CN102992751B - Preparation method of MnZn (Manganese-Zinc) soft magnetic ferrite material containing modified tree ash - Google Patents
Preparation method of MnZn (Manganese-Zinc) soft magnetic ferrite material containing modified tree ash Download PDFInfo
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- CN102992751B CN102992751B CN201210483111.3A CN201210483111A CN102992751B CN 102992751 B CN102992751 B CN 102992751B CN 201210483111 A CN201210483111 A CN 201210483111A CN 102992751 B CN102992751 B CN 102992751B
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Abstract
The invention discloses a preparation method of a MnZn (Manganese-Zinc) soft magnetic ferrite material containing modified tree ash. The preparation method comprises the following steps of: preparing main materials, preparing auxiliary materials, pre-burning, mixing and secondarily ball-milling the main materials and the auxiliary materials, shaping and sintering to obtain a MnZn soft magnetic ferrite magnetic core of modified tree ash. Through the addition of the modified tree ash, the MnZn soft magnetic ferrite material can play a bridge combination role among different raw materials; the used raw materials have the advantages of better distribution, high density, high grain boundary resistivity, low porosity and great and even grains; the prescription of the raw materials is reasonably improved, so that the magnetic core has higher magnetic conductivity after firing; and the indexes such as power loss, frequency feature, curie temperature, saturation flux density and the like are greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material that contains modification trees ashes.
Background technology
High magnetic conductivity ferrite magnetic, magnetic core is to realize program control communication, digital technique, in the electronicss such as network communication colour TV, be used as inducer, wave filter, the products such as pulse transformer make its miniaturization, the requisite electronic material of lightweight, improve constantly the initial permeability in magneticsubstance, it is the pursuit of being engaged in these professional engineering technical personnel and production firm always, the history of traditional existing four more than ten years of conventional ceramic technique development high-permeability material for China, up to the present, with conventional ceramic technique produce high-permeability material can only reach 10000 left and right, and the performance index of material, as loss, frequency response characteristic, Curie temperature etc. are all unsatisfactory.
Summary of the invention
In order to alleviate shortcomings and deficiencies of the prior art, the object of the present invention is to provide a kind of preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material that contains modification trees ashes.
The present invention adopts following technical scheme to achieve these goals:
The preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material that contains modification trees ashes, comprises the following steps:
(1) join major ingredient: be Fe in molar ratio
2o
351-53mol, MnO 33-35mol, ZnO 12-15mol, iron powder 0.1-0.2mol and Co2O30.1-0.2mol prepare burden;
(2) join auxiliary material: be equivalent to the modification trees ashes of major ingredient 0.02-0.03wt%, the MoO of 0.005-0.01wt%
3, 0.03-0.04wt% V
2o
5, 0.02-0.03wt% Bi
2o
3zrO with 0.025-0.035wt%
2; Described modification trees ashes are prepared by the following method:
A, trees ashes are soaked after 2-3 hour with the sodium hydroxide solution of 8-12%;
B, use 8-12% hydrochloric acid soln soak 2-3 hour;
C, with deionized water wash repeatedly, be neutral to trees ashes, dry;
D, be ground to 0.8-1.0 μ m powder, obtain modification trees ashes;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 3-4 hour a time with dispersion agent, then spraying is dry, carries out pre-burning, and calcined temperature is 880-920 DEG C, and the pre-burning time is 2-2.5 hour;
(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added to the auxiliary material of removing outside modification trees ashes, add water and dispersion agent to carry out secondary ball milling 2-3 hour, spraying is dried, built in 180-220 order pellet;
(5) moulding: secondary ball abrasive material is mixed with modification trees ashes, 10000-12000 rev/min, high speed dispersion 2-4 hour, is then pressed into base;
(6) sintering: put the moulded blank after above-mentioned moulding into sintering oven, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, be first warming up to 750-770 DEG C with 180-220 DEG C/h of speed, insulation 1-2 hour; In the nitrogen atmosphere of 0. 5%-1% oxygen volume content, while being warming up to 880-950 DEG C with 150-170 DEG C/h of speed, insulation 0.5-1 hour; In the nitrogen atmosphere of 3%-5% oxygen volume content, then be warming up to 1300-1350 DEG C with 90-110 DEG C/h of speed, the sintered heat insulating time is 3-4 hour; After sintering, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, after cooling, obtain the MnZn magnetic ferrite magnetic core of modification trees ashes.
Beneficial effect of the present invention:
1, the present invention is by adding modification trees ashes composition, can be used as the bridge keying action between different material, use feed distribution is better, density is high, grain boundary resistance rate is high, void content is low, crystal grain is large and even, rational modification composition of raw materials, after magnetic core is fired, there is higher magnetic permeability;
2, there is higher DC superposition characteristic, solve the loose problem of magnetic core surface tissue, thereby the raising of product physical strength, magnetic permeability rising, loss are reduced;
3, the index such as power loss, frequency response characteristic, Curie temperature, saturation magnetic flux density all has greatly improved.
Embodiment
Embodiment 1: the preparation method of the manganese zinc (Mn-Zn) soft magnetic ferrite material that contains modification trees ashes, comprises the following steps:
(1) join major ingredient: be Fe in molar ratio
2o
352mol, MnO 34.2mol, ZnO 13.5mol, iron powder 0.15mol and Co2O3 0.15mol prepare burden;
(2) join auxiliary material: be equivalent to the modification trees ashes of major ingredient 0.025wt%, the MoO of 0.008wt%
3, 0.035wt% V
2o
5, 0.025wt% Bi
2o
3zrO with 0.03wt%
2; Described modification trees ashes are prepared by the following method:
A, trees ashes are soaked after 2-3 hour with 10% sodium hydroxide solution;
B, with 10% hydrochloric acid soln soak 2-3 hour;
C, with deionized water wash repeatedly, be neutral to trees ashes, dry;
D, be ground to 0.9 μ m powder, obtain modification trees ashes;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 3-4 hour a time with dispersion agent, then spraying is dry, carries out pre-burning, and calcined temperature is 900 DEG C, and the pre-burning time is 2.3 hours;
(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added to the auxiliary material of removing outside modification trees ashes, add water and dispersion agent to carry out secondary ball milling 2-3 hour, spraying is dried, built in 180-220 order pellet;
(5) moulding: secondary ball abrasive material is mixed with modification trees ashes, 10000-12000 rev/min, high speed dispersion 2-4 hour, is then pressed into base;
(6) sintering: put the moulded blank after above-mentioned moulding into sintering oven, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, be first warming up to 760 DEG C with 200 DEG C/h of speed, insulation 1-2 hour; In the nitrogen atmosphere of 0. 5%-1% oxygen volume content, while being warming up to 930 DEG C with 160 DEG C/h of speed, insulation 0.5-1 hour; In the nitrogen atmosphere of 3%-5% oxygen volume content, then be warming up to 1330 DEG C with 100 DEG C/h of speed, the sintered heat insulating time is 3-4 hour; After sintering, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, after cooling, obtain the MnZn magnetic ferrite magnetic core of modification trees ashes.
The performance data of the magnetic ferrite magnetic core making by above-described embodiment:
Claims (1)
1. a preparation method who contains the manganese zinc (Mn-Zn) soft magnetic ferrite material of modification trees ashes, is characterized in that comprising the following steps:
(1) join major ingredient: be Fe in molar ratio
2o
351-53mol, MnO 33-35mol, ZnO 12-15mol, iron powder 0.1-0.2mol and Co
2o
30.1-0.2mol prepares burden;
(2) join auxiliary material: be equivalent to the modification trees ashes of major ingredient 0.02-0.03wt%, the MoO of 0.005-0.01wt%
3, 0.03-0.04wt% V
2o
5, 0.02-0.03wt% Bi
2o
3zrO with 0.025-0.035wt%
2; Described modification trees ashes are prepared by the following method:
A, trees ashes are soaked after 2-3 hour with the sodium hydroxide solution of 8-12%;
B, use 8-12% hydrochloric acid soln soak 2-3 hour;
C, with deionized water wash repeatedly, be neutral to trees ashes, dry;
D, be ground to 0.8-1.0 μ m powder, obtain modification trees ashes;
(3) pre-burning: the major ingredient that step (1) is prepared adds water and carries out ball milling 3-4 hour a time with dispersion agent, then spraying is dry, carries out pre-burning, and calcined temperature is 880-920 DEG C, and the pre-burning time is 2-2.5 hour;
(4) major ingredient, auxiliary material mix and secondary ball milling: pre-burning major ingredient is added to the auxiliary material of removing outside modification trees ashes, add water and dispersion agent to carry out secondary ball milling 2-3 hour, spraying is dried, built in 180-220 order pellet;
(5) moulding: secondary ball abrasive material is mixed with modification trees ashes, 10000-12000 rev/min, high speed dispersion 2-4 hour, is then pressed into base;
(6) sintering: put the moulded blank after above-mentioned moulding into sintering oven, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, be first warming up to 750-770 DEG C with 180-220 DEG C/h of speed, insulation 1-2 hour; In the nitrogen atmosphere of 0. 5%-1% oxygen volume content, while being warming up to 880-950 DEG C with 150-170 DEG C/h of speed, insulation 0.5-1 hour; In the nitrogen atmosphere of 3%-5% oxygen volume content, then be warming up to 1300-1350 DEG C with 90-110 DEG C/h of speed, the sintered heat insulating time is 3-4 hour; After sintering, in the nitrogen atmosphere of 0.05%-0.1% oxygen volume content, after cooling, obtain the MnZn magnetic ferrite magnetic core of modification trees ashes.
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| CN105070449A (en) * | 2015-08-10 | 2015-11-18 | 天长市昭田磁电科技有限公司 | Low-temperature sintered iron-based magnetic core material |
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