CN103964829A - Preparation and sintering of single-aperture blank of oxygen self-supported permanent magnetic ferrite pre-sintering material - Google Patents
Preparation and sintering of single-aperture blank of oxygen self-supported permanent magnetic ferrite pre-sintering material Download PDFInfo
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- CN103964829A CN103964829A CN201410190994.8A CN201410190994A CN103964829A CN 103964829 A CN103964829 A CN 103964829A CN 201410190994 A CN201410190994 A CN 201410190994A CN 103964829 A CN103964829 A CN 103964829A
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Abstract
The invention relates to preparation and sintering of a single-aperture blank of an oxygen self-supported permanent magnetic ferrite pre-sintering material and belongs to the technical field of preparation of magnetic functional materials. The technical scheme is carried out according to a main-phase molecular formula: Srl-xBaxO.nFe (12-y)/nRy/nO3, wherein x is not less than 0 and is not greater than 0.998, and n is not less than 5.75 and not greater than 6.15, 0 & 1t; y is not greater than 0.6, and R is Mn and is secondarily added with one or more than two of industrial pure oxides CeO2, GeO2 and MnO2. To the prepared pre-sintering material and a high-performance permanent magnetic ferrite material prepared from auxiliary secondary adding, the residual magnetism Br value is at least 392 mT, the Hcj value is at least 343.1 kA/m, and the BHmax value is at least 27.9 kJ/m<3>. The preparation and sintering have the advantages that a certain amount of K2MnO4 is added to a raw material of the ferrite pre-sintering material prepared by one-time sintering and meanwhile MnO2 is added into a secondary adding auxiliary material, so that the uniformity of performance of the same batch of products is improved, and the grain refinement is facilitated at the same time; the problem of the restriction of residual magnetic flux density Br and Hcj is effectively solved, and the prepared permanent magnetic ferrite has high Br and Hcj.
Description
Technical field
The invention belongs to magnetic functional material preparing technical field, specially refer to a kind of preparation and sintering process from oxygen supply type permanent ferrite prefiring material single aperture blank.
Background technology
M type permanent-magnet ferrite belongs to hexagonal system, because it has very high monadic magnetocrystalline anisotropy, superior cost performance, the higher feature such as Curie temperature and chemical stability, be used as a kind of important permanent magnet material and magnetic recording material, be widely used in the every field such as household electrical appliances, computer, automobile, communication.
Along with improving constantly that product miniaturization, lightness, slimming and environmental protection and energy saving require, the demand of permanent-magnet ferrite material is increased greatly in recent years.Therefore explore and research and develop single batch and become product more substantial permanent-magnet ferrite material and technology of preparing thereof, to meeting industrialization user demand, have great importance, be all also one of emphasis of magneticsubstance research field all the time.
The main technique of producing at present ferrite prefiring material is: the ball milling-pressed compact-sintering-powder process of proportioning raw materials-batch mixing.Wherein, in pressed compact link, in order to improve the abundant sintering of ferrite blank, prepared base cake need to maintain aperture conventionally, the base cake suppressed incomplete right cylinder, but there is single aperture at center.Can keep to a certain extent more like this surface-area that in blank, ferrite contacts with oxygen, the performance uniformity of material after raising sintering; But, general single aperture blank at present, in actual production process, because the temperature of different positions in sintering oven is different with density of air, sintering is incomplete in final some region of finished product Preburning material, has affected the performance with batch products.If the aperture quantity of blank is increased, although can add the oxygen-supplying amount of blank in sintering process, the ferrite prefiring material output of single batch of SINTERING PRODUCTION but reduces greatly, is unfavorable for energy-conserving and environment-protective, the utilization of high efficiency of energy.
Single aperture blank, prepares permanent ferrite prefiring material at present, and the product performance of its Preburning material only reach remanent magnetism B
rreach>=200mT of value, HCJ H
cjreach>=125kA/m of value, magnetic energy product (BH)
maxreach>=18.7kJ/m of value
3; Adopt this Preburning material to carry out the performance of the magnetic material after secondary interpolation thereby affected.The Preburning material that adopts the present invention to prepare, and auxiliary secondary adds the high-performance permanent magnetic ferrite material remanent magnetism B of preparation
rreach>=392mT of value, HCJ H
cjreach>=343.1kA/m of value, magnetic energy product (BH)
maxreach>=27.9kJ/m of value
3.
Summary of the invention
The present invention aims to provide that a kind of technique is relatively simple, cost is relatively low and be beneficial to high-performance permanent magnetic ferrite material of industrialized mass production and preparation method thereof, and the high-performance permanent magnetic ferrite material of preparing by the method has higher remanent magnetism, HCJ and maximum magnetic energy product.
For achieving the above object, the technical solution adopted in the present invention is:
From preparation and the sintering process of oxygen supply type permanent ferrite prefiring material single aperture blank, it is characterized in that: described permanent-magnet ferrite material is hexaplanar, its chemical structural formula is Sr
1-xba
xonFe
(12-y)/nr
y/no
3, wherein 0≤x≤0.998,5.75≤n≤6.15,0<y≤0.6, R is Mn; Its concrete preparation method comprises the following steps:
(1) batch mixing: press chemical structural formula Sr
1-xba
xonFe
(12-y)/nr
y/no
3composition requirement, after mixing with the corresponding oxidation raw material of contained component and carbonate raw material powder, complete Primary batching system, and once add and account for added raw material (Sr
1-xba
xonFe
(12-y)/nr
y/no
3moiety summation) weight ratio be respectively the SiO of 0.1～1.0wt%
2, the CaCO of 0.1～1.0wt%
3; With water, steel ball is according to material: the weight ratio of water: ball=1:1.5:15 is mixed, and carries out ball milling 1～4 hour, and obtaining suspended particle median size is the batch mixing of 1.0 μ m～1.5 μ m;
(2) pre-burning: through filtering, after dry and granulation, carry out pre-burning at 1150～1350 DEG C, soaking time 1～8 hour, prepares permanent ferrite prefiring material by gained batch mixing in step (1);
(3) powder process: by prepared permanent ferrite prefiring material in step (2), utilize pulverizer fragmentation, cross 120 mesh sieves, obtain permanent ferrite prefiring powder;
(4) secondary ball milling: the CaCO by the permanent ferrite prefiring powder of preparation in step (3) with the secondary additive 0.1～1.8wt% that will add
3, 0.1～1.0wt% SiO
2, 0.1～1.0wt% H
3bO
3, 0.1～2.0wt% SrCO
3, the calglucon of 0.1～1.0wt%, the K of 0.1～1.0wt%
2mnO
4, with water, steel ball is still according to material: the weight ratio of water: ball=1:1.5:15 is mixed, and carries out secondary ball milling, obtains the slip that suspended particle median size is 0.50～1.00 μ m; The diameter of institute's employing steel ball is respectively 3mm, 4mm, 5mm, and weight proportion is 1:1:1;
(5) compacting green compact: according to actual operation requirements, control the size of mold shape, suppress green compact in alignment magnetic field>=380kA/m, forming pressure is 6～12MPa, and pressurize 10～20s is pressed into density > 3.6g/cm
3center single aperture right cylinder green compact;
(6) sintering: the green compact in step (5) are incubated to 30 minutes at 650 DEG C, at 1130～1250 DEG C, carry out sintering in atmospheric oxygen voltinism atmosphere subsequently, soaking time is 1～6 hour, and temperature rise rate is 5 DEG C/min;
(7) grinding and measurement: the magnetic patch that is cooled to room temperature after sintering is cut and grinding, test, measure according to GB/T3217-92 national standard.
A kind of high-performance permanent magnetic ferrite material as above and preparation method thereof, is characterized in that: the oxide raw material described in step (1) comprises Fe
2o
3, Fe
3o
4, K
2mnO
4, carbonate raw material comprises SrCO
3and BaCO
3; And be industrial pure material.
A kind of high-performance permanent magnetic ferrite material as above and preparation method thereof, is characterized in that: the secondary additive in step (4) also comprises commercially pure oxide compound CeO
2, GeO
2, MnO
2one or more, oxide compound (CeO
2, Ga
2o
3, MoO
3one or more) total amount to account for Preburning material weight ratio be 0.01～10.0wt%.
Adopt Preburning material of the present invention to carry out secondary auxiliary material and add sintering, in the time that sintering temperature is 1130 DEG C～1200 DEG C, the reach>=392mT of high-performance permanent magnetic ferrite material remanent magnetism Br value of preparation, HCJ H
cjreach>=343.1kA/m of value, magnetic energy product (BH)
maxreach>=27.9kJ/m of value
3.
The present invention adopts in ferrite prefiring material raw material, add a certain amount of K once sintered preparation
2mnO
4, add in auxiliary material and add MnO at secondary simultaneously
2, K wherein
2mnO
4in sintering process, decompose the oxygen producing, can improve ferritic sintering degree in pre-burning process, improve the performance uniformity of same batch products; The product KMnO of its decomposition simultaneously
4play the effect of dispersion agent, in sintering process, ferrite nucleation intergranule has been produced to coating function, be beneficial to the refinement of crystal grain, not only effectively solved current domestic conventional conventional additive (CaCO
3, H
3bO
3deng) can not solve residual magnetic flux density B
rwith HCJ H
cjbetween the difficult problem of " restriction or checking relation in five elements ", and the permanent-magnet ferrite Sr of preparation
1-xba
xonFe
(12-y)/nr
y/no
3have higher remanent magnetism and HCJ.High-performance permanent magnetic ferrite material of the present invention, compared with traditional strontium barium ferrite, has reduced sintering temperature, has reduced the energy consumption of production identical weight ferrite prefiring material, has increased the performance uniformity of product; Compared with rear-earth-doped permanent magnetism strontium or barium ferrite, cost performance is higher; By the experience coating function in once sintered process, play the effect of grain refining, reduce the shared ratio of ultrafine powder particle simultaneously, thereby avoided the magnetic part difficult forming causing because particle is meticulous, improve the efficiency manufacturing a product.
For achieving the above object, the present invention determines thing phase composite and pattern by X-ray diffractometer (XRD) and scanning electronic microscope (SEM), with B-H magnetic property survey meter measurement permanent magnetism characteristic parameter.
Brief description of the drawings
Fig. 1 is the XRD diffracting spectrum that adopts high-performance permanent magnetic ferrite material prepared by patent Preburning material of the present invention in embodiment 1;
Fig. 2 is the SEM shape appearance figure of the high-performance permanent magnetic ferrite material described in Fig. 1;
Fig. 3 is the demagnetizing curve of the high-performance permanent magnetic ferrite material described in Fig. 1.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in limiting the scope of the invention for the present invention is described.The present invention can implement by the either type described in summary of the invention.
Embodiment 1
Press chemical structural formula Sr
1-xba
xonFe
(12-y)/nr
y/no
3(x=0.0, n=6.0, y=0.2, the composition requirement that R is Mn, taking industrial iron oxide red (purity is as 99.5%), Strontium carbonate powder (purity is as 99.05%) and commercially pure K
2mnO
4for raw material, carry out Primary batching system, and add 0.2wt%CaCO simultaneously
3, 0.3wt%SiO
2as an additive, with water, steel ball is according to material: the weight ratio of water: ball=1:1.5:15 is mixed, and carries out ball milling 2 hours, obtains the batch mixing that suspended particle median size is 1.0～1.5 μ m.
Batch mixing after filtration, after dry and granulation, pre-burning at 1290 DEG C, is incubated 3 hours, prepares M type permanent ferrite prefiring material;
In the preburning powdered material obtaining, add secondary additive subsequently after pulverizing, sieving, additive each component addition is as follows respectively with the preburning powdered material weight ratio that will add: 1.1wt%CaCO
3, 0.3wt%SiO
2, 0.2wt%H
3bO
3, 1.5wt%SrCO
3with 0.5wt% calglucon, 0.1wt%MnO
2.Carry out secondary ball milling with roller milling machine, be milled to the powder that median size is 0.65 μ m;
Be 380kA/m at alignment magnetic field, forming pressure is 10MPa, pressurize 12s, and being pressed into mean density is 3.54g/cm
3green compact.
Green compact are at 1176 DEG C in sintering temperature, and in atmospheric oxygen voltinism atmosphere, sintering obtains finished product in 2 hours, and temperature rise rate is 6 DEG C/min.
The prepared permanent-magnet ferrite product of the present embodiment is after testing: residual magnetization Br is 401.4mT; Magneticinduction coercivity H b is 302.9kA/m; HCJ H
cjfor 343.1kA/m; Maximum magnetic energy product (BH)
maxfor 30.5kJ/m
3.
Embodiment 2
Press chemical structural formula Sr
1-xba
xonFe
(12-y)/nr
y/no
3(x=0.0, n=6.0, y=0.25, the composition requirement that R is Mn, taking industrial iron oxide red (purity is as 99.5%), Strontium carbonate powder (purity is as 99.05%) and commercially pure K
2mnO
4for raw material, carry out Primary batching system, and add 0.2wt%CaCO simultaneously
3, 0.3wt%SiO
2as an additive, with water, steel ball is according to material: the weight ratio of water: ball=1:1.5:15 is mixed, and carries out ball milling 2 hours, obtains the batch mixing that suspended particle median size is 1.0～1.5 μ m.
Batch mixing after filtration, after dry and granulation, pre-burning at 1290 DEG C, is incubated 3 hours, prepares M type permanent ferrite prefiring material.
In the preburning powdered material obtaining, add secondary additive subsequently after pulverizing, sieving, additive each component addition is as follows respectively with the preburning powdered material weight ratio that will add: 1.1wt%CaCO
3, 0.3wt%SiO
2, 0.2wt%H
3bO
3, 1.5wt%SrCO
3with 0.5wt% calglucon, 0.8wt%CeO
2.Carry out secondary ball milling with roller milling machine, be milled to the powder that median size is 0.64 μ m;
Be 380kA/m at alignment magnetic field, forming pressure is 10MPa, pressurize 10s, and being pressed into mean density is 3.34g/cm
3green compact.
Green compact are at 1155 DEG C in sintering temperature, and in atmospheric oxygen voltinism atmosphere, sintering obtains finished product in 2 hours, and temperature rise rate is 5 DEG C/min.
The prepared permanent-magnet ferrite product of the present embodiment is after testing: residual magnetization Br is 398.1mT; Magneticinduction coercive force H
cbfor 295.8kA/m; HCJ H
cjfor 356.3kA/m; Maximum magnetic energy product (BH)
maxfor 30.1kJ/m
3.
Embodiment 3
Press chemical structural formula Sr
1-xba
xonFe
(12-y)/nr
y/no
3(x=0.0, n=6.0, y=0.3, the composition requirement that R is Mn, taking industrial iron oxide red (purity is as 99.5%), Strontium carbonate powder (purity is as 99.05%), technical pure K
2mnO
4for raw material, carry out Primary batching system, and add 0.2wt%CaCO simultaneously
3, 0.3wt%SiO
2as an additive, with water, steel ball is according to material: the weight ratio of water: ball=1:1.5:15 is mixed, and carries out ball milling 2 hours, obtains the batch mixing that suspended particle median size is 1.0～1.5 μ m.
Batch mixing after filtration, after dry and granulation, pre-burning at 1290 DEG C, is incubated 3 hours, prepares M type permanent ferrite prefiring material sample piece;
In the preburning powdered material obtaining, add secondary additive subsequently after pulverizing, sieving, additive each component addition is as follows respectively with the preburning powdered material weight ratio that will add: 1.1wt%CaCO
3, 0.3wt%SiO
2, 0.05wt%MoO
3, 0.2wt%H
3bO
3, 1.5wt%SrCO
3with 0.5wt% calglucon, 0.7wt%, GeO
2.Carry out secondary ball milling with roller milling machine, be milled to the powder that median size is 0.65 μ m;
Be 380kA/m at alignment magnetic field, forming pressure is 10MPa, pressurize 12s, and being pressed into mean density is 3.44g/cm
3green compact.
Green compact are at 1185 DEG C in sintering temperature, and in atmospheric oxygen voltinism atmosphere, sintering obtains finished product in 2 hours, and temperature rise rate is 5 DEG C/min.
The prepared permanent-magnet ferrite product of the present embodiment is after testing: residual magnetization Br is 396.7mT; Magneticinduction coercive force H
cbfor 295.0kA/m; HCJ H
cjfor 362.7kA/m; Maximum magnetic energy product (BH)
maxfor 30.4kJ/m
3.
Embodiment 4
Press chemical structural formula Sr
1-xba
xonFe
(12-y)/nr
y/no
3(x=0.15, n=6.0, y=0.15, R is Mn, taking industrial iron oxide red (purity is as 99.5%), Strontium carbonate powder (purity is as 99.05%), barium carbonate and commercially pure K
2mnO
4for raw material, carry out Primary batching system, and add 0.2wt%CaCO simultaneously
3, 0.3wt%SiO
2as an additive, with water, steel ball is according to material: the weight ratio of water: ball=1:1.5:15 is mixed, and carries out ball milling 2 hours, obtains the batch mixing that suspended particle median size is 1.0～1.5 μ m.
Batch mixing after filtration, after dry and granulation, pre-burning at 1290 DEG C, is incubated 3 hours, prepares M type permanent ferrite prefiring material.
In the preburning powdered material obtaining, add secondary additive subsequently after pulverizing, sieving, additive each component addition is as follows respectively with the preburning powdered material weight ratio that will add: 1.1wt%CaCO
3, 0.3wt%SiO
2, 0.15wt%CeO
2, 0.2wt%H
3bO
3, 1.5wt%SrCO
3with 0.5wt% calglucon, 0.3wt%, MnO
2.Carry out secondary ball milling with roller milling machine, be milled to the powder that median size is 0.64 μ m.
Be 380kA/m at alignment magnetic field, forming pressure is 8MPa, pressurize 12s, and being pressed into mean density is 3.14g/cm
3green compact.
Green compact are at 1185 DEG C in sintering temperature, and in atmospheric oxygen voltinism atmosphere, sintering obtains finished product in 2 hours, and temperature rise rate is 5 DEG C/min.
The prepared permanent-magnet ferrite product of the present embodiment is after testing: residual magnetization Br is 392.5mT; Magneticinduction coercive force H
cbfor 292.4kA/m; HCJ H
cjfor 373.0kA/m; Maximum magnetic energy product (BH)
maxfor 30.4kJ/m
3.
Claims (3)
1. from preparation and the sintering of oxygen supply permanent ferrite prefiring material single aperture blank, it is characterized in that: described permanent-magnet ferrite material is hexaplanar, its chemical structural formula is Sr
1-xba
xonFe
(12-y)/nr
y/no
3, wherein 0≤x≤0.998,5.75≤n≤6.15,0<y≤0.6, R is Mn; Its concrete preparation method comprises the following steps:
(1) batch mixing: press chemical structural formula Sr
1-xba
xonFe
(12-y)/nr
y/no
3composition requirement, after mixing with the corresponding oxidation raw material of contained component and carbonate raw material powder, complete Primary batching system, and once add and account for added raw material (Sr
1-xba
xonFe
(12-y)/nr
y/no
3moiety summation) weight ratio be respectively the SiO of 0.1～1.0wt%
2, the CaCO of 0.1～1.0wt%
3; With water, steel ball is according to material: the weight ratio of water: ball=1:1.5:15 is mixed, and carries out ball milling 1～4 hour, and obtaining suspended particle median size is the batch mixing of 1.0 μ m～1.5 μ m;
(2) pre-burning: through filtering, after dry and granulation, carry out pre-burning at 1150～1350 DEG C, soaking time 1～8 hour, prepares permanent ferrite prefiring material by gained batch mixing in step (1);
(3) powder process: by prepared permanent ferrite prefiring material in step (2), utilize pulverizer fragmentation, cross 120 mesh sieves, obtain permanent ferrite prefiring powder;
(4) secondary ball milling: the CaCO by the permanent ferrite prefiring powder of preparation in step (3) with the secondary additive 0.1～1.8wt% that will add
3, 0.1～1.0wt% SiO
2, 0.1～1.0wt% H
3bO
3, 0.1～2.0wt% SrCO
3, the calglucon of 0.1～1.0wt%, the K of 0.1～1.0wt%
2mnO
4, with water, steel ball is still according to material: the weight ratio of water: ball=1:1.5:15 is mixed, and carries out secondary ball milling, obtains the slip that suspended particle median size is 0.50～1.00 μ m; The diameter of institute's employing steel ball is respectively 3mm, 4mm, 5mm, and weight proportion is 1:1:1;
(5) compacting green compact: according to actual operation requirements, control the size of mold shape, suppress green compact in alignment magnetic field>=380kA/m, forming pressure is 6～12MPa, and pressurize 10～20s is pressed into density > 3.6g/cm
3center single aperture right cylinder green compact;
(6) sintering: the green compact in step (5) are incubated to 30 minutes at 650 DEG C, at 1130～1250 DEG C, carry out sintering in atmospheric oxygen voltinism atmosphere subsequently, soaking time is 1～6 hour, and temperature rise rate is 5 DEG C/min;
(7) grinding and measurement: the magnetic patch that is cooled to room temperature after sintering is cut and grinding, test, measure according to GB/T3217-92 national standard.
2. a kind of high-performance permanent magnetic ferrite material according to claim 1 and preparation method thereof, is characterized in that: the oxide raw material described in step (1) comprises Fe
2o
3, Fe
3o
4, K
2mnO
4, carbonate raw material comprises SrCO
3and BaCO
3; And be industrial pure material.
3. a kind of high-performance permanent magnetic ferrite material according to claim 1 and preparation method thereof, is characterized in that: the secondary additive in step (4) also comprises commercially pure oxide compound CeO
2, GeO
2, MnO
2one or more, oxide compound (CeO
2, GeO
2, MnO
2one or more) total amount to account for Preburning material weight ratio be 0.01～10.0wt%.
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|---|---|---|---|---|
| CN104817319A (en) * | 2015-04-17 | 2015-08-05 | 南通万宝实业有限公司 | Magnetic powder |
| CN106083023A (en) * | 2016-06-23 | 2016-11-09 | 中钢天源(马鞍山)通力磁材有限公司 | The preparation method of a kind of high mechanical properties strontium ferrite magnet and product |
| CN106145917A (en) * | 2016-06-23 | 2016-11-23 | 南京航空航天大学 | A kind of coercitive secondary of permanently magnetic strontium ferrite that improves is combined adding method |
| CN107573055A (en) * | 2017-10-23 | 2018-01-12 | 安徽中磁高科有限公司 | The processing method of magneto magnetic material |
| CN111892961A (en) * | 2020-07-31 | 2020-11-06 | 日照钢铁控股集团有限公司 | Fuel additive for sintering process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104817319A (en) * | 2015-04-17 | 2015-08-05 | 南通万宝实业有限公司 | Magnetic powder |
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| CN107573055A (en) * | 2017-10-23 | 2018-01-12 | 安徽中磁高科有限公司 | The processing method of magneto magnetic material |
| CN111892961A (en) * | 2020-07-31 | 2020-11-06 | 日照钢铁控股集团有限公司 | Fuel additive for sintering process |
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Application publication date: 20140806 |