CN113072368A - Atmosphere sintering method of high-performance M-type ferrite - Google Patents
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Abstract
The invention discloses an atmosphere sintering method of a high-performance M-type ferrite, which comprises the steps of batching, presintering, pulping, molding and atmosphere sintering, wherein the whole atmosphere sintering process is divided into a plurality of atmosphere sintering stages, such as a binder removal stage, a first heat preservation stage, a second heat preservation stage, a first cooling stage, a second cooling stage, a third cooling stage and the like. The invention can obtain the single domain M-type ferrite with uniform grain size by respectively controlling the oxygen partial pressure in different sintering stages and avoid Co2+Oxidation of ions and Fe3+The reduction of the ions effectively improves the intrinsic magnetic property and the coercive force of the M-type ferrite. The method of the invention is compatible with the existing production equipment and has great practical value.
Description
Technical Field
The invention belongs to the technical field of electronic materials and components, and particularly relates to an atmosphere sintering method of high-performance M-type ferrite.
Background
In recent years, with the development of light, thin, short and small electronic products and the increasing stability of electronic materials in extreme fields such as aerospace, there is an urgent need to develop devices such as motors and generators with high temperature stability, wherein the core is to develop permanent magnetic materials with high coercivity. The M-type ferrite is a hexagonal magnetoplumbite-type ferrite, can obtain high magnetocrystalline anisotropy, and has the advantages of rich raw materials, low price, high temperature resistance, corrosion resistance and the like. At present, M-type ferrite with high coercivity is vigorously developed at home and abroad, but due to defects caused by a material preparation process, the coercivity of the M-type permanent magnetic ferrite is far lower than a theoretical value, related electronic components are easy to demagnetize under the action of a reverse magnetization field, and the stability of the components is greatly reduced.
Patent CN201410149524.7 discloses an ion substitution method for M-type hexaferrite, which uses La-Co substitution to greatly improve the magnetic properties of the material, but La-Co is expensive and not suitable for adding a large amount of La-Co. Patents CN201510101140.2 and CN201380031855.4 relate to a method for preparing M-type ferrites, which achieve high permanent magnetic properties by adding alkali metal compounds such as potassium salt and sodium salt, and simultaneously adding zinc compound during the sintering of the ferrites. Patent CN201410066917.1 discloses a preparation method for improving coercivity of M-type permanent magnetic ferrite, which adopts a molten salt method to prepare high-performance permanent magnetic ferrite, effectively improves microstructure and magnetic performance, but the above process requiring addition of molten salt cleaning is not suitable for large-scale production and use. Co in La-Co substituted M-type ferrites2+And Fe3+The valence is easy to change, and abnormal growth of crystal grains is easy to occur in the sintering process, and the crystal grains deviate from a single-domain structure, so that the coercive force is obviously reduced.
Disclosure of Invention
Aiming at the problems, the invention aims to provide an atmosphere sintering method of high-performance M-type ferrite, which can control the problems of grain growth, ion valence change and the like by regulating and controlling the sintering atmosphere in a plurality of heat preservation and cooling processes, improve the magnetocrystalline anisotropy of the material, obtain a uniform single-domain microstructure and further improve the coercive force of the M-type ferrite.
The invention is realized by the following technical scheme:
1) preparing materials: weighing Fe in stoichiometric ratio2O3Powder, CaCO3Powder, La2O3Powder, Co2O3Powder, SrCO3Powder and/or BaCO3Ball-milling the powder in a ball-milling tank and drying;
2) pre-burning: preserving the heat of the mixture obtained in the step 1) at 1100-;
3) pulping: adding a grinding aid and a dispersing agent into the pre-sintering material obtained in the step 2) in a ball milling tank, and carrying out ball milling to obtain slurry, wherein the average particle size of ferrite in the slurry is 0.8 +/-0.2 mu m;
4) molding: precipitating and filtering the slurry obtained in the step 3) until the water content is 20-45%, and forming under a 1.0-1.6T magnetic field to obtain a biscuit;
5) atmosphere sintering: placing the biscuit obtained in the step 4) in an atmosphere furnace, and dividing the sintering process into three heat preservation processes and three cooling processes: a first heat preservation process: heating to 400 ℃ at the speed of 0.5-1 ℃/min, preserving heat and realizing the discharge of organic matters in the biscuit in the air atmosphere; and a second heat preservation process: rapidly heating to 1000-1100 ℃ at the speed of 20-50 ℃/min, preserving the heat for 10-30min, controlling the oxygen partial pressure to be less than 1% (less than the ferrite decomposition pressure at the temperature), promoting the coarsening of fine particles and ensuring the uniform grain size; a third heat preservation process: raising the temperature to 1250-; a first cooling process: controlling the oxygen partial pressure to be 1-4.5% in the temperature reduction region of 1350-2+Is not oxidized into Co3 +(ii) a And a second cooling process: in the temperature reduction region of 1200-1000 ℃, the oxygen partial pressure is 0.5-2%, which is slightly higher than the equilibrium oxygen partial pressure of M-type ferrite, so as to ensure Fe2+Is completely oxidized; and a third cooling process: and naturally cooling in an air atmosphere within a temperature reduction range of less than 1000 ℃.
Preferably, the grain size of the high-performance M-type ferrite is 0.8 +/-1 mu M, the compactness is more than 96%, the intrinsic coercive force Hcj is more than 430kA/M, the remanence Br is more than 460mT, and the maximum magnetic energy product is more than 41kJ/M3。
Preferably, the stoichiometric ratio of the high-performance M-type ferrite is as follows: a. the1-x-yCaxLay(Fe12-u-vCou)O19Wherein A represents at least one of Sr and Ba, x, y, u and v are molar ratios, x is more than or equal to 0.01 and less than or equal to 0.3, y is more than or equal to 0.1 and less than or equal to 0.5, and y is more than or equal to 0.1 and less than or equal to 0.1u≤0.3，0.1≤v≤0.5。
Preferably, in the step 1), the ratio of the material balls to the water is 1:10:2, and the rotating speed is 100-.
Preferably, step 2), and keeping the temperature for 1-4 h.
Preferably, in the step 3), the ratio of the material balls to the water is 1:10:2, and the rotating speed is 100-.
The invention has the positive effects that: the traditional M-type ferrite sintering method generally adopts air sintering, is not beneficial to the refinement and homogenization of ferrite grain structure, and can cause the oxidation of metal ions. The invention divides the sintering process into three heat preservation processes and three cooling processes, and respectively adjusts and controls the grain size, the grain uniformity and the oxidation reduction of various ions in each stage in a targeted manner, so that the valence state change of various metal ions can be effectively controlled, uniform single-domain grains are obtained, and the coercivity is improved.
Detailed Description
Preferred embodiments of the present invention are explained below.
Example 1:
according to the composition Ba0.5Ca0.15La0.35(Fe11.5Co0.2)O19Proportioning and calculating the mass of each raw material to weigh Fe2O3Powder, CaCO3Powder, La2O3Powder, Co2O3Powder and BaCO3And (3) powder, namely putting the powder mixture into a ball milling tank, ball milling for 2 hours at the ball milling water ratio of 1:10:2 and the rotating speed of 200 r/min. And preserving the heat at 1300 ℃ for 2.5h to obtain the pre-sintered material. And (3) putting the pre-sintered material into a ball milling tank, wherein the ball-to-water ratio of the material is 1:10:2, the rotating speed is 200r/min, adding a grinding aid and a dispersing agent, and carrying out ball milling for 2h to obtain slurry, wherein the average particle size of ferrite in the slurry is 0.82 mu m. And precipitating and filtering the slurry to obtain a slurry with the water content of 35%, and forming under a 1.3T magnetic field to obtain a biscuit. Placing the biscuit in a sintering furnace for sintering: heating to 400 ℃ at the speed of 1 ℃/min, and keeping the temperature for 1h in the air atmosphere; rapidly heating to 1100 deg.C at a speed of 50 deg.C/min, maintaining for 10min, and oxygen partial pressure of 0.6%; heating to 1350 deg.C at a speed of 10 deg.C/min, maintaining for 1.5h, and oxygen partial pressure of 0.07%; controlling the oxygen partial pressure to be 3.5 percent in a temperature reduction range of 1350-;in the temperature reduction region of 1200-plus-1000 ℃, the oxygen partial pressure is 1.6 percent; and naturally cooling in an air atmosphere within a temperature reduction range of less than 1000 ℃.
The average grain size of the obtained M-type ferrite is 0.8 mu M, the compactness is 98.1 percent, the intrinsic coercive force Hcj 438kA/M, the remanence Br465mT and the maximum magnetic energy product of 41.5kJ/M are measured3。
Example 2:
according to the component Sr0.6Ca0.1La0.3(Fe11.7Co0.15)O19Proportioning and calculating the mass of each raw material to weigh Fe2O3Powder, CaCO3Powder, La2O3Powder, Co2O3Powder and BaCO3And (3) powder, namely putting the powder mixture into a ball milling tank, ball milling for 1.5h at the ball milling water ratio of 1:10:2 and the rotating speed of 150 r/min. And preserving the heat for 3 hours at 1280 ℃ to obtain the pre-sintered material. And (3) putting the pre-sintered material into a ball milling tank, wherein the ball-to-water ratio of the material is 1:10:2, the rotating speed is 180r/min, adding a grinding aid and a dispersing agent, and carrying out ball milling for 2h to obtain slurry, wherein the average particle size of ferrite in the slurry is 0.75 mu m. And (3) precipitating and filtering the slurry to obtain a water content of 38%, and forming under a 1.5T magnetic field to obtain a biscuit. Placing the biscuit in a sintering furnace for sintering: heating to 380 ℃ at the speed of 1 ℃/min, and keeping the temperature for 1h in the air atmosphere; rapidly heating to 1050 deg.C at 40 deg.C/min, maintaining for 20min, and oxygen partial pressure of 0.8%; heating to 1350 ℃ at the speed of 8 ℃/min, preserving heat for 1.5h, and controlling the oxygen partial pressure to be 0.03%; controlling the oxygen partial pressure to be 3% in a temperature reduction range of 1350-; in the temperature reduction region of 1200-plus-1000 ℃, the oxygen partial pressure is 1.2 percent; and naturally cooling in an air atmosphere within a temperature reduction range of less than 1000 ℃.
The average grain size of the obtained M-type ferrite is 0.9 mu M, the compactness is 97.8 percent, the intrinsic coercive force Hcj is 440kA/M, the remanence Br468mT and the maximum magnetic energy product of 42kJ/M are measured3。
Example 3:
according to the component Sr0.3Ba0.3Ca0.2La0.2(Fe11.6Co0.1)O19Proportioning and calculating the mass of each raw material to weigh Fe2O3Powder, CaCO3Powder, La2O3Powder, Co2O3Powder and BaCO3And (3) powder, namely putting the powder mixture into a ball milling tank, ball milling for 2 hours at the ball milling water ratio of 1:10:2 and the rotating speed of 180 r/min. And preserving the heat for 3 hours at 1200 ℃ to obtain the pre-sintered material. And (3) putting the pre-sintered material into a ball milling tank, wherein the ball-to-water ratio of the material is 1:10:2, the rotating speed is 200r/min, adding a grinding aid and a dispersing agent, and carrying out ball milling for 2h to obtain slurry, wherein the average particle size of ferrite in the slurry is 0.88 mu m. And (3) precipitating and filtering the slurry to obtain a slurry with the water content of 36%, and forming under a 1.2T magnetic field to obtain a biscuit. Placing the biscuit in a sintering furnace for sintering: heating to 350 deg.C at a rate of 0.5 deg.C/min, and maintaining for 1.5h in air atmosphere; rapidly heating to 1000 deg.C at a speed of 35 deg.C/min, maintaining for 15min, and oxygen partial pressure of 0.8%; heating to 1320 ℃ at the speed of 8 ℃/min, preserving the heat for 1.5h, and controlling the oxygen partial pressure to be 0.02 percent; controlling the oxygen partial pressure to be 2.7 percent in a temperature reduction range of 1350-; in the temperature reduction region of 1200-plus-1000 ℃, the oxygen partial pressure is 1.4 percent; and naturally cooling in an air atmosphere within a temperature reduction range of less than 1000 ℃.
The average grain size of the obtained M-type ferrite is 0.7 mu M, the compactness is 96.8 percent, the intrinsic coercive force Hcj is 432kA/M, the remanence Br is 470mT, and the maximum magnetic energy product is 42.8kJ/M3。
The invention can obtain the single domain M-type ferrite with uniform grain size by respectively controlling the oxygen partial pressure in different sintering stages and avoid Co2+Oxidation of ions and Fe3+The reduction of the ions effectively improves the intrinsic magnetic property and the coercive force of the M-type ferrite. The method of the invention is compatible with the existing production equipment and has great practical value.
It should be understood that the preferred embodiments described above are only for illustrating and explaining the features of the present invention, and the purpose is to enable those skilled in the art to understand the contents of the present invention and to implement the same, without any limitation to the scope of the present invention.
Claims (6)
1. An atmosphere sintering method of high-performance M-type ferrite is characterized by comprising the following steps:
1) weighing Fe in stoichiometric ratio2O3Powder of、CaCO3Powder, La2O3Powder, Co2O3Powder, SrCO3Powder and/or BaCO3Ball-milling the powder in a ball-milling tank and drying;
2) preserving the heat of the mixture obtained in the step 1) at 1100-;
3) adding a grinding aid and a dispersing agent into the pre-sintering material obtained in the step 2) in a ball milling tank, and carrying out ball milling to obtain slurry, wherein the average particle size of ferrite in the slurry is 0.8 +/-0.2 mu m;
4) precipitating and filtering the slurry obtained in the step 3) to obtain a slurry with a water content of 20-45%, and forming the slurry under a 1.0-1.6T magnetic field to obtain a biscuit;
5) placing the biscuit obtained in the step 4) in an atmosphere furnace, firstly heating to 300-400 ℃ at the speed of 0.5-1 ℃/min, and keeping the air atmosphere; then rapidly heating to 1000-1100 ℃ at the speed of 20-50 ℃/min, and preserving heat, wherein the oxygen partial pressure is controlled to be less than 1%; then raising the temperature to 1250-; beginning to cool, and controlling the oxygen partial pressure to be 1-4.5% in a cooling region of 1350-; controlling the oxygen partial pressure to be 0.5-2% in a temperature reduction region of 1200-plus-1000 ℃; and then naturally cooling in an air atmosphere within a temperature reduction interval of less than 1000 ℃.
2. The atmosphere sintering method of high performance M-type ferrite according to claim 1, characterized in that: the grain size of the high-performance M-type ferrite is 0.8 +/-1 mu M, the compactness is more than 96%, the intrinsic coercive force Hcj is more than 430kA/M, the remanence Br is more than 460mT, and the maximum magnetic energy product is more than 41kJ/M3。
3. The atmosphere sintering method of high performance M-type ferrite according to claim 1, characterized in that: the stoichiometric ratio of the high-performance M-type ferrite is as follows: a. the1-x-yCaxLay(Fe12-u-vCou)O19Wherein A represents at least one of Sr and Ba, x, y, u and v are molar ratios, x is more than or equal to 0.01 and less than or equal to 0.3, y is more than or equal to 0.1 and less than or equal to 0.5, u is more than or equal to 0.1 and less than or equal to 0.3, and v is more than or equal to 0.1 and less than or equal to 0.5.
4. An atmosphere sintering method of high performance M-type ferrite according to any of claims 1-3, characterized in that: step 1), the ratio of the material balls to the water is 1:10:2, and the rotating speed is 100-.
5. An atmosphere sintering method of high performance M-type ferrite according to any of claims 1-3, characterized in that: and 2), preserving heat for 1-4 h.
6. An atmosphere sintering method of high performance M-type ferrite according to any of claims 1-3, characterized in that: and step 3), the ratio of the material balls to the water is 1:10:2, and the rotating speed is 100-.
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| CN114031376A (en) * | 2021-12-24 | 2022-02-11 | 武汉理工大学 | Preparation method of high-hardness fine-grain ZTA system complex phase ceramic material |
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| CN114031376A (en) * | 2021-12-24 | 2022-02-11 | 武汉理工大学 | Preparation method of high-hardness fine-grain ZTA system complex phase ceramic material |
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Application publication date: 20210706 Assignee: CHANGZHOU HOUDE RENEWABLE RESOURCES TECHNOLOGY Co.,Ltd. Assignor: HANGZHOU DIANZI University Contract record no.: X2022330000489 Denomination of invention: A Method of High Performance M-type Ferrite Sintering in Atmosphere Granted publication date: 20220513 License type: Common License Record date: 20220926 |