CN109336578A - A kind of NiCuZn Ferrite Material and its preparation method and application - Google Patents

A kind of NiCuZn Ferrite Material and its preparation method and application Download PDF

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CN109336578A
CN109336578A CN201811256074.6A CN201811256074A CN109336578A CN 109336578 A CN109336578 A CN 109336578A CN 201811256074 A CN201811256074 A CN 201811256074A CN 109336578 A CN109336578 A CN 109336578A
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ball
raw material
drying
nio
zno
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於扬栋
王媛珍
单震
包宇航
苏艳锋
徐君
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Hengdian Group DMEGC Magnetics Co Ltd
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Hengdian Group DMEGC Magnetics Co Ltd
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Abstract

The present invention provides a kind of NiCuZn Ferrite Material and its preparation method and application.The NiCuZn Ferrite Material is mainly by Fe2O3, ZnO, NiO and CuO composition, by the integral molar quantity of the NiCuZn Ferrite Material be 100% in terms of, Fe2O3Mole percent be 49~50mol%, the mole percent of ZnO is 32~34mol%, and the mole percent of NiO is 8.1~10mol%, and the mole percent of CuO is 8~10.9mol%.Preparation method provided by the invention includes: (1) ingredient wet-mixing and is crushed, and then dries, obtains powder；(2) pre-burning is carried out after powder heating up；(3) crushing drying；(4) green compact are made；(5) it is sintered.NiCuZn Ferrite Material provided by the invention is functional, and complex permeability real part μ ' is high, and complex permeability imaginary part μ is " low.

Description

A kind of NiCuZn Ferrite Material and its preparation method and application
Technical field
The invention belongs to technical field of electronic materials more particularly to a kind of NiCuZn Ferrite Material and preparation method thereof and Purposes.
Background technique
With making rapid progress for the fast development of electronics and information industry, especially intelligent mobile terminal product, such as intelligent hand The consumer electronics products function such as machine, smartwatch tends to diversification, however the charging unit of most of electronic product is not mutually simultaneous Hold, power supply line is mixed and disorderly.Currently, the induction wireless charging system of technology maturation the most is preferable by its compatibility, carry Convenient, the advantages such as safety height are shown one's talent, but its existing significant deficiency is charge efficiency far below wired charging.
It is in induction wireless charging there are the reason of above problem, emitting end-coil and receiving end-coil is Separation, therefore the gap between two coupling coils is larger, causes coil coupling not close, there are biggish leakage inductances.In addition, due to assembly Limited space, coil are in metal environment, and the change in magnetic flux density between two coils is weakened severely, and then affects energy Efficiency of transmission.To solve the above problems, engineering staff's selection receives end-coil and metal in wireless charging system One piece of soft magnetic ferrite is added between piece as antifreeze plate, it is desirable that antifreeze plate has high magnetic permeability, low-loss, i.e. antifreeze plate The real part of complex permeability is big, and imaginary part is small.
Currently, magnetic material antifreeze plate major part in the market is all NiZnCu ferrite antifreeze plate.More generally The 44 type NiZnCu Ferrite Material of Material of Fair Rite company, magnetic property is between 100~200kHz, ferrite magnetic Piece real part also can only achieve 500, imaginary part 10 or so.So improving its receiving end antifreeze plate from the point of view of with regard to the development of current wireless charging Magnetic conductivity real part, reduce imaginary part be still problem to be solved.
104030674 A of CN discloses a kind of NiZnCu Ferrite Material and preparation method thereof, and main composition is with moles hundred Divide ratio are as follows: Fe2O3: 48.5~49.5mol%；ZnO:25~29mol%；NiO:11.5~20.5mol%；CuO:5~ 9.5mol%；Adulterate composition mass percent are as follows: 0≤V2O5≤ 0.12wt%.The NiCuZn Ferrite Material prepared is 100 ~200kHz frequency separation, initial permeability μ rate area are 950~1000；
104909736 A of CN discloses a kind of nickel-zinc-ferrite material and preparation method thereof, raw material composition include it is main at Point and accessory ingredient, content of the principal component in terms of respective reference substance are as follows: 49.6mol%≤Fe2O3≤ 50.5mol%, 12.5mol% ≤ NiO≤13.5mol%, 29.2mol%≤ZnO≤32mol%, 7mol%≤CuO≤9mol%.Opposite principal component, it is secondary at Divide the content in terms of reference substance are as follows: 0.01wt%≤MoO3≤ 0.1wt%, 0.01wt%≤Nd2O3≤ 0.05wt%.The nickel Zn ferrite is prepared using traditional conventional ceramic technique, in the frequency separation of 100~200kHz, magnetic conductivity 700≤μ '≤900.
105837195 A of CN discloses a kind of NiZnCu Ferrite Material and preparation method thereof.The NiZnCu ferrite material Expect that its formula is NixZnyCu1-x-yFe2-aO3-3a/2, 0.24≤x≤0.25,0.58≤y≤0.61,0.02≤a≤0.03, original Expect that main composition is NiO, ZnO, CuO and Fe2O3, non-impurity-doped；At 1MHz, magnet ring is sintered under conditions of 1000 DEG C, plural magnetic conductance The real part μ ' of rate is 1300~1400, and imaginary part μ " is 150~160.
In the above-mentioned published patent, material property is all using the performance of magnetic core test, and corresponding is wireless charging with firmly Matter magnetic sheet, and limited by the receiving end condition of wireless charging, it generallys use with ferrite sheet flexible, in order to realize ferrite Piece has good stickiness and flexibility, and ferrite sheet upper and lower surfaces after sintering are bonded PET (poly- terephthaldehyde respectively Sour glycol ester) sliver processing is carried out after one side glue and PSA (acrylate pressure sensitive adhesive) double-sided adhesive, ferrite sheet is broken into several Small pieces.But since there are air gaps between ferrite fragment after sliver, lead to the real part μ ' and void of the complex permeability of ferrite sheet Portion μ " can have greater attenuation, the experiment proved that, according to the complex permeability index announced in above-mentioned patent, wireless charging is made The magnetic permeability μ of the flexible ferrite sheet of receiving end ' be also not achieved 500, causes wireless charging efficiency low.
Summary of the invention
Aiming at the above shortcomings existing in the prior art, the purpose of the present invention is to provide a kind of NiCuZn Ferrite Materials And its preparation method and application.NiCuZn Ferrite Material magnetic conductivity real part provided by the invention is high, and loss is low, and performance is stablized, Lower production costs can be used for induction wireless charging technology, particularly suitable for flexibility needed for wireless charging receiving terminal Ferrite antifreeze plate.
To achieve this purpose, the present invention adopts the following technical scheme:
In a first aspect, the present invention provides a kind of NiCuZn Ferrite Material, the NiCuZn Ferrite Material mainly by Fe2O3, ZnO, NiO and CuO composition, by the integral molar quantity of the NiCuZn Ferrite Material be 100% in terms of, Fe2O3Moles hundred Score is 49~50mol%, and the mole percent of ZnO is 32~34mol%, and the mole percent of NiO is 8.1~10mol%, The mole percent of CuO is 8~10.9mol%.
It is Fe in terms of 100% by the integral molar quantity of the NiCuZn Ferrite Material in the present invention2O3Mole percent be 49~50mol%, such as 49mol%, 49.2mol%, 49.4mol%, 49.6mol%, 49.8mol% or 50mol% etc., but It is not limited in cited numerical value, other unlisted numerical value are equally applicable in the numberical range；
The mole percent of ZnO is 32~34mol%, such as 32mol%, 32.5mol%, 33mol%, 33.5mol% Or 34mol% etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable；
The mole percent of NiO be 8.1~10mol%, such as 8.1mol%, 8.5mol%, 9mol%, 9.5mol% or 10mol% etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable；
The mole percent of CuO be 8~10.9mol%, such as 8mol%, 9mol%, 10mol% or 10.9mol% etc., It is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
The formula of the iron deficiency or positive score value that use in the present invention, it requires above-mentioned Fe2O3Molar ratio be not more than 50%. Since Ferrite Material is in the formula of iron deficiency and positive score value, sintering process is less prone to Fe2+, so that it is higher to obtain resistivity Material, so that NiZnCu ferrite has compared with low-loss.
Heretofore described ZnO content requires control within the scope of 32.0~34.0mol%, because in NiZnCu iron oxygen In body, the Ferrite Material of high magnetic permeability is obtained, it is desirable that ZnO content is improved, with Zn2+Content increases, it can be A original On Fe3+Ion is extruded into B, and the molecular magnetic moment in material will increase, and then magnetic conductivity is caused to rise.But in view of in the present invention Material be applied in the mobile terminal devices such as smart phone, it is desirable that it requires its Curie's temperature with desired operating temperatures thus Degree is not less than 95 DEG C.In Ferrite Material, with the increase of ZnO content, Curie temperature Tc can be substantially reduced, this is because Zn2+It is more with zinc ion is contained in ferrite for non magnetic ion, A and the magnetic ion number on the position B are reduced, so that A Superexchange interaction between position and B weakens, so as to cause Curie temperature Tc decline.
Heretofore described NiO content requirement controls whole NiO and Fe within the scope of 8.1~10.0mol%2O3Hair Raw reaction generates Ni ferrite, and Ni ferrite is magnetic phase；If NiO content is lower than 8.0mol%, NiZnCu Ferrite Material Magnetic conductivity can reduce.Further, it is also possible to using Ni2O3As raw material, according to the molar ratio calculated weight of nickel content.
Suitable CuO is added in the ferritic main formula of NiZn in the present invention, can achieve reduces sintering temperature and mention The purpose of high densifying materials.
Within the scope of 100~300kHz, the real part μ ' of complex permeability is NiZnCu Ferrite Material provided by the invention ≤ 50,100kHz of 1900~2300 and imaginary part μ ", 1194A/m, saturation induction density Bs >=255mT at 25 DEG C, coercivity H ≤ 65A/m, 100kHz, 200mT, power loss Pcv is 300~400mW/m at 25 DEG C3, Curie temperature Tc is 95~110 DEG C.
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 technical purpose and beneficial effect of the invention.
It further include MoO in the NiCuZn Ferrite Material as currently preferred technical solution3, with Fe2O3、ZnO、 The gross mass of NiO and CuO is 100% meter, the MoO3Mass percent in terms of reference substance is 0.01~0.1wt%, such as 0.01wt%, 0.03wt%, 0.05wt%, 0.07wt%, 0.09wt% or 0.1wt% etc., it is not limited to cited Numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
It preferably, further include Bi in the NiCuZn Ferrite Material2O3, with Fe2O3, ZnO, NiO and CuO gross mass For 100% meter, the Bi2O3Mass percent in terms of reference substance is 0.0~0.1wt%.Such as 0.0wt%, 0.01wt%, 0.03wt%, 0.05wt%, 0.07wt%, 0.09wt% or 0.1wt% etc., it is not limited to cited numerical value, the number It is equally applicable to be worth other unlisted numerical value in range.
In the present invention, MoO3And Bi2O3For accessory ingredient, they are low melting point, and appropriate addition can promote material to cause Densification.MoO3The growth that can promote crystal grain improves the initial permeability of material, reduces sintering temperature to a certain extent, and It can show and reduce Bi2O3Additive amount, but it is also not easy excess, because of MoO3For namagnetic substance, NiZnCu ferrite A, B can be weakened The superexchange interaction of interdigit leads to the reduction of material Curie temperature Tc and saturation induction density Bs.Experiments have shown that in NiZnCu Bi is added in Ferrite Material2O3More than 0.2wt%, it is easy to when manufactured ferrite sheet lamination is sintered, between piece and piece glutinous Even, and there is " big crystal grain " of discrete distribution in sintered ferrite sheet surface.In addition, because MoO3And Bi2O3Content pole It is low, therefore be not included in the integral molar quantity or gross mass of the NiCuZn Ferrite Material when calculating, but directly with Fe2O3, ZnO, NiO and CuO gross mass as measure MoO3And Bi2O3The standard of additional amount.
Preferably, the NiCuZn Ferrite Material is flaky material.
Second aspect, the present invention provides a kind of preparation method of NiCuZn Ferrite Material as described in relation to the first aspect, described Method the following steps are included:
(1) to the Fe of formula ratio2O3Raw material, ZnO raw material, NiO raw material and CuO raw material carry out wet-mixing and are crushed, then Drying, obtains powder；
(2) to pre-burning is carried out after the heating of step (1) powder, preburning powdered material is obtained；
(3) step (2) described preburning powdered material is crushed, is then dried, obtain drying powder；
(4) green compact are made in step (3) the drying powder；
(5) step (4) described green compact are sintered, obtain the NiCuZn Ferrite Material.
The mutual cooperation of each step of preparation method provided by the invention ensure that the NiCuZn Ferrite Material prepared Excellent performance, while process is short, technique is easily controllable, and product stability is good, is conducive to mass production.
As currently preferred technical solution, step (1) described Fe2O3Fe in raw material2O3Mass fraction >= 99.4wt%, such as 99.4wt%, 99.5wt%, 99.6wt%, 99.7wt%, 99.8wt% or 99.9wt% etc., i.e., preferably Fe2O3Purity >=99.4wt% of raw material.
Preferably, in step (1) the ZnO raw material ZnO mass fraction >=98.0wt%, such as 98wt%, 98.5wt%, 99wt% or 99.5wt% etc., i.e., purity >=98.0wt% of preferred ZnO raw material.
Preferably, in step (1) the NiO raw material NiO mass fraction >=99.0wt%, such as 99.0wt%, 99.2wt%, 99.4wt%, 99.6wt% or 99.8wt% etc., i.e., purity >=99.0wt% of preferred NiO raw material.
Preferably, in step (1) the CuO raw material CuO mass fraction >=98.0wt%, such as 98wt%, 98.5wt%, 99wt% or 99.5wt% etc., i.e., purity >=98.0wt% of preferred CuO raw material.
Preferably, step (1) wet-mixing and broken method are ball milling.
Preferably, in the mechanical milling process, the mass ratio of raw material to be broken, water and zirconium ball is 1:1:5, the mechanical milling process Middle water is solvent, and zirconium ball is ball-milling medium.The mass ratio of raw material, water and zirconium ball is not limited to said ratio in the present invention.
Preferably, the ball milling carries out in planetary ball mill, horizontal ball mill or sand mill, preferably in sand mill Middle progress.
Preferably, when the ball milling carries out in a planetary ball mill, Ball-milling Time be 1~2h, such as 1h, 1.5h or 2h etc., rotational speed of ball-mill are 250~300r/min, such as 250r/min, 260r/min, 270r/min, 280r/min, 290r/min Or 300r/min etc..
Preferably, when the ball milling carries out in horizontal ball mill, zirconium bulb diameter is usedWithTwo kinds Size,Zirconium ball andThe mass ratio of zirconium ball is 1:1.
Preferably, when the ball milling carries out in horizontal ball mill, Ball-milling Time is 2~6h, such as 2h, 3h, 4h, 5h Or 6h etc., rotational speed of ball-mill are 40~80r/min, such as 40r/min, 50r/min, 60r/min, 70r/min or 80r/min etc..
In the present invention, the mass ratio of zirconium bulb diameter and size and zirconium ball is not limited to above range.
Preferably, when the ball milling carries out in sand mill, Ball-milling Time be 1~2h, such as 1h, 1.5h or 2h etc., Rotational speed of ball-mill is 50~100r/min, such as 50r/min, 60r/min, 70r/min, 80r/min, 90r/min or 100r/min Deng.
Preferably, when the ball milling carries out in sand mill, the size of zirconium ball isIn the present invention, zirconium Bulb diameter and size are not limited to above range.
Preferably, step (1) drying carries out in baking oven or spray-drying installation.The spray-drying installation includes Pressure spray dryer device or centrifugal spray drying device.
Preferably, when step (1) drying carries out in an oven, drying temperature is 100~120 DEG C, such as 100 DEG C, 105 DEG C, 110 DEG C, 115 DEG C or 120 DEG C etc., it is not limited to cited numerical value, other are unlisted in the numberical range Numerical value it is equally applicable.
Preferably, when step (1) drying carries out in spray-drying installation, the import of the spray-drying installation Temperature is 350~400 DEG C, such as 350 DEG C, 360 DEG C, 370 DEG C, 380 DEG C or 400 DEG C etc., outlet temperature is 95~115 DEG C, example Such as 95 DEG C, 100 DEG C, 105 DEG C, 110 DEG C or 115 DEG C, it is not limited to cited numerical value, in the numberical range, other are not The numerical value enumerated is equally applicable.
Preferably, when step (1) drying carries out in spray-drying installation, in wet-mixing and broken process Middle addition polyvinyl alcohol (PVA) aqueous solution, the concentration of polyvinyl alcohol (PVA) aqueous solution are 10wt%, the polyvinyl alcohol Additional amount be Fe2O36~8wt% of the gross mass of raw material, ZnO raw material, NiO raw material and CuO raw material, such as 6wt%, 6.5wt%, 7wt%, 7.5wt% or 8wt% etc..It is not limited to cited numerical value, interior other of the numberical range are not arranged The numerical value of act is equally applicable.
As currently preferred technical solution, in step (2), step (1) described powder is first placed in aluminium oxide saggar And/or in zirconium oxide saggar after carry out pre-burning again.
Preferably, the heating rate of step (2) described heating is 2~4 DEG C/min, such as 2 DEG C/min, 3 DEG C/min or 4 DEG C/min etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, the temperature of step (2) described pre-burning be 860~940 DEG C, such as 860 DEG C, 870 DEG C, 880 DEG C, 890 DEG C, 900 DEG C, 910 DEG C, 920 DEG C, 930 DEG C or 940 DEG C etc., it is not limited to cited numerical value, in the numberical range, other are not The numerical value enumerated is equally applicable.
Preferably, the time of step (2) described pre-burning is 2~3h, such as 2h, 2.5h or 3h etc., it is not limited to institute The numerical value enumerated, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, step (2) described pre-burning carries out in pushed bat kiln, roller kilns or rotary kiln
Preferably, when step (2) described pre-burning carries out in rotary kiln, kiln bore is 1~1.8m, the length of high-temperature region Degree is 5~10m, and high-temperature region set temperature is 860~940 DEG C, and the rotation speed of rotary kiln is 5~20r/min, rotary kiln charging Amount is 80~200kg/ hours.
As currently preferred technical solution, in step (3), further includes: the MoO of formula ratio is added before broken3With/ Or Bi2O3。
Preferably, step (3) the broken method is ball milling.
Preferably, the ball milling carries out in the ball mill.
Preferably, the ball milling slurry granularity control is in 1.0~1.4 μ ms in D50.
Preferably, the time of the ball milling is 1~2h, such as 1h, 1.5h or 2h etc., the revolving speed of ball milling is 250~300r/ Min, such as 250r/min, 260r/min, 270r/min, 280r/min, 290r/min or 300r/min etc., it is not limited to Cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, in the mechanical milling process, the mass ratio of material to be broken, water and zirconium ball is 1:1.25:5.
Preferably, the temperature of step (3) described drying be 100~200 DEG C, such as 100 DEG C, 120 DEG C, 140 DEG C, 160 DEG C, 180 DEG C or 200 DEG C etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, step (3) drying carries out in an oven.
As currently preferred technical solution, in step (4), the method that green compact are made includes: by step (3) institute It states sieving after drying powder is mixed with binder and is granulated simultaneously compression moulding, obtain green compact.This blank-making method is finally obtaining Ferrite bead is for test material performance.
Preferably, the binder includes polyvinyl alcohol (PVA) aqueous solution.The polyvinyl alcohol is that the concentration of aqueous solution is 10wt%.
Preferably, the additional amount of the binder be step (3) it is described drying powder and binder gross mass 6wt~ 8wt%, such as 6wt%, 6.5wt%, 7wt%, 7.5wt% or 8wt% etc., it is not limited to cited numerical value, the number It is equally applicable to be worth other unlisted numerical value in range.
Preferably, the pressure of the compression moulding is 5~8MPa, such as 5MPa, 6MPa, 7MPa or 8MPa etc., but not It is only limitted to cited numerical value, other unlisted numerical value are equally applicable in the numberical range.
Preferably, the compression moulding suppresses green compact circlewise.Magnet ring is made, can be used for detecting Ferrite Material Performance.
Preferably, in step (4), the method that green compact are made includes: to mix to step (3) the drying powder Slurry carries out tape casting to obtained slurry, obtains green compact, and the green compact are sheet.The method of this green compact processed can be most After obtain flexible ferrite sheet material.
As currently preferred technical solution, the temperature of step (5) described sintering is 940~1000 DEG C, such as 940 DEG C, 960 DEG C, 980 DEG C or 1000 DEG C etc., it is not limited to cited numerical value, other unlisted numbers in the numberical range It is worth equally applicable.
Preferably, the time of step (5) described sintering is 2~3h, such as 2h, 2.5h or 3h etc., it is not limited to institute The numerical value enumerated, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, step (5) further include: when step (4) green compact are sheet, in the obtained NiCuZn iron oxygen The two sides of body material is bonded polyethylene terephthalate (PET) one side glue and acrylate pressure sensitive adhesive (PSA) double-sided adhesive respectively Sliver processing is carried out afterwards, obtains flexible NiCuZn ferrite sheet material.
As the further preferred technical solution of preparation method of the present invention, the preparation method comprises the following steps:
(1) to the Fe of formula ratio2O3Raw material, ZnO raw material, NiO raw material and CuO raw material carry out ball milling, ball milling in the ball mill Time is 1~2h, and rotational speed of ball-mill is 250~300r/min, and in mechanical milling process, the mass ratio of raw material to be broken, water and zirconium ball is Then 1:1:5 dries 100~120 DEG C in an oven, obtains powder；
(2) step (1) described powder is placed in aluminium oxide saggar and/or zirconium oxide saggar, with the liter of 2~4 DEG C/min Warm rate carries out pre-burning after being warming up to 860~940 DEG C, the time of pre-burning is 2~3h, obtains preburning powdered material；
(3) MoO of formula ratio is added into step (2) described preburning powdered material3And/or Bi2O3Afterwards, it carries out in the ball mill Ball milling, time of ball milling are 1~2h, and the revolving speed of ball milling is 250~300r/min, in mechanical milling process, material, water and zirconium to be broken The mass ratio of ball is 1:1.25:5, then 100~200 DEG C of drying in an oven, obtains drying powder；
(4) slurry is carried out to step (3) the drying powder, tape casting is carried out to obtained slurry, obtains green compact, institute Stating green compact is sheet；
(5) step (4) described green compact are sintered at 940~1000 DEG C, the time of sintering is 2~3h, after sintering It is bonded polyethylene terephthalate (PET) one side glue and acrylic acid respectively on the two sides of obtained NiCuZn Ferrite Material Sliver processing is carried out after pressure sensitive adhesive (PSA) double-sided adhesive, obtains flexible NiCuZn ferrite sheet material.
The third aspect, the present invention provides a kind of purposes of NiCuZn Ferrite Material as described in relation to the first aspect, described NiCuZn Ferrite Material is used for wireless charging field.NiCuZn Ferrite Material provided by the invention is particularly well suited as nothing Flexible ferrite antifreeze plate needed for line charge electricity receiving end.
Compared with prior art, the invention has the following advantages:
(1) present invention is realized using reasonable formula by controlling each constituent of NiZnCu Ferrite Material NiZnCu Ferrite Material has high magnetic conductivity and lower power loss.Within the scope of 100~300kHz, complex permeability Real part μ ' be 1900~2300, imaginary part μ "≤50；Saturation induction density is tested under the conditions of 100kHz, 1194A/m, 25 DEG C Bs >=255mT, coercivity H≤65A/m；350~450mW/m of its power loss under conditions of 100kHz, 200mT, 25 DEG C3； Curie temperature Tc is 95~110 DEG C.The flexible ferrite sheet prepared in the present invention using above-mentioned NiZnCu Ferrite Material, Within the scope of 100~300kHz, the real part μ ' of complex permeability is that 650~850, imaginary part μ " is 1~20, Curie temperature Tc be 95~ 110℃.Above-mentioned flexibility ferrite sheet is applied to the receiving end of wireless charging, and the efficiency of wireless charging is increased to 75~85%.
(2) preparation method process provided by the invention is short, and technique is easily controllable, and product stability is good, is conducive to batch metaplasia It produces.
Detailed description of the invention
Fig. 1 is the complex permeability magnetic spectrum for the NiCuZn ferrite bead that the embodiment of the present invention 1 provides；
Fig. 2 is the hysteresis loop BH curve for the NiCuZn ferrite bead that the embodiment of the present invention 1 provides；
Fig. 3 is the magnetic permeability μ for the NiCuZn ferrite bead that the embodiment of the present invention 9 provides and the variation relation figure of temperature T；
Fig. 4 is the complex permeability magnetic spectrum for the NiCuZn ferrite sheet that the embodiment of the present invention 9 provides.
Specific embodiment
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, below further specifically to the present invention It is bright.But following embodiments is only simple example of the invention, does not represent or limit the scope of the present invention, this Invention protection scope is subject to claims.
The following are typical but non-limiting embodiments of the invention:
Embodiment 1
The present embodiment is prepared as follows NiCuZn Ferrite Material:
(1) constituent Fe is pressed2O3It is for 49.85mol%, ZnO 32.95mol%, NiO 8.1mol%, CuO The formula of 9.1mol% weighs raw material；Wherein, the purity requirement of raw material are as follows: Fe2O3It is for 99.46wt%, ZnO 98.15wt%, NiO 99.38wt%, CuO 98.26wt%.By gained ingredient, ball milling 1h, revolving speed are in planetary ball mill 275r/min, the mass ratio of raw material, water and zirconium ball are 1:1:5；Wherein, zirconium ball isThe mixing of 1:1 in mass ratio makes With.Obtained slurry is put into baking oven, obtains powder in 120 DEG C of drying.
(2) by pre-burning in the obtained powder merging zirconium oxide saggar of step (1), temperature is that 880 DEG C of heating rates are 2 DEG C/min, soaking time 2.5h.
(3) principal component (i.e. Fe is mixed in the obtained material of step (2) pre-burning2O3, NiO, ZnO and CuO) gross mass The MoO of 0.05wt%3, then ball milling 1h in a planetary ball mill, revolving speed 275r/min, the quality of raw material, water and zirconium ball it Than for 1:1.25:5.Secondary ball milling slurry granularity is D50:1.23 μm.The obtained slurry of ball milling is put into baking oven, at 120 DEG C Drying obtains powder.
(4) polyvinyl alcohol (PVA) aqueous solution of the 7wt% of gross mass, poly- second are added in step (3) obtained powder The concentration of enol (PVA) aqueous solution is 10wt%, is uniformly mixed, and sieving is granulated, compression moulding magnet ring green compact.Briquetting pressure control In 6MPa.
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 968 DEG C, keep the temperature 2.5h after it is naturally cold with furnace But, sintered magnet ring is obtained.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 968 DEG C Ferrite sintered body piece is obtained after sintering, then is bonded PET one side glue and PSA double-sided adhesive respectively in ferrite sintered body piece upper and lower surfaces Sliver processing is carried out afterwards, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 1.
Fig. 1 is the complex permeability magnetic spectrum of the NiCuZn ferrite bead provided in the present embodiment, it can be seen that test When frequency f=300kHz, it " is 30.62 that μ ', which is 2136.38, μ,；In addition, can be seen that by the magnetic spectrum for being sintered magnet ring as frequency f Within the scope of=100~300kHz, the real part μ ' of the ferritic complex permeability of NiCuZn is 1900~2300 and imaginary part μ "≤50.
Fig. 2 is the hysteresis loop BH curve of the NiCuZn ferrite bead provided in the present embodiment, it can be seen that When test condition is 100kHz, 1194A/m, 25 DEG C, the ferritic saturation induction density Bs >=255mT of NiCuZn, coercivity Hc≤65A/m。
Embodiment 2
The present embodiment is prepared as follows NiCuZn Ferrite Material:
(1) constituent Fe is pressed2O3It is for 49.5mol%, ZnO 33.0mol%, NiO 8.15mol%, CuO The formula of 9.35mol% weighs raw material；Wherein to consider the purity of raw material, the purity requirement of raw material are as follows: Fe2O3For 99.46wt%, ZnO 98.15wt%, NiO 99.38wt%, CuO 98.26wt%.By gained ingredient in sand mill into Row grinding, the milling time of sand mill are 1h, revolving speed 72r/min, and the mass ratio of raw material, water and zirconium ball is 1:1:5, zirconium ball Sphere diameter isWherein, polyvinyl alcohol (PVA) aqueous solution of the 6wt% of raw material gross mass, polyvinyl alcohol (PVA) is added The concentration of aqueous solution is 10wt%, is mixed together ball milling.Obtained slurry is poured into stirring pool, using the side of press atomization Method implements granulating and drying, inlet temperature are as follows: and 350~400 DEG C, outlet temperature are as follows: 95~115 DEG C.
(2) by the obtained powder merging storage hopper of step (1), hopper tail end accesses rotary kiln entrance, using revolution Kiln carries out pre-burning.The kiln bore of rotary kiln is 1.5m, and the length of high-temperature region is 8m, and high-temperature region set temperature is 910 DEG C, revolution The rotation speed of kiln is 12r/min, and inlet amount is 140kg/ hours.
Step (3) and (4) are same as Example 1.Wherein in step (3), secondary ball milling slurry granularity is D50:1.26 μm.
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 972 DEG C, keep the temperature 2h after cooling be sintered Magnet ring afterwards.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 972 DEG C Ferrite sintered body piece is obtained after sintering, then is bonded PET one side glue and PSA double-sided adhesive respectively in ferrite sintered body piece upper and lower surfaces Sliver processing is carried out afterwards, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 1.
Embodiment 3
The present embodiment is prepared as follows NiCuZn Ferrite Material:
(1) constituent Fe is pressed2O3It is for 49.5mol%, ZnO 33.15mol%, NiO 8.5mol%, CuO The formula of 8.85mol% weighs raw material；The purity requirement of raw material are as follows: Fe2O3For 99.46wt%, ZnO 98.15wt%, NiO is 99.38wt%, CuO 98.26wt%.By gained ingredient in planetary ball mill ball milling 1h, revolving speed 275r/min, The mass ratio of raw material, water and zirconium ball is 1:1:5；Wherein, zirconium ball is1:1 is used in mixed way in mass ratio.By gained To slurry material be put into baking oven, obtain powder in 120 DEG C of drying.
Step (2), (3) and (4) is same as Example 1.Wherein in step (3), principal component (i.e. Fe is mixed2O3、NiO、ZnO And CuO) gross mass 0.05wt% MoO3With the Bi of 0.05wt%2O3Secondary ball milling is carried out, ball milling slurry granularity is D50: 1.21μm。
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 963 DEG C, keep the temperature 3h after cooling be sintered Magnet ring afterwards.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 963 DEG C Ferrite sintered body piece is obtained after sintering, then is bonded PET one side glue and PSA double-sided adhesive respectively in ferrite sintered body piece upper and lower surfaces Sliver processing is carried out afterwards, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 1.
Embodiment 4
The present embodiment is prepared as follows NiCuZn Ferrite Material:
(1) constituent Fe is pressed2O3It is for 49.2mol%, ZnO 33.45mol%, NiO 8.75mol%, CuO The formula of 8.6mol% weighs raw material；Wherein, the purity requirement of raw material are as follows: Fe2O3It is for 99.46wt%, ZnO 98.15wt%, NiO 99.38wt%, CuO 98.26wt%.By gained ingredient, ball milling 1h, revolving speed are in planetary ball mill 275r/min, the mass ratio of raw material, water and zirconium ball are 1:1:5；Wherein, zirconium ball isThe mixing of 1:1 in mass ratio makes With.Obtained slurry is put into baking oven, obtains powder in 120 DEG C of drying.
Step (2), (3) and (4) is same as Example 1.Wherein in step (3), principal component (i.e. Fe is mixed2O3、NiO、ZnO And CuO) gross mass 0.05wt% MoO3With the Bi of 0.05wt%2O3Secondary ball milling is carried out, ball milling slurry granularity is D50: 1.27μm。
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 965 DEG C, keep the temperature 2.5h after cooling burnt Magnet ring after knot.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 965 DEG C Ferrite sintered body piece is obtained after sintering, then is bonded PET one side glue and PSA double-sided adhesive respectively in ferrite sintered body piece upper and lower surfaces Sliver processing is carried out afterwards, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 1.
Embodiment 5
The specific preparation method of the present embodiment is referring to embodiment 2, and difference is, in step (1), by constituent Fe2O3For 49.0mol%, ZnO 34.0mol%, NiO 9.0mol%, CuO are that the formula of 8.0mol% weighs raw material.Step (3) In, mix principal component (i.e. Fe2O3, NiO, ZnO and CuO) gross mass 0.01wt% MoO3With the Bi of 0.01wt%2O3。
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 2.
Embodiment 6
The present embodiment is prepared as follows NiCuZn Ferrite Material:
(1) constituent Fe is pressed2O3It is for 50.0mol%, ZnO 32.0mol%, NiO 10.0mol%, CuO The formula of 8.0mol% weighs raw material.Wherein, the purity requirement of raw material are as follows: Fe2O3It is for 99.46wt%, ZnO 98.15wt%, NiO 99.38wt%, CuO 98.26wt%.By gained ingredient, ball milling 1h, revolving speed are in planetary ball mill 275r/min, the mass ratio of raw material, water and zirconium ball are 1:1:5；Wherein, zirconium ball isThe mixing of 1:1 in mass ratio makes With.Obtained slurry is put into baking oven, obtains powder in 120 DEG C of drying.
Step (2), (3) and (4) is same as Example 1.Wherein in step (3), principal component (i.e. Fe is mixed2O3、NiO、ZnO And CuO) gross mass 0.10wt% MoO3With the Bi of 0.10wt%2O3Secondary ball milling is carried out, ball milling slurry granularity is D50: 1.26μm。
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 950 DEG C, keep the temperature 2.0h after cooling burnt Magnet ring after knot.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 950 DEG C Ferrite sintered body piece is obtained after sintering, then is bonded PET one side glue and PSA double-sided adhesive respectively in ferrite sintered body piece upper and lower surfaces Sliver processing is carried out afterwards, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 2.
Embodiment 7
The specific preparation method of the present embodiment is referring to embodiment 2, and difference is, in step (1), by constituent Fe2O3For 49.0mol%, ZnO 32.0mol%, NiO 8.1mol%, CuO are that the formula of 10.9mol% weighs raw material.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 2.
Embodiment 8
(1) constituent Fe is pressed2O3It is for 49.85mol%, ZnO 32.95mol%, NiO 8.1mol%, CuO The formula of 9.1mol% weighs raw material；Wherein, the purity requirement of raw material are as follows: Fe2O3It is for 99.46wt%, ZnO 98.15wt%, NiO 99.38wt%, CuO 98.26wt%.By gained ingredient, ball milling 2h, revolving speed are in planetary ball mill 250r/min, the mass ratio of raw material, water and zirconium ball are 1:1:5；Wherein, zirconium ball isThe mixing of 1:1 in mass ratio makes With.Obtained slurry is put into baking oven, obtains powder in 110 DEG C of drying.
(2) by pre-burning in the obtained powder merging zirconium oxide saggar of step (1), temperature is that 860 DEG C of heating rates are 3 DEG C/min, soaking time 3h.
(3) principal component (i.e. Fe is mixed in the obtained material of step (2) pre-burning2O3, NiO, ZnO and CuO) gross mass The MoO of 0.05wt%3, then ball milling 1.5h in a planetary ball mill, revolving speed 255r/min, the quality of raw material, water and zirconium ball The ratio between be 1:1.25:5.Secondary ball milling slurry granularity is D50:1.23 μm.The obtained slurry of ball milling is put into baking oven, 100 DEG C drying obtains powder.
(4) polyvinyl alcohol (PVA) aqueous solution of the 6wt% of gross mass, poly- second are added in step (3) obtained powder The concentration of enol (PVA) aqueous solution is 10%, is uniformly mixed, and sieving is granulated, compression moulding magnet ring green compact.Briquetting pressure control exists 5MPa。
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 940 DEG C, keep the temperature 2.5h after it is naturally cold with furnace But, sintered magnet ring is obtained.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 940 DEG C Ferrite sintered body piece is obtained after sintering, then is bonded PET one side glue and PSA double-sided adhesive respectively in ferrite sintered body piece upper and lower surfaces Sliver processing is carried out afterwards, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 3.
Embodiment 9
(1) constituent Fe is pressed2O3It is for 49.85mol%, ZnO 32.95mol%, NiO 8.1mol%, CuO The formula of 9.1mol% weighs raw material；Wherein, the purity requirement of raw material are as follows: Fe2O3It is for 99.46wt%, ZnO 98.15wt%, NiO 99.38wt%, CuO 98.26wt%.By gained ingredient in planetary ball mill ball milling 1.5h, revolving speed For 300r/min, the mass ratio of raw material, water and zirconium ball is 1:1:5；Wherein, zirconium ball isThe mixing of 1:1 in mass ratio makes With.Obtained slurry material is put into baking oven, obtains powder in 100 DEG C of drying.
(2) by pre-burning in the obtained powder merging zirconium oxide saggar of step (1), temperature is that 940 DEG C of heating rates are 4 DEG C/min, soaking time 2h.
(3) principal component (i.e. Fe is mixed in the obtained material of step (2) pre-burning2O3, NiO, ZnO and CuO) gross mass The MoO of 0.05wt%3, then ball milling 2h in a planetary ball mill, revolving speed 300r/min, the quality of raw material, water and zirconium ball it Than for 1:1.25:5.Secondary ball milling slurry granularity is D50:1.23 μm.The obtained slurry of ball milling is put into baking oven, at 200 DEG C Drying obtains powder.
(4) polyvinyl alcohol (PVA) aqueous solution of the 8wt% of gross mass, poly- second are added in step (3) obtained powder The concentration of enol (PVA) aqueous solution is 10%, is uniformly mixed, and sieving is granulated, compression moulding magnet ring green compact.Briquetting pressure control exists 8MPa。
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 1000 DEG C, keep the temperature 2.0h after it is naturally cold with furnace But, sintered magnet ring is obtained.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 1000 Ferrite sintered body piece is obtained after DEG C sintering, then is bonded PET one side glue respectively in ferrite sintered body piece upper and lower surfaces and PSA is two-sided Sliver processing is carried out after glue, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 3.
Fig. 3 is the magnetic permeability μ of the NiCuZn ferrite bead provided in the present embodiment and the variation diagram of temperature T, by the figure It can be seen that μ starts to decay, according to Curie temperature computing rule, i.e. 0.8 μ at 100 DEG CmaxWith 0.2 μmaxThe company of two o'clock The temperature of line and the intersection point of μ=1, can extrapolate the ferritic Curie temperature of NiCuZn is about 105 DEG C.
Fig. 4 is the complex permeability magnetic spectrum of NiCuZn flexibility ferrite sheet provided in this embodiment, it can be seen that test When frequency f=300kHz, it " is 11.39 that μ ', which is 809.27, μ,；In addition, by the magnetic spectrum can be seen that when frequency f=100~ Within the scope of 300kHz, the complex permeability real part μ ' of NiCuZn flexibility ferrite sheet is 650~850 and imaginary part μ "≤20.
Embodiment 10
Referring to embodiment 1, difference is the specific preparation method of the present embodiment, and in step (1), gained ingredient is being sanded It is ground in machine, the milling time of sand mill is 1.5h, and the mass ratio of revolving speed 100r/min, raw material, water and zirconium ball are 1:1:5, zirconium ball sphere diameter areWherein, polyvinyl alcohol (PVA) aqueous solution of the 7wt% of raw material gross mass, poly- second is added The concentration of enol (PVA) aqueous solution is 10wt%, is mixed together ball milling.Obtained slurry is poured into stirring pool, using pressure The spraying method of power implements granulating and drying, inlet temperature are as follows: and 350~380 DEG C, outlet temperature are as follows: 95~100 DEG C.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 3.
Embodiment 11
Referring to embodiment 1, difference is the specific preparation method of the present embodiment, and in step (1), gained ingredient is being sanded It is ground in machine, the milling time of sand mill is 2h, revolving speed 50r/min, and the mass ratio of raw material, water and zirconium ball is 1:1: 5, zirconium ball sphere diameter isWherein, polyvinyl alcohol (PVA) aqueous solution of the 8wt% of raw material gross mass, polyvinyl alcohol is added (PVA) concentration of aqueous solution is 10wt%, is mixed together ball milling.Obtained slurry is poured into stirring pool, is sprayed using pressure The method of mist implements granulating and drying, inlet temperature are as follows: and 380~400 DEG C, outlet temperature are as follows: 110~115 DEG C.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of the present embodiment step (5) obtain It is shown in Table 3.
Comparative example 1
Step (1), (2), (3) and (4) is same as Example 1.Wherein, in step (1), by constituent Fe2O3For 48.6mol%, ZnO 34.20mol%, NiO 8.0mol%, CuO are that the formula of 9.20mol% weighs raw material；Wherein, The purity requirement of raw material are as follows: Fe2O3It is for 99.46wt%, ZnO 98.15wt%, NiO 99.38wt%, CuO 98.26wt%.In step (3), secondary ball milling slurry granularity is D50:1.31 μm.
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 970 DEG C, keep the temperature 3h after cooling be sintered Magnet ring afterwards.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 970 DEG C Ferrite sintered body piece is obtained after sintering, then is bonded PET one side glue and PSA double-sided adhesive respectively in ferrite sintered body piece upper and lower surfaces Sliver processing is carried out afterwards, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of this comparative example step (5) obtain It is shown in Table 1.
Comparative example 2
Step (1), (2), (3) and (4) is same as Example 1.Wherein, in step (1), by constituent Fe2O3For 49.3mol%, ZnO 32.5mol%, NiO 10.2mol%, CuO are that the formula of 8.0mol% weighs raw material；Wherein, former The purity requirement of material are as follows: Fe2O3It is for 99.46wt%, ZnO 98.15wt%, NiO 99.38wt%, CuO 98.26wt%.In step (3), secondary ball milling slurry granularity is D50:1.24 μm.
(5) by step (4) obtained by molding to magnet ring green compact be sintered at 973 DEG C, keep the temperature 2h after cooling be sintered Magnet ring afterwards.
It (6) is laminar green compact by tape casting by powder slurry obtained in step (3), slurry, green compact are through 973 DEG C Ferrite sintered body piece is obtained after sintering, then is bonded PET one side glue and PSA double-sided adhesive respectively in ferrite sintered body piece upper and lower surfaces Sliver processing is carried out afterwards, ferrite sheet powder is broken into several small pieces, and flexible ferrite sheet is just made.
The performance test results for the flexible ferrite sheet that the obtained magnet ring and step (6) of this comparative example step (5) obtain It is shown in Table 1.
Performance test methods
Magnet ring and flexible ferrite sheet to various embodiments of the present invention and comparative example are tested for the property, specifically: it adopts With the real part of Agilent E4990A impedance analyzer test magnet ring or the ferrite sheet complex permeability when frequency is 300kHz μ ' and imaginary part μ "；Using rock rugged communication SY-8218 type B-H tester test magnet ring or ferrite sheet 100kHz, 1194A/m, Saturation induction density Bs and coercivity H and 100kHz, 200mT when 25 DEG C of conditions, the power loss under the conditions of 25 DEG C Pcv, using the curve of electric inductance measuring-testing instrument test magnetic permeability μ and temperature T variation, calculate Curie temperature Tc.Specific test result list It is as follows:
Table 1
Table 2
Table 3
Based on the above embodiments with comparative example it is found that NiZnCu Ferrite Material provided by the invention is using reasonable formula And suitable preparation method, obtained higher magnetic conductivity real part and lower magnetic conductivity imaginary part, saturation induction density is high, It is functional, it is suitable for wireless charging field, comparative example do not use the solution of the present invention, thus can not obtain of the invention excellent Good effect.
The Applicant declares that the present invention is explained by the above embodiments method detailed of the invention, but the present invention not office Be limited to above-mentioned method detailed, that is, do not mean that the invention must rely on the above detailed methods to 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, selection of concrete mode etc., all of which fall within the scope of protection and disclosure of the present invention.

Claims (10)

1. a kind of NiCuZn Ferrite Material, which is characterized in that the NiCuZn Ferrite Material is mainly by Fe2O3、ZnO、NiO It is formed with CuO, is Fe in terms of 100% by the integral molar quantity of the NiCuZn Ferrite Material2O3Mole percent be 49~ The mole percent of 50mol%, ZnO are 32~34mol%, and the mole percent of NiO is 8.1~10mol%, mole of CuO Percentage is 8~10.9mol%.
2. NiCuZn Ferrite Material according to claim 1, which is characterized in that in the NiCuZn Ferrite Material also Including MoO3, with Fe2O3, ZnO, NiO and CuO gross mass be 100% meter, the MoO3Mass percent in terms of reference substance For 0.01~0.1wt%；
It preferably, further include Bi in the NiCuZn Ferrite Material2O3, with Fe2O3, ZnO, NiO and CuO gross mass be 100% meter, the Bi2O3Mass percent in terms of reference substance is 0~0.1wt%；
Preferably, the NiCuZn Ferrite Material is flaky material.
3. a kind of preparation method of NiCuZn Ferrite Material as claimed in claim 1 or 2, which is characterized in that the method Including lower step:
(1) to the Fe of formula ratio2O3Raw material, ZnO raw material, NiO raw material and CuO raw material carry out wet-mixing and are crushed, and then dry It is dry, obtain powder；
(2) to pre-burning is carried out after the heating of step (1) powder, preburning powdered material is obtained；
(3) step (2) described preburning powdered material is crushed, is then dried, obtain drying powder；
(4) green compact are made in step (3) the drying powder；
(5) step (4) described green compact are sintered, obtain the NiCuZn Ferrite Material.
4. preparation method according to claim 3, which is characterized in that step (1) described Fe2O3Fe in raw material2O3Quality Score >=99.4wt%；
Preferably, in step (1) the ZnO raw material ZnO mass fraction >=98.0wt%；
Preferably, in step (1) the NiO raw material NiO mass fraction >=99.0wt%；
Preferably, in step (1) the CuO raw material CuO mass fraction >=98.0wt%；
Preferably, step (1) wet-mixing and broken method are ball milling；
Preferably, in the mechanical milling process, the mass ratio of raw material to be broken, water and zirconium ball is 1:1:5；
Preferably, the ball milling carries out in planetary ball mill, horizontal ball mill or sand mill, preferably in sand mill into Row；
Preferably, when the ball milling carries out in a planetary ball mill, Ball-milling Time be 1~2h, rotational speed of ball-mill be 250~ 300r/min；
Preferably, when the ball milling carries out in horizontal ball mill, Ball-milling Time is 2~6h, and rotational speed of ball-mill is 40~80r/ min；
Preferably, when the ball milling carries out in sand mill, Ball-milling Time is 1~2h, and rotational speed of ball-mill is 50~100r/min；
Preferably, step (1) drying carries out in baking oven or spray-drying installation；
Preferably, when step (1) drying carries out in an oven, drying temperature is 100~120 DEG C；
Preferably, when step (1) drying carries out in spray-drying installation, the inlet temperature of the spray-drying installation It is 350~400 DEG C, outlet temperature is 95~115 DEG C；
Preferably, when step (1) drying carries out in spray-drying installation, wet-mixing and it is broken during plus Enter polyvinyl alcohol water solution, the concentration of the polyvinyl alcohol water solution is 10%, and the additional amount of the polyvinyl alcohol water solution is Fe2O36~8wt% of the gross mass of raw material, ZnO raw material, NiO raw material and CuO raw material.
5. preparation method according to claim 3 or 4, which is characterized in that in step (2), first by step (1) powder Pre-burning is carried out again after being placed in aluminium oxide saggar and/or zirconium oxide saggar；
Preferably, the heating rate of step (2) described heating is 2~4 DEG C/min；
Preferably, the temperature of step (2) described pre-burning is 860~940 DEG C；
Preferably, the time of step (2) described pre-burning is 2~3h；
Preferably, step (2) described pre-burning carries out in pushed bat kiln, roller kilns or rotary kiln；
Preferably, when step (2) described pre-burning carries out in rotary kiln, kiln bore is 1~1.8m, and the length of high-temperature region is 5~10m, high-temperature region set temperature are 860~940 DEG C, and the rotation speed of rotary kiln is 5~20r/min, and rotary kiln inlet amount is 80~200kg/ hours.
6. according to the described in any item preparation methods of claim 3-5, which is characterized in that in step (3), further includes: broken The preceding MoO that formula ratio is added3And/or Bi2O3；
Preferably, step (3) the broken method is ball milling；
Preferably, the ball milling carries out in the ball mill；
Preferably, the time of the ball milling is 1~2h, and the revolving speed of ball milling is 250~300r/min；
Preferably, in the mechanical milling process, the mass ratio of material to be broken, water and zirconium ball is 1:1.25:5；
Preferably, the temperature of step (3) described drying is 100~200 DEG C；
Preferably, step (3) drying carries out in an oven.
7. according to the described in any item preparation methods of claim 3-6, which is characterized in that in step (4), the green compact that are made Method includes: sieving granulation and compression moulding after mixing step (3) the drying powder with binder, obtains green compact；
Preferably, the binder includes polyvinyl alcohol water solution, and the concentration of polyvinyl alcohol water solution is 10wt%；
Preferably, the additional amount of the binder is 6~8wt% of the gross mass of step (3) described drying powder and binder；
Preferably, the pressure of the compression moulding is 5~8MPa；
Preferably, the compression moulding suppresses green compact circlewise；
Preferably, in step (4), the method that green compact are made includes: to carry out slurry to step (3) the drying powder, right Obtained slurry carries out tape casting, obtains green compact, and the green compact are sheet.
8. according to the described in any item preparation methods of claim 3-7, which is characterized in that the temperature of step (5) described sintering is 940~1000 DEG C；
Preferably, the time of step (5) described sintering is 2~3h；
Preferably, step (5) further include: when step (4) green compact are sheet, in the obtained NiCuZn ferrite material The two sides of material carries out sliver processing after being bonded polyethylene terephthalate one side glue and acrylate pressure sensitive adhesive double-sided adhesive respectively, Obtain flexible NiCuZn ferrite sheet material.
9. according to the described in any item preparation methods of claim 3-8, which is characterized in that the described method comprises the following steps:
(1) to the Fe of formula ratio2O3Raw material, ZnO raw material, NiO raw material and CuO raw material carry out ball milling, Ball-milling Time in the ball mill For 1~2h, rotational speed of ball-mill is 250~300r/min, and in mechanical milling process, the mass ratio of raw material to be broken, water and zirconium ball is 1:1: 5,100~120 DEG C are then dried in an oven, obtain powder；
(2) step (1) described powder is placed in aluminium oxide saggar and/or zirconium oxide saggar, with the heating speed of 2~4 DEG C/min Rate carries out pre-burning after being warming up to 860~940 DEG C, the time of pre-burning is 2~3h, obtains preburning powdered material；
(3) MoO of formula ratio is added into step (2) described preburning powdered material3And/or Bi2O3Afterwards, ball milling is carried out in the ball mill, The time of ball milling is 1~2h, and the revolving speed of ball milling is 250~300r/min, in mechanical milling process, material to be broken, water and zirconium ball Mass ratio is 1:1.25:5, then 100~200 DEG C of drying in an oven, obtains drying powder；
(4) slurry is carried out to step (3) the drying powder, tape casting is carried out to obtained slurry, obtains green compact, the life Base is sheet；
(5) step (4) described green compact are sintered at 940~1000 DEG C, the time of sintering is 2~3h, is being obtained after sintering To be bonded polyethylene terephthalate one side glue and acrylate pressure sensitive adhesive respectively double the two sides of NiCuZn Ferrite Material Sliver processing is carried out after the glue of face, obtains flexible NiCuZn ferrite sheet material.
10. a kind of purposes of NiCuZn Ferrite Material as claimed in claim 1 or 2, which is characterized in that the NiCuZn iron Ferrite is used for wireless charging field.
CN201811256074.6A 2018-06-22 2018-10-26 A kind of NiCuZn Ferrite Material and its preparation method and application Pending CN109336578A (en)

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CN112759380B (en) * 2020-12-31 2022-05-31 横店集团东磁股份有限公司 Microwave ferrite material and preparation method and application thereof
CN113816734A (en) * 2021-10-08 2021-12-21 横店集团东磁股份有限公司 NiCuZn ferrite material and preparation method and application thereof
CN113816734B (en) * 2021-10-08 2023-02-17 横店集团东磁股份有限公司 NiCuZn ferrite material and preparation method and application thereof

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