effect:
By the present invention, be on the one hand possible to prevent magnetic together with resin firmly coagulation, another
Aspect can stably be allowed to by mesh screen pulverize.Thus, it is possible to manufacture efficiently, there is homogeneous grain
The granules (hereinafter also referred to as " prilling powder ") in footpath.
Further, so obtained prilling powder, not only mobility is preferable, will not cause products formed quality
Decline, but also form die will not be damaged, production efficiency can be improved.
Accompanying drawing explanation
Fig. 1 is to represent that how the relative permeability of ring structure iron core (Troidal Core) is along with molding pressure
The increase of power and the chart that changes, these ring structure iron cores are using carbonyl iron dust or silicon steel as raw material, logical
Cross the manufacture method of granules of the present invention to manufacture prilling powder, and use these prilling powders respectively
Prepare.
Fig. 2 is to represent the Δ μ (%) of above-mentioned 2 ring structure iron cores is how to change along with the rising of frequency
Chart.
Fig. 3 A is to represent when 100kHz, the relative permeability of above-mentioned 2 ring structure iron cores be how with
And be added in the intensity in magnetic field thereon and rise and the chart that changes.
Fig. 3 B is to represent when 100kHz, the Δ μ (%) of above-mentioned 2 ring structure iron cores be how along with
The chart being added in magnetic field intensity thereon rising and change.
Fig. 4 is to represent when 50mT, the Pcv (kW/m of above-mentioned 2 ring structure iron cores3) be how along with
The rising of frequency and the chart that changes.
Detailed description of the invention
The present invention below be will be described in closer detail.As it has been described above, the present invention is to include: (A) mixture
Manufacturing step；(B) the 1st drying steps；(C) granulate step；And (D) the 2nd is dried step
The manufacture method of rapid granules.
Here, in said mixture manufacturing step, mixing (a1) Magnaglo, (a2) resin,
(a3) low boiling solvent and (a4) high boiling point solvent manufacture pulp-like mixture.It addition,
In above-mentioned 1st drying steps, (b1) heats above-mentioned pulp-like mixture, and (b2) makes above-mentioned low
Boiling point solvent evaporates, and (b3) manufactures unguentum shape mixture.Then, in above-mentioned granulate step, (c1)
With mesh screen pulverize above-mentioned unguentum shape mixture, (c2) granulate and obtain particle.Finally, above-mentioned
In two drying steps, (d1) heats above-mentioned particle, and (d2) makes above-mentioned high boiling point solvent evaporate, from
And obtain magnetic particle.
Here, as above-mentioned Magnaglo, it is possible to use carbonyl iron dust (Carbonyl Iron Powder,
Hereinafter also referred to " CIP "), noncrystalline straight iron powder, silicon steel, permalloy (Permalloy) and ferrum
Alusil alloy (Sendust Alloy) etc..
CIP, is the iron powder of spherical shape homogenizing, has the particle size distribution of diameter 1～8 μm.Noncrystalline pure
Iron powder, is the one of the low-loss metal material not having crystal structure, and it is as main one-tenth using Fe
The Fe base amorphous metal material divided, compared with orientation silicon steel plate, has the characteristic that non-loaded loss is little.
Silicon steel is containing the soft magnetic material of about 3% silicon in ferrum, and it is higher that it has pcrmeability, resistance,
The less characteristic of magnetic hystersis loss.
Permalloy is iron-nickel alloy, and is non-retentive alloy, is again strong magnetic material.It has
Magnetic conductivity is the highest, magnetic flux easily by character.
Ferrum alusil alloy is the one of the alloy with high magnetic permeability.Comprise 9.5% silicon, 55.5%
The ferroalloy of aluminum, has the high magnetic permeability being equal to mutually with permalloy.Additionally saturation flux density is the most very
High.Because stone and crisp, there is the characteristic being difficult to the processing such as forging and extension.
In above-mentioned Magnaglo, owing to pcrmeability is high, direct current overlapping features can be improved, it is advantageous to
Use CIP.
Above-mentioned resin can use as the binding agent of bonding Magnaglo.Hardening temperature 150 DEG C
Above thermosetting resin due to heat-resist, intensity is high, can be used as this resin.Specifically, may be used
To use epoxy resin (Epoxy Resin), silicones (Silicone), phenolic resin (Phenol
Formaldehyde Resin), unsaturated polyester resin (Unsaturated Polyester Resin) and
Amino resins (Amino Resin) etc..
Above-mentioned low boiling solvent is in order to improve resin dispersion in magnetic powder and to use.
In order to increase the kind of the solvent used as low boiling solvent, it is advantageous to boiling point is 90 DEG C
Following organic solvent.For ease of processing and relatively reliable, this low boiling solvent can be from by butanone
(Methyl Ethyl Ketone), acetone (Acetone), toluene (Toluene), ethyl acetate
(Ethyl Acetate), benzene (Benzene), methanol (Methanol), ethanol (Ethanol)
The group formed with isopropanol (Isopropanol) selects any one.Among these, due to it relatively
High volatility and be prone to make manufacturing time shorten, so further preferably using butanone and acetone.
Above-mentioned high boiling point solvent is in order to manufacture the prilling powder of homogeneous particle size distribution and to use.
This is in order to the most volatile in the 1st drying steps, and temperature in this step is not reaching to tree
Fat starts the temperature of hardening, it is advantageous to the organic solvent that boiling point is in the range of 110～200 DEG C.Especially
Solvent that boiling point be 145～175 DEG C scopes is preferably used.
From being easily handled and reliability, this kind of high boiling point solvent is preferably by butyl cellosolve (Butyl
Cellosolve), isobutyrone (Diisobutyl Ketone), terpineol (Terpineol),
Amylalcohol (Pentanol), isoamyl alcohol (Isopentanol), dimethylbenzene (Xylene), and n-acetic acid
The group that butyl ester (n Butyl Acetate) is formed is selected any one.Wherein, due to steam
Pressure is high, and drying-granulating powder can be made to be dried with the lower temperature of about 110～130 DEG C, so entering
One step is preferably used butyl cellosolve (Butyl Cellosolve) and isobutyrone (Diisobutyl
Ketone)。
It is mixed together to manufacture by above-mentioned resin, low boiling solvent and high boiling point solvent and Magnaglo
Slurry.For making resin and Magnaglo can mix equably and disperse, the resin concentration in this slurry is excellent
Elect 1.5～3.5 weight % of the gross weight of slurry as.By using this scope, resin energy can be made
It is scattered in fully in Magnaglo.Further, for the prilling powder of homogenizing can be obtained, the tree in slurry
2.6～3.4 weight % of lipid concentration, preferably slurry gross weight.
It addition, in order to improve resin dispersibility in the slurry and shorten the activity duration, the height in slurry
400～500 weight % of the weight of boiling point solvent and the gross weight of low boiling solvent, preferably resin.
In order to obtain the unguentum of state described later, with in order to unguentum described later can keep soft when pelletize
Soft state, the amount of the high boiling point solvent used the when of manufacturing slurry is preferably weight resin
10～45 weight %.
Further, for the prilling powder of homogenizing can be obtained, the amount of high boiling point solvent more preferably resin
20～30 weight % of weight.
In other words, this pulp-like mixture, relative to the gross weight to slurry, it is preferably used
The Magnaglo of 80～95 weight %, 4～15 low boiling solvent, 0.2～1.5 weight % of weight %
The resin of high boiling point solvent and 1.5～3.5 weight % manufactures.
Further, for the prilling powder of homogenizing can be obtained, this slurry, further preferably use 80～90
The Magnaglo of weight %, the low boiling solvent of 6.9～14.2 weight %, the high boiling of 0.5～1.0 weight %
Point solvent, and the resin of 2.6～3.4 weight %.
Slurry obtained as described above is dried 15～30 minutes at about 50～60 DEG C, and makes low boiling
Solvent evaporates and prepares unguentum.That is, unguentum is to include Magnaglo, resin and high boiling point solvent, and
Will not firmly coagulation be together between Magnaglo.
This unguentum broken granulate is wiped with mesh screen (metal gauze).It is preferably used and there is target prilling powder
The above-mentioned mesh screen of mesh diameter of 2～5 times of particle diameter.Further, in order to obtain homogenizing, desired
The prilling powder of particle diameter, so further preferably having 2～4 times of the particle diameter of target prilling powder
The mesh screen of mesh diameter.
Such as, if using mesh diameter to be about the sieve of 200～500 μm, about 100 μm can be obtained
The prilling powder of particle diameter.
The state keeping the resin in above-mentioned unguentum to harden, heats the crushed and unguentum of granulate,
Evaporate high boiling point solvent and carry out pelletize.And specifically, it is preferable to be heated to the temperature in the range of 110～130 DEG C
Degree.As previously discussed, the prilling powder having uniform particle size can just be obtained.It addition, with the side of the present invention
The prilling powder that method prepares, because being coated with resin on Magnaglo, the therefore intensity meeting after thermmohardening
While being improved, insulating properties is also improved.Further, rust-proof effect is the most fine.
Then, electronic component is manufactured with prilling powder prepared above.Below by with manufacturing inductance
As a example by situation, illustrate.
First, the above-mentioned prilling powder of ormal weight is put in punch die.Here, desired volume will have been wound
The winding of number assembles, and is then placed in prilling powder, covers winding.Pressurize to punch die, with pelletize
The temperature more than temperature that resin in powder can harden, the time desired by heating, makes hardening of resin.
Heating-up temperature preferably 150～200 DEG C.Further, when resin is epoxy resin preferably 150 DEG C, tree
When fat is silicones preferably 200 DEG C.
The prilling powder of the present invention is because mobility is fine, and dispersity have also been obtained raising, so
Packed density can be improved when putting into punch die.It is possible to improve pcrmeability, make according to above-mentioned simultaneously
The when of making electronic component, yield rate also can be improved.
Embodiment:
Hereinafter, the present invention will be illustrated in greater detail by embodiment.It addition, the invention is not limited in
Below example.
The manufacture of (embodiment 1) example of the present invention 1～3 prilling powder
Using particle diameter in the present invention is that the carbonyl iron dust of 3～5 μm is as Magnaglo.This iron powder
Consist of Fe: Si: Cr=100:0:0.With the sieve that mesh diameter is 255～500 μm by this magnetic
Property powder classification.
And employ the thermosetting epoxy resin that vitrification point is 130～140 DEG C.Use butanone respectively
As low boiling solvent, use butyl cellosolve as high boiling point solvent.
The butanone of 15.0g and the butyl cellosolve of 1.0g and the ring of 3.2g is mixed in the cup of macromolecule
Epoxy resins, and be sufficiently stirred for making mixed liquor.(ratio of their mixing is total relative to slurry
Weight, butanone accounts for 12%(w/w), butyl cellosolve accounts for about 1%(w/w), epoxy resin accounts for about 2%
(w/w).
Then, the carbonyl iron dust of 100g is mixed with above-mentioned whole blended liquid phases, is sufficiently stirred for making ring
Epoxy resins is sufficiently dispersed in carbonyl iron dust, manufactures slurry.The mixed proportion of carbonyl iron dust, phase
For the gross weight of slurry, about 85% (w/w).
Then, this slurry is put into high temperature groove, heat 30 points with about 50 DEG C (the 1st baking temperatures)
Clock makes butanone evaporate, thus prepares soft solid-state unguentum.
Then, with the mesh screen (sieve) that mesh diameter is 355 μm, wipe this unguentum broken, thus obtain
Particle.
Then, particle obtained above is put into high temperature groove, add with 110 DEG C (the 2nd baking temperatures)
Heat makes methyl cellosolve evaporate in 25～35 minutes, and granulate, thus has obtained pelletizing.
As it has been described above, just obtained the prilling powder of example 1 of the present invention.As obtained above to example 1 of the present invention
The particle diameter of prilling powder, when measuring with sieve, particle diameter is discontented with the particle (D of 75 μmS) content
It is about 5%, more than the particle (D of 500 μmL) content be about 10%, mean diameter about 100 μm.
The manufacture of the prilling powder of (embodiment 2) example 2 of the present invention
In addition to the 2nd baking temperature in embodiment 1 is changed to 120 DEG C, remaining and embodiment 1
Equally, the prilling powder of example 2 of the present invention thus has just been obtained.Obtained example of the present invention 2 pelletizing
D in endSAnd DLRatio, and mean diameter is same as in Example 1.
The manufacture of the prilling powder of (embodiment 3) example 3 of the present invention
In addition to the 2nd baking temperature in embodiment 1 is changed to 130 DEG C, remaining and embodiment 1
Equally, the prilling powder of example 3 of the present invention thus has just been obtained.Obtained example of the present invention 3 pelletizing
D in endSAnd DLRatio and mean diameter same as in Example 1.
The manufacture of the prilling powder of (embodiment 4) example 4 of the present invention
Except by the 1st baking temperature in embodiment 1 from about 50 DEG C bring up to about 60 DEG C in addition to, remaining
Similarly to Example 1, the prilling powder of example 4 of the present invention thus has just been obtained.The obtained present invention
D in example 4 prilling powderSAnd DLRatio and mean diameter same as in Example 1.
The manufacture of the prilling powder of (embodiment 5) example 5 of the present invention
Except by the 1st baking temperature in embodiment 2 from about 50 DEG C bring up to about 60 DEG C in addition to, remaining
Similarly to Example 2, the prilling powder of example 5 of the present invention thus has just been obtained.The obtained present invention
D in example 5 prilling powderSAnd DLRatio and mean diameter same as in Example 1.
The manufacture of the prilling powder of (embodiment 6) example 6 of the present invention
Except by the 1st baking temperature in embodiment 3 from about 50 DEG C bring up to about 60 DEG C in addition to, remaining
Similarly to Example 3, the prilling powder of example 6 of the present invention thus has just been obtained.The obtained present invention
D in example 6 prilling powderSAnd DLRatio and mean diameter same as in Example 1.
The manufacture of the prilling powder of (embodiment 7) example 7 of the present invention
Except the addition of the high boiling point solvent relative to resin in embodiment 2 is changed from 30wt%
Beyond 10wt%, remaining similarly to Example 2, thus has just obtained the pelletizing of example 7 of the present invention
End.The obtained D in example of the present invention 7 prilling powderSRatio be about 9%, DLRatio be about
11%。
The manufacture of the prilling powder of (embodiment 8) example 8 of the present invention
Except the addition of the high boiling point solvent relative to resin in embodiment 2 is changed from 30wt%
Beyond 20wt%, remaining similarly to Example 2, thus has just obtained the pelletizing of example 8 of the present invention
End.The obtained D in example of the present invention 8 prilling powderSRatio be about 7%, DLRatio be about
11%.Prilling powder 1 obtained by the character of the prilling powder of example 8 of the present invention and embodiment 1 is substantially
Upper identical.
The manufacture of the prilling powder of (embodiment 9) example 9 of the present invention
Except the addition of the high boiling point solvent relative to resin in embodiment 2 is changed from 30wt%
Beyond 40wt%, remaining similarly to Example 2, thus has just obtained the pelletizing of example 9 of the present invention
End.The obtained D in example of the present invention 9 prilling powderSRatio be about 4%, DLRatio be about
14%。
The manufacture of the prilling powder of (embodiment 10) example 10 of the present invention
Except the addition of the high boiling point solvent relative to resin in embodiment 2 is changed from 30wt%
Beyond 45wt%, remaining similarly to Example 2, thus has just obtained the pelletizing of example 10 of the present invention
End.The obtained D in example of the present invention 10 prilling powderSRatio be about 4%, DLRatio be
About 18%.
The manufacture of the prilling powder of (embodiment 11) example 11 of the present invention
Except the addition of the low boiling solvent relative to resin in embodiment 2 is changed from 350wt%
Beyond 250wt%, remaining similarly to Example 2, thus has just obtained the pelletize of example 11 of the present invention
Powder.
The manufacture of the prilling powder of (embodiment 12) example 12 of the present invention
Except the addition of the low boiling solvent relative to resin in embodiment 2 is changed from 350wt%
Beyond 450wt%, remaining similarly to Example 2, thus has just obtained the pelletize of example 12 of the present invention
Powder.
The manufacture of the prilling powder of (embodiment 13) example 13 of the present invention
Except changing the high boiling point solvent of inner for embodiment 2 use into propylene glycol monomethyl ether from butyl cellosolve
In addition, remaining similarly to Example 2, thus has just obtained the prilling powder of example 13 of the present invention.
The manufacture of the prilling powder of (embodiment 14) example 14 of the present invention
Except changing the high boiling point solvent of inner for embodiment 2 use into hexamethylene from butyl cellosolve
(cyclohexane), beyond, remaining similarly to Example 2, thus has just obtained example 14 of the present invention
Prilling powder.
The manufacture of the prilling powder of (embodiment 15) example 15 of the present invention
Except changing the high boiling point solvent of inner for embodiment 2 use into isobutyrone from butyl cellosolve
In addition, remaining similarly to Example 2, thus has just obtained the prilling powder of example 15 of the present invention.
The manufacture of the prilling powder of (embodiment 16) example 16 of the present invention
Except changing the low boiling solvent of inner for embodiment 2 use into acetone from butanone, and will be relative to resin
The weight set of low boiling solvent be beyond 250wt%, remaining similarly to Example 2, thus must
Arrive the prilling powder of example 16 of the present invention.
The manufacture of the prilling powder of (embodiment 17) example 17 of the present invention
Except by the low boiling solvent of inner for embodiment 2 use in addition to butanone changes acetone into, remaining with
Embodiment 2 is same, thus has just obtained the prilling powder of example 17 of the present invention.
The manufacture of the prilling powder of (embodiment 18) example 18 of the present invention
Except changing the low boiling solvent of inner for embodiment 2 use into acetone from butanone, and will be relative to tree
The weight set of the low boiling solvent of fat is beyond 450wt%, remaining similarly to Example 2, thus just
Obtain the prilling powder of example 18 of the present invention.
The manufacture of the prilling powder of (embodiment 19) example 19 of the present invention
Except by embodiment 2 relative to prilling powder epoxy resin addition from 3.5wt% change
Beyond 2.0wt%, remaining similarly to Example 2, thus has just obtained the pelletize of example 19 of the present invention
Powder.
The manufacture of the prilling powder of (embodiment 20) example 20 of the present invention
Except by embodiment 2 relative to prilling powder epoxy resin addition from 3.5wt% change
Beyond 2.5wt%, remaining similarly to Example 2, thus has just obtained the pelletize of example 20 of the present invention
Powder.
The manufacture of the prilling powder of (embodiment 21) example 21 of the present invention
Except by embodiment 2 relative to prilling powder epoxy resin addition from 3.5wt% change
Beyond 3.0wt%, remaining similarly to Example 2, thus has just obtained the pelletize of example 21 of the present invention
Powder.
The manufacture of the prilling powder of (embodiment 22) example 22 of the present invention
While the epoxy resin of inner for embodiment 2 use is changed to silicones, and by resin
Addition is changed to beyond 3.7 weight % from 3.5 weight %, remaining similarly to Example 2, thus just
Obtain the prilling powder of example 22 of the present invention.
The manufacture of the prilling powder of (embodiment 23) example 23 of the present invention
Except changing the high boiling point solvent of inner for embodiment 22 use into propylene glycol list first from butyl cellosolve
Beyond ether (propylene glycol methyl ether), remaining is identical with embodiment 22, thus must
Arrive the prilling powder of example 23 of the present invention.
The manufacture of the prilling powder of (embodiment 24) example 24 of the present invention
Except by the high boiling point solvent of inner for embodiment 22 use in addition to butyl cellosolve changes hexamethylene into,
Remaining is identical with embodiment 22, thus has just obtained the prilling powder of example 24 of the present invention.
The manufacture of the prilling powder of (embodiment 25) example 25 of the present invention
Except changing the high boiling point solvent of inner for embodiment 22 use into diisobutyl first from butyl cellosolve
Beyond ketone, remaining is identical with embodiment 22, thus has just obtained the prilling powder of example 25 of the present invention.
The manufacture of the prilling powder of (comparative example 1) comparative example 1
Except the butyl cellosolve of inner for embodiment 1 use being changed into butanone, and only use beyond butanone,
Remaining is same as in Example 1, thus has just obtained the prilling powder of comparative example 1.
The manufacture of the prilling powder of (comparative example 2) comparative example 2
Except by the 2nd baking temperature in embodiment 1 from 110 DEG C be changed to 100 DEG C in addition to, remaining with
Embodiment 1 is identical, thus has just obtained the prilling powder of comparative example 2.
The manufacture of the prilling powder of (comparative example 3) comparative example 3
Except by the 2nd baking temperature in embodiment 1 from 110 DEG C be changed to 140 DEG C in addition to, remaining with
Embodiment 1 is identical, thus has just obtained the prilling powder of comparative example 3.
The manufacture of the prilling powder of (comparative example 4) comparative example 4
Except the addition of the high boiling point solvent relative to amount of resin in embodiment 2 is become from 30wt%
Beyond more 8wt%, remaining is same as in Example 2, thus has just obtained the prilling powder of comparative example 4.
The manufacture of the prilling powder of (comparative example 5) comparative example 5
Except the addition of the high boiling point solvent relative to amount of resin in embodiment 2 is become from 30wt%
Beyond more 50wt%, remaining is same as in Example 2, thus has just obtained the pelletizing of comparative example 5
End.
The manufacture of the prilling powder of (comparative example 6) comparative example 6
Except changing the high boiling point solvent of inner for embodiment 2 use into methylisobutylketone from butyl cellosolve
Beyond (Methyl Isobutyl Ketone), remaining is same as in Example 2, thus is just compared
The prilling powder of example 6.
The manufacture of the prilling powder of (comparative example 7) comparative example 7
Except changing the high boiling point solvent of inner for embodiment 2 use into n-butanol from butyl cellosolve
Beyond (n Butylalcohol), remaining is same as in Example 2, thus has just obtained comparative example 7
Prilling powder.
The manufacture of the prilling powder of (comparative example 8) comparative example 8
Except changing the high boiling point solvent of inner for embodiment 2 use into diethylene glycol mono butyl from butyl cellosolve
Beyond ether (2-(2-Butoxyethoxy) ethanol), remaining is same as in Example 2, thus just obtains
The prilling powder of comparative example 8.
The manufacture of the prilling powder of (comparative example 9) comparative example 9
Except by the resin content in embodiment 2 in addition to 3.5 weight % are changed to 1.5 weight %,
Remaining is same as in Example 2, thus has just obtained the prilling powder of comparative example 9.
The manufacture of the prilling powder of (comparative example 10) comparative example 10
Except the resin of inner for embodiment 2 use is changed to silicones from epoxy resin, and by high boiling point
Solvent is changed to beyond butanone from butyl cellosolve, and remaining is same as in Example 2, thus is compared
The relatively prilling powder of example 10.
The manufacture of the prilling powder of (comparative example 11) comparative example 11
Except by the high boiling point solvent of inner for embodiment 10 use in addition to butyl cellosolve is changed to butanol,
Remaining is same as in Example 10, thus has just obtained the prilling powder of comparative example 11.
The manufacture of the prilling powder of (comparative example 12) comparative example 12
Except the high boiling point solvent of inner for embodiment 10 use is changed to diethylene glycol from butyl cellosolve
Beyond monobutyl ether, remaining is same as in Example 10, thus has just obtained the prilling powder of comparative example 12.
Example of the present invention 1～25 and the manufacturing condition of comparative example 1～12 prilling powder and each prilling powder
Physical property together, is represented by table 1 and table 2.
Abbreviations in table 1 and table 2 etc. are as described below.
*1: relative to the weight of prilling powder
*2: MEK: butanone
BCS: butyl cellosolve
PGM: propylene glycol methyl ether acetate (Propylene Glycol Monomethylether
Acetate)
CHEX: hexamethylene
DIB: isobutyrone
ACT: acetone
MIB: butanone
NBA: butanol
BEE: diethylene glycol monobutyl ether
*3: low boiling solvent (LBS)/high boiling point solvent (HBS)
*4: be discontented with the amount (DS) of the particle of 75 μm by particle diameter and more than the particle of 500 μm
The amount (DL) ratio shared by particle entirety is evaluated.
Ar=DSIt is less than 5%, and DLIt is less than 10%
Br=DSIt is less than 10%, and DLIt is more than 10%, less than 20%
Cr=DSIt is more than 10%, and DLMore than 20%
*5: pcrmeability is measured when 100kHz.Briquetting pressure is 4ton/cm2。
*6: direct current overlapping features is to measure (Δ μ-20%) at 100kHz
*7: Pcv is to measure under conditions of 100kHz, and 50mT.
Drying property is good with Ad(), Bd(is the best), or Cd(is bad) evaluate.
Pcrmeability is good with Am(), Bm(is the best), or Cm(is bad) evaluate.
DC stacked property is good with Ah(), Bh(is the best), or Ch(is bad) evaluate.
Pcv is good with Ap(), Bp(is the best), or Cp(is bad) evaluate.
Table 1
Table 2
Evaluation to prepared each prilling powder
The prilling powder of example 1～25 of the present invention is all DSBelow 10%, and DL20% with
In lower particle size range, the deviation of particle diameter is less.
In contrast, the prilling powder of comparative example 1～12, it is dried good, no when 1 drying steps
Crossing, in addition to the prilling powder of comparative example 1 and 9, the drying regime when 2 drying steps is equal
For bad.When the temperature of the 2nd drying steps is 100 DEG C, the residual of high boiling point solvent is more, institute
Mesh screen cannot be passed through with prepared unguentum.Thus prove to obtain the prilling powder of desired particle diameter.
It addition, in the case of the temperature of the 2nd drying steps is 140 DEG C, epoxy resin can be speculated
In hardening state, mouldability during pressure forming can deteriorate, thus causes pcrmeability to reduce.
The prilling powder of comparative example 1,4,6,7,10 and 11 in drying steps, unguentum be dried
Carrying out long, the error causing particle diameter is the biggest.It addition, because the pelletize of comparative example 5,8 and 12
In powder, the residual volume of high boiling point solvent is more, so mesh screen cannot be passed through, so after just cannot be carried out
The molding stated.
The manufacture of (embodiment 26) electronic component
Use example 1 of the present invention and general magnetic powder (Fe: Si: Cr=92:4:4), according to following
Condition manufactures ring structure iron core, and compares its characteristic.
(1) material
Use the prilling powder that example 1 of the present invention is similar with quoting document 2, manufacture ring structure iron core respectively,
And measure and compare relative permeability, μ frequency, direct current overlapping features and core losses characteristic.
Ring structure iron core: φ 15mm × 2.5mmt(briquetting pressure 4t/cm2)
The number of turn: example 1 Magnaglo (CIP)=19T of the present invention
General Magnaglo (Fe-Si-Cr)=10T
In pcrmeability, the pcrmeability when 100kHz and briquetting pressure (ton/cm2) relation, use
Impedance analyzer measures.It addition, about μ frequency, frequency and the pcrmeability when 100kHz
Change, by impedance analyzer, the frequency band till 100kHz～10MHz is investigated.Close
In direct current overlapping features, use impedance analyzer, increase the DC current to coil supply lentamente,
Analyze input magnetic field and the change of pcrmeability.
About core losses, it is with B-H analyzer, the frequency between 100kHz～10MHz to be brought into
Go investigation.With above-mentioned table 1 and 2, also Fig. 1～Fig. 4 represents result.
As it is shown in figure 1, the pcrmeability of above-mentioned 2 ring structure iron cores, it is 2 tons/cm in briquetting pressure2's
Time, use a side of general Magnaglo higher, even if molding pressure uprises, its gap is not the most received
Contracting.
It is indicated above that as product, in order to obtain the same inductance (L), be necessary for increasing the number of turn,
Or apply higher molding pressure.
On the other hand, as shown in Figure 4, for core losses, 100kHz when, compared with making
With the ring structure iron core of general Magnaglo, employ the ring-like ferrum of the Magnaglo of example 1 of the present invention
The core losses of core is less, and when frequency uprises, its gap can become big.Thus, in surpassing shown in Fig. 2
Cross in the range of 1.5MHz, use the ring structure iron core of the Magnaglo of example 1 of the present invention, due to iron core
Loss is few, so the relative permeability near the self-resonant frequency of coil has the biggest rising.Another
Aspect, employs the ring structure iron core of general Magnaglo, owing to core losses is relatively big, goes out on the contrary
Show reduction tendency.
As shown in Fig. 3 (A) and (B), about direct current overlapping features, use the magnetic of example 1 of the present invention
The ring structure iron core of property powder, more preferable than the result of the ring structure iron core with general Magnaglo.
In Fig. 3 (A), it is set to owing to the number of turn of above-mentioned Fe-Si-Cr being set to the number of turn of 10T, CIP
19T is also measured, so initial permeability difference., even if supposing pcrmeability one
In the case of sample, due to this
The difference of the Magnaglo of bright example 1 and the pcrmeability of general Magnaglo is about 1.3 times, so
It is believed that the ring structure iron core employing the Magnaglo of example 1 of the present invention has better direct current weight
Folded characteristic.
Thus, use the Magnaglo that the inventive method manufactures, in addition to relative permeability, its
Remaining characteristic is the best.
Present invention can be suitably applied to the manufacture field of electronic component.
Claims (13)
1. the manufacture method of a prilling powder, it is characterised in that including:
It is mixed together to Magnaglo, resin, low boiling solvent and high boiling point solvent manufacture slurry
The mixture manufacturing step of material shape mixture；
Heat described pulp-like mixture, make described low boiling solvent be able to evaporation and mix to manufacture unguentum shape
First drying steps of compound；
With mesh screen, described unguentum shape mixture is pulverized and granulate, thus obtain the granulate step of particle；
And
Heat described particle, make the evaporation of described high boiling point solvent obtain the second of magnetic particle and be dried step
Suddenly.
The manufacture method of prilling powder the most according to claim 1, it is characterised in that described magnetic
Property powder is formed from by carbonyl iron dust, noncrystalline iron powder, silicon steel, permalloy and ferrum alusil alloy
Group in arbitrarily select.
The manufacture method of prilling powder the most according to claim 1, it is characterised in that described tree
Fat is hardening temperature resin more than 150 DEG C.
The manufacture method of prilling powder the most according to claim 1, it is characterised in that described tree
Fat is from by epoxy resin, phenolic resin, silicones, unsaturated polyester resin and amino resins institute
The group of composition selects.
The manufacture method of prilling powder the most according to claim 1, it is characterised in that described low
Boiling point solvent is boiling point organic solvent below 90 DEG C.
The manufacture method of prilling powder the most according to claim 5, it is characterised in that described low
Boiling point solvent is from by butanone, acetone, toluene, ethyl acetate, benzene, methanol, ethanol and isopropyl
The group that alcohol is formed is selected.
The manufacture method of prilling powder the most according to claim 1, it is characterised in that described height
Boiling point solvent is boiling point organic solvent in the range of 110 DEG C～200 DEG C.
The manufacture method of prilling powder the most according to claim 7, it is characterised in that described height
Boiling point solvent be from by butyl cellosolve, isobutyrone, terpineol, amylalcohol, isoamyl alcohol, two
The group of toluene and n-butyl acetate composition selects.
The manufacture method of prilling powder the most according to claim 1, it is characterised in that described height
The weight of boiling point solvent is the 10～60% of the weight of described resin.
The manufacture method of prilling powder the most according to claim 9, it is characterised in that described
The weight of high boiling point solvent is the 10～45% of the weight of described resin.
The manufacture method of 11. prilling powders according to claim 1, it is characterised in that in institute
State in the first drying steps, heat with 50 DEG C～60 DEG C.
The manufacture method of 12. prilling powders according to claim 1, it is characterised in that in institute
State in the second drying steps, heat with 110 DEG C～130 DEG C.
The manufacture method of 13. prilling powders according to claim 1, it is characterised in that in institute
Stating the mesh screen used in granulate step, 2～5 times of the particle diameter with above-mentioned prilling powder are big
Mesh diameter.
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| JP2005336513A (en) * | 2004-05-24 | 2005-12-08 | Sumitomo Electric Ind Ltd | Method for manufacturing soft-magnetic material and soft-magnetic material, and method for manufacturing dust core and dust core |
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| JP2007012744A (en) * | 2005-06-29 | 2007-01-18 | Sumitomo Electric Ind Ltd | Dust core and manufacturing method thereof |
| CN101536125A (en) * | 2006-10-31 | 2009-09-16 | 索尼化学&信息部件株式会社 | Process for the production of laminate-type soft magnetic sheets |
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