CN112562958A - Preparation method of low-temperature sintered manganese-zinc soft magnetic ferrite material - Google Patents
Preparation method of low-temperature sintered manganese-zinc soft magnetic ferrite material Download PDFInfo
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- CN112562958A CN112562958A CN202011352058.4A CN202011352058A CN112562958A CN 112562958 A CN112562958 A CN 112562958A CN 202011352058 A CN202011352058 A CN 202011352058A CN 112562958 A CN112562958 A CN 112562958A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/342—Oxides
- H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
- H01F1/37—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles in a bonding agent
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0206—Manufacturing of magnetic cores by mechanical means
- H01F41/0246—Manufacturing of magnetic circuits by moulding or by pressing powder
Abstract
The invention discloses a preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material, which comprises the following steps: weighing the main materials according to the formula, mixing the main materials with water, performing primary ball milling, drying, and performing heat preservation and presintering to obtain a pre-sintered material; then weighing appropriate amount of CaCO3、CoO、SiO2、V2O5、Bi2O3An additive, which is mixed with the pre-sintering material, and then added with 2-phosphonic butane-1, 2, 4-tricarboxylic acid and water for secondary ball milling to obtain a mixture; and mixing the mixture with a polyvinyl alcohol binder, heating and preserving heat, then carrying out spray granulation and compression molding to obtain a blank, and sintering at a low temperature to obtain the manganese-zinc soft magnetic ferrite material. The invention can reduce the sintering temperature and the sintering process by optimizing the formula of the manganese-zinc soft magnetic ferrite and the low-temperature sintering processThe prepared manganese-zinc soft magnetic ferrite material has the advantages of high saturation magnetic induction intensity, low loss and excellent soft magnetic performance while the energy consumption is low.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite materials, in particular to a preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material.
Background
The soft magnetic ferrite material is a magnetic material with small coercive force and easy magnetization, and is used for manufacturing important electronic components such as transformers, filters, inductors and the like in electricians and electronic equipment. The Mn-Zn soft magnetic ferrite material is one of the most applied soft magnetic ferrite materials, has the characteristics of high initial permeability, low power loss and the like, is favorable for reducing energy loss, and is widely applied to the fields of communication, automobiles, illumination, household appliances and the like. At present, the sintering temperature of the manganese-zinc soft magnetic ferrite is usually 1300-. Moreover, with the continuous development of the technology, electronic components gradually tend to be miniaturized, and higher requirements are put forward on the performance of the manganese-zinc soft magnetic ferrite material. Therefore, the preparation of the manganese-zinc soft magnetic ferrite material with high saturation magnetic induction and low loss has important significance under the low-temperature sintering process.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material.
The invention provides a preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material, which comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 52.5-54.0 mol% Fe2O338.5-40.5 mol% MnO and the balance of ZnO;
s2, mixing the main material with water, and performing primary ball milling, drying, heat preservation and presintering to obtain a presintering material;
s3, weighing CaCO 0.05-0.08% of the mass of the pre-sintered material30.03-0.05% of CoO, 0.01-0.02% of SiO20.01-0.02% of V2O50.005-0.01% of Bi2O3Mixing the mixture with the pre-sintered material, adding 2-phosphonic butane-1, 2, 4-tricarboxylic acid and water, and performing secondary ball milling to obtain a mixture;
s4, mixing the mixture with a polyvinyl alcohol aqueous solution, performing heat preservation treatment at the temperature of 140 ℃ and 180 ℃, and then granulating and pressing to form a blank;
and S5, heating the blank to 1050-.
Preferably, the mass of the 2-phosphonobutane-1, 2, 4-tricarboxylic acid is 0.25-0.3% of the mass of the pre-sintering material.
Preferably, the mass of the polyvinyl alcohol is 0.7-0.75% of the mass of the pre-sintering material.
Preferably, in the step S5, the blank is first heated to 240 ℃ at a heating rate of 2-2.5 ℃/min, then heated to 480 ℃ at 440-.
Preferably, in the step S5, the time for the heat preservation sintering is 4-6 h.
Preferably, in the step S4, the time of the heat preservation process is 2-4 h.
Preferably, in the step S2, the temperature for the heat preservation and pre-sintering is 800-950 ℃, and the time is 1.5-3 h.
Preferably, the mass concentration of the polyvinyl alcohol aqueous solution is 8-10%.
The invention has the following beneficial effects:
according to the invention, the appropriate additive is added into the material, so that the sintering temperature can be reduced, and the manganese-zinc soft magnetic ferrite material is prepared under the low-temperature sintering process, but the reduction of the sintering temperature can also bring about the problems of insufficient grain growth, large pores, reduced sintering density and the like, so that the soft magnetic performance of the material is reduced, and the improvement of the saturation magnetic induction intensity of the material and the reduction of loss are not facilitated; according to the invention, a proper amount of 2-phosphonic butane-1, 2, 4-tricarboxylic acid is added as a dispersing agent in the ball milling process of the pre-sintering material and the additive, compared with the conventional dispersing agent, the 2-phosphonic butane-1, 2, 4-tricarboxylic acid can be more effectively adsorbed on the surface of the powder, and the repulsive force between the powder is increased, so that a better dispersing effect is achieved, the agglomeration degree of the pre-sintering material powder is reduced, the particle size is reduced, the solid phase reaction activity is enhanced, the porosity is reduced, the sintering density is improved, and the saturation magnetic induction intensity of the material and the loss are favorably improved; and after the polyvinyl alcohol binder is added, proper heating and heat preservation treatment is carried out, carboxyl in 2-phosphonic acid butane-1, 2, 4-tricarboxylic acid and hydroxyl in polyvinyl alcohol are subjected to proper esterification and crosslinking, so that the binding effect of the binder is improved, the using amount of the binder is reduced, the porosity is reduced, the sintering density is improved, the saturation magnetic induction intensity of the material is improved, and the loss is reduced. By optimizing the formula of the manganese-zinc soft magnetic ferrite and the low-temperature sintering process, the invention can reduce the sintering temperature and the energy consumption, and simultaneously ensure that the prepared manganese-zinc soft magnetic ferrite material has the advantages of high saturation magnetic induction intensity, low loss and excellent soft magnetic performance.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 52.5 mol% Fe2O338.5 mol% MnO and the balance of ZnO;
s2, mixing the main material with water, performing primary ball milling, drying, and pre-burning at 800 ℃ for 3 hours to obtain a pre-burnt material;
s3, weighing CaCO accounting for 0.05 percent of the mass of the pre-sintered material30.03% of CoO, 0.01% of SiO20.01% of V2O50.005% of Bi2O3After being mixed with the pre-sintering material, 2-phosphonic butane-1, 2, 4-tricarboxylic acid and water are added for secondary ball milling to obtain a mixture, wherein the mass of the 2-phosphonic butane-1, 2, 4-tricarboxylic acid is 0.25 percent of that of the pre-sintering material;
s4, mixing the mixture with a polyvinyl alcohol aqueous solution with the mass concentration of 8%, carrying out heat preservation treatment for 4 hours at 140 ℃, and then granulating, pressing and forming to obtain a blank, wherein the mass of the polyvinyl alcohol is 0.7% of that of the pre-sintered material;
and S5, heating the blank to 220 ℃ at a heating rate of 2 ℃/min, heating to 440 ℃ at a heating rate of 1 ℃/min, heating to 850 ℃ at a heating rate of 2.5 ℃/min, heating to 1050 ℃ at a heating rate of 1 ℃/min, and carrying out heat preservation sintering for 6h to obtain the manganese-zinc soft magnetic ferrite material.
Example 2
A preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 54.0 mol% Fe2O340.5 mol% MnO and the balance of ZnO;
s2, mixing the main material with water, performing primary ball milling, drying, and pre-burning at 950 ℃ for 1.5 hours to obtain a pre-burnt material;
s3, weighing CaCO accounting for 0.08 percent of the mass of the pre-sintered material30.05% of CoO, 0.02% of SiO20.02% of V2O50.01% of Bi2O3After being mixed with the pre-sintering material, 2-phosphonic butane-1, 2, 4-tricarboxylic acid and water are added for secondary ball milling to obtain a mixture, wherein the mass of the 2-phosphonic butane-1, 2, 4-tricarboxylic acid is 0.3 percent of that of the pre-sintering material;
s4, mixing the mixture with a polyvinyl alcohol aqueous solution with the mass concentration of 10%, carrying out heat preservation treatment for 2 hours at 180 ℃, and then granulating, pressing and forming to obtain a blank, wherein the mass of the polyvinyl alcohol is 0.75% of that of the pre-sintered material;
s5, heating the blank to 240 ℃ at a heating rate of 2.5 ℃/min, heating to 480 ℃ at a heating rate of 1.5 ℃/min, heating to 880 ℃ at a heating rate of 3 ℃/min, heating to 1150 ℃ at a heating rate of 1.5 ℃/min, and carrying out heat preservation and sintering for 4 hours to obtain the manganese-zinc soft magnetic ferrite material.
Example 3
A preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 53 mol% Fe2O339.5 mol% MnO, and the balance ZnO;
s2, mixing the main material with water, performing primary ball milling, drying, and pre-burning at 850 ℃ for 2 hours to obtain a pre-burnt material;
s3, weighing CaCO accounting for 0.06 percent of the mass of the pre-sintered material30.04% ofCoO, 0.015% SiO20.015% of V2O50.008% of Bi2O3After being mixed with the pre-sintering material, 2-phosphonic butane-1, 2, 4-tricarboxylic acid and water are added for secondary ball milling to obtain a mixture, wherein the mass of the 2-phosphonic butane-1, 2, 4-tricarboxylic acid is 0.28 percent of that of the pre-sintering material;
s4, mixing the mixture with a polyvinyl alcohol aqueous solution with the mass concentration of 9%, carrying out heat preservation treatment for 3 hours at 160 ℃, and then granulating, pressing and forming to obtain a blank, wherein the mass of the polyvinyl alcohol is 0.72% of that of the pre-sintered material;
s5, heating the blank to 235 ℃ at a heating rate of 2.5 ℃/min, heating to 460 ℃ at a heating rate of 1 ℃/min, heating to 860 ℃ at a heating rate of 2.5 ℃/min, heating to 1100 ℃ at a heating rate of 1 ℃/min, and carrying out heat preservation sintering for 5h to obtain the manganese-zinc soft magnetic ferrite material.
Comparative example 1
A preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material comprises the following steps:
s1, weighing the main materials according to the following molar percentage: 53 mol% Fe2O339.5 mol% MnO, and the balance ZnO;
s2, mixing the main material with water, performing primary ball milling, drying, and pre-burning at 850 ℃ for 2 hours to obtain a pre-burnt material;
s3, weighing CaCO accounting for 0.06 percent of the mass of the pre-sintered material30.04% of CoO, 0.015% of SiO20.015% of V2O50.008% of Bi2O3Mixing the ammonium citrate with the pre-sintering material, adding ammonium citrate and water, and performing secondary ball milling to obtain a mixture, wherein the mass of the ammonium citrate is 0.4% of that of the pre-sintering material;
s4, mixing the mixture with a polyvinyl alcohol aqueous solution with the mass concentration of 9%, granulating, and performing compression molding to obtain a blank, wherein the mass of the polyvinyl alcohol is 0.9% of that of the pre-sintered material;
s5, heating the blank to 200 ℃ at a heating rate of 2.5 ℃/min, heating to 400 ℃ at a heating rate of 1 ℃/min, heating to 860 ℃ at a heating rate of 2.5 ℃/min, heating to 1100 ℃ at a heating rate of 1 ℃/min, and carrying out heat preservation sintering for 5h to obtain the manganese-zinc soft magnetic ferrite material.
The performance of the manganese-zinc soft magnetic ferrite materials prepared in examples 1 to 3 and comparative example 1 was tested by using a magnetic measuring instrument, and the test sample was ring-shaped, and had an outer diameter of 30mm, an inner diameter of 15mm and a height of 5 mm. The test results are shown in table 1:
TABLE 1 ferrite Material Performance test results
| Test items | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Bs(mT) | 432 | 435 | 441 | 405 |
| tgδ/μi(×10-6) | 1.45 | 1.48 | 1.39 | 1.77 |
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. A preparation method of a low-temperature sintered manganese-zinc soft magnetic ferrite material is characterized by comprising the following steps:
s1, weighing the main materials according to the following molar percentage: 52.5-54.0 mol% Fe2O338.5-40.5 mol% MnO and the balance of ZnO;
s2, mixing the main material with water, and performing primary ball milling, drying, heat preservation and presintering to obtain a presintering material;
s3, weighing CaCO 0.05-0.08% of the mass of the pre-sintered material30.03-0.05% of CoO, 0.01-0.02% of SiO20.01-0.02% of V2O50.005-0.01% of Bi2O3Mixing the mixture with the pre-sintered material, adding 2-phosphonic butane-1, 2, 4-tricarboxylic acid and water, and performing secondary ball milling to obtain a mixture;
s4, mixing the mixture with a polyvinyl alcohol aqueous solution, performing heat preservation treatment at the temperature of 140 ℃ and 180 ℃, and then granulating and pressing to form a blank;
and S5, heating the blank to 1050-.
2. The method of preparing a low temperature sintered manganese-zinc soft magnetic ferrite material according to claim 1, wherein the mass of 2-phosphonobutane-1, 2, 4-tricarboxylic acid is 0.25-0.3% of the mass of the pre-sintering material.
3. The method for preparing a low-temperature sintered manganese-zinc soft magnetic ferrite material according to claim 1 or 2, wherein the mass of the polyvinyl alcohol is 0.7-0.75% of the mass of the pre-sintering material.
4. The method for preparing a low-temperature sintered manganese-zinc soft magnetic ferrite material according to any one of claims 1 to 3, wherein in the step S5, the blank is heated to 240 ℃ at a heating rate of 2 to 2.5 ℃/min, then heated to 480 ℃ at 440-.
5. The method for preparing a low-temperature sintered manganese-zinc soft magnetic ferrite material according to any one of claims 1 to 4, wherein the time for the heat-preservation sintering in step S5 is 4 to 6 hours.
6. The method for preparing a low temperature sintered manganese-zinc soft magnetic ferrite material according to any one of claims 1 to 5, wherein the time of the heat preservation treatment in step S4 is 2 to 4 hours.
7. The method for preparing a low-temperature sintered manganese-zinc soft magnetic ferrite material according to any one of claims 1 to 6, wherein in the step S2, the temperature for the heat preservation and pre-sintering is 800-950 ℃ for 1.5-3 h.
8. The method for preparing a low-temperature sintered manganese-zinc soft magnetic ferrite material according to any one of claims 1 to 7, wherein the mass concentration of the polyvinyl alcohol aqueous solution is 8 to 10%.
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Cited By (1)
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| CN115368125A (en) * | 2022-06-18 | 2022-11-22 | 信丰天科磁业有限公司 | Manganese-zinc soft magnetic ferrite material with high breaking strength and manufacturing method thereof |
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