CN113698192A - Method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as raw material - Google Patents

Method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as raw material Download PDF

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CN113698192A
CN113698192A CN202111061878.2A CN202111061878A CN113698192A CN 113698192 A CN113698192 A CN 113698192A CN 202111061878 A CN202111061878 A CN 202111061878A CN 113698192 A CN113698192 A CN 113698192A
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ultrapure
particle size
average particle
magnetite concentrate
concentrate
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徐斌
姜涛
周玉娟
杨永斌
李骞
钟寿国
陈羽峰
吴金甜
李光辉
郭宇峰
范晓慧
黄柱成
张元波
彭志伟
甘敏
易凌云
杨凌志
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Central South University
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Abstract

A method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as a raw material comprises the following steps: drying and completely pre-oxidizing the ultrapure magnetite concentrate, and then carrying out fine grinding treatment; weighing the finely ground ultrapure magnetite concentrate, strontium carbonate, lanthanum oxide, cobalt oxide and calcium carbonate, carrying out primary burdening, carrying out wet ball milling on the prepared materials, and then granulating and presintering in a rotary kiln; crushing the pre-sintered material, adding calcium carbonate, silicon dioxide, boric acid, aluminum oxide and a dispersing agent, wet-grinding and uniformly mixing; and then filtering the slurry, magnetizing, pressing, molding, sintering and grinding to obtain the permanent magnetic ferrite. The invention takes the ultrapure magnet concentrate as the raw material for preparing the ferrite material, the purity of the ultrapure magnet concentrate after full oxidation is higher than that of the common iron oxide red material, and the ultrapure magnet concentrate does not contain manganese and chlorine impurities which have negative effects on the ferrite material, thereby being beneficial to accurate batching and further ensuring the consistency and stability of the performance of the ferrite product.

Description

Method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as raw material
Technical Field
The invention belongs to the field of preparation of permanent magnetic ferrite materials, and particularly relates to a method for preparing a permanent magnetic ferrite by taking ultrapure magnet concentrate as a raw material.
Background
The permanent magnetic ferrite material is an important basic functional material, and plays an important role in the development of magnetic materials by virtue of the advantages of wide raw material source, low price, excellent magnetic property and the like. The permanent magnetic ferrite material is widely applied to the industries of household electrical appliances, automobile motors and related electronic devices, and along with the increasingly wide application of the permanent magnetic ferrite material in new energy, electric automobiles, smart cities, smart earth and other emerging fields, the application market has increasingly high requirements on the performance of the permanent magnetic material, and the high-performance permanent magnetic ferrite material is more in short supply.
In order to meet the market demand, after the japanese TDK company releases FB9, FB12 and 14 series high-performance permanent magnetic ferrite products, domestic manufacturers explore ways for improving the magnetic performance of the permanent magnetic ferrite from the aspects of primary and secondary ingredient formulas, production processes and the like. The magnetic performance of the ferrite is improved by adjusting the material composition, and the most effective mode at present adopts the joint replacement of La-Co ions. In early studies, researchers used iron oxide red as the starting material and La was used3+Substituted moiety Sr2+By Co2+By substitution of part of Fe3+Finally form a film having Sr1-xLaxFe12-yCoyO19A Sr-La-Co ferrite with a structure. In recent years, Ca has been adopted2+Substituted moiety Sr2+And further improve La3+And Co2+The performance of the material is further improved. However, with the further strictness and regulations of environmental protection policy, the traditional Ruthner method for preparing iron oxide red is gradually replaced by the fluidized bed method because waste slag generated by desiliconization, waste gas generated in the production process and the like have influence on the environment, and the production efficiency of iron oxide red is greatly reduced. In addition, since iron oxide red, a by-product of the steel industry, is defined as solid waste, the state strictly closes the input amount of imported iron oxide red (ocean refuse), and the iron oxide red is continuously increasing in price and is in short supply.
Moreover, the conventional process for preparing the permanent magnetic ferrite by using the high-purity magnetite concentrate (TFe > 71.5%) as a raw material needs to be subjected to strong mixing, pelletizing, chainbi drying and pre-oxidation operations as shown in FIG. 1, and the process flow is quite complex.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings in the background art and provide a method for preparing a permanent magnetic ferrite by using ultrapure magnetite concentrate as a raw material.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as a raw material comprises the following steps:
(1) according to the chemical formula Sr1-x-yCayLaxFeB-AxCoAxO19Weighing ultrapure magnetite concentrate, strontium carbonate, lanthanum oxide, cobalt oxide and calcium carbonate for one-time batching, wherein the weight ratio of the ultrapure magnetite concentrate to the strontium carbonate to the lanthanum oxide to the cobalt oxide to the calcium carbonate is 0.2<x<0.4,0.25<y<0.45,0.2<A<0.8,11.2<B<11.8;
(2) Performing wet ball milling on the material prepared in the step (1), and then granulating and presintering in a rotary kiln;
(3) crushing the pre-burned material in the step (2), adding calcium carbonate, silicon dioxide, boric acid, aluminum oxide and a dispersing agent, wet-grinding and uniformly mixing;
(4) and (4) filtering the slurry obtained in the step (3), magnetizing, pressing and forming, sintering and grinding to obtain the permanent magnetic ferrite.
Preferably, in the method, in the step (1), the total iron grade of the ultrapure magnetite concentrate is more than 72%, the purity is more than 99.5%, and the contents of silicon and aluminum elements are both below 0.10%; the preparation method comprises the steps of carrying out high-temperature treatment before burdening of the ultrapure magnetite concentrate to dry and thoroughly pre-oxidize the ultrapure magnetite concentrate, controlling ferrous content of the ultrapure magnetite concentrate to be below 0.5% after pre-oxidation, and then carrying out fine grinding treatment.
The ultra-pure magnetite concentrate is used as a raw material, so that the consistency and performance stability of a ferrite product can be ensured. The silicon-aluminum element impurities in the ultra-pure magnetite concentrate are all lower than 0.1 percent, the silicon-aluminum element impurities in the common high-purity iron concentrate are all higher than 0.2 percent, the purity of the raw materials is directly influenced by the high content of the silicon-aluminum impurities, so that accurate batching is influenced, and a large amount of low-melting-point nonmagnetic substances (SrSiO) can be generated by the silicon-aluminum impurities in the pre-sintering process3、FeSiO3、xAl2O3·ySiO2Etc.) resulting in a reduction in the magnetic properties of the product.
In the above method, preferably, in the step (1), the strontium carbonate and the calcium carbonate both have an average particle size of 1-2 microns and a purity of more than 98%; the average particle size of the lanthanum oxide and the average particle size of the cobalt oxide are both 1-5 micrometers, and the purity of the lanthanum oxide and the cobalt oxide is over 99 percent.
In the method, preferably, in the step (2), the average particle size of the slurry after wet ball milling is 1 to 5 micrometers.
Preferably, in the step (2), the pre-sintering process comprises the steps of firstly preserving heat for 2-6 hours at 200-800 ℃, then continuously heating to 1220-1280 ℃, preserving heat for 1-4 hours, and completing granulation, drying and pre-sintering of the slurry in a rotary kiln. Specifically, the slurry is dried for 2-6 h at a low temperature of 200-800 ℃, and rolls along with the rotary kiln to form small balls, and the small balls are fully pre-sintered for 1-4 h at a high temperature of 1220-1280 ℃ to generate ferrite pre-sintered material.
In the above method, in the step (3), the slurry after wet grinding preferably has an average particle size of 0.55 to 0.8 μm.
In the above method, preferably, in the step (3), the calcium carbonate has an average particle size of 1 to 2 μm and is added in an amount of 0.2 wt% to 1.6 wt%; the average particle size of the silicon dioxide is 1-2 micrometers, and the addition amount of the silicon dioxide is 0.1-0.4 wt%; the boric acid has an average particle size of 1-2 micrometers, and the addition amount of 0.05-0.55 wt%; the average grain size of the aluminum oxide is 1-2 micrometers, and the addition amount is 0.05-0.55 wt%; the dispersing agent comprises calcium gluconate and sorbitol, the addition amount of the calcium gluconate is 0.02 wt% -0.50 wt%, and the addition amount of the sorbitol is 0.02 wt% -0.50 wt%.
Preferably, in the step (4), in the magnetizing and press-forming process, the forming magnetic field is 6000Gs to 10000Gs, and the forming pressure is 100 kg/cm to 400kg/cm2. More preferably, the molding pressure is 200 to 250kg/cm2
In the method, preferably, in the step (4), the sintering temperature is 1150-1200 ℃, and the sintering time is 1-4 h.
Compared with the prior art, the invention has the advantages that:
(1) the method takes the ultrapure magnet concentrate with the purity of more than 99.5 percent as the raw material for preparing the ferrite material, the purity of the ultrapure magnet concentrate after full oxidation is higher than that of the common iron oxide red material, and the ultrapure magnet concentrate does not contain manganese and chlorine impurities which have negative effects on the ferrite material, so that the method is favorable for accurate batching, and the consistency and the stability of the performance of the ferrite product are ensured; meanwhile, the ultrapure magnetite concentrate is oxidized to obtain ferric oxide, the reaction activity of the iron oxide is more active than that of an iron red raw material, and the high-temperature presintering process is more suitable for carrying out ion substitution reaction, so that the utilization rate of elements such as lanthanum and cobalt is effectively improved, and the production cost is reduced.
(2) The ultra-pure magnetite concentrate adopted by the invention can be obtained by a simple ore dressing and purification method from high-quality magnetite concentrate, large magnetite mines in Sichuan, Anhui and inner Mongolia of China can supply a large amount of high-quality magnetite concentrate, the product performance is stable, no waste gas and waste residue is generated in the production process, and the method is green, environment-friendly and economic and sustainable compared with the iron oxide red production process.
(3) The invention cancels the procedures of dry mixing, strong mixing, pelletizing and oxidation of the traditional preparation process of the high-purity magnetite concentrate ferrite by optimizing the procedures of pre-oxidation, mixed grinding and rotary kiln granulation pre-sintering, simplifies the process and further improves the production efficiency.
(4) The performance of the high-performance permanent magnetic ferrite material reaches the level of TDK FB9 series and above, and the high-performance permanent magnetic ferrite material has considerable market application value.
Drawings
FIG. 1 is a process flow diagram of the prior art for preparing permanent magnetic ferrite by using high-purity magnetite concentrate (TFe > 71.5%) as a raw material.
FIG. 2 is a process flow diagram of the preparation of permanent magnetic ferrite according to the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1: (this example compares ferrite properties at different sintering temperatures)
The method for preparing the permanent magnetic ferrite by taking the ultrapure magnetite concentrate as the raw material has the process flow chart shown in figure 2, and comprises the following steps:
(1) the method comprises the steps of pre-burning ultra-pure magnet concentrate with the total iron grade of 72.10%, the purity of 99.6% and the contents of silicon and aluminum elements of 0.08% and 0.06%, drying and completely pre-oxidizing the ultra-pure magnet concentrate, controlling the ferrous content of the pre-oxidized ultra-pure magnet concentrate to be below 0.5%, and then finely grinding until the average grain size is 1.2 microns for later use. Strontium carbonate and calcium carbonate with the granularity of 1.0 micron and the purity of 99 percent, and lanthanum oxide and cobalt oxide with the average grain diameter of 2 microns and the purity of 99.7 percent are dried for later use.
(2) According to Sr0.3Ca0.3La0.4Fe11.5Co0.2O19Mixing ultrapure magnetite concentrate, strontium carbonate, lanthanum oxide, cobalt oxide and calcium carbonate, fully and mixedly grinding the materials by a wet method until the average particle size is 1.2 microns, then putting the materials into a rotary kiln for drying, granulating and presintering, drying the materials for 4 hours at a low temperature region of 800 ℃, forming small balls along with the rolling of the rotary kiln, fully presintering the small balls for 2 hours at a high temperature region of 1250 ℃, cooling the presintering materials to room temperature, and crushing and finely grinding the materials to presintering material powder with the average particle size of 2.5 mm.
(3) Adding calcium carbonate with the average particle size of 1.5 micrometers, silicon dioxide with the average particle size of 1.2 micrometers, boric acid with the average particle size of 1.2 micrometers, aluminum oxide with the average particle size of 1.5 micrometers, a small amount of dispersants of calcium gluconate and sorbitol into the pre-sintering powder in the step (2), wherein the addition amount of the calcium carbonate is 0.5 wt% of the pre-sintering powder, the addition amount of the silicon dioxide is 0.2 wt%, the addition amount of the boric acid is 0.3 wt%, the addition amount of the aluminum oxide is 0.1 wt%, and the addition amount of the calcium gluconate is 0.3 wt%, then finely grinding the mixture in a roller ball mill (ball: water: 20:1:1.5) for 18 hours, and the average particle size of the secondary slurry is 0.71 micrometers.
(4) Standing the ball-milled and mixed material obtained in the step (3), draining, controlling the water content to be 35%, then performing wet pressing forming in a magnetic field of 10000Gs, and performing wet pressing forming at 250kg/cm2The pressure of the pressure was adjusted to obtain a magnetic cake having a diameter of 40cm by a height of 15 cm.
(5) And (3) insulating the magnetic cakes pressed in the step (4) for 3 hours in batches at the sintering temperature of 1180 ℃, 1185 ℃ and 1190 ℃, cooling, grinding, and then detecting the magnetic property, wherein the results are shown in Table 1.
TABLE 1 magnetic Properties of ferrite materials at different sintering temperatures in example 1
Figure BDA0003256958540000041
As can be seen from Table 1, the residual magnetism and the magnetic energy product of the ferrite magnetic cake are improved along with the increase of the sintering temperature, the intrinsic coercive force and the magnetic induction coercive force are slightly reduced, the product squareness ratio is 0.92 or more, and the detection indexes reach the requirements of TDK FB9 products.
Example 2:
the method for preparing the permanent magnetic ferrite by taking the ultrapure magnetite concentrate as the raw material has the process flow chart shown in figure 2, and comprises the following steps:
(1) high-temperature pre-burning ultrapure magnet concentrate with the total iron grade of 72.10%, the purity of 99.6% and the contents of silicon and aluminum elements of 0.08% and 0.06%, drying and completely pre-oxidizing the ultrapure magnet concentrate, controlling the ferrous content of the ultrapure magnet concentrate to be below 0.5% after pre-oxidation, and then finely grinding the ultrapure magnet concentrate until the average particle size is 1.2 microns; strontium carbonate and calcium carbonate having a particle size of 1.0 μm and a purity of 99%, and lanthanum oxide and cobalt oxide each having an average particle size of 2 μm and a purity of 99.7% were dried.
(2) According to Sr0.3Ca0.3La0.4Fe11.5Co0.2O19After accurately weighing the oxides according to the theoretical formula of (1), mixingMixing ultrapure magnetite concentrate, strontium carbonate, lanthanum oxide, cobalt oxide and calcium carbonate, fully mixing and grinding the materials by a wet method until the average particle size is 1.3 microns, then putting the materials into a rotary kiln for drying, granulating and presintering, drying the materials at a low temperature region of 800 ℃ for 4 hours, rolling the materials along with the rotary kiln to form small balls, fully presintering the small balls for 2 hours at a high temperature region of 1250 ℃, cooling the presintering materials to room temperature, and crushing and finely grinding the materials to presintering material powder with the average particle size of 2.5 mm.
(3) Adding calcium carbonate with the average particle size of 1.5 micrometers, silicon dioxide with the average particle size of 1.2 micrometers, boric acid with the average particle size of 1.2 micrometers, aluminum oxide with the average particle size of 1.5 micrometers, a small amount of dispersants of calcium gluconate and sorbitol into the pre-sintered and fine-ground material in the step (2), wherein the addition amount of the calcium carbonate is 0.8 wt%, the addition amount of the silicon dioxide is 0.2 wt%, the addition amount of the boric acid is 0.3 wt%, the addition amount of the aluminum oxide is 0.2 wt%, and the addition amount of the calcium gluconate is 0.3 wt%, then finely grinding the mixture in a roller ball mill (ball: water: 20:1:1.5) for 18 hours, and the average particle size of secondary slurry is 0.75 micrometers.
(4) Standing the ball-milled and mixed material obtained in the step (3), draining, controlling the water content to be 35%, and then carrying out wet pressing forming in a magnetic field of 10000Gs, wherein the magnetic field is 300kg/cm2The pressure of the pressure was adjusted to obtain a magnetic cake having a diameter of 40cm by a height of 15 cm.
(5) And (3) respectively keeping the magnetic cakes pressed in the step (4) at the sintering temperature of 1185 ℃ for 3 hours, cooling, grinding and processing, and detecting the magnetic property, wherein the results are shown in Table 2.
Comparative example 1:
the method for preparing the permanent magnetic ferrite according to the comparative example is different from example 2 only in that the raw material ultrapure magnetite concentrate is replaced by the primary iron oxide red (purity is 99.4%, silicon content is 0.01%, chlorine content is 0.1%, average particle size is 1.2 μm), other processes and parameters are completely the same as those of example 2, and the results of the prepared magnetic bodies are shown in table 2.
TABLE 2 magnetic properties of high performance ferrite materials prepared from ultrapure magnetite concentrate and iron oxide red
Figure BDA0003256958540000051
As can be seen from table 2, under the same experimental conditions, the performance of the permanent magnetic ferrite prepared from the ultra-pure magnetite concentrate is basically equivalent to that of ferrite prepared from iron oxide red in terms of coercive force, and the performance of the permanent magnetic ferrite prepared from iron oxide red is slightly superior in terms of remanence and magnetic energy product.
Example 3:
the method for preparing the permanent magnetic ferrite by taking the ultrapure magnetite concentrate as the raw material has the process flow chart shown in figure 2, and comprises the following steps:
(1) high-temperature pre-burning ultrapure magnet concentrate with a total iron grade of 72.14%, a purity of 99.7% and contents of silicon and aluminum elements of 0.09% and 0.07% respectively to dry and thoroughly pre-oxidize the ultrapure magnet concentrate, controlling ferrous iron of the ultrapure magnet concentrate to be below 0.5% after pre-oxidation, and then finely grinding to an average particle size of 1.2 microns; strontium carbonate and calcium carbonate with the granularity of 1 micron and the purity of 99 percent, and lanthanum oxide and cobalt oxide with the average grain diameter of 2 microns and the purity of 99.7 percent are dried and dried.
(2) According to Sr0.35Ca0.3La0.35Fe11.62Co0.18O19The method comprises the following steps of mixing ultrapure magnetite concentrate, strontium carbonate, lanthanum oxide, cobalt oxide and calcium carbonate, fully and uniformly grinding the materials by a wet method until the average particle size is 1.2 micrometers, then putting the materials into a rotary kiln for drying, granulating and presintering, drying for 4 hours at a low temperature region of 800 ℃, forming small balls by rolling along with the rotary kiln, fully presintering the small balls for 2 hours at a high temperature region of 1250 ℃, cooling the presintering materials to room temperature, and crushing and finely grinding the presintering materials to presintering material powder with the average particle size of 2.5 mm.
(3) Adding calcium carbonate with the average particle size of 1.5 micrometers, silicon dioxide with the average particle size of 1.2 micrometers, boric acid with the average particle size of 1.2 micrometers, aluminum oxide with the average particle size of 1.5 micrometers, a small amount of dispersants of calcium gluconate and sorbitol into the pre-sintered material subjected to pre-sintering and fine grinding in the step (2), wherein the addition amount of calcium carbonate is 0.5 wt%, the addition amount of silicon dioxide is 0.2 wt%, the addition amount of boric acid is 0.3 wt%, the addition amount of aluminum oxide is 0.1 wt%, the addition amount of calcium gluconate is 0.05 wt%, the addition amount of sorbitol is 0.05 wt%, and then performing fine grinding in a roller mill (ball: material: water is 20:1:1.5) for 18 hours, wherein the average particle size of secondary slurry is 0.71 micrometers.
(4) Standing the ball-milled and mixed material obtained in the step (3), draining, controlling the water content to be 35%, then performing wet pressing forming in a magnetic field of 10000Gs, and performing wet pressing forming at 250kg/cm2The pressure of the pressure was adjusted to obtain a magnetic cake having a diameter of 40cm by a height of 15 cm.
(5) And (3) respectively keeping the magnetic cakes pressed in the step (4) at the sintering temperature of 1185 ℃ for 3 hours, cooling, grinding and processing, and detecting the magnetic property, wherein the results are shown in Table 3.
Comparative example 2:
the comparative example is a method for preparing a permanent magnetic ferrite by adopting a conventional ferrite preparation process, and the preparation process comprises the following steps:
(1) the ultra-pure magnetite concentrate with the total iron grade of 72.14 percent, the purity of 99.7 percent and the contents of silicon and aluminum elements of 0.09 percent and 0.07 percent respectively is dried and partially pre-oxidized in a drying kiln, the highest temperature of the drying kiln is 850 ℃, the temperature is kept for 3 hours, the dried material is cooled to the room temperature, and the material is finely ground until the average grain diameter is 1.2 microns.
(2) Reference theoretical formula Sr0.35Ca0.3La0.35Fe11.62Co0.18O19Accurately weighing the ultrapure magnet concentrate obtained in the step (1), adding calcium carbonate, lanthanum oxide, cobalt oxide and strontium carbonate, carrying out dry mixing grinding, then carrying out strong mixing, adding 9% of water into the mixed material to prepare green pellets with the diameter of 6mm, drying and further oxidizing the green pellets in a heba machine, fully presintering the green pellets for 2 hours in a kiln with the highest temperature of 1250 ℃, cooling the presintering material to room temperature, and crushing and finely grinding the presintering material to obtain presintering material powder with the average particle size of 2.5 mm.
(3) The pre-sintered powder was prepared in exactly the same manner as in the steps (3), (4) and (5) of example 3 to prepare ferrites, the magnetic properties of which are shown in Table 3.
TABLE 3 magnetic Properties of ferrite materials prepared by the conventional Process and the Process of the present invention
Figure BDA0003256958540000061
As can be seen from Table 3, the ferrite prepared by the process of the present invention has higher magnetic coercive force and intrinsic coercive force than the ferrite material prepared by the conventional process, which indicates that the ferrite prepared by the present invention has uniform and fine crystal grains and uniform particles.

Claims (9)

1. A method for preparing permanent magnetic ferrite by taking ultrapure magnetite concentrate as a raw material is characterized by comprising the following steps:
(1) according to the chemical formula Sr1-x-yCayLaxFeB-AxCoAxO19Weighing ultrapure magnetite concentrate, strontium carbonate, lanthanum oxide, cobalt oxide and calcium carbonate for one-time batching, wherein the weight ratio of the ultrapure magnetite concentrate to the strontium carbonate to the lanthanum oxide to the cobalt oxide to the calcium carbonate is 0.2<x<0.4,0.25<y<0.45,0.2<A<0.8,11.2<B<11.8;
(2) Performing wet ball milling on the material prepared in the step (1), and then granulating and presintering in a rotary kiln;
(3) crushing the pre-burned material in the step (2), adding calcium carbonate, silicon dioxide, boric acid, aluminum oxide and a dispersing agent, wet-grinding and uniformly mixing;
(4) and (4) filtering the slurry obtained in the step (3), magnetizing, pressing and forming, sintering and grinding to obtain the permanent magnetic ferrite.
2. The method according to claim 1, wherein in the step (1), the ultrapure magnetite concentrate has an all-iron grade of more than 72%, a purity of more than 99.5%, and contents of both silicon and aluminum elements of less than 0.10%; high-temperature pre-oxidation and fine grinding treatment are carried out before the ultra-pure magnetite concentrate is proportioned.
3. The method according to claim 1, wherein in the step (1), the strontium carbonate and the calcium carbonate both have an average particle size of 1-2 μm and a purity of 98% or more; the average particle size of the lanthanum oxide and the average particle size of the cobalt oxide are both 1-5 micrometers, and the purity of the lanthanum oxide and the cobalt oxide is over 99 percent.
4. The method according to claim 1, wherein in the step (2), the average particle size of the slurry after wet ball milling is 1 to 5 microns.
5. The method of claim 1, wherein in the step (2), the pre-burning process comprises firstly preserving heat at 200-800 ℃ for 2-6 h, then continuously raising the temperature to 1220-1280 ℃ and preserving heat for 1-4 h.
6. The method of claim 1, wherein in step (3), the slurry after wet grinding has an average particle size of 0.55 to 0.8 μm.
7. The method according to claim 1, wherein in the step (3), the calcium carbonate has an average particle size of 1 to 2 μm and is added in an amount of 0.2 to 1.6 wt%; the average particle size of the silicon dioxide is 1-2 micrometers, and the addition amount of the silicon dioxide is 0.1-0.4 wt%; the boric acid has an average particle size of 1-2 micrometers, and the addition amount of 0.05-0.55 wt%; the average grain size of the aluminum oxide is 1-2 micrometers, and the addition amount is 0.05-0.55 wt%; the dispersing agent comprises calcium gluconate and sorbitol, the addition amount of the calcium gluconate is 0.02 wt% -0.50 wt%, and the addition amount of the sorbitol is 0.02 wt% -0.50 wt%.
8. The method according to claim 1, wherein in the step (4), the molding magnetic field is 6000Gs to 10000Gs and the molding pressure is 100 kg/cm to 400kg/cm during the magnetizing and press-molding process2
9. The method according to claim 1, wherein in the step (4), the sintering temperature is 1150-1200 ℃, and the sintering time is 1-4 h.
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