CN110767406A - High-frequency high-impedance manganese-zinc ferrite and preparation method thereof - Google Patents

High-frequency high-impedance manganese-zinc ferrite and preparation method thereof Download PDF

Info

Publication number
CN110767406A
CN110767406A CN201910916643.3A CN201910916643A CN110767406A CN 110767406 A CN110767406 A CN 110767406A CN 201910916643 A CN201910916643 A CN 201910916643A CN 110767406 A CN110767406 A CN 110767406A
Authority
CN
China
Prior art keywords
sintering
temperature
frequency
manganese
sanding
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910916643.3A
Other languages
Chinese (zh)
Inventor
李申华
黄有东
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CHANGSHU SANJIA MAGNETIC Co Ltd
Original Assignee
CHANGSHU SANJIA MAGNETIC Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by CHANGSHU SANJIA MAGNETIC Co Ltd filed Critical CHANGSHU SANJIA MAGNETIC Co Ltd
Priority to CN201910916643.3A priority Critical patent/CN110767406A/en
Publication of CN110767406A publication Critical patent/CN110767406A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • H01F1/36—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 in the form of particles
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B35/2608—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead
    • C04B35/2633—Compositions containing one or more ferrites of the group comprising manganese, zinc, nickel, copper or cobalt and one or more ferrites of the group comprising rare earth metals, alkali metals, alkaline earth metals or lead containing barium, strontium or calcium
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
    • C04B2235/3263—Mn3O4
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3275—Cobalt oxides, cobaltates or cobaltites or oxide forming salts thereof, e.g. bismuth cobaltate, zinc cobaltite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6562—Heating rate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
    • C04B2235/6567—Treatment time
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • 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
    • C04B2235/6583—Oxygen containing atmosphere, e.g. with changing oxygen pressures

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Power Engineering (AREA)
  • Magnetic Ceramics (AREA)
  • Soft Magnetic Materials (AREA)

Abstract

The invention discloses a high-frequency high-impedance manganese-zinc ferrite and a preparation method thereof, wherein the high-frequency high-impedance manganese-zinc ferrite comprises a main component and a doping component; the main component comprises Fe2O372.0-73.0Wt%, ZnO 4.0-5.6Wt%, and Mn for the rest3O4The total amount is 100%; the doping component comprises Ca, Nb, Si, Zr, NiO and Co, and accounts for 0.21-1.7% of the total mass of the main component. The invention ensures higher use frequency and lower magnetic conductivity by adjusting the proportion of the main components; the crystal structure of the material is improved by improving the composition and the proportion of the doping components, so that the grains are fine and uniform, and the high-frequency low power consumption of the material is improved; and through a specific nitrogen kiln sintering process, crystal grains are refined, the resistivity of the product is improved, and the method further improves the yield of the productThe frequency of use is increased.

Description

High-frequency high-impedance manganese-zinc ferrite and preparation method thereof
Technical Field
The invention relates to the field of manganese-zinc ferrite magnetic rings, in particular to a high-frequency high-impedance manganese-zinc ferrite and a preparation method thereof.
Background
The soft magnetic ferrite is a soft magnetic material used earlier in a switching power supply transformer, and corresponding materials are developed one generation after another along with the increasing working frequency of the switching power supply. In the early 70 s, in order to meet the requirements of the switching power supply market, the first-generation power ferrite material is developed and is only suitable for civil switching power supplies with the working frequency of about 20 kHz. In the early 80 s, a second-generation power ferrite material appeared, which has negative temperature coefficient power consumption, the power consumption is in a descending trend along with the temperature rise, and the applicable working frequency is about 100 kHz. In the later 80 s, in order to adapt to the development of high-frequency switching power supplies, third-generation power ferrite materials are developed, and the working frequency of the third-generation power ferrite materials is about 250 kHz. In recent 2 years, due to the continuous development of electronic communication and network technology, the information technology puts higher demands on the miniaturization and the chip type of devices, the working frequency of the material is improved and gradually increased from 500kHz to 1MHZ, which contributes to the further lightness, smallness and thinness of the switching power supply,
soft magnetic ferrite materials are widely used and have a wide variety of functional materials. With the recent requirements of information technology and new green lighting, materials are further developed toward high frequency, high impedance and low loss. The devices are developed to miniaturization, sheet type and surface mounting.
At present, manufacturers for producing manganese-zinc ferrite materials in China cannot meet the requirements of the market, and the materials are urgently needed to be developed in small-batch production.
Disclosure of Invention
The invention mainly solves the technical problems that: aiming at the defects of the prior art, the high-frequency high-impedance manganese-zinc ferrite and the preparation method thereof are provided, have higher use frequency and lower magnetic conductivity, and also have the characteristics of low power consumption and high Curie temperature of the material.
In order to solve the technical problems, the invention adopts a technical scheme that: the high-frequency high-impedance manganese-zinc ferrite comprises a main component and a doping component; the main component comprises Fe2O372.0-73.0Wt%, ZnO 4.0-5.6Wt%, and Mn for the rest3O4The total amount is 100%; the doping component comprises Ca, Nb, Si, Zr, NiO and Co, and accounts for 0.21-1.7% of the total mass of the main component.
In a preferred embodiment of the invention, the Ca is controlled to be 0.03-0.1%, the Nb is controlled to be 0.02-0.06%, the Si is controlled to be 0.005-0.01%, the Zr is controlled to be 0.01-0.03%, the NiO is controlled to be 0.1-1.0%, and the Co is controlled to be 0.05-0.5%.
Also provides a preparation method of the high-frequency high-impedance manganese-zinc ferrite, which comprises the following steps:
(100) weighing: weighing the main component and the doped component according to the formula for later use;
(200) primary sanding: putting the weighed main components in the step (100) into a sand mill for sanding, and then drying to obtain a primary sand abrasive;
(300) pre-burning: putting the primary sand grinding material obtained in the step (200) into a pre-sintering furnace for pre-sintering to obtain pre-sintered powder;
(400) secondary sanding: adding the weighed doping components in the step (100) into the pre-sintering powder obtained in the step (300), then placing the pre-sintering powder into a sand mill for sanding, and then drying to obtain secondary sand abrasive;
(500) and (3) granulation: adding PVA with the concentration of 6-8% into the secondary sand grinding material obtained in the step (400) for granulation, and performing compression molding to obtain a molding material;
(600) and (3) sintering: and (5) placing the molding material obtained in the step (500) in a bell jar furnace, and sintering and molding at a certain sintering temperature according to an atmosphere curve of balanced oxygen partial pressure to obtain the high-frequency high-impedance manganese-zinc ferrite.
In a preferred embodiment of the invention, the total mass of the body components weighed in said step (100) is 2 kg.
In a preferred embodiment of the present invention, the duration of one sanding in the step (200) is 60 minutes.
In a preferred embodiment of the present invention, the temperature of the pre-firing in the step (300) is 960 ℃, and the time is 2.5 hours.
In a preferred embodiment of the present invention, the duration of the secondary sanding in the step (400) is 150 minutes.
In a preferred embodiment of the present invention, the sintering temperature in the step (600) is 1280-1300 ℃.
In a preferred embodiment of the present invention, during the sintering in the step (600), the temperature is first raised from room temperature to 650 ℃ at a heating rate of 1-1.5 ℃/min in the atmospheric atmosphere, then raised from 650 ℃ to 1080 ℃ at a heating rate of 1-1.5 ℃/min under the condition of balanced oxygen partial pressure, and then raised from 1080 ℃ to 1280-1300 ℃ at a heating rate of 5-7 ℃/min, and the temperature is maintained for 3.5-6.5 h.
In a preferred embodiment of the present invention, during the cooling in the step (600), the temperature is first decreased from 1280-1300 ℃ to 1080 ℃ at a temperature decrease rate of 1.5-2 ℃/min under an oxygen partial pressure of 1-3%, then decreased from 1080 ℃ to 500 ℃ at a temperature decrease rate of 5-7 ℃/min under an oxygen partial pressure of 0.5-1.5%, and finally decreased to room temperature at a temperature decrease rate of 2.5-3 ℃/min under an oxygen partial pressure of 0.01-0.05%.
The invention has the beneficial effects that: the main composition formula of the product is changed into an iron-rich formula and the content of zinc oxide is reduced by adjusting the proportion of main components, so that higher use frequency and lower magnetic conductivity are ensured; the crystal structure of the material is improved by improving the composition and the proportion of the doping components, so that the grains are fine and uniform, and the high-frequency low power consumption of the material is improved; and through a specific nitrogen kiln sintering process, crystal grains are refined, the resistivity of the product is improved, and the use frequency is further improved.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
Example one
A high-frequency high-impedance manganese-zinc ferrite comprises a main component and a doping component; the main component comprises Fe2O372.0wt%、ZnO 4.0Wt%，Mn3O424 Wt% to ensure higher use frequency and lower magnetic permeability; the doping component comprises Ca, Nb, Si, Zr, NiO and Co, and accounts for 0.215 percent of the total mass of the main component; wherein the content of Ca is 0.03%, the content of Nb is 0.02%, the content of Si is 0.005%, the content of Zr is 0.01%, the content of NiO is 0.1%, and the content of Co is 0.05%. By selecting high-purity and high-specific surface area raw materials, the density of the product is increased, crystal grains are refined, the crystal structure is improved, and the product is further improvedHigh Bs and low power consumption, and improves the use frequency.
The preparation method of the high-frequency high-impedance manganese-zinc ferrite comprises the following steps:
(100) weighing: weighing the main component and the doped component according to the formula for later use; the total mass of the main components is 2 kg;
(200) primary sanding: putting the weighed main components in the step (100) into a sand mill, sanding for 60 minutes, and then drying to obtain a primary sand abrasive;
(300) pre-burning: putting the primary sand grinding material obtained in the step (200) into a pre-sintering furnace for pre-sintering, wherein the temperature during pre-sintering is 960 ℃, and the time is 2.5 hours, so as to obtain pre-sintered powder;
(400) secondary sanding: adding the weighed doping components in the step (100) into the pre-sintering powder obtained in the step (300), then placing the pre-sintering powder into a sand mill for sanding for 150 minutes, and then drying to obtain a secondary sand abrasive;
(500) and (3) granulation: adding PVA with the concentration of 6% into the secondary sand grinding material obtained in the step (400) for granulation, and performing compression molding to obtain a molding material;
(600) and (3) sintering: placing the molding material obtained in the step (500) in a bell jar furnace, and sintering and molding at a sintering temperature of 1280 ℃ according to an atmosphere curve of balanced oxygen partial pressure, wherein the specific steps are as follows: firstly, in the atmosphere, heating from room temperature to 650 ℃ at the heating rate of 1 ℃/min, then under the condition of balanced oxygen partial pressure, heating from 650 ℃ to 1080 ℃ at the heating rate of 1 ℃/min, then heating from 1080 ℃ to 1280 ℃ at the heating rate of 5 ℃/min, and preserving heat for 3.5 hours; then firstly reducing the temperature from 1280 ℃ to 1080 ℃ at the cooling rate of 1.5 ℃/min under the oxygen partial pressure of 1 percent, then reducing the temperature from 1080 ℃ to 500 ℃ at the cooling rate of 5 ℃/min under the oxygen partial pressure of 0.5 percent, and finally reducing the temperature to the room temperature at the cooling rate of 2.5 ℃/min under the oxygen partial pressure of 0.01 percent to obtain the high-frequency high-impedance manganese zinc ferrite with the specification of 25mm multiplied by 15 mm multiplied by 8 mm.
Example two
A high-frequency high-impedance manganese-zinc ferrite comprises a main component and a doping component; the main component comprises Fe2O373.0wt%、ZnO 5.6Wt%，Mn3O421.4 Wt% to ensure higher use frequency and lower magnetic permeability; the doping component comprises Ca, Nb, Si, Zr, NiO and Co, and accounts for 1.7% of the total mass of the main component; wherein the content of Ca is 0.1%, the content of Nb is 0.06%, the content of Si is 0.01%, the content of Zr is 0.03%, the content of NiO is 1.0%, and the content of Co is 0.5%. By selecting raw materials with high purity and high specific surface area, the density of the product is improved, crystal grains are refined, the crystal structure is improved, Bs (saturation area) is further improved, the power consumption is low, and the use frequency is improved.
The preparation method of the high-frequency high-impedance manganese-zinc ferrite comprises the following steps:
(100) weighing: weighing the main component and the doped component according to the formula for later use; the total mass of the main components is 2 kg;
(200) primary sanding: putting the weighed main components in the step (100) into a sand mill, sanding for 60 minutes, and then drying to obtain a primary sand abrasive;
(300) pre-burning: putting the primary sand grinding material obtained in the step (200) into a pre-sintering furnace for pre-sintering, wherein the temperature during pre-sintering is 960 ℃, and the time is 2.5 hours, so as to obtain pre-sintered powder;
(400) secondary sanding: adding the weighed doping components in the step (100) into the pre-sintering powder obtained in the step (300), then placing the pre-sintering powder into a sand mill for sanding for 150 minutes, and then drying to obtain a secondary sand abrasive;
(500) and (3) granulation: adding PVA with the concentration of 8% into the secondary sand grinding material obtained in the step (400) for granulation, and performing compression molding to obtain a molding material;
(600) and (3) sintering: and (3) placing the molding material obtained in the step (500) in a bell jar furnace, and sintering and molding at the sintering temperature of 1300 ℃ according to the atmosphere curve of the balanced oxygen partial pressure, wherein the specific steps are as follows: firstly, in the atmosphere, the temperature is increased from room temperature to 650 ℃ at the temperature increase rate of 1.5 ℃/min, then under the condition of balanced oxygen partial pressure, the temperature is increased from 650 ℃ to 1080 ℃ at the temperature increase rate of 1.5 ℃/min, then the temperature is increased from 1080 ℃ to 1300 ℃ at the temperature increase rate of 7 ℃/min, and the temperature is kept for 6.5 hours; then firstly reducing the temperature from 1300 ℃ to 1080 ℃ at the cooling rate of 2 ℃/min under the oxygen partial pressure of 3 percent, then reducing the temperature from 1080 ℃ to 500 ℃ at the cooling rate of 7 ℃/min under the oxygen partial pressure of 1.5 percent, and finally reducing the temperature to the room temperature at the cooling rate of 3 ℃/min under the oxygen partial pressure of 0.05 percent to obtain the high-frequency high-impedance manganese-zinc ferrite with the specification of 25mm multiplied by 15 mm multiplied by 8 mm.
EXAMPLE III
A high-frequency high-impedance manganese-zinc ferrite comprises a main component and a doping component; the main component comprises Fe2O373.0wt%、ZnO 5.6Wt%，Mn3O421.4 Wt% to ensure higher use frequency and lower magnetic permeability; the doping component comprises Ca, Nb, Si, Zr, NiO and Co, and accounts for 0.96% of the total mass of the main component; wherein the content of Ca is 0.065%, the content of Nb is 0.04%, the content of Si is 0.01%, the content of Zr is 0.02%, the content of NiO is 0.55%, and the content of Co is 0.275%. By selecting raw materials with high purity and high specific surface area, the density of the product is improved, crystal grains are refined, the crystal structure is improved, Bs (saturation area) is further improved, the power consumption is low, and the use frequency is improved.
The preparation method of the high-frequency high-impedance manganese-zinc ferrite comprises the following steps:
(100) weighing: weighing the main component and the doped component according to the formula for later use; the total mass of the main components is 2 kg;
(200) primary sanding: putting the weighed main components in the step (100) into a sand mill, sanding for 60 minutes, and then drying to obtain a primary sand abrasive;
(300) pre-burning: putting the primary sand grinding material obtained in the step (200) into a pre-sintering furnace for pre-sintering, wherein the temperature during pre-sintering is 960 ℃, and the time is 2.5 hours, so as to obtain pre-sintered powder;
(400) secondary sanding: adding the weighed doping components in the step (100) into the pre-sintering powder obtained in the step (300), then placing the pre-sintering powder into a sand mill for sanding for 150 minutes, and then drying to obtain a secondary sand abrasive;
(500) and (3) granulation: adding PVA with the concentration of 7% into the secondary sand grinding material obtained in the step (400) for granulation, and performing compression molding to obtain a molding material;
(600) and (3) sintering: and (3) placing the molding material obtained in the step (500) in a bell jar furnace, and sintering and molding at the sintering temperature of 1290 ℃ according to the atmosphere curve of the balanced oxygen partial pressure, wherein the specific steps are as follows: firstly, in the atmosphere, heating from room temperature to 650 ℃ at the heating rate of 1 ℃/min, then under the condition of balanced oxygen partial pressure, heating from 650 ℃ to 1080 ℃ at the heating rate of 1.5 ℃/min, then heating from 1080 ℃ to 1290 ℃ at the heating rate of 6 ℃/min, and keeping the temperature for 4.5 h; then firstly reducing the temperature from 1290 ℃ to 1080 ℃ at the cooling rate of 1.5 ℃/min under the oxygen partial pressure of 2 percent, then reducing the temperature from 1080 ℃ to 500 ℃ at the cooling rate of 6 ℃/min under the oxygen partial pressure of 1 percent, and finally reducing the temperature to room temperature at the cooling rate of 2.5 ℃/min under the oxygen partial pressure of 0.03 percent to obtain the high-frequency high-impedance manganese-zinc ferrite with the specification of 25mm multiplied by 15 mm multiplied by 8 mm.
The high-frequency high-impedance manganese-zinc ferrite obtained by the method has the initial magnetic conductivity of 1200 +/-25% at 25 ℃ through testing; the power loss is 180Kw/m under the test conditions of 500KHZ, 50mT and 25 DEG C3The power loss is 120Kw/m under the test condition of 1MHZ, 30mT and 100 DEG C3(ii) a Curie temperature is more than or equal to 240 ℃; the saturation magnetic flux density Bs is more than or equal to 480mT under the conditions of 25 ℃ and 1200A/m; under the condition of 100 ℃ and H =1200A/m, the saturation magnetic flux density Bs is not less than 415 mT.
The invention discloses a high-frequency high-impedance manganese-zinc ferrite and a preparation method thereof, wherein a main composition formula of a product is changed into an iron-rich formula and the content of zinc oxide is reduced through the proportioning adjustment of main components so as to ensure higher use frequency and lower magnetic conductivity; the crystal structure of the material is improved by improving the composition and the proportion of the doping components, so that the grains are fine and uniform, and the high-frequency low power consumption of the material is improved; and through a specific nitrogen kiln sintering process, crystal grains are refined, the resistivity of the product is improved, and the use frequency is further improved.
In the description of the present invention, it should be noted that the terms "upper", "lower", "left", "right", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown or the orientations or positional relationships that the products of the present invention usually place when using, and are used only for convenience of describing the present invention and simplifying the description, but do not indicate or imply that the device or the element that is referred to must have a specific orientation, be constructed in a specific orientation, and operate, and thus, should not be construed as limiting the present invention. The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. The high-frequency high-impedance manganese-zinc ferrite is characterized by comprising a main component and a doping component; the main component comprises Fe2O372.0-73.0Wt%, ZnO 4.0-5.6Wt%, and Mn for the rest3O4The total amount is 100%; the doping component comprises Ca, Nb, Si, Zr, NiO and Co, and accounts for 0.21-1.7% of the total mass of the main component.
2. The manganese-zinc-ferrite with high frequency and high impedance as claimed in claim 1, wherein said Ca is controlled to be 0.03-0.1%, said Nb is controlled to be 0.02-0.06%, said Si is controlled to be 0.005-0.01%, said Zr is controlled to be 0.01-0.03%, said NiO is controlled to be 0.1-1.0%, and said Co is controlled to be 0.05-0.5%.
3. A method for preparing a high frequency high impedance manganese zinc ferrite as claimed in any one of claims 1 to 2, comprising the steps of:
(100) weighing: weighing the main component and the doped component according to the formula for later use;
(200) primary sanding: putting the weighed main components in the step (100) into a sand mill for sanding, and then drying to obtain a primary sand abrasive;
(300) pre-burning: putting the primary sand grinding material obtained in the step (200) into a pre-sintering furnace for pre-sintering to obtain pre-sintered powder;
(400) secondary sanding: adding the weighed doping components in the step (100) into the pre-sintering powder obtained in the step (300), then placing the pre-sintering powder into a sand mill for sanding, and then drying to obtain secondary sand abrasive;
(500) and (3) granulation: adding PVA with the concentration of 6-8% into the secondary sand grinding material obtained in the step (400) for granulation, and performing compression molding to obtain a molding material;
(600) and (3) sintering: and (5) placing the molding material obtained in the step (500) in a bell jar furnace, and sintering and molding at a certain sintering temperature according to an atmosphere curve of balanced oxygen partial pressure to obtain the high-frequency high-impedance manganese-zinc ferrite.
4. The method for preparing high-frequency high-impedance manganese-zinc-ferrite according to claim 3, wherein the total mass of the bulk components weighed in the step (100) is 2 kg.
5. The method for preparing high-frequency high-impedance manganese-zinc ferrite according to claim 3, wherein the duration of one-time sanding in the step (200) is 60 minutes.
6. The method as claimed in claim 3, wherein the pre-sintering in the step (300) is performed at a temperature of 960 ℃ for 2.5 hours.
7. The method for preparing high-frequency high-impedance manganese-zinc ferrite according to claim 3, wherein the duration of the secondary sanding in the step (400) is 150 minutes.
8. The method as claimed in claim 3, wherein the sintering temperature in step (600) is 1280-1300 ℃.
9. The method as claimed in claim 8, wherein the step (600) of sintering is performed by first raising the temperature from room temperature to 650 ℃ at a rate of 1-1.5 ℃/min in an atmospheric atmosphere, then raising the temperature from 650 ℃ to 1080 ℃ at a rate of 1-1.5 ℃/min under the condition of balanced oxygen partial pressure, and then raising the temperature from 1080 ℃ to 1280 ℃ and 1300 ℃ at a rate of 5-7 ℃/min, and keeping the temperature for 3.5-6.5 h.
10. The method as claimed in claim 8, wherein the cooling in step (600) is performed by cooling from 1280 ℃. — > 1300 ℃ to 1080 ℃ at a cooling rate of 1.5-2 ℃/min under an oxygen partial pressure of 1-3%, cooling from 1080 ℃ to 500 ℃ at a cooling rate of 5-7 ℃/min under an oxygen partial pressure of 0.5-1.5%, and finally cooling to room temperature at a cooling rate of 2.5-3 ℃/min under an oxygen partial pressure of 0.01-0.05%.
CN201910916643.3A 2019-09-26 2019-09-26 High-frequency high-impedance manganese-zinc ferrite and preparation method thereof Pending CN110767406A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910916643.3A CN110767406A (en) 2019-09-26 2019-09-26 High-frequency high-impedance manganese-zinc ferrite and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910916643.3A CN110767406A (en) 2019-09-26 2019-09-26 High-frequency high-impedance manganese-zinc ferrite and preparation method thereof

Publications (1)

Publication Number Publication Date
CN110767406A true CN110767406A (en) 2020-02-07

Family

ID=69330421

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910916643.3A Pending CN110767406A (en) 2019-09-26 2019-09-26 High-frequency high-impedance manganese-zinc ferrite and preparation method thereof

Country Status (1)

Country Link
CN (1) CN110767406A (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1793020A (en) * 2005-11-17 2006-06-28 上海交通大学 High performant low consumption manganese zine ferrite material and preparation process thereof
CN104211385A (en) * 2013-05-28 2014-12-17 Tdk株式会社 Ferrite core and transformer
CN106007696A (en) * 2016-05-13 2016-10-12 泰州茂翔电子器材有限公司 Wide-temperature-range high-Bs ferrite material and preparing technology thereof
JP2017149610A (en) * 2016-02-25 2017-08-31 株式会社トーキン Ferrite, ferrite core and method for producing ferrite core
CN108129143A (en) * 2018-01-18 2018-06-08 常熟市三佳磁业有限公司 High superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1793020A (en) * 2005-11-17 2006-06-28 上海交通大学 High performant low consumption manganese zine ferrite material and preparation process thereof
CN104211385A (en) * 2013-05-28 2014-12-17 Tdk株式会社 Ferrite core and transformer
JP2017149610A (en) * 2016-02-25 2017-08-31 株式会社トーキン Ferrite, ferrite core and method for producing ferrite core
CN106007696A (en) * 2016-05-13 2016-10-12 泰州茂翔电子器材有限公司 Wide-temperature-range high-Bs ferrite material and preparing technology thereof
CN108129143A (en) * 2018-01-18 2018-06-08 常熟市三佳磁业有限公司 High superimposed characteristics wide temperature low-power consumption Mn-Zn soft magnetic ferrite and preparation method thereof

Similar Documents

Publication Publication Date Title
CN108129143B (en) High-superposition-characteristic wide-temperature low-power-consumption manganese-zinc soft magnetic ferrite and preparation method thereof
CN107324794B (en) Manganese-zinc ferrite material with wide frequency band, high impedance and high Curie temperature and preparation method thereof
CN111943658B (en) Wide-temperature-range low-loss MnZn ferrite material and preparation method thereof
CN111233452B (en) High-frequency high-impedance lean iron manganese zinc ferrite and preparation method thereof
CN111205075B (en) Nickel-zinc ferrite material and preparation method thereof
CN110204325B (en) Ferrite material and preparation method thereof
CN101807463A (en) MnZn ferrite material of high initial permeability and low loss and preparation method thereof
CN108863336B (en) Nickel microwave ferrite substrate material and preparation method thereof
CN108706968A (en) A kind of anti-direct current biasing NiCuZn ferrites of low-temperature sintering and preparation method
CN108275994B (en) Manganese-zinc ferrite with wide temperature range, low power consumption and high direct current superposition characteristic and preparation method thereof
CN107176830A (en) A kind of preparation method of high permeability MnZn ferrite
CN114195500B (en) Wide-temperature high-frequency high-magnetic-flux-density manganese-zinc soft magnetic ferrite for charging pile and preparation method thereof
CN104529426A (en) High-Bs low-loss manganese-zinc ferrite material applicable to 120-160 DEG C and manufacturing method thereof
CN112194482B (en) Ultralow-loss wide-temperature-power MnZn ferrite, preparation method and application thereof in 5G communication field
CN111116188B (en) Manganese-zinc high-magnetic-permeability high-Curie-temperature high-frequency high-magnetic-flux material and preparation method thereof
CN110767406A (en) High-frequency high-impedance manganese-zinc ferrite and preparation method thereof
CN115340372B (en) Low-stress-sensitivity high-frequency manganese zinc ferrite material and preparation method thereof
WO2012151714A1 (en) Nicuzn ferrite material with high magnetic conductivity
CN114031388B (en) Mn-Zn ferrite material and preparation method thereof
CN115894005A (en) Nickel-zinc ferrite material and preparation method and application thereof
CN114773047A (en) Broadband high-impedance manganese-zinc ferrite material and preparation method and application thereof
CN109320230B (en) Preparation method of manganese-zinc soft magnetic ferrite material with four high characteristics
JP2007297232A (en) Method for producing oxide magnetic material
US20240006103A1 (en) MnZn-BASED FERRITE AND METHOD FOR PRODUCING SAME
CN113636838A (en) Nickel-zinc ferrite material and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20200207