CN104108925A - A preparing method of a high-frequency manganese zinc ferrite material - Google Patents

A preparing method of a high-frequency manganese zinc ferrite material Download PDF

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Publication number
CN104108925A
CN104108925A CN201410261891.6A CN201410261891A CN104108925A CN 104108925 A CN104108925 A CN 104108925A CN 201410261891 A CN201410261891 A CN 201410261891A CN 104108925 A CN104108925 A CN 104108925A
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ferrite material
zno
mno
preparation
high frequency
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李前军
沈建元
王步猛
张金兵
陈维兆
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TIANCHANG ZHONGDE ELECTRONICS CO Ltd
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TIANCHANG ZHONGDE ELECTRONICS CO Ltd
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Abstract

A preparing method of a high-frequency manganese zinc ferrite material is disclosed. Raw materials of the ferrite material comprise Fe2O3, ZnO, MnO, SiO2, CaCO3, V2O5, TiO2, and ZrO2, wherein the molar ratio of the Fe2O3, the MnO and the ZnO is (53-56):(38-41):(5-8); and based on the weight sum of the Fe2O3, the MnO and the ZnO, the weight percentages of the SiO2, the CaCO3, the V2O5, the TiO2 and the ZrO2 are respectively 20-70 ppm, 100-800 ppm, 100-500 ppm, 200-2400 ppm and 100-500 ppm. In a preparing process, after each of the raw materials is weighed, the ferrite material is obtained by combination of a plurality of process steps including mixing, vibrating grinding, moulding, pre-sintering, smashing, pulping, powder preparation, humidifying, moulding, sintering and grinding.

Description

A kind of preparation method of high frequency MnZn ferrite material
Technical field
The invention belongs to core material technical field, relate in particular to a kind of preparation method of high frequency MnZn ferrite material.
Background technology
Continuous progress along with Power Electronic Technique, complete electronic set system is to integrated intelligent, mounting of plane, miniaturization and development, thereby require to develop to high frequencyization as the power supply of the requisite integral part of machine system, and the core of high frequency power supply is the Ferrite Material of high-frequency low-consumption.Require above-mentioned Ferrite Material to there is high magnetic permeability, high-density and there is high saturation induction density, high-curie temperature, high resistivity to ensure, thereby there is low-power consumption.At present, Ferrite Material can't well meet service requirements, needs to continue to improve.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of preparation method of high frequency MnZn ferrite material.
The preparation method of a kind of high frequency MnZn ferrite material that the present invention proposes, its raw material comprises: Fe 2o 3, ZnO, MnO, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2, Fe wherein 2o 3: the mol ratio of MnO:ZnO is (53～56): (38～41): (5～8), and with Fe 2o 3, ZnO, MnO three's quality and be benchmark, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2massfraction be respectively 20～70ppm, 100～800ppm, 100～500ppm, 200～2400ppm, 100～500ppm;
In preparation process, S1: take each raw material by proportioning; S2: by the Fe taking in S1 2o 3, ZnO, MnO, CaCO 3, TiO 2after mixing, carry out successively vibration, roll after sheet and Shape correction, utilize retort furnace or rotary kiln to carry out preheating, obtain pre-burning material; S3: by the pre-burning material obtaining in S2 carry out that coarse reduction, fine powder are broken, after slurrying, by spray-drier, make Ferrite Material powder, and above-mentioned Ferrite Material powder is carried out to powder damping, moulding, obtain base substrate, wherein, in pulping process, add the SiO taking in S1 2, V 2o 5, ZrO 2; S4: the base substrate obtaining in S3 is carried out to sintering, in sintering process with the temperature rise rate of 4～5 ℃/min from room temperature rises to 1205～1225 ℃ of insulation 160～180min, cooling, grind, clean, obtain Ferrite Material, wherein, in sintering process, keeping oxygen partial pressure is 5～8%.
Preferably, in S4, in sintering process, with the temperature rise rate of 4～5 ℃/min, from room temperature, rise to 1220 ℃ and be incubated.
Preferably, in S4, soaking time is 175min.
Preferably, in S4, in sintering process, keeping oxygen partial pressure is 6%.
In the present invention, by adopting suitable Fe 2o 3, ZnO, MnO three's proportioning, make ZnO excessive on the one hand, thereby increase substantially initial permeability,, coordinate with Fe meanwhile 2o 3excessive, also contribute to promote initial permeability, on the other hand, regulated and controled Fe 2o 3with the proportionlity of ZnO, can make material obtain applicable Curie temperature, adopt SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2carry out doping treatment to improve the performance of material, wherein, the TiO of interpolation 2, due to Ti 4+electronics can be pinned to Fe 2+on position, thereby reduce Fe 2+, keep electronic equilibrium, reduce material anisotropy Changshu, thereby reduce core loss, the CaCO adding 3, ZrO 2, Ca meeting fractional condensation, on grain boundary, forms high resistance grain boundary, can suppress grain growing simultaneously, make the maximization of crystal boundary face and improve resistivity, and prevention forms double microtexture, V 2o 5can crystal grain thinning, reduce the void content of material, promote ferritic initial permeability, SiO 2can play hydrotropy effect, effectively lower the loss of material, and improve density, by preparation technology is optimized, adopt and mix, vibration, shaping, pre-burning, pulverize, slurrying, powder process, damping, moulding, sintering, grind cooperatively interacting of Alternative step, each composition effect can be given full play to, in sintering process, control sintering temperature and soaking time, make on the one hand crystal grain can grow up and evenly, crystal boundary attenuation, get rid of pore, be conducive to initial permeability and sintered density at better state, on the other hand, prevent that excess Temperature from causing Zn to volatilize and causing internal stress excessive and reduce the initial permeability of material and increase loss, simultaneously, in sintering process, oxygen partial pressure is controlled, between initial permeability and loss, obtain balance, thereby obtain high performance high frequency MnZn ferrite material.
The properties of the high frequency MnZn ferrite material that test makes, performance data is as shown in table 1.
In above-mentioned table 1, data show, Ferrite Material disclosed in this invention has good high frequency magnetic core loss characteristic.
Embodiment
Below in conjunction with specific examples, the present invention is described in detail; should understand; embodiment is only for the present invention is described, rather than for the present invention is limited, and any modification of making on basis of the present invention, is equal to replacement etc. all in protection scope of the present invention.
Embodiment 1
A preparation method for high frequency MnZn ferrite material, its raw material comprises: Fe 2o 3, ZnO, MnO, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2, Fe wherein 2o 3: the mol ratio of MnO:ZnO is 54:39:6, with Fe 2o 3, ZnO, MnO three's quality and be benchmark, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2massfraction be respectively 50ppm, 400ppm, 300ppm, 1200ppm, 300ppm;
According to said ratio, be prepared according to the following steps described high frequency MnZn ferrite material:
S1: take each raw material by proportioning;
S2: by the Fe taking in S1 2o 3, ZnO, MnO, CaCO 3, TiO 2after mixing, carry out successively vibration, roll after sheet and Shape correction, utilize retort furnace or rotary kiln to carry out preheating, obtain pre-burning material;
S3: by the pre-burning material obtaining in S2 carry out that coarse reduction, fine powder are broken, after slurrying, by spray-drier, make Ferrite Material powder, and above-mentioned Ferrite Material powder is carried out to powder damping, moulding, obtain base substrate, wherein, in pulping process, add the SiO taking in S1 2, V 2o 5, ZrO 2;
S4: the base substrate obtaining in S3 is carried out to sintering, in sintering process with the temperature rise rate of 4.5 ℃/min from room temperature rises to 1220 ℃ of insulation 175min, cooling, grind, clean, obtain Ferrite Material, wherein, in sintering process, keeping oxygen partial pressure is 6%.
Embodiment 2
A preparation method for high frequency MnZn ferrite material, its raw material comprises: Fe 2o 3, ZnO, MnO, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2, Fe wherein 2o 3: the mol ratio of MnO:ZnO is 55:40:7, with Fe 2o 3, ZnO, MnO three's quality and be benchmark, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2massfraction be respectively 40ppm, 500ppm, 200ppm, 1000ppm, 200ppm;
According to said ratio, be prepared according to the following steps described high frequency MnZn ferrite material:
S1: take each raw material by proportioning;
S2: by the Fe taking in S1 2o 3, ZnO, MnO, CaCO 3, TiO 2after mixing, carry out successively vibration, roll after sheet and Shape correction, utilize retort furnace or rotary kiln to carry out preheating, obtain pre-burning material;
S3: by the pre-burning material obtaining in S2 carry out that coarse reduction, fine powder are broken, after slurrying, by spray-drier, make Ferrite Material powder, and above-mentioned Ferrite Material powder is carried out to powder damping, moulding, obtain base substrate, wherein, in pulping process, add the SiO taking in S1 2, V 2o 5, ZrO 2;
S4: the base substrate obtaining in S3 is carried out to sintering, in sintering process with the temperature rise rate of 4.8 ℃/min from room temperature rises to 1215 ℃ of insulation 170min, cooling, grind, clean, obtain Ferrite Material, wherein, in sintering process, keeping oxygen partial pressure is 7%.
Embodiment 3
A preparation method for high frequency MnZn ferrite material, its raw material comprises: Fe 2o 3, ZnO, MnO, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2, Fe wherein 2o 3: the mol ratio of MnO:ZnO is 56:41:8, with Fe 2o 3, ZnO, MnO three's quality and be benchmark, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2massfraction be respectively 70ppm, 800ppm, 500ppm, 2400ppm, 500ppm;
According to said ratio, be prepared according to the following steps described high frequency MnZn ferrite material:
S1: take each raw material by proportioning;
S2: by the Fe taking in S1 2o 3, ZnO, MnO, CaCO 3, TiO 2after mixing, carry out successively vibration, roll after sheet and Shape correction, utilize retort furnace or rotary kiln to carry out preheating, obtain pre-burning material;
S3: by the pre-burning material obtaining in S2 carry out that coarse reduction, fine powder are broken, after slurrying, by spray-drier, make Ferrite Material powder, and above-mentioned Ferrite Material powder is carried out to powder damping, moulding, obtain base substrate, wherein, in pulping process, add the SiO taking in S1 2, V 2o 5, ZrO 2;
S4: the base substrate obtaining in S3 is carried out to sintering, in sintering process with the temperature rise rate of 5 ℃/min from room temperature rises to 1225 ℃ of insulation 180min, cooling, grind, clean, obtain Ferrite Material, wherein, in sintering process, keeping oxygen partial pressure is 8%.
Embodiment 4
A preparation method for high frequency MnZn ferrite material, its raw material comprises: Fe 2o 3, ZnO, MnO, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2, Fe wherein 2o 3: the mol ratio of MnO:ZnO is 53:38:5, with Fe 2o 3, ZnO, MnO three's quality and be benchmark, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2massfraction be respectively 20ppm, 100ppm, 100ppm, 200ppm, 100ppm;
According to said ratio, be prepared according to the following steps described high frequency MnZn ferrite material:
S1: take each raw material by proportioning;
S2: by the Fe taking in S1 2o 3, ZnO, MnO, CaCO 3, TiO 2after mixing, carry out successively vibration, roll after sheet and Shape correction, utilize retort furnace or rotary kiln to carry out preheating, obtain pre-burning material;
S3: by the pre-burning material obtaining in S2 carry out that coarse reduction, fine powder are broken, after slurrying, by spray-drier, make Ferrite Material powder, and above-mentioned Ferrite Material powder is carried out to powder damping, moulding, obtain base substrate, wherein, in pulping process, add the SiO taking in S1 2, V 2o 5, ZrO 2;
S4: the base substrate obtaining in S3 is carried out to sintering, in sintering process with the temperature rise rate of 4 ℃/min from room temperature rises to 1205 ℃ of insulation 160min, cooling, grind, clean, obtain Ferrite Material, wherein, in sintering process, keeping oxygen partial pressure is 5%.

Claims (4)

1. a preparation method for high frequency MnZn ferrite material, is characterized in that, its raw material comprises: Fe 2o 3, ZnO, MnO, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2, Fe wherein 2o 3: the mol ratio of MnO:ZnO is (53～56): (38～41): (5～8), and with Fe 2o 3, ZnO, MnO three's quality and be benchmark, SiO 2, CaCO 3, V 2o 5, TiO 2, ZrO 2massfraction be respectively 20～70ppm, 100～800ppm, 100～500ppm, 200～2400ppm, 100～500ppm;
In preparation process, S1: take each raw material by proportioning; S2: by the Fe taking in S1 2o 3, ZnO, MnO, CaCO 3, TiO 2after mixing, carry out successively vibration, roll after sheet and Shape correction, utilize retort furnace or rotary kiln to carry out preheating, obtain pre-burning material; S3: by the pre-burning material obtaining in S2 carry out that coarse reduction, fine powder are broken, after slurrying, by spray-drier, make Ferrite Material powder, and above-mentioned Ferrite Material powder is carried out to powder damping, moulding, obtain base substrate, wherein, in pulping process, add the SiO taking in S1 2, V 2o 5, ZrO 2; S4: the base substrate obtaining in S3 is carried out to sintering, in sintering process with the temperature rise rate of 4～5 ℃/min from room temperature rises to 1205～1225 ℃ of insulation 160～180min, cooling, grind, clean, obtain Ferrite Material, wherein, in sintering process, keeping oxygen partial pressure is 5～8%.
2. the preparation method of high frequency MnZn ferrite material according to claim 1, is characterized in that, in S4, rises to 1220 ℃ be incubated in sintering process with the temperature rise rate of 4～5 ℃/min from room temperature.
3. the preparation method of high frequency MnZn ferrite material according to claim 1, is characterized in that, in S4, soaking time is 175min.
4. the preparation method of high frequency MnZn ferrite material according to claim 1, is characterized in that, in S4, in sintering process, keeping oxygen partial pressure is 6%.
CN201410261891.6A 2014-06-12 2014-06-12 A preparing method of a high-frequency manganese zinc ferrite material Pending CN104108925A (en)

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CN104446422A (en) * 2014-12-24 2015-03-25 宜宾盈泰光电有限公司 Method for sintering manganese zinc ferrite magnetic core by adding zinc ingots in densifying atmosphere
CN106810233A (en) * 2017-01-19 2017-06-09 东莞易力禾电子有限公司 High frequency low-loss manganese zine ferrite and its manufacture method

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Application publication date: 20141022