CN108147805B - Manganese-zinc ferrite and preparation method thereof - Google Patents

Manganese-zinc ferrite and preparation method thereof Download PDF

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CN108147805B
CN108147805B CN201711493894.2A CN201711493894A CN108147805B CN 108147805 B CN108147805 B CN 108147805B CN 201711493894 A CN201711493894 A CN 201711493894A CN 108147805 B CN108147805 B CN 108147805B
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韩爱文
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Nantong guanyouda Magnetic Industry Co.,Ltd.
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C04B35/62615—High energy or reactive ball milling
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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    • C04B35/645—Pressure sintering
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
    • C04B2235/658—Atmosphere during thermal treatment
    • C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
    • C—CHEMISTRY; METALLURGY
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

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  • Inorganic Chemistry (AREA)
  • Magnetic Ceramics (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention provides a preparation method of manganese-zinc ferrite, which comprises the following steps: providing and mixing Fe2O3、Mn3O4ZnO, CoO, NiO and CuO powder to obtain first mixed powder; carrying out first ball milling on the first mixed powder to obtain second mixed powder; performing first sintering treatment on the second mixed powder to obtain a first block; crushing the first block to obtain third mixed powder; performing second ball milling on the third mixed powder to obtain fourth mixed powder; and carrying out hot-pressing sintering treatment on the fourth mixed powder. Aiming at the defects of the traditional ferrite formula, the invention designs a new ferrite formula, improves the magnetic property and the mechanical property of the ferrite, optimizes the hot-pressing sintering process, greatly improves the compactness of a finished product after the hot-pressing sintering treatment, improves the crystal grain structure, and improves the magnetic property and the mechanical property.

Description

Manganese-zinc ferrite and preparation method thereof
Technical Field
The invention relates to ferrite and a preparation method thereof, in particular to manganese-zinc ferrite and a preparation method thereof.
Background
The application of soft magnetic ferrite in the switch power supply is the most active field in the electronic technology, the switch power supply is used for replacing the traditional power supply and is called as the revolution of the power supply technology in the world, and the soft magnetic ferrite material for the switch power supply accounts for more than 40 percent of the whole soft magnetic ferrite market. The MnZn ferrite which is dominant in the production and use of the soft magnetic ferrite is MnZn ferrite which means MnFe with a spinel structure2O4、ZnFe2O4And from small amounts of Fe3O4A solid solution of the composition. The MnZn ferrite material is still the soft magnetic ferrite material with the largest production quantity and the most extensive application, wherein the high-frequency power ferrite material and the high-permeability material have the greatest development prospect.
In order to obtain a ferrite material having excellent soft magnetic properties, a great deal of research has been conducted on ferrite materials in the prior art. The prior art proposes a method for preparing manganese zinc ferrite, which proposes a method for preparing manganese zinc ferrite using two ball milling processes, but such a method has at least the following disadvantages: 1. the method uses the traditional components to prepare the manganese-zinc ferrite, the traditional components limit the limit performance of the manganese-zinc ferrite, and the fact proves that the mechanical property of the ferrite of the traditional components is poor; 2. ball milling is carried out in the air atmosphere, so that a large amount of oxygen is adsorbed in the powder, and the oxygen reacts with the powder under the action of high temperature in the sintering process, so that the chemical components of a finished product deviate from the designed values, and the magnetic performance of the finished product is not ideal; 3. the particle size of the powder is not limited, so that a large amount of mechanical energy of ball milling is used for refining the particle size of the powder, and the aim of fully mixing the powder cannot be achieved; 4. the sintering process temperature is too low, hot-pressing sintering is not adopted, so that the structure of a finished product is not compact, the crystal grain structure is disordered, and the phenomenon of poor magnetic performance is reflected finally.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The invention aims to provide manganese-zinc ferrite and a preparation method thereof, thereby overcoming the defects of the prior art.
In order to achieve the purpose, the invention provides a preparation method of manganese-zinc ferrite, which is characterized by comprising the following steps: the preparation method comprises the following steps: providing and mixing Fe2O3、Mn3O4ZnO, CoO, NiO and CuO powder to obtain first mixed powder; carrying out first ball milling on the first mixed powder to obtain second mixed powder; performing first sintering treatment on the second mixed powder to obtain a first block; crushing the first block to obtain third mixed powder; performing second ball milling on the third mixed powder to obtain fourth mixed powder; and carrying out hot-pressing sintering treatment on the fourth mixed powder.
Preferably, in the above technical solution, in the first mixed powder, Mn is present in a weight percentage3O420-25 percent of ZnO, 4-7 percent of ZnO, 1-3 percent of CoO, 2-4 percent of NiO, 1-2 percent of CuO and the balance of Fe2O3。
Preferably, in the above technical solution, the first ball milling is performed in an argon atmosphere, and the process of the first ball milling is as follows: the rotating speed is 1000 plus 1500rpm, and the ball milling time is 30-40 min.
Preferably, in the above technical solution, the first sintering process is performed under a vacuum condition, and the conditions of the first sintering process are as follows: the air pressure is 0.01-0.05Pa, the sintering temperature is 850-870 ℃, and the sintering time is 5-7 h.
Preferably, in the above technical solution, the particle size of the third mixed powder is 50 to 100 μm.
Preferably, in the above technical solution, the second ball milling is performed in an argon atmosphere, and the process of the second ball milling is as follows: the rotating speed is 1500 plus 2000rpm, and the ball milling time is 45-60 min.
Preferably, in the above technical solution, the hot pressing sintering process is performed under a vacuum condition, and the conditions of the hot pressing sintering process are as follows: the air pressure is 0.01-0.05Pa, the pressure is 50-100MPa, the sintering temperature is 1400 ℃ and 1500 ℃, and the sintering time is 5-7 h.
The invention also provides manganese-zinc ferrite prepared by the method.
Compared with the prior art, the invention has the following beneficial effects:
1. aiming at the defects of the traditional ferrite formula, the invention designs a new ferrite formula, and by using the new formula, the magnetic property and the mechanical property of the ferrite are improved; 2. ball milling is carried out in argon atmosphere, so that the powder is prevented from adsorbing oxygen, and various properties of the powder are finally improved; 3. the particle size of the powder is particularly limited in the crushing process, so that the subsequent ball milling process can be smoothly carried out, and an ideal powder mixing effect is obtained; 4. the hot-pressing sintering process is optimized, so that the compactness of a finished product is greatly improved after the hot-pressing sintering treatment, the crystal grain structure is improved, and the magnetic property and the mechanical property are improved.
Detailed Description
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component. The device is a conventional device in the field, the raw materials used by the device can be purchased from chemical product stores, and the bending strength, fracture toughness, saturation magnetization and coercive force experiments are carried out according to related national standards.
Example 1
The manganese-zinc ferrite is prepared by the following method: providing and mixing Fe2O3、Mn3O4ZnO, CoO, NiO and CuO powder to obtain first mixed powder; carrying out first ball milling on the first mixed powder to obtain second mixed powder; performing first sintering treatment on the second mixed powder to obtain a first block; crushing the first block to obtain third mixed powder; performing second ball milling on the third mixed powder to obtain fourth mixed powder; and carrying out hot-pressing sintering treatment on the fourth mixed powder. In the first mixed powder, Mn in weight percent3O420 percent of ZnO, 4 percent of ZnO, 1 percent of CoO, 2 percent of NiO and 1 percent of CuO, and the balance being Fe2O3. The first ball milling is carried out in argon atmosphere, and the first ball milling process comprises the following steps: the rotating speed is 1000rpm, and the ball milling time is 40 min. The first sintering treatment is carried out under vacuum conditions, and the conditions of the first sintering treatment are as follows: the air pressure is 0.01Pa, the sintering temperature is 850 ℃, and the sintering time is 7 h. The particle size of the third mixed powder was 50 μm. The second ball milling is carried out in argon atmosphere, and the second ball milling process comprises the following steps: the rotating speed is 1500rpm, and the ball milling time is 60 min. The hot-pressing sintering treatment is carried out under the vacuum condition, and the conditions of the hot-pressing sintering treatment are as follows: the air pressure is 0.01Pa, the pressure is 100MPa, the sintering temperature is 1400 ℃, and the sintering time is 7 h.
Example 2
The manganese-zinc ferrite is prepared by the following method: providing and mixing Fe2O3、Mn3O4ZnO, CoO, NiO and CuO powder to obtain first mixed powder; carrying out first ball milling on the first mixed powder to obtain second mixed powder; performing first sintering treatment on the second mixed powder to obtain a first block; crushing the first block to obtain third mixed powder; performing second ball milling on the third mixed powder to obtain fourth mixed powder; and carrying out hot-pressing sintering treatment on the fourth mixed powder. In the first mixed powder, Mn in weight percent3O425 percent, 7 percent of ZnO, 3 percent of CoO, 4 percent of NiO and 2 percent of CuO, and the balance being Fe2O3. The first ball milling is carried out in argon atmosphere, and the first ball milling process comprises the following steps: the rotating speed is 1500rpm, and the ball milling time is 30 min. The first sintering treatment is carried out under vacuum conditions, and the conditions of the first sintering treatment are as follows: the air pressure is 0.05Pa, the sintering temperature is 870 ℃, and the sintering time is 5 h. The particle size of the third mixed powder was 100. mu.m. The second ball milling is carried out in argon atmosphere, and the second ball milling process comprises the following steps: the rotating speed is 2000rpm, and the ball milling time is 45 min. The hot-pressing sintering treatment is carried out under the vacuum condition, and the conditions of the hot-pressing sintering treatment are as follows: the air pressure is 0.05Pa, the pressure is 50MPa, the sintering temperature is 1500 ℃, and the sintering time is 5 h.
Example 3
The manganese-zinc ferrite is prepared by the following method: providing and mixing Fe2O3、Mn3O4ZnO, CoO, NiO and CuO powder to obtain first mixed powder; carrying out first ball milling on the first mixed powder to obtain second mixed powder; performing first sintering treatment on the second mixed powder to obtain a first block; crushing the first block to obtain third mixed powder; performing second ball milling on the third mixed powder to obtain fourth mixed powder; and carrying out hot-pressing sintering treatment on the fourth mixed powder. In the first mixed powder, Mn in weight percent3O423 percent, 6 percent of ZnO, 2 percent of CoO, 3 percent of NiO and 1.5 percent of CuO, and the balance being Fe2O3. The first ball milling is carried out in argon atmosphere, and the first ball milling process comprises the following steps: the rotating speed is 1200rpm, and the ball milling time is 35 min. The first sintering treatment is carried out under vacuum conditions, and the conditions of the first sintering treatment are as follows: the air pressure is 0.01Pa, the sintering temperature is 860 ℃ and the sintering time is 6 h. The particle size of the third mixed powder was 70 μm. The second ball milling is carried out in argon atmosphere, and the second ball milling process comprises the following steps: the rotating speed is 1800rpm, and the ball milling time is 50 min. The hot-pressing sintering treatment is carried out under the vacuum condition, and the conditions of the hot-pressing sintering treatment are as follows: the air pressure is 0.01Pa, the pressure is 70MPa, the sintering temperature is 1450 ℃, and the sintering time is 6 h.
Example 4
The manganese-zinc ferrite is prepared by the following method: providing and mixing Fe2O3、Mn3O4ZnO, CoO, NiO and CuO powder to obtain first mixed powder; carrying out first ball milling on the first mixed powder to obtain second mixed powder; and carrying out hot-pressing sintering treatment on the second mixed powder to obtain a finished product, wherein the hot-pressing sintering treatment process is the same as that of the example 3, and crushing and secondary ball milling are not carried out. The remaining conditions, processes, steps and parameters were the same as in example 3.
Example 5
The second mixed powder was subjected to cold isostatic pressing at a pressure of 300MPa for 30min without the first sintering treatment. The remaining conditions, processes, steps and parameters were the same as in example 3.
Example 6
In the first mixed powder, Mn in weight percent3O415% of ZnO and the balance of conditions, processes, steps and parameters were the same as those in example 3.
Example 7
In the first mixed powder, Mn in weight percent3O435% of ZnO and 5% of ZnO, and the other conditions, processes, steps and parameters were the same as those in example 3.
Example 8
In the first mixed powder, CoO was 5% by weight, and the remaining conditions, processes, steps, and parameters were the same as in example 3.
Example 9
The first mixed powder contained no CoO, and the remaining conditions, processes, steps, and parameters were the same as in example 3.
Example 10
In the first mixed powder, NiO accounted for 6% by weight, and the remaining conditions, processes, steps, and parameters were the same as in example 3.
Example 11
In the first mixed powder, NiO was 0.5% by weight, and the remaining conditions, processes, steps, and parameters were the same as in example 3.
Example 12
In the first mixed powder, CuO was 5% by weight, and the remaining conditions, processes, steps, and parameters were the same as those in example 3.
Example 13
In the first mixed powder, CuO was present in an amount of 0.5% by weight, and the remaining conditions, processes, steps, and parameters were the same as those in example 3.
Example 14
The first mixed powder contained no CuO and no NiO in percentage by weight, and the other conditions, processes, steps and parameters were the same as those of example 3.
Example 15
The first ball milling was carried out in an air atmosphere, and the remaining conditions, processes, steps, and parameters were the same as those in example 3.
Example 16
The first ball milling process comprises the following steps: the rotating speed is 800rpm, the ball milling time is 60min, and the rest conditions, processes, steps and parameters are the same as those of the embodiment 3.
Example 17
The conditions of the first sintering treatment were: the pressure is 0.01Pa, the sintering temperature is 800 ℃, the sintering time is 8h, and the rest conditions, processes, steps and parameters are the same as those of the embodiment 3.
Example 18
The conditions of the first sintering treatment were: the pressure is 0.01Pa, the sintering temperature is 900 ℃, the sintering time is 4h, and the rest conditions, processes, steps and parameters are the same as those of the embodiment 3.
Example 19
The particle size of the third mixed powder was 200 μm, and the remaining conditions, processes, steps, and parameters were the same as in example 3.
Example 20
The second ball milling process comprises the following steps: the rotating speed is 1000rpm, the ball milling time is 100min, and the rest conditions, processes, steps and parameters are the same as those of the embodiment 3.
Example 21
The second ball milling process comprises the following steps: the rotating speed is 2500rpm, the ball milling time is 100min, and the rest conditions, processes, steps and parameters are the same as those of the example 3.
Example 22
The conditions of the hot-pressing sintering treatment are as follows: the pressure is 70MPa, the sintering temperature is 1300 ℃, and the sintering time is 6 h. The remaining conditions, processes, steps and parameters were the same as in example 3.
Example 23
The hot-pressing sintering treatment is carried out under the vacuum condition, and the conditions of the hot-pressing sintering treatment are as follows: the pressure is 70MPa, the sintering temperature is 1600 ℃, and the sintering time is 6 h.
Example 24
The hot-pressing sintering treatment is carried out under the vacuum condition, and the conditions of the hot-pressing sintering treatment are as follows: the pressure is 70MPa, the sintering temperature is 1450 ℃, and the sintering time is 9 h.
Example 25
The hot-pressing sintering treatment is carried out under the vacuum condition, and the conditions of the hot-pressing sintering treatment are as follows: the pressure is 120MPa, the sintering temperature is 1450 ℃, and the sintering time is 4 h.
The labels manufactured in examples 1-25 were tested for flexural strength, fracture toughness, saturation magnetization, and coercivity, which are all well known in the art and are not described again. For comparison, the results of the flexural strength, fracture toughness, saturation magnetization, and coercive force were normalized with respect to the value of example 1. The results are shown in Table 1.
TABLE 1
Figure BDA0001536048890000081
Figure BDA0001536048890000091
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (1)

1. A preparation method of manganese-zinc ferrite is characterized by comprising the following steps: the preparation method comprises the following steps: providing and mixing Fe2O3、Mn3O4ZnO, CoO, NiO and CuO powder to obtain first mixed powder; carrying out first ball milling on the first mixed powder to obtain second mixed powder; performing first sintering treatment on the second mixed powder to obtain a first block; crushing the first block to obtain third mixed powder; performing second ball milling on the third mixed powder to obtain fourth mixed powder; and carrying out hot-pressing sintering treatment on the fourth mixed powder, wherein the Mn accounts for the weight percentage of the fourth mixed powder in the first mixed powder3O423 percent, 6 percent of ZnO, 2 percent of CoO, 3 percent of NiO and 1.5 percent of CuO, and the balance being Fe2O3The first ball milling is carried out in argon atmosphere, and the process of the first ball milling is as follows: the rotating speed is 1200rpm, the ball milling time is 35min, the first sintering treatment is carried out under the vacuum condition, and the conditions of the first sintering treatment are as follows: the pressure is 0.01Pa, the sintering temperature is 860 ℃, the sintering time is 6h, the particle size of the third mixed powder is 70 μm, the second ball milling is carried out in argon atmosphere, and the process of the second ball milling is as follows: the rotating speed is 1800rpm, the ball milling time is 50min, the hot pressing sintering treatment is carried out under the vacuum condition, and the conditions of the hot pressing sintering treatment are as follows: the air pressure is 0.01Pa, the pressure is 70MPa, the sintering temperature is 1450 ℃, and the sintering time is 6 h.
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Publication number Priority date Publication date Assignee Title
CN101429017A (en) * 2008-12-06 2009-05-13 广东风华高新科技股份有限公司 Ferrite magnetic core for network communication and method for producing the same
CN103265277A (en) * 2013-06-14 2013-08-28 南通飞来福磁铁有限公司 Preparation method of permanent magnetic ferrite
JP2014524873A (en) * 2011-08-09 2014-09-25 株式会社豊田中央研究所 Ferrite particles and manufacturing method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101429017A (en) * 2008-12-06 2009-05-13 广东风华高新科技股份有限公司 Ferrite magnetic core for network communication and method for producing the same
JP2014524873A (en) * 2011-08-09 2014-09-25 株式会社豊田中央研究所 Ferrite particles and manufacturing method thereof
CN103265277A (en) * 2013-06-14 2013-08-28 南通飞来福磁铁有限公司 Preparation method of permanent magnetic ferrite

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