CN113896522A - Permanent magnetic ferrite and preparation method thereof - Google Patents

Permanent magnetic ferrite and preparation method thereof Download PDF

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CN113896522A
CN113896522A CN202111340639.0A CN202111340639A CN113896522A CN 113896522 A CN113896522 A CN 113896522A CN 202111340639 A CN202111340639 A CN 202111340639A CN 113896522 A CN113896522 A CN 113896522A
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CN113896522B (en
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杨永花
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Shenzhen Xinyi Magnetic Material Co ltd
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Abstract

The invention discloses a permanent magnetic ferrite and a preparation method thereof, belonging to the technical field of semiconductor magnetic materials. The ferrite of the invention is prepared from the following raw materials in parts by weight: 130 portions of ferric oxide, 1.5 to 2.5 portions of strontium carbonate, 0.5 to 1 portion of lanthanum oxide, 3 to 6 portions of manganese oxide, 1 to 3 portions of calcium carbonate, 10 to 20 portions of boric acid, 3 to 5 portions of silicon dioxide and 0.5 to 1.5 portions of cobalt oxide. According to the invention, by reasonably adjusting the dosage proportion of La, Fe, Co and rare earth elements, the prepared permanent magnetic ferrite has excellent magnetic properties, and the magnetic accumulation can reach 62kJ/m at most3The intrinsic coercive force can reach 425.8kA/m, the residual magnetization can reach 599.6mT, the magnetic performance of the material is remarkably improved, and the comprehensive performance is excellent.

Description

Permanent magnetic ferrite and preparation method thereof
Technical Field
The invention belongs to the technical field of semiconductor magnetic materials, and particularly relates to a permanent magnetic ferrite and a preparation method thereof.
Background
The ferrite magnetic material is a non-metallic magnetic material of a composite oxide sintered body, and is generally divided into a soft magnetic ferrite and a permanent magnetic ferrite magnetic material.
The permanent magnetic ferrite magnetic material comprises barium ferrite and strontium ferrite, has high resistivity and belongs to a semiconductor type, so the eddy current loss is small, the coercive force is large, and the permanent magnetic ferrite magnetic material can be effectively applied to a magnetic circuit with a large air gap and is particularly suitable for being used as a permanent magnet of a small generator and a motor. The permanent magnetic ferrite magnetic material has rich raw material sources, uncomplicated process and low cost, thereby having higher cost performance and being widely applied to various high-power, high-rotating-speed and high-torque motors, such as high-grade automobile motors, motorcycle starting motors, household appliances, electric tool motors and other fields.
The final magnetic properties of permanent magnetic ferrites are generally measured by remanence (Br), intrinsic coercivity (HcJ). Among them, the high performance permanent magnetic ferrite generally means that the ferrite has higher residual magnetic induction and stronger demagnetization resistance. At present, in order to improve the magnetic performance of ferrite, the method is basically started from two aspects of raw material proportioning and preparation process optimization.
In terms of raw materials, the magnetic property is generally improved by doping rare earth elements and the like, and La3+-Co2+The substitution is proved to be a very effective method, which can greatly improve the intrinsic magnetic property of the material, thus being widely applied to the batch production of high-performance ferrite permanent magnetic materials. However, this method requires a large consumption of La and Co. As is well known, La belongs to rare earth elements and has a limited earth reserve; cobalt is a strategic resource, mainly produced in south america, africa and oceania, and is very expensive. Therefore, in the view of raw materials, the prior art basically changes the added elements with different components and different proportions to realize the improvement of material performance, but due to the limited and manufacturing cost, the magnetic performance is difficult to be greatly improved and the actual application and popularization are difficult to obtain, so that the application of the magnetic material in the semiconductor industry is hindered, and the innovation and the progress of the semiconductor technology cannot be promoted.
In the aspect of preparation process, the preparation process mainly influences the microstructure of the material, different synthetic methods are adopted, and the microstructure difference of the produced permanent magnetic ferrite has important influence on the coercive force. According to different preparation methods of ferrite magnetic powder, the production of the permanent magnetic ferrite can be divided into dry synthesis and wet synthesis. The dry synthesis method adopts oxides as raw materials, has poor activity and difficult complete reaction degree, but has simple process and more common application; the wet synthesis process is complex, but because the chemical activity of the raw materials is higher, the magnetic performance of the ferrite is better, and various industrial byproducts can be fully utilized, thereby being convenient for improving the quality and reducing the cost and having development prospect.
How to optimize the preparation process and optimize the material composition to realize the preparation of the ferrite material with low cost and high performance is a technical problem to be solved urgently in the field of the semiconductor magnetic material at present.
Disclosure of Invention
The invention aims to improve the magnetic performance of the permanent magnetic ferrite by adjusting the type proportion of the metal oxides and controlling the grain size and the particle size distribution of the ferrite so as to greatly improve the overall performance of the material.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
the permanent magnetic ferrite comprises the following raw materials in parts by weight: 130 portions of ferric oxide, 1.5 to 2.5 portions of strontium carbonate, 0.5 to 1 portion of lanthanum oxide, 3 to 6 portions of manganese oxide, 1 to 3 portions of calcium carbonate, 10 to 20 portions of boric acid, 3 to 5 portions of silicon dioxide and 0.5 to 1.5 portions of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 1-3h to obtain a premix;
(2) drying the premix obtained in the step (1), pre-sintering at the sintering temperature of 1200 ℃ and 1300 ℃ for 3-5h, and naturally cooling to obtain pre-sintered powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 10-13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, namely heating to 500 ℃ at a heating rate of 1-2 ℃/min and keeping the temperature for 1h, then heating to 1150-1200 ℃ at a heating rate of 5-8 ℃/min and keeping the temperature for 1-3h, and naturally cooling to obtain a finished product.
Preferably, the mass ratio of the raw materials, the water and the steel balls in the step (1) is 1:2:20, and the rotating speed is 80-100 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
Preferably, the addition amount of the organic auxiliary agent in the step (3) is 3% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, and the organic auxiliary agent is obtained by mixing dioctyl ester and vinyl trimethoxy silane according to the mass ratio of 1: 1.
Preferably, the ratio of the raw materials and the steel balls in the secondary ball milling in the step (3) is 1:20, and the ball milling rotating speed is 100-. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
The final magnetic properties of permanent magnetic ferrites are generally measured by remanence (Br), intrinsic coercivity (HcJ). Among them, the high performance permanent magnetic ferrite generally means that the ferrite has higher residual magnetic induction and stronger demagnetization resistance. The ferrite is produced by using iron oxide and carbonates of Sr or Ba as raw materials and by a powder metallurgy method. With the development of various motors towards light weight, miniaturization and high efficiency, higher requirements are put forward on the preparation process and performance of the permanent magnetic ferrite, the magnet is required to be smaller and smaller, and the comprehensive magnetic performance is higher. The doping substitution of rare earth elements such as La, La-Co, Ca-La-Co and the like can greatly improve the intrinsic property of the magnetic material. However, the coercive force HcJ and other properties are not only related to doping, but also related to the microstructure of the grains, and the average particle size and the particle size distribution after the powder is refined influence the morphology of the ferrite grains.
Therefore, the invention firstly adjusts the raw material composition, adds rare earth elements to improve the magnetic property, and replaces part of the rare earth elements with part of manganese oxide to reduce the addition of rare earth metals such as La-Co and the like; adding calcium carbonate and silicon dioxide in the secondary ball milling process to promote densification growth of the magnet in the sintering process, and simultaneously adding an organic auxiliary agent obtained by mixing dioctyl ester and vinyl trimethoxy silane according to the mass ratio of 1: 1; in the powder ball milling process, under the action of liquid bridge force, chemical 'hard' agglomeration can be generated among anisotropic permanent magnetic ferrite powder particles; in the subsequent drying process, the powder particles are physically 'soft' agglomerated under the action of van der Waals force and electrostatic force. The addition of the dioctyl ester can play a good role in lubricating and dispersing, and the vinyl trimethoxy silane is very easily adsorbed on the surface of solid particles, so that particle agglomeration is reduced, the dioctyl ester is cooperated with the dioctyl ester, the ball milling efficiency is improved, the particle size is reduced, the dioctyl ester and the vinyl trimethoxy silane are fully decomposed through programmed heating and sintering, microcracks are reduced, and the material density is improved.
Has the advantages that:
according to the invention, by reasonably adjusting the dosage ratio of La, Fe, Co and rare earth elements, the prepared permanent magnetic ferrite has excellent magnetic properties, the magnetic accumulation can be as high as 62kJ/m3, the intrinsic coercive force can be 425.8kA/m, the residual magnetization can be 599.6mT, the magnetic property of the material is obviously improved, and the comprehensive properties are excellent.
Drawings
FIG. 1 is a view showing the structure of a microstructure in example 3 of the present invention;
FIG. 2 is a graph comparing particle size distributions of example 3 of the present invention and comparative example 1.
Detailed Description
The technical solution of the present invention is further described below with reference to specific embodiments, but is not limited thereto.
Example 1
The permanent magnetic ferrite comprises the following raw materials in parts by weight: 100 parts of ferric oxide, 1.5 parts of strontium carbonate, 0.5 part of lanthanum oxide, 3 parts of manganese oxide, 1 part of calcium carbonate, 10 parts of boric acid, 3 parts of silicon dioxide and 0.5 part of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 1h to obtain a premix;
(2) drying the premix obtained in the step (1), presintering at the sintering temperature of 1200 ℃ for 3h, and naturally cooling to obtain presintering powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 10 hours, and filtering to obtain slurry;
(4) and (3) pressing the slurry obtained in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, namely heating from the heating speed of 1 ℃/min to 500 ℃ and keeping the temperature for 1h, then heating to 1150 ℃ at the heating speed of 5 ℃/min, keeping the temperature for 1h, and naturally cooling to obtain a finished product.
The mass ratio of the raw materials, water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 80 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
The addition amount of the organic auxiliary agent in the step (3) is 3% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, and the organic auxiliary agent is obtained by mixing dioctyl ester and vinyl trimethoxy silane according to the mass ratio of 1: 1.
The proportion of the raw materials and the steel balls of the secondary ball milling in the step (3) is 1:20, and the ball milling rotating speed is 100 r/min. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
Example 2
The permanent magnetic ferrite comprises the following raw materials in parts by weight: 110 parts of ferric oxide, 2 parts of strontium carbonate, 0.7 part of lanthanum oxide, 5 parts of manganese oxide, 2 parts of calcium carbonate, 15 parts of boric acid, 4 parts of silicon dioxide and 1 part of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 3 hours to obtain a premix;
(2) drying the premix obtained in the step (1), presintering at 1300 ℃ for 5h, and naturally cooling to obtain presintering powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry obtained in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, wherein the temperature is raised to 500 ℃ from the heating speed of 2 ℃/min and is preserved for 1h, then the temperature is raised to 1200 ℃ from the heating speed of 8 ℃/min and is preserved for 3h, and the temperature is naturally reduced to obtain a finished product.
The mass ratio of the raw materials, water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 100 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
The addition amount of the organic auxiliary agent in the step (3) is 3% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, and the organic auxiliary agent is obtained by mixing dioctyl ester and vinyl trimethoxy silane according to the mass ratio of 1: 1.
The proportion of the raw materials and the steel balls of the secondary ball milling in the step (3) is 1:20, and the ball milling speed is 150 r/min. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
Example 3
The permanent magnetic ferrite comprises the following raw materials in parts by weight: 130 parts of ferric oxide, 2.5 parts of strontium carbonate, 1 part of lanthanum oxide, 6 parts of manganese oxide, 3 parts of calcium carbonate, 20 parts of boric acid, 5 parts of silicon dioxide and 1.5 parts of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 3 hours to obtain a premix;
(2) drying the premix obtained in the step (1), presintering at 1300 ℃ for 5h, and naturally cooling to obtain presintering powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry obtained in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, wherein the temperature is raised to 500 ℃ from the heating speed of 2 ℃/min and is preserved for 1h, then the temperature is raised to 1200 ℃ from the heating speed of 8 ℃/min and is preserved for 3h, and the temperature is naturally reduced to obtain a finished product.
The mass ratio of the raw materials, water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 100 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
The addition amount of the organic auxiliary agent in the step (3) is 3% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, and the organic auxiliary agent is obtained by mixing dioctyl ester and vinyl trimethoxy silane according to the mass ratio of 1: 1.
The proportion of the raw materials and the steel balls of the secondary ball milling in the step (3) is 1:20, and the ball milling speed is 150 r/min. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
Comparative example 1
The permanent magnetic ferrite comprises the following raw materials in parts by weight: 130 parts of ferric oxide, 2.5 parts of strontium carbonate, 1 part of lanthanum oxide, 6 parts of manganese oxide, 3 parts of calcium carbonate, 20 parts of boric acid, 5 parts of silicon dioxide and 1.5 parts of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 3 hours to obtain a premix;
(2) drying the premix obtained in the step (1), presintering at 1300 ℃ for 5h, and naturally cooling to obtain presintering powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid and silicon dioxide, carrying out secondary ball milling for 13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry obtained in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, wherein the temperature is raised to 500 ℃ from the heating speed of 2 ℃/min and is preserved for 1h, then the temperature is raised to 1200 ℃ from the heating speed of 8 ℃/min and is preserved for 3h, and the temperature is naturally reduced to obtain a finished product.
The mass ratio of the raw materials, water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 100 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
The proportion of the raw materials and the steel balls of the secondary ball milling in the step (3) is 1:20, and the ball milling speed is 150 r/min. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
This comparative example is the same as example 3 except that no organic auxiliary is added.
Comparative example 2
The permanent magnetic ferrite comprises the following raw materials in parts by weight: 130 parts of ferric oxide, 2.5 parts of strontium carbonate, 1 part of lanthanum oxide, 6 parts of manganese oxide, 3 parts of calcium carbonate, 20 parts of boric acid, 5 parts of silicon dioxide and 1.5 parts of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 3 hours to obtain a premix;
(2) drying the premix obtained in the step (1), presintering at 1300 ℃ for 5h, and naturally cooling to obtain presintering powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry obtained in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, wherein the temperature is raised to 500 ℃ from the heating speed of 2 ℃/min and is preserved for 1h, then the temperature is raised to 1200 ℃ from the heating speed of 8 ℃/min and is preserved for 3h, and the temperature is naturally reduced to obtain a finished product.
The mass ratio of the raw materials, water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 100 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
The addition amount of the organic auxiliary agent in the step (3) is 1% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, and the organic auxiliary agent is obtained by mixing dioctyl ester and vinyl trimethoxy silane according to the mass ratio of 1: 1.
The proportion of the raw materials and the steel balls of the secondary ball milling in the step (3) is 1:20, and the ball milling speed is 150 r/min. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
The comparative example is the same as example 3 except that the added organic auxiliary agent is 1% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, namely the added amount is reduced.
Comparative example 3
The permanent magnetic ferrite comprises the following raw materials in parts by weight: 130 parts of ferric oxide, 2.5 parts of strontium carbonate, 1 part of lanthanum oxide, 6 parts of manganese oxide, 3 parts of calcium carbonate, 20 parts of boric acid, 5 parts of silicon dioxide and 1.5 parts of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 3 hours to obtain a premix;
(2) drying the premix obtained in the step (1), presintering at 1300 ℃ for 5h, and naturally cooling to obtain presintering powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry obtained in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, wherein the temperature is raised to 500 ℃ from the heating speed of 2 ℃/min and is preserved for 1h, then the temperature is raised to 1200 ℃ from the heating speed of 8 ℃/min and is preserved for 3h, and the temperature is naturally reduced to obtain a finished product.
The mass ratio of the raw materials, water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 100 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
The addition amount of the organic auxiliary agent in the step (3) is 5% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, and the organic auxiliary agent is obtained by mixing dioctyl ester and vinyl trimethoxy silane according to the mass ratio of 1: 1.
The proportion of the raw materials and the steel balls of the secondary ball milling in the step (3) is 1:20, and the ball milling speed is 150 r/min. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
The comparative example is the same as example 3 except that the added organic auxiliary agent is 5% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, namely the added amount is increased.
Comparative example 4
The permanent magnetic ferrite comprises the following raw materials in parts by weight: 130 parts of ferric oxide, 2.5 parts of strontium carbonate, 1 part of lanthanum oxide, 6 parts of manganese oxide, 3 parts of calcium carbonate, 20 parts of boric acid, 5 parts of silicon dioxide and 1.5 parts of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 3 hours to obtain a premix;
(2) drying the premix obtained in the step (1), presintering at 1300 ℃ for 5h, and naturally cooling to obtain presintering powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry obtained in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, wherein the temperature is raised to 500 ℃ from the heating speed of 2 ℃/min and is preserved for 1h, then the temperature is raised to 1200 ℃ from the heating speed of 8 ℃/min and is preserved for 3h, and the temperature is naturally reduced to obtain a finished product.
The mass ratio of the raw materials, water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 100 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
The addition amount of the organic auxiliary agent in the step (3) is 3% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, and the organic auxiliary agent is dioctyl phthalate.
The proportion of the raw materials and the steel balls of the secondary ball milling in the step (3) is 1:20, and the ball milling speed is 150 r/min. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
The comparative example is the same as example 3 except that only dioctyl ester is added as an organic auxiliary.
Comparative example 5
The permanent magnetic ferrite comprises the following raw materials in parts by weight: 130 parts of ferric oxide, 2.5 parts of strontium carbonate, 1 part of lanthanum oxide, 6 parts of manganese oxide, 3 parts of calcium carbonate, 20 parts of boric acid, 5 parts of silicon dioxide and 1.5 parts of cobalt oxide.
A preparation method of a permanent magnetic ferrite comprises the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 3 hours to obtain a premix;
(2) drying the premix obtained in the step (1), presintering at 1300 ℃ for 5h, and naturally cooling to obtain presintering powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry obtained in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, wherein the temperature is raised to 500 ℃ from the heating speed of 2 ℃/min and is preserved for 1h, then the temperature is raised to 1200 ℃ from the heating speed of 8 ℃/min and is preserved for 3h, and the temperature is naturally reduced to obtain a finished product.
The mass ratio of the raw materials, water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 100 r/min. After primary ball milling, the particle size of the slurry is controlled between 0.60 and 0.70 mu m; the diameter of the steel ball is 5-8 mm.
The addition amount of the organic auxiliary agent in the step (3) is 3% of the mass of the mixture of the pre-sintering powder, the calcium carbonate, the boric acid and the silicon dioxide, and the organic auxiliary agent is vinyl trimethoxy silane.
The proportion of the raw materials and the steel balls of the secondary ball milling in the step (3) is 1:20, and the ball milling speed is 150 r/min. After secondary ball milling, the granularity of ball milling slurry is controlled between 0.60 and 0.80 mu m; the diameter of the steel ball is selected to be 5-8 mm.
This comparative example is the same as example 3 except that vinyltrimethoxysilane is used as the organic assistant.
Performance testing
The average particle size (APD) and particle size distribution of the finely ground magnetic powder were measured using a WPL-202 type particle size tester. The magnetic property of the sintered sample is measured by using a DMT-1 permanent magnetic property tester of China institute of metrology science, and the microstructure of the section of the sample is observed by using a JSM-7600F scanning electron microscope.
Table 1 results of performance testing
Figure BDA0003351864890000081
As can be seen from Table 1, the permanent magnetic ferrite material obtained in the embodiment of the invention has better magnetic accumulation energy, intrinsic coercivity, residual magnetization intensity and other properties than comparative examples 1-5 with changed process parameters, the magnetic accumulation energy can reach 62kJ/m3 to the maximum, the intrinsic coercivity can reach 425.8kA/m, and the residual magnetization intensity can reach 599.6mT, and the magnetic properties of the permanent magnetic ferrite are remarkably improved. The addition amount of the organic auxiliary agent is too small to play a role in promoting dispersion, while the addition amount of the organic auxiliary agent is too large to cause cracking, and the single addition of one auxiliary agent has a single function and cannot play a role in synergy. Therefore, under the formula and the preparation process of the invention, the improvement of the overall performance of the permanent magnetic ferrite material can be realized.
From SEM images, the permanent magnetic ferrite material obtained by the invention has compact structure and uniform granularity, which is important for actually improving the magnetic performance of the material. Particle size distribution it can also be seen that the particle size distribution of the examples of the invention is narrower and the particles are more uniform.
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.

Claims (5)

1. The permanent magnetic ferrite is characterized by comprising the following raw materials in parts by weight: 130 portions of ferric oxide, 1.5 to 2.5 portions of strontium carbonate, 0.5 to 1 portion of lanthanum oxide, 3 to 6 portions of manganese oxide, 1 to 3 portions of calcium carbonate, 10 to 20 portions of boric acid, 3 to 5 portions of silicon dioxide and 0.5 to 1.5 portions of cobalt oxide.
2. A method for preparing the permanent magnetic ferrite according to claim 1, which is characterized by comprising the following steps:
(1) adding steel balls and water into ferric oxide, strontium carbonate, lanthanum oxide, manganese oxide and cobalt oxide according to the weight parts, and carrying out primary ball milling for 1-3h to obtain a premix;
(2) drying the premix obtained in the step (1), pre-sintering at the sintering temperature of 1200 ℃ and 1300 ℃ for 3-5h,
naturally cooling to obtain pre-sintered powder;
(3) mixing the pre-sintered powder obtained in the step (2) with calcium carbonate, boric acid, silicon dioxide and an organic auxiliary agent, carrying out secondary ball milling for 10-13h, and filtering to obtain slurry;
(4) and (3) pressing the slurry in the step (3) into a green body by using a mold, sintering the green body, and performing programmed heating in the sintering way, namely heating to 500 ℃ at a heating rate of 1-2 ℃/min and keeping the temperature for 1h, then heating to 1150-1200 ℃ at a heating rate of 5-8 ℃/min and keeping the temperature for 1-3h, and naturally cooling to obtain a finished product.
3. The method for preparing the permanent magnetic ferrite according to claim 2, wherein the mass ratio of the raw material, the water and the steel ball in the step (1) is 1:2:20, and the rotating speed is 80-100 r/min.
4. The method for preparing a permanent magnetic ferrite according to claim 2, wherein the addition amount of the organic auxiliary agent in the step (3) is 3% of the mass of the mixture of the pre-sintered powder, the calcium carbonate, the boric acid and the silica, and the organic auxiliary agent is obtained by mixing dioctyl ester and vinyl trimethoxy silane according to the mass ratio of 1: 1.
5. The method for preparing a permanent magnetic ferrite according to claim 2, wherein the ratio of the raw materials and the steel balls in the secondary ball milling in the step (3) is 1:20, and the ball milling rotation speed is 100-.
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