CN1367499A - Preparation method of soft magnetic ferrimagnetics - Google Patents

Preparation method of soft magnetic ferrimagnetics Download PDF

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Publication number
CN1367499A
CN1367499A CN 02114822 CN02114822A CN1367499A CN 1367499 A CN1367499 A CN 1367499A CN 02114822 CN02114822 CN 02114822 CN 02114822 A CN02114822 A CN 02114822A CN 1367499 A CN1367499 A CN 1367499A
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soft magnetic
suspension system
preparation
percentage
monomer solution
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CN1152395C (en
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车晓舟
朱敏
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South China University of Technology SCUT
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South China University of Technology SCUT
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Abstract

The preparation method of magnetically soft ferrite magnet includes the following steps: in deionized water adding (wt%) 5-30% of mixture of ethylol methacrylate and tetraglycol diacrylate (according to the mixing weight ratio of 10-50:1), 0-20% of water-soluble macromolecular material, 3-20% of dispersing agent and 0.17-2% of initiating agent, mixing them and preparing them into monomer solution, adding the magnetically soft ferrite powder into monomer solution, mixing them to obtain suspension system, pouring the suspension system into foring mould, heating, heat-insulating, demoulding and drying so as to obtain the invented product. The described monomer aqueous solution is non-toxic, and the ammonium persulfate can be adopted as initiating agent.

Description

A kind of preparation method of soft magnetic ferrimagnetics
(1) technical field
The present invention relates to magnet forming processing technology field, specifically be meant a kind of preparation method of soft magnetic ferrimagnetics.
(2) background technology
Soft magnetic ferrite is the basic material that a kind of purposes is wide, output is big, cost is low, it is one of important pillar product of electronics, mechanotronics, it apply the development that directly has influence on electronic information, household electrical appliances industry, computer and communication, environmental protection and power-saving technology, also be one of sign of weighing a national economy development degree.The practicability of soft magnetic ferrite, so far half world, because it has high magnetic permeability, high resistivity, low-loss and Standpoint of Ceramic Wear-resisting Function, thereby be used widely in fields such as the electron beam deflection coils of television set, kickback transformer, broadcast receiver choke, middle all transformers, inductor, Switching Power Supply, communication apparatus, filter, computer, electric ballasts; Along with popularizing that electronic technology increasingly extensive application, particularly digital circuit and Switching Power Supply are used, the electromagnetic interference (EMI) problem becomes more and more important, and countries in the world are more and more higher to the standard of electronic instrument and the anti-electromagnetic interference performance proposition of measuring equipment.Therefore, EMI magnetic element development based on soft magnetic ferrite is rapid, product category is various, as electromagnetic interference eliminator, electric wave absorbing materials, frequency multiplier, modulator etc., has become modern military electronic equipment, industry and the indispensable part of civil electronic instrument.The forming method of soft magnetic ferrimagnetics mainly comprises mold pressing, extruding and injection moulding, its main technique be with ferromagnetic oxide powder with after a certain amount of binding agent mixes, make base substrate at forming under the pressure or by injection moulding.According to the serviceability requirement, base substrate directly uses as magnet or uses behind sintering.
Gel casting forming is a kind of ceramic powders precise forming new technology that U.S.'s Oak Ridge National Laboratory was invented for reduction forming process of ceramics processing cost in phase earlier 1990s.Because this technology is in the incomparable superiority of other forming process of ceramics technology that is had aspect the heavy in section of the nearly final size of preparation or the complex-shaped ceramic component, the nearly common concern that is subjected to home and abroad forming process of ceramics research institution and enterprise during the last ten years, the molding research that has been widely used in various ceramic powders, and progressively promote to field of industrialized production.The technical process for preparing ceramic component with the gel casting forming technology is summarized as follows: ceramic powders is scattered in the solution of organic monomer, form the suspended substance of high solid loading and Grapefruit Essential Oil, then in the injection moulding mould, form macromolecule " skeleton " by home position polymerization reaction, make powder be maintained fixed shape, form base substrate with higher-strength and certain density through dehydrating the back.The gel casting forming technology is used for the moulding of ferrimagnet, at first can reduce equipment investment, because gel casting forming does not need large-tonnage press and expensive injection-moulding device, and Mold Making is simple, cost is low, thereby will reduce production costs greatly.Secondly, utilize the intensity of the base substrate of gel-casting method preparation to be higher than the mold pressing blank far away, can carry out a series of machining, when using as bonded permanent magnet, its particle content is higher than the mold pressing magnet, and forming process finishes under static state, helps magnet is carried out magnetic field orientating, can obtain the desirable degree of orientation, thereby obtain better magnetic property.Compare with the injection moulding magnet, except that having magnetic property that particle content height, orientation bring easily significantly improves, when using as the sintered magnet base substrate, come unstuck much easier than injection moulding magnet base, and aspect preparation heavy in section, complex-shaped device characteristics, be that any prior art is all incomparable.At present, the home and abroad uses the most general water-soluble monomer to be mainly third rare acid amides and the N in gel injection molding and forming technology, N '-di-2-ethylhexylphosphine oxide third rare acid amides (crosslinking agent), and third rare acid amides toxicity wherein is big and have carcinogenic danger.Third rare acid amides toxicity becomes the bottleneck of this skilled industry application of restriction except that technological factor.
(3) summary of the invention
Purpose of the present invention is exactly in order to overcome the deficiencies in the prior art, and a kind of preparation method of soft magnetic ferrimagnetics is provided, and this method adopts nontoxic monomer solution system when utilizing the gel casting forming technology, overcome toxicity problem.
The preparation method of a kind of soft magnetic ferrimagnetics of the present invention, it is characterized in that, it comprises the steps and process conditions: the first step, with the two acrylic acid esters (TEGA) of methyl-prop diluted acid hydroxyl ethyl ester (HEMA) and tetraethylene-glycol according to weight ratio 10~50: 1 mixes; Second step, in deionized water, add the methyl-prop diluted acid hydroxyl ethyl ester (HEMA) and the mixture of the two acrylic acid esters (TEGA) of tetraethylene-glycol, the water-soluble high-molecular material of 0~20% percentage by weight, the dispersant of 3~20% percentage by weights, the initator of 0.17~2% percentage by weight of 5~30% percentage by weights, make monomer solution; The 3rd step added soft magnetic ferrite powder in the monomer solution, made suspension system; The 4th step was poured into suspension system in the mould, was heated to 60~70 ℃, was incubated 2~8 hours, the demoulding, drying.Wherein, initator can be Ammonium Persulfate 98.5.
Principle of the present invention is: as the methyl-prop diluted acid hydroxyl ethyl ester (HEMA) of key component with as the two acrylic acid esters (TEGA) of the tetraethylene-glycol of crosslinking agent, under the effect of initator and temperature, form the cross-linked polymer skeleton by polymerization reaction, with the ceramic powders fixed-site, and make it to have shape, the size identical with the mould die cavity.The main effect of adding water-soluble high-molecular material comprises: (1) reduces the oxygen inhibition effect; (2) improve the flowability of suspension; (3) form stable suspension system.Dispersant is mainly used in the surface characteristic of improving ceramic particle, alleviates agglomeration, improves solid contents.The adding of water-soluble high-molecular material mainly is for ceramic powders is suspended in solution, thereby forms the stable suspension system that is suitable for pouring into a mould.Polymerization time mainly changes according to the difference that adds initiator content.After the demoulding was finished in polymerization, the starting stage of dry run will suitably be controlled high and dry speed, prevents blank cracking, in order to improve rate of drying, raised the efficiency, and after insulation in 3 hours, temperature can be risen to 80~100 ℃.
The present invention compared with prior art has the following advantages and beneficial effect:
1. the present invention adopts gel casting process to prepare soft magnetic ferrimagnetics, and the magnet moulding process is simple, and the appointed condition requirement is low, investment is little, and mold materials can be selected metal, glass, pottery, plastics, wax, timber etc. for use, and Mould Machining is easy, cost is low.
2. the present invention utilizes gel casting process to prepare soft magnetic ferrimagnetics, and non magnetic phase content is low, and degree of orientation height can significantly improve magnet performance and device class.Add upper magnet blank strength height, presentation quality is good, dimensional accuracy is high.
3. the monomer solution of the present invention's use is nontoxic, and toxicity is the topmost unfavorable factor that restricts the gel-casting technology production application at present except that technological factor, and succeeding in developing for the extensive use of gel-casting technology of non-toxic formulation and corresponding shaping technology is significant.
4. the present invention adopts the Ammonium Persulfate 98.5 aqueous solution as initator, cause the polymerization reaction of methyl-prop diluted acid hydroxyl ethyl ester (HEMA) aqueous solution, has overcome the shortcoming that methyl-prop diluted acid hydroxyl ethyl ester can not be used for the water-soluable gel casting.
(4) embodiment
Embodiment one
The two acrylic acid esters (TEGA) of methyl-prop diluted acid hydroxyl ethyl ester (HEMA) and tetraethylene-glycol are mixed according to weight ratio at 10: 1; Adding percentage by weight in deionized water is this mixture of 5%, 3% dispersant Duramax TMD-3005,0.17% Ammonium Persulfate 98.5 fully mix, and make monomer solution; Soft magnetic ferrite powder is added in the monomer solution, fully mix, make stable suspension system; Suspension system is poured in the mould, is heated to 70 ℃, be incubated 3 hours, temperature is risen to 100 ℃ subsequently, be incubated 5 hours, the demoulding, drying.As mentioned above, can realize the present invention preferably.
Embodiment two
The two acrylic acid esters (TEGA) of methyl-prop diluted acid hydroxyl ethyl ester (HEMA) and tetraethylene-glycol are mixed according to weight ratio at 20: 1; Adding percentage by weight in deionized water is this mixture of 10%, 5% dispersant Duramax TMD-3007,5% water-soluble high-molecular material PEO, 0.33% Ammonium Persulfate 98.5 fully mix, and make monomer solution; Soft magnetic ferrite powder is added in the monomer solution, fully mix, make stable suspension system; Suspension system is poured in the mould, is heated to 65 ℃, be incubated 6.5 hours, the demoulding, drying.As mentioned above, can realize the present invention preferably.
Embodiment three
The two acrylic acid esters (TEGA) of methyl-prop diluted acid hydroxyl ethyl ester (HEMA) and tetraethylene-glycol are mixed according to weight ratio at 30: 1; Adding percentage by weight in deionized water is this mixture of 20%, 10% dispersant Duramax TMD-3005,10% water-soluble high-molecular material PVP, 0.67% Ammonium Persulfate 98.5 fully mix, and make monomer solution; Soft magnetic ferrite powder is added in the monomer solution, fully mix, make stable suspension system; Suspension system is poured in the mould, is heated to 60 ℃, be incubated 3 hours, temperature is risen to 80 ℃ subsequently, be incubated 0.5 hour, the demoulding, drying.As mentioned above, can realize the present invention preferably.
Embodiment four
The two acrylic acid esters (TEGA) of methyl-prop diluted acid hydroxyl ethyl ester (HEMA) and tetraethylene-glycol are mixed according to weight ratio at 40: 1; Adding percentage by weight in deionized water is this mixture of 25%, 16% dispersant Duramax TMD-3007,15% water-soluble high-molecular material PVP, 1.33% Ammonium Persulfate 98.5 fully mix, and make monomer solution; Soft magnetic ferrite powder is added in the monomer solution, fully mix, make stable suspension system; Suspension system is poured in the mould, is heated to 60 ℃, be incubated 3 hours, the demoulding, drying.As mentioned above, can realize the present invention preferably.
Embodiment five
The two acrylic acid esters (TEGA) of methyl-prop diluted acid hydroxyl ethyl ester (HEMA) and tetraethylene-glycol are mixed according to weight ratio at 50: 1; Adding percentage by weight in deionized water is this mixture of 30%, 20% dispersant Duramax TMD-3005,20% water-soluble high-molecular material PVP, 2% Ammonium Persulfate 98.5 fully mix, and make monomer solution; Soft magnetic ferrite powder is added in the monomer solution, fully mix, make stable suspension system; Suspension system is poured in the mould, is heated to 60 ℃, be incubated 2 hours, the demoulding, drying.As mentioned above, can realize the present invention preferably.

Claims (3)

1. the preparation method of a soft magnetic ferrimagnetics is characterized in that, it comprises the steps and process conditions: the first step, with the two acrylic acid esters of methyl-prop diluted acid hydroxyl ethyl ester and tetraethylene-glycol according to weight ratio 10~50: 1 mixes; Second step, in deionized water, add the mixture that the first step of 5~30% percentage by weights makes, the water-soluble high-molecular material of 0~20% percentage by weight, the dispersant of 3~20% percentage by weights, the initator of 0.17~2% percentage by weight, make monomer solution; The 3rd step added soft magnetic ferrite powder in the monomer solution, made suspension system; The 4th step was poured into suspension system in the mould, was heated to 60~70 ℃, was incubated 2~8 hours, the demoulding, drying.
2. the preparation method of a kind of soft magnetic ferrimagnetics according to claim 1 is characterized in that, initator can be Ammonium Persulfate 98.5.
3. the preparation method of a kind of soft magnetic ferrimagnetics according to claim 1, it is characterized in that, in the 4th step, suspension system is poured in the mould, is heated to 60~70 ℃, be incubated 2~8 hours, wherein after insulation 3 hours, temperature can be risen to 80~100 ℃ and continue insulation, the demoulding then, drying.
CNB021148228A 2002-02-06 2002-02-06 Preparation method of soft magnetic ferrimagnetics Expired - Fee Related CN1152395C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100567206C (en) * 2006-11-30 2009-12-09 横店集团东磁股份有限公司 Mixing method of particle material for soft magnetic ferrite molding
CN1764991B (en) * 2004-03-31 2010-05-05 Tdk株式会社 Magnetic field generating apparatus, method for manufacturing ferrite magnet, and mold
CN104356561A (en) * 2014-11-12 2015-02-18 铜陵天海流体控制有限公司 Preparation method of liner rubber material for soft seal gate valve plates
CN107512905A (en) * 2017-09-27 2017-12-26 佛山金志通电子科技有限公司 A kind of soft magnetic manganese-zinc ferrite magnetic core blank aqueous slurries note solidification forming method

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100347126C (en) * 2005-05-11 2007-11-07 华南理工大学 Magnetic brick with electromagnetic shielding and decoration functions and its preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1764991B (en) * 2004-03-31 2010-05-05 Tdk株式会社 Magnetic field generating apparatus, method for manufacturing ferrite magnet, and mold
CN100567206C (en) * 2006-11-30 2009-12-09 横店集团东磁股份有限公司 Mixing method of particle material for soft magnetic ferrite molding
CN104356561A (en) * 2014-11-12 2015-02-18 铜陵天海流体控制有限公司 Preparation method of liner rubber material for soft seal gate valve plates
CN107512905A (en) * 2017-09-27 2017-12-26 佛山金志通电子科技有限公司 A kind of soft magnetic manganese-zinc ferrite magnetic core blank aqueous slurries note solidification forming method

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