CN104609847A - Preparation method for improving manganese zinc power ferrite material resistivity - Google Patents

Preparation method for improving manganese zinc power ferrite material resistivity Download PDF

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Publication number
CN104609847A
CN104609847A CN201410787315.5A CN201410787315A CN104609847A CN 104609847 A CN104609847 A CN 104609847A CN 201410787315 A CN201410787315 A CN 201410787315A CN 104609847 A CN104609847 A CN 104609847A
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ball milling
preparation
carry out
resistivity
sno2
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CN201410787315.5A
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陈玮
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YUYAO YIWEI ELECTRONIC TECHNOLOGY Co Ltd
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YUYAO YIWEI ELECTRONIC TECHNOLOGY Co Ltd
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Abstract

The invention discloses a preparation method for improving manganese zinc power ferrite material resistivity, the preparation method is as follows: main material and auxiliary material preparation, first ball milling, presintering, second ball milling, granulating, forming and the like, before the first ball milling, TiO2 and SnO2 are doped, or SnO2 is doped; before the second ball milling, CaCO3, SiO2, Ta2O5 ,Nb2O5 and / or V2O5 are doped; the effect of doping of SnO2 / TiO2 before the first ball milling is better than doping of SnO2 / TiO2 before the second ball milling, and the ferrite material property improving effects of SnO2 and TiO2 can be more effectively played, and by adding of trace impurities and changing of the order of doping, the material resistivity can be improved obviously to achieve the purpose of reducing the loss.

Description

A kind of preparation method improving manganese-zinc power ferrite resistivity of material
Technical field
The invention belongs to ferrimagnetism soft magnetic materials technical field, relate to a kind of manganese-zinc power ferrite material.
Background technology
Mn-Zn ferrite has the advantages such as resistivity is high, eddy-current loss is little, low price, is adapted at alternating magnetic field particularly in high frequency and the application of ultra-high frequency field, is mainly divided into high magnetic conductivity ferrite and power ferrite.The latter is a wherein most widely used class material, constantly towards the future development of high-frequency low-consumption.
Ferrite magnetic core loss, comprises magnetic hysteresis loss, eddy-current loss and residual loss.Along with the rising of frequency of utilization, eddy-current loss becomes dominant loss, and magnetic permeability can be caused to reduce rapidly.This kind of loss can be reduced by improving resistivity.
Resistivity comprises intra-die resistivity and grain boundary resistivity.Conduction root mainly a small amount of Fe of intra-die 2+existence, can by high valence ion as Ti 4+, Nb 5+deng and Fe 2+form electron pair, reduce electronic migration.Promoting grain boundary resistance rate mainly makes impurity enriched at grain boundary place by the mode of doping, forms resistive formation.
The most frequently used additive is CaCO 3and SiO 2, and V 2o 5, SnO 2, Nb 2o 5add Deng combination, resistivity can be promoted further.Nb 5+ca can be stoped 2+, Si 4+plasma enters lattice, makes it be enriched in grain boundaries.V 5+also crystal boundary is enriched in, and Ca 2+, Si 4+common formation resistive formation.Sn 4+both be present in crystal boundary, and can enter again in lattice and Fe 2+form stable electron pair.Ta 5+not only there is grain boundaries, also can refining grain size, increase grain boundary area, can resistivity be improved equally.In addition some hotchpotch is become from secondary doping and once adulterate, make it can play a role in pre-burning and subsequent technique, also can effectively promote ferrite resistivity.
Summary of the invention
The object of this invention is to provide a kind of preparation method improving manganese-zinc power ferrite resistivity of material.
It is as follows that the present invention realizes the technical scheme that above-mentioned purpose adopts:
The preparation method of manganese-zinc power ferrite material, comprises the steps:
(1) major ingredient is joined: the molar ratio ingredient by following component and content: Fe 2o 351.6-53.8mol%, MnO 31.5-37.2mol%, ZnO 11.2-15.7mol;
(2) auxiliary material is joined: the CaCO being equivalent to major ingredient 0.02-0.06wt% 3, 0.002-0.005wt% SiO 2, 0.01-0.04wt% V 2o 5, 0.01-0.03wt% TiO 2, 0.05-0.15wt% SnO 2, 0.01-0.04wt% Nb 2o 5, 0.02wt%-0.04wt% Ta 2o 5;
(3) ball millings: by three kinds of major ingredients and SnO 2and/or TiO 2after impurity mixing, carry out a ball milling, the time is 1.5 hours;
(4) dry, pre-burning: spraying dry, then carry out pre-burning, calcined temperature is: 800-850 DEG C, and burn-in time is 1.5-2.5 hour;
(5) broken pulverizing, doping, secondary ball milling: Preburning material is pulverized, mixes impurity CaCO 3, SiO 2, V 2o 5, Ta 2o 5, Nb 2o 5, carry out secondary ball milling after mixing, the time is 1.5-2.5 hour;
(6) shaping, sintering: after oven dry, add 8% PVAC polyvinylalcohol and carry out granulation, then on press, granular powder is pressed into base, put into sintering oven, the sintering temperature of 1320-1380 DEG C, be incubated 4-4.5 hour under the oxygen partial pressure of 4%-15%, make MnZn ferrite material.
The present invention passes through interpolation and the adjustment doping order of trace impurity, significantly improves the resistivity of material, reaches the object reduced the wastage.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Implementation method 1:
Step 1, the molar ratio ingredient by following component and content: Fe 2o 352.4%, MnO 33.9%, ZnO 13.7%, be equivalent to the SnO of major ingredient 0.1wt% 2, 0.03wt% TiO 2;
Step 2, a ball milling: by three kinds of major ingredients and SnO 2, TiO 2carry out a ball milling after mixing, the time is 1.5 hours;
Step 3, dry, pre-burning: spraying dry, then carry out pre-burning, calcined temperature is: 850 DEG C, and burn-in time is 2 hours;
Step 4, doping, secondary ball milling: Preburning material is pulverized, mixes the CaCO being equivalent to major ingredient 0.02wt% 3, 0.004wt% SiO 2, 0.025wt% V 2o 5, 0.03wt% Ta 2o 5, 0.025wt% Nb 2o 5, carry out secondary ball milling after mixing, the time is 2 hours;
Step 5, shaping, sintering: after oven dry, add 8% PVAC polyvinylalcohol and carry out granulation, then on press, granular powder is pressed into base, puts into sintering oven, the sintering temperature of 1340 DEG C, be incubated 4.5 hours under the oxygen partial pressure of 6%, make MnZn ferrite material.
Implementation method 2:
Step 1, the molar ratio ingredient by following component and content: Fe 2o 352.7%, MnO 34.71%, ZnO 12.59%, and be equivalent to the SnO of major ingredient 0.1wt% 2mixing;
Step 2, a ball milling: by three kinds of major ingredients and SnO 2carry out a ball milling after mixing, the time is 1.5 hours;
Step 3, dry, pre-burning: spraying dry, then carry out pre-burning, calcined temperature is: 850 DEG C, and burn-in time is 2 hours;
Step 4, doping, secondary ball milling: Preburning material is pulverized, mixes the CaCO being equivalent to major ingredient 0.02wt% 3, 0.004wt% SiO 2, 0.025wt% V 2o 5, 0.03wt% Ta 2o 5, 0.025wt% Nb 2o 5, carry out secondary ball milling after mixing, the time is 2 hours;
Step 5, shaping, sintering: after oven dry, add 8% PVAC polyvinylalcohol and carry out granulation, then on press, granular powder is pressed into base, puts into sintering oven, the sintering temperature of 1340 DEG C, be incubated 4.5 hours under the oxygen partial pressure of 6%, make MnZn ferrite material.
Implementation method 3:
Step 1, the molar ratio ingredient by following component and content: Fe 2o 353.8%, MnO 32.5%, ZnO 13.7%, be equivalent to the SnO of major ingredient 0.1wt% 2, 0.03wt% TiO 2;
Step 2, a ball milling: by three kinds of major ingredients and SnO 2, TiO 2carry out a ball milling after mixing, the time is 1.5 hours;
Step 3, dry, pre-burning: spraying dry, then carry out pre-burning, calcined temperature is: 850 DEG C, and burn-in time is 2 hours;
Step 4, doping, secondary ball milling: Preburning material is pulverized, mixes the CaCO being equivalent to major ingredient 0.02wt% 3, 0.004wt% SiO 2, 0.025wt% V 2o 5, 0.03wt% Ta 2o 5, 0.025wt% Nb 2o 5, carry out secondary ball milling after mixing, the time is 2 hours;
Step 5, shaping, sintering: after oven dry, add 8% PVAC polyvinylalcohol and carry out granulation, then on press, granular powder is pressed into base, puts into sintering oven, the sintering temperature of 1340 DEG C, be incubated 4.5 hours under the oxygen partial pressure of 6%, make MnZn ferrite material.
Implementation method 4:
Step 1, the molar ratio ingredient by following component and content: Fe 2o 352.8%, MnO 31.5%, ZnO15.7%, is equivalent to the SnO of major ingredient 0.1wt% 2;
Step 2, a ball milling: by three kinds of major ingredients and SnO 2carry out a ball milling after mixing, the time is 1.5 hours;
Step 3, dry, pre-burning: spraying dry, then carry out pre-burning, calcined temperature is: 850 DEG C, and burn-in time is 2 hours;
Step 4, doping, secondary ball milling: Preburning material is pulverized, mixes the CaCO being equivalent to major ingredient 0.02wt% 3, 0.004wt% SiO 2, 0.025wt% V 2o 5, 0.03wt% Ta 2o 5, 0.025wt% Nb 2o 5, carry out secondary ball milling after mixing, the time is 2 hours;
Step 5, shaping, sintering: after oven dry, add 8% PVAC polyvinylalcohol and carry out granulation, then on press, granular powder is pressed into base, puts into sintering oven, the sintering temperature of 1340 DEG C, be incubated 4.5 hours under the oxygen partial pressure of 6%, make MnZn ferrite material.
Implementation method 5:
Step 1, the molar ratio ingredient by following component and content: Fe 2o 351.6%, MnO 37.2%, ZnO11.2%, is equivalent to the SnO of major ingredient 0.1wt% 2;
Step 2, a ball milling: by three kinds of major ingredients and SnO 2carry out a ball milling after mixing, the time is 1.5 hours;
Step 3, dry, pre-burning: spraying dry, then carry out pre-burning, calcined temperature is: 850 DEG C, and burn-in time is 2 hours;
Step 4, doping, secondary ball milling: Preburning material is pulverized, mixes the CaCO being equivalent to major ingredient 0.02wt% 3, 0.004wt% SiO 2, 0.025wt% V 2o 5, 0.03wt% Ta 2o 5, 0.025wt% Nb 2o 5, carry out secondary ball milling after mixing, the time is 2 hours;
Step 5, shaping, sintering: after oven dry, add 8% PVAC polyvinylalcohol and carry out granulation, then on press, granular powder is pressed into base, puts into sintering oven, the sintering temperature of 1340 DEG C, be incubated 4.5 hours under the oxygen partial pressure of 6%, make MnZn ferrite material.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (3)

1. improve a preparation method for manganese-zinc power ferrite resistivity of material, it is characterized in that, comprise manganese oxide, ferric oxide, zinc oxide three kinds of main ingredients, these three kinds of components are mixed in proportion and prepare burden, then mix micro-additive TiO 2and/or SnO 2, carry out ball milling, pre-burning, then mix micro-additive CaCO 3, SiO 2, Ta 2o 5, Nb 2o 5and/or V 2o 5, carry out secondary ball milling, granulation, shaping.
2. a kind of preparation method improving manganese-zinc power ferrite resistivity of material according to claim 1, it is characterized in that: three kinds of described major constituents, the mol ratio of its content is respectively: ferric oxide 51.6-53.8mol%, manganese oxide 31.5-37.2mol%, zinc oxide 11.2-15.7mol%.
3. a kind of preparation method improving manganese-zinc power ferrite resistivity of material according to claim 1, is characterized in that, the weight percent of described micro-additive and described three kinds of major constituent sums is: CaCO 30.02-0.06wt%, SiO 20.002-0.005wt%, V 2o 50.01-0.04wt%, TiO 20.01-0.03wt%, SnO 20.05-0.15wt%, Nb 2o 50.01-0.04wt%, Ta 2o 50.02wt%-0.04wt%.
CN201410787315.5A 2014-12-18 2014-12-18 Preparation method for improving manganese zinc power ferrite material resistivity Pending CN104609847A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111116189A (en) * 2019-12-30 2020-05-08 苏州冠达磁业有限公司 High-frequency high-impedance manganese-zinc ferrite and preparation method thereof
CN113620701A (en) * 2021-09-29 2021-11-09 海安南京大学高新技术研究院 Preparation method of superfine-crystal high-temperature-resistant high-frequency manganese-zinc ferrite
CN116864293A (en) * 2023-08-02 2023-10-10 山东春光磁电科技有限公司 Preparation process of high-frequency ferrite material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111116189A (en) * 2019-12-30 2020-05-08 苏州冠达磁业有限公司 High-frequency high-impedance manganese-zinc ferrite and preparation method thereof
CN113620701A (en) * 2021-09-29 2021-11-09 海安南京大学高新技术研究院 Preparation method of superfine-crystal high-temperature-resistant high-frequency manganese-zinc ferrite
CN116864293A (en) * 2023-08-02 2023-10-10 山东春光磁电科技有限公司 Preparation process of high-frequency ferrite material
CN116864293B (en) * 2023-08-02 2024-05-24 山东春光磁电科技有限公司 Preparation process of high-frequency ferrite material

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