CN108711481A - A kind of MnZn ferrites magnetic sheet and its preparation method and application - Google Patents
A kind of MnZn ferrites magnetic sheet and its preparation method and application Download PDFInfo
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- CN108711481A CN108711481A CN201810756353.2A CN201810756353A CN108711481A CN 108711481 A CN108711481 A CN 108711481A CN 201810756353 A CN201810756353 A CN 201810756353A CN 108711481 A CN108711481 A CN 108711481A
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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
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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
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- 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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- C04B2235/656—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
- 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
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Abstract
The present invention provides a kind of MnZn ferrites magnetic sheets and its preparation method and application.The MnZn ferrites magnetic sheet includes ferro element, manganese element and Zn-ef ficiency, and wherein ferro element presses Fe2O3Form meter, Zn-ef ficiency is based on ZnO forms, and manganese element is based on MnO forms, Fe in the MnZn ferrites magnetic sheet2O3Mole percent be 48.5~50mol%, the mole percent of ZnO is 15~24mol%, and the thickness of surplus MnO, the MnZn ferrites magnetic sheet are 0.03~0.3mm.The preparation method includes：(1) dispensing, (2) pre-burning, (3) are once ground, (4) secondary grinding and slurrying, (5) curtain coating and sintering.MnZn ferrites magnetic sheet thickness provided by the invention is thin, and magnetic conductivity is high, and saturation induction density is high and Curie temperature is high.
Description
Technical field
The invention belongs to technical field of electronic materials more particularly to a kind of MnZn ferrites magnetic sheet and preparation method thereof and use
On the way.
Background technology
Wireless charging technology (wireless charging technology) is a kind of power transmission skill without wiring
Art, also referred to as non-contact inductive charge transfer the energy to power device, transmitting terminal (charger) and reception by power supply unit
Do not have to conducting wire between end (power device) to connect.Since the charging unit is convenient for carrying and is used, first in intelligent movable equipment
In shown wide application prospect.Wireless charging technology is by modes such as electromagnetic induction, magnetic resonance, radio waves come real
It is existing.
The fast electromagnetic induction technology of market speedup and the mr techniques that have a extensive future are for magnetic material at present
Demand is huge, and the magnetic material being related to includes soft magnetic materials and permanent magnet.Soft magnetic ferrite is due to higher initial
Magnetic conductivity and higher resistivity, and it is easy to lightening processing using casting technique making, so being risen in wireless charging system
Increase the effect of induced field intensity and shielded coil magnetic field.The soft magnetic ferrite used at present for NiZn ferrites, but
It is since NiZn Ferrite Material magnetic conductivity highests only have 500~700, Curie temperature there was only 90 degree, saturation induction density Bs
In 300mT hereinafter, so the wireless charging magnetic sheet made using NiZn materials is caused to will appear charge efficiency in use
The low, disadvantages such as temperature in use is low.
CN103117146A discloses a kind of high-curie temperature low loss and high strength ferrite magnetic patch and preparation method thereof.It should
The ferrite magnetic patch primary raw material that scheme provides includes iron oxide, manganese oxide and zinc oxide, and auxiliary material includes calcium carbonate, oxidation
The group of titanium, cobalt oxide, silica, chromium oxide, niobium oxide, nickel oxide and copper oxide, primary raw material is divided into：55-61mol%'s presses
Fe2O3The zinc oxide of the iron oxide of calculating, the manganese oxide of 33-40mol% calculated by MnO and 5-10mol% calculated by ZnO；
Relative to the total weight of the primary raw material, the additive amount of the auxiliary material is：CaCO3:500-3000ppm, TiO2:80-
3000ppm, Co2O3:50-1200ppm, ultra-fine SiO2：20-200ppm, Cr2O3:100-1500ppm, Nb2O5:100-
1500ppm, NiO：600-2000ppm and CuO：600-2000ppm.
CN102795851A discloses a kind of ferrite composition and electronic component, the ferrite composition, including by
With Fe2O3Iron oxide that the content of conversion is 63.3~65.5 moles of % with the ZnO contents to convert is 11.6~15.8 moles of %
Zinc oxide, surplus manganese oxide constitute principal component, which is characterized in that relative to 100 weight % of the principal component, with SiO2
The silica content of conversion is 60~250ppm, is 360~1000ppm with the CaO calcium oxide contents to convert, is converted with element
The Cd contents that Pb contents are 7ppm or less, are converted with element is 7ppm or less.
CN102964117A discloses a kind of wide warm MnZn power ferrite material, the Ferrite Material by principal component and
Auxiliary element forms, wherein the molar percentage of each component of the principal component is：Fe2O3It is for 52.7~52.8mol%, ZnO
9.2~9.8mol%, MnO surplus；The auxiliary element accounts for the 0.505%~0.685% of principal component total weight, the auxiliary at
Divide by CaCO3、ZrO2、Nb2O5、SnO2And Co2O3Composition.The present invention has low loss within the temperature range of 25 DEG C and 140 DEG C
Characteristic, while taking into account the characteristic of high Bs.
However said program is required for that additive component is added in MnZn Ferrite Materials, improves manufacturing cost, and
And MnZn ferrite magnetic sheets can not be made very thin to meet the needs of wireless charging.
Therefore develop it is a kind of thinner, more inexpensively, and with magnetic conductivity height, saturation induction density Bs high,
The MnZn ferrites magnetic sheet for the advantages that Curie temperature is high has this field important meaning.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide a kind of MnZn ferrites magnetic sheet and its preparation
Method and purposes, MnZn ferrites magnetic sheet very thin thickness provided by the invention, and the high, saturation induction density with magnetic conductivity
The advantages that Bs high, high Curie temperature.
For this purpose, the present invention uses following technical scheme：
In a first aspect, the present invention provides a kind of MnZn ferrites magnetic sheet, the MnZn ferrites magnetic sheet includes ferro element, manganese
Element and Zn-ef ficiency, wherein ferro element press Fe2O3Form meter, for Zn-ef ficiency based on ZnO forms, manganese element is described based on MnO forms
Fe in MnZn ferrite magnetic sheets2O3Mole percent be 48.5~50mol%, the mole percent of ZnO is 15~24mol%,
Surplus is MnO, and the thickness of the MnZn ferrites magnetic sheet is 0.03~0.3mm.
Fe in MnZn ferrites magnetic sheet of the present invention2O3Mole percent be 48.5~50mol%, such as
48.5mol%, 48.8mol%, 49mol%, 49.2mol%, 49.5mol%, 49.7mol% or 50mol% etc., but simultaneously not only
It is limited to cited numerical value, other unrequited numerical value are equally applicable in the numberical range.The mole percent of ZnO be 15~
24mol%, for example, 15mol%, 16mol%, 17mol%, 18mol%, 19mol%, 20mol%, 21mol%, 22mol%,
23mol% or 24mol% etc., it is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are same
It is applicable in.
In the present invention, the thickness of the MnZn ferrites magnetic sheet is 0.03~0.3mm, such as 0.03mm, 0.06mm,
0.1mm, 0.15mm, 0.2mm, 0.25mm or 0.3mm etc., it is not limited to cited numerical value, in the numberical range other
Unrequited numerical value is equally applicable.
The thickness of MnZn ferrites magnetic sheet provided by the invention is very thin, this is very beneficial for wireless charging application, and
Magnetic conductivity height, saturation induction density Bs high, Curie temperature Tc high, electricalresistivityρ are high.And MnZn ferrite magnetics provided by the invention
The component proportion of piece properly also plays important role, such as Fe for obtaining such effect2O3Mole percent relatively
It is low, contribute to the raising of resistivity.Auxiliary element is not included in MnZn ferrites magnetic sheet provided by the invention.
It is used as currently preferred technical solution below, but not as the limitation to technical solution provided by the invention, leads to
Following preferred technical solution is crossed, can preferably reach and realize the technical purpose and advantageous effect of the present invention.
As currently preferred technical solution, the area of the MnZn ferrites magnetic sheet is 0.25~160cm2, such as
0.25cm2、0.5cm2、1cm2、10cm2、20cm2、40cm2、60cm2、80cm2、100cm2、120cm2、140cm2Or 160cm2Deng,
It is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.Such big MnZn
The area of ferrite magnetic sheet is conducive to the practical application of magnetic sheet, and because MnZn ferrite magnetics piece performance provided by the invention is excellent
Different, flatness is high, therefore can just obtain area big in this way.
Preferably, polyethylene terephthalate film is posted on the MnZn ferrites magnetic sheet two sides.
Thickness provided by the invention is 0.03~0.3mm magnetic sheets has following performance after pad pasting, sliver：At 25 DEG C,
Under the conditions of 128KHz and 0.25mT, magnetic conductivity real part μ ' is about 600~1500；At 25 DEG C, under the conditions of 50Hz and 1194A/m, satisfy
It is about 280~450mT with magnetic induction density B s；Curie temperature Tc is about 90~120 DEG C, and electricalresistivityρ is about 20~3 × 103
Ω·m。
Second aspect, the present invention provide a kind of preparation method of the ferrite magnetic sheets of MnZn as described in relation to the first aspect, the system
Preparation Method includes the following steps：
(1) metal oxide starting material of formula ratio is mixed and is crushed, be then granulated, obtain mixed material；
(2) pre-burning is carried out to step (1) mixed material, obtains preburning powdered material；
(3) step (2) described preburning powdered material is crushed, then dries, obtains dry powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and is ground, starched
Material；
(5) step (4) described slurry is cast, obtains raw cook, the raw cook is warming up to 950~1200 DEG C, into
Row sintering, two benches cool down after sintering, obtain the MnZn ferrites magnetic sheet.
In step (5) of the present invention, raw cook is warming up to 950~1200 DEG C of sintering temperature, for example, 950 DEG C, 1000 DEG C,
1050 DEG C, 1100 DEG C, 1150 DEG C or 1200 DEG C etc., it is not limited to cited numerical value, interior other of the numberical range do not arrange
The numerical value of act is equally applicable.In the present invention, if the temperature of sintering is too low, the magnetic conductivity real part of MnZn ferrite magnetic sheets can be caused
Decline with saturation induction density Bs, seriously affects properties of product；If the temperature of sintering is excessively high, MnZn ferrite magnetics can be caused
Piece surrounding warpage, intermediate muster, out-of-flatness can not use.
In preparation method provided by the invention, the sintering process in step (5) is smooth for solving MnZn ferrite magnetic sheets
Degree problem plays an important roll.
As currently preferred technical solution, in step (1), the metal oxide starting material includes Fe2O3、Mn3O4With
ZnO。
Preferably, the mixing and broken method are to be sanded.
Preferably, the sand milling carries out in sand mill.
Preferably, water is added during the sand milling.
Preferably, step (1) mixing and broken time are 20~60min, for example, 20min, 30min, 40min,
50min or 60min etc., it is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.
Preferably, step (1) further includes：After mixing and being crushed, it is granulated again after 5~15min of cycle mixing.It is described to follow
Ring mixing time be 5-15min, such as 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min,
14min or 15min etc., it is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.
Preferably, the mixed method of the cycle is to be stirred in stirring pool.
Preferably, the method for step (1) described granulation is mist projection granulating.
As currently preferred technical solution, the temperature of step (2) described pre-burning is 750~950 DEG C, such as 750 DEG C,
775 DEG C, 800 DEG C, 825 DEG C, 850 DEG C, 875 DEG C, 900 DEG C, 925 DEG C or 950 DEG C etc., it is not limited to cited numerical value,
Other unrequited numerical value are equally applicable in the numberical range.
Preferably, the time of step (2) described pre-burning is 1~3h, such as 1h, 1.5h, 2h, 2.5h or 3 etc., but simultaneously not only
It is limited to cited numerical value, other unrequited numerical value are equally applicable in the numberical range.
Preferably, step (3) the broken method is that is sanded
Preferably, the sand milling carries out in sand mill.
Preferably, water is added during the sand milling.
Preferably, step (3) the broken time be 20~60min, such as 20min, 30min, 40min, 50min or
60min etc., it is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.
Preferably, the method for step (3) described drying is drying or spray drying.
Preferably, the water content of the powder of step (3) described drying 0.1% hereinafter, such as 0.09%, 0.08%,
0.07%, 0.06%, 0.05% or 0.04% etc..
As currently preferred technical solution, step (4) described organic solvent includes ethyl alcohol.
Preferably, step (4) described adhesive includes polyvinyl alcohol.
Preferably, step (4) the plasticizer includes dioctyl phthalate.
Preferably, the time of step (4) described grinding is 8~20h, such as 8h, 10h, 12h, 14h, 16h, 18h or 20h
Deng it is not limited to cited numerical value, other unrequited numerical value are equally applicable in the numberical range.
As currently preferred technical solution, the thickness of step (5) described raw cook is 0.03~0.3mm, such as
0.03mm, 0.06mm, 0.1mm, 0.15mm, 0.2mm, 0.25mm or 0.3mm etc., it is not limited to cited numerical value, it should
Other unrequited numerical value are equally applicable in numberical range.
The detailed process of step (5) the of the present invention curtain coating is：Slurry through casting apparatus according to setting thickness equably
Coated on polyethylene terephthalate (PET) basement membrane, ferrite life can be obtained after the epilamellar slurry dryings of PET
Piece.
Preferably, step (5) sintering carries out in sintering furnace.
Preferably, in step (5), the raw cook places into sintering furnace on smooth alumina plate or zirconium oxide plate.
Preferably, in step (5), heating rate≤0.8 DEG C/min of the heating, such as 0.8 DEG C/min, 0.7 DEG C/
Min, 0.6 DEG C/min, 0.5 DEG C/min or 0.4 DEG C/min etc..
Preferably, in step (5), time of the sintering is 1~5h, such as 1h, 2h, 3h, 4h or 5h etc., but simultaneously not only
It is limited to cited numerical value, other unrequited numerical value are equally applicable in the numberical range.
Preferably, in step (5), the oxygen content of the sintering is 1%~21%, such as 1%, 5%, 10%, 15%,
20% or 21% etc., it is not limited to cited numerical value, other interior unrequited numerical value of the numberical range are equally applicable.
Preferably, in step (5), the rate of temperature fall of the first stage of the two benches cooling is 1.0~3.0 DEG C/min,
Such as 1 DEG C/min, 1.5 DEG C/min, 2 DEG C/min, 2.5 DEG C/min or 3 DEG C/min etc., it is not limited to cited numerical value,
Other unrequited numerical value are equally applicable in the numberical range.
Preferably, in step (5), temperature is reduced to 900 DEG C by the first stage of the two benches cooling.
Preferably, in step (5), the oxygen content of the first stage of two benches cooling is 1%~8%, such as 1%,
2%, 3%, 4%, 5%, 6%, 7% or 8% etc., it is not limited to cited numerical value, interior other of the numberical range do not arrange
The numerical value of act is equally applicable.
Preferably, in step (5), the rate of temperature fall of the second stage of the two benches cooling is 1.0~3.0 DEG C/min,
Such as 1 DEG C/min, 1.5 DEG C/min, 2 DEG C/min, 2.5 DEG C/min or 3 DEG C/min etc., it is not limited to cited numerical value,
Other unrequited numerical value are equally applicable in the numberical range.
Preferably, in step (5), temperature is reduced to 20~30 DEG C by the second stage of the two benches cooling, that is, is cooled down
To room temperature.
Preferably, in step (5), the oxygen content of the second stage of two benches cooling is in 500ppm hereinafter, for example
500ppm, 450ppm, 400ppm or 300ppm etc..
As currently preferred technical solution, the preparation method further includes step (6)：To step (5) MnZn
Ferrite magnetic sheet carries out pad pasting, then carries out sliver and punching, obtains MnZn ferrite magnetic flake products.
Preferably, pad pasting is all carried out on the two sides of MnZn ferrite magnetic sheets.
Preferably, the film used in the pad pasting is polyethylene terephthalate (PET) film.
As the further preferred technical solution of preparation method of the present invention, the described method comprises the following steps：
(1) metal oxide starting material of formula ratio is placed in sand mill, water is added, is sanded, the sand milling time 20~
Then 60min is stirred 5~15min in stirring pool, then carries out mist projection granulating again, obtain mixed material；
(2) pre-burning is carried out at 750~950 DEG C to step (1) described mixed material, the time of pre-burning is 1~3h, is obtained
Preburning powdered material；
(3) step (2) described preburning powdered material is placed in sand mill, be added water, be sanded, be sanded the time be 20~
Then 60min is dried or is spray-dried, obtain water content 0.1% drying below powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and are ground, grinding when
Between be 8~20h, obtain slurry；
(5) step (4) described slurry is cast, obtain thickness be 0.03~0.3mm raw cooks, by the raw cook with≤
The heating rate of 0.8 DEG C/min is warming up to 950~1200 DEG C, is sintered, and the oxygen content of sintering is 1%~21%, when sintering
Between be 1~5h, two benches cool down after sintering, and the first stage is cooled to 900 DEG C with the rate of temperature fall of 1.0~3.0 DEG C/min, first
The oxygen content in stage is 1%~8%, and second stage is cooled to 20~30 DEG C with the rate of temperature fall of 1.0~3.0 DEG C/min, second
The oxygen content in stage is in 500ppm hereinafter, obtaining the MnZn ferrites magnetic sheet；
(6) polyethylene terephthalate film is all sticked in the two sides of step (5) the MnZn ferrites magnetic sheet, then
Sliver and punching are carried out, MnZn ferrite magnetic flake products are obtained；
Wherein, the metal oxide starting material is Fe2O3、Mn3O4And ZnO.
The third aspect, the present invention provide a kind of purposes of the ferrite magnetic sheets of MnZn as described in relation to the first aspect, the MnZn iron
Oxysome magnetic sheet is used for wireless charging field.MnZn ferrites magnetic sheet provided by the invention can be preferably applied for wireless charging neck
Domain makes wireless charging efficiency higher.
Compared with prior art, the invention has the advantages that：
(1) MnZn ferrites magnetic sheet thickness provided by the invention is thin, magnetic conductivity height, saturation induction density Bs high and Curie
Temperature Tc high, magnetic conductivity real part is up to 1490, and saturation induction density Bs is up to 450mT.
(2) preparation method flow provided by the invention is short, easy to operate, of low cost, is given birth on a large scale suitable for industrialization
Production, the excellent performance for MnZn ferrite magnetic sheets provide important leverage.
Specific implementation mode
For the present invention is better described, it is easy to understand technical scheme of the present invention, below further specifically to the present invention
It is bright.But following embodiments is only the simple example of the present invention, does not represent or limit the scope of the present invention, this
Invention protection domain is subject to claims.
Embodiment 1
The present embodiment is prepared as follows MnZn ferrite magnetic sheets：
(1) according to Fe2O3Mole percent be 49.5mol%, the mole percent of ZnO is 21.2mol%, and surplus is
The molar ratio of MnO, is scaled Fe2O3、Mn3O4It is weighed with the quality of ZnO, by load weighted Fe2O3、Mn3O4With
ZnO is placed in sand mill, and water is added, is sanded, and time 40min is sanded, is then stirred 10min in stirring pool again,
Mist projection granulating is carried out again, obtains mixed material；
(2) pre-burning is carried out at 850 DEG C to step (1) described mixed material, the time of pre-burning is 2h, obtains pre-burning powder
Material；
(3) step (2) described preburning powdered material being placed in sand mill, water is added, is sanded, the sand milling time is 40min,
Then dried or be spray-dried, obtain water content 0.1% drying below powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and are ground, grinding when
Between be 14h, slurry is made；
(5) step (4) described slurry is cast, it is 0.1mm, area 100cm to obtain thickness2Raw cook, by institute
It states raw cook and is warming up to 1080 DEG C with the heating rate of 0.6 DEG C/min, be sintered, the oxygen content of sintering is 11%, sintering time
For 3h, two benches cool down after sintering, and the first stage is cooled to 900 DEG C with the rate of temperature fall of 2.0 DEG C/min, and the oxygen of first stage contains
Amount is 4.5%, and second stage is cooled to 25 DEG C with the rate of temperature fall of 2.0 DEG C/min, the oxygen content of second stage 500ppm with
Under, the MnZn ferrites magnetic sheet is obtained, the MnZn ferrite magnetic sheets are smooth；
(6) polyethylene terephthalate film is all sticked in the two sides of step (5) the MnZn ferrites magnetic sheet, then
It carries out sliver and is punched into outer diameter 20mm, the ring of internal diameter 10mm tests magnetic conductivity real part μ ', use with AGILENT E4990A
CH3302 and baking oven test Curie temperature Tc, and the survey of saturation flux density Bs is carried out with the SY8218 instruments of Japanese Yan Qi companies
Examination.
By test, magnetic conductance of the MnZn ferrite magnetics loop that the present embodiment obtains at 128KHz, 0.25mT and 25 DEG C
Rate real part μ ' is 1050, and the saturation flux density Bs at 50Hz, 1194A/m and 25 DEG C is 420mT, and Curie temperature Tc is 112
DEG C, electricalresistivityρ is 1.6 × 103Ω·m。
Embodiment 2
The present embodiment is prepared as follows MnZn ferrite magnetic sheets：
(1) according to Fe2O3Mole percent be 49.8mol%, the mole percent of ZnO is 23.0mol%, and surplus is
The molar ratio of MnO, is scaled Fe2O3、Mn3O4It is weighed with the quality of ZnO, by load weighted Fe2O3、Mn3O4With
ZnO is placed in sand mill, and water is added, is sanded, and time 40min is sanded, is then stirred 10min in stirring pool again,
Mist projection granulating is carried out again, obtains mixed material；
(2) pre-burning is carried out at 850 DEG C to step (1) described mixed material, the time of pre-burning is 2h, obtains pre-burning powder
Material；
(3) step (2) described preburning powdered material being placed in sand mill, water is added, is sanded, the sand milling time is 40min,
Then dried or be spray-dried, obtain water content 0.1% drying below powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and are ground, grinding when
Between be 14h, slurry is made；
(5) step (4) described slurry is cast, it is 0.1mm, area 100cm to obtain thickness2Raw cook, by institute
It states raw cook and is warming up to 1200 DEG C with the heating rate of 0.6 DEG C/min, be sintered, the oxygen content of sintering is 11%, sintering time
For 3h, two benches cool down after sintering, and the first stage is cooled to 900 DEG C with the rate of temperature fall of 2.0 DEG C/min, and the oxygen of first stage contains
Amount is 4.5%, and second stage is cooled to 25 DEG C with the rate of temperature fall of 2.0 DEG C/min, the oxygen content of second stage 500ppm with
Under, the MnZn ferrites magnetic sheet is obtained, the MnZn ferrite magnetic sheets are smooth；
(6) polyethylene terephthalate film is all sticked in the two sides of step (5) the MnZn ferrites magnetic sheet, then
It carries out sliver and is punched into outer diameter 20mm, the ring of internal diameter 10mm tests magnetic conductivity real part μ ', use with AGILENT E4990A
CH3302 and baking oven test Curie temperature Tc, and the survey of saturation flux density Bs is carried out with the SY8218 instruments of Japanese Yan Qi companies
Examination.
By test, magnetic conductance of the MnZn ferrite magnetics loop that the present embodiment obtains at 128KHz, 0.25mT and 25 DEG C
Rate real part μ ' is 1350, and the saturation flux density Bs at 50Hz, 1194A/m and 25 DEG C is 390mT, and Curie temperature Tc is 105
DEG C, electricalresistivityρ is 630 Ω m.
Embodiment 3
The present embodiment is prepared as follows MnZn ferrite magnetic sheets：
(1) according to Fe2O3Mole percent be 48.8mol%, the mole percent of ZnO is 22.5mol%, and surplus is
The molar ratio of MnO, is scaled Fe2O3、Mn3O4It is weighed with the quality of ZnO, by load weighted Fe2O3、Mn3O4With
ZnO is placed in sand mill, and water is added, is sanded, and time 40min is sanded, is then stirred 10min in stirring pool again,
Mist projection granulating is carried out again, obtains mixed material；
(2) pre-burning is carried out at 850 DEG C to step (1) described mixed material, the time of pre-burning is 2h, obtains pre-burning powder
Material；
(3) step (2) described preburning powdered material being placed in sand mill, water is added, is sanded, the sand milling time is 40min,
Then dried or be spray-dried, obtain water content 0.1% drying below powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and are ground, grinding when
Between be 14h, slurry is made；
(5) step (4) described slurry is cast, it is 0.1mm, area 100cm to obtain thickness2Raw cook, by institute
It states raw cook and is warming up to 950 DEG C with the heating rate of 0.6 DEG C/min, be sintered, the oxygen content of sintering is 11%, and sintering time is
3h, two benches cool down after sintering, and the first stage is cooled to 900 DEG C with the rate of temperature fall of 2.0 DEG C/min, the oxygen content of first stage
Be 4.5%, second stage is cooled to 25 DEG C with the rate of temperature fall of 2.0 DEG C/min, the oxygen content of second stage in 500ppm hereinafter,
The MnZn ferrites magnetic sheet is obtained, the MnZn ferrite magnetic sheets are smooth；
(6) polyethylene terephthalate film is all sticked in the two sides of step (5) the MnZn ferrites magnetic sheet, then
It carries out sliver and is punched into outer diameter 20mm, the ring of internal diameter 10mm tests magnetic conductivity real part μ ', use with AGILENT E4990A
CH3302 and baking oven test Curie temperature Tc, and the survey of saturation flux density Bs is carried out with the SY8218 instruments of Japanese Yan Qi companies
Examination.
By test, magnetic conductance of the MnZn ferrite magnetics loop that the present embodiment obtains at 128KHz, 0.25mT and 25 DEG C
Rate real part μ ' is 623, and the saturation flux density Bs at 50Hz, 1194A/m and 25 DEG C is 285mT, and Curie temperature Tc is 96 DEG C,
Electricalresistivityρ is 2.2 × 103Ω·m。
Embodiment 4
The present embodiment is prepared as follows MnZn ferrite magnetic sheets：
(1) according to Fe2O3Mole percent be 48.5mol%, the mole percent of ZnO is 15mol%, surplus MnO
Molar ratio, be scaled Fe2O3、Mn3O4It is weighed with the quality of ZnO, by load weighted Fe2O3、Mn3O4It is set with ZnO
In sand mill, water is added, is sanded, time 20min is sanded, is then stirred 5min in stirring pool again, then carry out
Mist projection granulating obtains mixed material；
(2) pre-burning is carried out at 750 DEG C to step (1) described mixed material, the time of pre-burning is 1h, obtains pre-burning powder
Material；
(3) step (2) described preburning powdered material being placed in sand mill, water is added, is sanded, the sand milling time is 20min,
Then dried or be spray-dried, obtain water content 0.1% drying below powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and are ground, grinding when
Between be 8h, slurry is made；
(5) step (4) described slurry is cast, it is 0.03mm, area 0.25cm to obtain thickness2Raw cook, will
The raw cook is warming up to 1200 DEG C with the heating rate of 0.6 DEG C/min, is sintered, and the oxygen content of sintering is 1%, sintering time
For 1h, two benches cool down after sintering, and the first stage is cooled to 900 DEG C with the rate of temperature fall of 1.0 DEG C/min, and the oxygen of first stage contains
Amount is 1%, and second stage is cooled to 20 DEG C with the rate of temperature fall of 1.0 DEG C/min, the oxygen content of second stage in 500ppm hereinafter,
The MnZn ferrites magnetic sheet is obtained, the MnZn ferrite magnetic sheets are smooth；
(6) polyethylene terephthalate film is all sticked in the two sides of step (5) the MnZn ferrites magnetic sheet, then
It carries out sliver and is punched into outer diameter 20mm, the ring of internal diameter 10mm tests magnetic conductivity real part μ ', use with AGILENT E4990A
CH3302 and baking oven test Curie temperature Tc, and the survey of saturation flux density Bs is carried out with the SY8218 instruments of Japanese Yan Qi companies
Examination.
By test, magnetic conductance of the MnZn ferrite magnetics loop that the present embodiment obtains at 128KHz, 0.25mT and 25 DEG C
Rate real part μ ' is 608, and the saturation flux density Bs at 50Hz, 1194A/m and 25 DEG C is 285mT, and Curie temperature Tc is 125
DEG C, electricalresistivityρ is 3 × 103Ω·m。
Embodiment 5
The present embodiment is prepared as follows MnZn ferrite magnetic sheets：
(1) according to Fe2O3Mole percent be 50mol%, the mole percent of ZnO is 24mol%, and surplus is MnO's
Molar ratio is scaled Fe2O3、Mn3O4It is weighed with the quality of ZnO, by load weighted Fe2O3、Mn3O4It is placed in ZnO
In sand mill, water is added, is sanded, time 60min is sanded, is then stirred 15min in stirring pool again, then sprayed
Mist is granulated, and obtains mixed material；
(2) pre-burning is carried out at 950 DEG C to step (1) described mixed material, the time of pre-burning is 3h, obtains pre-burning powder
Material；
(3) step (2) described preburning powdered material being placed in sand mill, water is added, is sanded, the sand milling time is 60min,
Then dried or be spray-dried, obtain water content 0.1% drying below powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and are ground, grinding when
Between be 20h, slurry is made；
(5) step (4) described slurry is cast, it is 0.3mm, area 160cm to obtain thickness2Raw cook, by institute
It states raw cook and is warming up to 1200 DEG C with the heating rate of 0.6 DEG C/min, be sintered, the oxygen content of sintering is 21%, sintering time
For 5h, two benches cool down after sintering, and the first stage is cooled to 900 DEG C with the rate of temperature fall of 3.0 DEG C/min, and the oxygen of first stage contains
Amount is 8%, and second stage is cooled to 30 DEG C with the rate of temperature fall of 3.0 DEG C/min, the oxygen content of second stage in 500ppm hereinafter,
The MnZn ferrites magnetic sheet is obtained, the MnZn ferrite magnetic sheets are smooth；
(6) polyethylene terephthalate film is all sticked in the two sides of step (5) the MnZn ferrites magnetic sheet, then
It carries out sliver and is punched into outer diameter 20mm, the ring of internal diameter 10mm tests magnetic conductivity real part μ ', use with AGILENT E4990A
CH3302 and baking oven test Curie temperature Tc, and the survey of saturation flux density Bs is carried out with the SY8218 instruments of Japanese Yan Qi companies
Examination.
By test, magnetic conductance of the MnZn ferrite magnetics loop that the present embodiment obtains at 128KHz, 0.25mT and 25 DEG C
Rate real part μ ' is 1490, and the saturation flux density Bs at 50Hz, 1194A/m and 25 DEG C is 450mT, and Curie temperature Tc is 118
DEG C, electricalresistivityρ is 22 Ω m.
Comparative example 1
The specific implementation mode of this comparative example is with reference to embodiment 1, and difference lies in step (5), sintering temperature is 900 DEG C.
Although smooth after the ferrite sheet sintering that this comparative example obtains, by test, the MnZn that this comparative example obtains
Magnetic conductivity real part μ ' of the ferrite magnetic loop at 128KHz, 0.25mT and 25 DEG C is only 430, in 50Hz, 1194A/m and 25 DEG C
Under saturation flux density Bs be only 260mT, Curie temperature Tc is 112 DEG C, and electricalresistivityρ is 4.7 × 103Ω·m。
Comparative example 2
The specific implementation mode reference embodiment 1 of this comparative example, difference lies in, in step (5), sintering temperature 1250
℃。
Surrounding warpage, intermediate muster, out-of-flatness can not use the ferrite sheet that this comparative example obtains after sintering.
Comparative example 3
The specific embodiment party of this comparative example is with reference to embodiment 1, and difference lies in step (1), according to Fe2O3Moles hundred
Score is 60mol%, and the mole percent of ZnO is 10mol%, and surplus is the molar ratio of MnO, is scaled Fe2O3、
Mn3O4It is weighed with the quality of ZnO.
By test, magnetic conductance of the MnZn ferrite magnetics loop that this comparative example obtains at 128KHz, 0.25mT and 25 DEG C
Rate real part μ ' is only 360, and the saturation flux density Bs at 50Hz, 1194A/m and 25 DEG C is 420mT, and Curie temperature Tc is 210
DEG C, electricalresistivityρ is 0.5 Ω m.
Based on the above embodiments with comparative example it is found that MnZn ferrites magnetic sheet provided by the invention is because component ratio closes
Suitable, preparation method is appropriate, thus thickness is thin, magnetic conductivity height, saturation induction density Bs high, resistivity height and Curie temperature Tc
It is high.Comparative example does not have scheme using the present invention, thus can not obtain the excellent results of the present invention.
Applicant states that the present invention illustrates the method detailed of the present invention, but the present invention not office by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, the selection etc. of concrete mode, all fall within protection scope of the present invention and the open scope.
Claims (10)
1. a kind of MnZn ferrites magnetic sheet, which is characterized in that the MnZn ferrites magnetic sheet includes ferro element, manganese element and zinc member
Element, wherein ferro element press Fe2O3Form meter, Zn-ef ficiency is based on ZnO forms, and manganese element is based on MnO forms, the MnZn ferrites
Fe in magnetic sheet2O3Mole percent be 48.5~50mol%, the mole percent of ZnO is 15~24mol%, surplus MnO,
The thickness of the MnZn ferrites magnetic sheet is 0.03~0.3mm.
2. MnZn ferrites magnetic sheet according to claim 1, which is characterized in that the area of the MnZn ferrites magnetic sheet is
0.25~160cm2；
Preferably, polyethylene terephthalate film is posted on the MnZn ferrites magnetic sheet two sides.
3. a kind of preparation method of MnZn ferrites magnetic sheet as claimed in claim 1 or 2, which is characterized in that the method packet
Include following steps：
(1) metal oxide starting material of formula ratio is mixed and is crushed, be then granulated, obtain mixed material；
(2) pre-burning is carried out to step (1) mixed material, obtains preburning powdered material；
(3) step (2) described preburning powdered material is crushed, then dries, obtains dry powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and is ground, obtain slurry；
(5) step (4) described slurry is cast, obtains raw cook, the raw cook is warming up to 950~1200 DEG C, is burnt
Knot, two benches cool down after sintering, obtain the MnZn ferrites magnetic sheet.
4. preparation method according to claim 3, which is characterized in that in step (1), the metal oxide starting material includes
Fe2O3、Mn3O4And ZnO；
Preferably, the mixing and broken method are to be sanded；
Preferably, the sand milling carries out in sand mill；
Preferably, water is added during the sand milling；
Preferably, step (1) time for mixing and being crushed is 20~60min；
Preferably, step (1) further includes：After mixing and being crushed, it is granulated again after 5~15min of cycle mixing；
Preferably, the mixed method of the cycle is to be stirred in stirring pool；
Preferably, the method for step (1) described granulation is mist projection granulating.
5. preparation method according to claim 3 or 4, which is characterized in that the temperature of step (2) described pre-burning be 750~
950℃；
Preferably, the time of step (2) described pre-burning is 1~3h；
Preferably, step (3) the broken method is to be sanded；
Preferably, the sand milling carries out in sand mill；
Preferably, water is added during the sand milling；
Preferably, step (3) the broken time is 20~60min；
Preferably, the method for step (3) described drying is drying or spray drying；
Preferably, the water content of the powder of step (3) described drying is below 0.1%.
6. preparation method according to any one of claims 1-5, which is characterized in that step (4) the organic solvent packet
Include ethyl alcohol；
Preferably, step (4) described adhesive includes polyvinyl alcohol；
Preferably, step (4) the plasticizer includes dioctyl phthalate；
Preferably, the time of step (4) described grinding is 8~20h.
7. according to the preparation method described in any one of claim 1-6, which is characterized in that the thickness of step (5) described raw cook
For 0.03~0.3mm；
Preferably, step (5) sintering carries out in sintering furnace；
Preferably, in step (5), the raw cook places into sintering furnace on smooth alumina plate or zirconium oxide plate；
Preferably, in step (5), heating rate≤0.8 DEG C≤min of the heating；
Preferably, in step (5), the time of the sintering is 1~5h；
Preferably, in step (5), the oxygen content of the sintering is 1%~21%；
Preferably, in step (5), the rate of temperature fall of the first stage of the two benches cooling is 1.0~3.0 DEG C≤min；
Preferably, in step (5), temperature is reduced to 900 DEG C by the first stage of the two benches cooling；
Preferably, in step (5), the oxygen content of the first stage of the two benches cooling is 1%~8%；
Preferably, in step (5), the rate of temperature fall of the second stage of the two benches cooling is 1.0~3.0 DEG C≤min；
Preferably, in step (5), temperature is reduced to 20~30 DEG C by the second stage of the two benches cooling；
Preferably, in step (5), the oxygen content of the second stage of the two benches cooling is in 500ppm or less.
8. according to the preparation method described in any one of claim 1-7, which is characterized in that the preparation method further includes step
(6)：Pad pasting is carried out to step (5) the MnZn ferrites magnetic sheet, sliver and punching is then carried out, obtains MnZn ferrite magnetic sheets
Product；
Preferably, pad pasting is all carried out on the two sides of MnZn ferrite magnetic sheets；
Preferably, the film used in the pad pasting is polyethylene terephthalate film.
9. according to the preparation method described in any one of claim 3-8, which is characterized in that the described method comprises the following steps：
(1) metal oxide starting material of formula ratio is placed in sand mill, water is added, is sanded, the sand milling time 20~
Then 60min is stirred 5~15min in stirring pool, then carries out mist projection granulating again, obtain mixed material；
(2) pre-burning is carried out at 750~950 DEG C to step (1) described mixed material, the time of pre-burning is 1~3h, obtains pre-burning
Powder；
(3) step (2) described preburning powdered material being placed in sand mill, water is added, is sanded, the sand milling time is 20~60min,
Then dried or be spray-dried, obtain water content 0.1% drying below powder；
(4) powder, organic solvent, adhesive and plasticizer of step (3) described drying are mixed and is ground, the time of grinding is
8~20h obtains slurry；
(5) step (4) described slurry is cast, it is 0.03~0.3mm raw cooks to obtain thickness, by the raw cook with≤0.8
DEG C≤heating rate of min is warming up to 950~1200 DEG C, it is sintered, the oxygen content of sintering is 1%~21%, sintering time
For 1~5h, two benches cool down after sintering, and the first stage is cooled to 900 DEG C with the rate of temperature fall of 1.0~3.0 DEG C≤min, and first
The oxygen content in stage is 1%~8%, and second stage is cooled to 20~30 DEG C with the rate of temperature fall of 1.0~3.0 DEG C≤min, second
The oxygen content in stage is in 500ppm hereinafter, obtaining the MnZn ferrites magnetic sheet；
(6) polyethylene terephthalate film is all sticked in the two sides of step (5) the MnZn ferrites magnetic sheet, then carried out
Sliver and punching obtain MnZn ferrite magnetic flake products；
Wherein, the metal oxide starting material is Fe2O3、Mn3O4And ZnO.
10. a kind of purposes of MnZn ferrites magnetic sheet as claimed in claim 1 or 2, which is characterized in that the MnZn ferrites
Magnetic sheet is used for wireless charging field.
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Denomination of invention: A MnZn ferrite magnetic sheet and its preparation method and application Effective date of registration: 20230522 Granted publication date: 20200605 Pledgee: Dongyang Branch of China Construction Bank Co.,Ltd. Pledgor: HENGDIAN GROUP DMEGC MAGNETICS Co.,Ltd. Registration number: Y2023330000949 |