CN109928670A - A kind of water-based tape casting preparation method of sheet FeSiAl electromagnetism interference fexible film - Google Patents
A kind of water-based tape casting preparation method of sheet FeSiAl electromagnetism interference fexible film Download PDFInfo
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Abstract
This application discloses a kind of water-based tape casting preparation methods of sheet FeSiAl electromagnetism interference fexible film, in turn include the following steps: the surface oxidation-resistant processing of S1 iron sial powder；The flaking of S2 iron sial powder is handled；S3 is added the ball millings such as binder, plasticizer and prepares aqueous casting slurry；S4 tape casting.The present invention passes through the processing of alkaline solution and silane coupling agent, and the insulating layer uniformly coated is formd on magnetic powder surface, helps to improve magnetic property, improves resistivity, reduces loss；Sheet iron aluminum silicon powder dispersibility in the slurry, stability are more preferably, it has higher magnetic conductivity and lower dielectric constant compared to the iron aluminum silicon powder of irregular form simultaneously, make it in absorber thickness, impedance matching property and high-absorbility etc. have preferable advantage；The preparation process of waterborne film-forming material is easy, and residue is few, the characteristic for having low toxicity harmless, environmental-friendly；Film thickness made from casting technique is uniform, easy to operate, high production efficiency, is suitable for industrialization large-scale production.
Description
Technical field
The invention belongs to electronic element device materials technology fields, and in particular to a kind of sheet FeSiAl electromagnetism interference is flexible
The aqueous casting slurry of film and its preparation method of film.
Background technique
In recent years, as the Highgrade integration in electric equipment products field develops, wireless power transmission technology is grown rapidly.
Its functional diversities, it is convenient beautiful and in terms of be excellent in while, there are spatial electromagnetic loss and leakages, electricity
The safety problems such as electromagnetic pollution, fever.The electromagnetic interference between bring electronic component, emc issue are increasingly prominent therewith
Out.Therefore, electromagnetic interference between elimination electronic component, realizes that electromagnetic compatibility has become one of significant challenge at this stage.
Patent (105644060 B of CN) discloses a kind of preparation method of ferrite sheet, by ferrite powder, has
Solvent, binder, plasticizer mixing and ball milling are cast into after raw cook and carry out plate or suppress, cut, be sintered, is plastic packaging, soft
Chemical conversion type.The method suppresses sheet material, is crushed, crimps after sintering；The use of acetone and other organic solvent increases production cost, and
Cause serious environmental pollution；Entire production procedure is of long duration, is unfavorable for being mass produced.Patent (105985583 A of CN) is public
A kind of preparation method of wireless charging rubber and plastic soft magnetism antifreeze plate is opened.Method particularly includes: after rubber or thermoplastic material mill,
It is kneaded uniformly with sheet soft magnet powder, vulcanizing agent, anti-aging agent, coupling agent, toughener, vulcanizing treatment is carried out after calendering formation, can be made
For the magnetic sheet gone out with a thickness of 0.3mm.Due to rubber, thermoplastic material elasticity it is larger, plasticity is poor, can not prepare thickness <
The ultra-thin sheet material of 0.2mm；Thermal-oxidative ageing is easy to happen in mixing process, it is easy to crack when making tabletting, and while using, is easy to aging, makes
The problems such as not long at service life.Patent (109337189 A of CN) discloses a kind of flexible magnetic conduction film system of low energy loss
Preparation Method.Method particularly includes: shear-mixed, extrusion and the calendering formation of flat soft magnetic powder and polyolefin grinding can be obtained
With a thickness of the sheet material of 0.2-1mm.The material property of the invention is preferable, but process flow limits higher, complex process, production efficiency
It is low, it is unfavorable for being mass produced.With this, replaces main body organic solvent to can effectively reduce cost using water-based solvent, reduce environment
Dustiness, it can be achieved that product without toxic residual；Casting technique preparation simultaneously is convenient, efficient, can be used for being mass produced, and is cast
Film thickness out is adjustable, not easy to crack, curling, and productivity effect is high.
Summary of the invention
The purpose of the present invention is to overcome the shortcomings of the existing technology, and phase between metal magnetic can effectively be prevented by providing one kind
Mutually contact, improves the preparation method of the sheet magnetic powder of its antioxygenic property.Another object of the present invention is to provide a kind of sheets
The aqueous casting slurry of metal magnetic and its preparation method of film.
The purpose of the present invention is achieved through the following technical solutions: a kind of sheet FeSiAl electromagnetism interference fexible film
Water-based tape casting preparation method, it is characterised in that its raw material includes: 100 parts of FeSiAl alloy powder by weight, deionized water
150-350 parts, 50-150 parts of dehydrated alcohol, 0.5-3 parts of dispersing agent, 5-10 parts of binder, 2.5-5 parts of plasticizer, toughener
0.5-2 parts, 0.1-0.5 parts of 2mol/L sodium hydroxide, 0.1-5 parts of coupling agent.
The sendust powder diameter is 300 mesh.
The dispersing agent is one or more of triethanolamine, polyethylene glycol.
The binder is one or more of polyvinyl alcohol, polyacrylic acid, aqueous polyurethane.
The plasticizer is one or more of glycerine, dibutyl phthalate.
The toughener is YM-004 toughener.
The coupling agent is silane coupling agent KH-560.
The aqueous casting slurry of above-mentioned electromagnetism interference fexible film and its preparation method of film, including following step
It is rapid:
S1 powder surface oxidation-resistant processing: according to 1:(0.3-0.6): the mass ratio of (0.01-0.03) weighs FeSiAl alloyed powder
End, dehydrated alcohol, sodium hydroxide solution, with the revolving speed mechanical stirring 20-60min of 200-300r/min on magnetic stirring apparatus,
It filters；According to 1:(0.3-0.6): the mass ratio of (0.01-0.03), which deserves to be called, states FeSiAl alloy powder, dehydrated alcohol, silane idol
Join agent, with the revolving speed mechanical stirring 20-60min of 200-300r/min on magnetic stirring apparatus, filters, the vacuum at 60-80 DEG C
Heat drying；
The processing of S2 flaking: the processed magnetic powder of step (1), deionized water, dispersing agent are weighed in proportion, is added to ball grinder
In (ratio of grinding media to material 10:1), 10~20h of ball milling, rotational speed of ball-mill 250-500r/min, vacuum and heating drying is standby at 60-80 DEG C
With；
The preparation of S3 slurry: the processed magnetic powder of S2, deionized water, binder, plasticizer, toughener are weighed in proportion, is added to
In ball grinder (ratio of grinding media to material 4:1), 10~20h of ball milling, rotational speed of ball-mill 250-500r/min are filtered to remove undissolved binder
With plasticizer and the magnetic powder reunited, casting slurry is obtained；
S4 film casting: by slurry obtained by S3 carried out under the subnormal ambient of 0.1~0.5MPa vacuum defoamation 0.5~
2h is cast on casting machine.
The present invention has the following advantages and effects with respect to the prior art:
1, the immersion of alkaline solution is passed through on magnetic powder surface ,-OH the active group on magnetic powder surface is increased, so that magnetic powder is more easier
It is combined with coupling agent；
2, the use of coupling agent forms a layer insulating on sheet magnetic powder surface, effectively prevents the phase mutual connection between magnetic powder
Touching, reduces the resistivity of material, and material is made to have higher electromagnetic shielding performance；
3, the sheet magnetic powder of ball-milling technology preparation, effectively reduces finished product thickness, dispersibility, stability in the slurry obtains
It improves, the magnetic conductivity of finished product is also improved；
4, the use of water-based film-forming material, effectively reduces production cost, reduces environmental pollution, realizes the harmless life of low toxicity
It produces；
5, casting technique is easy to operate, and finished product thickness uniformity substantially increases production efficiency, and it is raw can to carry out extensive batch
It produces.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The some embodiments recorded in application, for those of ordinary skill in the art, without creative efforts,
It is also possible to obtain other drawings based on these drawings.
Fig. 1 show the electron scanning micrograph of sheet FeSiAl alloy powder obtained in the embodiment of the present invention 1.
Fig. 2 show thin-film material magnetic conductivity test chart obtained in the embodiment of the present invention 1.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.
Example 1
S1 alloy powder surface treatment: according to the mass ratio of 1:0.35:0.015 weigh FeSiAl alloy powder, dehydrated alcohol,
Sodium hydroxide solution is filtered with the revolving speed mechanical stirring 30min of 300r/min on magnetic stirring apparatus；According to 1:0.35:0.01
Mass ratio deserve to be called and state FeSiAl alloy powder, dehydrated alcohol, KH-560 silane coupling agent, with 300r/ on magnetic stirring apparatus
The revolving speed mechanical stirring 30min of min is filtered, and vacuum and heating drying is spare at 70 DEG C；
S2 flaking processing: weigh the processed magnetic powder of 100 mass of surface, 150 mass parts deionized waters, 2 mass parts three
Ethanol amine is added in ball grinder (ratio of grinding media to material 10:1), ball milling 15h, rotational speed of ball-mill 300r/min, the heating in vacuum at 70 DEG C
Drying for standby；
The preparation of S3 slurry: it is aqueous poly- that the sheet Fe-Si-Al magnetics of 100 mass parts, 80 mass parts deionized waters, 6 mass parts are weighed
Urethane, 3.2 mass parts glycerine, 0.5 mass parts toughener, are added in ball grinder (ratio of grinding media to material 4:1), ball milling 15h, ball milling
Revolving speed 400r/min, the magnetic powder for being filtered to remove undissolved binder and plasticizer and reuniting, obtains casting slurry；
S4 film casting: vacuum defoamation 0.5h is carried out under the subnormal ambient of 0.3MPa, is cast on casting machine, substrate material
Material is PET film, and bringing-up section temperature is 40 DEG C of first segment, 80 DEG C of second segment, and curtain coating speed is 0.35m/min, and the viscosity of slurry is
1600PaS, scraper height are 0.1mm.
Example 2
The surface treatment of S1 alloy powder: FeSiAl alloy powder, dehydrated alcohol, hydrogen are weighed according to the mass ratio of 1:0.4:0.01
Sodium hydroxide solution is filtered with the revolving speed mechanical stirring 40min of 250r/min on magnetic stirring apparatus；According to 1:0.4:0.015's
Mass ratio, which deserves to be called, states FeSiAl alloy powder, dehydrated alcohol, KH-560 silane coupling agent, with 250r/min on magnetic stirring apparatus
Revolving speed mechanical stirring 40min, filter, vacuum and heating drying is spare at 75 DEG C；
The processing of S2 flaking: the processed magnetic powder of 100 mass of surface, 120 mass parts deionized waters, 1.5 mass parts are weighed
Polyethylene glycol is added in ball grinder (ratio of grinding media to material 10:1), and ball milling 10h, rotational speed of ball-mill 450r/min, vacuum adds at 75 DEG C
Heated drying is spare；
The preparation of S3 slurry: sheet Fe-Si-Al magnetic, 90 mass parts deionized waters, the 8 mass parts polyethylene of 100 mass parts are weighed
Alcohol, 4.5 mass parts dibutyl phthalates, 0.4 mass parts toughener, are added in ball grinder (ratio of grinding media to material 4:1), ball milling
12h, rotational speed of ball-mill 450r/min, the magnetic powder for being filtered to remove undissolved binder and plasticizer and reuniting are flowed
Prolong slurry；
S4 film casting: vacuum defoamation 1h is carried out under the subnormal ambient of 0.4MPa, is cast on casting machine, base material
For PET film, bringing-up section temperature is 60 DEG C of first segment, 120 DEG C of second segment, and curtain coating speed is 0.4m/min, and the viscosity of slurry is
2400PaS, scraper height are 0.2mm.
Example 3
The surface treatment of S1 alloy powder: FeSiAl alloy powder, dehydrated alcohol, hydrogen are weighed according to the mass ratio of 1:0.45:0.02
Sodium hydroxide solution is filtered with the revolving speed mechanical stirring 50min of 200r/min on magnetic stirring apparatus；According to 1:0.45:0.02's
Mass ratio, which deserves to be called, states FeSiAl alloy powder, dehydrated alcohol, KH-560 silane coupling agent, with 200r/min on magnetic stirring apparatus
Revolving speed mechanical stirring 50min, filter, vacuum and heating drying is spare at 80 DEG C；
The processing of S2 flaking: it is poly- that the processed magnetic powder of 100 mass of surface, 180 mass parts deionized waters, 2.5 mass parts are weighed
Ethylene glycol is added in ball grinder (ratio of grinding media to material 10:1), ball milling 10h, rotational speed of ball-mill 500r/min, the heating in vacuum at 80 DEG C
Drying for standby；
The preparation of S3 slurry: sheet Fe-Si-Al magnetic, the 100 mass parts deionized waters, 10 mass parts poly- third of 100 mass parts are weighed
Olefin(e) acid, 5.3 mass parts glycerine, 0.5 mass parts toughener, are added in ball grinder (ratio of grinding media to material 4:1), ball milling 10h, ball milling
Revolving speed 500r/min, the magnetic powder for being filtered to remove undissolved binder and plasticizer and reuniting, obtains casting slurry；
S4 film casting: vacuum defoamation 1h is carried out under the subnormal ambient of 0.3MPa, is cast on casting machine, base material
For PET film, bringing-up section temperature is 50 DEG C of first segment, 100 DEG C of second segment, and curtain coating speed is 0.35m/min, and the viscosity of slurry is
2000PaS, scraper height are 0.15mm.
This embodiment is just an exemplary description of this patent and does not limit its protection scope, and those skilled in the art are also
Local change can be carried out to it, as long as it does not exceed the essence of this patent, all be considered as the equivalent replacement to this patent, all
Within the protection scope of this patent.
Claims (9)
1. a kind of water-based tape casting preparation method of sheet FeSiAl electromagnetism interference fexible film, which is characterized in that its raw material is pressed
Parts by weight meter includes: 100 parts of FeSiAl alloy powder, and 150-350 parts of deionized water, 50-150 parts of dehydrated alcohol, dispersing agent
0.5-3 parts, 5-10 parts of binder, 2.5-5 parts of plasticizer, 0.5-2 parts of toughener, 0.1-0.5 parts of 2mol/L sodium hydroxide, coupling
0.1-5 parts of agent.
2. a kind of water-based tape casting preparation method of sheet FeSiAl electromagnetism interference fexible film, which is characterized in that its preparation side
Method the following steps are included:
S1 powder surface oxidation-resistant processing: according to 1:(0.3-0.6): the mass ratio of (0.01-0.03) weighs FeSiAl alloyed powder
End, dehydrated alcohol, sodium hydroxide solution are filtered with the revolving speed mechanical stirring 20-60min of 200-300r/min；According to 1:
(0.3-0.6): the mass ratio of (0.01-0.03), which deserves to be called, states FeSiAl alloy powder, dehydrated alcohol, silane coupling agent, with 200-
The revolving speed mechanical stirring 20-60min of 300r/min is filtered, the vacuum and heating drying at 60-80 DEG C；
The processing of S2 flaking: the processed magnetic powder of S1, deionized water, dispersing agent are weighed in proportion, is added in ball grinder (ball
Material is than being 10:1), 10~20h of ball milling, rotational speed of ball-mill 250-500r/min, vacuum and heating drying is spare at 60-80 DEG C；
The preparation of S3 slurry: the processed magnetic powder of S2, deionized water, binder, plasticizer, toughener are weighed in proportion, is added to
In ball grinder (ratio of grinding media to material 4:1), 10~20h of ball milling, rotational speed of ball-mill 250-500r/min are filtered to remove undissolved binder
With plasticizer and the magnetic powder reunited, casting slurry is obtained；
S4 film casting: by slurry obtained by S3 carried out under the subnormal ambient of 0.1~0.5MPa vacuum defoamation 0.5~
2h is cast on casting machine.
3. the preparation method of aqueous casting slurry according to claim 2, it is characterised in that: the dispersing agent is three ethyl alcohol
One or more of amine, polyethylene glycol.
4. the preparation method of aqueous casting slurry according to claim 2, it is characterised in that: the binder is polyethylene
One or more of alcohol, polyacrylic acid, aqueous polyurethane.
5. the preparation method of aqueous casting slurry according to claim 2, it is characterised in that: the plasticizer be glycerine,
One or more of dibutyl phthalate.
6. the preparation method of aqueous casting slurry according to claim 2, it is characterised in that: the toughener is YM-004 increasing
Tough dose.
7. the preparation method of aqueous casting slurry according to claim 2, it is characterised in that: the coupling agent is KH-560.
8. the preparation method of aqueous casting slurry according to claim 2, it is characterised in that: ground described in step S2, S3
Ball is diameter 6mm, diameter 10mm steel ball is used in mixed way with the quantity ratio of 4:1.
9. the preparation method of electromagnetism interference fexible film according to claim 2, it is characterised in that: flowed described in step S4
Prolong the control condition of technique are as follows: the viscosity of slurry is 1200~2800PaS, curtain coating speed is 0.3~0.5m/min, scrapes knife up
Degree is 0.02~2mm, drying temperature is 40~160 DEG C.
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| CN110719727A (en) * | 2019-10-28 | 2020-01-21 | 横店集团东磁股份有限公司 | Low-dielectric composite FeSiAl powder material and preparation method thereof |
| CN111057457A (en) * | 2019-12-31 | 2020-04-24 | 江门江益磁材有限公司 | Water-resistant and environment-friendly water-based wave absorbing plate and preparation method thereof |
| CN112207283A (en) * | 2020-10-22 | 2021-01-12 | 合肥工业大学 | Preparation method of flaky ferrosilicon aluminum powder with uniform particle size, micron-sized particles with large diameter-thickness ratio and particle morphology |
| CN113292755A (en) * | 2021-05-27 | 2021-08-24 | 浙江工业大学 | Method for preparing membrane based on evaporation self-assembly |
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2019
- 2019-04-01 CN CN201910256934.4A patent/CN109928670A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110719727A (en) * | 2019-10-28 | 2020-01-21 | 横店集团东磁股份有限公司 | Low-dielectric composite FeSiAl powder material and preparation method thereof |
| CN110719727B (en) * | 2019-10-28 | 2020-11-10 | 横店集团东磁股份有限公司 | Low-dielectric composite FeSiAl powder material and preparation method thereof |
| CN111057457A (en) * | 2019-12-31 | 2020-04-24 | 江门江益磁材有限公司 | Water-resistant and environment-friendly water-based wave absorbing plate and preparation method thereof |
| CN111057457B (en) * | 2019-12-31 | 2021-08-27 | 江门江益磁材有限公司 | Water-resistant and environment-friendly water-based wave absorbing plate and preparation method thereof |
| CN112207283A (en) * | 2020-10-22 | 2021-01-12 | 合肥工业大学 | Preparation method of flaky ferrosilicon aluminum powder with uniform particle size, micron-sized particles with large diameter-thickness ratio and particle morphology |
| CN112207283B (en) * | 2020-10-22 | 2022-05-20 | 合肥工业大学 | Preparation method of flaky iron-silicon-aluminum powder with uniform particle size and micron-sized large diameter-thickness ratio particles |
| CN113292755A (en) * | 2021-05-27 | 2021-08-24 | 浙江工业大学 | Method for preparing membrane based on evaporation self-assembly |
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