CN109400958A - A kind of flexible soft magnetic ferrite composite material and preparation method for electromagnetic shielding - Google Patents
A kind of flexible soft magnetic ferrite composite material and preparation method for electromagnetic shielding Download PDFInfo
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- CN109400958A CN109400958A CN201811228784.8A CN201811228784A CN109400958A CN 109400958 A CN109400958 A CN 109400958A CN 201811228784 A CN201811228784 A CN 201811228784A CN 109400958 A CN109400958 A CN 109400958A
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention discloses a kind of flexible soft magnetic ferrite composite materials and preparation method for electromagnetic shielding.The soft magnetic ferrite composite material is made by following steps: a, will be adjusted pH value in trihydroxy methyl amino silane, manganese-zinc ferrite core powder, dehydrated alcohol addition deionized water, is formed mixed solution；B, Dopamine hydrochloride and heating stirring reaction is added, the manganese-zinc ferrite of poly-dopamine cladding is made；C, with rubber mix inject mold after it is hot-forming, the flexible soft magnetic ferrite composite material for electromagnetic shielding is made.The method has the advantages that the present invention can be uniformly dispersed in rubber by the manganese-zinc-ferrite powder of modification activation, the initial permeability of product obtained is high, it can satisfy electromagnetic shielding and electromagnetism interference conventional design demand under room temperature, product flexibility is good, it is easy to process, it is hardly damaged, can be used for lining, wireless charging mobile phone receiving end, electromagnetic shielding test cabinet, household Radiation-roof wallpaper of radiation protection clothing etc..
Description
Technical field
The present invention relates to electromagnetic shielding fields, and in particular to the preparation of flexible composite is used for more particularly, to one kind
The flexible soft magnetic ferrite composite material and preparation method of electromagnetic shielding.
Background technique
It with the development of electronic communication, protects information from full spectrum of threats and interference by electromagnetic shielding, is to guarantee information
The important means of safety.Biggest threat has been constituted to electronic system in electromagnetic interference now, has seriously affected mentioning for equipment performance
High and performance, the also personal safety to public environment and the mankind and military security, national defense safety cause very big harm.Cause
The technology of this research and development electromagnetism interference is then the task of top priority, has become a particularly important project of countries in the world.
By improving the interference rejection ability of disturbed equipment, the susceptibility to interference can be reduced.
Several measures for inhibiting interference at present are essentially all using the coupling between cutting electromagnetic interference source and disturbed equipment
Channel is closed, basic skills is exactly to shield, be grounded and filter.In actual electromagnetic shielding application, effective shield effectiveness standard is
20dB.Due to the integrated and facilitation of all kinds of electronic communication devices, to lightweight, thin layer, High Performance Shielding demand
It is more more and more urgent.It realizes High Performance Shielding, on the one hand can develop the material with high dielectric loss characteristics, realize electrical loss
；On the other hand, exploitation has the material of high magnetic loss characteristic, realizes magnetic loss, passes through the common reinforcing material electromagnetic screen of electro magnetic
Cover efficiency.The present maximum soft magnetic ferrite of dosage has manganese-zinc ferrite, nickel-zinc ferrite, MgZn ferrite etc., wherein
Manganese-zinc ferrite bulk permeability highest, usage range are most wide.
Number of patent application 201610833212.7 discloses the system of a kind of iron sial/ferrite composite magnetic powder and its powder core
Preparation Method.The following steps are included: preparing the Fe-Si-Al magnetic of flattening first, then Fe-Si-Al magnetic is placed in Fe-Zn-Mn and is mixed
In nitrate solution, by hydro-thermal reaction in flat Fe-Si-Al magnetic surface in situ synthesizing of ferrite clad, by washing
With, with binder, mix lubricant, iron sial/ferrite composite magnetic powder is cold-pressed into powder core, then destressing is moved back after drying
Fire.
Number of patent application 201210034964.9 discloses a kind of neodymium doping manganese-zinc ferrite-polyaniline compound wave-absorbing material
Preparation method, the invention is according to Mn0.4Zn0.6NdxFe2-xO4The stoichiometric of (x=0.025 ~ 0.1), using chemical coprecipitation
Area method prepares the different neodymium doping manganese-zinc ferrite of doping；Then with the quality of neodymium doping manganese-zinc ferrite and aniline monomer
Than 1 ~ 4:20, (5 ~ 20%) neodymium doping manganese-zinc ferrite-polyaniline compound wave-absorbing material is prepared using in-situ compositing.
Number of patent application 201610452875.4 discloses a kind of ultrathin flexible electromagnetic shielding film and preparation method thereof.This hair
Bright to prepare conductive-nano-fibers film by electrostatic spinning technique, product is made of fibre-forming polymer and functional nanoparticles；
Or it is made of fibre-forming polymer, conducting polymer and functional nanoparticles.
Number of patent application 201510621819.4 discloses kind of a carbon nanotubes net base layer of resin shape electromagnetic shielding material, packet
At least one layer of conductive layer is included, conductive layer is the carbon nano-tube network made of carbon nanotube；Conductive layer both side surface is respectively equipped with viscous
Tie oxidant layer；Adhesive layer is to contain the resin of magnetic ferrites particle as binder；Resin includes thermosetting resin, thermoplasticity
Resin；Thermosetting resin includes epoxy resin, phenolic resin, unsaturated polyester resin；Thermoplastic resin includes polyethylene, poly- third
Alkene, nylon, polyester, ABS resin.
It can be seen that the soft magnetic ferrite in the prior art for electromagnetic shielding is equal, it is generally raw using ceramic process
It produces, haves the defects that product is very hard and crisp, cause it to collide in use and easily damage, when some product requirements are very thin
Using being restricted, and the performance of existing flexible electromagnetic shielding material is undesirable.
Summary of the invention
Effectively to solve above-mentioned technical problem, it is multiple that the invention proposes a kind of flexible soft magnetic ferrites for electromagnetic shielding
Condensation material and preparation method can effectively improve the flexibility of magnetic ferrite material, and initial permeability is high, effectiveness
It is good.
The specific technical solution of the present invention is as follows:
A kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding, the composite material is more by hydrochloric acid
Bar amine in-situ polymerization forms clad in manganese-zinc ferrite core powder surface, then uniform and hot-forming with rubber mix
And it is made, specific preparation step are as follows:
A, trihydroxy methyl amino silane is dissolved in deionized water, dilute hydrochloric acid is then added and adjusts pH value, then by manganese-zinc ferrite
Magnetic core is ground into powder addition system, adds dehydrated alcohol, and ultrasonic disperse forms mixed solution；
B, Dopamine hydrochloride is added in mixed solution made from step a, heating stirring reaction, then is centrifuged, washs, dries,
The manganese-zinc ferrite of poly-dopamine cladding is made；
C, the manganese-zinc ferrite of the cladding of poly-dopamine made from step b and rubber mix is uniform, it injects in mold, is hot pressed into
The flexible soft magnetic ferrite composite material for electromagnetic shielding is made in type.
Preferably, in the step a, pH value is adjusted to 7.5 ~ 9.5.
Preferably, in the step a, 3 ~ 5 parts by weight of trihydroxy methyl amino silane, manganese-zinc ferrite core powder 30 ~ 40
Parts by weight, 6 ~ 10 parts by weight of dehydrated alcohol, 45 ~ 61 parts by weight of deionized water.
Preferably, in the step a, the ultrasonic power density of ultrasonic disperse is 0.5 ~ 1W/cm2, the time be 20 ~
40min。
Preferably, in the step b, 12 ~ 25 parts by weight of Dopamine hydrochloride, 75 ~ 88 parts by weight of mixed solution.
Preferably, in the step b, the temperature being stirred to react is 80 ~ 90 DEG C, and the time is 3 ~ 5h.
Preferably, in the step c, rubber is natural rubber, ethylene propylene diene rubber, butyl rubber, nitrile rubber, butylbenzene
One of rubber.
Preferably, in the step c, 20 ~ 30 parts by weight of manganese-zinc ferrite, 70 ~ 80 weight of rubber of poly-dopamine cladding
Part.
Preferably, in the step c, hot-forming temperature is 130 ~ 160 DEG C, and pressure is 3 ~ 5MPa, and the dwell time is
10~20s。
Dopamine can occur to aoxidize self-polymeric reaction under the conditions of weak base, in organic and inorganic materials surface successful deposition DOPA
Amine coating improves the surface-active of material, and the dopamine coating of material surface can be used as secondary function platform, by Michael plus
At or the compound of schiff base reaction and C-terminal and amino terminal carry out page turning, assign the more performances of material.The present invention is logical
It crosses MnZn ferrite material surface and is successfully introduced into functional group (hydroxyl and amino) after DOPA is amine-modified and not only provides and continue instead
The active group answered, and increase the compatibility between manganese-zinc ferrite and rubber.
Above content of the present invention also proposes a kind of flexible soft magnetic ferrite composite material for electromagnetic shielding, by following step
It is rapid to be made: a, pH value will be adjusted in trihydroxy methyl amino silane, manganese-zinc ferrite core powder, dehydrated alcohol addition deionized water,
Form mixed solution；B, Dopamine hydrochloride and heating stirring reaction is added, the manganese-zinc ferrite of poly-dopamine cladding is made；C, with
Rubber mix inject mold after it is hot-forming to get.
The invention has the benefit that
1. proposing the flexible soft magnetic ferrite composite material using the amine-modified manganese-zinc ferrite preparation of DOPA for electromagnetic shielding
Method.
2. the present invention can be uniformly dispersed in rubber by the manganese-zinc-ferrite powder of modification activation, product obtained
Initial permeability it is high, can satisfy electromagnetic shielding and electromagnetism interference conventional design demand under room temperature.
3. product flexibility produced by the present invention is good, easy to process, it is hardly damaged, can be used for lining, the nothing of radiation protection clothing
Line charge mobile phone receiving end, electromagnetic shielding test cabinet, household Radiation-roof wallpaper etc..
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A, trihydroxy methyl amino silane is dissolved in deionized water, it is 8.5 that dilute hydrochloric acid, which is then added, and adjusts pH value, then by MnZn iron
Ferrite core is ground into powder addition system, adds dehydrated alcohol, and ultrasonic disperse forms mixed solution, and ultrasonic disperse surpasses
Acoustic power density is 0.8W/cm2, time 30min；Wherein, 4 parts by weight of trihydroxy methyl amino silane, manganese-zinc ferrite magnetic
35 parts by weight of core powder, 8 parts by weight of ethyl alcohol, 53 parts by weight of deionized water；
B, Dopamine hydrochloride is added in mixed solution made from step a, heating stirring reaction, the temperature being stirred to react is 85
DEG C, time 4h, then be centrifuged, wash, dry, the manganese-zinc ferrite of poly-dopamine cladding is made；Wherein, 18 weight of Dopamine hydrochloride
Measure part, 82 parts by weight of mixed solution；
C, the manganese-zinc ferrite that poly-dopamine made from step b coats is uniformly mixed with natural rubber, is injected in mold, hot pressing
Molding, hot-forming temperature are 145 DEG C, pressure 4MPa, dwell time 15s, are made soft for the flexibility of electromagnetic shielding
Magnetic ferrites composite material；Wherein, 25 parts by weight of manganese-zinc ferrite, 75 parts by weight of rubber of poly-dopamine cladding.
Embodiment 2
A, trihydroxy methyl amino silane is dissolved in deionized water, it is 8 that dilute hydrochloric acid, which is then added, and adjusts pH value, then by manganese-zinc ferrite
Body magnetic core is ground into powder addition system, adds dehydrated alcohol, and ultrasonic disperse forms mixed solution, the ultrasound of ultrasonic disperse
Wave power density is 0.6W/cm2, time 36min；Wherein, 3 parts by weight of trihydroxy methyl amino silane, manganese-zinc ferrite core
33 parts by weight of powder, 7 parts by weight of ethyl alcohol, 57 parts by weight of deionized water；
B, Dopamine hydrochloride is added in mixed solution made from step a, heating stirring reaction, the temperature being stirred to react is 82
DEG C, time 4.5h, then be centrifuged, wash, dry, the manganese-zinc ferrite of poly-dopamine cladding is made；Wherein, Dopamine hydrochloride 15
Parts by weight, 85 parts by weight of mixed solution；
C, the manganese-zinc ferrite that poly-dopamine made from step b coats is uniformly mixed with ethylene propylene diene rubber, is injected in mold,
Hot-forming, hot-forming temperature is 140 DEG C, pressure 3.5MPa, dwell time 18s and is made for electromagnetic shielding
Flexible soft magnetic ferrite composite material；Wherein, 23 parts by weight of manganese-zinc ferrite, 77 parts by weight of rubber of poly-dopamine cladding.
Embodiment 3
A, trihydroxy methyl amino silane is dissolved in deionized water, it is 7.5 that dilute hydrochloric acid, which is then added, and adjusts pH value, then by MnZn iron
Ferrite core is ground into powder addition system, adds dehydrated alcohol, and ultrasonic disperse forms mixed solution, and ultrasonic disperse surpasses
Acoustic power density is 0.5W/cm2, time 40min；Wherein, 3 parts by weight of trihydroxy methyl amino silane, manganese-zinc ferrite magnetic
30 parts by weight of core powder, 6 parts by weight of ethyl alcohol, 61 parts by weight of deionized water；
B, Dopamine hydrochloride is added in mixed solution made from step a, heating stirring reaction, the temperature being stirred to react is 80
DEG C, time 5h, then be centrifuged, wash, dry, the manganese-zinc ferrite of poly-dopamine cladding is made；Wherein, 12 weight of Dopamine hydrochloride
Measure part, 88 parts by weight of mixed solution；
C, the manganese-zinc ferrite that poly-dopamine made from step b coats is uniformly mixed with butyl rubber, is injected in mold, hot pressing
Molding, hot-forming temperature are 130 DEG C, pressure 3MPa, dwell time 20s, are made soft for the flexibility of electromagnetic shielding
Magnetic ferrites composite material；Wherein, 20 parts by weight of manganese-zinc ferrite, 80 parts by weight of rubber of poly-dopamine cladding.
Embodiment 4
A, trihydroxy methyl amino silane is dissolved in deionized water, it is 9 that dilute hydrochloric acid, which is then added, and adjusts pH value, then by manganese-zinc ferrite
Body magnetic core is ground into powder addition system, adds dehydrated alcohol, and ultrasonic disperse forms mixed solution, the ultrasound of ultrasonic disperse
Wave power density is 0.9W/cm2, time 28min；Wherein, 5 parts by weight of trihydroxy methyl amino silane, manganese-zinc ferrite core
36 parts by weight of powder, 9 parts by weight of ethyl alcohol, 50 parts by weight of deionized water；
B, Dopamine hydrochloride is added in mixed solution made from step a, heating stirring reaction, the temperature being stirred to react is 88
DEG C, time 3.5h, then be centrifuged, wash, dry, the manganese-zinc ferrite of poly-dopamine cladding is made；Wherein, Dopamine hydrochloride 22
Parts by weight, 78 parts by weight of mixed solution；
C, the manganese-zinc ferrite that poly-dopamine made from step b coats is uniformly mixed with nitrile rubber, is injected in mold, hot pressing
Molding, hot-forming temperature are 150 DEG C, pressure 4.5MPa, dwell time 13s and the flexibility for electromagnetic shielding are made
Soft magnetic ferrite composite material；Wherein, 28 parts by weight of manganese-zinc ferrite, 72 parts by weight of rubber of poly-dopamine cladding.
Embodiment 5
A, trihydroxy methyl amino silane is dissolved in deionized water, it is 9.5 that dilute hydrochloric acid, which is then added, and adjusts pH value, then by MnZn iron
Ferrite core is ground into powder addition system, adds dehydrated alcohol, and ultrasonic disperse forms mixed solution, and ultrasonic disperse surpasses
Acoustic power density is 1W/cm2, time 20min；Wherein, 5 parts by weight of trihydroxy methyl amino silane, manganese-zinc ferrite core
40 parts by weight of powder, 10 parts by weight of ethyl alcohol, 45 parts by weight of deionized water；
B, Dopamine hydrochloride is added in mixed solution made from step a, heating stirring reaction, the temperature being stirred to react is 90
DEG C, time 3h, then be centrifuged, wash, dry, the manganese-zinc ferrite of poly-dopamine cladding is made；Wherein, 25 weight of Dopamine hydrochloride
Measure part, 75 parts by weight of mixed solution；
C, the manganese-zinc ferrite that poly-dopamine made from step b coats is uniformly mixed with butadiene-styrene rubber, is injected in mold, hot pressing
Molding, hot-forming temperature are 160 DEG C, pressure 5MPa, and the flexible soft magnetism for electromagnetic shielding is made in the dwell time 10
Ferrite composite material；Wherein, 30 parts by weight of manganese-zinc ferrite, 70 parts by weight of rubber of poly-dopamine cladding.
Comparative example 1
A, trihydroxy methyl amino silane is dissolved in deionized water, it is 8.5 that dilute hydrochloric acid, which is then added, and adjusts pH value, then by MnZn iron
Ferrite core is ground into powder addition system, adds dehydrated alcohol, and ultrasonic disperse forms mixed solution, and ultrasonic disperse surpasses
Acoustic power density is 0.8W/cm2, time 30min；Wherein, 4 parts by weight of trihydroxy methyl amino silane, manganese-zinc ferrite magnetic
35 parts by weight of core powder, 8 parts by weight of ethyl alcohol, 53 parts by weight of deionized water；
B, by mixed solution heating stirring made from step a, the temperature being stirred to react is 85 DEG C, time 4h, then is centrifuged, washes
It washs, dry, manganese-zinc ferrite is made；
C, manganese-zinc ferrite made from step b is uniformly mixed with natural rubber, is injected in mold, it is hot-forming, it is hot-forming
Temperature be 145 DEG C, pressure 4MPa, dwell time 15s, the soft magnetic ferrite composite material for electromagnetic shielding is made；
Wherein, 25 parts by weight of manganese-zinc ferrite, 75 parts by weight of rubber.
Soft magnetic ferrite composite material made from above-described embodiment 1 ~ 5 and comparative example 1, tests its initial permeability, folding
Number, method or the condition for testing characterization are as follows:
Initial permeability: any soft magnetic ferrite composite material produced by the present invention is taken, using Changzhou Tong Hui TH2817 type LCR number
The inductance of word bridge test sample, thus corresponding initial permeability at calculating.
Soft magnetic ferrite composite material produced by the present invention: being cut into the sample of 13cm × 3cm by folding number (flexibility),
Tested using MK-NZ-C anti-bending detector, test angle be 180 °, bending speed be 30 times/min, testing load 300g,
Folding stroke 6cm, the folding number of test sample.
The results are shown in Table 1.
Table 1:
Claims (10)
1. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding, it is characterised in that: described compound
Material be by Dopamine hydrochloride in-situ polymerization, manganese-zinc ferrite core powder surface formed clad, then with rubber mix
It is uniform and hot-forming and obtained, specific preparation step are as follows:
A, trihydroxy methyl amino silane is dissolved in deionized water, dilute hydrochloric acid is then added and adjusts pH value, then by manganese-zinc ferrite
Magnetic core is ground into powder addition system, adds dehydrated alcohol, and ultrasonic disperse forms mixed solution；
B, Dopamine hydrochloride is added in mixed solution made from step a, heating stirring reaction, then is centrifuged, washs, dries,
The manganese-zinc ferrite of poly-dopamine cladding is made；
C, the manganese-zinc ferrite of the cladding of poly-dopamine made from step b and rubber mix is uniform, it injects in mold, is hot pressed into
The flexible soft magnetic ferrite composite material for electromagnetic shielding is made in type.
2. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding according to claim 1,
Be characterized in that: in the step a, pH value is adjusted to 7.5 ~ 9.5.
3. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding according to claim 1,
Be characterized in that: in the step a, 3 ~ 5 parts by weight of trihydroxy methyl amino silane, 30 ~ 40 parts by weight of manganese-zinc ferrite core powder,
6 ~ 10 parts by weight of dehydrated alcohol, 45 ~ 61 parts by weight of deionized water.
4. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding according to claim 1,
Be characterized in that: in the step a, the ultrasonic power density of ultrasonic disperse is 0.5 ~ 1W/cm2, the time is 20 ~ 40min.
5. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding according to claim 1,
It is characterized in that: in the step b, 12 ~ 25 parts by weight of Dopamine hydrochloride, 75 ~ 88 parts by weight of mixed solution.
6. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding according to claim 1,
Be characterized in that: in the step b, the temperature being stirred to react is 80 ~ 90 DEG C, and the time is 3 ~ 5h.
7. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding according to claim 1,
Be characterized in that: in the step c, rubber is natural rubber, in ethylene propylene diene rubber, butyl rubber, nitrile rubber, butadiene-styrene rubber
One kind.
8. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding according to claim 1,
It is characterized in that: in the step c, 20 ~ 30 parts by weight of manganese-zinc ferrite, 70 ~ 80 parts by weight of rubber of poly-dopamine cladding.
9. a kind of preparation method of the flexible soft magnetic ferrite composite material for electromagnetic shielding according to claim 1,
Be characterized in that: in the step c, hot-forming temperature is 130 ~ 160 DEG C, and pressure is 3 ~ 5MPa, and the dwell time is 10 ~ 20s.
10. a kind of flexible soft magnetic ferrite for electromagnetic shielding that any one of claim 1 ~ 9 the method is prepared is multiple
Condensation material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479435A (en) * | 2021-12-30 | 2022-05-13 | 昆山科运新型工程材料科技有限公司 | Preparation method of electromagnetic shielding magnetic-conducting polymer alloy and product thereof |
| CN114654823A (en) * | 2022-03-29 | 2022-06-24 | 重庆科技学院 | Mn-Zn ferrite-FeSiAl composite wave-absorbing material and preparation method thereof |
| CN114775267A (en) * | 2022-04-12 | 2022-07-22 | 南通大学 | Electromagnetic shielding non-woven fabric and preparation method thereof |
-
2018
- 2018-10-22 CN CN201811228784.8A patent/CN109400958A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114479435A (en) * | 2021-12-30 | 2022-05-13 | 昆山科运新型工程材料科技有限公司 | Preparation method of electromagnetic shielding magnetic-conducting polymer alloy and product thereof |
| CN114654823A (en) * | 2022-03-29 | 2022-06-24 | 重庆科技学院 | Mn-Zn ferrite-FeSiAl composite wave-absorbing material and preparation method thereof |
| CN114775267A (en) * | 2022-04-12 | 2022-07-22 | 南通大学 | Electromagnetic shielding non-woven fabric and preparation method thereof |
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