CN101792306A - Method for producing mnzn ferrite - Google Patents
Method for producing mnzn ferrite Download PDFInfo
- Publication number
- CN101792306A CN101792306A CN201010004303A CN201010004303A CN101792306A CN 101792306 A CN101792306 A CN 101792306A CN 201010004303 A CN201010004303 A CN 201010004303A CN 201010004303 A CN201010004303 A CN 201010004303A CN 101792306 A CN101792306 A CN 101792306A
- Authority
- CN
- China
- Prior art keywords
- temperature
- raw material
- manufacture method
- based ferrite
- ferrite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Magnetic Ceramics (AREA)
- Soft Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
Abstract
A method for producing MnZn ferrite which can produce specified shapes of cores without setting a presintering process, includes a raw material preparation process for preparing raw material of the main constituent, a mixing crushing process for weighing raw material and mixing weighing object by a wet method or dry method and crushing, a prilling and shaping process for prilling the crushed powder into particles and shaping as specified shapes, and a sintering process for sintering the shaped article at prescribed conditions, wherein all Zn ingredients prepared in the raw material preparation process are ferrite compounds, the rest all or a part of Fe ingredient and Mn ingredient are monomer oxides.
Description
Technical field
The present invention relates to simplify the manufacture method of the MnZn based ferrite (ferrite) of manufacturing process, particularly relate to and keeping excellent ferrite characteristic, promptly obtain high saturation magnetic flux density and core loss is controlled to be lower in, can realize the manufacture method of new MnZn based ferrite of the reduction of manufacturing cost.
Background technology
In recent years, the miniaturization of electronic equipments, the sharply development of high outputization.Follow in this, various parts highly integrated, high speed processingization is also developed, requires the big electric currentization of supply lead of supply capability.Parts such as transformer, choke coil are also sought driving under big electric power.In addition, consider that the temperature that the heating when driving causes rises, also require the stable and driving reliably under the high temperature.
In order to adapt to such requirement,, need under operating temperature, have low core loss and high saturation magnetic flux density as to constituting the desired characteristic of Ferrite Material of transformer, choke coil etc.
In order to obtain high saturation magnetic flux density, need in ferrite, increase the amount of Fe.In case yet the increase of the amount of Fe, core loss also increases.Generally speaking, only can not obtain high saturation magnetic flux density and these two good characteristics of low core loss with adjusting the ferritic component of formation.
Attempted following method (for example with reference to Japanese kokai publication hei 6-267726 communique, No. 3707781 communique of Japan's special permission) for this reason.Promptly with Fe
2O
3, MnO and ZnO be principal constituent, thereby additive such as suitably selected Si, Ca, Zr, Nb, Ta, V, Bi, Mo, Sn in this principal constituent and add and constitute Ferrite Material, in addition, adjust the firing condition of the sintering process of Ferrite Material, thereby obtain the characteristic of high saturation magnetic flux density and low core loss.
Generally speaking, the ferritic manufacture method of MnZn (particularly wet method-wet method operation) is made of following operation successively, be about to carry out (2) wet-mixed operation, (3) spraying drying operation, (4) pre-burning operation, (5) coarse reduction operation, the broken operation of (6) fine powder, (7) mist projection granulating operation, (8) forming process and (9) firing process after main raw material (1) the weighing specified amount of ferriferous oxide, zinc oxide, Mn oxide.
In a series of like this manufacturing process, (1) weighing specified amount, (2) wet-mixed operation and (3) spraying drying operation are used to make the raw material uniform mixing.In (4) pre-burning operation, make a part of raw material reaction, become ferrite with spinel structure.Owing to be attended by volumetric expansion at this phase time of formation, the generation of crackle or distortion in the time of need preventing main burning till by this pre-burning operation.Utilize after this (5) coarse reduction operation and the broken operation of (6) fine powder, pulverize pre-burning powder, uniform mixing trace additive utilizes (7) mist projection granulating operation to form particle simultaneously, makes the ferrite core body by (8) forming process and (9) firing process.
Yet a series of like this manufacturing process repeats to mix, the high operation of energy consumption such as drying, thermal treatment.Can think that for this reason if realize the simplification of technology and the rationalization of energy consumption, then the possibility of cost reduction is very big.Certainly, its prerequisite is the characteristic quality of the product that guarantees to produce.
(prior art document)
Japanese kokai publication hei 6-267726 communique, No. 3707781 communique of Japan's special permission
Summary of the invention
Under this present situation, intention of the present invention has been proposed, its purpose is to provide a kind of manufacture method of new MnZn based ferrite, keeping excellent ferrite characteristic, promptly obtaining high saturation magnetic flux density and core loss is being controlled to be under the lower state, the simplification of manufacturing process can be realized, and the reduction of manufacturing cost can be realized.
The inventor of the present invention ferritic operation of concentrating on studies for a long time, it found that when formation had the ferrite of spinel structure, the major cause that produces volumetric expansion was to be accompanied by ZnO and Fe
2O
3The rapid variation of lattice parameter of reaction, the volume change that is accompanied by reaction in addition is all less.Think based on this point, if do not cause the ZnO and the Fe of volumetric expansion
2O
3Reaction, whether also the pre-burning operation can be set.If do not carry out this reaction, even then do not carry out pre-burning, there is not bigger volumetric expansion when burning till leading yet, therefore can significantly reduce process number.
Based on above-mentioned viewpoint, inventor of the present invention is based on a large amount of experiments, by making initial feed and firing condition optimization, utilize process number to be about half mixing pulverizing, granulation, shaping, firing process of existing operation, successfully produce ferrite with equal performance.
Being the present invention makes the manufacture method of MnZn based ferrite of the core body of regulation shape for the pre-burning operation is not set, and this method constitutes: comprise raw material preparation process, prepare the raw material of principal constituent; Mix pulverizing process, raw materials weighing is also mixed weighed object by wet method or dry method and is also pulverized; The granulation formation operation is a particle with pulverized powder granulation and be configured as the regulation shape; And firing process, burning till the shaping thing, all Zn compositions of preparing in described raw material preparation process are ferrite compounds (Zn ferrite), remaining all or part of Fe composition and Mn composition are monomeric oxide compound.
In addition, as preferred embodiment of the present invention, all the Mn compositions in the raw material of described raw material preparation process are monomeric oxide compound.
In addition, as preferred embodiment of the present invention, in described raw material preparation process, the principal constituent raw material is ZnFe
2O
4, Fe
2O
3, Mn
3O
4
In addition, as preferred embodiment of the present invention, also prepare the Ni raw material in described raw material preparation process, the Ni composition of part or all in this Ni raw material is monomeric oxide compound.
In addition, as preferred embodiment of the present invention, described firing process has warming temperature portion, high temperature successively and keeps operating portion, cooling operating portion, and described warming temperature portion makes firing temperature from room temperature begin to rise gradually operating area until reaching top temperature; It is to make the top temperature former state that reaches keep the operating area of the state of specified time that described high temperature keeps operating portion; Described cooling operating portion is to make the top temperature that reaches drop near the operating area of room temperature gradually; Described warming temperature portion is from room temperature begin to rise gradually operating area until reaching top temperature, wherein, till room temperature begins firing atmosphere transformation temperature Tv until reaching intensification midway, is to be operation under the condition of 5～21vo1% at oxygen concn; Tv is a boundary with this firing atmosphere transformation temperature, and in the high-temperature zone of the warming temperature portion that is higher than this temperature, making atmosphere is that oxygen concentration is the following substantial oxygen-free atmosphere of 1Vol%.
In addition, as preferred embodiment of the present invention, be boundary with described firing atmosphere transformation temperature Tv, in the high-temperature zone of the warming temperature portion that is higher than this temperature, realize from the conversion of air atmosphere to nitrogen atmosphere.
In addition, as preferred embodiment of the present invention, with described firing atmosphere transformation temperature Tv is boundary, carrying out the mode of the switching of oxygen concn atmosphere smoothly, make in during till temperature reaches Tv in the atmosphere oxygen concn from air atmosphere (oxygen concn is about 21vol%) gradually or staged ground descend.
In addition, as preferred embodiment of the present invention, as described firing atmosphere transformation temperature Tv, the temperature in selected 1000～1200 ℃ of scopes.In addition, as the embodiment of present invention further optimization, as described firing atmosphere transformation temperature Tv, the temperature in selected 1050～1200 ℃ of scopes.
In addition, as preferred embodiment of the present invention, contain by with Fe
2O
3Be scaled 50～65 moles of % ferric oxide, with ZnO be scaled 2～25 moles of % zinc oxide, be scaled the manganese oxide of 25～40 moles of % and be scaled the principal constituent that the nickel oxide of 0～10 mole of % constitutes with MnO with NiO.
In addition, as preferred embodiment of the present invention, as the characteristic of MnZn based ferrite, have following characteristic: the saturation magnetic flux density Bs in the time of 100 ℃ (condition determination: 1194A/m) above for 380mT, (condition determination: 100kHz 200mT) is 800kW/m to the core loss Pcv 100 ℃ the time
3Below.
In addition, as preferred embodiment of the present invention,, contain and be selected from more than at least a among Si, Ca, Zr, Nb, Ta, V, Bi, Mo, the Sn as minor component.
The present invention makes the manufacture method of MnZn based ferrite of the core body of regulation shape for the pre-burning operation is not set, this method comprises the raw material preparation process of the raw material of preparing principal constituent, raw materials weighing and the mixing pulverizing process that mixes weighed object and pulverize by wet method or dry method, with pulverized powder granulation is particle and the granulation formation operation that is configured as the regulation shape, and the firing process that under prescribed condition, burns till the shaping thing, all Zn compositions of preparing in described raw material preparation process are ferrite compounds, and remaining all or part of Fe composition and Mn composition are monomeric oxide compound.Therefore, not only can keep excellent ferrite characteristic, promptly obtain high saturation magnetic flux density and core loss is controlled to be lower, can also realize the simplification of manufacturing process, and realize the reduction of manufacturing cost.
Can calculate, compare that the manufacturing process of the present invention that the pre-burning operation is not set is in the energy consumption (the different changes to some extent of component) that approximately can cut down 40～70% in forming the particulate operation with existing manufacturing process with pre-burning operation.
Embodiment
Below describe the manufacture method of MnZn based ferrite of the present invention in detail.
MnZn based ferrite as manufacturing object of the present invention at first is described.
(to explanation) as the MnZn based ferrite of manufacturing object of the present invention
MnZn based ferrite as manufacturing object of the present invention constitutes: contain with Fe
2O
3Be scaled 50～65 moles of % (preferred 53～61.5 moles of %, more preferably 53～59 moles of %) ferric oxide, with ZnO be scaled 2～25 moles of % (preferred 4～16 moles of %, more preferably 6～13 moles of %) zinc oxide, all the other are that manganese oxide (MnO) is used as principal constituent.
Can further contain the nickel oxide that is scaled 0～10 mole of % (preferred 2～7 moles of %, more preferably 3～6 moles of %) with NiO as principal constituent.
In the said components scope, if Fe
2O
3Then there is the trend that is difficult to obtain desired high saturation magnetic flux density characteristic in 50 moles of % of less than, and if Fe
2O
3Surpass 65 moles of %, then exist core loss to become big trend, thereby can not get desired low core loss characteristic.
In addition, if then there is the less trend of so-called relative density in 2 moles of % of ZnO less than, thereby be difficult to realize low core lossization.And, then have the lower trend of Curie temperature, thereby there is the trend of the undesirable condition of the saturation magnetic flux density reduction that produces under the high temperature if ZnO surpasses 25 moles of %.
In addition, by containing NiO, there is both sides' characteristic isostatic MnZn based ferrite of realizing high saturation magnetic flux density and low core loss easily.Yet raw materials cost increases to some extent.
As the MnZn based ferrite of manufacturing object of the present invention, can contain as minor component and to be selected from more than at least a among Si, Ca, Zr, Nb, Ta, V, Bi, Mo, the Sn.Preferred content is as follows:
SiO
2：0.005～0.03wt％
CaO：0.008～0.17wt％
Nb
2O
5：0.005～0.03wt％
Ta
2O
5：0.01～0.1wt％
V
2O
5：0.01～0.1wt％
ZrO
2：0.005～0.03wt％
Bi
2O
3：0.005～0.04wt％
MoO
3：0.005～0.04wt％
Wherein, preferred especially silicon oxide, calcium oxide, niobium oxides, zirconium white.
The manufacture method of MnZn based ferrite of the present invention then, is described.
(explanation of the manufacture method of MnZn based ferrite)
The manufacture method of MnZn based ferrite of the present invention, the constitutive material of preparing in initial raw material preparation process is greatly different with the existing method of carrying out, and thus, can significantly omit or simplify necessary operation in the existing method.
For example, after the main raw material of weighing specified amount, do not need in operation after this, to carry out to think to it will be further appreciated that the wet-mixed operation, the spraying drying operation that repeat, do not need the pre-burning operation.At this,, need in firing process, carry out technique improvement for the quality characteristic that does not make burned material reduces.
Next coming in order describe.
Basic, the manufacture method of MnZn based ferrite of the present invention is made the manufacture method of MnZn based ferrite of the core body of regulation shape for the pre-burning operation is not set.
(1) raw material preparation process
At first carry out raw material preparation process, prepare the raw material of principal constituent.All Zn compositions of preparing in this raw material preparation process are by ferrite compounds (ZnFe
2O
4) constitute.
Remaining all or part of Fe composition and Mn composition is made of monomeric oxide compound.So-called " remaining whole Fe composition and Mn compositions is made of monomeric oxide compound " is meant that whole remaining Fe compositions and Mn composition are by Fe
2O
3And Mn
3O
4, Mn
2O
3Constitute etc. monomeric oxide compound.Also can comprise as MnCO
3Such pass through the salt that heating is decomposed into oxide compound.
So-called " the Fe composition and the Mn composition of a remaining part are made of monomeric oxide compound " be meant, for example MnFe
2O
4With Fe as monomeric oxide compound
2O
3, Mn
3O
4, Mn
2O
3Exist Deng mixing.Particularly a part of Mn composition is that monomeric oxide compound is meant, for example MnFe
2O
4With Mn
3O
4, Mn
2O
3Mix and exist.In addition, also can comprise as MnCO
3Such pass through the salt that heating is decomposed into oxide compound.
All Mn compositions in the raw material also can be monomeric oxide compound.
As preferred concrete example, the principal constituent raw material uses ZnFe
2O
4, Fe
2O
3And Mn
3O
4In this case, remaining whole Fe composition and Mn composition are made of monomeric oxide compound.
In addition, under the situation of mixing Ni, prepare the Ni raw material, part or all Ni composition in the Ni raw material uses as monomeric oxide compound.
(2) mix pulverizing process
Then, the raw material weighing thing of weighing is mixed by wet method or dry method, and with its pulverizing.
Usually, in this mixing pulverizing process, add minor component.
(3) granulation formation operation
Then, for the forming process after making it is carried out smoothly, be particle by chippy powder granulation.At this moment, preferably in pulverized powder, add suitable binding agent, for example polyvinyl alcohol (PVA) on a small quantity.The particle grain size that preferably obtains is about 80～200 μ m.With the prilling powder press molding.Form for example molding of annular shape.
(4) firing process
Warming temperature portion, beginning from room temperature to rise gradually until the operating area that reaches top temperature, till room temperature begins firing atmosphere transformation temperature Tv until reaching intensification midway, be to be operation (for example air atmosphere (oxygen concn is about 21vol%)) under the condition of 5～21vol% at oxygen concn, Tv is a boundary with this firing atmosphere transformation temperature, in the high-temperature zone of the warming temperature portion that is higher than this temperature, making atmosphere is that oxygen concentration is the following substantial oxygen-free atmosphere of 1Vol%.
Be boundary promptly, in the high-temperature zone of the warming temperature portion that is higher than this temperature, realized from the displacement fully of air atmosphere to nitrogen atmosphere with this firing atmosphere transformation temperature Tv.Under the temperature more than the firing atmosphere transformation temperature Tv, preferably making atmosphere is the atmosphere of complete anaerobic, yet has the generation of the oxygen that causes by burning till, and therefore we can say to be difficult to realize oxygen-free atmosphere completely.Based on this viewpoint, in the present invention, use the form of presentation of " oxygen concentration is the following substantial oxygen-free atmosphere of 1Vol% ".
Firing atmosphere transformation temperature Tv is chosen to be 1000～1200 ℃, be preferably 1050～1200 ℃, the temperature in 1100～1170 ℃ the scope more preferably.
If 1000 ℃ of this temperature T v less thaies then exist the density that produces resulting core body low, the trend of the undesirable condition that the core loss change is big.And if this temperature T v above 1200 ℃, then existing up to arriving keeps the time of temperature too short, utilizing the nitrogen displacement to be difficult to make becomes substantial oxygen-free atmosphere in the firing furnace, have the trend of the undesirable condition that the density that produces resulting core body is low, the core loss change is big.
In addition, for the switching that makes atmosphere can be carried out smoothly, make in preferably during till temperature reaches Tv in the atmosphere oxygen concn from air atmosphere (oxygen concn is about 21vol%) gradually or staged ground descend.For example, be under 1150 ℃ the situation making Tv, if make 1000 ℃ oxygen concn drop to 10vol%, make 1100 ℃ oxygen concn drop to 5vol%, making atmosphere since 1150 ℃ is substantial oxygen-free atmosphere, then is easy to controlled atmosphere correctly.Make from Tv and begin until the heat-up rate that keeps temperature in the scope of 50～300 ℃/hr, preferred 50～150 ℃/hr.
High temperature keeps operating portion, and interior the suiting of scope that high temperature keeps the high temperature in the operating portion to maintain the temperature at about 1250～1400 ℃ set.
Usually, the oxygen partial pressure (PO in the firing atmosphere of high temperature maintenance operating portion
2) be set at oxygen partial pressure value by obtaining with the equilibrium relationship of service temperature.
The cooling operating portion, usually, the oxygen partial pressure (PO in the firing atmosphere of cooling operating portion
2) be set at oxygen partial pressure value by obtaining with the equilibrium relationship of service temperature.
Preferred cooling rate is 30～150 ℃/hr, is preferably 50～100 ℃/hr especially.
(embodiment)
Below, enumerate specific embodiment and further describe the present invention.
(embodiment A-1)
(1) raw material preparation process:, prepare zinc ferrite powder, Mn as the raw material of principal constituent
3O
4Powder, Fe
2O
3Powder as the raw material of minor component, is prepared SiO
2Powder, CaCO
3Powder, ZrO
2Powder and Nb
2O
5Powder.
(2) mix pulverizing process: to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of A in the following table 1 carries out wet-mixed, pulverizing.
In this mixing pulverizing process, add minor component.Represent that with wtppm minor component is SiO with respect to principal constituent
2=100wtppm, as CaO composition CaCO
3=1000wtppm, ZrO
2=100wtppm and Nb
2O
5=200wtppm.
(3) granulation formation operation: adding a spot of polyvinyl alcohol (PVA) in the mixed powder that obtains mix pulverizing, will be after the particulate state by chippy powder granulation, and the press molding prilling powder forms the molding of annular shape.
(4) firing process
Warming temperature portion: set Tv=1150 ℃ of firing atmosphere transformation temperature.Promptly rise gradually until the zone of the warming temperature portion that reaches 1300 ℃ of top temperatures beginning from room temperature, making the intensification atmosphere till room temperature begins to reach Tv=1150 ℃ of firing atmosphere transformation temperature the intensification midway is that air atmosphere (oxygen concn is about 21vol%) is operated.With Tv=1150 ℃ of this firing atmosphere transformation temperature is boundary, in the high-temperature area of the warming temperature portion that is higher than this temperature, switches to nitrogen atmosphere, operates in oxygen concentration is substantial oxygen-free atmosphere below the 1Vol%.
Making the heat-up rate till 900 ℃ is 300 ℃/hr, and the heat-up rate till 900 ℃ of temperature that keep operating portion to high temperature is 100 ℃/hr.
High temperature keeps operating portion: keep the high temperature of operating portion to keep temperature to be set at 1300 ℃ high temperature.Hold-time is 4hr.Oxygen partial pressure (PO in the firing atmosphere of high temperature maintenance operating portion
2) be set at oxygen partial pressure value by obtaining with the equilibrium relationship of service temperature.
Cooling operating portion: the oxygen partial pressure (PO in the firing atmosphere of cooling operating portion
2) be set at oxygen partial pressure value by obtaining with the equilibrium relationship of service temperature.
Making the cooling rate that keeps the temperature of operating portion to be reduced to till 1050 ℃ from high temperature is 75 ℃/hr, is 300 ℃/hr from 1050 ℃ of cooling rates that are reduced to room temperature.
Utilize such working order, obtain the ferrite core body of annular shape.The ferrite core body is of a size of external diameter 20mm, internal diameter 10mm, thickness 5mm.
To resulting ferrite sample, measure respectively 100 ℃ saturation magnetic flux density Bs (condition determination: 1194A/m), core loss Pcv (condition determination: 100kHz, 200mT).The results are shown in following table 2.
(embodiment A-2)
Firing atmosphere transformation temperature among the foregoing description A-1 is changed to Tv=1050 ℃.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-1.The results are shown in following table 2.
(embodiment A-3)
Firing atmosphere transformation temperature among the foregoing description A-1 is changed to Tv=1200 ℃.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-1.The results are shown in following table 2.
(embodiment A-4)
Firing atmosphere transformation temperature among the foregoing description A-1 is changed to Tv=1220 ℃.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-1.The results are shown in following table 2.
(embodiment A-5)
Firing atmosphere transformation temperature among the foregoing description A-1 is changed to Tv=990 ℃.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-1.The results are shown in following table 2.
(Embodiment B-1)
In the mixing pulverizing process of the foregoing description A-1, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of B in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-1.The results are shown in following table 2.
(Embodiment B-2)
In the mixing pulverizing process of the foregoing description A-2, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of B in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-2.The results are shown in following table 2.
(Embodiment B-3)
In the mixing pulverizing process of the foregoing description A-3, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of B in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-3.The results are shown in following table 2.
(Embodiment B-4)
In the mixing pulverizing process of the foregoing description A-4, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of B in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-4.The results are shown in following table 2.
(Embodiment B-5)
In the mixing pulverizing process of the foregoing description A-5, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of B in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-5.The results are shown in following table 2.
(Embodiment C-1)
In the mixing pulverizing process of the foregoing description A-1, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of C in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-1.The results are shown in following table 2.
(Embodiment C-2)
In the mixing pulverizing process of the foregoing description A-2, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of C in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-2.The results are shown in following table 2.
(Embodiment C-3)
In the mixing pulverizing process of the foregoing description A-3, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of C in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-3.The results are shown in following table 2.
(Embodiment C-4)
In the mixing pulverizing process of the foregoing description A-4, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of C in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-4.The results are shown in following table 2.
(Embodiment C-5)
In the mixing pulverizing process of the foregoing description A-5, to the ferrite principal constituent (Fe after burning till
2O
3, MnO, ZnO) ratio of component be that the principal constituent raw material that is numbered the ferritic mode weighing of C in the following table 1 carries out wet-mixed, pulverizing.
In addition, similarly made ferrite core body sample, carried out same performance evaluation with the foregoing description A-5.The results are shown in following table 2.
(table 1)
Wherein, the magnetic properties shown in the right side of table 1 is the physics value of the sample of the existing manufacture method manufacturing of the usefulness of object as a comparison, is target value of the present invention.At this, existing method (wet method-wet method operation) is after main raw material (1) the weighing specified amount with ferriferous oxide, zinc oxide, Mn oxide, carries out the method for (2) wet-mixed operation, (3) spraying drying operation, (4) pre-burning operation, (5) coarse reduction operation, the broken operation of (6) fine powder, (7) mist projection granulating operation, (8) forming process and (9) firing process successively.
(table 2)
| The ferrite sample | The ferrite numbering | ??Tv(℃) | Saturation magnetic flux density Bs (mT) | Core loss Pcv (kW/m3) |
| Embodiment A-1 | ??A | ??1150 | ??396 | ??338 |
| Embodiment A-2 | ??A | ??1050 | ??392 | ??353 |
| Embodiment A-3 | ??A | ??1200 | ??393 | ??363 |
| Embodiment A-4 | ??A | ??1220 | ??382 | ??412 |
| Embodiment A-5 | ??A | ??990 | ??388 | ??432 |
| Embodiment B-1 | ??B | ??1150 | ??426 | ??287 |
| Embodiment B-2 | ??B | ??1050 | ??424 | ??298 |
| Embodiment B-3 | ??B | ??1200 | ??423 | ??302 |
| Embodiment B-4 | ??B | ??1220 | ??421 | ??331 |
| Embodiment B-5 | ??B | ??990 | ??422 | ??338 |
| Embodiment C-1 | ??C | ??1150 | ??470 | ??544 |
| Embodiment C-2 | ??C | ??1050 | ??469 | ??576 |
| Embodiment C-3 | ??C | ??1200 | ??468 | ??582 |
| Embodiment A-4 | ??C | ??1220 | ??466 | ??632 |
| Embodiment C-5 | ??C | ??990 | ??467 | ??643 |
Manufacture method of the present invention, its process number compare with existing manufacturing process about reduction half, not only in the energy consumption that can cut down about 40～70% in forming the particulate operation, and (magnetic properties under the situation of the resulting magnetic properties of A-1～A-3, B-1～B-3 and C-1～C-3) and the existing method manufacturing of the utilization shown in the table 1 is roughly the same to utilize each embodiment of table 2.
Utilize above-mentioned experimental result can understand effect of the present invention.Being the present invention makes the manufacture method of MnZn based ferrite of the core body of regulation shape for the pre-burning operation is not set, and this method comprises: raw material preparation process, prepare the raw material of principal constituent; Mix pulverizing process, raw materials weighing is also mixed weighed object by wet method or dry method and is also pulverized; The granulation formation operation is a particle with pulverized powder granulation and be configured as the regulation shape; And firing process, under defined terms, burning till the shaping thing, all Zn compositions of preparing in described raw material preparation process are ferrite compounds, remaining all or part of Fe composition and Mn composition are monomeric oxide compound.Therefore, not only can keep excellent ferrite characteristic, promptly obtain high saturation magnetic flux density and core loss is controlled to be lower, simplification that can also accomplished manufacturing process, realize the extremely excellent effects such as reduction of manufacturing cost.
Can calculate, compare, the manufacturing process of the present invention of pre-burning operation is not set, in the energy consumption that in forming the particulate operation, approximately can cut down 40～70% with existing manufacturing process with pre-burning operation.
(possibility of utilizing on the industry)
The manufacture method of MnZn based ferrite of the present invention can be widely used in various electric component industries.
Claims (12)
1. the manufacture method of a MnZn based ferrite is characterized in that,
Be the pre-burning operation not to be set and the manufacture method of MnZn based ferrite of making the core body of regulation shape,
This method comprises:
Raw material preparation process, the raw material of preparation principal constituent;
Mix pulverizing process, raw materials weighing is also mixed weighed object by wet method or dry method and is also pulverized;
The granulation formation operation will be a particle by chippy powder granulation and be configured as the regulation shape; And
Firing process burns till the shaping thing,
All Zn compositions of preparing in described raw material preparation process are ferrite compounds (Zn ferrite), and remaining all or part of Fe composition and Mn composition are monomeric oxide compound.
2. the manufacture method of MnZn based ferrite as claimed in claim 1 is characterized in that,
All Mn compositions in the raw material of described raw material preparation process are monomeric oxide compound.
3. the manufacture method of MnZn based ferrite as claimed in claim 1 or 2 is characterized in that,
In described raw material preparation process, the principal constituent raw material is ZnFe
2O
4, Fe
2O
3, Mn
3O
4
4. as the manufacture method of any described MnZn based ferrite in the claim 1 to 3, it is characterized in that,
Also prepare the Ni raw material in described raw material preparation process, the Ni composition of part or all in this Ni raw material is monomeric oxide compound.
5. as the manufacture method of any described MnZn based ferrite in the claim 1 to 4, it is characterized in that,
Described firing process has warming temperature portion successively, high temperature keeps operating portion, cooling operating portion,
Described warming temperature portion makes firing temperature from room temperature begin to rise gradually operating area until reaching top temperature,
It is to make the top temperature former state that reaches keep the operating area of the state of specified time that described high temperature keeps operating portion,
Described cooling operating portion is to make the top temperature that reaches drop near the operating area of room temperature gradually,
Described warming temperature portion is from room temperature begin to rise gradually operating area until reaching top temperature, wherein, till room temperature begins firing atmosphere transformation temperature Tv until reaching intensification midway, is to be operation under the condition of 5～21vol% at oxygen concn,
Tv is a boundary with this firing atmosphere transformation temperature, and in the high-temperature zone of the warming temperature portion that is higher than this temperature, making atmosphere is that oxygen concentration is the following substantial oxygen-free atmosphere of 1Vol%.
6. the manufacture method of MnZn based ferrite as claimed in claim 5 is characterized in that,
With described firing atmosphere transformation temperature Tv is boundary, in the high-temperature zone of the warming temperature portion that is higher than this temperature, realizes from the conversion of air atmosphere to nitrogen atmosphere.
7. the manufacture method of MnZn based ferrite as claimed in claim 6 is characterized in that,
With described firing atmosphere transformation temperature Tv is boundary, carrying out the mode of the switching of oxygen concn atmosphere smoothly, make in during till temperature reaches Tv in the atmosphere oxygen concn from air atmosphere (oxygen concn is about 21Vol%) gradually or staged ground descend.
8. as the manufacture method of any described MnZn based ferrite in the claim 5 to 7, it is characterized in that,
As described firing atmosphere transformation temperature Tv, the temperature in selected 1000～1200 ℃ of scopes.
9. as the manufacture method of any described MnZn based ferrite in the claim 5 to 7, it is characterized in that,
As described firing atmosphere transformation temperature Tv, the temperature in selected 1050～1200 ℃ of scopes.
10. as the manufacture method of any described MnZn based ferrite in the claim 1 to 9, it is characterized in that,
Described MnZn based ferrite contains the principal constituent that is made of following material:
With Fe
2O
3Be scaled the ferric oxide of 50～65 moles of %;
Be scaled the zinc oxide of 2～25 moles of % with ZnO;
Be scaled the manganese oxide of 25～40 moles of % with MnO; And
Be scaled the nickel oxide of 0～10 mole of % with NiO.
11. the manufacture method as any described MnZn based ferrite in the claim 1 to 10 is characterized in that,
As the characteristic of MnZn based ferrite, have following characteristic:
Saturation magnetic flux density Bs in the time of 100 ℃ (condition determination: be more than the 380mT 1194A/m);
(condition determination: 100kHz 200mT) is 800kW/m to core loss Pcv in the time of 100 ℃
3Below.
12. the manufacture method as any described MnZn based ferrite in the claim 1 to 11 is characterized in that,
As minor component, contain and be selected from more than at least a among Si, Ca, Zr, Nb, Ta, V, Bi, Mo, the Sn.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2009017655A JP2010173888A (en) | 2009-01-29 | 2009-01-29 | METHOD FOR PRODUCING MnZn FERRITE |
| JP2009-017655 | 2009-01-29 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101792306A true CN101792306A (en) | 2010-08-04 |
Family
ID=42585257
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010004303A Pending CN101792306A (en) | 2009-01-29 | 2010-01-20 | Method for producing mnzn ferrite |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP2010173888A (en) |
| CN (1) | CN101792306A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102299257A (en) * | 2011-06-22 | 2011-12-28 | 泉州师范学院 | Method for preparing zinc-oxide-doped-iron room-temperature magnetic semiconductor |
| CN102403080A (en) * | 2011-11-24 | 2012-04-04 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | Composition for sintering MnZn ferrite magnetic core, product and manufacture method of product |
| CN102424583A (en) * | 2011-09-05 | 2012-04-25 | 吕佳佳 | Magnetic powder for bonding hard ferrite |
| CN102924070A (en) * | 2012-11-05 | 2013-02-13 | 四川省眉山市力达电子有限责任公司 | Wide-temperature, high-frequency and low-power-consumption manganese zinc iron oxidation material and method for manufacturing same |
| CN105503169A (en) * | 2015-12-15 | 2016-04-20 | 无锡斯贝尔磁性材料有限公司 | Method for decreasing sintering temperature of manganese zinc ferrite powder |
| CN107021746A (en) * | 2017-04-01 | 2017-08-08 | 浙江工业大学 | A kind of MnZn ferrite material and preparation method thereof |
| CN109071262A (en) * | 2016-05-02 | 2018-12-21 | 保德科技股份有限公司 | Ferrite powder, resin combination, electromagnetic shielding material, electronic circuit board, electronic circuit component and casting of electronic device |
| CN110937887A (en) * | 2019-12-13 | 2020-03-31 | 横店集团东磁股份有限公司 | High-frequency low-loss MnZn ferrite material and preparation method thereof |
| CN115611624A (en) * | 2022-10-27 | 2023-01-17 | 海宁联丰磁业股份有限公司 | Wide-temperature-range high-Tc high-permeability manganese-zinc ferrite material and preparation method thereof |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5017438B2 (en) * | 2010-09-06 | 2012-09-05 | Ｊｆｅケミカル株式会社 | Cooking device for electromagnetic wave absorption heating element and microwave oven |
| CN102030523A (en) * | 2010-11-05 | 2011-04-27 | 清华大学 | Method for preparing stannic oxide-based low-residual voltage ratio voltage-sensitive ceramic material |
| CN103011790B (en) * | 2012-12-11 | 2014-01-08 | 海宁联丰磁业股份有限公司 | Preparation method of high-permeability manganese zinc ferrite |
| CN113493344A (en) * | 2020-04-01 | 2021-10-12 | 上海继胜磁性材料有限公司 | Magnetic core and manufacturing method thereof |
| CN115132442A (en) * | 2022-07-12 | 2022-09-30 | 广州大学 | Ultrahigh-magnetic-saturation manganese-zinc ferrite magnetic core material and preparation method thereof |
| CN117945742A (en) * | 2022-10-18 | 2024-04-30 | 横店集团东磁股份有限公司 | Manganese zinc ferrite material and preparation method thereof |
-
2009
- 2009-01-29 JP JP2009017655A patent/JP2010173888A/en not_active Withdrawn
-
2010
- 2010-01-20 CN CN201010004303A patent/CN101792306A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102299257B (en) * | 2011-06-22 | 2014-06-04 | 泉州师范学院 | Method for preparing zinc-oxide-doped-iron room-temperature magnetic semiconductor |
| CN102299257A (en) * | 2011-06-22 | 2011-12-28 | 泉州师范学院 | Method for preparing zinc-oxide-doped-iron room-temperature magnetic semiconductor |
| CN102424583A (en) * | 2011-09-05 | 2012-04-25 | 吕佳佳 | Magnetic powder for bonding hard ferrite |
| CN102403080A (en) * | 2011-11-24 | 2012-04-04 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | Composition for sintering MnZn ferrite magnetic core, product and manufacture method of product |
| CN102403080B (en) * | 2011-11-24 | 2015-08-26 | 江苏省晶石磁性材料与器件工程技术研究有限公司 | A kind of MnZn FERRITE CORE sintering composition, goods and article fabrication methods |
| CN102924070A (en) * | 2012-11-05 | 2013-02-13 | 四川省眉山市力达电子有限责任公司 | Wide-temperature, high-frequency and low-power-consumption manganese zinc iron oxidation material and method for manufacturing same |
| CN102924070B (en) * | 2012-11-05 | 2014-07-30 | 四川省眉山市力达电子有限责任公司 | Wide-temperature, high-frequency and low-power-consumption manganese zinc iron oxidation material and method for manufacturing same |
| CN105503169B (en) * | 2015-12-15 | 2018-11-23 | 无锡斯贝尔磁性材料有限公司 | A method of reducing manganese-zinc ferrite powder sintering temperature |
| CN105503169A (en) * | 2015-12-15 | 2016-04-20 | 无锡斯贝尔磁性材料有限公司 | Method for decreasing sintering temperature of manganese zinc ferrite powder |
| CN109071262B (en) * | 2016-05-02 | 2020-05-15 | 保德科技股份有限公司 | Ferrite powder, resin composition, electromagnetic wave shielding material, electronic circuit board, electronic circuit component, and electronic device case |
| CN109071262A (en) * | 2016-05-02 | 2018-12-21 | 保德科技股份有限公司 | Ferrite powder, resin combination, electromagnetic shielding material, electronic circuit board, electronic circuit component and casting of electronic device |
| US11032955B2 (en) | 2016-05-02 | 2021-06-08 | Powdertech Co., Ltd. | Ferrite powder, resin composition, electromagnetic shielding material, electronic circuit substrate, electronic circuit component, and electronic device housing |
| CN107021746A (en) * | 2017-04-01 | 2017-08-08 | 浙江工业大学 | A kind of MnZn ferrite material and preparation method thereof |
| CN110937887A (en) * | 2019-12-13 | 2020-03-31 | 横店集团东磁股份有限公司 | High-frequency low-loss MnZn ferrite material and preparation method thereof |
| CN110937887B (en) * | 2019-12-13 | 2021-02-12 | 横店集团东磁股份有限公司 | High-frequency low-loss MnZn ferrite material and preparation method thereof |
| CN115611624A (en) * | 2022-10-27 | 2023-01-17 | 海宁联丰磁业股份有限公司 | Wide-temperature-range high-Tc high-permeability manganese-zinc ferrite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2010173888A (en) | 2010-08-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101792306A (en) | Method for producing mnzn ferrite | |
| CN101593596B (en) | Ferrite sintered body and manufacturing method therefor | |
| KR100639770B1 (en) | Method for producing Mn-Zn ferrite | |
| CN101038807B (en) | Ferrite material | |
| CN101274846B (en) | Method of producing MnZn-base ferrite | |
| CN101552074A (en) | A NiZnCu ferrite material and preparing method thereof | |
| CN101169996B (en) | A low power consumption Mn-Zn ferrite magnetic material for ultra-high temperature condition and its making method | |
| CN104230321A (en) | M-type calcium permanent magnetic ferrite and preparation method thereof | |
| CN104230322A (en) | M-type calcium permanent magnetic ferrite and preparation method thereof | |
| JP2008184363A (en) | MnZn-BASED FERRITE AND METHOD FOR PRODUCING THE SAME | |
| JP2012180258A (en) | MnZn-BASED FERRITE POWDER, MnZn-BASED FERRITE GRANULES, METHOD OF MANUFACTURING MnZn-BASED FERRITE CORE AND MnZn-BASED FERRITE CORE | |
| CN109704749B (en) | Ultrahigh frequency low-loss soft magnetic ferrite material and preparation method and application of magnetic core | |
| CN111466000B (en) | Ferrite pre-sintered body, ferrite sintered magnet, and method for producing same | |
| CN115215642B (en) | Ferrite composition, electronic component, and power supply device | |
| JP2007297232A (en) | Method for producing oxide magnetic material | |
| KR20210123213A (en) | Ferrite composition, electronic component, and power supply device | |
| CN114605142A (en) | Composite ferrite substrate material for LTCF transformer and preparation method thereof | |
| CN116323491A (en) | MnZn ferrite and method for producing same | |
| JP2008290907A (en) | METHOD OF MANUFACTURING MnZn-BASED FERRITE | |
| JP2003338406A (en) | Method for manufacturing soft magnetic ferrite powder and ferrite core, and ferrite core | |
| KR20120036535A (en) | Nizncu ferrite composition, method of preparing the same, and multi layered chip materials comprising the same | |
| CN115490507B (en) | Broadband high-strength heat shock-resistant nickel-zinc ferrite core and preparation method thereof | |
| JP2008290906A (en) | METHOD OF MANUFACTURING MnZn-BASED FERRITE | |
| JP5929119B2 (en) | Ferrite composition and electronic component | |
| JP5660698B2 (en) | Magnetic oxide material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100804 |