CN108711481B - MnZn ferrite magnetic sheet and preparation method and application thereof - Google Patents

MnZn ferrite magnetic sheet and preparation method and application thereof Download PDF

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CN108711481B
CN108711481B CN201810756353.2A CN201810756353A CN108711481B CN 108711481 B CN108711481 B CN 108711481B CN 201810756353 A CN201810756353 A CN 201810756353A CN 108711481 B CN108711481 B CN 108711481B
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magnetic sheet
ferrite magnetic
mnzn ferrite
sintering
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CN108711481A (en
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王朝明
於扬栋
赵旭
卢飞翔
陈新彬
吕飞雨
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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    • 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
    • C—CHEMISTRY; METALLURGY
    • 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
    • C04B35/2658—Other ferrites containing manganese or zinc, e.g. Mn-Zn ferrites
    • 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
    • H01F41/02—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 for manufacturing cores, coils, or magnets
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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
    • C04B2235/656—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
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    • 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
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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
    • C04B2235/656—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
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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Abstract

The invention provides a MnZn ferrite magnetic sheet and a magnetic sheet thereofA preparation method and application. The MnZn ferrite magnetic sheet comprises iron element, manganese element and zinc element, wherein the iron element is Fe2O3In the form of ZnO, zinc in the form of ZnO, manganese in the form of MnO, and Fe in said MnZn ferrite magnetic sheet2O3The MnZn ferrite magnetic sheet comprises 48.5-50 mol% of ZnO, 15-24 mol% of ZnO and the balance of MnO, and the thickness of the MnZn ferrite magnetic sheet is 0.03-0.3 mm. The preparation method comprises the following steps: (1) proportioning, (2) presintering, (3) primary grinding, (4) secondary grinding and pulping, (5) casting and sintering. The MnZn ferrite magnetic sheet provided by the invention has the advantages of thin thickness, high magnetic conductivity, high saturation magnetic induction intensity and high Curie temperature.

Description

MnZn ferrite magnetic sheet and preparation method and application thereof
Technical Field
The invention belongs to the technical field of electronic materials, and particularly relates to a MnZn ferrite magnetic sheet and a preparation method and application thereof.
Background
Wireless charging technology (wireless charging technology) is a power transmission technology without wiring, also called non-contact inductive charging, in which power is transmitted to a power consumption device by a power supply device, and a transmitting end (charger) and a receiving end (power consumption device) are not connected by a wire. Because this charging device conveniently carries and uses, at first showed wide application prospect in mobile intelligent equipment. The wireless charging technology is realized by means of electromagnetic induction, magnetic resonance, radio waves and the like.
At present, the demand of the electromagnetic induction technology with fast market speed and the magnetic resonance technology with wide prospect on magnetic materials is huge, and the related magnetic materials comprise soft magnetic materials and permanent magnets. The soft magnetic ferrite material has higher initial permeability and higher resistivity, and is manufactured by a casting process and is easy to thin and process, so that the soft magnetic ferrite material plays a role in increasing the induction magnetic field strength and shielding the coil magnetic field in a wireless charging system. The soft magnetic ferrite material adopted at present is NiZn ferrite, but the highest magnetic permeability of the NiZn ferrite material is only 500-700, the Curie temperature is only 90 ℃, and the saturation magnetic induction density Bs is below 300mT, so that the wireless charging magnetic sheet made of the NiZn material has the defects of low charging efficiency, low use temperature and the like in the use process.
CN103117146A discloses a ferrite magnetic block with high Curie temperature, low loss and high strength and a preparation method thereof. The ferrite magnetic block provided by the scheme mainly comprises iron oxide, manganese oxide and zinc oxide, the auxiliary raw materials comprise calcium carbonate, titanium oxide, cobalt oxide, silicon oxide, chromium oxide, niobium oxide, nickel oxide and copper oxide, and the main raw materials comprise the following components: 55-61 mol% Fe2O3Iron oxide calculated, manganese oxide calculated as MnO in an amount of 33 to 40 mol% and zinc oxide calculated as ZnO in an amount of 5 to 10 mol%; the addition amount of the auxiliary raw materials relative to the total weight of the main raw materials is as follows: CaCO3:500-3000ppm，TiO2:80-3000ppm，Co2O350-1200ppm of superfine SiO2：20-200ppm，Cr2O3:100-1500ppm，Nb2O5100 and 1500ppm, NiO: 600-2000ppm and CuO: 600 and 2000 ppm.
CN102795851A discloses a ferrite composition and an electronic component, the ferrite composition comprises Fe2O3Iron oxide in a content of 63.3 to 65.5 mol% in terms of ZnO, zinc oxide in a content of 11.6 to 15.8 mol% in terms of ZnO, and the balance manganese oxide, wherein the main component is composed of SiO in an amount of 100 wt% of the main component2The silica content is 60 to 250ppm in terms of silica, the calcium oxide content is 360 to 1000ppm in terms of CaO, the Pb content is 7ppm or less in terms of element, and the Cd content is 7ppm or less in terms of element.
CN102964117A discloses a wide temperature MnZn power ferrite material, which is composed of a main component and an auxiliary component, wherein the mole percentages of the components of the main component are: fe2O352.7-52.8 mol%, ZnO 9.2-9.8 mol%, and MnO in balance; the auxiliary component accounts for 0.505 to 0.685 percent of the total weight of the main component, and the auxiliary component is CaCO3、ZrO2、Nb2O5、SnO2And Co2O3And (4) forming. The invention has low loss characteristic in the temperature range of 25 ℃ and 140 ℃ and simultaneously has the characteristic of high Bs.
However, the above schemes require the addition of additive components to the MnZn ferrite material, which increases the manufacturing cost, and cannot make the MnZn ferrite magnetic sheet thin to meet the requirement of wireless charging.
Therefore, it is important to develop a MnZn ferrite magnetic sheet having a thinner thickness and a lower cost, and having advantages of a high magnetic permeability, a high saturation magnetic induction Bs, a high curie temperature, and the like, in the art.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a MnZn ferrite magnetic sheet and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a MnZn ferrite magnetic sheet comprising an iron element, a manganese element and a zinc element, wherein the iron element is Fe2O3In the form of ZnO, zinc in the form of ZnO, manganese in the form of MnO, and Fe in said MnZn ferrite magnetic sheet2O3The MnZn ferrite magnetic sheet comprises 48.5-50 mol% of ZnO, 15-24 mol% of ZnO and the balance of MnO, and the thickness of the MnZn ferrite magnetic sheet is 0.03-0.3 mm.
Fe in MnZn ferrite magnetic sheet of the invention2O3The molar percentage of (b) is 48.5 to 50 mol%, for example, 48.5 mol%, 48.8 mol%, 49 mol%, 49.2 mol%, 49.5 mol%, 49.7 mol% or 50 mol%, etc., but not limited to the values listed, and other values not listed in the numerical range are also applicable. The ZnO is 15 to 24 mol%, for example, 15 mol%, 16 mol%, 17 mol%, 18 mol%, 19 mol%, 20 mol%, 21 mol%, 22 mol%, 23 mol%, or 24 mol%, but is not limited to the values listed, and other values not listed within the numerical range are also applicable.
In the present invention, the thickness of the MnZn ferrite magnetic sheet is 0.03 to 0.3mm, for example, 0.03mm, 0.06mm, 0.1mm, 0.15mm, 0.2mm, 0.25mm, or 0.3mm, but is not limited to the values listed above, and other values not listed above within the range of the values are also applicable.
The MnZn ferrite magnetic sheet provided by the invention is very thin, is very beneficial to wireless charging application, and has high magnetic conductivity, high saturation magnetic induction density Bs, high Curie temperature Tc and high resistivity rho. The proper component ratio of the MnZn ferrite magnetic sheet provided by the present invention also plays an important role in achieving such effects, for example, Fe2O3Is relatively low, contributing to an increase in resistivity. The MnZn ferrite magnetic sheet provided by the invention does not contain auxiliary components.
The following is a preferred technical solution of the present invention, but not a limitation to the technical solution provided by the present invention, and the technical objects and advantageous effects of the present invention can be better achieved and achieved by the following preferred technical solution.
As the preferable technical scheme of the invention, the area of the MnZn ferrite magnetic sheet is 0.25-160 cm2E.g. 0.25cm2、0.5cm2、1cm2、10cm2、20cm2、40cm2、60cm2、80cm2、100cm2、120cm2、140cm2Or 160cm2And the like, but are not limited to the recited values, and other values not recited within the numerical range are also applicable. Such a large area of the MnZn ferrite magnetic sheet is advantageous for practical use of the magnetic sheet, and since the MnZn ferrite magnetic sheet provided by the present invention is excellent in properties and high in flatness, such a large area can be obtained.
Preferably, polyethylene terephthalate films are attached to both surfaces of the MnZn ferrite magnetic sheet.
The magnetic sheet with the thickness of 0.03-0.3 mm provided by the invention has the following properties after being pasted with a film and split: under the conditions of 25 ℃, 128KHz and 0.25mT, the real part mu' of the magnetic conductivity is about 600-1500; saturation magnetic induction at 25 deg.C, 50Hz and 1194A/mBs is about 280-450 mT; curie temperature Tc of about 90 to 120 ℃, resistivity rho of about 20 to 3 x 103Ω·m。
In a second aspect, the present invention provides a method for producing a MnZn ferrite magnetic sheet as described in the first aspect, comprising the steps of:
(1) mixing and crushing the metal oxide raw materials according to the formula amount, and then granulating to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) to obtain pre-burned powder;
(3) crushing the pre-sintering powder in the step (2), and then drying to obtain dried powder;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer to obtain slurry;
(5) and (3) carrying out tape casting on the slurry obtained in the step (4) to obtain a green sheet, heating the green sheet to 950-1200 ℃, sintering, and cooling in two stages after sintering to obtain the MnZn ferrite magnetic sheet.
In the step (5) of the present invention, the green sheet is heated to a sintering temperature of 950 to 1200 ℃, for example, 950 ℃, 1000 ℃, 1050 ℃, 1100 ℃, 1150 ℃, 1200 ℃ or the like, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned range of values are also applicable. In the invention, if the sintering temperature is too low, the real part of the magnetic conductivity and the saturation magnetic induction intensity Bs of the MnZn ferrite magnetic sheet are reduced, and the product performance is seriously influenced; if the sintering temperature is too high, the MnZn ferrite magnetic sheet is warped around, bulged in the middle, uneven and unusable.
In the preparation method provided by the invention, the sintering process in the step (5) plays an important role in solving the flatness problem of the MnZn ferrite magnetic sheet.
As a preferable technical scheme of the invention, in the step (1), the metal oxide raw material comprises Fe2O3、Mn3O4And ZnO.
Preferably, the method of mixing and crushing is sanding.
Preferably, the sanding is performed in a sand mill.
Preferably, water is added during the sanding.
Preferably, the mixing and crushing time in step (1) is 20-60 min, such as 20min, 30min, 40min, 50min or 60min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, step (1) further comprises: and mixing and crushing, circularly mixing for 5-15min, and then granulating. The time of the cyclic mixing is 5-15min, such as 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min or 15min, but is not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the method of circulating mixing is stirring in a stirring tank.
Preferably, the granulation method in step (1) is spray granulation.
In a preferred embodiment of the present invention, the temperature of the pre-firing in the step (2) is 750 to 950 ℃, for example, 750 ℃, 775 ℃, 800 ℃, 825 ℃, 850 ℃, 875 ℃, 900 ℃, 925 ℃ or 950 ℃, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range of values are also applicable.
Preferably, the time for the pre-firing in the step (2) is 1 to 3 hours, for example, 1 hour, 1.5 hours, 2 hours, 2.5 hours or 3 hours, but is not limited to the values listed, and other values not listed in the range of the values are also applicable.
Preferably, the crushing method in step (3) is sand grinding.
Preferably, the sanding is performed in a sand mill.
Preferably, water is added during the sanding.
Preferably, the time for the crushing in step (3) is 20-60 min, such as 20min, 30min, 40min, 50min or 60min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, the drying method in step (3) is drying or spray drying.
Preferably, the moisture content of the dried powder of step (3) is below 0.1%, such as 0.09%, 0.08%, 0.07%, 0.06%, 0.05%, or 0.04%, etc.
As a preferred technical scheme of the invention, the organic solvent in the step (4) comprises ethanol.
Preferably, the binder of step (4) comprises polyvinyl alcohol.
Preferably, the plasticizer of step (4) comprises dioctyl phthalate.
Preferably, the grinding time in step (4) is 8-20 h, such as 8h, 10h, 12h, 14h, 16h, 18h or 20h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
As a preferable embodiment of the present invention, the thickness of the green sheet in the step (5) is 0.03 to 0.3mm, for example, 0.03mm, 0.06mm, 0.1mm, 0.15mm, 0.2mm, 0.25mm, or 0.3mm, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned numerical range are also applicable.
The specific process of the tape casting in the step (5) of the invention is as follows: the slurry is uniformly coated on a polyethylene terephthalate (PET) base film according to a set thickness by a casting device, and a ferrite green sheet can be obtained after the slurry on the PET base film is dried.
Preferably, the sintering of step (5) is performed in a sintering furnace.
Preferably, in step (5), the green sheet is mounted on a flat alumina plate or zirconia plate and then placed in a sintering furnace.
Preferably, in step (5), the temperature raising rate of the temperature raising is less than or equal to 0.8 ℃/min, such as 0.8 ℃/min, 0.7 ℃/min, 0.6 ℃/min, 0.5 ℃/min, 0.4 ℃/min and the like.
Preferably, in the step (5), the sintering time is 1-5 h, such as 1h, 2h, 3h, 4h or 5h, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, in step (5), the sintered oxygen content is 1% to 21%, for example 1%, 5%, 10%, 15%, 20%, 21%, etc., but is not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, in step (5), the first stage of the two-stage cooling has a cooling rate of 1.0 to 3.0 ℃/min, such as 1 ℃/min, 1.5 ℃/min, 2 ℃/min, 2.5 ℃/min, or 3 ℃/min, but not limited to the recited values, and other values not recited within the range of values are also applicable.
Preferably, in step (5), the first stage of the two-stage cooling reduces the temperature to 900 ℃.
Preferably, in step (5), the oxygen content of the first stage of the two-stage temperature reduction is 1% to 8%, such as 1%, 2%, 3%, 4%, 5%, 6%, 7%, or 8%, but not limited to the recited values, and other values not recited within the range of values are equally applicable.
Preferably, in step (5), the cooling rate of the second stage of the two-stage cooling is 1.0-3.0 ℃/min, such as 1 ℃/min, 1.5 ℃/min, 2 ℃/min, 2.5 ℃/min, or 3 ℃/min, but not limited to the recited values, and other values not recited in the range of the values are also applicable.
Preferably, in the step (5), the temperature is reduced to 20-30 ℃ in the second stage of the two-stage temperature reduction, namely, the temperature is reduced to room temperature.
Preferably, in step (5), the oxygen content in the second stage of the two-stage temperature reduction is below 500ppm, such as 500ppm, 450ppm, 400ppm or 300 ppm.
As a preferable technical scheme of the invention, the preparation method further comprises the following step (6): and (5) pasting the MnZn ferrite magnetic sheet obtained in the step (5), and then splitting and punching to obtain the MnZn ferrite magnetic sheet product.
Preferably, the MnZn ferrite magnetic sheet is coated on both surfaces.
Preferably, the film used in the sticker is a polyethylene terephthalate (PET) film.
As a further preferable technical scheme of the preparation method, the method comprises the following steps:
(1) placing the metal oxide raw material with the formula amount into a sand mill, adding water, sanding for 20-60 min, stirring and mixing in a stirring pool for 5-15min, and performing spray granulation to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) at 750-950 ℃, wherein the pre-burning time is 1-3 h, and pre-burning powder is obtained;
(3) placing the pre-sintered powder in the step (2) into a sand mill, adding water, performing sand milling for 20-60 min, and then drying or spray drying to obtain dried powder with the water content of below 0.1%;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer for 8-20 hours to obtain slurry;
(5) carrying out tape casting on the slurry obtained in the step (4) to obtain a green sheet with the thickness of 0.03-0.3 mm, heating the green sheet to 950-1200 ℃ at a heating rate of less than or equal to 0.8 ℃/min, sintering, wherein the sintered oxygen content is 1-21%, the sintering time is 1-5 h, cooling in two stages after sintering, cooling in the first stage to 900 ℃ at a cooling rate of 1.0-3.0 ℃/min, cooling in the first stage to 20-30 ℃ at a cooling rate of 1.0-3.0 ℃/min, and cooling in the second stage to below 500ppm to obtain the MnZn ferrite magnetic sheet;
(6) attaching polyethylene glycol terephthalate films to both sides of the MnZn ferrite magnetic sheet in the step (5), and then performing splitting and punching to obtain a MnZn ferrite magnetic sheet product;
wherein the metal oxide raw material is Fe2O3、Mn3O4And ZnO.
In a third aspect, the present invention provides a use of the MnZn ferrite magnetic sheet according to the first aspect, for a wireless charging field. The MnZn ferrite magnetic sheet provided by the invention can be better applied to the field of wireless charging, so that the wireless charging efficiency is higher.
Compared with the prior art, the invention has the following beneficial effects:
(1) the MnZn ferrite magnetic sheet provided by the invention has the advantages of thin thickness, high magnetic conductivity, high saturation magnetic induction Bs and high Curie temperature Tc, the real part of the magnetic conductivity can reach 1490, and the saturation magnetic induction Bs can reach 450 mT.
(2) The preparation method provided by the invention has the advantages of short flow, simple operation and low cost, is suitable for industrial large-scale production, and provides important guarantee for the excellent performance of the MnZn ferrite magnetic sheet.
Detailed Description
In order to better illustrate the present invention and facilitate the understanding of the technical solutions of the present invention, the present invention is further described in detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Example 1
This example prepares MnZn ferrite magnetic sheets as follows:
(1) according to Fe2O3The molar percentage of (3) was 49.5 mol%, the molar percentage of ZnO was 21.2 mol%, and the balance was the molar ratio of MnO, which was converted to Fe2O3、Mn3O4And ZnO, and weighing the weighed Fe2O3、Mn3O4And ZnO are placed in a sand mill, water is added, sand milling is carried out for 40min, then stirring and mixing are carried out for 10min in a stirring tank, and then spray granulation is carried out to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) at 850 ℃ for 2 hours to obtain pre-burned powder;
(3) putting the pre-sintered powder in the step (2) into a sand mill, adding water, sanding for 40min, and then drying or spray drying to obtain dried powder with the water content of less than 0.1%;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer for 14 hours to prepare slurry;
(5) casting the slurry obtained in the step (4) to obtain the slurry with the thickness of0.1mm, area of 100cm2Heating the green sheet to 1080 ℃ at a heating rate of 0.6 ℃/min, sintering, wherein the sintered oxygen content is 11 percent, the sintering time is 3 hours, cooling in two stages after sintering, the first stage is cooled to 900 ℃ at a cooling rate of 2.0 ℃/min, the oxygen content in the first stage is 4.5 percent, the second stage is cooled to 25 ℃ at a cooling rate of 2.0 ℃/min, and the oxygen content in the second stage is below 500ppm, so as to obtain the MnZn ferrite magnetic sheet, wherein the MnZn ferrite magnetic sheet is flat;
(6) polyethylene terephthalate films were attached to both sides of the MnZn ferrite magnetic sheet in the step (5), and then, the split and die-cut rings having an outer diameter of 20mm and an inner diameter of 10mm were tested for the real part of permeability μ' with an AGILENT E4990A, the Curie temperature Tc with CH3302 and an oven, and the saturated magnetic flux density Bs with a SY8218 apparatus from Kawasaki corporation were tested.
Through tests, the real part mu' of the magnetic permeability of the MnZn ferrite magnetic sheet ring obtained in the embodiment under the conditions of 128KHz, 0.25mT and 25 ℃ is 1050, the saturation magnetic flux density Bs under the conditions of 50Hz, 1194A/m and 25 ℃ is 420mT, the Curie temperature Tc is 112 ℃, and the resistivity rho is 1.6 multiplied by 103Ω·m。
Example 2
This example prepares MnZn ferrite magnetic sheets as follows:
(1) according to Fe2O3The molar percentage of (3) was 49.8 mol%, the molar percentage of ZnO was 23.0 mol%, and the balance was the molar ratio of MnO, and this was converted to Fe2O3、Mn3O4And ZnO, and weighing the weighed Fe2O3、Mn3O4And ZnO are placed in a sand mill, water is added, sand milling is carried out for 40min, then stirring and mixing are carried out for 10min in a stirring tank, and then spray granulation is carried out to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) at 850 ℃ for 2 hours to obtain pre-burned powder;
(3) putting the pre-sintered powder in the step (2) into a sand mill, adding water, sanding for 40min, and then drying or spray drying to obtain dried powder with the water content of less than 0.1%;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer for 14 hours to prepare slurry;
(5) carrying out tape casting on the slurry obtained in the step (4) to obtain the slurry with the thickness of 0.1mm and the area of 100cm2Heating the green sheet to 1200 ℃ at a heating rate of 0.6 ℃/min, sintering, wherein the sintered oxygen content is 11 percent, the sintering time is 3 hours, cooling in two stages after sintering, wherein the temperature is reduced to 900 ℃ at a cooling rate of 2.0 ℃/min in the first stage, the oxygen content is 4.5 percent in the first stage, the temperature is reduced to 25 ℃ at a cooling rate of 2.0 ℃/min in the second stage, and the oxygen content is below 500ppm in the second stage, so that the MnZn ferrite magnetic sheet is obtained, and the MnZn ferrite magnetic sheet is flat;
(6) polyethylene terephthalate films were attached to both sides of the MnZn ferrite magnetic sheet in the step (5), and then, the split and die-cut rings having an outer diameter of 20mm and an inner diameter of 10mm were tested for the real part of permeability μ' with an AGILENT E4990A, the Curie temperature Tc with CH3302 and an oven, and the saturated magnetic flux density Bs with a SY8218 apparatus from Kawasaki corporation were tested.
Through tests, the real part mu' of the magnetic permeability of the MnZn ferrite magnetic sheet ring obtained in the embodiment at 128KHz, 0.25mT and 25 ℃ is 1350, the saturation magnetic flux density Bs at 50Hz, 1194A/m and 25 ℃ is 390mT, the Curie temperature Tc is 105 ℃, and the resistivity rho is 630 omega m.
Example 3
This example prepares MnZn ferrite magnetic sheets as follows:
(1) according to Fe2O3The molar percentage of (3) was 48.8 mol%, the molar percentage of ZnO was 22.5 mol%, and the balance was the molar ratio of MnO, and this was converted to Fe2O3、Mn3O4And ZnO, and weighing the weighed Fe2O3、Mn3O4And ZnO are placed in a sand mill, water is added, sand milling is carried out for 40min, then stirring and mixing are carried out for 10min in a stirring tank, and then spray granulation is carried out to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) at 850 ℃ for 2 hours to obtain pre-burned powder;
(3) putting the pre-sintered powder in the step (2) into a sand mill, adding water, sanding for 40min, and then drying or spray drying to obtain dried powder with the water content of less than 0.1%;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer for 14 hours to prepare slurry;
(5) carrying out tape casting on the slurry obtained in the step (4) to obtain the slurry with the thickness of 0.1mm and the area of 100cm2Heating the green sheet to 950 ℃ at a heating rate of 0.6 ℃/min, sintering, wherein the sintered oxygen content is 11 percent, the sintering time is 3 hours, cooling in two stages after sintering, wherein the temperature is reduced to 900 ℃ at a cooling rate of 2.0 ℃/min in the first stage, the oxygen content is 4.5 percent in the first stage, the temperature is reduced to 25 ℃ at a cooling rate of 2.0 ℃/min in the second stage, and the oxygen content is below 500ppm in the second stage, so that the MnZn ferrite magnetic sheet is obtained, and the MnZn ferrite magnetic sheet is flat;
(6) polyethylene terephthalate films were attached to both sides of the MnZn ferrite magnetic sheet in the step (5), and then, the split and die-cut rings having an outer diameter of 20mm and an inner diameter of 10mm were tested for the real part of permeability μ' with an AGILENT E4990A, the Curie temperature Tc with CH3302 and an oven, and the saturated magnetic flux density Bs with a SY8218 apparatus from Kawasaki corporation were tested.
Through tests, the real part mu' of the magnetic permeability of the MnZn ferrite magnetic sheet ring obtained in the embodiment under the conditions of 128KHz, 0.25mT and 25 ℃ is 623, the saturation magnetic flux density Bs under the conditions of 50Hz, 1194A/m and 25 ℃ is 285mT, the Curie temperature Tc is 96 ℃, and the resistivity rho is 2.2 multiplied by 103Ω·m。
Example 4
This example prepares MnZn ferrite magnetic sheets as follows:
(1) according to Fe2O3The molar percentage of (3) is 48.5 mol%, the molar percentage of ZnO is 15 mol%, and the balance is the molar ratio of MnO, and the molar ratio is converted into Fe2O3、Mn3O4And ZnO, and weighing the weighed Fe2O3、Mn3O4And ZnO are placed in a sand mill, water is added, sand milling is carried out for 20min, then stirring and mixing are carried out for 5min in a stirring tank, and then spray granulation is carried out to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) at 750 ℃ for 1h to obtain pre-burned powder;
(3) putting the pre-sintered powder in the step (2) into a sand mill, adding water, sanding for 20min, and then drying or spray drying to obtain dried powder with the water content of less than 0.1%;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer for 8 hours to prepare slurry;
(5) carrying out tape casting on the slurry obtained in the step (4) to obtain the slurry with the thickness of 0.03mm and the area of 0.25cm2Heating the green sheet to 1200 ℃ at a heating rate of 0.6 ℃/min, sintering, wherein the sintered oxygen content is 1%, the sintering time is 1h, cooling in two stages after sintering, wherein the temperature is reduced to 900 ℃ at a cooling rate of 1.0 ℃/min in the first stage, the oxygen content is 1% in the first stage, the temperature is reduced to 20 ℃ at a cooling rate of 1.0 ℃/min in the second stage, and the oxygen content is less than 500ppm in the second stage, so as to obtain the MnZn ferrite magnetic sheet, wherein the MnZn ferrite magnetic sheet is flat;
(6) polyethylene terephthalate films were attached to both sides of the MnZn ferrite magnetic sheet in the step (5), and then, the split and die-cut rings having an outer diameter of 20mm and an inner diameter of 10mm were tested for the real part of permeability μ' with an AGILENT E4990A, the Curie temperature Tc with CH3302 and an oven, and the saturated magnetic flux density Bs with a SY8218 apparatus from Kawasaki corporation were tested.
Through tests, the real part mu' of the magnetic permeability of the MnZn ferrite magnetic sheet ring obtained in the embodiment under the conditions of 128KHz, 0.25mT and 25 ℃ is 608, the saturation magnetic flux density Bs under the conditions of 50Hz, 1194A/m and 25 ℃ is 285mT, the Curie temperature Tc is 125 ℃, and the resistivity rho is 3 multiplied by 103Ω·m。
Example 5
This example prepares MnZn ferrite magnetic sheets as follows:
(1) according to Fe2O3Is 50 mol%, the mol% of ZnO is 24 mol%, and the balance is the mol ratio of MnO, and the mol ratio is converted into Fe2O3、Mn3O4And ZnO, and weighing the weighed Fe2O3、Mn3O4And ZnO are placed in a sand mill, water is added, sand milling is carried out for 60min, then stirring and mixing are carried out for 15min in a stirring tank, and then spray granulation is carried out to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) at 950 ℃, wherein the pre-burning time is 3 hours, and pre-burning powder is obtained;
(3) putting the pre-sintered powder in the step (2) into a sand mill, adding water, sanding for 60min, and then drying or spray drying to obtain dried powder with the water content of less than 0.1%;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer for 20 hours to prepare slurry;
(5) carrying out tape casting on the slurry obtained in the step (4) to obtain the slurry with the thickness of 0.3mm and the area of 160cm2Heating the green sheet to 1200 ℃ at a heating rate of 0.6 ℃/min, sintering, wherein the sintered oxygen content is 21 percent, the sintering time is 5 hours, cooling in two stages after sintering, wherein the temperature is reduced to 900 ℃ at a cooling rate of 3.0 ℃/min in the first stage, the oxygen content is 8 percent in the first stage, the temperature is reduced to 30 ℃ at a cooling rate of 3.0 ℃/min in the second stage, and the oxygen content is below 500ppm in the second stage, so as to obtain the MnZn ferrite magnetic sheet, wherein the MnZn ferrite magnetic sheet is flat;
(6) polyethylene terephthalate films were attached to both sides of the MnZn ferrite magnetic sheet in the step (5), and then, the split and die-cut rings having an outer diameter of 20mm and an inner diameter of 10mm were tested for the real part of permeability μ' with an AGILENT E4990A, the Curie temperature Tc with CH3302 and an oven, and the saturated magnetic flux density Bs with a SY8218 apparatus from Kawasaki corporation were tested.
Through tests, the real part mu' of the magnetic permeability of the MnZn ferrite magnetic sheet ring obtained in the embodiment at 128KHz, 0.25mT and 25 ℃ is 1490, the saturation magnetic flux density Bs at 50Hz, 1194A/m and 25 ℃ is 450mT, the Curie temperature Tc is 118 ℃, and the resistivity rho is 22 omega. m.
Comparative example 1
The present comparative example was conducted in accordance with example 1 except that, in step (5), the sintering temperature was 900 ℃.
Although the ferrite sheet obtained in the comparative example was flat after sintering, the real part of permeability μ' of the MnZn ferrite sheet ring obtained in the comparative example was only 430 at 128KHz, 0.25mT and 25 ℃, the saturation magnetic flux density Bs at 50Hz, 1194A/m and 25 ℃ was only 260mT, the Curie temperature Tc was 112 ℃, and the resistivity ρ was 4.7 × 103Ω·m。
Comparative example 2
The present comparative example was conducted in accordance with example 1 except that, in step (5), the sintering temperature was 1250 ℃.
The ferrite sheet obtained in this comparative example was warped around, swollen in the middle, and uneven after sintering, and could not be used.
Comparative example 3
A specific embodiment of this comparative example is that of reference example 1, except that in step (1), in terms of Fe2O3The molar percentage of (3) is 60 mol%, the molar percentage of ZnO is 10 mol%, and the balance is the molar ratio of MnO, and the molar ratio is converted into Fe2O3、Mn3O4And the mass of ZnO.
Through tests, the real part mu' of the magnetic permeability of the MnZn ferrite magnetic sheet ring obtained by the comparative example is only 360 at 128KHz, 0.25mT and 25 ℃, the saturation magnetic flux density Bs at 50Hz, 1194A/m and 25 ℃ is 420mT, the Curie temperature Tc is 210 ℃, and the resistivity rho is 0.5 omega.m.
It can be seen from the above examples and comparative examples that the MnZn ferrite magnetic sheet provided by the present invention has a thin thickness, a high magnetic permeability, a high saturation magnetic induction Bs, a high electrical resistivity and a high Curie temperature Tc because of the appropriate component ratio and the appropriate preparation method. The comparative example did not adopt the scheme of the present invention, and thus the excellent effects of the present invention could not be obtained.
The applicant states that the present invention is illustrated in detail by the above examples, but the present invention is not limited to the above detailed methods, i.e. it is not meant that the present invention must rely on the above detailed methods for its implementation. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (36)

1. A MnZn ferrite magnetic sheet, characterized in that the MnZn ferrite magnetic sheet comprises an iron element, a manganese element and a zinc element, wherein the iron element is Fe2O3In the form of ZnO, zinc in the form of ZnO, manganese in the form of MnO, and Fe in said MnZn ferrite magnetic sheet2O3The MnZn ferrite magnetic sheet comprises 48.5-50 mol% of ZnO, 15-24 mol% of ZnO and the balance of MnO, wherein the thickness of the MnZn ferrite magnetic sheet is 0.03-0.3 mm;
the MnZn ferrite magnetic sheet is prepared by the following method:
(1) mixing and crushing the metal oxide raw materials according to the formula amount, and then granulating to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) to obtain pre-burned powder;
(3) crushing the pre-sintering powder in the step (2), and then drying to obtain dried powder;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer to obtain slurry;
(5) carrying out tape casting on the slurry obtained in the step (4) to obtain a green sheet, heating the green sheet to 1000-1200 ℃, sintering, and cooling in two stages after sintering to obtain the MnZn ferrite magnetic sheet;
the temperature reduction rate of the first stage of the two-stage temperature reduction is 1.0-3.0 ℃/min, the oxygen content is 4-8%, the temperature is reduced to 900 ℃ in the first stage, the temperature reduction rate of the second stage is 1.0-3.0 ℃/min, and the oxygen content is below 500 ppm.
2. The MnZn ferrite magnetic sheet according to claim 1, wherein the area of the MnZn ferrite magnetic sheet is 0.25 to 160cm2。
3. The MnZn ferrite magnetic sheet according to claim 1, wherein polyethylene terephthalate films are attached to both faces of the MnZn ferrite magnetic sheet.
4. A method for producing a MnZn ferrite magnetic sheet according to claim 1 or 2, comprising the steps of:
(1) mixing and crushing the metal oxide raw materials according to the formula amount, and then granulating to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) to obtain pre-burned powder;
(3) crushing the pre-sintering powder in the step (2), and then drying to obtain dried powder;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer to obtain slurry;
(5) carrying out tape casting on the slurry obtained in the step (4) to obtain a green sheet, heating the green sheet to 1000-1200 ℃, sintering, and cooling in two stages after sintering to obtain the MnZn ferrite magnetic sheet;
the temperature reduction rate of the first stage of the two-stage temperature reduction is 1.0-3.0 ℃/min, the oxygen content is 4-8%, the temperature is reduced to 900 ℃ in the first stage, the temperature reduction rate of the second stage is 1.0-3.0 ℃/min, and the oxygen content is below 500 ppm.
5. The production method according to claim 4, wherein in the step (1), the metal oxide raw material comprises Fe2O3、Mn3O4And ZnO.
6. The method of claim 4, wherein the mixing and crushing method is sand milling.
7. A method of manufacturing as claimed in claim 6, wherein the sanding is performed in a sand mill.
8. The method of claim 6, wherein water is added during the sanding.
9. The preparation method according to claim 4, wherein the mixing and crushing time in step (1) is 20-60 min.
10. The method of claim 4, wherein step (1) further comprises: and mixing and crushing, circularly mixing for 5-15min, and then granulating.
11. The method of claim 10, wherein the circulating mixing is performed by stirring in a stirring tank.
12. The method according to claim 4, wherein the granulation in step (1) is spray granulation.
13. The method of claim 4, wherein the pre-firing in step (2) is carried out at a temperature of 750 to 950 ℃.
14. The method of claim 4, wherein the pre-firing time in step (2) is 1 to 3 hours.
15. The method of claim 4, wherein the step (3) is carried out by sand grinding.
16. The method of claim 15, wherein the sanding is performed in a sand mill.
17. The method of claim 15, wherein water is added during the sanding.
18. The preparation method according to claim 4, wherein the time for the crushing in the step (3) is 20-60 min.
19. The method according to claim 4, wherein the drying in step (3) is oven drying or spray drying.
20. The method according to claim 4, wherein the moisture content of the dried powder in the step (3) is 0.1% or less.
21. The method according to claim 4, wherein the organic solvent of step (4) comprises ethanol.
22. The method of claim 4, wherein the binder of step (4) comprises polyvinyl alcohol.
23. The method of claim 4, wherein the plasticizer of step (4) comprises dioctyl phthalate.
24. The preparation method according to claim 4, wherein the grinding time in the step (4) is 8-20 h.
25. The production method according to claim 4, wherein the green sheet in the step (5) has a thickness of 0.03 to 0.3 mm.
26. The production method according to claim 4, wherein the sintering of step (5) is performed in a sintering furnace.
27. The production method according to claim 4, wherein in the step (5), the green sheet is mounted on a flat alumina plate or zirconia plate and then placed in a sintering furnace.
28. The method according to claim 4, wherein in the step (5), the temperature rise rate of the temperature rise is not more than 0.8 ℃/min.
29. The preparation method according to claim 4, wherein in the step (5), the sintering time is 1-5 h.
30. The method according to claim 4, wherein in the step (5), the sintered oxygen content is 1% to 21%.
31. The method according to claim 4, wherein in the step (5), the temperature is reduced to 20-30 ℃ in the second stage of the two-stage temperature reduction.
32. The production method according to claim 4, characterized by further comprising step (6): and (5) pasting the MnZn ferrite magnetic sheet obtained in the step (5), and then splitting and punching to obtain the MnZn ferrite magnetic sheet product.
33. The production method as claimed in claim 32, wherein the MnZn ferrite magnetic sheet is filmed on both sides.
34. The production method according to claim 32, wherein the film used in the patch is a polyethylene terephthalate film.
35. The method for preparing according to claim 4, characterized in that it comprises the following steps:
(1) placing the metal oxide raw material with the formula amount into a sand mill, adding water, sanding for 20-60 min, stirring and mixing in a stirring pool for 5-15min, and performing spray granulation to obtain a mixed material;
(2) pre-burning the mixed material obtained in the step (1) at 750-950 ℃, wherein the pre-burning time is 1-3 h, and pre-burning powder is obtained;
(3) placing the pre-sintered powder in the step (2) into a sand mill, adding water, performing sand milling for 20-60 min, and then drying or spray drying to obtain dried powder with the water content of below 0.1%;
(4) mixing and grinding the dried powder material obtained in the step (3), an organic solvent, an adhesive and a plasticizer for 8-20 hours to obtain slurry;
(5) carrying out tape casting on the slurry obtained in the step (4) to obtain a green sheet with the thickness of 0.03-0.3 mm, heating the green sheet to 950-1200 ℃ at a heating rate of less than or equal to 0.8 ℃/min, sintering, wherein the sintered oxygen content is 1-21%, the sintering time is 1-5 h, cooling in two stages after sintering, cooling in the first stage to 900 ℃ at a cooling rate of 1.0-3.0 ℃/min, cooling in the first stage to 20-30 ℃ at a cooling rate of 1.0-3.0 ℃/min, and cooling in the second stage to below 500ppm to obtain the MnZn ferrite magnetic sheet;
(6) attaching polyethylene glycol terephthalate films to both sides of the MnZn ferrite magnetic sheet in the step (5), and then performing splitting and punching to obtain a MnZn ferrite magnetic sheet product;
wherein the metal oxide raw material is Fe2O3、Mn3O4And ZnO.
36. Use of a MnZn ferrite magnetic sheet according to any one of claims 1 to 3, for wireless charging applications.
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