CN103382106A - High-conductive and high-loss NiCuZn ferrite material, magnetic sheets and preparation method thereof - Google Patents

High-conductive and high-loss NiCuZn ferrite material, magnetic sheets and preparation method thereof Download PDF

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CN103382106A
CN103382106A CN2013102650029A CN201310265002A CN103382106A CN 103382106 A CN103382106 A CN 103382106A CN 2013102650029 A CN2013102650029 A CN 2013102650029A CN 201310265002 A CN201310265002 A CN 201310265002A CN 103382106 A CN103382106 A CN 103382106A
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magnetic sheet
ball milling
ferrite
nicuzn
damage
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梁迪飞
杨宏伟
张先智
张楠
陈良
谢建良
邓龙江
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University of Electronic Science and Technology of China
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Abstract

A high-conductive and high-loss NiCuZn ferrite material, magnetic sheets and a preparation method thereof relate to the electronic material technology. The ferrite material comprises main components and a mixed component, and is characterized in that the main components and the mixed component are all calculated in the oxide form. The main components comprise following components in mole percentage: 50 mol% to 52 mol% of Fe2O3, 18 mol% to 29 mol% of ZnO, 18 mol% to 28 mol% of Ni and 2.5 mol% to 6 mol% of CuO. The mixed component is the following component in weight percentage: 0 to 0.6 wt% of Co2O3. The preparation method prepares high-conductive and high-loss NiCuZn ferrite material, ferrite sheets through an oxide sintering technology, which is simple in process, non-polluted and suitable for mass production.

Description

Height is led the high NiCuZn of damage Ferrite Material, magnetic sheet and preparation method
Technical field
The present invention relates to electronic material technology.
Background technology
Along with the development of the technology such as information, communication, test, under the finite space and frequency resource condition, the seriousness of electromagnetic interference (EMI) more and more receives people's concern.The ability of the electromagnetic disturbance that electromagnetic compatibility (EMC) refers to equipment or system can work in its electromagnetic environment and can not bear anything formation in this environment.As far back as the thirties in 20th century, some developed countries just begin one's study EMC designing technique, material technology etc., and form a series of standard and be applied, i.e. EMC standard.China will just announce to carry out the EMC standard in the end of the year 1998, lag behind developed country aspect material technology and product.The all parts of the world district substantially all is provided with the corresponding market access authentication of EMC at present; in order to the competitive edge of the electromagnetic environment of protecting this area and this native produce, be all " pass " that enters these markets as FCC, the NEBC authentication of North America, the CE authentication of European Union, the VCCEI authentication of Japan, the BSMI authentication of Taiwan, the 3C authentication of China etc.In developed country, the equipment that can not satisfy EMC Standard does not allow to sell.
The expert generally believes both at home and abroad, the NiCuZn ferrite has high resistivity, higher Curie temperature and good high-gradient magnetism energy, therefore the NiCuZn ferrite can be used for the surface mount device of anti-electromagnetic interference and power and anti-interference integral etc., in order to solve the problem of electromagnetic interference.
If the NiCuZn ferrite is used for anti-electromagnetic interference, its complex impedance can be expressed as: Z=j ω L 0(μ '-j μ ")=ω L 0μ "+j ω L 0μ ', in formula, angular frequency=2 π f, the magnetic permeability real part of μ ' expression magneticsubstance, μ " the magnetic permeability imaginary part of expression magneticsubstance, and impedance Z is larger, the effect of anti-EMI is better.So when the NiCuZn Ferrite Material is used for solving electromagnetic compatibility problem, its μ ' and μ " higher, namely have high magnetic permeability, high loss, the restraining effect to noise is just stronger so, thereby reaches the purpose of anti-electromagnetic interference.
Summary of the invention
Technical problem to be solved by this invention is, provides that a kind of magnetic permeability real part is high, also high Ferrite Material of imaginary part, and the ferrite magnetic sheet and the preparation method that are prepared into of Ferrite Material thus.
The technical scheme that the present invention solve the technical problem employing is, height is led the high NiCuZn of damage Ferrite Material, comprises principal constituent and doping composition, it is characterized in that, principal constituent formula and doping composition are all by oxide compound; Calculate with molar percentage, the principal constituent formula is:
Figure BDA00003423161100021
Calculate by percentage to the quality, be doping to and be divided into:
Co 2O 3 0～0.6wt%。
Further, the principal constituent formula is:
Figure BDA00003423161100022
Figure BDA00003423161100031
Be doping to and be divided into: Co 2O 30～0.4wt%.
The present invention also provides by aforementioned height and leads the magnetic sheet that the high NiCuZn of damage Ferrite Material is made.
The present invention also provides height to lead the preparation method of the high NiCuZn of damage ferrite magnetic sheet, comprises the following steps:
1) ball milling: the material composition of principal constituent is put into ball mill after by the preset blending ratio weighing carry out ball milling one time;
2) pre-burning: with a good material oven dry of ball milling, put it into afterwards pre-burning between 850 ℃～1050 ℃ in High Temperature Furnaces Heating Apparatus, soaking time 1～3h, atmosphere is air;
3) secondary ball milling: the Co that mixes 0～0.6wt% in pre-burned material 2O 3, put into ball mill and carry out secondary ball milling;
4) moulding of ferrite magnetic sheet: the material after secondary ball milling and macromolecule resin are mixed, then it is rolled film or curtain coating on request, reducing at last is required size;
5) magnetic sheet sintering: the magnetic sheet of moulding is stacked 3～6 layers, sintering between 1000 ℃～1150 ℃, soaking time 2～6h, atmosphere is air.
6) magnetic sheet is peeled off and pad pasting: the magnetic sheet after sintering is peeled away, and note is enclosed glue-line and PET film on every magnetic sheet.
Mean particle size after the step 3) secondary ball milling is between 0.9 μ m～1.4 μ m.
The invention has the beneficial effects as follows, the present invention's and oxidesintering technique that be suitable for produce simple, pollution-free by technique has prepared Ferrite Material, the ferrite magnetic sheet with high magnetic permeability, high loss, wherein one group is 317, μ at the 10MHz μ ' of place " be 32; Be 318, μ 13.56MHz locate μ ' " be 113; The μ ' of 100MHz place is 42, μ " is 88.And the characteristics such as this magnetic sheet has, and size is adjustable, smooth surface is smooth, can be suitably crooked.
Description of drawings
Fig. 1 is ferrite magnetic sheet viscose glue and pad pasting schematic diagram.
Fig. 2 is embodiment 1 Ferrite Material magnetic spectrum graphic representation.
Fig. 3 is embodiment 2 Ferrite Material magnetic spectrum graphic representations.
Fig. 4 is embodiment 3 Ferrite Material magnetic spectrum graphic representations.
Embodiment
Height is led the high Ferrite Material that damages, and comprises main formula composition and doping composition, it is characterized in that, main formula composition and doping composition are all by oxide compound; Wherein, calculate with molar percentage, the main formula composition is:
Figure BDA00003423161100041
That is, calculate with molar percentage, all main formula composition sum is 100%.
Calculate by percentage to the quality, be doping to and be divided into:
Co 2O 3 0～0.6wt%。
That is, calculate by percentage to the quality, if the main formula composition is 100 mass units, is doping to and is divided into 0～0.6 mass unit.
Further, each component is:
Figure BDA00003423161100042
Figure BDA00003423161100051
The present invention also provides and has adopted aforementioned height to lead the high ferrite magnetic sheet that damages the Ferrite Material preparation, and its size is adjustable, suitably crooked, thickness is 0.08mm～0.3mm.
The preparation method of ferrite magnetic sheet of the present invention comprises the steps:
1) ball milling: each material composition is put into ball mill after by the preset blending ratio weighing carry out ball milling one time;
2) pre-burning: with a good material oven dry of ball milling, put it into afterwards pre-burning between 850 ℃～1050 ℃ in High Temperature Furnaces Heating Apparatus, soaking time 1～3h, atmosphere is air;
3) secondary ball milling: the Co that mixes 0～0.6wt% in the pre-burned material 2O 3, put into ball mill and carry out secondary ball milling;
4) moulding of ferrite magnetic sheet: the material after secondary ball milling and macromolecule resin are mixed, then it is rolled film or curtain coating on request, reducing at last is required size;
5) magnetic sheet sintering: the magnetic sheet of moulding is stacked 3～5 layers, sintering between 1000 ℃～1150 ℃, soaking time 2～6h, atmosphere is air.
6) magnetic sheet is peeled off and pad pasting: the magnetic sheet after sintering is peeled away, and note is enclosed glue-line and PET film on every magnetic sheet.
Further, above-mentioned steps 5) sintering rule is: between 25 ℃～450 ℃, heat-up rate is 1 ℃/min, between 450 ℃～800 ℃, heat-up rate is 1.5 ℃/min, 800 ℃ to heat-up rate between sintering temperature be 1 ℃/min, soaking time 2～6h, atmosphere is air, and temperature-fall period is naturally cooling in stove.
Below by embodiment, technical scheme of the present invention is further described in detail.
Height provided by the invention is led the Fe that the high starting material that damage Ferrite Material are selected 2O 3Purity more than or equal to 99.4%, the purity of ZnO more than or equal to 98%, the purity of NiO more than or equal to 99.4%, the purity of CuO more than or equal to 98.4%, Co 2O 3Middle Co is more than or equal to 72%.
Embodiment 1:
1) Composition Design: Fe 2O 3Be 50mol%, ZnO is 21.5mol%, and NiO is 24.5mol%, and CuO is 4mol%.
2) ball milling: the raw material that weighs up is put into ball mill, add tap water and ball, wherein the mass ratio of material, water, ball is 1:1:3.The setting rotating speed is 250r/min, and the time is 2h.
3) pre-burning: the material oven dry that mix grinding is good, put into the sintering oven pre-burning, calcined temperature is 900 ℃, insulation 2h, atmosphere is air, naturally cooling in stove after pre-burning.
4) secondary ball milling: the material that pre-burning finishes is smashed to pieces, put into ball mill, add tap water and ball, wherein the mass ratio of material, water, ball is 1:1:3.The setting rotating speed is 250r/min, and the time is 3h.
5) moulding of ferrite magnetic sheet: with the oven dry of the material after secondary ball milling, add macromolecule resin to mix, the material that then will mix carries out the film that rolls of different thickness as requested, and wherein the thickness of film is adjustable between 0.08mm～0.3mm.
6) sintering: the magnetic sheet of moulding is stacked 3～5 layers, put into sintering oven, heat-up rate is 1 ℃/min between 25 ℃～450 ℃, between 450 ℃～800 ℃, heat-up rate is 1.5 ℃/min, between 800 ℃～1100 ℃, heat-up rate is 1 ℃/min, at 1100 ℃ of insulation 3h, atmosphere is air, naturally cooling in stove after sintering.
7) magnetic sheet is peeled off and pad pasting: the magnetic sheet after sintering is peeled away, and note is enclosed double faced adhesive tape and PET film on every magnetic sheet, wherein double faced adhesive tape thickness is between 0.02mm～0.03mm, and the PET film thickness is between 0.03mm～0.05mm.
Embodiment 2:
1) Composition Design: Fe 2O 3Be 50mol%, ZnO is 24.5mol%, and NiO is 21.5mol%, and CuO is 4mol%.
2) ball milling: the raw material that weighs up is put into ball mill, add tap water and ball, wherein the mass ratio of material, water, ball is 1:1:3.The setting rotating speed is 250r/min, and the time is 2h.
3) pre-burning: the material oven dry that mix grinding is good, put into the sintering oven pre-burning, calcined temperature is 900 ℃, insulation 2h, atmosphere is air, naturally cooling in stove after pre-burning.
4) secondary ball milling: the material that pre-burning finishes is smashed to pieces, put into ball mill, add tap water and ball, wherein the mass ratio of material, water, ball is 1:1:3.The setting rotating speed is 250r/min, and the time is 3h.
5) moulding of ferrite magnetic sheet: with the oven dry of the material after secondary ball milling, add macromolecule resin to mix, the material that then will mix carries out the film that rolls of different thickness as requested, and wherein the thickness of film is adjustable between 0.08mm～0.3mm.
6) sintering: the magnetic sheet of moulding is stacked 3～5 layers, put into sintering oven, heat-up rate is 1 ℃/min between 25 ℃～450 ℃, between 450 ℃～800 ℃, heat-up rate is 1.5 ℃/min, between 800 ℃～1100 ℃, heat-up rate is 1 ℃/min, at 1100 ℃ of insulation 3h, atmosphere is air, naturally cooling in stove after sintering.
7) magnetic sheet is peeled off and pad pasting: the magnetic sheet after sintering is peeled away, and note is enclosed double faced adhesive tape and PET film on every magnetic sheet, wherein double faced adhesive tape thickness is between 0.02mm～0.03mm, and the PET film thickness is between 0.03mm～0.05mm.
Embodiment 3:
1) Composition Design: Fe 2O 3Be 50mol%, ZnO is 24.5mol%, and NiO is 21.5mol%, and CuO is 4mol%, doping composition Co 2O 3Be 0.3wt%.
2) ball milling: the raw material that weighs up is put into ball mill, add tap water and ball, wherein the mass ratio of material, water, ball is 1:1:3.The setting rotating speed is 250r/min, and the time is 2h.
3) pre-burning: the material oven dry that mix grinding is good, put into the sintering oven pre-burning, calcined temperature is 900 ℃, insulation 2h, atmosphere is air, naturally cooling in stove after pre-burning.
4) secondary ball milling: the material that pre-burning finishes is smashed to pieces, put into ball mill, and mix therein the Co of 0.3wt% 2O 3, add tap water and ball, wherein the mass ratio of material, water, ball is 1:1:3.The setting rotating speed is 250r/min, and the time is 3h.
5) moulding of ferrite magnetic sheet: with the oven dry of the material after secondary ball milling, add macromolecule resin to mix, the material that then will mix carries out the film that rolls of different thickness as requested, and wherein the thickness of film is adjustable between 0.08mm～0.3mm.
6) sintering: the magnetic sheet of moulding is stacked 3～5 layers, put into sintering oven, heat-up rate is 1 ℃/min between 25 ℃～450 ℃, between 450 ℃～800 ℃, heat-up rate is 1.5 ℃/min, between 800 ℃～1100 ℃, heat-up rate is 1 ℃/min, at 1100 ℃ of insulation 3h, atmosphere is air, naturally cooling in stove after sintering.
7) magnetic sheet is peeled off and pad pasting: the magnetic sheet after sintering is peeled away, and note is enclosed double faced adhesive tape and PET film on every magnetic sheet, wherein double faced adhesive tape thickness is between 0.02mm～0.03mm, and the PET film thickness is between 0.03mm～0.05mm.
The sample ring of the same material for preparing by above-described embodiment is tested on E4991A low-frequency impedance analyser, can find, the present invention is by principal constituent formula and doping Co 2O 3Adjusting, can the Effective Regulation material by frequency f r, and make the Ferrite Material of high magnetic permeability, high loss, and the ferrite magnetic sheet thickness and the size that make are adjustable, and smooth surface is smooth.

Claims (6)

1. height is led the high NiCuZn of damage Ferrite Material, comprises principal constituent and doping composition, it is characterized in that, principal constituent formula and doping composition are all by oxide compound; Calculate with molar percentage, the principal constituent formula is:
Figure FDA00003423161000011
Calculate by percentage to the quality, be doping to and be divided into:
Co 2O 3 0～0.6wt%。
2. height as claimed in claim 1 is led the high NiCuZn of damage Ferrite Material, it is characterized in that, the principal constituent formula is:
Figure FDA00003423161000012
3. height as claimed in claim 2 is led the high NiCuZn of damage Ferrite Material, it is characterized in that, is doping to be divided into: Co 2O 30～0.4wt%.
4. lead by height claimed in claim 1 the magnetic sheet that the high NiCuZn of damage Ferrite Material is made.
5. the high preparation method who leads the high NiCuZn of damage ferrite magnetic sheet, is characterized in that, comprises the following steps:
1) ball milling: the material composition of principal constituent is put into ball mill after by the preset blending ratio weighing carry out ball milling one time;
2) pre-burning: with a good material oven dry of ball milling, put it into afterwards pre-burning between 850 ℃～1050 ℃ in High Temperature Furnaces Heating Apparatus, soaking time 1～3h, atmosphere is air;
3) secondary ball milling: the Co that mixes 0～0.6wt% in pre-burned material 2O 3, put into ball mill and carry out secondary ball milling;
4) moulding of ferrite magnetic sheet: the material after secondary ball milling and macromolecule resin are mixed, then it is rolled film or curtain coating on request, reducing at last is required size;
5) magnetic sheet sintering: the magnetic sheet of moulding is stacked 3～6 layers, sintering between 1000 ℃～1150 ℃, soaking time 2～6h, atmosphere is air.
6) magnetic sheet is peeled off and pad pasting: the magnetic sheet after sintering is peeled away, and note is enclosed glue-line and PET film on every magnetic sheet.
6. height as claimed in claim 5 is led the preparation method of the high NiCuZn of damage ferrite magnetic sheet, it is characterized in that, the mean particle size after the step 3) secondary ball milling is between 0.9 μ m～1.4 μ m.
CN2013102650029A 2013-06-27 2013-06-27 High-conductive and high-loss NiCuZn ferrite material, magnetic sheets and preparation method thereof Pending CN103382106A (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN103693949A (en) * 2013-11-19 2014-04-02 横店集团东磁股份有限公司 Soft magnetic NiCuZn ferrite material with characteristics of wide temperature range, low temperature coefficient, high frequency and low loss, and preparation method thereof
CN105161279A (en) * 2015-09-17 2015-12-16 无锡斯贝尔磁性材料有限公司 Production process of wireless-charging magnetic sheet
CN105669179A (en) * 2015-12-30 2016-06-15 安泰科技股份有限公司 Ultrathin magnetic shielding sheet material and preparation method thereof
CN106830912A (en) * 2017-01-17 2017-06-13 杭州安费诺飞凤通信部品有限公司 A kind of Ni-Zn soft magnetic ferrite magnetic sheet and preparation method thereof
CN107230541A (en) * 2017-06-08 2017-10-03 东莞信柏结构陶瓷股份有限公司 Magnetic material and preparation method thereof
CN108774056A (en) * 2018-06-14 2018-11-09 横店集团东磁股份有限公司 A kind of NiZn ferrites magnetic sheet and its preparation method and application
CN108773858A (en) * 2018-07-10 2018-11-09 电子科技大学 A kind of pattern-band Surface Wave Absorbing Material and preparation method thereof
CN109574646A (en) * 2018-12-17 2019-04-05 苏州世诺新材料科技有限公司 A kind of ferrite sheet and preparation method thereof suitable for 6.78MHz

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CN102701720A (en) * 2012-05-15 2012-10-03 电子科技大学 High conductivity and low loss ferrite material, ferrite thin film and preparation method thereof
CN102800456A (en) * 2011-05-23 2012-11-28 Tdk株式会社 Ferrite core and electric parts
CN102956338A (en) * 2012-11-20 2013-03-06 无锡常安通用金属制品有限公司 Metal material for magnetic core and preparation method thereof

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CN101552074A (en) * 2009-01-04 2009-10-07 贵阳晶华电子材料有限公司 A NiZnCu ferrite material and preparing method thereof
CN102800456A (en) * 2011-05-23 2012-11-28 Tdk株式会社 Ferrite core and electric parts
CN102701720A (en) * 2012-05-15 2012-10-03 电子科技大学 High conductivity and low loss ferrite material, ferrite thin film and preparation method thereof
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103693949A (en) * 2013-11-19 2014-04-02 横店集团东磁股份有限公司 Soft magnetic NiCuZn ferrite material with characteristics of wide temperature range, low temperature coefficient, high frequency and low loss, and preparation method thereof
CN105161279A (en) * 2015-09-17 2015-12-16 无锡斯贝尔磁性材料有限公司 Production process of wireless-charging magnetic sheet
CN105669179A (en) * 2015-12-30 2016-06-15 安泰科技股份有限公司 Ultrathin magnetic shielding sheet material and preparation method thereof
CN105669179B (en) * 2015-12-30 2018-08-17 安泰科技股份有限公司 Ultra-thin magnetic screen sheet material and preparation method thereof
CN106830912A (en) * 2017-01-17 2017-06-13 杭州安费诺飞凤通信部品有限公司 A kind of Ni-Zn soft magnetic ferrite magnetic sheet and preparation method thereof
CN107230541A (en) * 2017-06-08 2017-10-03 东莞信柏结构陶瓷股份有限公司 Magnetic material and preparation method thereof
CN108774056A (en) * 2018-06-14 2018-11-09 横店集团东磁股份有限公司 A kind of NiZn ferrites magnetic sheet and its preparation method and application
CN108774056B (en) * 2018-06-14 2021-04-20 横店集团东磁股份有限公司 NiZn ferrite magnetic sheet and preparation method and application thereof
CN108773858A (en) * 2018-07-10 2018-11-09 电子科技大学 A kind of pattern-band Surface Wave Absorbing Material and preparation method thereof
CN109574646A (en) * 2018-12-17 2019-04-05 苏州世诺新材料科技有限公司 A kind of ferrite sheet and preparation method thereof suitable for 6.78MHz
CN109574646B (en) * 2018-12-17 2020-10-23 苏州世诺新材料科技有限公司 Ferrite sheet suitable for 6.78MHz and preparation method thereof

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Application publication date: 20131106