CN115448373A - Preparation method of manganese ferrite material - Google Patents

Preparation method of manganese ferrite material Download PDF

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CN115448373A
CN115448373A CN202211292123.8A CN202211292123A CN115448373A CN 115448373 A CN115448373 A CN 115448373A CN 202211292123 A CN202211292123 A CN 202211292123A CN 115448373 A CN115448373 A CN 115448373A
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manganese
ferrite material
manganese ferrite
slurry
particle size
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CN115448373B (en
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朱航飞
单震
石枫
唐子舜
付亚奇
刘立东
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Hengdian Group DMEGC Magnetics Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/0018—Mixed oxides or hydroxides
    • C01G49/0072—Mixed oxides or hydroxides containing manganese
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
    • H01F1/342—Oxides
    • H01F1/344—Ferrites, e.g. having a cubic spinel structure (X2+O)(Y23+O3), e.g. magnetite Fe3O4
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/30—Three-dimensional structures
    • C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/42—Magnetic properties

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention relates to a preparation method of a manganese ferrite material, which comprises the following steps: (1) Mixing manganese oxide and iron oxide, and then sequentially carrying out primary wet sanding and drying to obtain mixed powder; (2) Pre-burning the mixed powder obtained in the step (1) to obtain a pre-burnt material; (3) Carrying out secondary wet sanding on the pre-sintered material obtained in the step (2) to obtain slurry; (4) And (4) carrying out spray pyrolysis on the slurry obtained in the step (3) to obtain the manganese ferrite material. The preparation method provided by the invention can remarkably improve the magnetic property of the manganese ferrite material and keep lower magnetic loss by comprehensively controlling the particle size of the manganese ferrite material and improving the dispersibility of the manganese ferrite material, thereby achieving higher quality factor.

Description

Preparation method of manganese ferrite material
Technical Field
The invention relates to the technical field of ferrite magnetic materials, in particular to a preparation method of a manganese ferrite material.
Background
Manganese ferrite material (MnFe) 2 O 4 ) The magnetic material is a soft magnetic material with a spinel structure, is also called manganese spinel or manganese ferrite, has the characteristics of high saturation magnetization, high initial permeability, low coercive force and the like, and is widely applied to electronic equipment such as electronics, communication, navigation, radar, telemetering and the like.
At present, the preparation methods of manganese ferrite materials are many, including a hydrothermal method, a coprecipitation method, a sol-gel method, a high-temperature spreading method, an ultrasonic chemical method, a ball milling method and the like. The various preparation methods have the defects of low yield, incapability of realizing large-scale production, high production energy consumption, poor product dispersibility, low purity, various and high content of impurities, long production period and the like.
CN104495943A discloses a preparation method of manganese ferrite nano-powder, which prepares manganese salt and ferric salt into a mixed solution; then adding sodium dodecyl benzene sulfonate for dissolving, and uniformly mixing; then adjusting the pH value of the microwave hydrothermal reaction system; adding the solution with the adjusted pH value into a microwave digestion tank, sealing and placing the tank in a microwave digestion instrument for microwave hydrothermal reaction; and after the reaction is finished, taking out the solution, filtering, washing the precipitate for multiple times by using distilled water and absolute ethyl alcohol, and drying to obtain a microwave hydrothermal product, namely the manganese ferrite nano powder. However, the method is complex in process and difficult to realize large-scale mass production.
CN113072370A discloses a manganese-zinc ferrite magnetic core and a preparation method thereof, the method comprises the steps of grinding raw materials of iron oxide, manganese oxide and zinc oxide, then placing the raw materials in a sintering furnace for sintering treatment, then grinding the pre-sintered mixed material again, and then sequentially pressing and sintering to obtain the manganese-zinc ferrite magnetic core. The magnetic core material obtained by the method is easy to agglomerate, so that the magnetic property is reduced.
Therefore, the preparation method which can obviously improve the magnetic property of the manganese ferrite material, has simple process and can be applied industrially has important significance.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a method for preparing a manganese ferrite material, wherein the method provided by the present invention can significantly improve the magnetic properties of the manganese ferrite material and maintain a low magnetic loss by comprehensively controlling the particle size of the manganese ferrite material and improving the dispersibility of the manganese ferrite material, so as to achieve a high quality factor.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a manganese ferrite material, which comprises the following steps:
(1) Mixing manganese oxide and iron oxide, and then sequentially carrying out primary wet sanding and drying to obtain mixed powder;
(2) Pre-burning the mixed powder obtained in the step (1) to obtain a pre-burnt material;
(3) Performing secondary wet sanding on the pre-sintered material obtained in the step (2) to obtain slurry;
(4) And (4) carrying out spray pyrolysis on the slurry obtained in the step (3) to obtain the manganese ferrite material.
On one hand, the preparation method provided by the invention is characterized in that the manganese ferrite material is prepared by the combination of pre-sintering and spray pyrolysis, the preliminary solid-phase reaction is carried out by the pre-sintering, and then the raw materials are prepared by the spray pyrolysis. On the other hand, the preparation method provided by the invention controls the particle size of the manganese ferrite material by a three-step method on the basis of the combination of pre-sintering and spray pyrolysis, and firstly, the particle size is preliminarily controlled by one-time wet sanding, so that the mixing is promoted and the subsequent reaction is facilitated; then, controlling the particle size again through secondary wet sanding, and grinding the pre-sintered material into fine particles to prepare for subsequent spray pyrolysis; and finally, the combination of the particles is promoted again by a spray pyrolysis mode, the particle size of the particles is adjusted by controlling the spray pyrolysis condition, and the manganese ferrite material with fine particles, good dispersibility and uniform particle size is finally obtained, so that the magnetic property of the manganese ferrite material is further improved.
Preferably, the manganese oxide of step (1) includes Mn 3 O 4 。
Preferably, the iron oxide comprises Fe 2 O 3 。
Preferably, the molar ratio of manganese to iron in the oxides of manganese and iron oxides is 1 (1-3), and may be, for example, 1:1, 1.2, 1.4, 1.6, 1.
Preferably, the one-time wet sanding in the step (1) is performed for 1 to 4 hours, and may be, for example, 1 hour, 1.2 hours, 1.4 hours, 1.6 hours, 1.8 hours, 2 hours, 2.2 hours, 2.5 hours, 2.8 hours, 3 hours, 3.2 hours, 3.5 hours, 3.8 hours or 4 hours, but is not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the temperature of the drying is 100-110 ℃, for example, 100 ℃, 102 ℃, 104 ℃, 106 ℃, 108 ℃ or 110 ℃, but not limited to the recited values, and other values not recited in the range of values are also applicable.
Preferably, the drying time is 4-10h, for example, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h, 8h, 8.5h, 9h, 9.5h or 10h, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
Preferably, the powder mixture has an average particle size of 0.1 to 1 μm, for example, 0.1 μm, 0.2 μm, 0.3 μm, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm or 1 μm, but is not limited to the values listed, and other values not listed in the numerical ranges are equally applicable.
Preferably, the temperature increase rate of the pre-sintering in step (2) is 2-3 ℃/min, such as 2 ℃/min, 2.2 ℃/min, 2.4 ℃/min, 2.6 ℃/min, 2.8 ℃/min or 3 ℃/min, but not limited to the values recited, and other values not recited in the range of values are also applicable.
Preferably, the pre-firing end point temperature is 750 to 950 ℃, for example, 750 ℃, 760 ℃, 770 ℃, 780 ℃, 790 ℃, 800 ℃, 820 ℃, 840 ℃, 860 ℃, 880 ℃, 900 ℃, 920 ℃, 940 ℃ or 950 ℃, but not limited to the recited values, and other values not recited in the numerical range are also applicable.
The invention preferably controls the pre-burning temperature in a specific range, can promote the generation reaction of the manganese ferrite to be fully carried out, achieves higher magnetic performance and prevents the performance from being reduced due to high temperature.
Preferably, the burn-in holding time is 2 to 4 hours, for example, 2 hours, 2.2 hours, 2.4 hours, 2.6 hours, 2.8 hours, 3 hours, 3.2 hours, 3.4 hours, 3.6 hours, 3.8 hours or 4 hours, but not limited to the recited values, and other values not recited in the range of values are also applicable.
The invention preferably controls the heat preservation time of the presintering within a specific range, can promote the generation reaction of the manganese ferrite to be fully carried out, and leads the product to achieve higher magnetic performance.
Preferably, the time of the secondary wet sanding in the step (3) is 1 to 4 hours, for example, 1 hour, 1.2 hours, 1.4 hours, 1.6 hours, 1.8 hours, 2 hours, 2.2 hours, 2.5 hours, 2.8 hours, 3 hours, 3.2 hours, 3.5 hours, 3.8 hours or 4 hours, but not limited to the enumerated values, and other unrecited values in the numerical range are also applicable.
Preferably, the particles in the slurry have an average particle size of 0.1 to 1 μm, and may be, for example, 0.1 μm, 0.2 μm, 0.3 μm, 0.4 μm, 0.5 μm, 0.6 μm, 0.7 μm, 0.8 μm, 0.9 μm or 1 μm, but are not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the slurry of step (4) is fed at a flow rate of 0.1 to 1L/h, such as 0.1L/h, 0.2L/h, 0.3L/h, 0.4L/h, 0.5L/h, 0.6L/h, 0.7L/h, 0.8L/h, 0.9L/h or 1L/h, but not limited to the values recited, and other values not recited within the range of values are equally applicable.
Preferably, the carrier gas has a flow rate of 0.6 to 6L/h, for example 0.6L/h, 1L/h, 1.5L/h, 2L/h, 2.5L/h, 3L/h, 3.5L/h, 4L/h, 4.5L/h, 5L/h, 5.5L/h or 6L/h, but not limited to the values recited, and other values not recited in the range of values are equally applicable.
The invention preferably controls the flow rate of the carrier gas in a specific range, can promote the manganese ferrite to be fully formed, and further controls the grain diameter of the ferrite material, so that the ferrite material keeps higher magnetic performance.
Preferably, the temperature of the spray pyrolysis in step (4) is 1050-1250 ℃, for example 1050 ℃, 1060 ℃, 1070 ℃, 1080 ℃, 1090 ℃, 1200 ℃, 1210 ℃, 1220 ℃, 1230 ℃, 1240 ℃ or 1250 ℃, but not limited to the recited values, and other values not recited in the range of values are equally applicable.
The present invention preferably controls the temperature of spray pyrolysis within a specific range, which can further promote the sufficient formation of manganese ferrite and prevent the magnetic properties from being degraded due to an excessively high temperature.
Preferably, the temperature of the exit gas stream from the spray pyrolysis in step (4) is in the range of from 90 to 110 ℃, for example 90 ℃, 92 ℃, 94 ℃, 96 ℃, 98 ℃, 100 ℃, 102 ℃, 104 ℃, 106 ℃, 108 ℃ or 110 ℃, but is not limited to the recited values, and other values not recited in the range of values are equally applicable.
Preferably, the manganese ferrite material of step (4) has an average particle size of 0.1 to 2 μm, and may be, for example, 0.1 μm, 0.2 μm, 0.4 μm, 0.6 μm, 0.8 μm, 1 μm, 1.2 μm, 1.4 μm, 1.6 μm, 1.8 μm or 2 μm, but is not limited to the values recited, and other values not recited within the range of values are equally applicable.
As a preferred technical scheme of the invention, the preparation method comprises the following steps:
(1) Mixing manganese oxide and iron oxide, wherein the molar ratio of manganese to iron in the manganese oxide and the iron oxide is 1 (1-3), performing primary wet sanding for 1-4h, and drying at 100-110 ℃ for 4-10h to obtain mixed powder, wherein the average particle size of the mixed powder is 0.1-1 mu m;
(2) Heating the mixed powder obtained in the step (1) to 750-950 ℃ at a speed of 2-3 ℃/min for pre-sintering, and preserving heat for 2-4h to obtain a pre-sintered material;
(3) Carrying out secondary wet sanding on the pre-sintered material obtained in the step (2) for 1-4h to obtain slurry, wherein the average particle size of particles in the slurry is 0.1-1 mu m;
(4) Feeding the slurry obtained in the step (3) at a speed of 0.1-1L/h, carrying out spray pyrolysis under the conditions that the flow rate of carrier gas is 0.6-6L/h and the temperature is 1050-1250 ℃, wherein the temperature of outlet gas flow of the spray pyrolysis is 90-110 ℃, and obtaining the manganese ferrite material, wherein the average particle size of the manganese ferrite material is 0.1-2 mu m.
Compared with the prior art, the invention has the following beneficial effects:
(1) The preparation method provided by the invention can prepare the manganese ferrite material with smaller granularity, good dispersibility and uniform granularity by the combined process of pre-burning and spray pyrolysis and the control of the particle size in multiple steps, effectively avoids the problem of particle agglomeration of the ferrite material, is beneficial to improving the magnetic property of the manganese ferrite material, and keeps lower magnetic loss, thereby achieving higher quality factor, mu 'can reach more than 4.0, mu' can reach less than 0.127, and Q value can reach more than 35.433.
(2) The preparation method provided by the invention is simple in process, can be used for large-scale mass production, and is beneficial to industrial popularization.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a preparation method of a manganese ferrite material, which comprises the following steps:
(1) Mixed Mn 3 O 4 And Fe 2 O 3 The Mn of 3 O 4 And Fe 2 O 3 The molar ratio of medium manganese to iron is 1:2, then primary wet sanding is carried out for 2 hours, and then drying is carried out for 7 hours at 105 ℃ to obtain mixed powder, wherein the average particle size of the mixed powder is 0.5 mu m;
(2) Heating the mixed powder obtained in the step (1) to 850 ℃ at the speed of 2.5 ℃/min for pre-sintering, and preserving heat for 3 hours to obtain a pre-sintered material;
(3) Carrying out secondary wet sanding on the pre-sintered material obtained in the step (2) for 2.5 hours to obtain slurry, wherein the average particle size of particles in the slurry is 0.5 mu m;
(4) Feeding the slurry obtained in the step (3) at a speed of 0.5L/h, and carrying out spray pyrolysis under the conditions that the flow rate of a carrier gas is 3.3L/h and the temperature is 1150 ℃, wherein the temperature of an outlet gas flow of the spray pyrolysis is 100 ℃, so as to obtain a manganese ferrite material, wherein the average particle size of the manganese ferrite material is 1 mu m.
Example 2
The embodiment provides a preparation method of a manganese ferrite material, which comprises the following steps:
(1) Mixed Mn 3 O 4 And Fe 2 O 3 Said Mn is 3 O 4 And Fe 2 O 3 The molar ratio of medium manganese to iron is 1:1, then primary wet sanding is carried out for 1h, and then drying is carried out for 10h at 100 ℃ to obtain mixed powder, wherein the average particle size of the mixed powder is 1 mu m;
(2) Heating the mixed powder obtained in the step (1) to 950 ℃ at a speed of 2 ℃/min for pre-sintering, and preserving heat for 2h to obtain a pre-sintered material;
(3) Carrying out secondary wet sanding on the pre-sintered material obtained in the step (2) for 4 hours to obtain slurry, wherein the average particle size of particles in the slurry is 0.1 mu m;
(4) Feeding the slurry obtained in the step (3) at a speed of 1L/h, carrying out spray pyrolysis under the conditions that the flow rate of carrier gas is 6L/h and the temperature is 1050 ℃, wherein the temperature of outlet gas flow of the spray pyrolysis is 110 ℃, and obtaining the manganese ferrite material, wherein the average particle size of the manganese ferrite material is 0.1 mu m.
Example 3
The embodiment provides a preparation method of a manganese ferrite material, which comprises the following steps:
(1) Mixed Mn 3 O 4 And Fe 2 O 3 Said Mn is 3 O 4 And Fe 2 O 3 The molar ratio of medium manganese to iron is 1:3, then primary wet sanding is carried out for 4 hours, and then drying is carried out for 4 hours at 110 ℃ to obtain mixed powder, wherein the average grain diameter of the mixed powder is 0.1 mu m;
(2) Heating the mixed powder obtained in the step (1) to 750 ℃ at a speed of 3 ℃/min for pre-sintering, and preserving heat for 4h to obtain a pre-sintered material;
(3) Carrying out secondary wet sanding on the pre-sintered material obtained in the step (2) for 1h to obtain slurry, wherein the average particle size of particles in the slurry is 1 mu m;
(4) Feeding the slurry obtained in the step (3) at a speed of 0.1L/h, carrying out spray pyrolysis under the conditions that the flow rate of carrier gas is 0.6L/h and the temperature is 1250 ℃, wherein the temperature of outlet gas flow of the spray pyrolysis is 90 ℃, and obtaining the manganese ferrite material, wherein the average particle size of the manganese ferrite material is 2 microns.
Example 4
This example provides a method for preparing a manganese ferrite material, which is different from example 1 only in that the pre-firing temperature is 700 ℃.
Example 5
This example provides a method for preparing a manganese ferrite material, which is different from example 1 only in that the pre-firing temperature is 1000 ℃.
Example 6
This example provides a method for preparing a manganese ferrite material, which is different from example 1 only in that the pre-sintering time is 1h.
Example 7
This example provides a method for preparing a manganese ferrite material, which is different from example 1 only in that the pre-sintering time is 5 hours.
Example 8
This example provides a method of preparing a manganese ferrite material, differing from example 1 only in that the temperature of the spray pyrolysis is 1000 ℃.
Example 9
This example provides a method of preparing a manganese ferrite material, differing from example 1 only in that the temperature of the spray pyrolysis is 1300 ℃.
Example 10
This example provides a method for preparing a manganese ferrite material, which is different from example 1 only in that the flow rate of the carrier gas is 0.1L/h.
Example 11
This example provides a method for preparing a manganese ferrite material, which is different from example 1 only in that the flow rate of the carrier gas is 10L/h.
Comparative example 1
This comparative example provides a method for preparing a manganese ferrite material, which is different from example 1 only in that the step (2) and the step (3) are not performed, and the powder mixture obtained in the step (1) is directly subjected to spray pyrolysis.
Mu' and mu "of the manganese ferrite materials obtained in examples 1 to 11 and comparative example 1 were measured at 80MHz using a microwave vector network analyzer (Agilent N5235A) and an electromagnetic property testing jig (PRD 706RT, dow-Town microwave science Co., ltd.), and the results are shown in Table 1. Wherein, mu' represents the real part component of the complex permeability of the magnetic medium and represents the stored energy of the magnetic material; μ "represents the imaginary component of the magnetic medium's complex permeability, representing the magnetic loss.
Q of the manganese ferrite materials obtained in examples 1 to 11 and comparative example 1 was calculated, Q representing the quality factor, by the following calculation method: q = μ'/μ ".
TABLE 1
Figure BDA0003899338040000091
Figure BDA0003899338040000101
From table 1, the following points can be seen:
(1) It can be seen from the data of examples 1 to 11 that the preparation method provided by the invention can significantly improve the magnetic properties of the manganese ferrite material and reduce the magnetic loss of the manganese ferrite material, mu 'can reach more than 4.0, mu' can reach less than 0.127, and Q value can reach more than 35.433.
(2) Comparing the data of example 1 and examples 4-5 together, it can be seen that the temperature of the pre-sintering in example 1 is 850 ℃, compared with 700 ℃ and 1000 ℃ in examples 4-5, respectively, the μ' and Q in example 1 are significantly higher than those in examples 4-5, and therefore, the invention preferably controls the pre-sintering temperature, and can further improve the magnetic performance of the manganese ferrite material.
(3) It can be seen from the combination of the data of the embodiment 1 and the data of the embodiments 6 to 7 that the holding time of the pre-sintering in the embodiment 1 is 3h, and compared with the holding time of 1h and 5h in the embodiments 6 to 7, respectively, the μ' and the Q in the embodiment 1 are obviously higher than those in the embodiments 6 to 7, so that the invention preferably controls the holding time of the pre-sintering, and can further improve the magnetic performance of the manganese ferrite material.
(4) Comparing the data of example 1 and examples 8-9 together, it can be seen that the temperature of spray pyrolysis in example 1 is 1150 ℃, and compared with 1000 ℃ and 1300 ℃ in examples 8-9, respectively, μ' and Q in example 1 are significantly higher than those in examples 8-9, so that the present invention preferably controls the temperature of spray pyrolysis to further improve the magnetic properties of the manganese ferrite material.
(5) Comparing the data of example 1 and examples 10-11 together, it can be seen that the flow rate of the carrier gas in example 1 is 3.3L/h, and compared with 0.1L/h and 10L/h in examples 10-11, respectively, the flow rates of μ' and Q in example 1 are significantly higher than those in examples 10-11, so that the magnetic properties of the manganese ferrite material can be further improved by controlling the flow rate of the carrier gas preferably.
(6) Comparing the data of example 1 and comparative example 1 together, it can be seen that comparative example 1 is different from example 1 only in that step (2) and step (3) are not performed, and μ' and Q in example 1 are significantly higher than those in comparative example 1, and thus it can be seen that the present invention can significantly improve the magnetic properties of the manganese ferrite material by adopting the combined process of pre-sintering and spray pyrolysis.
In conclusion, the manganese ferrite material with small particle size, good dispersibility and uniform particle size can be prepared by the preparation method provided by the invention, the magnetic property of the manganese ferrite material is favorably improved, and the low magnetic loss is kept.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.

Claims (10)

1. The preparation method of the manganese ferrite material is characterized by comprising the following steps of:
(1) Mixing manganese oxide and iron oxide, and then sequentially carrying out primary wet sanding and drying to obtain mixed powder;
(2) Pre-burning the mixed powder obtained in the step (1) to obtain a pre-burnt material;
(3) Carrying out secondary wet sanding on the pre-sintered material obtained in the step (2) to obtain slurry;
(4) And (4) carrying out spray pyrolysis on the slurry obtained in the step (3) to obtain the manganese ferrite material.
2. The method according to claim 1, wherein the manganese oxide of step (1) comprises Mn 3 O 4 ；
Preferably, the iron oxide comprises Fe 2 O 3 ；
Preferably, the molar ratio of manganese to iron in the manganese oxide and the iron oxide is 1 (1-3).
3. The method for preparing the resin composition according to claim 1 or 2, wherein the one-time wet sanding in the step (1) is performed for 1 to 4 hours;
preferably, the drying temperature is 100-110 ℃;
preferably, the drying time is 4-10h;
preferably, the average particle size of the powder mixture is 0.1 to 1 μm.
4. The production method according to any one of claims 1 to 3, wherein the temperature increase rate of the pre-firing in the step (2) is 2 to 3 ℃/min;
preferably, the end point temperature of the pre-sintering is 750-950 ℃;
preferably, the heat preservation time of the pre-burning is 2-4h.
5. The method of any one of claims 1 to 4, wherein the time for the secondary wet sanding in step (3) is 1 to 4 hours;
preferably, the particles in the slurry have an average particle size of from 0.1 to 1 μm.
6. The method according to any one of claims 1 to 5, wherein the slurry in step (4) is fed at a flow rate of 0.1 to 1L/h;
preferably, the flow rate of the carrier gas is 0.6 to 6L/h.
7. The method according to any one of claims 1 to 6, wherein the temperature of the spray pyrolysis in the step (4) is 1050 to 1250 ℃.
8. The process according to any one of claims 1 to 7, wherein the temperature of the exit gas stream from the spray pyrolysis in step (4) is from 90 to 110 ℃.
9. The production method according to any one of claims 1 to 8, wherein the average particle size of the manganese ferrite material in step (4) is 0.1 to 2 μm.
10. The method of any one of claims 1 to 9, comprising the steps of:
(1) Mixing manganese oxide and iron oxide, wherein the molar ratio of manganese to iron in the manganese oxide and the iron oxide is 1 (1-3), performing primary wet sanding for 1-4h, and drying at 100-110 ℃ for 4-10h to obtain mixed powder, wherein the average particle size of the mixed powder is 0.1-1 mu m;
(2) Heating the mixed powder obtained in the step (1) to 750-950 ℃ at a speed of 2-3 ℃/min for pre-sintering, and preserving heat for 2-4h to obtain a pre-sintered material;
(3) Carrying out secondary wet sanding on the pre-sintered material obtained in the step (2) for 1-4h to obtain slurry, wherein the average particle size of particles in the slurry is 0.1-1 mu m;
(4) Feeding the slurry obtained in the step (3) at a speed of 0.1-1L/h, carrying out spray pyrolysis under the conditions that the flow rate of carrier gas is 0.6-6L/h and the temperature is 1050-1250 ℃, wherein the temperature of outlet gas flow of the spray pyrolysis is 90-110 ℃, and obtaining the manganese ferrite material, wherein the average particle size of the manganese ferrite material is 0.1-2 mu m.
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JPH06275421A (en) * 1993-03-17 1994-09-30 Tdk Corp Method and device for manufacturing soft ferrite
JP2007112695A (en) * 2005-09-22 2007-05-10 Tdk Corp METHOD FOR PRODUCING Mn FERRITE
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