CN106365626B - A kind of anisotropic ferritic manufacturing method of dry-pressing - Google Patents

A kind of anisotropic ferritic manufacturing method of dry-pressing Download PDF

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Publication number
CN106365626B
CN106365626B CN201610791751.9A CN201610791751A CN106365626B CN 106365626 B CN106365626 B CN 106365626B CN 201610791751 A CN201610791751 A CN 201610791751A CN 106365626 B CN106365626 B CN 106365626B
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dry
pressing
milling
anisotropic
dispersing agent
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CN106365626A (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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    • H01F1/10—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 hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
    • H01F1/11—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 hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
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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
    • H01F41/0253—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 for manufacturing permanent magnets
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    • C04B2235/605—Making or treating the green body or pre-form in a magnetic field

Abstract

The invention discloses a kind of anisotropic ferritic manufacturing methods of dry-pressing.It is specific steps are as follows: first carry out secondary wet-milling for permanent ferrite prefiring material；Slurry after secondary wet-milling is put into drying box to be dried；Material block after drying, first Magnaglo is made in sieving, then adds adhesive, mixes in dry mix machine, pulverize and sieve by high speed disintegrator, and dry-pressing opposite sex ferrite powder is made；It is pressed into magnet steel on experiment press, applies the high current of pulsed on coil, generates an instantaneous pulse magnetic field；First carry out degumming process, after be sintered.The beneficial effects of the present invention are: powdered camphor can be directly sufficiently mixed with Magnaglo；Using the high current of pulsed, so that the degree of orientation of dry-pressing opposite sex ferromagnetic oxide powder improves；Additive helps to improve the coercivity of product；Dispersing agent makes the magnet powder partial size after grinding more uniform, while still increasing to the performance of dry-pressing product.

Description

A kind of anisotropic ferritic manufacturing method of dry-pressing
Technical field
The present invention relates to magnetic material correlative technology fields, refer in particular to a kind of anisotropic ferritic manufacturing method of dry-pressing.
Background technique
Traditional permanent-magnet ferrite manufacturing method has dry-pressing formed and two kinds of Wet-pressing molding.Wherein Wet-pressing molding has orientation It spends, the high feature of magnetic properties such as remanent magnetism, is applied on a large scale at present.But the dry-pressing formed application neck for also having oneself Domain, it has the characteristics that shaping efficiency is high, has a wide range of application, product shape is diversified, can be applied to many miniaturizations and shape The irregular product of shape.
In the manufacturing 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 camphor and calcium stearate, and wherein the addition manner of camphor has Two kinds, one kind being dissolved in alcohol addition, this part that will cause powder is reunited；Another is directly to add, due to common Camphor is easy agglomeration, is also unfavorable for being uniformly mixed with magnet powder.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 application one is constant on the direction for need magnetic field orientating Magnetic field, but the size in this constant magnetic field is directly proportional to the bundle number of line packet coil, and for placing on moulding press The space of line packet is limited, this just determines that the size of this stationary magnetic field is limited, so that the dry-pressing opposite sex ferromagnetic oxide powder degree of orientation It is not high.
Summary of the invention
The present invention is in order to overcome the above deficiencies in the prior art, it is anisotropic to provide a kind of dry-pressing that the degree of orientation is high Ferritic manufacturing method.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of anisotropic ferritic manufacturing method of dry-pressing, specific steps are as follows:
(1) permanent ferrite prefiring material first ball-milling technology: is subjected to secondary wet-milling；
(2) stoving process: being put into drying box for the slurry after secondary wet-milling and be dried, and the magnetic powder after drying is aqueous Rate is within 0.3wt%；
(3) flouring technology: the material block after drying, first Magnaglo is made in sieving, adhesive is then added, in dry mix It is mixed in machine, crushed 40~60 mesh screens by high speed disintegrator, dry-pressing opposite sex ferrite powder is made；
(4) dry pressuring forming process: it is pressed into magnet steel on experiment press, applies the high current of pulsed on coil, is generated One instantaneous pulse magnetic field is not less than 20000Oe；
(5) it sintering process: in 300~500 degrees Celsius of progress degumming process, is then sintered at 1230~1260 degrees Celsius 0.5~2 hour.
First in flouring technology, suitable adhesive is chosen, allows to directly be sufficiently mixed with Magnaglo；Then In dry pressuring forming process, apply the high current of pulsed on coil, an instantaneous pulse magnetic field is generated, to avoid The phenomenon that stationary magnetic field situation lower coil is easily generated heat, while the degree of orientation of dry-pressing opposite sex ferromagnetic oxide powder is improved.
Preferably, permanent ferrite prefiring material is the hexagonal ferrite for including A, R, B and Fe in step (1) Body, and molecular formula with the following characteristics: A1~xRx[(Fe3+ aFe2+ b)12-yBy]zO19, wherein A represent one of Sr, Ba or Two kinds of elements；R, which is represented, 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 chemical valence of Co element are positive trivalent；Wherein a+b is equal to 1；Z is 0.9~1.1；The range of x and y be respectively as follows: 0≤x≤ O.54,0≤y≤0.45.
Preferably, it is 0.001~0.03 that a, which is 0.97~0.999, b,；The value range of x and y are as follows: 1.0≤x/y ≤ 1.5, z 1.
Preferably, additive and dispersing agent are first added in permanent ferrite prefiring material in step (1), it is rear to carry out Secondary wet-milling, in which: additive includes SiO2And CaCO3, dispersing agent is at least one of boric acid and organic dispersing agent, addition The total weight percent that the total addition level of agent and dispersing agent accounts for permanent ferrite prefiring material is 0~1.5wt%.SiO2、CaCO3Add The addition for adding agent helps to form crystal boundary in sintering process, hinders growing up for ferrite crystal grains, to effectively improve rectifying for product Stupid power；The addition of dispersing agent, on the one hand plays the role of grinding aid in crushing process, so that the magnet powder partial size after grinding More uniformly；On the other hand it also increases to the performance of dry-pressing product.
Preferably, adhesive includes one in polyvinyl alcohol, polyethylene glycol, camphor and calcium stearate in step (3) Kind is a variety of, and must contain camphor, and wherein the shape of camphor is powdered, and it is pre- that the additive amount of adhesive accounts for permanent-magnet ferrite The total weight percent of imitation frosted glass is 1~5wt%.The characteristics of above-mentioned camphor, makes it not agglomerate in addition, is conducive to and magnet powder End is sufficiently mixed.
The beneficial effects of the present invention are: powdered camphor can be directly sufficiently mixed with Magnaglo；Using pulsed High current, so that the degree of orientation of dry-pressing opposite sex ferromagnetic oxide powder improves；Additive helps to improve the coercivity of product；Dispersing agent So that the magnet powder partial size after grinding is more uniform, while still increasing to the performance of dry-pressing product.
Specific embodiment
The present invention will be further described With reference to embodiment.
Embodiment 1:
It prepares a kind of with Sr0.75La0.25Fe11.8Co0.2O19The Preburning material of ferrite main phase, weighs Fe according to the ratio2O3It is (pure Degree >=99.3wt%, Cl-≤ 0.1wt%, original mean particle≤1.5um of particle), La2O3(purity >=99.3wt%, particle Original mean particle≤5um), Co2O3(Co content >=72wt%, original mean particle≤3um of particle), SrCO3(purity >=97wt%, original mean particle≤1.5um of particle) etc. raw material carry out ball milling of wet process, Ball-milling Time 5 hours, mix Average particle size after conjunction is O.8um, then to dry slurry in an oven, is handled through 10MPa pressure precompressed, then 1210 DEG C of pre-burnings in air soaking time 1 hour, obtain blocky Preburning material.Preburning material is handled through dry type coarse crushing, coarse powder The average grain diameter of powder is 4um after broken.Dry-pressing it is anisotropic ferritic the specific process is as follows:
1, ball-milling technology
Permanent ferrite prefiring material is first subjected to secondary wet-milling, adds the CaCO of 1.07wt%3, 0.3wt% SiO2、 The boric acid of 0.15wt%, technique is such as the secondary wet-grinding technology and relative device in traditional permanent-magnet ferrite production.
2, stoving process
Slurry after secondary ball milling is put into drying box to be dried 20 hours with 120 degrees Celsius, it is desirable that the magnetic after drying Property powder moisture content is within 0.3wt%.
3, flouring technology
Material block after drying first crosses 20 mesh screens, Magnaglo is made；Then add 3wt% powdered camphor and 0.5wt% calcium stearate (sieves with 100 mesh sieve), after mixing 1 hour in dry mix machine, crushed 40 mesh by high speed disintegrator Dry-pressing opposite sex ferrite powder is made in sieve.
4, dry pressuring forming process
Magnet steel is pressed on 100 tons of experiment press, pressure 1MPa applies the high current of pulsed on coil, produces A raw instantaneous pulse magnetic field 20000Oe.
5, sintering process
In 300~500 degrees Celsius of progress degumming process, then it was sintered with temperature 1 hour of 1230 degrees Celsius, wherein Heating and cooling velocity are slow, avoid generating cracking.
Finally, being tested for the property to product, test result is shown in Table 1.
Embodiment 2:
Preburning material and embodiment 1 in embodiment 2 is identical, and preparation process in addition to following flouring technology remaining technique with Embodiment 1 is identical.
3, flouring technology
Material block after drying first crosses 20 mesh screens, Magnaglo is made；Then the powdered camphor (mistake of 4wt% is added 100 meshes), it after mixing 1 hour in dry mix machine, crushed 40 mesh screens by high speed disintegrator, it is anisotropic that dry-pressing be made Ferrite powder.
Finally, being tested for the property to product, test result is shown in Table 1.
Embodiment 3:
Preburning material and embodiment 1 in embodiment 3 is identical, and preparation process is in addition to following powder processed and dry pressuring forming process Remaining technique is same as Example 1.
3, flouring technology
Material block after drying first crosses 20 mesh screens, Magnaglo is made；Then the powdered camphor (mistake of 4wt% is added 100 meshes), it after mixing 1 hour in dry mix machine, crushed 40 mesh screens by high speed disintegrator, it is anisotropic that dry-pressing be made Ferrite powder.
4, dry pressuring forming process
Magnet steel is pressed on 100 tons of experiment press, pressure 1MPa applies the high current of pulsed on coil, produces A raw instantaneous pulse magnetic field 30000Oe.
Finally, being tested for the property to product, test result is shown in Table 1.
Comparative example 1:
Preburning material and embodiment 1 in comparative example 1 is identical, and preparation process is in addition to following powder processed and dry pressuring forming process Remaining technique is same as Example 1.
3, flouring technology
Material block after drying first crosses 20 mesh screens, Magnaglo is made；Then by camphor and alcohol with (1 gram: 1 milliliter) Ratio mixing, be made solution, then this solution and Magnaglo are added with 3% ratio, and 0.5wt% calcium stearate is added (sieving with 100 mesh sieve) crushed 40 mesh screens by high speed disintegrator after mixing 1 hour in dry mix machine, and it is different that dry-pressing is made Property ferrite powder.
4, dry pressuring forming process
Magnet steel, pressure 1MPa, forming magnetic field 10000Oe are pressed on 100 tons of experiment press.
Finally, being tested for the property to product, test result is shown in Table 1.
Comparative example 2:
Preburning material and embodiment 1 in comparative example 2 is identical, and preparation process is in addition to following powder processed and dry pressuring forming process Remaining technique is same as Example 1.
3, flouring technology
Material block after drying first crosses 20 mesh screens, Magnaglo is made；Then add 3wt% powdered camphor and 0.5wt% calcium stearate (sieves with 100 mesh sieve), after mixing 1 hour in dry mix machine, crushed 40 mesh by high speed disintegrator Dry-pressing opposite sex ferrite powder is made in sieve.
4, dry pressuring forming process
Magnet steel, pressure 1MPa, forming magnetic field 10000Oe are pressed on 100 tons of experiment press.
Finally, being tested for the property to product, test result is shown in Table 1.
1 embodiment 1-3 of table 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 (3)

1. a kind of anisotropic ferritic manufacturing method of dry-pressing, characterized in that specific steps are as follows:
(1) permanent ferrite prefiring material first ball-milling technology: is subjected to secondary wet-milling；Permanent ferrite prefiring material be include A, R, The hexgonal screw of B and Fe, and molecular formula with the following characteristics: A1~xRx[(Fe3+ aFe2+ b)12-yBy]zO19, wherein A Represent one of Sr, Ba or two kinds of elements；R, which is represented, is selected from one of rare earth element and Bi element；B represent Co, Ti, One of Mn, Zn, Ge, As and W element, the chemical valence of Co element are positive trivalent；Wherein a+b is equal to 1；Z is 0.9~1.1；x It is respectively as follows: 0≤x≤0.54,0≤y≤0.45 with the range of y；
(2) stoving process: being put into drying box for the slurry after secondary wet-milling and be dried, and the magnetic powder moisture content after drying exists Within 0.3wt%；
(3) flouring technology: the material block after drying, first Magnaglo is made in sieving, adhesive is then added, in dry mix machine Mixing, crushed 40~60 mesh screens by high speed disintegrator, and dry-pressing opposite sex ferrite powder is made；Described adhesive includes poly- One or more of vinyl alcohol, polyethylene glycol, camphor and calcium stearate, and camphor must be contained, the wherein shape of camphor To be powdered, the total weight percent that the additive amount of adhesive accounts for permanent ferrite prefiring material is 1~5wt%；
(4) dry pressuring forming process: it is pressed into magnet steel on experiment press, applies the high current of pulsed on coil, generates one Instantaneous pulse magnetic field is not less than 20000Oe；
(5) sintering process: in 300~500 degrees Celsius of progress degumming process, 0.5~2 then is sintered at 1230~1260 degrees Celsius Hour.
2. a kind of anisotropic ferritic manufacturing method of dry-pressing according to claim 1, characterized in that a is 0.97~ 0.999, b is 0.001~0.03；The value range of x and y are as follows: 1.0≤x/y≤1.5, z 1.
3. the anisotropic ferritic manufacturing method of a kind of dry-pressing according to claim 1 or 2, characterized in that in step (1) In, additive and dispersing agent are first added in permanent ferrite prefiring material, carries out secondary wet-milling afterwards, in which: additive includes SiO2And CaCO3, dispersing agent is at least one of boric acid and organic dispersing agent, and the total addition level of additive and dispersing agent accounts for forever The total weight percent of magnetic ferrites Preburning material is 0~1.5wt%.
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JP7047530B2 (en) * 2018-03-28 2022-04-05 Tdk株式会社 Ferrite Sintered Magnet and Ferrite Sintered Magnet Manufacturing Method
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
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