CN104496457A - Rare earth-containing permanent magnetic ferrite and manufacturing method thereof - Google Patents
Rare earth-containing permanent magnetic ferrite and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a rare earth-containing permanent magnetic ferrite with improved comprehensive magnetic properties and a manufacturing method thereof. The permanent magnetic ferrite mainly comprises: 75-90mass% of Fe2O3, 0.1-3mass% of CaCO3, 0.1-5mass% of La2O3, 0.1-3mass% of Co2O3, 0.1-6mass% of SrCO3, and 0.1-3mass% of BaCO3. The average particle size of the raw materials is required to be less than 5 micrometers. Specifically, the Fe2O3 in the permanent magnetic ferrite comes from ferric oxide raw material, and the ferric oxide raw material contains Mn with a content controlled less than 0.1mass%, the average size of permanent magnetic ferrite grains is about 1.2 micrometers, wherein 10% of the grains is less than 0.8 micromter, 10% of the grains is larger than 1.8 micrometers, the size of the rest grains is in the range, and the ratio of length to diameter is 1.2-2.5. Compared with the prior art, the ball milling process is improved at the same time of ion substitution in the invention, the particles of two particle size systems are mixed to coordinate with each other, and the prepared magnet has higher comprehensive magnetic performance.
Description
Technical field
The present invention relates to magneticsubstance correlative technology field, refer in particular to a kind of permanent-magnet ferrite containing rare earth and manufacture method thereof.
Background technology
As everyone knows, weigh permanent magnet material magnetic property and mainly comprise three parameters, i.e. residual flux density (Br), coercive force (magnetic strength coercivity H b and HCJ Hcj) and maximum magnetic energy product (BH) max, but the squareness recently as the parameter-demagnetizing curve of assessment permanent magnet material demagnetizing curve perfect condition comes into one's own increasingly, which characterizes the stability of magnet under dynamic operating condition.The squareness of so-called demagnetizing curve refers to Hk/Hcj, and wherein Hk is defined as the magneticstrength on permanent magnetism permanent magnet material J-H demagnetizing curve corresponding to 0.9Br.Theoretical investigation shows, the squareness major influence factors of permanent magnet material demagnetizing curve is the orientation degree of material main phase grain, and simultaneously the microstructure of material is also an important influence factor.In the actual fabrication process of material, every composition and engineering that can have influence on above-mentioned two improves the demagnetization curve rectangularity that all effectively can promote material.
M type permanent-magnet ferrite has good magnetic property, and cost performance is given prominence to, and is widely used in the fields such as an electric notor, sensor, stopper, office equipment, automobile motor, medical facilities.M type permanent-magnet ferrite is a kind of oxide compound with ferrimagnetism, and its composition and engineering is all relatively ripe, but has also occurred some new development in recent years, mainly comprises composition and engineering two aspect.
In formula, particularly compared with former permanent-magnet ferrite Patents, mainly add a certain amount of Ca element in main formula, and the comparision contents of corresponding La and Co is high; But because the interpolation of the restriction La-Co being subject to the conditions such as ion-conductance balance and lattice distortion is also conditional.Such as: China Patent Publication No. CN101552069A, described Br value is maximum when adding Ca in Sr-La-Co can increase about 100Gs, but squareness decline more, easily cause demagnetization in high temperature environments; Chinese Patent Application No. CN200810061540.5 makes mean particle size in slip increase remanent magnetism and coercive force below 0.5 μm by Ultrafine Grinding, but Ultrafine Grinding technique requires higher when production operation, be unsuitable for scale operation and add cost; Chinese Patent Application No. CN201310174549.8 adds coercive force by secondary additive, but causes remanent magnetism to decrease because introduced non-magnetic phase; Chinese Patent Application No. 201110153849.9 is mentioned and is introduced rare earth element to improve magnetic property in Fe position, but in the process of preparation, it is difficult that rare earth ion occupies exactly on Fe position.
At process aspect, patent WO/2008/105449 have employed the novel process of two sections of pulverizing and subsequent heat treatment, control the median size of material at 0.1 ~ 0.2 μm, but this technique is owing to having very low median size, is difficult to realize in actual production.
Summary of the invention
There is above-mentioned deficiency to overcome in prior art in the present invention, provides a kind of permanent-magnet ferrite containing rare earth and the manufacture method thereof of carrying high comprehensive magnetic properties.
To achieve these goals, the present invention is by the following technical solutions:
Containing a permanent-magnet ferrite for rare earth, the major ingredient of this permanent-magnet ferrite has Fe
2o
3content 75 ~ 90mass%, CaCO
3content 0.1 ~ 3mass%, La
2o
3content 0.1 ~ 5mass%, Co
2o
3content 0.1 ~ 3mass%, SrCO
3content 0.1 ~ 6mass%, BaCO
3content 0.1 ~ 3mass%, each raw material mean particle size requires below 5 μm.
As preferably, the Fe in described permanent-magnet ferrite
2o
3from raw iron oxide material, and containing Mn in raw iron oxide material, wherein Mn content controls at below 0.1mass%.By the content of impurity element Mn in controlled oxidization iron material, permanent-magnet ferrite comprehensive magnetic can be improved.
As preferably, described permanent-magnet ferrite average grain size is at about 1.2 μm, and wherein 10% crystal grain is less than 0.8 μm, 10% crystal grain is greater than 1.8 μm, and between, length-to-diameter ratio is 1.2 ~ 2.5 to the size of all the other crystal grain.
In addition, present invention also offers the manufacture method of the above-mentioned permanent-magnet ferrite containing rare earth, concrete operation step is as follows:
(1) prepare burden: according to each constituent mass, accurate weighing also mixes;
(2) ball millings: the raw material mixed is put into ball grinder ball milling 3 ~ 6 hours, rotating speed is 70r/min, and pellet water ratio is 1: 14: 1.5;
(3) pre-burning: the material dehvery pump mixed after above-mentioned ball milling is delivered to heating rotary kiln and carries out pre-burning, sintering temperature is 1150 ~ 1350 DEG C, soaking time 3 hours;
(4) secondary ball milling: above-mentioned Preburning material is fed into tuber grinder and carries out after dry type is ground into 4 ~ 6 μm of particles, take Preburning material, by secondary ball milling after the some required secondary additives of quality proportioning interpolation and additive, time is 16 hours, and the mean sizes of particle is about 0.8 ~ 1.1 μm; Weighed by above-mentioned quality proportioning by another part Preburning material and carry out secondary ball milling, the time is the mean sizes obtaining particle for 22 hours is about 0.6 ~ 0.8 μm; Two portions slip is mixed ball milling 0.5 hour;
(5) compression moulding: the slip water ratio obtaining above-mentioned steps is 30 ~ 40%, and then shaping in 10000Oe magnetic field, forming pressure is 3 ~ 10MPa, obtains formed body;
(6) sinter: base substrate is incubated 1 hour to remove moisture at 200 ~ 300 DEG C, then 1150 ~ 1350 DEG C of insulations 0.1 ~ 3 hour;
(7) aftertreatment: grinding, cleaning, detects.
In the present invention, by improving ball-milling technology, the particle of two kinds of particle diameter systems being mixed and works in coordination, make the magnet prepared have higher comprehensive magnetic energy.
As preferably, in the secondary ball milling technique of step (4), described secondary additive and additive have H
3bO
3, CaCO
3, SiO
2, Co
2o
3, dispersion agent, the weight percent that its each component accounts for major ingredient is the H of 0.1-0.3%
3bO
3, 0.6-2.6% CaCO
3, 0.4-0.8% SiO
2, 0-0.4% Co
2o
3, 0.5-0.7% dispersion agent.
As preferably, described dispersion agent is one or more combinations in maltose alcohol, hydroxyl isomaltulose, erythritol, Sorbitol Powder or calglucon.
As preferably, in the compression moulding technique of step (5), the formed body diameter obtained is 6cm, high 3cm.
As preferably, in the sintering process of step (6), while intensification, pass into the air containing 0.1-0.5% ozone, the speed that air passes into is 0.5-2m
3/ h.
As preferably, in the sintering process of step (6), its temperature rise rate is 150 DEG C/h.
As preferably, in the aftertreatment technology of step (7), obtain ferrite sintered magnet, after grinding cleaning, magnet is incubated 24 hours at 23 DEG C, and then detects.Improve the tolerance range detecting data.
The invention has the beneficial effects as follows: compare prior art and mainly contain the oxide compound adding La, Co, Ca; carry out the formula technique of substitutional ion and pursue minimizing of slip particle; the present invention improves ball-milling technology while carrying out substitutional ion; the particle of two kinds of particle diameter systems is mixed work in coordination, the magnet of preparation has higher comprehensive magnetic energy.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
The present inventor finds when the particle mean size of slip is below 1.1 μm in long-term practice, time shaping in the magnetic field of 10000Oe, orientation degree can reach about 98%, when mean sizes is reduced to 0.5 μm, orientation degree is substantially constant, and the squareness of magnet declines obviously.Below in conjunction with specific embodiment, technical scheme of the present invention is described further.
Embodiment 1:
Permanent-magnet ferrite major ingredient has Fe
2o
3content 85mass%, CaCO
3content 2.5mass%, La
2o
3content 4.5mass%, Co
2o
3content 2.5mass%, SrCO
3content 5.4mass%, BaCO
3content 0.1mass%, each raw material mean particle size requires below 5 μm, and gross weight is 250Kg.Put into ball grinder ball milling after having joined material 5 hours, rotating speed is 70r/min, and pellet water ratio is 1: 14: 1.5; The material dehvery pump mixed after above-mentioned ball milling is delivered to heating rotary kiln and carries out pre-burning, sintering temperature is 1250 DEG C, soaking time 3 hours; Preburning material is fed into tuber grinder to carry out after dry type is ground into 4 ~ 6 μm of particles, taking 100Kg Preburning material, add secondary ball milling after some required secondary additives and additive by quality proportioning, the time is 16 hours, and the mean sizes of particle is about 1.0 μm; Weighed by above-mentioned quality proportioning by another part Preburning material 100Kg and carry out secondary ball milling, the time is 22 hours, and the mean sizes obtaining particle is about 0.8 μm.Two portions slip is put together ball milling 0.5 hour, shaping in the magnetic field at 10000Oe when slurry dewatering is 30 ~ 40% to water ratio, forming pressure is 5MPa, and the diameter obtaining formed body is 6cm, high 3cm.Base substrate is incubated 1 hour to remove moisture at 250 DEG C, is warmed up to 1220 DEG C with 150 DEG C per hour, while heating up, pass into the air containing 0.1-0.5% ozone, the speed that air passes into is 0.5m
3/ h, then 1220 DEG C of insulations 1 hour.Obtain ferrite sintered magnet, after grinding cleaning, magnet is incubated 24 hours at 23 DEG C, then measure magnetic property and obtain Br=4640Gs, Hcb=4250Oe, Hcj=5550Oe, Hk/Hcj=95%, (BH) max=5.35MGOe.
Comparative example 1:
Permanent-magnet ferrite major ingredient has Fe
2o
3content 85mass%, CaCO
3content 2.5mass%, La
2o
3content 4.5mass%, Co
2o
3content 2.5mass%, SrCO
3content 5.4mass%, BaCO
3content 0.1mass%, each raw material mean particle size requires below 5 μm, and gross weight is 250Kg.Put into ball grinder ball milling after having joined material 5 hours, rotating speed is 70r/min, and pellet water ratio is 1: 14: 1.5; The material dehvery pump mixed after above-mentioned ball milling is delivered to heating rotary kiln and carries out pre-burning, sintering temperature is 1250 DEG C, 3 hours time; Preburning material is fed into tuber grinder to carry out after dry type is ground into 4 ~ 6 μm of particles, taking 100Kg Preburning material, add secondary ball milling after some required secondary additives and additive by quality proportioning, the time is 16 hours, and the mean sizes of particle is about 1.0 μm; Weighed by above-mentioned quality proportioning by another part Preburning material 100Kg and carry out secondary ball milling, the time is 22 hours, and the mean sizes obtaining particle is about 0.8 μm.Shaping in magnetic field at 10000Oe when slurry dewatering is 30 ~ 40% to water ratio, forming pressure is 5MPa, and the diameter obtaining molding is 6cm, high 3cm.Base substrate is incubated 1 hour to remove moisture at 250 DEG C, is warmed up to 1220 DEG C with 150 DEG C per hour, while heating up, pass into the air containing 0.1-0.5% ozone, the speed that air passes into is 0.5m
3/ h, then 1220 DEG C of insulations 1 hour.Obtain ferrite sintered magnet, after grinding cleaning, magnet is incubated 24 hours at 23 DEG C, then measures magnetic property.Be 16 hours when the secondary ball milling time, record Br=4650Gs, Hcb=4050Oe, Hcj=4800Oe, Hk/Hcj=98%, (BH) max=5.16MGOe; Be 22 hours when the secondary ball milling time, record Br=4620Gs, Hcb=3900Oe, Hcj=5650Oe, Hk/Hcj=88%, (BH) max=5.05MGOe.
The magnetic property of table 1 different process permanent-magnet ferrite
Table 1 is the magnetic property table of embodiment 1 and comparative example 1 gained magnet, and show excellent over-all properties by after 2 kinds of particle mixing as shown in Table 1, magnetic energy product is up to 5.35MGOe.And in comparative example 1-1, the particle size obtained for 16 hours due to secondary ball milling is larger, the size departing from single domain is larger, therefore the HCJ Hcj of gained magnet is less, but squareness Hk/Hcj now reaches 98%, carry out observation to the microtexture of this crystal grain further to find, now the length-to-diameter ratio of magnet crystal grain is 1.5 ~ 2.5.In comparative example 1-2, the particle size obtained for 22 hours due to secondary ball milling is less, and magnet easily obtains higher Hcj, and simultaneously because the fine particle of less than 0.2 μm increases, the reunion between them makes magnet remanent magnetism slightly reduce.Embodiment 1 combines the particle of two kinds of particle diameter systems, prepared magnet performance is superior, carry out observation to its microtexture can obtain, magnet average grain size is at about 1.2 μm, wherein 10% crystal grain is less than 0.8 μm, 10% crystal grain is greater than 1.8 μm, in between, length-to-diameter ratio is 1.2 ~ 2.5 to the size of all the other crystal grain.
Embodiment 2:
Choose 3 kinds of different ferric oxide, its composition is as shown in table 2, according to permanent-magnet ferrite major ingredient Fe
2o
3content 88mass%, CaCO
3content 1.6mass%, La
2o
3content 4.2mass%, Co
2o
3content 2mass%, SrCO
3content 4.1mass%, BaCO
3content 0.1mass%, each raw material mean particle size requires below 5 μm, obtains each 250Kg of compound.By the raw material that 3 kinds mix, put into ball grinder ball milling separately 3 hours, rotating speed is 70r/min, and pellet water ratio is 1: 14: 1.5; The material dehvery pump mixed after above-mentioned ball milling is delivered to heating rotary kiln and carries out pre-burning, sintering temperature is 1150 DEG C, 3 hours time; Preburning material is fed into tuber grinder to carry out after dry type is ground into 4 ~ 6 μm of particles, taking 100Kg Preburning material, add secondary ball milling after some required secondary additives and additive by quality proportioning, the time is 22 hours, and the mean sizes of particle is about 0.8 μm; Shaping in magnetic field at 10000Oe when slurry dewatering is 30 ~ 40% to water ratio, forming pressure is 3MPa, and the diameter obtaining molding is 6cm, high 3cm.Base substrate is incubated 1 hour to remove moisture at 250 DEG C, is warmed up to 1200 DEG C with 150 DEG C per hour, while heating up, pass into the air containing 0.1-0.5% ozone, the speed that air passes into is 2m
3/ h, then 1200 DEG C of insulations 1 hour.Obtain ferrite sintered magnet, measure magnetic property 23 DEG C of insulations after 24 hours after grinding cleaning as shown in table 3.
Table 2 raw iron oxide material component list
Permanent-magnet ferrite magnetic property prepared by the different raw iron oxide material of table 3
Execute the Fe used in routine 2-1,2-2,2-3
2o
3be respectively ferric oxide 1, ferric oxide 2, ferric oxide 3.By table 2 and table 3 known along with in ferric oxide impurity Mn content raise, magnet performance prepared by same process has very large difference.When in ferric oxide, Mn content is at 0.09mass%, the magnet performance obtained is best, Br=4648Gs, Hcb=4265Oe, Hcj=5500Oe, Hk/Hcj=96%, (BH) max=5.32MGOe; Along with in ferric oxide, Mn content is elevated to 0.38mass%, and Br, Hcb, Hcj etc. have decline.Its reason is because Mn is non-magnetic phase, and due to when La-Co combines replacement Co occupy 2a, 4f position, therefore Mn is present in grain boundaries or intra-die with the form of MnO in the case, therefore a small amount of Mn content is conducive to magnet and obtains high Hcj, squareness, and simultaneously Mn is excessive also easily causes non-magnetic phase to increase affecting Br and magnetocrystalline anisotropy.
Claims (10)
1., containing a permanent-magnet ferrite for rare earth, it is characterized in that, the major ingredient of this permanent-magnet ferrite has Fe
2o
3content 75 ~ 90mass%, CaCO
3content 0.1 ~ 3mass%, La
2o
3content 0.1 ~ 5mass%, Co
2o
3content 0.1 ~ 3mass%, SrCO
3content 0.1 ~ 6mass%, BaCO
3content 0.1 ~ 3mass%, each raw material mean particle size requires below 5 μm.
2. a kind of permanent-magnet ferrite containing rare earth according to claim 1, is characterized in that, the Fe in described permanent-magnet ferrite
2o
3from raw iron oxide material, and containing Mn in raw iron oxide material, wherein Mn content controls at below 0.1mass%.
3. a kind of permanent-magnet ferrite containing rare earth according to claim 1 and 2, it is characterized in that, described permanent-magnet ferrite average grain size is at about 1.2 μm, wherein 10% crystal grain is less than 0.8 μm, 10% crystal grain is greater than 1.8 μm, in between, length-to-diameter ratio is 1.2 ~ 2.5 to the size of all the other crystal grain.
4., as claimed in claim 1 containing a manufacture method for the permanent-magnet ferrite of rare earth, it is characterized in that, concrete operation step is as follows:
(1) prepare burden: according to each constituent mass, accurate weighing also mixes;
(2) ball millings: the raw material mixed is put into ball grinder ball milling 3 ~ 6 hours, rotating speed is 70r/min, and pellet water ratio is 1: 14: 1.5;
(3) pre-burning: the material dehvery pump mixed after above-mentioned ball milling is delivered to heating rotary kiln and carries out pre-burning, sintering temperature is 1150 ~ 1350 DEG C, soaking time 3 hours;
(4) secondary ball milling: above-mentioned Preburning material is fed into tuber grinder and carries out after dry type is ground into 4 ~ 6 μm of particles, take Preburning material, by secondary ball milling after the some required secondary additives of quality proportioning interpolation and additive, time is 16 hours, and the mean sizes of particle is about 0.8 ~ 1.1 μm; Weighed by above-mentioned quality proportioning by another part Preburning material and carry out secondary ball milling, the time is the mean sizes obtaining particle for 22 hours is about 0.6 ~ 0.8 μm; Two portions slip is mixed ball milling 0.5 hour;
(5) compression moulding: the slip water ratio obtaining above-mentioned steps is 30 ~ 40%, and then shaping in 10000Oe magnetic field, forming pressure is 3 ~ 10MPa, obtains formed body;
(6) sinter: base substrate is incubated 1 hour to remove moisture at 200 ~ 300 DEG C, then 1150 ~ 1350 DEG C of insulations 0.1 ~ 3 hour;
(7) aftertreatment: grinding, cleaning, detects.
5. the manufacture method of the permanent-magnet ferrite containing rare earth according to claim 4, it is characterized in that, in the secondary ball milling technique of step (4), described secondary additive and additive have H
3bO
3, CaCO
3, SiO
2, Co
2o
3, dispersion agent, the weight percent that its each component accounts for major ingredient is the H of 0.1-0.3%
3bO
3, 0.6-2.6% CaCO
3, 0.4-0.8% SiO
2, 0-0.4% Co
2o
3, 0.5-0.7% dispersion agent.
6. the manufacture method of the permanent-magnet ferrite containing rare earth according to claim 5, is characterized in that, described dispersion agent is one or more combinations in maltose alcohol, hydroxyl isomaltulose, erythritol, Sorbitol Powder or calglucon.
7. the manufacture method of the permanent-magnet ferrite containing rare earth according to claim 4, it is characterized in that, in the compression moulding technique of step (5), the formed body diameter obtained is 6cm, high 3cm.
8. the manufacture method of the permanent-magnet ferrite containing rare earth according to claim 4, is characterized in that, in the sintering process of step (6), while intensification, pass into the air containing 0.1-0.5% ozone, the speed that air passes into is 0.5-2m
3/ h.
9. the manufacture method of the permanent-magnet ferrite containing rare earth according to claim 4 or 8, it is characterized in that, in the sintering process of step (6), its temperature rise rate is 150 DEG C/h.
10. the manufacture method of the permanent-magnet ferrite containing rare earth according to claim 4, it is characterized in that, in the aftertreatment technology of step (7), obtain ferrite sintered magnet, after grinding cleaning, magnet is incubated 24 hours at 23 DEG C, and then detects.
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| CN105837193A (en) * | 2016-03-14 | 2016-08-10 | 安徽天宇磁业有限公司 | Ferrite and preparation method thereof |
| CN106116561A (en) * | 2016-06-28 | 2016-11-16 | 南通万宝实业有限公司 | Permanent-magnet ferrite magnetic material |
| CN106116560A (en) * | 2016-06-28 | 2016-11-16 | 南通万宝实业有限公司 | The preparation method of permanent-magnet ferrite magnetic material |
| CN107680770A (en) * | 2016-09-09 | 2018-02-09 | 杨甫进 | Soft magnetic ferrite green compact Carving Machining technique |
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| CN109836148A (en) * | 2019-02-22 | 2019-06-04 | 横店集团东磁股份有限公司 | One kind is without La, Co element permanent-magnet ferrite material and preparation method thereof |
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| CN105439551A (en) * | 2015-11-12 | 2016-03-30 | 海安南京大学高新技术研究院 | High-magnetic-energy-product La-Co codoped strontium ferrite magnetic powder and preparation method thereof |
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| CN109836148A (en) * | 2019-02-22 | 2019-06-04 | 横店集团东磁股份有限公司 | One kind is without La, Co element permanent-magnet ferrite material and preparation method thereof |
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| CN116102344A (en) * | 2023-02-10 | 2023-05-12 | 安徽万磁电子股份有限公司 | High-density permanent magnetic ferrite magnet and production process thereof |
| CN116102344B (en) * | 2023-02-10 | 2024-04-16 | 安徽万磁电子股份有限公司 | High-density permanent magnetic ferrite magnet and production process thereof |
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