CN109311763A - Rod-shaped MnZn FERRITE CORE and its manufacturing method and antenna - Google Patents
Rod-shaped MnZn FERRITE CORE and its manufacturing method and antenna Download PDFInfo
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- CN109311763A CN109311763A CN201780006414.7A CN201780006414A CN109311763A CN 109311763 A CN109311763 A CN 109311763A CN 201780006414 A CN201780006414 A CN 201780006414A CN 109311763 A CN109311763 A CN 109311763A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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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
- H01F1/34—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 non-metallic substances, e.g. ferrites
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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
- H01F1/34—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 non-metallic substances, e.g. ferrites
- H01F1/36—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 non-metallic substances, e.g. ferrites in the form of particles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F3/00—Cores, Yokes, or armatures
- H01F3/08—Cores, Yokes, or armatures made from powder
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Abstract
A kind of rod-shaped MnZn FERRITE CORE contains iron as basis: with Fe2O3Conversion meter 51.5~54.5 moles of %, zinc: 10.0~17.0 moles of %, manganese in terms of ZnO conversion: surplus；As accessory ingredient, contain SiO2: 50~300 mass ppm, CaO:100~1300 mass ppm and Nb2O5: 100~400 mass ppm, wherein the sintered density of the MnZn FERRITE CORE is set as 4.85g/cm3The average value of the maximum valley depth of contour curve when above and in based on the observation of the surface texture of JIS B 0601 by n=50 is set as 17 μm hereinafter, 23 DEG C of realization simultaneously, the initial permeability μ under 100kHz as a result,iThe occurrence rate of magnetic core of the intensity less than 100MPa is 4% or less such high intensity when measuring three-point bending strength for 1800 or more such high magnetic permeabilities and with n=50.
Description
Technical field
The present invention relates to high-intensitive and high magnetic permeability rod-shaped MnZn FERRITE COREs and its manufacturing method, especially want
The MnZn FERRITE CORE for being suitble to the purposes for the magnetic core as coil for antenna is provided.
Moreover, it relates to use the antenna of above-mentioned rod-shaped MnZn FERRITE CORE production.
Background technique
MnZn ferrite is the magnetic core of the noise filter for being widely used as Switching Power Supply etc., transformer, coil for antenna
Material.Its advantage can be enumerated: be high magnetic permeability, low-loss in the region kilohertz (kHz) in soft magnetic material；In addition, with
Amorphous metal etc. is compared, cheap.
Magnetic core at these on the way, as the mainly coil for antenna used in vehicle-mounted, it is desirable that its initial permeability
It is high.The reason for this is that for the coil of the purposes, it is desirable that inductance is high.When only improving inductance, increasing the number of turns is
Can, but gone back on the way in the use while requiring to minimize, therefore, it is not preferred for increasing the mode of the number of turns.If MnZn iron oxygen
The initial permeability of body is high, then does not need to increase the number of turns, therefore can be realized the miniaturization of antenna.
About the MnZn ferrite of the magnetic core purposes towards coil for antenna, various exploitations had been carried out in the past, can arrange
Citing such as patent document 1,2,3.
Existing technical literature
Patent document
Patent document 1: Japanese Unexamined Patent Publication 10-270232 bulletin
Patent document 2: Japanese Unexamined Patent Publication 2006-206355 bulletin
Patent document 3: Japanese Unexamined Patent Publication 2006-210493 bulletin
Summary of the invention
Problem to be solved by the invention
In general, reducing magnetic anisotropy in order to improve the ferritic initial permeability of MnZn and magnetostriction being that have
Effect.In order to realize these purposes, needing will be as the Fe of the ferritic main component of MnZn2O3, ZnO and MnO use level tune
It is whole to arrive range appropriate.In addition, sufficiently heated in firing process and make grain growth in ferrite to coarse, thus, it is possible to
The movement for magnetizing the neticdomain wall in the crystal grain in process is become easy, as a result can be improved initial permeability.But excessive
It, can be due to the influence of eddy-current loss although grain growth can improve the initial permeability in the frequency field of 1~10kHz or so
And decline the initial permeability of 100kHz or more.About this point, the additive for the ingredient being segregated in grain boundaries is added and gives birth to
At appropriate and uniform thickness crystal boundary, thus make initial permeability until 100kHz is maintained at sufficient value.
About the magnetic core of coil for antenna, other than above-mentioned magnetic characteristic, especially in the vehicle-mounted characteristic paid attention on the way
For intensity.The reason for this is that coil for antenna magnetic core mainly to be referred to as rod-shaped elongated cuboid, columned shape is come
It uses.In general, mostly be in length and breadth number mm and length be its 10 times or so 60~100mm come using.Therefore, in order to
It prevents from requiring the intensity measured with three-point bending strength high magnetic core as the inductance decline of magnetic core coil caused by damaged.In addition,
In the case where product, strong request does not occur the low low-intensity magnetic core of three-point bending strength.
Based on the above reasons, for the magnetic core of coil for antenna, it is desirable that take into account magnetic characteristic as high initial permeability and
Reduce high intensity as the occurrence rate of the low low-intensity magnetic core of three-point bending strength.
But although being referred in patent document 1 for realizing the composition of desired magnetic characteristic and in order to realize intensity
And control the necessity of average crystallite particle diameter, but due to as low as 3 μm of partial size hereinafter, therefore initial permeability is low, by embodiment Lai
It sees, the maximum value of the initial permeability under 100kHz also only terminates in 1500.
In addition, being also only the influence for referring to average crystallite particle diameter about intensity, not about aftermentioned heavy in the present invention
Want the record of the factor.Therefore, the MnZn ferrite based on the condition production recorded in patent document 1 not while having as vehicle
Carry required for the magnetic core of the coil for antenna of purposes etc., magnetic characteristic as high initial permeability and three-point bending strength it is high this
High-intensitive the two of sample.
In addition, report in patent document 2,3 keeps the temperature characterisitic of initial permeability excellent by the regulation of ingredient
MnZn ferrite, but in embodiment, 20 DEG C, the peak of initial permeability under 100kHz also only terminate in 1700, it is difficult to say
It is sufficient.Further, there is no record for intensity critically important for the coil for antenna for vehicle-mounted purposes etc.,
Therefore, from the point of view of magnetic characteristic and intensity the two viewpoints, the MnZn ferrite based on the condition production recorded in patent document 2,3
And do not have preferred characteristic.
The method for solving problem
Therefore, inventor first to can be improved 23 DEG C, the ferritic Fe of MnZn of initial permeability under 100kHz2O3
Amount, ZnO amount are studied, it was found that compositing range appropriate.
And it finds out, if magnetic anisotropy and magnetostriction are small in the compositing range, is also able to maintain necessary
Resistivity is further able to that the temperature characterisitic of initial permeability is made to show that the secondary peak of maximum also nearby occurs at 23 DEG C, therefore,
High initial permeability can be obtained under the same conditions.
In addition it finds out, by the way that suitable SiO as the non-magnetic constituents being segregated in grain boundaries is added2, CaO and Nb2O5And
It is capable of forming uniform crystal boundary, thus resistivity rises, so as to further increase initial permeability.
Further, also obtain following opinion in addition to these: there is also preferred ranges for firing condition, especially,
If not keeping temperature and its retention time to control in range appropriate highest, sintered density can not be improved, therefore be obtained not
To desired initial permeability.
Maximum temperature more than a certain temperature is kept and certain more than certain time holding can promote in initial permeability
Rise indispensable sintering and grain growth.Therefore, it is necessary to sintered density setting regulation, select firing condition appropriate from
And it can be realized the sintered density.
It the above are for improving means necessary to initial permeability, but also finds out: for for coil for antenna
For MnZn ferrite, it is also necessary to while reducing the occurrence rate of the low low-intensity magnetic core of three-point bending strength.
Therefore, inventor is then investigated from this viewpoint, is as a result found out, firstly, improving sintered density to pass
Important, in order to realize the target, the highest for needing to carry out above-mentioned firing condition keeps temperature and the optimization of retention time.That is, logical
Raising sintered density is crossed, initial permeability can not only be improved, and can reduce the occurrence rate of low-intensity magnetic core.
Further, inventor is conceived to the small bumps for being present in surface according to the observation of the surface of magnetic core, finds out: should
Recess portion can become starting point when destroying, it is therefore desirable to limitation be arranged to the depth of recess portion.The recess portion is being observed with maximum valley depth
Depth when, it is low strong if average value when n=50 is there is the deep recess portion for becoming the starting point being easily destroyed more than certain
The occurrence rate for spending magnetic core increases.In order to make the occurrence rate of low-intensity magnetic core be down to desired value, not only need to inhibit to be used for example as
The block of the organic matter of the PVA of binder etc is mixed into, and is needed not add used in common FERRITE CORE, forming
When the solid organic matters ingredient such as release agent so that the value of maximum valley depth does not become larger.
If it is the rod-shaped magnetic core as object of the present invention, due to being and the contact area of mold is small, the shape that is easily formed
Therefore shape can make not using the release agent as solid organic matters.In addition, being conceived to the grain of pelletizing simultaneously
Degree distribution, also finds out: in the case that the compression strength of situation and pelletizing more than the coarse powder is excessively high, when forming, is easy in pelletizing
Between residual clearance, the gap after sintering in the form of recess portion remain.Therefore, it also requires the size distribution for making pelletizing and resists
Compressive Strength is fallen into appropriate range.
But as previously mentioned, the value of initial permeability is insufficient in patent document 1, in addition, only referring to about intensity
The inhibition of average crystallite particle diameter, therefore the occurrence rate of low-intensity magnetic core cannot be reduced.
In addition, not only the value of initial permeability is insufficient, but also absolutely not refers to intensity about patent document 2,3, because
This cannot inhibit the appearance of low-intensity magnetic core, therefore, can not make merely with these opinions and practical useful be suitable for using
In the MnZn ferrite of the magnetic core of the coil of antenna core.
The present invention is developed based on above-mentioned opinion and after various researchs are repeated.
That is, purport composition of the invention is as follows.
1. a kind of rod-shaped MnZn FERRITE CORE, which is characterized in that as basis, contain iron: with Fe2O3Conversion
Count 51.5~54.5 moles of %, zinc: 10.0~17.0 moles of %, manganese in terms of ZnO conversion: surplus；
As accessory ingredient, contain SiO2: 50~300 mass ppm, CaO:100~1300 mass ppm and Nb2O5: 100~
400 mass ppm,
Wherein,
The sintered density of the MnZn FERRITE CORE is 4.85g/cm3More than,
In the surface texture observation based on JIS B 0601, the average value of the maximum valley depth of contour curve when n=50
It is 17 μm or less.
2. a kind of rod-shaped MnZn FERRITE CORE, by the iron as basis: with Fe2O3Conversion meter 51.5~54.5
Mole %, zinc: 10.0~17.0 moles of %, manganese in terms of ZnO conversion: surplus；SiO as accessory ingredient2: 50~300 mass
The mass of ppm, CaO:100~1300 ppm and Nb2O5: 100~400 mass ppm；And inevitably impurity is constituted, wherein
The sintered density of the MnZn FERRITE CORE is 4.85g/cm3More than,
In the surface texture observation based on JIS B 0601, the average value of the maximum valley depth of contour curve when n=50
It is 17 μm or less.
3. the rod-shaped MnZn FERRITE CORE according to aforementioned 1 or 2, wherein as accessory ingredient, further contain
CoO:3500 mass ppm or less.
4. the rod-shaped MnZn FERRITE CORE according to any one of aforementioned 1 to 3, wherein aforementioned rod-shaped MnZn
Initial permeability μ of the FERRITE CORE at 23 DEG C, 100kHziIt is 1800 or more.
5. the rod-shaped MnZn FERRITE CORE according to any one of aforementioned 1 to 4, wherein with n=50 to aforementioned rod
When the MnZn FERRITE CORE of shape measures three-point bending strength, the occurrence rate of magnetic core of the intensity less than 100MPa is 4% or less.
6. the rod-shaped MnZn FERRITE CORE according to any one of aforementioned 1 to 5, wherein aforementioned rod-shaped MnZn
FERRITE CORE is the MnZn ferrite formed by forming-sintered body that the value of size distribution d90 is 300 μm of pelletizings below
Magnetic core.
7. the rod-shaped MnZn FERRITE CORE according to any one of aforementioned 1 to 6, wherein aforementioned rod-shaped MnZn
FERRITE CORE is the MnZn FERRITE CORE that forming-sintered body of the pelletizing by compression strength less than 1.5MPa is formed.
8. a kind of manufacturing method of rod-shaped MnZn FERRITE CORE, includes
The pre-burning process of pre-burning is carried out to the mixture of basis；
Mixing-the grinders for adding accessory ingredient into the pre-burning powder obtained by above-mentioned pre-burning process and being mixed, being crushed
Sequence；
The granulation work adding binder into the comminuted powder obtained by above-mentioned mixing-pulverizing process and being granulated after mixing
Sequence；
The forming process that the pelletizing obtained by above-mentioned granulating working procedure is formed；With
The formed products obtained as above-mentioned forming process are burnt into MnZn described in obtaining any one of aforementioned 1 to 5
The firing process of FERRITE CORE.
9. the manufacturing method of MnZn FERRITE CORE according to aforementioned 8, wherein the size distribution of aforementioned pelletizing
The value of d90 is 300 μm or less.
10. the manufacturing method of MnZn FERRITE CORE according to aforementioned 8 or 9, wherein the pressure resistance of aforementioned pelletizing
Degree is less than 1.50MPa.
11. the manufacturing method of MnZn FERRITE CORE according to any one of aforementioned 8 to 10, wherein it is aforementioned at
It is formed in shape process without using release agent.
12. a kind of antenna, have MnZn FERRITE CORE is formed as described in any one of aforementioned 1 to 7 magnetic core and
In the electric wire of its periphery winding multi-turn.
Invention effect
Rod-shaped MnZn FERRITE CORE of the invention can obtain previous MnZn FERRITE CORE simultaneously can not the phase
Initial permeability μ hope, at 23 DEG C, 100kHziMeasure at 3 points for 1800 or more such high magnetic permeabilities and with n=50
The occurrence rate of magnetic core of the intensity less than 100MPa is 4% or less such high intensity when bending strength.
Therefore, rod-shaped MnZn FERRITE CORE of the invention is especially suitable for needing high magnetic permeability and high intensity simultaneously
Coil for antenna magnetic core.
Moreover, by that can obtain using rod-shaped MnZn FERRITE CORE of the invention as the magnetic core of coil for antenna
To the high-performance and not antenna of cracky is furthermore possible to realize the miniaturization of antenna.
Detailed description of the invention
Fig. 1 be shown as the concrete shape of rod-shaped MnZn FERRITE CORE of the invention rectangular shape (a) and
The figure of cylindrical shape (b).
Fig. 2 is to show using rod-shaped MnZn FERRITE CORE of the invention as magnetic core, in its periphery to be wound with multi-turn electricity
The figure of the state of line.
Specific embodiment
The present invention is specifically described below.
Firstly, to being illustrated at being grouped as the reasons why being limited to aforementioned range in the present invention by MnZn is ferritic.It needs
It is noted that for the iron, zinc, manganese that contain in the present invention as basis, to be converted into Fe2O3, ZnO, MnO
Value is shown.In addition, these Fe2O3, ZnO, MnO content shown with a mole %, on the other hand, the content of accessory ingredient is with opposite
It is shown in the quality ppm of FERRITE CORE entirety.
Fe2O3: 51.5~54.5 moles of %
In basis, Fe2O3When fewer than proper range, more than proper range when, not only magnetic anisotropy becomes larger, but also
Magnetostriction also becomes larger, therefore will lead to the decline of initial permeability.Therefore, minimum also to rub containing 51.5 in the present invention
The Fe of your %2O3Amount, using 54.5 moles of % as the upper limit.
ZnO:10.0~17.0 mole %
When ZnO is few, Curie temperature is excessively increased, and therefore, the initial permeability decline at 23 DEG C is therefore, minimum also to contain
There is the ZnO of 10.0 moles of %.But content be more than appropriate amount when, initial permeability show maximum secondary peak temperature can decline,
Therefore it will lead to the decline of the initial permeability at 23 DEG C.Therefore, the upper limit is set as 17.0 moles of %.
MnO: surplus
The present invention is MnZn ferrite, and the surplus of main component composition is necessary for MnO.The reason is that if not being
MnO, then cannot achieve initial permeability at 23 DEG C, 100kHz is 1800 or more.Here, preferred MnO amount for 30.0~
38.0 mole %.
Basis is illustrated above, it is as described below about accessory ingredient.
SiO2: 50~300 mass ppm
Known SiO2The homogenization for facilitating ferritic crystalline structure subtracts remaining hole in crystal grain with addition
It is few, resistivity is additionally improved, therefore, 23 DEG C, the initial permeability under 100kHz are promoted and adding in right amount, and pass through
It reduces coarse grain and reduces starting point when destroying, therefore be able to suppress the appearance of low-intensity magnetic core.Therefore, minimum also to contain
There is the SiO of 50 mass ppm2.But when additive amount is excessive, occur abnormal grain instead, when which can become destruction
Starting point, therefore there is low-intensity magnetic core, while be also remarkably decreased initial permeability, therefore, the upper limit be defined as 300 matter
Measure ppm.
The mass of CaO:100~1300 ppm
CaO has the function of in the ferritic grain boundaries segregation of MnZn, inhibits grain growth, can and adding in right amount
Resistivity is promoted, is able to ascend 23 DEG C, the initial permeability under 100kHz therewith.In addition, with the inhibition of grain growth, moreover it is possible to
Enough improve breakdown strength.Therefore, minimum also to contain the CaO of 100 mass ppm.But when additive amount is excessive, it may appear that different
Normal crystal grain, is not only remarkably decreased initial permeability, but also also results in the appearance of low-intensity magnetic core, it is therefore desirable to be limited to 1300 matter
Measure ppm or less.
Nb2O5: 100~400 mass ppm
Nb2O5Have the effect of in the ferritic grain boundaries segregation of MnZn, mitigate the stress for being applied to crystal grain.Therefore, lead to
It crosses appropriate addition and is able to ascend initial permeability, and grain growth can be inhibited by crystal boundary generation, thus can also
Improve breakdown strength.Therefore, minimum also to contain the Nb of 100 mass ppm2O5.But when additive amount is excessive, it may appear that abnormal
Crystal grain can not only be such that initial permeability is remarkably decreased, but also also result in the appearance of low-intensity magnetic core, it is therefore desirable to be limited to 400 matter
Measure ppm or less.
In addition, CoO can also be contained as optional member in the present invention.
CoO:3500 mass ppm or less
CoO is to contain the Co with positive magnetic anisotropy2+The ingredient of ion can make to originate by adding the ingredient
Magnetic conductivity shows that great temperature, the i.e. temperature width of secondary peak broaden.It, can not be with other ingredients but when additive amount is excessive
Possessed negative magnetic anisotropy is offset, therefore leads to being remarkably decreased for initial permeability.Therefore, in the case where addition,
Need to be limited to 3500 mass ppm or less.
The ferritic basis of MnZn, accessory ingredient and optional member of the invention are illustrated above, except this with
Outside, it is mixed into Cl, Na, Al ingredient etc. as impurity sometimes.But as long as these tramp materials add up to 500 mass ppm with
Under, then it will not especially become problem.
In addition, the various characteristics of MnZn FERRITE CORE of the invention are not only formed, also by the huge of various parameters
It influences.Wherein, following regulation is set in order to ensure the characteristic, i.e. magnetic characteristic and the strength characteristics that are even more important.
(1) sintered density: 4.85g/cm3More than
MnZn FERRITE CORE is sintered by firing processing and grain growth, to constitute crystal grain and crystal boundary.For
Realize the crystalline structure that can be realized high initial permeability, the non-magnetic constituents that should exist at the grain boundary suitably in crystalline substance
Segregation, the partial size of crystal grain holding appropriateness and the form by having uniform magnetic ingredient to constitute at boundary, it is necessary to make sintering reaction
Sufficiently carry out.In addition, intensity decline can be induced from the viewpoint of intensity, when being sintered insufficient, therefore not preferably.
The sintered density of MnZn FERRITE CORE is studied from the viewpoint of above, is as a result found out, need by
Sintered density is set as 4.85g/cm3More than.
In addition, by meeting the condition, can make for the first time 23 DEG C, it is 1800 or more initial permeability under 100kHz, same
When can the generation rate of low-intensity magnetic core by three-point bending strength less than 100MPa be suppressed to less than 4%.
It should be noted that needing to keep temperature to be set as 1290 DEG C highest when being burnt into realize the sintered density
It is set as 1 hour or more above and by the retention time at such a temperature.
In addition, sintered density can not improve when being abnormal grain growth, it is therefore desirable to abnormal brilliant according to avoiding the occurrence of
The mode of grain is made.It is therefore advantageous that no more than prescribed limit excessively adding accessory ingredient and being mixed into impurity
Amount inhibits within 500 mass ppm.
(2) in the surface texture observation based on JIS B 0601, the maximum valley depth of contour curve when n=50 is averaged
Value is 17 μm or less
MnZn FERRITE CORE can obtain by the following method: after pelletizing is filled in mold, by with about
The powder forming process that the pressure of 100MPa is compressed, is burnt into obtained formed body and makes its sintering.In the MnZn
There are small bumps, recess portions therein to be likely to become destruction when three-point bending strength measures on the surface of FERRITE CORE
Starting point, the presence of especially deep recess portion can improve the occurrence rate of anti-low-intensity magnetic core of the folding load less than 100MPa.Therefore, in order to
The MnZn FERRITE CORE of the high magnetic permeability that the present invention is expected and high intensity is obtained, needing will be based on the surface of JIS B 0601
The average value of the maximum valley depth of contour curve when in character observation, n=50 is suppressed to 17 μm or less.
It should be noted that in order to meet the condition, it is necessary first to inhibit the organic matters such as the PVA used as binder
Block is mixed into pelletizing.As its countermeasure, it is desirable that separate the powder and meal of pelletizing with sieve；In order to avoid from outside
Be mixed into organic matter, for pelletizing management when keeping method, also require be loaded into bucket and seal.In addition,
In forming, visual confirmation periodically is carried out to pelletizing, is finding that the mode for removing tramp material when being mixed into is effective.Into one
Step ground, object of the invention is the shape being readily formed, i.e. rod-shaped, therefore, is made even if not adding and being usually added to before forming
The release agent of the solid organic matters such as the metallic soap in grain powder is also able to carry out forming.
These block-like organic matters are decomposed in the initial stage of firing, and therefore, the trace of organic matter is to be sintered intracorporal sky
The form of gap retains as former state.The gap becomes deep recess portion, and when maximum valley depth average value reaches 17 μm or more, the depth recess portion is three
The starting point destroyed can be become when point bending strength measurement, therefore going out for anti-low-intensity magnetic core of the folding load less than 100MPa can be improved
Now rate.Therefore, being mixed into for the block of organic matter is inhibited to be important.
Furthermore it is preferred that being also provided with 2 regulations to the pelletizing to be formed simultaneously.
First is size distribution, when coarse powder is more, even if pressurizeing in forming, is also easy residual between pelletizing
It interspaces, therefore, is also easy to remain deep recess portion after firing.In addition, second be pelletizing compression strength, the compression strength
When excessively high, the recess portion residual after being burnt into as caused by the gap between pelletizing similarly will lead to.
Therefore, in order to by maximum valley depth be suppressed to less than 17 μm, inhibit it is anti-folding load be less than 100MPa low-intensity magnetic core
Occurrence rate, the value of the median particle diameter d90 of size distribution is preferably set as 300 μm or less and is set as compression strength
1.50MPa following.
It should be noted that about size distribution, using based on the laser diffraction scattering method recorded in JIS Z 8825
Granularmetric analysis is measured." d90 " indicates that the volume from small particle side in the size distribution curve has reached 90%
Partial size.In addition, the compression strength of pelletizing is measured by method specified in JIS Z8841.
Then, the manufacturing method of MnZn FERRITE CORE is illustrated.
Firstly, weighing Fe in the way of reaching defined composition ratio2O3, ZnO and MnO powder, these powder are abundant
Mixing, then carries out pre-burning.Then, obtained pre-burning powder is crushed.At this point, by additives such as accessory ingredients specified in the present invention
With the addition of defined composition ratio, crushed together with pre-burning powder.In this process, sufficiently homogenized to powder so that
There is no unevenness for the concentration of added ingredient, while pre-burning powder being miniaturize to the size of target average grain diameter.
Then, the organic matter binding agents such as polyvinyl alcohol are added in the powder formed to the target as above obtained, appropriate
Under the conditions of be granulated using spray drying process etc., thus obtain expectation granularity and compression strength sample.In spray drying process
In the case where, it is expected that temperature of outgoing air is set below 270 DEG C.About obtained pelletizing, when necessary by being adjusted for granularity
The processes such as sieving, taken care of in a manner of it will not be mixed into block-like organic matter, added after confirmation is not mixed into using forming machine
Pressure, after forming, is burnt under defined firing condition.It is expected that passing through from the sieve of 350 μm of meshes, and remove on sieve
Coarse powder.In addition, as described above, firing condition appropriate be highest keep temperature: 1290 DEG C or more and retention time: 1 hour with
On.
It should be noted that the processing such as surface grinding can also be implemented to obtained ferrite cemented body.
That the obtained MnZn FERRITE CORE realizes is that previous MnZn ferrite cannot achieve, 23 DEG C,
The value of initial permeability under 100kHz be 1800 or more and the three-point bending strength evaluation in n=50 in less than 100MPa
The occurrence rate of low-intensity magnetic core is 4% or less such excellent magnetic characteristic and strength characteristics.
It should be noted that as shown in Figure 1, " rod-shaped " in the present invention refers to: length is 30~150mm and diameter is 3
The cylindrical body (a) or length of~10mm is similarly 30~150mm and indulges as 3~10mm, the horizontal cuboid (b) for being 2~8mm.
Moreover, as shown in Fig. 2, by being wound using such rod-shaped MnZn FERRITE CORE as magnetic core 1, in its periphery
Multi-turn electric wire 2 makes antenna, and thereby, it is possible to obtain high-performance and the not antenna of cracky.In addition it is possible to realize antenna
Miniaturization.
Embodiment
Embodiment 1
Fe is weighed in the way of reaching composition ratio shown in table 12O3, ZnO and MnO, by each raw material powder ball mill
After mixing 16 hours, the pre-burning of 925 DEG C, 3 hours is carried out in air.Then, it weighs and is respectively equivalent to 150 mass ppm, 700
The SiO of the amount of quality ppm, 250 mass ppm2, CaO and Nb2O5After be added in the pre-burning powder, with ball mill crush 12 hours.
Then, polyvinyl alcohol is added into obtained crushing raw material, with 250 DEG C of progress spray drying granulations of temperature of outgoing air, then passes through
The sieve that 350 μm of mesh simultaneously removes coarse powder, and then after confirming being mixed into without organic matter, the pressure of load 118MPa and does not use
Release agent shapes toroidal core and rectangular parallelepiped core.It should be noted that the size distribution of pelletizing used in forming
D90 is 230 μm, compression strength 1.32MPa.
Then, these formed bodies are encased in firing furnace, with maximum temperature 1320 DEG C × 2 hours by nitrogen and air
Be burnt into air-flow made of properly mixing, obtain outer diameter 25mm, internal diameter 15mm, height 5mm sintered body toroidal core and
The sintered body rectangular parallelepiped core of vertical 4mm, horizontal 6mm, length 80mm.
It should be noted that the mixed volume of Cl, Na and Al as impurity etc. adds up to 100 mass ppm or less.
Using the rectangular parallelepiped core in obtained sample, it is close that sintering is measured based on JIS C 2560-2 Archimedes method
Degree.About initial permeability, 10 circle coilings are wound on toroidal core and are based on LCR instrument (being that Deco skill company manufactures
4980A) inductance measured calculates.The maximum valley depth of contour curve about surface, with laser microscope (Keyemce corporation
The VK9700 made) with multiplying power: 50 times are observed the surfaces of 50 rectangular parallelepiped cores, based on JIS B 0601 to entire viewing area
The maximum valley depth analysis of contour curve is carried out, and calculates its average value.50 rectangular parallelepiped cores are made about strength test
With the universal testing machine Autograph (Shimadzu Seisakusho Ltd. manufactures) based on JIS R1601 and fixture is destroyed, is according to fulcrum spacing
75mm, three point bending test is disposed and is implemented with a thickness of 4mm, the mode that width is 6mm, record three in 50 test films
The appearance quantity of magnetic core of the point bending strength less than 100MPa, calculates occurrence rate.
Obtained result is recorded in table 1 together.
[table 1]
As shown in the table, be 23 DEG C as embodiment 1-1~1-5 of example, the initial permeability under 100kHz is
1800 or more and the generation rate of magnetic core of the three-point bending strength less than 100MPa be 4% hereinafter, having good magnetic special simultaneously
Property and high intensity.
In contrast, only containing the Fe less than 51.5 moles of %2O3Comparative example (comparative example 1-1) and Fe2O3More than 54.5
In the comparative example (comparative example 1-2) of mole %, although can be realized high intensity, magnetic anisotropy and magnetostriction become larger, because
The decline of this initial permeability, is unsatisfactory for 1800 or more at 23 DEG C, 100kHz.
In addition, because Curie temperature excessively rises in the insufficient comparative example (comparative example 1-3) of ZnO, on the contrary containing than appropriate
Because initial permeability shows that the secondary peak of maximum declines in the comparative example (comparative example 1-4) of the more ZnO of range, 23 DEG C,
Initial permeability under 100kHz still not satisfies 1800 or more.
Embodiment 2
According to reaching Fe2O3: the mode of the composition of 53.0 moles %, ZnO:12.0 moles %, MnO:35.0 moles of % weighs
Raw material after being mixed 16 hours with ball mill, carries out the pre-burning of 925 DEG C, 3 hours in air.Then, it is added into the pre-burning powder
The SiO of amount shown in table 22、CaO、Nb2O5, CoO further is added into a part of sample, is crushed 12 hours with ball mill.
Then, polyvinyl alcohol is added into obtained crushing raw material, with 250 DEG C of progress spray drying granulations of temperature of outgoing air, then passes through
The sieve that 350 μm of mesh simultaneously removes coarse powder, and then after confirming being mixed into without organic matter, does not use release agent connection to load 118MPa
Pressure, shape toroidal core and rectangular parallelepiped core.It should be noted that the size distribution of pelletizing used in forming
D90 is 230 μm, compression strength 1.32MPa.
Then, these formed bodies are encased in firing furnace, with maximum temperature 1320 DEG C × 2 hours by nitrogen and air
Be burnt into air-flow made of properly mixing, obtain outer diameter 25mm, internal diameter 15mm, height 5mm sintered body toroidal core and
The sintered body rectangular parallelepiped core of vertical 4mm, horizontal 6mm, length 80mm.
It should be noted that the mixed volume of Cl, Na and Al as impurity add up to 100 mass ppm or less.
For above-mentioned each sample, respective characteristic is evaluated using method, apparatus same as Example 1.
Obtained result is recorded in table 2 together.
[table 2]
As shown in the table, SiO2、CaO、Nb2O5And the embodiment 2-1~2-8 of CoO amount in the appropriate range be 23 DEG C,
Initial permeability under 100kHz is 1800 or more and the generation rate of magnetic core of the three-point bending strength less than 100MPa is 4%
Hereinafter, good magnetic characteristic and high intensity can be taken into account.
In contrast, SiO2, CaO and Nb2O5Even if only a kind of comparative example 2-1,2- lower than appropriate amount in these three ingredients
In 3 and 2-5, the decline of initial permeability caused by being declined by resistivity is also observed, further, since the generation of crystal boundary is insufficient
And make the not of uniform size of crystal grain, therefore, the generation rate of low-intensity magnetic core of the three-point bending strength less than 100MPa is also got higher.
Even if in addition, being also not only due to occur abnormal in mentioned component in one kind excessive comparative example 2-2,2-4 and 2-6
Crystal grain and be remarkably decreased initial permeability, and sometimes due to sintering be suppressed and keep sintered density low, low-intensity magnetic core
Generation rate get higher.
Further, in CoO amount comparative example 2-7 excessive compared with proper range, by force, therefore magnetic anisotropy excessively becomes
Initial permeability decline.
Embodiment 3
Using by method, selection shown in embodiment 1,2 with embodiment 1-2 identical composition and with embodiment 2-7 phase
With this 2 composition conditions of composition and using be spray-dried and sieving condition obtain pelletizing (size distribution d90 be 230 μm,
Compression strength is 1.32MPa), production formed body (does not use release agent) when forming, by the formed body various temperature shown in table 3
It is burnt under the conditions of degree.
For obtained each sample, each characteristic is evaluated using method, apparatus same as Example 1.The knot that will be obtained
Fruit is recorded in table 3 together.
[table 3]
By keeping temperature to be set as 1290 DEG C or more highest when being burnt into and will be set as the retention time 1 hour or more making
Sintered density reaches 4.85g/cm3Above embodiment 3-1~3-10 is 23 DEG C, the initial permeability under 100kHz is 1800
Above and the generation rate for the magnetic core that three-point bending strength is less than 100MPa can be suppressed to 4% hereinafter, can take into account good
Magnetic characteristic and high intensity.
In contrast, firing temperature is less than 4.85g/ less than 1 hour, to sintered density lower than 1290 DEG C or retention time
cm3Comparative example 3-1~3-6 in, since sintered density is low, three-point bending strength is high less than the generation rate of 100MPa, this
Outside, keep the value of initial permeability also low since the grain growth based on firing is insufficient, only terminated in not at 23 DEG C, 100kHz
Foot 1800.
Embodiment 4
Use making by method shown in embodiment 1,2, selection composition identical with embodiment 1-2 and and embodiment
2-7 is identical to form this 2 composition conditions and (size distribution d90 is using the pelletizing being spray-dried and sieving condition obtains
230 μm, compression strength 1.32MPa), for part of it, the various SOLID ORGANICs of amount shown in table 4 are added before formation
Object release agent, and after mixing, the pressure of load 118MPa and shape toroidal core and rectangular parallelepiped core.Then, by this
Formed body is encased in firing furnace, with 1320 DEG C × 2 hours air-flows made of properly mixing nitrogen and air of maximum temperature
In be burnt into, obtain outer diameter 25mm, internal diameter 15mm, the sintered body toroidal core of height 5mm and vertical 4mm, horizontal 6mm, length
The sintered body rectangular parallelepiped core of 80mm.
For above-mentioned each sample, respective characteristic is evaluated using method, apparatus same as Example 1.By what is obtained
As a result it is recorded in table 4 together.
[table 4]
The maximum valley depth for not mixing the solid organic matters release agent, surface that usually add when manufacturing MnZn ferrite is average
Value in 17 μm of embodiment 1-2 and 2-7 below, 23 DEG C, the initial permeability under 100kHz be 1800 or more and can will
The generation rate of magnetic core of the three-point bending strength less than 100MPa is suppressed to 4% hereinafter, good magnetic characteristic and high-strength can be taken into account
Degree.
In contrast, it is added in comparative example 4-1~4-12 of release agent, trace remains in surface, therefore, surface
The average value of maximum valley depth reaches 17 μm or more, becomes break origins when failure test, therefore, three-point bending strength is less than
The generation rate of 100MPa is got higher, and cannot take into account good magnetic characteristic and high intensity.
Embodiment 5
Use making by method shown in embodiment 1,2, selection composition identical with embodiment 1-2 and and embodiment
The identical pelletizing (compression strength 1.32MPa) for forming this 2 composition conditions and being obtained using spray drying condition of 2-7,
Make the value of size distribution d90 shown in its table 5 by changing sieving condition, after confirmation being mixed into without organic matter, does not make
With the pressure of release agent connection to load 118MPa, toroidal core and rectangular parallelepiped core are shaped.Then, which is encased in burning
At in furnace, it was burnt into, is obtained in the air-flow made of properly mixing nitrogen and air with maximum temperature 1320 DEG C × 2 hours
Outer diameter 25mm, internal diameter 15mm, the sintered body toroidal core of height 5mm and vertical 4mm, horizontal 6mm, length 80mm sintered body cuboid
Magnetic core.
For above-mentioned each sample, respective characteristic is evaluated using method, apparatus same as Example 1.The knot that will be obtained
Fruit is recorded in table 5 together.
[table 5]
The value of pelletizing size distribution d90 does not have in excessive embodiment 1-2,2-7 and 5-1~5-2, is not easy residual forming
Shi Rongyi remains in the gap between thick pelletizing, it is thereby achieved that the maximum valley depth average value on sintered body surface be 17 μm with
Under, 23 DEG C, the initial permeability under 100kHz is 1800 or more and three-point bending strength can also be less than to the magnetic of 100MPa
The generation rate of core is suppressed to 4% hereinafter, good magnetic characteristic and high intensity can be taken into account.
In contrast, the gap between residual pelletizing is easy when being conceived to pelletizing size distribution d90 excessive, forming
Comparative example 5-1~5-6, the maximum valley depth average value on surface are greater than the starting point of 17 μm, its fracture when becoming failure test, because
This, generation rate of the three-point bending strength less than 100MPa is got higher, and cannot take into account good magnetic characteristic and high intensity.
Embodiment 6
The production of method shown in embodiment 1,2, selection composition identical with embodiment 1-2 and embodiment 2-7 will be passed through
This 2 composition conditions and the crushing raw material temperature of outgoing air shown in table 6 made under the conditions of, are spray-dried, and are thus resisted
The different pelletizing of Compressive Strength passes through 350 μm of mesh of sieves and removes coarse powder (size distribution d90 is 230 μm), further exists
After confirmation being mixed into without organic matter, without using release agent and applies the pressure of 118MPa, shape toroidal core and cuboid magnetic
Core.
Then, these formed bodies are encased in firing furnace, with maximum temperature 1320 DEG C × 2 hours by nitrogen and air
Be burnt into air-flow made of properly mixing, obtain outer diameter 25mm, internal diameter 15mm, height 5mm sintered body toroidal core and
The sintered body rectangular parallelepiped core of vertical 4mm, horizontal 6mm, length 80mm.
For above-mentioned each sample, respective characteristic is evaluated using method, apparatus same as Example 1.By what is obtained
As a result it is recorded in table 6 together.
[table 6]
The temperature of outgoing air of spray drying granulation does not have in excessively high embodiment 1-2,2-7 and 6-1~6-2, and pelletizing resists
Compressive Strength is less than 1.5MPa, and therefore, in forming, pelletizing is sufficiently broken, thus does not remain the gap between pelletizing, therefore,
Realize sintered body surface maximum valley depth average value be 17 μm hereinafter, 23 DEG C, the initial permeability under 100kHz be 1800 with
Above and the generation rate for the magnetic core that three-point bending strength is less than 100MPa can be suppressed to 4% hereinafter, can take into account good
Magnetic characteristic and high intensity.
In contrast, it is conceived to comparative example 6-1~6- that temperature of outgoing air is excessively high, pelletizing compression strength is 1.5MPa or more
6, the maximum valley depth average value on surface is greater than 17 μm, the starting point of fracture when as failure test, therefore, three-point bending strength
Generation rate less than 100MPa is got higher, and cannot take into account good magnetic characteristic and high intensity.
Symbol description
1 magnetic core
2 electric wires
Claims (12)
1. a kind of rod-shaped MnZn FERRITE CORE contains iron as basis: with Fe2O3Conversion meter 51.5~54.5 rubs
You are %, zinc: 10.0~17.0 moles of %, manganese in terms of ZnO conversion: surplus；
As accessory ingredient, contain SiO2: 50~300 mass ppm, CaO:100~1300 mass ppm and Nb2O5: 100~400 matter
Ppm is measured,
Wherein,
The sintered density of the MnZn FERRITE CORE is 4.85g/cm3More than,
In the surface texture observation based on JIS B 0601, the average value of the maximum valley depth of contour curve when n=50 is 17 μ
M or less.
2. a kind of rod-shaped MnZn FERRITE CORE, by the iron as basis: with Fe2O3Conversion meter 51.5~54.5 rubs
You are %, zinc: 10.0~17.0 moles of %, manganese in terms of ZnO conversion: surplus；SiO as accessory ingredient2: 50~300 mass ppm,
The mass of CaO:100~1300 ppm and Nb2O5: 100~400 mass ppm；And inevitably impurity is constituted, wherein
The sintered density of the MnZn FERRITE CORE is 4.85g/cm3More than,
In the surface texture observation based on JIS B 0601, the average value of the maximum valley depth of contour curve when n=50 is 17 μ
M or less.
3. rod-shaped MnZn FERRITE CORE according to claim 1 or 2, wherein as accessory ingredient, further contain
CoO:3500 mass ppm or less.
4. rod-shaped MnZn FERRITE CORE according to any one of claim 1 to 3, wherein the rod-shaped MnZn
Initial permeability μ of the FERRITE CORE at 23 DEG C, 100kHziIt is 1800 or more.
5. rod-shaped MnZn FERRITE CORE according to any one of claim 1 to 4, wherein with n=50 to the bar
When the MnZn FERRITE CORE of shape measures three-point bending strength, the occurrence rate of magnetic core of the intensity less than 100MPa is 4% or less.
6. rod-shaped MnZn FERRITE CORE according to any one of claim 1 to 5, wherein the rod-shaped MnZn
FERRITE CORE is the MnZn ferrite formed by forming-sintered body that the value of size distribution d90 is 300 μm of pelletizings below
Magnetic core.
7. rod-shaped MnZn FERRITE CORE according to any one of claim 1 to 6, wherein the rod-shaped MnZn
FERRITE CORE is the MnZn FERRITE CORE that forming-sintered body of the pelletizing by compression strength less than 1.5MPa is formed.
8. a kind of manufacturing method of rod-shaped MnZn FERRITE CORE, includes
The pre-burning process of pre-burning is carried out to the mixture of basis；
Mixing-the pulverizing process for adding accessory ingredient into the pre-burning powder obtained by above-mentioned pre-burning process and being mixed, being crushed；
The granulating working procedure adding binder into the comminuted powder obtained by above-mentioned mixing-pulverizing process and being granulated after mixing；
The forming process that the pelletizing obtained by above-mentioned granulating working procedure is formed；With
The formed products obtained as above-mentioned forming process are burnt into and obtain MnZn described in any one of claims 1 to 5
The firing process of FERRITE CORE.
9. the manufacturing method of MnZn FERRITE CORE according to claim 8, wherein the size distribution of the pelletizing
The value of d90 is 300 μm or less.
10. the manufacturing method of MnZn FERRITE CORE according to claim 8 or claim 9, wherein the pressure resistance of the pelletizing
Degree is less than 1.50MPa.
11. the manufacturing method of MnZn FERRITE CORE according to any one of claim 8 to 10, wherein it is described at
It is formed in shape process without using release agent.
12. a kind of antenna, have MnZn FERRITE CORE is formed as described in any one of claims 1 to 7 magnetic core and
In the electric wire of its periphery winding multi-turn.
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| JP2017-079223 | 2017-04-12 | ||
| JP2017079223 | 2017-04-12 | ||
| PCT/JP2017/047118 WO2018189967A1 (en) | 2017-04-12 | 2017-12-27 | Rod-shaped mnzn ferrite core and method for producing same, and antenna |
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| CN109311763A true CN109311763A (en) | 2019-02-05 |
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| JP (1) | JP6462959B1 (en) |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112041274A (en) * | 2019-03-18 | 2020-12-04 | 杰富意化学株式会社 | MnZn ferrite and method for producing same |
| CN112041273A (en) * | 2019-03-18 | 2020-12-04 | 杰富意化学株式会社 | MnZn ferrite and method for producing same |
| CN112041275A (en) * | 2019-03-18 | 2020-12-04 | 杰富意化学株式会社 | MnCoZn-based ferrite and method for producing same |
| CN114190088A (en) * | 2020-07-14 | 2022-03-15 | 杰富意化学株式会社 | MnZn ferrite |
| CN114206805A (en) * | 2020-07-14 | 2022-03-18 | 杰富意化学株式会社 | MnZn ferrite |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020158333A1 (en) * | 2019-01-31 | 2020-08-06 | Ｊｆｅケミカル株式会社 | Mnzn-based ferrite and method for manufacturing same |
| JP6732158B1 (en) * | 2019-03-18 | 2020-07-29 | Ｊｆｅケミカル株式会社 | MnZn-based ferrite and method for producing the same |
| WO2023182133A1 (en) * | 2022-03-23 | 2023-09-28 | 戸田工業株式会社 | MnZn-BASED FERRITE |
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| CN112041273A (en) * | 2019-03-18 | 2020-12-04 | 杰富意化学株式会社 | MnZn ferrite and method for producing same |
| CN112041275A (en) * | 2019-03-18 | 2020-12-04 | 杰富意化学株式会社 | MnCoZn-based ferrite and method for producing same |
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| CN112041275B (en) * | 2019-03-18 | 2022-12-27 | 杰富意化学株式会社 | MnCoZn-based ferrite and method for producing same |
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| CN114190088B (en) * | 2020-07-14 | 2023-03-21 | 杰富意化学株式会社 | MnZn ferrite |
Also Published As
| Publication number | Publication date |
|---|---|
| JPWO2018189967A1 (en) | 2019-04-18 |
| JP6462959B1 (en) | 2019-01-30 |
| WO2018189967A1 (en) | 2018-10-18 |
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