CN109836147A - A kind of permanent-magnet ferrite and preparation method thereof - Google Patents
A kind of permanent-magnet ferrite and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to permanent-magnet ferrite material technical fields, to solve the problems, such as traditional permanent-magnet ferrite material dependent on higher Co additive amount, at high cost, provide a kind of permanent-magnet ferrite and preparation method thereof, on the basis of permanent-magnet ferrite gross mass, the permanent-magnet ferrite is made of the Sr series ferrite material and 45wt% and Ca series ferrite material below of 55wt% or more;The Sr series ferrite material has Sr1‑xLaxFe3+ 2n‑yCoyO19Ferrite main phase;The Ca series ferrite material has Cax(Sr+Ba)yLa1‑x‑yFe3+ 2n‑ zCozO19Ferrite main phase.After the present invention passes through secondary ball milling, forming and sintering by two or more Preburning materials with different ferrite masters point, it is compounded to form a kind of material of new ferrite main phase;The additive amount for reducing Co simultaneously, obtains optimal magnetic property and cost performance.Preparation process is easy to operate, to equipment without particular/special requirement, is easy to large-scale industrial production.
Description
Technical field
The present invention relates to permanent-magnet ferrite material technical fields more particularly to a kind of permanent-magnet ferrite and preparation method thereof.
Background technique
As the permanent-magnet material being formed of oxide, well known M type (Magnetoplumbate-type) Sr ferrite for having hexagonal crystal system.Closely
Year, as electronic component develops towards miniaturization, high performance, for permanent-magnet ferrite material, also require high-performance.One
As for, permanent-magnet ferrite by addition lanthanum Co-substituted can be with substantially improving performance, especially new-energy automobile ternary material
The price of cobalt type oxide has been raised in the rapid development of material, leads to Ferrite Material cost increase.Therefore, how to reduce Co's
Additive amount, while excellent magnetic property is obtained, it is the research and development focus of current high performance magnetic material.
Summary of the invention
The present invention is in order to overcome the problems, such as that traditional permanent-magnet ferrite material dependent on higher Co additive amount, at high cost, provides
A kind of permanent-magnet ferrite being compounded to form by two or more different ferrite main phases, while reducing the additive amount of Co,
Obtain optimal magnetic property and cost performance.
The present invention also provides a kind of preparation methods of permanent-magnet ferrite, and this method is easy to operate, want to equipment without special
It asks, is easy to large-scale industrial production.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of permanent-magnet ferrite, which is characterized in that on the basis of permanent-magnet ferrite gross mass, the permanent-magnet ferrite is by 55wt%
Or more Sr series ferrite material and 45wt% and Ca series ferrite material below composition;The Sr series ferrite material tool
There is Sr1-xLaxFe3+ 2n-yCoyO19Ferrite main phase;The Ca series ferrite material has Cax(Sr+Ba)yLa1-x-yFe3+ 2n- zCozO19Ferrite main phase.
Preferably, in the Sr series ferrite material: 0.1≤x≤0.4,0.05≤y≤0.35,5.8≤n≤6.1.
Preferably, on the basis of the amount of Ca series ferrite material total material, oxygen corresponding to the Ca series ferrite material
The additive amount of compound are as follows: Fe2O380~90mol%, CaCO33.0~6.2mol%, La2O32.5~5.5mol% and Co2O3
1.8~3.4mol%, surplus BaCO3And/or SrCO3;Wherein 5.0≤n≤5.5.
A kind of preparation method of permanent-magnet ferrite, which comprises the following steps:
(1) it prepares Sr series ferrite material: weighing Fe according to said ratio2O3, La2O3, Co2O3And SrCO3It is primary to carry out wet process
Ball milling obtains the first slurry, the drying of the first slurry, precompressed processing, pre-burning is obtained the first Preburning material, then by the first Preburning material through dry type
Coarse crushing processing, obtains Sr series ferrite material;
(2) it prepares Ca series ferrite material: weighing Fe according to said ratio2O3, CaCO3, La2O3, Co2O3, SrCO3And BaCO3,
Grinding agent is added, carries out ball milling of wet process and obtains the second slurry, the drying of the second slurry, precompressed processing, pre-burning are obtained into the second pre-burning
Material;The second Preburning material is handled through dry type coarse crushing again, obtains Ca series ferrite material;
(3) according to said ratio, Ca system iron made from Sr series ferrite material made from step (1) and step (2) is weighed respectively
Ferrite, while adding SiO2、CaCO3, calcium gluconate mixture put into ball mill, Ball-milling Time control 20~
30h, then add deionized water and ground as ball-milling medium, obtain mixing slurry;
(4) step (3) slurry obtained that mixes is subjected to centrifugal dehydration, compression moulding obtains formed body;
(5) temperature at 100~600 DEG C is heat-treated formed body, is then sintered in air atmosphere to get permanent magnetism
Ferrite.
The present invention passes through secondary ball milling, forming and sintering by two or more Preburning materials with different ferrite masters point
Afterwards, it is compounded to form a kind of material of new ferrite main phase;The additive amount for reducing Co simultaneously, obtains optimal magnetic property and sexual valence
Than.
Preferably, the time of ball milling of wet process controls in 5~10h in step (1);The granularity of first slurry
Control is at 0.05~0.6 μm;The pressure of precompressed processing is controlled in 5~10MPa;Calcined temperature is controlled at 1200~1250 DEG C;Institute
The size controlling of Sr series ferrite material is stated at 2.0~3.0 μm.
Preferably, the time of ball milling of wet process controls in 5~10h in step (2);The granularity of second slurry
Control is at 0.05~0.6 μm;The pressure of precompressed processing is controlled in 5~10MPa;Calcined temperature is controlled at 1250~1300 DEG C;Institute
The size controlling of Ca series ferrite material is stated at 2.0~3.0 μm.
Preferably, the size controlling for mixing slurry is at 0.5~0.7 μm in step (3).
Preferably, the concentration of the mixing slurry after centrifugal dehydration is 50~70wt% in step (4).
Preferably, the magnetic field of compression moulding is controlled in 14000~15000Oe in step (4).
Preferably, in step (5), heating rate is 100~150 DEG C/h in sintering process, sintering temperature is 1200~
1210 DEG C, sintering time is controlled in 70~90min.
Preferably, the grinding agent is boric acid in step (2), additive amount of the boric acid in mixed raw material is 0.1
~0.2wt%.
Therefore, the invention has the following beneficial effects: pass through two or more Preburning materials with different ferrite masters point
After secondary ball milling, forming and sintering, it is compounded to form a kind of material of new ferrite main phase;The additive amount of Co is reduced simultaneously,
Obtain optimal magnetic property and cost performance.Preparation process is easy to operate, to equipment without particular/special requirement, is easy to large-scale industry metaplasia
It produces.
Specific embodiment
Below by specific embodiment, the technical solutions of the present invention will be further described.
In the present invention, if not refering in particular to, all devices and raw material is commercially available or the industry is common are following
Method in embodiment is unless otherwise instructed conventional method in that art.
Embodiment 1
(1) Sr series ferrite material is prepared: according to Sr0.6La0.4Fe11.6Co0.3O19Ferrite main phase proportion weighs Fe2O3(purity
>=99.3wt%, Cl-≤ 0.1wt%, original mean particle≤1.5 μm of particle), La2O3(purity >=99.3wt%, particle
Original mean particle≤5 μm), Co2O3(Co content >=72wt%, original mean particle≤3 μm of particle) and SrCO3(purity >=
97wt%, original mean particle≤1.5 μm of particle) carry out ball milling of wet process obtain the first slurry, the granularity control of the first slurry
System at 0.56 μm, Ball-milling Time 10h, by the drying of the first slurry, under 10Mpa pressure precompressed processing, then in air atmosphere
1230 DEG C of pre-burnings obtain the first Preburning material, then the first Preburning material is handled through dry type coarse crushing, obtain the Sr system that average grain diameter is 2.5 μm
Ferrite Material;
(2) Ca series ferrite material is prepared: according to Sr0.1Ba0.06Ca0.38La0.46Fe9.92Co0.28O19Proportion weighs Fe2O3(purity
>=99.3wt%, Cl-≤ 0.1wt%, original mean particle≤1.5 μm of particle), CaCO3(purity >=98.5wt%, particle
Original mean particle≤1.0 μm), La2O3(purity >=99.3wt%, original mean particle≤5um of particle), Co2O3(Co contains
Amount >=72wt%, original mean particle≤3 μm of particle), SrCO3(purity >=97wt%, the original mean particle of particle≤
1.5 μm) and BaCO3(purity >=97wt%, original mean particle≤1.5 μm of particle), be added addition 0.2wt% boric acid as
Grinding agent carries out ball milling of wet process and obtains the first slurry, and Ball-milling Time 10h, the granularity of the second slurry is 0.55 μm, by the second material
Slurry drying, precompressed is handled, then 1260 DEG C of pre-burnings obtain the second Preburning material in air atmosphere under 10Mpa pressure;Again by second
Preburning material is handled through dry type coarse crushing, obtains the Ca series ferrite material that average grain diameter is 2.0 μm;
(3) according to said ratio, Ca made from Sr series ferrite material 250g made from step (1) and step (2) is weighed respectively
Series ferrite material 250g, while adding 2.25g SiO2、8.03g CaCO3, 5.0g calcium gluconate mixture put into ball
Grinding machine, Ball-milling Time is controlled in 30h, then is added 1000mL deionized water and ground as ball-milling medium, and obtaining partial size is 0.63 μ
The mixing slurry of m;
(4) the obtained slurry that mixes of step (3) being subjected to centrifugal dehydration, the concentration of slurry is adjusted to 65wt%, compression moulding,
Pressing direction applies the forming magnetic field of 14000Oe, obtains formed body;Gained formed body is that diameter is 43.2mm, is highly 13mm
Cylindrical body, briquetting pressure 5MPa;
(5) 500 DEG C at a temperature of formed body is heat-treated, organic dispersing agent is completely removed, then in air atmosphere
It is sintered, heating rate is 150 DEG C/h, in 1210 DEG C of heat preservation 90min to get permanent-magnet ferrite.
Embodiment 2
(1) Sr series ferrite material is prepared: according to Sr0.6La0.4Fe11.6Co0.3O19Ferrite main phase proportion weighs Fe2O3(purity
>=99.3wt%, Cl-≤ 0.1wt%, original mean particle≤1.5 μm of particle), La2O3(purity >=99.3wt%, particle
Original mean particle≤5 μm), Co2O3(Co content >=72wt%, original mean particle≤3 μm of particle) and SrCO3(purity >=
97wt%, original mean particle≤1.5 μm of particle) carry out ball milling of wet process obtain the first slurry, the granularity control of the first slurry
System at 0.6 μm, Ball-milling Time 10h, by the drying of the first slurry, under 8Mpa pressure precompressed processing, then in air atmosphere
1200 DEG C of pre-burnings obtain the first Preburning material, then the first Preburning material is handled through dry type coarse crushing, obtain the Sr system that average grain diameter is 3.0 μm
Ferrite Material;(2) Ca series ferrite material is prepared: according to Sr0.1Ba0.06Ca0.38La0.46Fe9.92Co0.28O19Ferrite main phase
Proportion weighs Fe2O3(purity >=99.3wt%, Cl-≤ 0.1wt%, original mean particle≤1.5 μm of particle), CaCO3It is (pure
Degree >=98.5wt%, original mean particle≤1.0 μm of particle), La2O3(purity >=99.3wt%, the original average grain of particle
Degree≤5um), Co2O3(Co content >=72wt%, original mean particle≤3 μm of particle), SrCO3(purity >=97wt%, particle
Original mean particle≤1.5 μm) and BaCO3(purity >=97wt%, original mean particle≤1.5 μm of particle), addition adds
Add 0.2wt% boric acid as grinding agent, carries out ball milling of wet process and obtain the first slurry, Ball-milling Time 10h, the granularity of the second slurry
It is 0.6 μm, by the drying of the second slurry, precompressed is handled, then 1300 DEG C of pre-burnings obtain second in air atmosphere under 5Mpa pressure
Preburning material;The second Preburning material is handled through dry type coarse crushing again, obtains the Ca series ferrite material that average grain diameter is 2.8 μm;
(3) according to said ratio, Ca made from Sr series ferrite material 250g made from step (1) and step (2) is weighed respectively
Series ferrite material 250g, while adding 2.25g SiO2、8.03g CaCO3, 5.0g calcium gluconate mixture put into ball
Grinding machine, Ball-milling Time is controlled in 2h, then is added 1000mL deionized water and ground as ball-milling medium, and obtaining partial size is 0.66 μm
Mixing slurry;
(4) the obtained slurry that mixes of step (3) being subjected to centrifugal dehydration, the concentration of slurry is adjusted to 70wt%, compression moulding,
Pressing direction applies the forming magnetic field of 15000Oe, obtains formed body;Gained formed body is that diameter is 43.2mm, is highly 13mm
Cylindrical body, briquetting pressure 5MPa;
(5) temperature at 600 DEG C is heat-treated formed body, completely removes organic dispersing agent, then in air atmosphere into
Row sintering, heating rate is 100 DEG C/h, in 1200 DEG C of heat preservation 70min to get permanent-magnet ferrite.
Embodiment 3
(1) Sr series ferrite material is prepared: according to Sr0.6La0.4Fe11.6Co0.3O19Ferrite main phase proportion weighs Fe2O3(purity
>=99.3wt%, Cl-≤ 0.1wt%, original mean particle≤1.5 μm of particle), La2O3(purity >=99.3wt%, particle
Original mean particle≤5 μm), Co2O3(Co content >=72wt%, original mean particle≤3 μm of particle) and SrCO3(purity >=
97wt%, original mean particle≤1.5 μm of particle) carry out ball milling of wet process obtain the first slurry, the granularity control of the first slurry
System is at 0.45 μm, Ball-milling Time 10h, and by the drying of the first slurry, precompressed is handled, then in air atmosphere under 5~10Mpa pressure
In 1240 DEG C of pre-burnings obtain the first Preburning material, then the first Preburning material is handled through dry type coarse crushing, obtains the Sr that average grain diameter is 2.0 μm
Series ferrite material;
(2) Ca series ferrite material is prepared: according to Sr0.1Ba0.06Ca0.38La0.46Fe9.92Co0.28O19Ferrite main phase proportion claims
Take Fe2O3(purity >=99.3wt%, Cl-≤ 0.1wt%, original mean particle≤1.5 μm of particle), CaCO3(purity >=
98.5wt%, original mean particle≤1.0 μm of particle), La2O3(purity >=99.3wt%, original mean particle≤5 of particle
μm), Co2O3(Co content >=72wt%, original mean particle≤3 μm of particle), SrCO3(purity >=97wt%, the original of particle
Beginning average particle size≤1.5 μm) and BaCO3Addition is added in (purity >=97wt%, original mean particle≤1.5 μm of particle)
0.1wt% boric acid carries out ball milling of wet process and obtains the first slurry, Ball-milling Time 10h, the granularity of the second slurry is as grinding agent
0.05~0.6 μm, by the drying of the second slurry, under 5~10Mpa pressure precompressed processing, then in air atmosphere 1250 DEG C it is pre-
Burn to obtain the second Preburning material;The second Preburning material is handled through dry type coarse crushing again, obtains the Ca based ferrite material that average grain diameter is 2.0 μm
Material;
(3) according to said ratio, Ca made from Sr series ferrite material 250g made from step (1) and step (2) is weighed respectively
Series ferrite material 250g, while adding 2.25g SiO2、8.03g CaCO3, 5.0g calcium gluconate mixture put into ball
Grinding machine, Ball-milling Time is controlled in 25h, then is added 1000mL deionized water and ground as ball-milling medium, and obtaining partial size is 0.67 μ
The mixing slurry of m;
(4) the obtained slurry that mixes of step (3) being subjected to centrifugal dehydration, the concentration of slurry is adjusted to 50wt%, compression moulding,
Pressing direction applies the forming magnetic field of 14500Oe, obtains formed body;Gained formed body is that diameter is 43.2mm, is highly 13mm
Cylindrical body, briquetting pressure 5MPa;
(5) temperature at 450 DEG C is heat-treated formed body, completely removes organic dispersing agent, then in air atmosphere into
Row sintering, heating rate is 120 DEG C/h, in 1205 DEG C of heat preservation 80min to get permanent-magnet ferrite.
Comparative example 1
(1) Sr series ferrite material 500g made from 1 step of embodiment (1) is weighed, while adding 2.5gSiO2、6.0g
CaCO3, 5g calcium gluconate mixture put into ball mill, then add 1000mL deionized water and ground as ball-milling medium
It grinds, milling time 30h, the slurry average particle size after ball milling is 0.62 μm;
(2) slurry is subjected to centrifugal dehydration, the concentration of slurry is adjusted to 65wt%, and compression moulding applies in pressing direction
The forming magnetic field of 14000Oe, obtains formed body;Gained formed body is that diameter is 43.2mm, is highly the cylindrical body of 13mm, molding pressure
Power is 5MPa;
(3) 500 DEG C at a temperature of formed body is heat-treated, organic dispersing agent is completely removed, then in air atmosphere
It is sintered, heating rate is 150 DEG C/h, in 1210 DEG C of heat preservation 90min to get permanent-magnet ferrite.
Comparative example 2
(1) Ca series ferrite material 500g made from 1 step of embodiment (2) is weighed, while adding 2.25g SiO2、9.25g
CaCO3, 5g calcium gluconate mixture put into ball mill, then add 1000mL deionized water and ground as ball-milling medium
It grinds, milling time 30h, the slurry average particle size after ball milling is 0.62 μm;
(2) slurry is subjected to centrifugal dehydration, the concentration of slurry is adjusted to 65wt%, and compression moulding applies in pressing direction
The forming magnetic field of 14000Oe, obtains formed body;Gained formed body is that diameter is 43.2mm, is highly the cylindrical body of 13mm, molding pressure
Power is 5MPa;
(3) 500 DEG C at a temperature of formed body is heat-treated, organic dispersing agent is completely removed, then in air atmosphere
It is sintered, heating rate is 150 DEG C/h, in 1210 DEG C of heat preservation 90min to get permanent-magnet ferrite.
The upper and lower surface of permanent-magnet ferrite made from embodiment 1-3 and comparative example 1,2 is ground respectively, measures its remanence
Induction (Br), coercivity (Hcb), intrinsic coercivity (Hcj), maximum magnetic energy product (BH) max, the results are shown in Table 1:
1. testing result of table
Number | Br(Gs) | Hcb(Oe) | Hcj(Oe) | (BH)max |
Embodiment 1 | 4450 | 3950 | 5360 | 4.56 |
Embodiment 2 | 4480 | 3980 | 5260 | 4.58 |
Embodiment 3 | 4468 | 3965 | 5285 | 4.62 |
Comparative example 1 | 4410 | 3920 | 4520 | 4.45 |
Comparative example 2 | 4490 | 4012 | 5320 | 4.62 |
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, without departing from power
There are also other variations and modifications under the premise of technical solution documented by benefit requirement.
Claims (10)
1. a kind of permanent-magnet ferrite, which is characterized in that on the basis of permanent-magnet ferrite gross mass, the permanent-magnet ferrite by
The Sr series ferrite material and 45wt% of 55wt% or more and Ca series ferrite material below composition;The Sr based ferrite
Material has Sr1-xLaxFe3+ 2n-yCoyO19Ferrite main phase;The Ca series ferrite material has Cax(Sr+Ba)yLa1-x-yFe3 + 2n-zCozO19Ferrite main phase.
2. a kind of permanent-magnet ferrite according to claim 1, which is characterized in that in the Sr series ferrite material: 0.1≤
x≤0.4、0.05≤y≤0.35、5.8≤n≤6.1。
3. a kind of permanent-magnet ferrite according to claim 1, which is characterized in that with the amount of Ca series ferrite material total material
On the basis of, the additive amount of oxide corresponding to the Ca series ferrite material are as follows: Fe2O380~90mol%, CaCO33.0~
6.2mol%, La2O32.5~5.5mol% and Co2O31.8~3.4mol%, surplus BaCO3And/or SrCO3;Wherein 5.0
≤n≤5.5。
4. a kind of preparation method of permanent-magnet ferrite a method according to any one of claims 1-3, which is characterized in that including following step
It is rapid:
(1) it prepares Sr series ferrite material: weighing Fe according to said ratio2O3, La2O3, Co2O3And SrCO3Carry out ball of wet process
The first slurry is ground to obtain, the drying of the first slurry, precompressed processing, pre-burning are obtained into the first Preburning material, then the first Preburning material is thick through dry type
Pulverization process obtains Sr series ferrite material;
(2) it prepares Ca series ferrite material: weighing Fe according to said ratio2O3, CaCO3, La2O3, Co2O3, SrCO3And BaCO3,
Grinding agent is added, carries out ball milling of wet process and obtains the first slurry, the drying of the second slurry, precompressed processing, pre-burning are obtained into the second pre-burning
Material;The second Preburning material is handled through dry type coarse crushing again, obtains Ca series ferrite material;
(3) according to said ratio, Ca system iron made from Sr series ferrite material made from step (1) and step (2) is weighed respectively
Ferrite, while adding SiO2、CaCO3, calcium gluconate mixture put into ball mill, then add deionized water conduct
Ball-milling medium is ground, and mixing slurry is obtained;
(4) step (3) slurry obtained that mixes is subjected to centrifugal dehydration, compression moulding obtains formed body;
(5) temperature at 100~600 DEG C is heat-treated formed body, is then sintered in air atmosphere to get permanent magnetism
Ferrite.
5. the preparation method of permanent-magnet ferrite according to claim 4, which is characterized in that in step (1), ball of wet process
The time of mill controls in 5~10h;The granularity of first slurry is controlled at 0.05~0.6 μm;The pressure control of precompressed processing exists
5~10MPa;Calcined temperature is controlled at 1200~1250 DEG C;The size controlling of the Sr series ferrite material is at 2.0~3.0 μm.
6. the preparation method of permanent-magnet ferrite according to claim 4, which is characterized in that in step (2), ball of wet process
The time of mill controls in 5~10h;The granularity of second slurry is controlled at 0.05~0.6 μm;The pressure control of precompressed processing exists
5~10MPa;Calcined temperature is controlled at 1250~1300 DEG C;The size controlling of the Ca series ferrite material is at 2.0~3.0 μm.
7. the preparation method of permanent-magnet ferrite according to claim 4, which is characterized in that in step (3), the blended stock
The size controlling of slurry is at 0.5~0.7 μm.
8. the preparation method of permanent-magnet ferrite according to claim 4, which is characterized in that in step (4), after centrifugal dehydration
Mixing slurry concentration be 50~70wt%;The magnetic field of compression moulding is controlled in 14000~15000Oe.
9. the preparation method of permanent-magnet ferrite according to claim 4, which is characterized in that in step (5), in sintering process
Heating rate is 100~150 DEG C/h, and sintering temperature is 1200~1210 DEG C, and sintering time is controlled in 70~90min.
10. the preparation method of permanent-magnet ferrite according to claim 4, which is characterized in that in step (2), the grinding
Agent is boric acid, and additive amount of the boric acid in mixed raw material is 0.1~0.2wt%.
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CN111362687A (en) * | 2019-12-17 | 2020-07-03 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite and preparation method thereof |
CN111704452A (en) * | 2020-05-22 | 2020-09-25 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite material and preparation method thereof |
CN111995385A (en) * | 2020-07-29 | 2020-11-27 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite material with high radial and axial shrinkage consistency and preparation method thereof |
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JP2007176757A (en) * | 2005-12-28 | 2007-07-12 | Tdk Corp | Method of manufacturing ferrite magnetic material |
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JP2007176757A (en) * | 2005-12-28 | 2007-07-12 | Tdk Corp | Method of manufacturing ferrite magnetic material |
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CN111362687A (en) * | 2019-12-17 | 2020-07-03 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite and preparation method thereof |
CN111704452A (en) * | 2020-05-22 | 2020-09-25 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite material and preparation method thereof |
CN111995385A (en) * | 2020-07-29 | 2020-11-27 | 横店集团东磁股份有限公司 | Permanent magnetic ferrite material with high radial and axial shrinkage consistency and preparation method thereof |
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