CN109559865B - Preparation method of novel amorphous magnetic core binder - Google Patents
Preparation method of novel amorphous magnetic core binder Download PDFInfo
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- 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
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Abstract
The invention provides a newA preparation method of a type amorphous magnetic core binder relates to the technical field related to the preparation of bonded magnetic cores, and is based on MnZnFe2O4Molecular formula, preparation of FeSO4、MnSO4And ZnSO4Mixing the solution, adding n-hexanol and cetyl ammonium bromide as surfactant to obtain water-in-oil reverse emulsion, precipitating with NaOH solution, and adding H2O2Preparing manganese zinc ferrite powder as an oxidant, washing the manganese zinc ferrite powder with water, decompressing, desolventizing to obtain a methyl phenyl silicone resin base material, adding the graded manganese zinc ferrite powder and a coupling agent KH-550, mixing, stirring and grinding for 4 hours to obtain a finished product. The filler in the adhesive is replaced by the manganese-zinc ferrite powder from the silicon dioxide particles, so that the magnetic property of the magnetic core is improved, the coercive force of the magnetic core is reduced, the magnetic property of the magnetic core is improved, and the preparation process of the powder core is not influenced, so that the preparation method has the advantages of simple operation and cost reduction.
Description
Technical Field
The invention relates to the technical field related to preparation of bonded magnetic cores, in particular to a preparation method of a novel amorphous magnetic core binder.
Background
The amorphous alloy material shows a series of excellent soft magnetic properties due to the absence of crystal grains and grain boundaries, such as: easy magnetization, low coercive force, high magnetic permeability and large saturation magnetization, but the resistivity is lower, so the eddy current loss is larger. The amorphous magnetic core effectively increases the resistivity of the material and reduces the eddy current loss by adding the binder, but because the filler in the binder does not have magnetism, the resistivity is only singly improved, but the further improvement of the soft magnetic performance of the magnetic core is hindered.
Patent CN104067358A discloses a powder magnetic core, a coil component, and a method for manufacturing a powder magnetic core, which can reduce the core loss by dispersing copper powder particles in an alloy powder. However, the method is difficult to uniformly disperse the copper powder in the alloy powder, and the micron-sized copper powder is easy to oxidize, has high operation difficulty and high use cost.
Disclosure of Invention
The invention aims to provide a preparation method of a novel amorphous magnetic core binder, so as to solve the technical problems.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of a novel amorphous magnetic core binder comprises the following steps:
s1 preparing a binder filler: in FeSO4，MnSO4And ZnSO4Adding n-hexanol and cetyl ammonium bromide as surfactant to obtain water-in-oil reverse first emulsion and water-in-oil reverse second emulsionMixing the two emulsions to make the internal molecules of the two emulsions implement collision combination, then using NaOH solution as precipitant and H2O2As an oxidant, preparing manganese zinc ferrite powder;
s2: manganese-zinc ferrite powder is ground to 2um to 4um by airflow;
s3: grading manganese zinc ferrite powder;
s4 preparation of binder base: sequentially adding quantitative acetone, methyl trichlorosilane and dimethyl dichlorosilane, then dropwise adding an acetone water solution, filtering and separating to obtain a hydrolysate, then adding a certain amount of condensation catalyst, and then washing the condensation catalyst with water to remove a solvent under reduced pressure to finally obtain a methyl phenyl silicone resin base material;
s5: preparing methyl phenyl silicone resin into a solution with the mass fraction of 50% by using dimethylbenzene, and stirring and dispersing for 1 h;
s6: firstly, adding 10-15% of graded powder in mass fraction into the dispersed solution, then adding 1% of coupling agent KH-550 in mass fraction, mixing, stirring and grinding for 4h to obtain the finished product.
Preferably, when the NaOH solution is used as the precipitant in step S1, the temperature is controlled at 200-220E, the pH value of the medium is 7-12, and the precipitation time is 2 h.
Preferably, in step S2, the manganese-zinc-ferrite powder is pulverized by an air flow mill, and the particle size of the powder is 2um to 4 um.
Preferably, in step S3, the grading is such that 2um manganese zinc ferrite accounts for about 30% of the total weight of the powder, 3um manganese zinc ferrite accounts for about 50% of the total weight of the powder, and 4um manganese zinc ferrite accounts for about 20% of the total weight of the powder.
Preferably, in step S4, the hydrolysate is obtained with a stirring rate of 400prm, a hydrolysis time of 2.5h and a hydrolysis temperature of 15 ℃.
Preferably, in step S4, the dropping rate of the aqueous acetone solution is 25ml/h, the temperature after the dropping of the aqueous acetone solution is 45 ℃, and the reaction time is 20 h.
Preferably, in step S6, the filler of the binder is manganese zinc ferrite.
The invention has the beneficial effects that:
compared with the existing amorphous powder core preparation process, the invention has the advantages of simple operation and cost reduction because the filler in the binder is replaced by the manganese-zinc ferrite powder from the silicon dioxide particles, on one hand, the hardness of the manganese-zinc ferrite is far less than that of the silicon dioxide, so that the compaction density of the magnetic core is larger, the internal stress of the amorphous magnetic powder is smaller, the magnetic performance of the magnetic core is improved, and on the other hand, the magnetic performance of the magnetic core is also improved because the total magnetic substance is increased, and in addition, the invention only changes the composition of the binder and does not influence the powder core preparation process.
Detailed Description
The present invention will be further described with reference to specific embodiments for the purpose of facilitating an understanding of technical means, characteristics of creation, objectives and functions realized by the present invention, but the following embodiments are only preferred embodiments of the present invention, and are not intended to be exhaustive. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention. The experimental methods in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example one
According to MnZnFe2O4Molecular formula, preparation of FeSO4、MnSO4And ZnSO4Mixing the solution, adding n-hexanol and cetyl ammonium bromide as surfactant to obtain water-in-oil reverse emulsion, precipitating with NaOH solution, and adding H2O2Preparing manganese-zinc ferrite powder as an oxidant, grinding the manganese-zinc ferrite powder to 2-4 um by air flow, grading, wherein 30% of 2um powder, 50% of 3um powder and 20% of 4um powder are prepared into a mixed solution of acetone, methyltrichlorosilane and dimethyldichlorosilane, then dropwise adding an acetone aqueous solution, filtering and separating to obtain waterAdding a certain amount of condensation catalyst into the hydrolysate, washing the hydrolysate with water, reducing pressure and removing solvent to obtain a methyl phenyl silicone resin base material, preparing the methyl phenyl silicone resin into a solution with the mass fraction of 50% by using dimethylbenzene, stirring and dispersing for 1h, adding graded manganese zinc ferrite powder with the mass fraction of 12% into the dispersed solution, then adding a coupling agent KH-550 with the mass fraction of 1%, mixing, stirring and grinding for 4h to obtain a finished product.
Example two
According to MnZnFe2O4Molecular formula, preparation of FeSO4、MnSO4And ZnSO4Mixing the solution, adding n-hexanol and cetyl ammonium bromide as surfactant to obtain water-in-oil reverse emulsion, precipitating with NaOH solution, and adding H2O2Preparing manganese-zinc ferrite powder as an oxidant, grinding the manganese-zinc ferrite powder to 2-4 um by air flow, grading, wherein 30% of 2um powder, 50% of 3um powder and 20% of 4um powder are prepared into a mixed solution of acetone, methyltrichlorosilane and dimethyldichlorosilane, then dropwise adding an acetone aqueous solution, filtering and separating to obtain a hydrolysate, then adding a certain amount of a condensation catalyst, washing, decompressing and desolventizing the condensation catalyst to obtain a methylphenyl silicon resin base material, preparing the methylphenyl silicon resin into a solution with the mass fraction of 50% by using xylene, stirring and dispersing for 1h, adding the graded manganese-zinc ferrite powder with the mass fraction of 10% into the dispersed solution, then adding a coupling agent KH-550 with the mass fraction of 1%, mixing, stirring and grinding for 4h to obtain a finished product.
EXAMPLE III
According to MnZnFe2O4Molecular formula, preparation of FeSO4、MnSO4And ZnSO4Mixing the solution, adding n-hexanol and cetyl ammonium bromide as surfactant to obtain water-in-oil reverse emulsion, precipitating with NaOH solution, and adding H2O2Preparing manganese zinc ferrite powder as oxidant, grinding the manganese zinc ferrite powder to 2-4 um by air flow, and grading, wherein the powder of 2um is 30%, and the powder of 3um is 5%20% of powder of 0% and 4um, preparing a mixed solution of acetone, methyltrichlorosilane and dimethyldichlorosilane, then dropwise adding an acetone water solution, filtering and separating to obtain a hydrolysate, then adding a certain amount of a condensation catalyst, then washing, decompressing and desolventizing the condensation catalyst to obtain a methyl phenyl silicone base material, preparing the methyl phenyl silicone into a solution with the mass fraction of 50% by using xylene, stirring and dispersing for 1h, adding graded manganese zinc ferrite powder with the mass fraction of 15% into the dispersed solution, then adding a coupling agent KH-550 with the mass fraction of 1%, mixing, stirring and grinding for 4h to obtain a finished product.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and are not intended to limit the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. A preparation method of an amorphous magnetic core binder is characterized by comprising the following steps: the method comprises the following steps:
s1 preparing a binder filler: in FeSO4，MnSO4And ZnSO4Adding n-hexanol and cetyl ammonium bromide as surfactant into the mixed solution to obtain water-in-oil reverse first emulsion and water-in-oil reverse second emulsion, mixing the two emulsions, allowing the molecules in the two emulsions to collide, and precipitating with NaOH solution and H2O2As an oxidant, preparing manganese zinc ferrite powder;
s2: manganese-zinc ferrite powder is ground to 2um to 4um by airflow;
s3: grading manganese zinc ferrite powder;
s4 preparation of binder base: sequentially adding quantitative acetone, methyl trichlorosilane and dimethyl dichlorosilane, then dropwise adding an acetone water solution, filtering and separating to obtain a hydrolysate, then adding a certain amount of condensation catalyst, and then washing the condensation catalyst with water to remove a solvent under reduced pressure to finally obtain a methyl phenyl silicone resin base material;
s5: preparing methyl phenyl silicone resin into a solution with the mass fraction of 50% by using dimethylbenzene, and stirring and dispersing for 1 h;
s6: firstly, adding 10-15% of graded powder in mass fraction into the dispersed solution, then adding 1% of coupling agent KH-550 in mass fraction, mixing, stirring and grinding for 4h to obtain a finished product;
in the step S1, when the NaOH solution is used as the precipitant, the temperature is controlled at 200-220 ℃, the pH value of the medium is 7-12, and the precipitation time is 2 h;
in the step S2, the manganese-zinc ferrite powder is crushed by an air flow mill, and the particle size of the powder is 2-4 um;
in the step S3, the grading is that the manganese zinc ferrite with a particle size of 2um accounts for 30% of the total mass of the powder, the manganese zinc ferrite with a particle size of 3um accounts for 50% of the total mass of the powder, and the manganese zinc ferrite with a particle size of 4um accounts for 20% of the total mass of the powder;
in the step S4, the stirring speed of the obtained hydrolysate is 400prm, the hydrolysis time is 2.5h, and the hydrolysis temperature is 15 ℃;
in the step S4, the dropping rate of the acetone aqueous solution is 25ml/h, the temperature after the acetone aqueous solution is dropped is 45 ℃, and the reaction time is 20 h;
in step S6, the filler of the binder is manganese zinc ferrite.
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| CN102956342A (en) * | 2011-08-25 | 2013-03-06 | 太阳诱电株式会社 | Electronic part and manufacturing method thereof |
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| CN103567436A (en) * | 2013-11-28 | 2014-02-12 | 四川东阁科技有限公司 | Manufacturing method of iron-silicon material and iron-silicon magnetic powder core having permeability mu of 55 |
| CN103608409A (en) * | 2011-05-16 | 2014-02-26 | 田中精密工业株式会社 | Magnetically enhanced resin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3283918B2 (en) * | 1992-02-28 | 2002-05-20 | 呉羽化学工業株式会社 | High magnetic permeability composition |
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| CN1329745A (en) * | 1998-12-07 | 2002-01-02 | 住友金属矿山株式会社 | Resin-bonded magnet |
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| CN101723655A (en) * | 2008-10-21 | 2010-06-09 | 兰州大学 | Preparation method of Mn-Zn ferrite cobalt-doped nano material |
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| CN102585696A (en) * | 2012-02-13 | 2012-07-18 | 江苏大学 | Methyl phenyl silicone resin base high-temperature-resistant coating and preparation method thereof |
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