CN106365626A - Manufacturing method of dry-press anisotropic ferrite - Google Patents

Manufacturing method of dry-press anisotropic ferrite Download PDF

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Publication number
CN106365626A
CN106365626A CN201610791751.9A CN201610791751A CN106365626A CN 106365626 A CN106365626 A CN 106365626A CN 201610791751 A CN201610791751 A CN 201610791751A CN 106365626 A CN106365626 A CN 106365626A
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dry
press
powder
pressing
opposite sex
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CN106365626B (en
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叶华
丁伯明
胡良权
姚淦
韦晓阳
吕舒宏
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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    • 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
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Abstract

The invention discloses a manufacturing method of dry-press anisotropic ferrite. The method comprises the following steps: carrying out two-stage wet milling on a permanent magnetic ferrite presintered material; putting the slurry obtained by two-stage wet milling into a drying box, and drying; screening the dried material blocks to prepare magnetic powder, adding an adhesive, mixing in a dry-type stirrer, pulverizing by a high-speed pulverizer, and screening to obtain the dry-press anisotropic ferrite powder; pressing the dry-press anisotropic ferrite on an experimental press to obtain a steel magnet, and applying an impulse-type heavy current onto a coil to generate an instantaneous high-impulse magnetic field; and carrying out degumming treatment, and sintering. The powdery camphor can be directly sufficiently mixed with the magnetic powder; the impulse-type heavy current enhances the degree of orientation of the dry-press anisotropic ferrite magnetic powder; the additive is beneficial to enhancing the coercive force of the product; and the dispersing agent enhances the particle size uniformity of the ground magnet powder, and enhances the properties of the dry-press product.

Description

A kind of different in nature ferritic manufacture method of dry-pressing
Technical field
The present invention relates to magnetic material correlative technology field, refer in particular to a kind of ferritic manufacture method of dry-pressing opposite sex.
Background technology
Traditional permanent-magnet ferrite manufacture method has dry-pressing formed and two kinds of Wet-pressing molding.Wherein Wet-pressing molding has orientation Spend, the high feature of magnetic property such as remanent magnetism, applied on a large scale at present.But, dry-pressing formed also have the application of oneself to lead Domain, it has the features such as shaping efficiency height, applied range, product design variation, can apply to many miniaturizations and shape The irregular product of shape.
In the manufacture method of existing dry-pressing opposite sex ferromagnetic oxide powder, most critical be exactly magnetic powder manufacturing process and dry-pressing Moulding process.In the manufacturing process of magnetic powder, main additive has Camphora and calcium stearate, and the addition manner of wherein Camphora has Two kinds, one kind is dissolved in ethanol and adds, and this can cause the local of powder body to reunite；Another is direct interpolation, due to common Camphora easily lumps, and is also unfavorable for and magnet powder mix homogeneously.And in the dry pressuring forming process of magnetic powder, the orientation side in magnetic field Formula and magnetic field size are again particularly important, and current magnetic field orientating mode is that applying one is constant on the direction need magnetic field orientating Magnetic field, but the size in this constant magnetic field is directly proportional to the bundle number of line bag coil, and be available on moulding press place The limited space of line bag, this just determine this stationary magnetic field size limited so that dry-pressing the opposite sex ferromagnetic oxide powder degree of orientation Not high.
Content of the invention
The present invention is above-mentioned in order to overcome the shortcomings of to exist in prior art, there is provided a kind of high dry-pressing opposite sex of degree of orientation Ferritic manufacture method.
To achieve these goals, the present invention employs the following technical solutions:
A kind of different in nature ferritic manufacture method of dry-pressing, concrete operation step is as follows:
(1) ball-milling technology: first permanent ferrite prefiring material is carried out secondary wet grinding；
(2) stoving process: the slip after secondary wet grinding is put into drying baker and is dried, the magnetic powder after drying is aqueous Rate is within 0.3wt%；
(3) flouring technology: the material block after drying, first sieves and makes Magnaglo, then add binding agent, in dry mix Mix in machine, pulverized 40～60 eye mesh screens, prepared dry-pressing opposite sex ferrite powder through high speed disintegrator；
(4) dry pressuring forming process: be pressed into magnet steel on experiment press, the high current of pulsed is applied on coil, produce One instantaneous pulse magnetic field, is not less than 20000oe；
(5) sintering process: carry out degumming process at 300～500 degrees Celsius, then sinter at 1230～1260 degrees Celsius 0.5～2 hour.
First in flouring technology, choose suitable binding agent so as to can directly be sufficiently mixed with Magnaglo；Then The high current of pulsed, in dry pressuring forming process, being applied on coil, producing an instantaneous pulse magnetic field, thus avoiding The phenomenon of stationary magnetic field situation lower coil easily heating, makes the degree of orientation of dry-pressing opposite sex ferromagnetic oxide powder improve simultaneously.
Preferably, in step (1), permanent ferrite prefiring material is the hexagonal ferrite including a, r, b and fe Body, and there is the molecular formula of following feature: a1～xrx[(fe3+ afe2+ b)12-yby]zo19, wherein a represent one of sr, ba or Two kinds of elements；R represents and is selected from one of rare earth element and bi element；B represents one of co, ti, mn, zn, ge, as and w Element, the quantivalence of co element is positive trivalent；Wherein a+b is equal to 1；Z is 0.9～1.1；The scope of x and y be respectively as follows: 0≤x≤ O.54,0≤y≤0.45.
Preferably, described a is 0.97～0.999, b is 0.001～0.03；The span of x and y is: 1.0≤x/y ≤ 1.5, z are 1.
Preferably, in step (1), first in permanent ferrite prefiring material, add additive and dispersant, after carry out Secondary wet grinding, wherein: additive includes sio2And caco3, dispersant is at least one in boric acid and organic dispersing agent, adds The total weight percent that the total addition level of agent and dispersant accounts for permanent ferrite prefiring material is 0～1.5wt%.sio2、caco3Add Plus the addition of agent, contribute to being formed crystal boundary in sintering process, hinder growing up of ferrite crystal grains, thus effectively improving rectifying of product Stupid power；The addition of dispersant, that on the one hand plays grinding aid in crushing process acts on the magnet powder particle diameter so that after grinding It is more uniformly distributed；On the other hand the performance of dry-pressing product is also increased.
Preferably, in step (3), binding agent includes in polyvinyl alcohol, Polyethylene Glycol, Camphora and calcium stearate Kind or multiple, and Camphora must be contained, wherein Camphora be shaped as powder, it is pre- that the addition of binding agent accounts for permanent-magnet ferrite The total weight percent of imitation frosted glass is 1～5wt%.The feature of above-mentioned Camphora makes it not lump when adding, and is conducive to and magnet powder Last is sufficiently mixed.
The invention has the beneficial effects as follows: powder Camphora can directly be sufficiently mixed with Magnaglo；Using pulsed High current is so that the degree of orientation of dry-pressing opposite sex ferromagnetic oxide powder improves；Additive is favorably improved the coercivity of product；Dispersant So that the magnet powder particle diameter after grinding is more uniformly distributed, also the performance of dry-pressing product is also increased simultaneously.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1:
Preparation one kind has sr0.75la0.25fe11.8co0.2o19The Preburning material of ferrite principal phase, weighs fe by proportioning2o3(pure Degree >=99.3wt%, cl-≤ 0.1wt%, the original mean particle≤1.5um of granule), la2o3(purity >=99.3wt%, granule Original mean particle≤5um), co2o3(co content >=72wt%, the original mean particle≤3um of granule), srco3(purity >=97wt%, the original mean particle≤1.5um of granule) etc. raw material carry out ball milling of wet method, Ball-milling Time 5 hours, mix O.8um average particle size after conjunction is, is subsequently dried slip in an oven, processes through 10mpa pressure precompressed, subsequently 1210 DEG C of pre-burnings in atmosphere, temperature retention time 1 hour, obtain block Preburning material.Preburning material is processed through dry type coarse pulverization, coarse powder The mean diameter of broken rear powder body is 4um.The ferritic concrete technology of the dry-pressing opposite sex is as follows:
1st, ball-milling technology
First permanent ferrite prefiring material is carried out secondary wet grinding, add the caco of 1.07wt%3, the sio of 0.3wt%2、 The boric acid of 0.15wt%, its technique is such as the secondary wet-grinding technology and relative device in traditional permanent-magnet ferrite production.
2nd, stoving process
Slip after secondary ball milling is put into drying baker and is dried 20 hours the magnetic it is desirable to after drying with 120 degrees Celsius Property powder moisture content is within 0.3wt%.
3rd, flouring technology
Material block after drying, first crosses 20 eye mesh screens, makes Magnaglo；Then add 3wt% powder Camphora and 0.5wt% calcium stearate (crosses 100 mesh sieves), after mixing 1 hour, pulverizes 40 mesh through high speed disintegrator in dry mix machine Screen cloth, prepared dry-pressing opposite sex ferrite powder.
4th, dry pressuring forming process
100 tons of experiment press are pressed into magnet steel, its pressure is 1mpa, the high current of pulsed is applied on coil, produce Raw instantaneous pulse magnetic field 20000oe.
5th, sintering process
Carry out degumming process at 300～500 degrees Celsius, then with 1230 degrees Celsius of 1 hour sintering of temperature, wherein Rise gentle rate of cooling slow, it is to avoid produce cracking.
Finally, performance test is carried out to product, test result is shown in Table 1.
Embodiment 2:
Preburning material in embodiment 2 is identical with embodiment 1, and preparation technology in addition to following flouring technology remaining technique with Embodiment 1 is identical.
3rd, flouring technology
Material block after drying, first crosses 20 eye mesh screens, makes Magnaglo；Then add the powder Camphora (mistake of 4wt% 100 mesh sieves), after mixing 1 hour in dry mix machine, pulverized 40 eye mesh screens, the prepared dry-pressing opposite sex through high speed disintegrator Ferrite powder.
Finally, performance test is carried out to product, test result is shown in Table 1.
Embodiment 3:
Preburning material in embodiment 3 is identical with embodiment 1, and preparation technology is in addition to following powder processed and dry pressuring forming process Remaining technique is same as Example 1.
3rd, flouring technology
Material block after drying, first crosses 20 eye mesh screens, makes Magnaglo；Then add the powder Camphora (mistake of 4wt% 100 mesh sieves), after mixing 1 hour in dry mix machine, pulverized 40 eye mesh screens, the prepared dry-pressing opposite sex through high speed disintegrator Ferrite powder.
4th, dry pressuring forming process
100 tons of experiment press are pressed into magnet steel, its pressure is 1mpa, the high current of pulsed is applied on coil, produce Raw instantaneous pulse magnetic field 30000oe.
Finally, performance test is carried out to product, test result is shown in Table 1.
Comparative example 1:
Preburning material in comparative example 1 is identical with embodiment 1, and preparation technology is in addition to following powder processed and dry pressuring forming process Remaining technique is same as Example 1.
3rd, flouring technology
Material block after drying, first crosses 20 eye mesh screens, makes Magnaglo；Then by Camphora and ethanol with (1 gram: 1 milliliter) Ratio mixing, make solution, then this solution and Magnaglo added with 3% ratio, and add 0.5wt% calcium stearate (crossing 100 mesh sieves), after mixing 1 hour, pulverized 40 eye mesh screens through high speed disintegrator, prepared dry-pressing is different in dry mix machine Property ferrite powder.
4th, dry pressuring forming process
100 tons of experiment press are pressed into magnet steel, its pressure is 1mpa, forming magnetic field is 10000oe.
Finally, performance test is carried out to product, test result is shown in Table 1.
Comparative example 2:
Preburning material in comparative example 2 is identical with embodiment 1, and preparation technology is in addition to following powder processed and dry pressuring forming process Remaining technique is same as Example 1.
3rd, flouring technology
Material block after drying, first crosses 20 eye mesh screens, makes Magnaglo；Then add 3wt% powder Camphora and 0.5wt% calcium stearate (crosses 100 mesh sieves), after mixing 1 hour, pulverizes 40 mesh through high speed disintegrator in dry mix machine Screen cloth, prepared dry-pressing opposite sex ferrite powder.
4th, dry pressuring forming process
100 tons of experiment press are pressed into magnet steel, its pressure is 1mpa, forming magnetic field is 10000oe.
Finally, performance test is carried out to product, test result is shown in Table 1.
Table 1 embodiment 1-3 and comparative example 1-2 performance comparison
br(gs) hcb(oe) hcj(oe) (bh)max(mgoe)
Embodiment 1 3937 3429 4201 3.691
Embodiment 2 3964 3441 4191 3.695
Embodiment 3 3995 3488 4128 3.800
Comparative example 1 3873 3375 4192 3.476
Comparative example 2 3899 3301 4136 3.577

Claims (5)

1. the different in nature ferritic manufacture method of a kind of dry-pressing, is characterized in that, concrete operation step is as follows:
(1) ball-milling technology: first permanent ferrite prefiring material is carried out secondary wet grinding；
(2) stoving process: the slip after secondary wet grinding is put into drying baker and is dried, the magnetic powder moisture content after drying exists Within 0.3wt%；
(3) flouring technology: the material block after drying, first sieves and makes Magnaglo, then add binding agent, in dry mix machine Mixing, pulverized 40～60 eye mesh screens, prepared dry-pressing opposite sex ferrite powder through high speed disintegrator；
(4) dry pressuring forming process: be pressed into magnet steel on experiment press, the high current of pulsed is applied on coil, produce Instantaneous pulse magnetic field, is not less than 20000oe；
(5) sintering process: carry out degumming process at 300～500 degrees Celsius, then sinter 0.5～2 at 1230～1260 degrees Celsius Hour.
2. a kind of ferritic manufacture method of the dry-pressing opposite sex according to claim 1, is characterized in that, in step (1), forever Magnetic ferrites Preburning material is the hexgonal screw including a, r, b and fe, and has the molecular formula of following feature: a1～xrx [(fe3+ afe2+ b)12-yby]zo19, wherein a represents one of sr, ba or two kinds of elements；R represents and is selected from rare earth element and bi One of element；B represents one of co, ti, mn, zn, ge, as and w element, and the quantivalence of co element is positive trivalent；Its Middle a+b is equal to 1；Z is 0.9～1.1；The scope of x and y is respectively as follows: 0≤x≤0.54,0≤y≤0.45.
3. a kind of ferritic manufacture method of the dry-pressing opposite sex according to claim 2, is characterized in that, described a is 0.97～ 0.999, b is 0.001～0.03；The span of x and y is: 1.0≤x/y≤1.5, and z is 1.
4. the ferritic manufacture method of a kind of dry-pressing opposite sex according to claim 1 or 2 or 3, is characterized in that, in step (1), in, first in permanent ferrite prefiring material, add additive and dispersant, after carry out secondary wet grinding, wherein: additive includes sio2And caco3, dispersant is at least one in boric acid and organic dispersing agent, and the total addition level of additive and dispersant accounts for forever The total weight percent of magnetic ferrites Preburning material is 0～1.5wt%.
5. a kind of ferritic manufacture method of the dry-pressing opposite sex according to claim 1, is characterized in that, in step (3), glue Mixture includes one of polyvinyl alcohol, Polyethylene Glycol, Camphora and calcium stearate or multiple, and must contain Camphora, wherein Camphora be shaped as powder, the total weight percent that the addition of binding agent accounts for permanent ferrite prefiring material is 1～5wt%.
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CN108285348A (en) * 2018-02-08 2018-07-17 安徽盛美格新材料有限公司 A kind of manufacturing method of dry-pressing opposite sex permanent-magnet ferrite magnetic powder
CN109102977A (en) * 2018-08-20 2018-12-28 横店集团东磁股份有限公司 A kind of high density dry-pressing opposite sex ferrimagnet and its manufacturing method
CN110323027A (en) * 2018-03-28 2019-10-11 Tdk株式会社 The manufacturing method of ferrite sintered magnet and ferrite sintered magnet
CN110342923A (en) * 2019-06-17 2019-10-18 横店集团东磁股份有限公司 A kind of dry-pressing opposite sex ferrite fines preparation method and dry-pressing opposite sex permanent-magnet ferrite improving the degree of orientation and performance
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CN104496458A (en) * 2014-09-22 2015-04-08 横店集团东磁股份有限公司 Manufacturing method of dry-pressed anisotropic ferrite magnetic powder

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CN108285348A (en) * 2018-02-08 2018-07-17 安徽盛美格新材料有限公司 A kind of manufacturing method of dry-pressing opposite sex permanent-magnet ferrite magnetic powder
CN110323027A (en) * 2018-03-28 2019-10-11 Tdk株式会社 The manufacturing method of ferrite sintered magnet and ferrite sintered magnet
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CN109102977B (en) * 2018-08-20 2020-02-14 横店集团东磁股份有限公司 High-density dry-pressed anisotropic ferrite magnet and manufacturing method thereof
CN110342923A (en) * 2019-06-17 2019-10-18 横店集团东磁股份有限公司 A kind of dry-pressing opposite sex ferrite fines preparation method and dry-pressing opposite sex permanent-magnet ferrite improving the degree of orientation and performance
CN115010478A (en) * 2022-07-06 2022-09-06 横店集团东磁股份有限公司 Opposite-sex dry-pressed ferrite and preparation method thereof
CN115010478B (en) * 2022-07-06 2023-09-26 横店集团东磁股份有限公司 Different-polarity dry-pressed ferrite and preparation method thereof

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