CN105669179A - Ultrathin magnetic shielding sheet material and preparation method thereof - Google Patents

Ultrathin magnetic shielding sheet material and preparation method thereof Download PDF

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Publication number
CN105669179A
CN105669179A CN201511021314.0A CN201511021314A CN105669179A CN 105669179 A CN105669179 A CN 105669179A CN 201511021314 A CN201511021314 A CN 201511021314A CN 105669179 A CN105669179 A CN 105669179A
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ferrite
magnetic shielding
shielding sheet
preparation
sheet material
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CN105669179B (en
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周少雄
董帮少
张广强
阎有花
李宗臻
谢琰军
戚雯
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Advanced Technology and Materials Co Ltd
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Advanced Technology and Materials Co Ltd
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    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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Abstract

The invention provides an ultrathin magnetic shielding sheet material and a preparation method thereof. The ultrathin magnetic shielding sheet material is prepared from a ferrite, an adhesive, an additive and a surfactant and is 0.001-0.08 mm in thickness. The preparation method particularly includes: material preparation and blending, primary ball milling, pressing to form blocks, pre-sintering, secondary ball milling, paste preparation, spray coating and secondary sintering. The complex permeability of the ultrathin magnetic shielding sheet material is [mu]'=70-200, [mu]'' <= 3 under 13.56 MHz. The preparation method is simple and reliable, is high in yield, is energy-saving and environment-friendly and allows the thickness of the material to be freely controlled according to performance demand. The ultrathin magnetic shielding sheet material has excellent magnetic shielding performance, satisfies the development demands of lightening and thinning, functionalization and energy saving and environment protection, and can satisfies of further processing design demand on touch screens, electronic printing and the like.

Description

Ultra-thin magnetic shielding sheet material and its preparation method
Technical field
The present invention relates to a kind of ultra-thin magnetic shielding sheet material and its preparation method, belong to the technical field of Electromagnetic heating material.
Background technology
Along with the development of modern science and technology, thing is networked, cloud computing, mobile Internet, big data etc. are the fast development of the generation information Technology and equipment of mark, with wireless radio frequency discrimination RFID (RadioFrequencyIdentification, RF identification), wireless payment NFC (NearFieldCommunication, near-field communication), wireless charging technology etc. are the electronic product and technology that support, it is attractive in appearance, novelty, portability is more and more accepted by the public and promotes, further promote electronic product device lightening, high-effect direction is developed, particularly magnetic shielding sheet material faces the urgent market requirement.
Magnetic shielding sheet, has another name called antifreeze plate, is widely used in wireless charging, NFC and technical field of RFID, can be made into the antifreeze plate in the magnetic conduction sheet in wireless charger, NFC and RFID device. Electronics eddy current, in wireless charger, by high magnetic flux, to offer loop, charger sympathetic magnetic field, it is to increase efficiency, is isolated simultaneously, is prevented electronics eddy current from affecting circuit mainboard, make charger energy normal operation by magnetic conduction sheet. Antifreeze plate in NFC and RFID device can absorb metal reflection attenuation ripple, can strengthen again magnetic field induction distance, it is to increase communication sensitivity.
Existing antifreeze plate material mostly is ferrite, and its gauge is 0.08mm-0.5mm, and these ferrite sheets often adopt the caking agents such as ferrite powder and resin to mix and are pressed into sheet material, then is become by the method sintering of extrusion moulding, compression moulding or flow casting molding. Such as China Patent Publication No. is patent or the patent application of CN203521092U, CN202425285U, CN102976726A, CN101213896A, CN103377787A, CN104766686A, CN104496451A, CN104387090A.
Preparation technology aspect, extruding-out process adopts slurry particle content low, and after magnetic sheet sintering, density is relatively low, and magnetic property is poor;And compression moulding technique, the thin magnetic plate of below thickness 0.1mm cannot be prepared. Casting molding processes is the most frequently used technique of current NFC magnetic sheet, and its casting slurry forms primarily of ferrite powder and organic system, then prepares the raw sheet of ferrite of thickness 0.1mm with slurry, just obtains ferrite magnetic sheet after sintering.
But casting technique prepares the shortcoming that antifreeze plate material also exists many aspects. One is that the ferrite magnetic sheet thickness adopting casting technique to prepare is limited, and the thickness limit that can obtain at present is 0.08mm, and in technique gauge control, harsh for equipment Requirement, product yield rate is restricted. Two is that ferrite deposition layering easily occurs water soluble adhesive, and existing casting molding processes is produced, and adopts polyvinyl butyral acetal (PVB) to make caking agent more, and alcohol and dimethylbenzene make organic solvent. And dimethylbenzene is as the organic solvent that toluene type organic is that toxicity is stronger, a large amount of discharge meeting serious environment pollution when curtain coating, worsens working conditions and also damages HUMAN HEALTH. Three is that the step of casting technique is many, and the typical production flow process of tradition ferrite sheet is comparatively complicated, is specially: batching → doping → ball milling → pre-burning → secondary ball milling → curtain coating → row glue sintering → test. These processing step complicated operations, and equipment production line is long, floor space is big. Due to the shortcoming of these technical elements, cause current domestic employing casting technique batch to prepare producer's quantity of antifreeze plate material, it is only limitted to research and develop in the powerful several companies of strength.
As can be seen here, existing ferrite magnetic shield blade material is in the preparation, having that recovery rate is low, technique cost height, use range are limited and thickness relatively shortcoming such as big (more than 0.08mm), the mass production of the product such as wireless charging, NFC, RFID and technology is had bigger impact by this. Therefore, the magnetic shielding material of lightening, simple and reliable process and technology of preparing face great research and development demand.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to provide a kind of ultra-thin magnetic shielding sheet material, the feature that this material has thickness ultrathin, magnetic shield performance is excellent.
The two of the object of the present invention are to provide the preparation method of a kind of above-mentioned ultra-thin magnetic shielding sheet material. The method preparation technology is simple and reliable, lumber recovery height, energy-conserving and environment-protective, and magnetic sheet thickness freely can control according to performance demand.
For achieving the above object, the present invention is by the following technical solutions:
A kind of ultra-thin magnetic shielding sheet material, is made up of ferrite, caking agent, additive, tensio-active agent; Described ultra-thin magnetic shielding sheet material thickness is 0.001-0.08mm (such as 0.002mm, 0.005mm, 0.008mm, 0.012mm, 0.015mm, 0.02mm, 0.03mm, 0.04mm, 0.05mm, 0.06mm, 0.07mm, 0.075mm, 0.078mm).
At 13.56 mhz, when measuring condition is 25 DEG C, magnetic permeability real part the μ '=70-200 of described ultra-thin magnetic shielding sheet material, magnetic permeability imaginary part μ " < 5.
Above-mentioned ultra-thin magnetic shielding sheet material, as a kind of preferred implementation, described ferrite is at least one in NiZn ferrite, NiZnMn ferrite, NiZnCu ferrite, NiZnCuMn ferrite, more preferably, described ferritic it is of a size of 0.2-10 μm (such as 0.5 μm, 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm). Described ferrite is by Fe2O3, ZnO, CuO, NiO, MnO raw material make, by mole content, in described ferrite raw material, Fe2O3: 20-70%, ZnO:10-50%, CuO:0-15%, NiO:10-50%, MnO:0-25%.
Above-mentioned ultra-thin magnetic shielding sheet material, as a kind of preferred implementation, described caking agent is water soluble adhesive, and the paste composition that water soluble adhesive obtains is even, and mobility is strong, easy to clean, and environmentally safe; More preferably, described binding agent is carboxymethyl cellulose and/or polyvinyl alcohol.
Above-mentioned ultra-thin magnetic shielding sheet material, as a kind of preferred implementation, described additive is Bi2O3、WO3、Co2O3、PbO、MoO3With at least one in lead glass;
Above-mentioned ultra-thin magnetic shielding sheet material, as a kind of preferred implementation, described tensio-active agent is at least one in isooctyl alcohol, polyoxyethylene stearic acid ester, polyoxyethylene glycol.
Above-mentioned ultra-thin magnetic shielding sheet material, as a kind of preferred implementation, described additive quality is the 1-5% (such as 1.5%, 2%, 2.5%, 3.0%, 3.5%, 4.0%, 4.5%) of described ferritic total mass; The quality of described tensio-active agent is the 0.2-0.5% (such as 0.3%, 0.4%) of described ferritic total mass; The quality of described caking agent is the 5-20% (such as 6%, 8%, 12%, 16%, 18%, 19%) of described ferritic total mass.
The preparation method of above-mentioned ultra-thin magnetic shielding sheet material, comprises the steps:
S1, prepares burden according to above-mentioned ferritic feed composition and proportioning, after oven dry, adds described additive, obtains compound after mixing;
S2, carries out a ball milling to compound described in step S1, dries and obtains levigate compound;
S3, is pressed into block by the described levigate compound obtained in step S2;
S4, carries out presintering process by block described in step S3, obtains presintering block;
S5, carries out fragmentation to the block of presintering described in step S4, and carries out secondary ball milling, obtain powder material after oven dry;
S6, according to predetermined proportion, adds caking agent, water and tensio-active agent in powder material described in step S5, stirs evenly, obtains the slurry of ferrite magnetic sheet;
S7, according to different thickness demands, sprays on load bearing board by slurry described in step S6, to obtain the ferrite sheet of desired thickness;
S8, the load bearing board shove charge being loaded with ferrite sheet obtained by step S7 carries out magnetic sheet sintering, then carries out the stripping of magnetic sheet, final obtained described ultra-thin magnetic shielding sheet material.
In above-mentioned preparation method, as a kind of preferred implementation, in step S1, the consumption of described additive is the 1-5% (such as 1.2%, 1.5%, 1.8%, 2.2%, 1.8%, 3.2%, 3.6%, 4.2%, 4.8%) of described ferrite raw material total mass; More preferably, the consumption of described additive is the 2-3% of described ferrite raw material total mass. Further, described additive is by WO3、Bi2O3And Co2O3The mixture of composition, or by PbO, MoO3With the mixture of lead glass composition, or by PbO, Bi2O3With the mixture of lead glass composition. Additive can mineralising, flux, hinder crystalline substance, improve electromagnetic performance.
In above-mentioned preparation method, as a kind of preferred implementation, in step S2, the ratio of grinding media to material of a described ball milling is 8-12:1 (such as 9:1,10:1), revolution is 250-320r/min (such as 255r/min, 265r/min, 275r/min, 285r/min, 295r/min, 305r/min, 315r/min), and the ball milling time is 2-12h (such as 3h, 5h, 7h, 9h, 11h); The average particle diameter size of described levigate compound reaches 1-5 μm (such as 1.5 μm, 3 μm, 4 μm, 4.5 μm).
In above-mentioned preparation method, as a kind of preferred implementation, in step S3, the length of described block is 5-10cm, and wide is 4-10cm, and height is 0.5-3cm; The press pressure of described compacting is 10T, and the compacting time is 5s.
In above-mentioned preparation method, as a kind of preferred implementation, in step S4, the temperature of described presintering process is 500-1000 DEG C (such as 520 DEG C, 550 DEG C, 580 DEG C, 620 DEG C, 660 DEG C, 700 DEG C, 740 DEG C, 780 DEG C, 820 DEG C, 860 DEG C, 900 DEG C, 940 DEG C, 980 DEG C), and the time of described presintering process is 0.5-6h (such as 0.6h, 1.0h, 1.5h, 2.0h, 2.5h, 3.0h, 3.5h, 4.0h, 4.5h, 5.0h, 5.3h, 5.6h, 5.8h). Presintering can make ferrite generation densification, volumetric shrinkage.
In above-mentioned preparation method, as a kind of preferred implementation, in step S5, the ratio of grinding media to material of described secondary ball milling is 8-12:1 (such as 9:1,10:1), revolution is 250-280r/min (such as 255r/min, 265r/min, 275r/min), and the ball milling time is 2-48h (such as 2.0h, 5.0h, 7.0h, 10h, 15h, 18h, 20h, 25h, 30h, 35h, 40h, 45h, 48h); The median size of described powder material is 0.2-1 μm (such as 0.5 μm, 0.7 μm). Secondary ball milling by lumpy material grind into powder, for preparation mobility slurry.
In above-mentioned preparation method, as a kind of preferred implementation, in step S6, the add-on of described tensio-active agent is the 0.2-0.5% (such as 0.3%, 0.4%) of ferrite raw material total mass; The add-on of described caking agent is the 5-20% (such as 6%, 8%, 12%, 16%, 18%, 19%) of ferrite raw material total mass; The add-on of described water is the 10-40% (such as 12%, 15%, 18%, 25%, 30%, 33%, 36%, 38%) of ferrite raw material total mass.
In above-mentioned preparation method, as a kind of preferred implementation, in step S7, before described spraying, evenly smear load bearing board with releasing agent, with conveniently stripped; More preferably, described releasing agent is at least one in paraffin, beeswax, palm wax or normal paraffin.
In above-mentioned preparation method, as a kind of preferred implementation, in step S8, described load bearing board is zirconium white or aluminum oxide ceramic bearing burning plate.
In above-mentioned preparation method, as a kind of preferred implementation, in step S7, described spraying adopts spraying machine to complete, it is preferred to use with the spraying machine of agitating function. Above-mentioned spraying machine, adopts conventional spraying machine to satisfy the demands, and adopts the spraying machine better effects if with agitating function.
The present inventor finds, adopt and stir spraying coating process, it is possible to for substituting original casting technique, there is the unique advantage of three aspects: the thickness of (1) magnetic sheet adopts spraying method, the thinnest can accomplish 0.001mm, and the thickness of magnetic sheet can be customized according to demand; (2) spraying coating process step operation is easy, controling parameters is few, and applicable surface is wide, cost is low; (3) spraying coating process can be sprayed directly on pottery load bearing board, it is not necessary to adopts film-substrate to be used for curtain coating, preparation efficiency height.
In above-mentioned preparation method, as a kind of preferred implementation, in step S8, the temperature of described sintering is 800-1100 DEG C (such as 820 DEG C, 850 DEG C, 880 DEG C, 920 DEG C, 960 DEG C, 1000 DEG C, 1050 DEG C, 1080 DEG C, 1090 DEG C), and the time of described sintering is 0.5-5h (such as 0.8h, 1.2h, 1.5h, 2.0h, 2.5h, 3.0h, 3.5h, 4.0h, 4.5h, 4.8h).
Above-mentioned ultra-thin magnetic shielding sheet material can first be carried out one side film, directly obtain one side film magnetic shielding sheet. To one side film magnetic shielding sheet, laser cutting can also be adopted, or the broken broken magnetic of magnetic machine, then carry out another side overlay film, obtain there is flexible magnetic shielding sheet.
Above-mentioned magnetic shielding sheet can with aluminium foil or Copper Foil, carry out overlay film and become electromagnetic shielding sheet, not only armoured magnetic field, also electric field shielding.
Compared with prior art, the invention has the beneficial effects as follows:
(1) ultra-thin magnetic shielding sheet material provided by the invention, adopts and the method that slurry carries out spraying is prepared, and thickness is unrestricted, the thinnest can accomplish 0.001mm, and can freely regulate and control according to demand, and this is that existing other technologies method is difficult to accomplish.
(2) preparation method of ultra-thin magnetic shielding sheet material provided by the invention, easy and simple to handle, lumber recovery height, cost is low.
(3) ultra-thin magnetic shielding sheet material provided by the invention and its preparation method, employing be all common water soluble adhesive, for environmental nonpollution, belong to environmentally friendly material.
(4) the magnetic shielding sheet of the present invention and technology of preparing thereof, the material magnetic loss of acquisition is low, its μ " how below 3.
According to application demand, it is possible to paste the two-sided glue of last layer again at material surface easily, and protective membrane, centrifugal paper etc., the position that antenna modules, mobile phone shell, screen etc. need magnetic shielding can be adhered to so as required.
Embodiment
In order to make the content of the present invention be more likely to be clearly understood, below according to a particular embodiment of the invention, the present invention is further detailed explanation.
The all ingredients and the raw material that use in following examples are commercially available prod.
Embodiment 1
A kind of ultra-thin electromagnetic shield blade material of the present embodiment preparation, wherein ferrite thickness is 0.001mm, and concrete preparation process is as follows:
(1) according to 50mol%Fe2O3, 20mol%ZnO, 10mol%CuO, 20mol%NiO ratio prepare burden, add the WO of ferrite raw material powder total mass 0.3% after oven dry3, 1.5% Bi2O3, 0.2% Co2O3Mixture, as additive, obtains compound after mixing.
(2) above-mentioned compound is carried out a ball milling, adopt planetary ball mill, add the water of ferrite raw material powder total mass 1%, ratio of grinding media to material is 8, revolution 300r/min, ball milling time 2h so that the average particle diameter size of compound reaches 5 μm, carry out secondary drying simultaneously, obtain levigate compound.
(3) adopting press to be pressed into 10cm length, 5cm width, block that 1cm is high levigate compound, press pressure is 10T, and the compacting time is 5s.
(4) block of briquetting is carried out presintering process, pre-sintering temperature 800 DEG C, presintering time 3h, obtain presintering block;
(5) the presintering block of acquisition being carried out fragmentation, and carry out secondary ball milling, ratio of grinding media to material is 10, revolution 270r/min, and the ball milling time is 48h, obtains powder material, and its mean particle size is 0.3 μm;
(6) toward in above-mentioned powder material, caking agent and pure water is added respectively according to 12%, the 33% of ferrite raw material powder total mass, caking agent is carboxymethyl cellulose, add the tensio-active agent isooctyl alcohol of ferrite raw material powder total mass 0.5% simultaneously, stir evenly, obtain the slurry of ferrite magnetic sheet;
(7) slurry that will prepare, adopts spraying machine to spray on the zirconia ceramics load bearing board scribbling paraffin, the ferrite sheet of spraying 0.00105mm thickness;
(8) the zirconia ceramics load bearing board of ferrite sheet will be loaded with; shove charge carries out magnetic sheet sintering; sintering temperature 1000 DEG C; sintering time 5h; obtain the magnetic shielding sheet that thickness is 0.001mm; then carry out the stripping of magnetic shielding sheet, cover last layer PE protective membrane afterwards again and cut out, final obtained described ultra-thin magnetic shielding sheet material.
Adopting the method to produce 100 magnetic shielding sheets, yield rate is 92%.
Alloy magnetic shielding piece performance is measured at 25 DEG C. Complex permeability under adopting Agilent4294A electric impedance analyzer to measure 13.56HMz, magnetic permeability real part μ '=70, magnetic permeability imaginary part μ "=2.
Embodiment 2
A kind of ultra-thin electromagnetic shield blade material of the present embodiment preparation, wherein ferrite thickness is 0.08mm, and concrete preparation process is as follows:
(1) according to 70mol%Fe2O3, the ratio of 10mol%ZnO, 5mol%CuO, 15mol%NiO is prepared burden, and adds the WO of ferrite raw material powder total mass 0.5% after oven dry3, 2% Bi2O3, 0.5% Co2O3Mixture, as waiting additive, obtains compound after mixing.
(2) above-mentioned compound is carried out a ball milling, adopt planetary ball mill, add the water of ferrite raw material powder total mass 1%, ratio of grinding media to material is 8, revolution 300r/min, ball milling time 6h so that the average particle diameter size of compound reaches 2 μm, carry out secondary drying simultaneously, obtain levigate compound.
(3) adopting press to be pressed into 8cm length, 6cm width, block that 2cm is high levigate compound, press pressure is 10T, and the compacting time is 5s.
(4) block of briquetting is carried out presintering process, pre-sintering temperature 620 DEG C, presintering time 6h, obtain presintering block;
(5) the presintering block of acquisition being carried out fragmentation, and carry out secondary ball milling, ratio of grinding media to material is 10, revolution 270r/min, and the ball milling time is 16h, obtains powder material, and its mean particle size is 0.6 μm;
(6) toward in above-mentioned powder material, caking agent and pure water is added respectively according to 5%, the 40% of ferrite raw material powder total mass, caking agent is PVAC polyvinylalcohol 1788, add the tensio-active agent polyoxyethylene stearic acid ester (CAS:9005-00-9 of ferrite raw material powder total mass 0.2% simultaneously, purchased from lark prestige Science and Technology Ltd.), stir evenly, obtain the slurry of ferrite magnetic sheet;
(7) slurry that will prepare, adopts spraying machine to spray on the zirconia ceramics load bearing board scribbling beeswax, the ferrite sheet of spraying 0.065mm thickness;
(8) load bearing board of zirconia of ferrite sheet will be loaded with; shove charge carries out magnetic sheet sintering; sintering temperature 900 DEG C; sintering time 1h; obtain the magnetic shielding sheet that thickness is 0.06mm; then carry out the stripping of magnetic shielding sheet, cover last layer PE protective membrane afterwards again and cut out, final obtained described ultra-thin magnetic shielding sheet material.
Adopting the method to produce 100 magnetic shielding sheets, yield rate is 90%.
Alloy property is measured at 25 DEG C. Complex permeability under adopting Agilent4294A electric impedance analyzer to measure 13.56HMz, magnetic permeability real part μ '=110, magnetic permeability imaginary part μ "=3.
Embodiment 3
A kind of ultra-thin electromagnetic shield blade material of the present embodiment preparation, wherein ferrite thickness is 0.06mm, and concrete preparation process is as follows:
(1) according to 30mol%Fe2O3, 21mol%ZnO, 9mol%CuO, 15mol%NiO, 25%MnO proportioning raw materials prepare burden, add the PbO of ferrite raw material powder total mass 0.5%, the MoO of 2% after oven dry3, 0.5% lead glass mixture as additive, obtain compound after mixing.
(2) above-mentioned compound is carried out a ball milling, adopt planetary ball mill, add the water of ferrite raw material powder total mass 1%, ratio of grinding media to material is 12, revolution 270r/min, ball milling time 4h so that the average particle diameter size of compound reaches 5 μm, carry out secondary drying simultaneously, obtain levigate compound.
(3) adopting press to be pressed into 5cm length, 10cm width, block that 3cm is high above-mentioned levigate compound, press pressure is 10T, and the compacting time is 5s.
(4) block of briquetting is carried out presintering process, pre-sintering temperature 500 DEG C, presintering time 6h, obtain presintering block;
(5) the presintering block of acquisition being carried out fragmentation, and carry out secondary ball milling, ratio of grinding media to material is 10, and the revolution 270r/min ball milling time is 24h, obtains powder material, and its mean particle size is 0.8 μm;
(6) toward in above-mentioned powder material, caking agent and pure water is added respectively by 20%, the 10% of ferrite raw material powder total mass, caking agent is PVAC polyvinylalcohol 1788, add the surfactant polyethylene 400 of ferrite raw material powder total mass 0.3% simultaneously, stir evenly, obtain the slurry of ferrite magnetic sheet;
(7) slurry that will prepare, adopts spraying machine to spray on the zirconia ceramics load bearing board scribbling palm wax, the ferrite sheet of spraying 0.065mm thickness;
(8) the zirconia ceramics load bearing board of ferrite sheet will be loaded with; shove charge carries out magnetic sheet sintering; sintering temperature 1100 DEG C; sintering time 3h; obtain the magnetic shielding sheet that thickness is 0.06mm; then carry out the stripping of magnetic shielding sheet, cover last layer PE protective membrane afterwards again and cut out, final obtained described ultra-thin magnetic shielding sheet material.
Adopting the method to produce 100 magnetic shielding sheets, yield rate is 92%.
Alloy property is measured at 25 DEG C. Complex permeability under adopting Agilent4294A electric impedance analyzer to measure 13.56HMz, magnetic permeability real part μ '=200, magnetic permeability imaginary part μ "=2.5.
Embodiment 4
A kind of ultra-thin electromagnetic shield blade material of the present embodiment preparation, wherein ferrite thickness is 0.02mm, and concrete preparation process is as follows:
(1) by 40mol%Fe2O3, 10mol%ZnO, 50mol%NiO, prepare burden, after oven dry, add the PbO of ferrite raw material powder total mass 0.5%, the Bi of 2%2O3, 0.5% the additive such as lead glass mixture, obtain compound after mixing.
(2) above-mentioned compound is carried out a ball milling, adopt planetary ball mill, add the water of ferrite raw material powder total mass 1%, ratio of grinding media to material is 12, revolution 270r/min, ball milling time 24h so that the average particle diameter size of compound reaches 2 μm, dry simultaneously, obtain levigate compound.
(3) adopting press to be pressed into 10cm length, 10cm width, block that 0.5cm is high above-mentioned levigate compound, press pressure is 10T, and the compacting time is 5s.
(4) block of briquetting is carried out presintering process, pre-sintering temperature 1000 DEG C, presintering time 6h, obtain pre-burning block;
(5) the presintering block of acquisition being carried out fragmentation, and carry out secondary ball milling, ratio of grinding media to material is 10, revolution 260r/min, and the ball milling time is 18h, obtains powder material, and its mean particle size is 0.2 μm;
(6) toward in above-mentioned powder material, caking agent and pure water is added according to 12%, the 33% of ferrite raw material powder total mass, caking agent is PVAC polyvinylalcohol 1788, add the surfactant polyethylene 400 of ferrite raw material powder total mass 0.3% simultaneously, stir evenly, obtain the slurry of ferrite magnetic sheet;
(7) slurry that will prepare, adopts spraying machine to spray on the zirconia ceramics load bearing board scribbling palm wax, the ferrite sheet of spraying 0.022mm thickness;
(8) the zirconia ceramics load bearing board of ferrite sheet will be loaded with; shove charge carries out magnetic sheet sintering; sintering temperature 1100 DEG C; sintering time 1h; obtain the magnetic shielding sheet that thickness is 0.02mm; then carry out the stripping of magnetic shielding sheet, cover last layer PE protective membrane afterwards again and cut out, final obtained described ultra-thin magnetic shielding sheet material.
Adopting the method to produce 100 magnetic shielding sheets, yield rate is 93%.
Alloy property is measured at 25 DEG C. Complex permeability under adopting Agilent4294A electric impedance analyzer to measure 13.56HMz, magnetic permeability real part μ '=130, magnetic permeability imaginary part μ "=3.
Embodiment 5
A kind of ultra-thin electromagnetic shield blade material of the present embodiment preparation, wherein ferrite thickness is 0.04mm, and concrete preparation process is as follows:
(1) according to 40mol%Fe2O3, 50mol%ZnO, 10mol%NiO ratio prepare burden, add the WO of ferrite raw material powder total mass 0.3% after oven dry3, 1.5% Bi2O3, 0.2% Co2O3Mixture, as additive, obtains compound after mixing.
(2) above-mentioned compound is carried out a ball milling, adopt planetary ball mill, add the water of ferrite raw material powder total mass 1%, ratio of grinding media to material is 10, revolution 300r/min, ball milling time 32h so that the average particle diameter size of compound reaches 2.5 μm, carry out secondary drying simultaneously, obtain levigate compound.
(3) adopting press to be pressed into 5cm length, 4cm width, block that 1cm is high above-mentioned levigate compound, press pressure is 10T, and the compacting time is 5s.
(4) block of briquetting is carried out presintering process, pre-sintering temperature 700 DEG C, presintering time 3h, obtain presintering block;
(5) the presintering block of acquisition being carried out fragmentation, and carry out secondary ball milling, ratio of grinding media to material is 10, revolution 270r/min, and the ball milling time is 16h, obtains powder material, and its mean particle size is 0.4 μm;
(6) toward in above-mentioned powder material, caking agent and pure water is added respectively according to 12%, the 33% of ferrite raw material powder total mass, caking agent is carboxymethyl cellulose, add the tensio-active agent isooctyl alcohol of ferrite raw material powder total mass 0.5% simultaneously, stir evenly, obtain the slurry of ferrite magnetic sheet;
(7) slurry that will prepare, adopts spraying machine to spray on the zirconia ceramics load bearing board scribbling paraffin, the ferrite sheet of spraying 0.045mm thickness;
(8) the zirconia ceramics load bearing board of ferrite sheet will be loaded with; shove charge carries out magnetic sheet sintering; sintering temperature 900 DEG C; sintering time 5h; obtain the magnetic shielding sheet that thickness is 0.04mm; then carry out the stripping of magnetic shielding sheet, cover last layer PE protective membrane afterwards again and cut out, final obtained described ultra-thin magnetic shielding sheet material.
Adopting the method to produce 100 magnetic shielding sheets, yield rate is 92%.
Alloy magnetic shielding piece performance is measured at 25 DEG C. Complex permeability under adopting Agilent4294A electric impedance analyzer to measure 13.56HMz, magnetic permeability real part μ '=70, magnetic permeability imaginary part μ "=2.
Obviously, above-described embodiment is only for example is clearly described, and not to the restriction of the mode of enforcement. For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description. Here without the need to also cannot all enforcement modes be given exhaustive. And the apparent change thus extended out or variation are still among the protection domain of the invention.

Claims (10)

1. a ultra-thin magnetic shielding sheet material, it is characterised in that, described ultra-thin magnetic shielding sheet material is made up of ferrite, caking agent, additive, tensio-active agent; Described ultra-thin magnetic shielding sheet material thickness is 0.001-0.08mm.
2. ultra-thin magnetic shielding sheet material according to claim 1, it is characterised in that, described ferrite is at least one in NiZn ferrite, NiZnMn ferrite, NiZnCu ferrite, NiZnCuMn ferrite;More preferably, described ferrite is by Fe2O3, ZnO, CuO, NiO, MnO raw material make, by mole content, in described ferrite raw material, Fe2O3: 20-70%, ZnO:10-50%, CuO:0-15%, NiO:10-50%, MnO:0-25%; Preferably, described ferritic it is of a size of 0.2-10 μm.
3. ultra-thin magnetic shielding sheet material according to claim 1, it is characterised in that, described caking agent is water soluble adhesive; Preferably, described binding agent is carboxymethyl cellulose and/or polyvinyl alcohol; Described additive is Bi2O3、WO3、Co2O3、PbO、MoO3With at least one in lead glass; Described tensio-active agent is at least one in isooctyl alcohol, polyoxyethylene stearic acid ester, polyoxyethylene glycol.
4. ultra-thin magnetic shielding sheet material according to claim 1, it is characterised in that, described additive quality is the 1-5% of described ferritic total mass; The quality of described tensio-active agent is the 0.2-0.5% of described ferritic total mass; The quality of described caking agent is the 5-20% of described ferritic total mass.
5. the preparation method of the described ultra-thin magnetic shielding sheet material of the arbitrary item of claim 1-4, it is characterised in that, comprise the steps:
S1, prepares burden according to described ferritic feed composition and proportioning, after oven dry, adds described additive, obtains compound after mixing;
S2, carries out a ball milling to compound described in step S1, dries and obtains levigate compound;
S3, is pressed into block by the described levigate compound obtained in step S2;
S4, carries out presintering process by block described in step S3, obtains presintering block;
S5, carries out fragmentation to the block of presintering described in step S4, and carries out secondary ball milling, obtain powder material after oven dry;
S6, according to predetermined proportion, adds caking agent, water and tensio-active agent in powder material described in step S5, stirs evenly, obtains the slurry of ferrite magnetic sheet;
S7, according to different thickness demands, sprays on load bearing board by slurry described in step S6, to obtain the ferrite sheet of desired thickness;
S8, the load bearing board shove charge being loaded with ferrite sheet obtained by step S7 carries out magnetic sheet sintering, then carries out the stripping of magnetic sheet, final obtained described ultra-thin magnetic shielding sheet material.
6. preparation method according to claim 5, it is characterised in that, in step S1, the consumption of described additive is the 1-5% of described ferrite raw material total mass; Preferably, the consumption of described additive is the 2-3% of described ferrite raw material total mass; More preferably, described additive is by WO3、Bi2O3And Co2O3The mixture of composition, or by PbO, MoO3With the mixture of lead glass composition, or by PbO, Bi2O3With the mixture of lead glass composition.
7. preparation method according to claim 5, it is characterised in that, in step S2, the ratio of grinding media to material of a described ball milling is 8-12:1, and revolution is 250-320r/min, and the ball milling time is 2-12h; The average particle diameter size of described levigate compound reaches 1-5 μm; In step S5, the ratio of grinding media to material of described secondary ball milling is 8-12:1, and revolution is 250-280r/min, and the ball milling time is 2-48h; The median size of described powder material is 0.2-1 μm; Preferably, in step S3, the length of described block is 5-10cm, and wide is 4-10cm, and height is 0.5-3cm; The press pressure of described compacting is 10T, and the compacting time is 5s.
8. preparation method according to claim 5, it is characterised in that, in step S4, the temperature of described presintering process is 500-1000 DEG C, and the time of described presintering process is 0.5-6h.
9. preparation method according to claim 5, it is characterised in that, in step S6, the add-on of described tensio-active agent is the 0.2-0.5% of described ferrite raw material total mass; The add-on of described caking agent is the 5-20% of described ferrite raw material total mass; The add-on of described water is the 10-40% of described ferrite raw material total mass.
10. preparation method according to claim 5, it is characterised in that, in step S7, before described spraying, evenly smear load bearing board with releasing agent, with conveniently stripped; Preferably, described releasing agent is at least one in paraffin, beeswax, palm wax or normal paraffin; Described load bearing board is zirconium white or aluminum oxide ceramic bearing burning plate; Described spraying adopts the spraying machine with agitating function.
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CN113735573A (en) * 2021-08-27 2021-12-03 西安交通大学 Low-loss NiCuZn soft magnetic ferrite material for NFC and preparation method and application thereof
CN113716950A (en) * 2021-11-01 2021-11-30 天通控股股份有限公司 Low-temperature sintered flexible magnetic sheet and preparation method thereof

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