CN107293398A - A kind of preparation method of permanent-magnet ferrite material - Google Patents

A kind of preparation method of permanent-magnet ferrite material Download PDF

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Publication number
CN107293398A
CN107293398A CN201610202814.2A CN201610202814A CN107293398A CN 107293398 A CN107293398 A CN 107293398A CN 201610202814 A CN201610202814 A CN 201610202814A CN 107293398 A CN107293398 A CN 107293398A
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China
Prior art keywords
wet
permanent
fine grinding
milling
slurry
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Pending
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CN201610202814.2A
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Chinese (zh)
Inventor
吴永路
邱士星
袁小镇
匡雪冬
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Shanghai Meishan Iron and Steel Co Ltd
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Shanghai Meishan Iron and Steel Co Ltd
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Priority to CN201610202814.2A priority Critical patent/CN107293398A/en
Publication of CN107293398A publication Critical patent/CN107293398A/en
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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
    • H01F41/0253—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
    • H01F41/0266—Moulding; Pressing
    • 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
    • H01F1/032—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
    • 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

Abstract

The invention discloses a kind of preparation method of permanent-magnet ferrite material, mainly solve it is existing when substituting rare earth element additive using conventional trace mineral supplement and preparing permanent-magnet ferrite material, magnetism of material can difference technical problem.The inventive method comprises the following steps：The fine grinding of hot rolling iron scale is aoxidized；Prepare main material；Wet-milling batch mixing；Pre-burning；Coarse crushing；Wet-milling slurrying；Wet pressing pressing under magnetic field；Double sintering；Ripe base polishing.The present invention is using conventional trace mineral supplement, and preparation technology is simple, without increasing technological equipment newly, and the permanent-magnet ferrite material performance of preparation is stably reached prepares permanent-magnet ferrite material performance level using rare earth element additive；Present invention reduces the preparation cost of permanent-magnet ferrite material.

Description

A kind of preparation method of permanent-magnet ferrite material
Technical field
It is more particularly to a kind of using two types Fe the present invention relates to a kind of preparation method of permanent-magnet material2O3Raw material is mixed with The method of high-performance permanent magnetic ferrite material, belongs to the manufacture field of magnetic material.
Background technology
The high cost metals element such as Ni, Co and rare earth is not contained in M type permanent-magnet ferrite materials, with other magnetic material phases Than price is relatively low；Meanwhile, because its remanent magnetism is moderate, chemical stability is good, and relative mass is relatively low, and cost performance is higher than other magnetic Material；Therefore, permanent-magnet ferrite plays an important role in industries such as household electrical appliances, computer, automobile, communications, commercially Occupy an leading position.
M type hexgonal screws are expressed as：MO·6Fe2O3M is Ba, Sr, Pb etc. in formula, wherein, Fe2O3 Mainly there is acid washing iron red and two kinds of hot rolling iron scale in source.
With scientific and technological progress, electronic product is to the performance requirement more and more higher of permanent-magnet ferrite, and mostly in the market is by LaCo Addition Deng rare earth element improves ferrite magnetic performance, because rare earth element price is higher and it is larger to fluctuate, addition rare earth element Permanent-magnet ferrite material cost is of a relatively high.
Current permanent-magnet ferrite material when being prepared using conventional trace mineral supplement substitution rare earth element additive, magnetic property without Method reaches residual magnetic flux density Br >=415mT, coercivity H b >=290kA/m and HCJ Hcj >=305kA/m.
The content of the invention
It is an object of the invention to provide a kind of preparation method of permanent-magnet ferrite material, mainly solve existing using conventional trace element When additive replacement rare earth element additive prepares permanent-magnet ferrite material, the technical problem that magnetism of material can be poor.
The technical solution adopted by the present invention is：A kind of preparation method of permanent-magnet ferrite material, comprises the following steps：
1) fine grinding of hot rolling iron scale is aoxidized, and drying hot rolling iron scale is levigate using ball mill, obtains the iron powder that granularity is 2~8 μm, And fine grinding iron powder is aoxidized in atmosphere, temperature is 600~850 DEG C, and soaking time is 1~4 hour, obtains brown iron oxide, Granularity is 5~10 μm；
2) main material is prepared, the component and ratio of main material are：Brown iron oxide 17-35wt%, pickling iron oxide red 50-70wt%, Strontium carbonate is Fe in 13-14wt%, brown iron oxide2O3Weight percentage >=98%, acid washing iron red middle Fe2O3Weight percent SrCO in Content >=99%, strontium carbonate3Weight percentage >=97%；
3) wet-milling batch mixing, using water as wet-milling dispersion medium, main material and an additive is added in ball mill simultaneously, 1~10 is carried out The wet-milling batch mixing of hour, obtains wet-milling slurry, powder granularity is 0.7~1.5 μm after the drying of wet-milling slurry, and an additive is Industrial pure silicon dioxide, the adding proportion that an additive is counted using main material weight is SiO20.1-0.4wt%；
4) pre-burning, pre-burning is carried out by the slurry obtained through wet-milling batch mixing in atmosphere, and temperature is 1160~1350 DEG C, insulation 1~5 hour time, obtain a Preburning material；
5) coarse crushing, it is 1~6 μm of coarse powder that grade screening is carried out after a Preburning material is crushed using ball mill and obtains granularity；
6) wet-milling slurrying, carries out fine grinding with ball mill after adding secondary additive in the coarse powder that coarse crushing is obtained, is scattered using water Medium, obtains fine grinding slurry, powder granularity is 0.2~1.0 μm after the drying of fine grinding slurry, specific surface area is 1~12m2/ g, it is described Adding proportion of the secondary additive in terms of coarse powder weight be：CaCO30.8-1.5wt%, SiO20.1-0.5wt%, H3BO3 0.1-0.4wt%, Al2O30.1-0.4wt%, SrCO30-0.6wt%, calcium gluconae 0.1-0.6wt%；
7) wet pressing pressing under magnetic field, the fine grinding slurry concentration that fine grinding is obtained is the aqueous shaping slurry for being 35~55wt%, additional Magnetic field is that 8~18kOe, briquetting pressure are to be pressed into green compact under conditions of 19.6~78.4Mpa；
8) double sintering, obtained by molding green compact are sintered in atmosphere, and temperature is 1160~1230 DEG C, soaking time 2~6 Hour, obtain ripe base；
9) ripe base polishing, finished product is obtained after ripe base is polished using self-acting grinding machine.
The preparation technology provided by the present invention, permanent-magnet ferrite material is prepared with conventional trace mineral supplement, and remanence is made Induction Br >=415mT, coercivity H b >=290kA/m, HCJ Hcj >=305kA/m high-performance permanent oxygen Body material.
The present invention has following good effect compared with prior art：1st, the present invention prepares work using conventional trace mineral supplement Skill is simple, without increasing technological equipment newly, and the permanent-magnet ferrite material performance of preparation is stably reached to be prepared using rare earth element additive Permanent-magnet ferrite material performance level.2nd, present invention reduces the preparation cost of permanent-magnet ferrite material.
Embodiment
With reference to embodiment, the present invention is furture elucidated, it should be understood that following embodiments are merely to illustrate this hair Bright rather than limitation the scope of the present invention.
A kind of embodiment 1, preparation method of permanent-magnet ferrite material, comprises the following steps：
1) fine grinding of hot rolling iron scale is aoxidized, and drying hot rolling iron scale is levigate using ball mill, obtains the iron powder that granularity is 4.1 μm, and Fine grinding iron powder is aoxidized in atmosphere, temperature is 750 DEG C, soaking time is 3 hours, obtains brown iron oxide, and granularity is 8μm；
2) main material is prepared, the component and ratio of main material are：Brown iron oxide 25.9wt%, pickling iron oxide red 60.6wt%, Strontium carbonate is Fe in 13.5wt%, brown iron oxide2O3Content is 99wt%, acid washing iron red middle Fe2O3Content is 99.2wt%, carbon SrCO in sour strontium3Content is 97.5wt%；
3) wet-milling batch mixing, using water as wet-milling dispersion medium, main material and an additive is added in ball mill simultaneously, 4 are carried out The wet-milling batch mixing of hour, obtains wet-milling slurry, powder granularity is 0.95 μm after slurry drying, an additive is technical pure Silica, the adding proportion that an additive is counted using main material weight is SiO20.3wt%；
4) pre-burning, pre-burning is carried out by slurry obtained by compounding process in atmosphere, and temperature is 1260 DEG C, and soaking time 4 is small When, obtain a Preburning material；
5) coarse crushing, it is 3.1 μm of coarse powder that grade screening is carried out after an above-mentioned Preburning material is crushed using ball mill and obtains granularity；
6) wet-milling slurrying, secondary additive is added using ball mill progress fine grinding by coarse powder obtained by coarse crushing, using water as decentralized medium, Fine grinding slurry is obtained, powder granularity is 0.7 μm after the drying of fine grinding slurry, specific surface area is 1~12m2/ g, described secondary addition Adding proportion of the agent in terms of coarse powder weight be：CaCO31.2wt%, Al2O30.1wt%, SiO20.2wt%, H3BO30.2wt%, SrCO3=0.2wt%, calcium gluconae 0.5wt%；
7) wet pressing pressing under magnetic field, using wet method pressing under magnetic field, the fine grinding slurry concentration that above-mentioned fine grinding is obtained be it is aqueous be 40wt% Shaping slurry, be that 15kOe, briquetting pressure are cylinder that Φ 28.5mm are pressed under conditions of 34.3Mpa in externally-applied magnetic field Green compact；
8) double sintering, obtained by molding green compact are sintered in atmosphere, and temperature is 1180 DEG C, soaking time 2 hours, Obtain ripe base；
9) ripe base polishing, finished product is obtained after ripe base is polished using self-acting grinding machine.
Permanent-magnet ferrite material magnetic property is made from embodiment 1：Residual magnetic flux density Br=417.2mT, coercivity Hcb=294.8kA/m, HCJ Hcj=307.0kA/m, maximum magnetic energy product (BH) max=34.6kJ/m3。
A kind of embodiment 2, preparation method of permanent-magnet ferrite material, comprises the following steps：
1) fine grinding of hot rolling iron scale is aoxidized, and drying hot rolling iron scale is levigate using ball mill, obtains the iron powder that granularity is 4.1 μm, and Fine grinding iron powder is aoxidized in atmosphere, temperature is 780 DEG C, soaking time is 2 hours, obtains brown iron oxide, and granularity is 8μm；
2) main material is prepared, the component and ratio of main material are：Brown iron oxide 34.6wt%, pickling iron oxide red 51.9wt%, Strontium carbonate is Fe in 13.5wt%, brown iron oxide2O3Content is 99wt%, acid washing iron red middle Fe2O3Content is 99.2wt%, carbon SrCO in sour strontium3Content is 97.5wt%；
3) wet-milling batch mixing, using water as wet-milling dispersion medium, main material and an additive is added in ball mill simultaneously, 3 are carried out The wet-milling batch mixing of hour, obtains wet-milling slurry, powder granularity is 1.0 μm after slurry drying, an additive is technical pure Silica, the adding proportion that an additive is counted using main material weight is SiO20.25wt%；
4) pre-burning, pre-burning is carried out by slurry obtained by compounding process in atmosphere, and temperature is 1260 DEG C, and soaking time 4 is small When, obtain a Preburning material；
5) coarse crushing, it is 3.4 μm of coarse powder that grade screening is carried out after an above-mentioned Preburning material is crushed using ball mill and obtains granularity；
6) wet-milling slurrying, secondary additive is added using ball mill progress fine grinding by coarse powder obtained by coarse crushing, using water as decentralized medium, Fine grinding slurry is obtained, powder granularity is 0.7 μm after the drying of fine grinding slurry, specific surface area is 1~12m2/ g, described secondary addition Adding proportion of the agent in terms of coarse powder weight be：CaCO31.3wt%, Al2O30.1wt%, SiO20.2wt%, H3BO30.2wt%, Calcium gluconae 0.5wt%；
7) wet pressing pressing under magnetic field, using wet method pressing under magnetic field, the fine grinding slurry concentration that above-mentioned fine grinding is obtained be it is aqueous be 40wt% Shaping slurry, be that 15kOe, briquetting pressure are cylinder that Φ 28.5mm are pressed under conditions of 34.3Mpa in externally-applied magnetic field Green compact；
8) double sintering, obtained by molding green compact are sintered in atmosphere, and temperature is 1180 DEG C, soaking time 2 hours, Obtain ripe base；
9) ripe base polishing, finished product is obtained after ripe base is polished using self-acting grinding machine.
Permanent-magnet ferrite material magnetic property is made from embodiment 2：Residual magnetic flux density Br=418.2mT, coercivity Hcb=296.1kA/m, HCJ Hcj=306.2kA/m, maximum magnetic energy product (BH) max=34.6kJ/m3。
The content that this specification is not described in detail belongs to prior art known to professional and technical personnel in the field.

Claims (1)

1. a kind of preparation method of permanent-magnet ferrite material, it is characterized in that, described method comprises the following steps：
1) fine grinding of hot rolling iron scale is aoxidized, and drying hot rolling iron scale is levigate using ball mill, obtains the iron powder that granularity is 2~8 μm, And fine grinding iron powder is aoxidized in atmosphere, temperature is 600~850 DEG C, and soaking time is 1~4 hour, obtains brown iron oxide, Granularity is 5~10 μm；
2) main material is prepared, the component and ratio of main material are：Brown iron oxide 17-35wt%, pickling iron oxide red 50-70wt%, Strontium carbonate is Fe in 13-14wt%, brown iron oxide2O3Weight percentage >=98%, acid washing iron red middle Fe2O3Weight percent SrCO in Content >=99%, strontium carbonate3Weight percentage >=97%；
3) wet-milling batch mixing, using water as wet-milling dispersion medium, main material and an additive is added in ball mill simultaneously, 1~10 is carried out The wet-milling batch mixing of hour, obtains wet-milling slurry, powder granularity is 0.7~1.5 μm after the drying of wet-milling slurry, and an additive is Industrial pure silicon dioxide, the adding proportion that an additive is counted using main material weight is SiO20.1-0.4wt%；
4) pre-burning, pre-burning is carried out by the slurry obtained through wet-milling batch mixing in atmosphere, and temperature is 1160~1350 DEG C, insulation 1~5 hour time, obtain a Preburning material；
5) coarse crushing, it is 1~6 μm of coarse powder that grade screening is carried out after a Preburning material is crushed using ball mill and obtains granularity；
6) wet-milling slurrying, carries out fine grinding with ball mill after adding secondary additive in the coarse powder that coarse crushing is obtained, is scattered using water Medium, obtains fine grinding slurry, powder granularity is 0.2~1.0 μm after the drying of fine grinding slurry, specific surface area is 1~12m2/ g, it is described Adding proportion of the secondary additive in terms of coarse powder weight be：CaCO30.8-1.5wt%, SiO20.1-0.5wt%, H3BO3 0.1-0.4wt%, Al2O30.1-0.4wt%, SrCO30-0.6wt%, calcium gluconae 0.1-0.6wt%；
7) wet pressing pressing under magnetic field, the fine grinding slurry concentration that fine grinding is obtained is the aqueous shaping slurry for being 35~55wt%, additional Magnetic field is that 8~18kOe, briquetting pressure are to be pressed into green compact under conditions of 19.6~78.4Mpa；
8) double sintering, obtained by molding green compact are sintered in atmosphere, and temperature is 1160~1230 DEG C, soaking time 2~6 Hour, obtain ripe base；
9) ripe base polishing, finished product is obtained after ripe base is polished using self-acting grinding machine.
CN201610202814.2A 2016-04-01 2016-04-01 A kind of preparation method of permanent-magnet ferrite material Pending CN107293398A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110323025A (en) * 2018-03-28 2019-10-11 Tdk株式会社 Ferrite sintered magnet
CN110372362A (en) * 2019-07-15 2019-10-25 横店集团东磁股份有限公司 A kind of preparation method and permanent-magnet ferrite material of permanent-magnet ferrite material
CN110773743A (en) * 2019-10-28 2020-02-11 苏师大半导体材料与设备研究院(邳州)有限公司 Method for producing iron core from powder raw material
CN112876231A (en) * 2021-03-09 2021-06-01 中南大学 Preparation method of permanent magnetic ferrite and permanent magnetic ferrite
CN113620700A (en) * 2021-09-10 2021-11-09 中南大学 Short-process for preparing permanent magnetic ferrite
CN113698192A (en) * 2021-09-10 2021-11-26 中南大学 Method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as raw material
CN115784733A (en) * 2022-12-22 2023-03-14 矿冶科技集团有限公司 High-performance calcium lanthanum cobalt ferrite material and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104609843A (en) * 2014-12-11 2015-05-13 南京梅山冶金发展有限公司 Preparation method for non-rare-earth high-remanent-magnetism permanent-magnetism ferrite

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104609843A (en) * 2014-12-11 2015-05-13 南京梅山冶金发展有限公司 Preparation method for non-rare-earth high-remanent-magnetism permanent-magnetism ferrite

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110323025A (en) * 2018-03-28 2019-10-11 Tdk株式会社 Ferrite sintered magnet
CN110372362A (en) * 2019-07-15 2019-10-25 横店集团东磁股份有限公司 A kind of preparation method and permanent-magnet ferrite material of permanent-magnet ferrite material
CN110773743A (en) * 2019-10-28 2020-02-11 苏师大半导体材料与设备研究院(邳州)有限公司 Method for producing iron core from powder raw material
CN112876231A (en) * 2021-03-09 2021-06-01 中南大学 Preparation method of permanent magnetic ferrite and permanent magnetic ferrite
CN113620700A (en) * 2021-09-10 2021-11-09 中南大学 Short-process for preparing permanent magnetic ferrite
CN113698192A (en) * 2021-09-10 2021-11-26 中南大学 Method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as raw material
CN115784733A (en) * 2022-12-22 2023-03-14 矿冶科技集团有限公司 High-performance calcium lanthanum cobalt ferrite material and preparation method thereof
CN115784733B (en) * 2022-12-22 2023-12-01 矿冶科技集团有限公司 High-performance calcium lanthanum cobalt ferrite material and preparation method thereof

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Application publication date: 20171024