CN101921103A - Manganese zinc ferrite with high magnetic conductivity and preparation method thereof - Google Patents
Manganese zinc ferrite with high magnetic conductivity and preparation method thereof Download PDFInfo
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- CN101921103A CN101921103A CN 201010256561 CN201010256561A CN101921103A CN 101921103 A CN101921103 A CN 101921103A CN 201010256561 CN201010256561 CN 201010256561 CN 201010256561 A CN201010256561 A CN 201010256561A CN 101921103 A CN101921103 A CN 101921103A
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Abstract
The invention discloses a manganese zinc ferrite with a high magnetic conductivity and a preparation method thereof. The preparation method comprises the following steps of: preparing a mixed solution of ferrous sulphate, zinc sulfate, manganese sulfate and indium nitrate in a certain molar ratio; carrying out a constant-temperature coprecipitation reaction in a reactor by utilizing an ammonium bicarbonate solution as a precipitant for preparing a uniformly mixed precursor; then presintering the precursor at 800 DEG C, cooling and pressing for molding; and carrying out high-temperature sintering at a heat treatment temperature of 1,250-1,350 DEG C in an atmosphere furnace for obtaining the manganese zinc ferrite with a high magnetic conductivity. The invention can be used for preparing manganese zinc ferrite materials with different magnetic characteristics through changing the molar ratio of indium nitrate used as an additive and has the advantage of greatly improving the magnetic conductivity with less doping, for example, when the doping molar ratio is 0.1 percent, under the condition that the frequency is 10kHz, the magnetic conductivity can be improved to 9439 from 1712, which can better meet the requirements on the developments of the fields of automotive electronics, network communications, space flight and aviation, satellite communication, and the like.
Description
Technical field
The present invention relates to a kind of Mn-Zn ferrite and preparation method with high magnetic permeability, the Mn-Zn ferrite of high magnetic permeability is applied to magnetic core, the magnetic head materials of electronics, power industry etc.
Background technology
Mn-Zn ferrite belongs to the ferrimagnetism soft magnetic materials, compare with metal, alloy strong magnetic material, have the resistivity height, eddy-current loss is little, oxidation-resistance is strong and advantage such as low price, be adapted at alternating magnetic field, particularly use, therefore obtained important application at aspects such as radio communication, control automatically, computer technology, magnetic recording, radar, radio astronomies at high frequency and ultra-high frequency field.Mn-Zn ferrite mainly is divided into high magnetic conductivity ferrite and power ferrite by using.High magnetic conductivity ferrite from before simple basis of pursuing high magnetic permeability develop on the over-all properties to material, wish that the magnetic permeability of material and impedance have wide temperature characteristics and high aspects such as Curie temperature.The magnetic property of Mn-Zn ferrite and its structure are closely related, improve magnetic property and mainly concentrate in the following areas: 1. optimal preparation technology comprises aspects such as the quality of raw material and thermal treatment process; 2. adjust the material composition ratio; 3. add trace ingredients---doping vario-property.Wherein, the effect of doping vario-property is the most obvious, is subjected to extensive concern.At present, the kind of additive modification is a lot, and mainly be divided three classes with the mechanism of action according to additive existence form in ferrite: 1. additive is deposited on crystal boundary mutually with second, influences the eddy-current loss of grain boundary resistance rate and material, as Elements C aO, SiO
2Deng; 2. additive forms the liquid phase acceleration of sintering in sintering process, improves the microstructure of sample, as V
2O
5, Bi
2O
3Deng; 3. additive enters in the spinel structure, and the substituted metal ion influences the electromagnetic property of material, as NiO, SnO
2, CoO etc., but that the above-mentioned additive of single interpolation improves the manganese-zinc ferrite bulk permeability is not obvious.
In
2O
3Be a kind of dystectic oxide compound, be deposited on crystal boundary and can improve the sample microstructure, simultaneously In
3+Easily enter the spinel lattice and carry out ionic replacement, regulate electromagnetic property, be expected to improve the electromagnetic performance of sample.
Summary of the invention
One of purpose of the present invention is to provide a kind of Mn-Zn ferrite with high magnetic permeability in order to solve the problem that the magnetic permeability of Mn-Zn ferrite is lower in the prior art.
Two of purpose of the present invention provides a kind of preparation method with Mn-Zn ferrite of high magnetic permeability.
Technical scheme of the present invention
The present invention utilizes indium nitrate as additive raw material, adopts coprecipitation method to obtain the presoma that mixes, and then uses the high temperature sintering technology to prepare the Mn-Zn ferrite of the adulterated high magnetic permeability of indium.
A kind of preparation method with Mn-Zn ferrite of high magnetic permeability comprises the steps:
(1), the preparation of precursor
Ferrous sulfate, zinc sulfate, manganous sulfate and additive are hybridly prepared into the aqueous solution, then utilize ammonium bicarbonate soln as precipitation agent, adopt and add feed way and join that constant temperature (about 40 ℃) carries out coprecipitation reaction in the reactor, the reinforced back pH value of solution that finishes maintains about 8.0～10.0, and make solution continue standing demix behind the about 1h of reaction, remove the part supernatant liquid, rest part B suction filtration, it is dry to put into baking oven then, 100 ℃ of control drying temperatures, time is 3h, can obtain Mn-Zn ferrite precursor powder sample behind dry the end;
Wherein ferrous sulfate, zinc sulfate, manganous sulfate, each raw material blended mol ratio of additive are ferrous sulfate: zinc sulfate: manganous sulfate: additive is 60-65:15-20:15-20:0.05～0.3;
After mixing, each raw material of ferrous sulfate, zinc sulfate, manganous sulfate, additive is mixed with the aqueous solution, the used water yield, and by the total amount of substance of ferrous sulfate, zinc sulfate and manganous sulfate: water is 0.3mol:0.25L;
The precipitation agent that is added is that concentration is the 1.5mol/L ammonium bicarbonate soln, and the amount of adding is by the total amount of substance of ferrous sulfate, zinc sulfate and manganous sulfate: the 1.5mol/L ammonium bicarbonate soln is 0.3mol:0.375L;
Wherein said additive is an indium nitrate;
(2), pre-burning
With the pre-burning 3 hours in 800 ℃ retort furnace of the Mn-Zn ferrite precursor powder sample of step (1) gained, be pressed into ring then;
(3), thermal treatment
The ring that step (2) is suppressed in atmosphere furnace, under 1250 ℃～1350 ℃ thermal treatment temps, carry out high temperature sintering 3.5h get final product a kind of Mn-Zn ferrite with high magnetic permeability.
The Mn-Zn ferrite with high magnetic permeability of above-mentioned preparation method's gained, when the doping of additive indium nitrate was 0.1%, initial permeability can reach 9349 under the 10kHz condition.
Beneficial effect of the present invention
A kind of preparation method of the present invention with Mn-Zn ferrite of high magnetic permeability, by changing content of additive in the preparation process, can make the magnetic permeability characteristic of Mn-Zn ferrite of gained regulate easily, particularly compare with other additive, the magnetic permeability of sample obviously improves when not mixing, for example, when the doping of additive indium nitrate is 0.1%, initial permeability can reach 9349 under 10 kHz conditions, limiting frequency is higher, more can satisfy the demand for development in fields such as automotive electronics, network service, space flight and aviation and satellite communications.Technology of the present invention is simple, and the sample particle diameter is evenly tiny, helps commercial applications.
Description of drawings
Fig. 1 is that the initial permeability of different doping gained samples of the indium nitrate among the embodiment 1 is with the variation relation of frequency.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail, but does not limit the present invention.
A kind of preparation method of Mn-Zn ferrite of high magnetic permeability comprises the steps:
(1) coprecipitation method prepares precursor
By ferrous sulfate is that 63.10mol%, zinc sulfate are that 18.39mol%, manganous sulfate are that 18.51mol% takes by weighing 5 parts of metal-salt raw materials respectively, wherein 1 part as the blank indium nitrate that promptly do not mix, other 4 parts mix 0.05%, 0.1%, 0.15% respectively, the 0.3%(mol ratio) indium nitrate, above-mentioned raw materials is added dissolved in distilled water respectively;
The NH for preparing 1.5mol/L simultaneously
4HCO
3Solution is as precipitation agent (CO wherein
3 2-Amount of substance be 1.8 times of metal ion total amount);
After pouring them into separating funnel respectively, adopt and add feed way to join that (40 ℃) carry out coprecipitation reaction in the reactor, the reinforced back pH value of solution that finishes maintains about 8.0～9.0, and makes solution continue reaction 1h to make its precipitation fully.Standing demix is removed the part supernatant liquid, rest part B suction filtration, the BaCl with 5%
2Whether solution check washes clean, and it is dry to put into baking oven then, can obtain Mn-Zn ferrite precursor powder sample behind dry the end.
(2) pre-burning
With precursor pre-burning 3 hours in 800 ℃ retort furnace respectively, be pressed into 21.38 millimeters of external diameters then, 11.80 millimeters of internal diameters, thickness are 5～10 millimeters ring.
(3) thermal treatment
With the originally not thermal treatment 3.5 hours under 1250～1350 ℃ of thermal treatment temps in atmosphere furnace of the ring that suppresses, obtain to contain the Mn-Zn ferrite sample of the different dopings of indium nitrate.
Magnetic property characterizes
Fig. 1 is that the initial permeability of different doping gained samples of the indium nitrate among the embodiment 1 is with the variation relation of frequency.As can be seen from Figure 1, the magnetic permeability of sample obviously improves after the doped indium, slowly reduces with the increase initial permeability of frequency, and when the indium nitrate doping was 0.1%, at frequency 10kHz, initial permeability can reach 9349.
Above said content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (4)
1. the preparation method with Mn-Zn ferrite of high magnetic permeability is characterized in that comprising the steps:
(1), the preparation of precursor
Ferrous sulfate, zinc sulfate, manganous sulfate and additive are hybridly prepared into the aqueous solution, then utilize ammonium bicarbonate soln as precipitation agent, adopt and add feed way to join reactor inner control temperature be to carry out coprecipitation reaction about 40 ℃, the reinforced back pH value of solution that finishes maintains about 8.0～10.0, and make solution continue standing demix behind the about 1h of reaction, remove the part supernatant liquid, the rest part suction filtration, it is dry to put into baking oven then, 100 ℃ of control drying temperatures, time is 3h, can obtain Mn-Zn ferrite precursor powder sample behind dry the end;
The precipitation agent that is added is an ammonium bicarbonate soln;
Described additive is an indium nitrate;
(2), pre-burning
With the pre-burning 3 hours in 800 ℃ retort furnace of the Mn-Zn ferrite precursor powder sample of step (1) gained, be pressed into ring then;
(3), thermal treatment
The ring that step (2) is suppressed in atmosphere furnace, under 1250～1350 ℃ of thermal treatment temps, carry out high temperature sintering 3.5h get final product a kind of Mn-Zn ferrite with high magnetic permeability.
2. a kind of preparation method as claimed in claim 1 with Mn-Zn ferrite of high magnetic permeability, it is characterized in that the ferrous sulfate described in the step (1), zinc sulfate, manganous sulfate, each raw material blended mol ratio of additive are ferrous sulfate: zinc sulfate: manganous sulfate: additive is 60～65:15～20:15～20:0.05～0.3;
After mixing, each raw material of ferrous sulfate, zinc sulfate, manganous sulfate, additive is mixed with the aqueous solution, the used water yield, and by the total amount of substance of ferrous sulfate, zinc sulfate and manganous sulfate: water is 0.3 mol:0.25L;
The precipitation agent that is added is that concentration is the 1.5mol/L ammonium bicarbonate soln, and the amount of adding is by the total amount of substance of ferrous sulfate, zinc sulfate and manganous sulfate: the 1.5mol/L ammonium bicarbonate soln is 0.3 mol:0.375L.
3. a kind of preparation method with Mn-Zn ferrite of high magnetic permeability as claimed in claim 1 is characterized in that in the step (1):
Described ferrous sulfate, zinc sulfate, manganous sulfate, each raw material blended mol ratio of additive are ferrous sulfate: zinc sulfate: manganous sulfate: additive is preferably 63.10:18.39:18.51:0.1;
The described reinforced back pH value of solution that finishes preferably maintains about 8.0～9.0.
4. a kind of Mn-Zn ferrite with high magnetic permeability of preparation method's gained as claimed in claim 3, initial permeability can reach 9349 under the 10kHz condition.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174934A (en) * | 2015-08-31 | 2015-12-23 | 天长市中德电子有限公司 | Preparation method for soft magnetic ferrite with high saturation magnetic induction strength, wide temperature range and low loss |
| CN105174933A (en) * | 2015-08-31 | 2015-12-23 | 天长市中德电子有限公司 | Preparation method for soft magnetic ferrite with high saturation magnetic induction strength and high magnetic permeability |
| CN106098287A (en) * | 2016-05-30 | 2016-11-09 | 南通万宝实业有限公司 | A kind of preparation method of direct current generator Ferrite Material |
| CN110776314A (en) * | 2019-12-23 | 2020-02-11 | 贵州正业龙腾新材料开发有限公司 | Wide-high-frequency anti-EMI manganese-zinc ferrite material and preparation method thereof |
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2010
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| CN1709828A (en) * | 2005-05-30 | 2005-12-21 | 上海电力学院 | Method for preparing manganese-zinc ferrite by using waste dry batteries |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174934A (en) * | 2015-08-31 | 2015-12-23 | 天长市中德电子有限公司 | Preparation method for soft magnetic ferrite with high saturation magnetic induction strength, wide temperature range and low loss |
| CN105174933A (en) * | 2015-08-31 | 2015-12-23 | 天长市中德电子有限公司 | Preparation method for soft magnetic ferrite with high saturation magnetic induction strength and high magnetic permeability |
| CN106098287A (en) * | 2016-05-30 | 2016-11-09 | 南通万宝实业有限公司 | A kind of preparation method of direct current generator Ferrite Material |
| CN110776314A (en) * | 2019-12-23 | 2020-02-11 | 贵州正业龙腾新材料开发有限公司 | Wide-high-frequency anti-EMI manganese-zinc ferrite material and preparation method thereof |
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Application publication date: 20101222 |