CN110342923A - 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 - Google Patents
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 Download PDFInfo
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Abstract
The invention belongs to permanent-magnet ferrite material technical fields.The invention discloses a kind of dry-pressing opposite sex ferrite fines preparation methods for improving the degree of orientation and performance, its by raw material preparation, prepare Preburning material, secondary ball milling, sieving molding, tempering and etc. form, it is provided with high tempering processing, the granule-morphology of optimization dry-pressing fine powder makes easy to form, simultaneously by tempering process and the optimization to main formula, the dry-pressing opposite sex ferrite fines with more high level cadre's piezo-remanent magnetization are obtained;The invention also discloses a kind of dry-pressing opposite sex permanent-magnet ferrite, the dry-pressing opposite sex ferrite fines as made from the dry-pressing opposite sex ferrite fines preparation method of above-mentioned the raising degree of orientation and performance are made after molding and sintering;It especially has higher dry-pressing remanent magnetism with better magnetic property.
Description
Technical field
The present invention relates to permanent-magnet ferrite technical field, the dry-pressing more particularly, to a kind of raising degree of orientation and performance is anisotropic
Ferrite fines preparation method and dry-pressing opposite sex permanent-magnet ferrite.
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 by the production practices of decades.But with wet
Pressure pressing under magnetic field compares, drymagnetic shaping is high with shaping efficiency, shrinking percentage is small, product size is easy to control, qualification rate is high,
Have a wide range of application, the features such as product shape is diversified;High-performance drymagnetic shaping permanent-magnet ferrite is usually used in making various rulers
Very little smaller, in irregular shape, complex-shaped and various extremely radial oriented magnetic devices.But for dry-pressing opposite sex ferrite
For magnet, due to using dry-pressing formed, because there is no medium mitigation to lead to drymagnetic shaping its degree of orientation not between particle
And Wet-pressing molding and blank situations such as cracking is easy to happen after high temperature sintering, therefore its magnetic property will be wetter than same class
Die pressing product is slightly lower, and the dry pressure formed permanent-magnet ferrite for preparing also is caused to be somewhat limited in actual production.
Chinese patent publication No. CN105384434A discloses a kind of system of dry-pressing permanent-magnet ferrite on March 9th, 2016
Method is made, to cause magnetic powder in mould for there are the reason of stress and air gap on magnetic powder particle surface after the dispersion of passing technology high temperature
Blank has that crack influences yield rate after filling insufficient and then influence orientation and subsequent forming in tool type chamber, is directed to
Additive improves, and increase tempering process optimization magnetic powder particle pattern, improve to a certain extent magnetic powder at
The degree of orientation during type, but its that still there is the degrees of orientation is still not high enough, it is magnetic to be finally sintered permanent-magnet ferrite obtained
Can still there be no small gap in performance with the permanent-magnet ferrite of Wet-pressing molding.
Wang Yingquan, Teng Yangmin of northern mine magnetic material etc. delivered entitled " La- on " magnetic material and device " impurity in 2015
The development of Ca-Sr-Co series high-performance pressed Anisotropic permanent-magnet ferrite " text, wherein analyzing secondary additive and bonding
The influence of agent, lubricant to dry-pressing permanent-magnet ferrite magnetic property that define suitable secondary additive formula and binder, adds
Add the adding manner and additive amount of agent, favorable orientation can finally be made and has and traditional strontium permanent ferrite wet pressure magnet
Higher magnetic property, but the improved method actually mentioned in this article finally permanent-magnet ferrite obtained remanent magnetism performance still
Can not still there be certain gap compared with the permanent-magnet ferrite that Wet-pressing molding obtains.
Summary of the invention
To solve the above-mentioned problems, the present invention provides one kind to prepare high-orientation and high performance dry-pressing opposite sex iron
The dry-pressing opposite sex ferrite fines preparation method of oxysome fine powder;
The present invention also provides a kind of dry-pressing opposite sex permanent-magnet ferrites being prepared by above-mentioned dry-pressing opposite sex ferrite fines.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of dry-pressing opposite sex ferrite fines preparation method improving the degree of orientation and performance, comprising the following steps:
A) raw material preparation: main phase Sr is pressed(1-x-y)Ca(x)La(y)Fe(2n-z)Co(z)O19Stoichiometric ratio prepare Fe2O3、CaCO3、
La2O3、Co2O3And SrCO3, wherein 5.5≤n≤5.8,0.1≤x≤0.3,0.3≤y≤0.5,0.2≤z≤0.4;
B) prepare Preburning material: will preparation raw material mix after carry out wet ball grinding, pressure forming after drying, then 1200~
It is sintered 40~80 minutes at 1300 DEG C and pre- burning block is made, pre- burning block crushed, Preburning material is made;
C) SiO of 0.2~0.5wt% secondary ball milling: is added into Preburning material based on Preburning material weight2, 0.5~1.5wt%
CaCO3With the boric acid of 0.1~0.3wt%, then slurry is made in ball-milling treatment, and slurry is dried to obtain material block;
D) sieving molding: material block obtained, which is crushed, and crosses 10~30 meshes is made Magnaglo, then presses Magnaglo weight
Meter adds the camphor of 1.3~1.7wt% and the calcium stearate of 0.5~0.7wt% thereto, be stirred, smash it through 50~
Ferrite powder is made in 65 meshes;
E) tempering: by dry-pressing opposite sex ferrite powder at 150~200 DEG C tempering, be made dry-pressing opposite sex ferrite
Fine powder.
The additive amount for increasing strontium element in main phase of the present invention makes that the Preburning material with rich strontium phase, superfluous strontium oxide strontia is made
The growth that can promote main phase grain in Preburning material synthesis process can be improved consistency, and then improve magnetic property.
Preferably, in step a) raw material preparation, Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size
≤1.5μm;CaCO3Purity >=98.5wt%, average particle size≤1.0 μm;La2O3Purity >=99.3wt%, average particle size≤
5μm;Co2O3Original mean particle≤3 μm;SrCO3Purity >=97wt%, original mean particle≤1.5 μm.
The purity of control raw material reduces being mixed into for impurity, while controlling raw material particle size and providing just for subsequent mixing and crushing
Benefit.
Preferably, step b) is prepared in Preburning material, the average particle size of particle is 0.7~0.8 μm after wet ball grinding, pressure
Pressure is 9~11MPa when molding, and the average grain diameter of the Preburning material obtained after crushing is 3~5 μm.
The partial size of particle can enhance the mobility of the particle in forming process after control particle and crushing, can also be conducive to magnetic
Curvature of field line.
Preferably, making within ball-milling treatment 9~16 hours 0.75~0.95 μ of average grain diameter that slurry is made in step c)
m。
By the particle size control of fine powder at 0.8~0.95 μm, particle size is too small to easily lead to subsequent product cracking, reduces
Yield rate, and particle size is excessive easily causes product consistency obtained low, influences the magnetic property of product.
Preferably, expecting that the moisture content of block is not higher than 0.3wt% after drying in step c).
Preferably, in step d), camphor and calcium stearate are the powder of preparatory 60 mesh of mistake.
Camphor and calcium stearate pulverize and sieve in advance, preferably can uniformly mix with main phase and secondary additive, sufficiently divide
It dissipates, and enough can guarantee that both good binder and additive can be played the role of during subsequent forming.
Preferably, the time of tempering is 50~70 minutes in step e).
A kind of dry-pressing opposite sex permanent-magnet ferrite, by the dry-pressing opposite sex ferrite fines of above-mentioned the raising degree of orientation and performance
Dry-pressing opposite sex ferrite fines made from preparation method are made after molding and sintering;Sintering process when sintering is first 300
~500 DEG C of progress degumming process, are then sintered 50~90 minutes at 1200~1300 DEG C, are cooled to room temperature later.
Preferably, briquetting pressure is 0.9~1.1MPa when molding, forming magnetic field is 7000~11000Oe.
Preferably, heating rate is 120~180 DEG C/h when sintering, cooling rate is 120~180 DEG C/h;Degumming process
Time is 40~80 minutes.
Using lower heating and cooling rate, can crack to avoid the product as caused by too fast alternating temperature etc. influence at
The problem of product rate.
Therefore, the invention has the following advantages:
(1) fine powder made from dry-pressing opposite sex ferrite fines preparation method has excellent granule-morphology through the invention, is easy to
Field curve, while can also improve the magnetic property of final products;
(2) the dry-pressing opposite sex permanent-magnet ferrite in the present invention is made by above-mentioned dry-pressing opposite sex ferrite fines, and the degree of orientation is close
The Ferrite Material as made from Wet-pressing molding, and its magnetic property with higher, remanent magnetism performance especially with higher.
Specific embodiment
Further description of the technical solution of the present invention With reference to embodiment.
Obviously, the described embodiments are merely a part of the embodiments of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, all other reality obtained by those of ordinary skill in the art without making creative efforts
Example is applied, shall fall within the protection scope of the present invention.
In the present invention, if not refering in particular to, all equipment and raw material is commercially available or the industry is common,
Method in following embodiments is unless otherwise instructed conventional method in that art.
Embodiment 1
A kind of dry-pressing opposite sex ferrite fines preparation method improving the degree of orientation and performance, comprising the following steps:
A) raw material preparation: main phase Sr is pressed0.38Ca0.12La0.5Fe10.7Co0.3O19Stoichiometric ratio prepare Fe2O3、CaCO3、
La2O3、Co2O3And SrCO3;Wherein Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size≤1.5 μm;CaCO3
Purity >=98.5wt%, average particle size≤1.0 μm;La2O3Purity >=99.3wt%, average particle size≤5 μm;Co2O3Original
Beginning average particle size≤3 μm;SrCO3Purity >=97wt%, original mean particle≤1.5 μm;
B) it prepares Preburning material: being carried out wet ball grinding 5 hours after the raw material of preparation is mixed, the average particle size of particle after wet ball grinding
It is 0.75 μm, with the pressure forming of 10MPa after drying, is then sintered 60 minutes at 1250 DEG C and pre- burning block is made, by pre- burning block
It crushes and Preburning material is made, the average grain diameter of the Preburning material obtained after crushing is 3~5 μm;
C) SiO of 0.2wt% secondary ball milling: is added into Preburning material based on Preburning material weight2, 0.55wt% CaCO3With
Then the boric acid of 0.10wt% makes the slurry that 0.80 μm of average grain diameter is made for ball-milling treatment 16 hours, slurry is dried to obtain
Moisture content is not higher than the material block of 0.3wt%;
D) sieving molding: material block obtained, which is crushed, and crosses 10~30 meshes is made Magnaglo, then presses Magnaglo weight
Count the camphor and preparatory 60 mesh of mistake of 0.5~0.7wt% for adding the powder of preparatory 60 mesh of mistake of 1.3~1.7wt% thereto
The calcium stearate of powder is stirred, smashes it through the obtained ferrite powder of 50~65 meshes;
E) tempering: by dry-pressing opposite sex ferrite powder at 150 DEG C tempering 60 minutes, be made dry-pressing opposite sex ferrite
Fine powder.
A kind of dry-pressing opposite sex permanent-magnet ferrite, by the dry-pressing opposite sex ferrite fines of above-mentioned the raising degree of orientation and performance
Dry-pressing opposite sex ferrite fines made from preparation method are made after molding and sintering;When molding briquetting pressure be 0.9~
1.1MPa, forming magnetic field are 7000~11000Oe;Sintering process when sintering is first in 300~500 DEG C of progress degumming process 60
Minute, be then warming up at 1200~1300 DEG C with the heating rate of 150 DEG C/h and keep the temperature 50~90 minutes, later with 150 DEG C/
The cooling rate of h is cooled to room temperature.
Embodiment 2
A kind of dry-pressing opposite sex ferrite fines preparation method improving the degree of orientation and performance, comprising the following steps:
A) raw material preparation: main phase Sr is pressed0.4Ca0.3La0.3Fe10.86Co0.4O19Stoichiometric ratio prepare Fe2O3、CaCO3、La2O3、
Co2O3And SrCO3;Wherein Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size≤1.5 μm;CaCO3Purity
>=98.5wt%, average particle size≤1.0 μm;La2O3Purity >=99.3wt%, average particle size≤5 μm;Co2O3It is original average
Granularity≤3 μm;SrCO3Purity >=97wt%, original mean particle≤1.5 μm;
B) it prepares Preburning material: carrying out wet ball grinding after the raw material of preparation is mixed, the average particle size of particle is 0.7 after wet ball grinding
~0.8 μm, with the pressure forming of 9~11MPa after drying, obtained pre-burning in 40~80 minutes is then sintered at 1200~1300 DEG C
Pre- burning block is crushed and Preburning material is made by block, and the average grain diameter of the Preburning material obtained after crushing is 3~5 μm;
C) SiO of 0.3wt% secondary ball milling: is added into Preburning material based on Preburning material weight2, 0.8wt% CaCO3With
Then the boric acid of 0.2wt% makes the slurry that 0.90 μm of average grain diameter is made for ball-milling treatment 12 hours, slurry is dried and is contained
Water rate is not higher than the material block of 0.3wt%;
D) sieving molding: material block obtained, which is crushed, and crosses 10~30 meshes is made Magnaglo, then presses Magnaglo weight
Count the camphor and preparatory 60 mesh of mistake of 0.5~0.7wt% for adding the powder of preparatory 60 mesh of mistake of 1.3~1.7wt% thereto
The calcium stearate of powder is stirred, smashes it through the obtained ferrite powder of 50~65 meshes;
E) tempering: by dry-pressing opposite sex ferrite powder, after sixty minutes, dry-pressing opposite sex iron oxygen is made in tempering at 180 DEG C
Body fine powder.
A kind of dry-pressing opposite sex permanent-magnet ferrite, by the dry-pressing opposite sex ferrite fines of above-mentioned the raising degree of orientation and performance
Dry-pressing opposite sex ferrite fines made from preparation method are made after molding and sintering;When molding briquetting pressure be 0.9~
1.1MPa, forming magnetic field are 7000~11000Oe;Sintering process when sintering is first in 300~500 DEG C of progress degumming process 60
Minute, be then warming up at 1200~1300 DEG C with the heating rate of 150 DEG C/h and keep the temperature 50~90 minutes, later with 150 DEG C/
The cooling rate of h is cooled to room temperature.
Embodiment 3
A kind of dry-pressing opposite sex ferrite fines preparation method improving the degree of orientation and performance, comprising the following steps:
A) raw material preparation: main phase Sr is pressed0.4Ca0.2La0.4Fe11.38Co0.22O19Stoichiometric ratio prepare Fe2O3、CaCO3、
La2O3、Co2O3And SrCO3;Wherein Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size≤1.5 μm;CaCO3
Purity >=98.5wt%, average particle size≤1.0 μm;La2O3Purity >=99.3wt%, average particle size≤5 μm;Co2O3Original
Beginning average particle size≤3 μm;SrCO3Purity >=97wt%, original mean particle≤1.5 μm;
B) it prepares Preburning material: carrying out wet ball grinding after the raw material of preparation is mixed, the average particle size of particle is 0.7 after wet ball grinding
~0.8 μm, with the pressure forming of 9~11MPa after drying, obtained pre-burning in 40~80 minutes is then sintered at 1200~1300 DEG C
Pre- burning block is crushed and Preburning material is made by block, and the average grain diameter of the Preburning material obtained after crushing is 3~5 μm;
C) SiO of 0.5wt% secondary ball milling: is added into Preburning material based on Preburning material weight2, 1.4wt% CaCO3With
Then the boric acid of 0.3wt% makes the slurry that 0.95 μm of average grain diameter is made for ball-milling treatment 9 hours, slurry is dried and is contained
Water rate is not higher than the material block of 0.3wt%;
D) sieving molding: material block obtained, which is crushed, and crosses 10~30 meshes is made Magnaglo, then presses Magnaglo weight
Count the camphor and preparatory 60 mesh of mistake of 0.5~0.7wt% for adding the powder of preparatory 60 mesh of mistake of 1.3~1.7wt% thereto
The calcium stearate of powder is stirred, smashes it through the obtained ferrite powder of 50~65 meshes;
E) tempering: by dry-pressing opposite sex ferrite powder at 200 DEG C tempering 60 minutes, be made dry-pressing opposite sex ferrite
Fine powder.
A kind of dry-pressing opposite sex permanent-magnet ferrite, by the dry-pressing opposite sex ferrite fines of above-mentioned the raising degree of orientation and performance
Dry-pressing opposite sex ferrite fines made from preparation method are made after molding and sintering;When molding briquetting pressure be 0.9~
1.1MPa, forming magnetic field are 7000~11000Oe;Sintering process when sintering is first in 300~500 DEG C of progress degumming process 60
Minute, be then warming up at 1200~1300 DEG C with the heating rate of 150 DEG C/h and keep the temperature 50~90 minutes, later with DEG C/h
Cooling rate is cooled to room temperature.
Embodiment 4
A kind of dry-pressing opposite sex ferrite fines preparation method improving the degree of orientation and performance, comprising the following steps:
A) raw material preparation: main phase Sr is pressed0.4Ca0.1La0.5Fe10.8Co0.2O19Stoichiometric ratio prepare Fe2O3、CaCO3、La2O3、
Co2O3And SrCO3;Wherein Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size≤1.5 μm;CaCO3Purity
>=98.5wt%, average particle size≤1.0 μm;La2O3Purity >=99.3wt%, average particle size≤5 μm;Co2O3It is original average
Granularity≤3 μm;SrCO3Purity >=97wt%, original mean particle≤1.5 μm;
B) it prepares Preburning material: carrying out wet ball grinding after the raw material of preparation is mixed, the average particle size of particle is 0.7 after wet ball grinding
μm, it with the pressure forming of 9MPa after drying, is then sintered 40 minutes at 1200 DEG C and pre- burning block is made, pre- burning block is crushed and is made
Preburning material, the average grain diameter of the Preburning material obtained after crushing are 3 μm;
C) SiO of 0.2wt% secondary ball milling: is added into Preburning material based on Preburning material weight2, 0.5wt% CaCO3With
Then the boric acid of 0.1wt% makes the slurry that 0.75 μm of average grain diameter is made for ball-milling treatment 9 hours, slurry is dried and is contained
Water rate is not higher than the material block of 0.3wt%;
D) sieving molding: material block obtained is crushed and crosses the obtained Magnaglo of 10 meshes, then based on Magnaglo weight to
The calcium stearate of the camphor of the powder of preparatory 60 mesh of mistake of 1.3wt% and the powder of preparatory 60 mesh of mistake of 0.5wt% is wherein added,
It is stirred, smashes it through the obtained ferrite powder of 50 meshes;
E) tempering: by dry-pressing opposite sex ferrite powder at 150 DEG C tempering 50 minutes, be made dry-pressing opposite sex ferrite
Fine powder.
A kind of dry-pressing opposite sex permanent-magnet ferrite, by the dry-pressing opposite sex ferrite fines of above-mentioned the raising degree of orientation and performance
Dry-pressing opposite sex ferrite fines made from preparation method are made after molding and sintering;Briquetting pressure is 0.9MPa when molding, at
Type magnetic field is 7000Oe;Sintering process when sintering be first 300 DEG C progress degumming process 40 minutes, then with 120 DEG C/h's
Heating rate is warming up at 1200 DEG C and keeps the temperature 50 minutes, is cooled to room temperature later with the cooling rate of 120 DEG C/h.
Embodiment 5
A kind of dry-pressing opposite sex ferrite fines preparation method improving the degree of orientation and performance, comprising the following steps:
A) raw material preparation: main phase Sr is pressed0.2Ca0.3La0.5Fe11.2Co0.4O19Stoichiometric ratio prepare Fe2O3、CaCO3、La2O3、
Co2O3And SrCO3;Wherein Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size≤1.5 μm;CaCO3Purity
>=98.5wt%, average particle size≤1.0 μm;La2O3Purity >=99.3wt%, average particle size≤5 μm;Co2O3It is original average
Granularity≤3 μm;SrCO3Purity >=97wt%, original mean particle≤1.5 μm;
B) it prepares Preburning material: carrying out wet ball grinding after the raw material of preparation is mixed, the average particle size of particle is 0.8 after wet ball grinding
μm, it with the pressure forming of 11MPa after drying, is then sintered 80 minutes at 1300 DEG C and pre- burning block is made, pre- burning block is crushed and is made
Preburning material is obtained, the average grain diameter of the Preburning material obtained after crushing is 5 μm;
C) SiO of 0.5wt% secondary ball milling: is added into Preburning material based on Preburning material weight2, 1.5wt% CaCO3With
Then the boric acid of 0.3wt% makes the slurry that 0.95 μm of average grain diameter is made for ball-milling treatment 16 hours, slurry is dried and is contained
Water rate is not higher than the material block of 0.3wt%;
D) sieving molding: material block obtained is crushed and crosses the obtained Magnaglo of 30 meshes, then based on Magnaglo weight to
The calcium stearate of the camphor of the powder of preparatory 60 mesh of mistake of 1.7wt% and the powder of preparatory 60 mesh of mistake of 0.7wt% is wherein added,
It is stirred, smashes it through the obtained ferrite powder of 65 meshes;
E) tempering: by dry-pressing opposite sex ferrite powder at 200 DEG C tempering 70 minutes, be made dry-pressing opposite sex ferrite
Fine powder.
A kind of dry-pressing opposite sex permanent-magnet ferrite, by the dry-pressing opposite sex ferrite fines of above-mentioned the raising degree of orientation and performance
Dry-pressing opposite sex ferrite fines made from preparation method are made after molding and sintering;Briquetting pressure is 1.1MPa when molding, at
Type magnetic field is 11000Oe;Sintering process when sintering be first 500 DEG C progress degumming process 80 minutes, then with 180 DEG C/h's
Heating rate is warming up at 1300 DEG C and keeps the temperature 90 minutes, is cooled to room temperature later with the cooling rate of 180 DEG C/h.
Comparative example 1
This comparative example BMS-12 Preburning material is dry-pressing powder base-material, in terms of dry-pressing powder base-material, 0.80wt%CaCO3, 0.50wt%
SiO2, 0.50wt% (La2O3+CoO3) it is secondary additive, 0.8wt% camphor and 0.6wt% calcium stearate is added;After mixing
It forms under 8000Oe forming magnetic field and is sintered 2 hours at 1215 DEG C, sample is made in furnace cooling.
Comparative example 2
Particle is crushed to 1.0 μm using Y38 Preburning material as dry-pressing powder base-material by this comparative example, then adds dry-pressing powder base-material
Stearic acid, 1.2wt% alcohol camphor solution and the 0.2wt% talcum powder of 0.6wt% is uniformly mixed, and in 80 DEG C of temperings 1
Hour, it is formed in 8000Oe forming magnetic field, briquetting pressure 8MPa, obtains green body, green body is kept the temperature 2 hours at 370 DEG C and is taken off
Calcium stearate, then in 1200 DEG C of heat preservations, 1 hour obtained sample.
Comparative example 3
The BMS-9.2 Preburning material of mine magnetic material is wet pressing base-material to the north of this comparative example, then adds wet pressing base-material 0.8wt%'s
CaCO3, 0.3wt% Cr2O3, 0.2wt% boric acid, 0.4wt%SiO2, the slurry of 30~40wt% of water content is made after ball milling,
Slurry average particle size is 0.83 micron, and forms under 2MPa briquetting pressure, 8000Oe forming magnetic field and green compact are made, will be obtained
Green compact keep the temperature 1 hour at 1235 DEG C, and sample is made.
Comparative example 4
A kind of dry-pressing opposite sex ferrite fines preparation method improving the degree of orientation and performance, comprising the following steps:
A) raw material preparation: main phase Sr is pressed0.4La0.6Fe10.3Co0.5O19Stoichiometric ratio prepare Fe2O3、La2O3、Co2O3With
SrCO3;Wherein Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size≤1.5 μm;La2O3Purity >=
99.3wt%, average particle size≤5 μm;Co2O3Original mean particle≤3 μm;SrCO3Purity >=97wt%, original average grain
≤ 1.5 μm of degree;
B) it prepares Preburning material: carrying out wet ball grinding after the raw material of preparation is mixed, the average particle size of particle is 0.7 after wet ball grinding
~0.8 μm, with the pressure forming of 9~11MPa after drying, obtained pre-burning in 40~80 minutes is then sintered at 1200~1300 DEG C
Pre- burning block is crushed and Preburning material is made by block, and the average grain diameter of the Preburning material obtained after crushing is 3~5 μm;
C) SiO of 0.15wt% secondary ball milling: is added into Preburning material based on Preburning material weight2With the CaCO of 0.4wt%3, so
Make within ball-milling treatment 20 hours the slurry that 0.76 μm of average grain diameter is made afterwards, dries the slurry to obtain moisture content and be not higher than
The material block of 0.3wt%;
D) sieving molding: material block obtained, which is crushed, and crosses 10~30 meshes is made Magnaglo, then presses Magnaglo weight
Count the camphor and preparatory 60 mesh of mistake of 0.5~0.7wt% for adding the powder of preparatory 60 mesh of mistake of 1.3~1.7wt% thereto
The calcium stearate of powder is stirred, smashes it through the obtained dry-pressing opposite sex ferrite fines of 50~65 meshes.
A kind of dry-pressing opposite sex permanent-magnet ferrite, by the dry-pressing opposite sex ferrite fines of above-mentioned the raising degree of orientation and performance
Dry-pressing opposite sex ferrite fines made from preparation method are made after molding and sintering;When molding briquetting pressure be 0.9~
1.1MPa, forming magnetic field are 7000~11000Oe;Sintering process when sintering is first in 300~500 DEG C of progress degumming process 60
Minute, be then warming up at 1200~1300 DEG C with the heating rate of 150 DEG C/h and keep the temperature 50~90 minutes, later with 150 DEG C/
The cooling rate of h is cooled to room temperature.
Comparative example 5
A kind of dry-pressing opposite sex ferrite fines preparation method improving the degree of orientation and performance, comprising the following steps:
A) raw material preparation: main phase Sr is pressed0.45Ca0.35La0.2Fe11.7Co0.1O19Stoichiometric ratio prepare Fe2O3、CaCO3、
La2O3、Co2O3And SrCO3;Wherein Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size≤1.5 μm;CaCO3
Purity >=98.5wt%, average particle size≤1.0 μm;La2O3Purity >=99.3wt%, average particle size≤5 μm;Co2O3Original
Beginning average particle size≤3 μm;SrCO3Purity >=97wt%, original mean particle≤1.5 μm;
B) it prepares Preburning material: carrying out wet ball grinding after the raw material of preparation is mixed, the average particle size of particle is 0.7 after wet ball grinding
~0.8 μm, with the pressure forming of 9~11MPa after drying, obtained pre-burning in 40~80 minutes is then sintered at 1200~1300 DEG C
Pre- burning block is crushed and Preburning material is made by block, and the average grain diameter of the Preburning material obtained after crushing is 3~5 μm;
C) SiO of 0.6wt% secondary ball milling: is added into Preburning material based on Preburning material weight2, 2.0wt% CaCO3With
Then the boric acid of 0.4wt% makes the slurry that 0.97 μm of average grain diameter is made for ball-milling treatment 7 hours, slurry is dried and is contained
Water rate is not higher than the material block of 0.3wt%;
D) sieving molding: material block obtained, which is crushed, and crosses 10~30 meshes is made Magnaglo, then presses Magnaglo weight
Count the camphor and preparatory 60 mesh of mistake of 0.5~0.7wt% for adding the powder of preparatory 60 mesh of mistake of 1.3~1.7wt% thereto
The calcium stearate of powder is stirred, smashes it through the obtained dry-pressing opposite sex ferrite fines of 50~65 meshes.
A kind of dry-pressing opposite sex permanent-magnet ferrite, by the dry-pressing opposite sex ferrite fines of above-mentioned the raising degree of orientation and performance
Dry-pressing opposite sex ferrite fines made from preparation method are made after molding and sintering;When molding briquetting pressure be 0.9~
1.1MPa, forming magnetic field are 7000~11000Oe;Sintering process when sintering is first in 300~500 DEG C of progress degumming process 60
Minute, be then warming up at 1200~1300 DEG C with the heating rate of 150 DEG C/h and keep the temperature 50~90 minutes, later with 150 DEG C/
The cooling rate of h is cooled to room temperature.
Performance test:
Will as above-described embodiment 1~5 and dry-pressing opposite sex permanent-magnet ferrite made from comparative example 1~5 through it is two-sided it is parallel grind it is laggard
The magnetic property such as following table institute of row magnetism testing, above-described embodiment 1~5 and the obtained dry-pressing opposite sex permanent-magnet ferrite of comparative example 1~5
Show.
Br/Gs | Hcb/Oe | Hcj/Oe | (BH)max/MGOe | |
Embodiment 1 | 4262 | 4010 | 4371 | 4.497 |
Embodiment 2 | 4275 | 3995 | 4352 | 4.533 |
Embodiment 3 | 4246 | 4011 | 4393 | 4.459 |
Embodiment 4 | 4273 | 4005 | 4360 | 4.518 |
Embodiment 5 | 4269 | 4008 | 4368 | 4.486 |
Comparative example 1 | 4190 | 3718 | 4522 | 4.170 |
Comparative example 2 | 4205 | 3506 | 3635 | 4.300 |
Comparative example 3 | 4242 | 3856 | 4368 | 4.395 |
Comparative example 4 | 4107 | 3834 | 4388 | 4.211 |
Comparative example 5 | 4201 | 3847 | 4343 | 4.378 |
By above-described embodiment 1~5 it is known that (as increased after being optimized to the formula of Preburning material compared with comparative example 1
Content of strontium etc.) and tempering is carried out to powder after adding secondary additive can effectively improve the magnetic property of permanent magnet,
Especially improve the remanent magnetism and intrinsic coercivity of magnet;
Compared with comparative example 2 it is known that on the basis of adjusting formula, carries out high tempering and handle at compared to lonneal
Reason, can make the granule-morphology of fine powder more excellent, be easy to magnetic field orientating, and then obtain the coercivity of permanent magnet and intrinsic coercivity
Huge raising;
It is known that pressing ferritic property by the ferritic performance of dry-pressing produced by the present invention and conventional wet compared with comparative example 3
Can be similar, and it is better than conventional wet weight oxysome in partial properties;
It is known that having adjusted component in main phase, secondary additive component and will be corresponding in the present invention compared with comparative example 4,5
Constituent content controls in OK range, and optimal dry-pressing permanent-magnet ferrite can be made.
It should be understood that those skilled in the art, can be improved or be become according to the above description
It changes, and all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (10)
1. a kind of dry-pressing opposite sex ferrite fines preparation method for improving the degree of orientation and performance, it is characterised in that including following step
It is rapid:
A) raw material preparation: main phase Sr is pressed(1-x-y)Ca(x)La(y)Fe(2n-z)Co(z)O19Stoichiometric ratio prepare Fe2O3、CaCO3、
La2O3、Co2O3And SrCO3, wherein 5.5≤n≤5.8,0.1≤x≤0.3,0.3≤y≤0.5,0.2≤z≤0.4;
B) prepare Preburning material: will preparation raw material mix after carry out wet ball grinding, pressure forming after drying, then 1200~
It is sintered 40~80 minutes at 1300 DEG C and pre- burning block is made, pre- burning block crushed, Preburning material is made;
C) SiO of 0.2~0.5wt% secondary ball milling: is added into Preburning material based on Preburning material weight2, 0.5~1.5wt%
CaCO3With the boric acid of 0.1~0.3wt%, then slurry is made in ball-milling treatment, and slurry is dried to obtain material block;
D) sieving molding: material block obtained, which is crushed, and crosses 10~30 meshes is made Magnaglo, then presses Magnaglo weight
Meter adds the camphor of 1.3~1.7wt% and the calcium stearate of 0.5~0.7wt% thereto, is stirred, smashes it through 50~65
Ferrite powder is made in mesh;
E) tempering: by dry-pressing opposite sex ferrite powder at 150~200 DEG C tempering, be made dry-pressing opposite sex ferrite
Fine powder.
2. a kind of dry-pressing opposite sex ferrite fines preparation method for improving the degree of orientation and performance according to claim 1,
It is characterized in that:
In the step a) raw material preparation, Fe2O3Purity >=99.3wt%, Cl-≤ 0.1wt%, average particle size≤1.5 μm;CaCO3
Purity >=98.5wt%, average particle size≤1.0 μm;La2O3Purity >=99.3wt%, average particle size≤5 μm;Co2O3It is original
Average particle size≤3 μm;SrCO3Purity >=97wt%, original mean particle≤1.5 μm.
3. a kind of preparation method of dry-pressing opposite sex ferrite fines for improving the degree of orientation and performance according to claim 1,
It is characterized by:
The step b) is prepared in Preburning material, and the average particle size of particle is 0.7~0.8 μm after wet ball grinding, and when pressure forming presses
Power is 9~11MPa, and the average grain diameter of the Preburning material obtained after crushing is 3~5 μm.
4. a kind of preparation method of dry-pressing opposite sex ferrite fines for improving the degree of orientation and performance according to claim 1,
It is characterized by:
In the step c), make within ball-milling treatment 9~16 hours 0.75~0.95 μm of average grain diameter that slurry is made.
5. a kind of preparation side of dry-pressing opposite sex ferrite fines for improving the degree of orientation and performance according to claim 1 or 4
Method, it is characterised in that:
In the step c), expect that the moisture content of block is not higher than 0.3wt% after drying.
6. a kind of preparation method of dry-pressing opposite sex ferrite fines for improving the degree of orientation and performance according to claim 1,
It is characterized by:
In the step d), camphor and calcium stearate are the powder of preparatory 60 mesh of mistake.
7. a kind of preparation method of dry-pressing opposite sex ferrite fines for improving the degree of orientation and performance according to claim 1,
It is characterized by:
In the step e), the time of tempering is 50~70 minutes.
8. a kind of dry-pressing opposite sex permanent-magnet ferrite, it is characterised in that:
Its by claim 1~7 any the raising degree of orientation and performance dry-pressing opposite sex ferrite fines preparation method system
The dry-pressing opposite sex ferrite fines obtained are made after molding and sintering;The sintering process when sintering is first at 300~500 DEG C
Degumming process is carried out, is then sintered 50~90 minutes at 1200~1300 DEG C, is cooled to room temperature later.
9. a kind of dry-pressing opposite sex permanent-magnet ferrite according to claim 8, it is characterised in that:
When the molding, briquetting pressure is 0.9~1.1MPa, and forming magnetic field is 7000~11000 Oe.
10. a kind of dry-pressing opposite sex permanent-magnet ferrite according to claim 8, it is characterised in that:
Heating rate is 120~180 DEG C/h when the sintering, and cooling rate is 120~180 DEG C/h;The degumming process time is 40
~80 minutes.
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