CN109952013A - A kind of spiral shape electromagnetic shielding material and preparation method thereof - Google Patents
A kind of spiral shape electromagnetic shielding material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of spiral shape electromagnetic shielding materials and preparation method thereof.The electromagnetic shielding material modifies manganese carbonate on cotton fiber surface using the cotton fiber with similar DNA helical structure as template, by dopamine, then in its in situ Polymerization doped polyaniline, is finally handled using ammonium hydroxide contra-doping.The present invention organically combines the spiral structure of similar DNA, the dielectric loss of the absorbing property of manganese carbonate, doped polyaniline, induces effectively multiple relaxation, interfacial polarization, multipath reflection phenomenon, spiral shape electromagnetic shielding material is made to have excellent electromagnet shield effect.In addition, the contra-doping processing of ammonium hydroxide makes material and air have good impedance matching property, and then the spiral shape electromagnetic shielding material is significantly promoted to electromagnetic energy absorption percentage.Spiral shape electromagnetic shielding material provided by the invention has the characteristics that shield ranges are wide, shield effectiveness is high, inexpensive, preparation process is simple.
Description
Technical field
The invention belongs to electro-magnetic screen function field of material technology, specifically, being related to a kind of electricity with helical structure
Magnetic shielding material and a kind of prepared by the method for dopamine auto polymerization and in situ chemical oxidative polymerization have spiral shape electromagnetism
The method of shielding material.
Background technique
With the fast development of modern electronics industry, more and more electronics, electrical equipment are widely used in medical, logical
The fields such as letter, business.A large amount of electromagnetic waves present in space not only will affect the normal operation of electronic equipment, also can be to the mankind
Health brings harm.Electromagnetic pollution has become sky gas and water, the 4th class pollution outside noise pollution.Use electromagnetic shielding material
Material is one of the effective measures for alleviating the above problem.
Traditional electromagnetic shielding material, such as metal material have the shortcomings that perishable, density is high, price is higher, limitation
Its application in some occasions.For other eigenstate organic conductive macromolecules, doped polyaniline has cost of material
Cheaply, the advantages that it is convenient to synthesize, good thermal stability and chemical stability, lossy microwave characteristic and excellent electromagnetic performance, quilt
It is considered most promising one of electromagnetic shielding material.Doped polyaniline is compound with other materials, the material of preparation
Can have many advantages, such as that light specific gravity, electromagnetic shielding performance are excellent, cost is relatively low in conjunction with the advantage between different component, be electromagnetic screen
Cover an important development direction of material.In addition, most of material with high electromagnet shield effect is due to material and air
Impedance mismatch causes relatively low (the Acs Applied Materials&Interfaces of the electromagnetic energy absorption percentage of material
2017,9,809-818.) the secondary pollution problem of electromagnetic wave, is caused to a certain extent.Therefore, developing has high electromagnetic energy
Absorption, high shield effectiveness, light, inexpensive electromagnetic shielding material have important practical value.
103450681 A of patent of invention CN discloses a kind of nickel plating spiral carbon nanotubes/polyaniline composite electromagnetic screen material
The preparation method of material.This kind of method after being sensitized, activating to it, is existed using spring like spiral carbon nanotubes as template using chemical plating
Its surface modification nickel particle, is then heat-treated it, sodium hydroxide solution stirring, after washing to neutrality, using situ aggregation method
Polyaniline is coated on its surface, hydrochloric acid solution secondary doping is finally used, it is multiple to obtain nickel plating spiral carbon nanotubes/polyaniline ternary
Close electromagnetic shielding material.This kind of method preparation process is relatively complicated, and spring-like structures of spiral carbon nano pipe and irregular,
The electromagnetic shielding performance of material is reduced to a certain extent.
Summary of the invention
A kind of that the object of the present invention is to provide shield effectiveness is high, electromagnetic energy absorption is strong spiral shape electromagnetic shielding material and
Preparation method.
Spiral shape electromagnetic shielding material provided by the invention, it is characterised in that the electromagnetic shielding material has similar
The helical structure of DNA.
Spiral shape electromagnetic shielding material provided by the invention, it is characterised in that the electromagnetic shielding material has multilayer knot
Structure；Outermost layer is doped polyaniline layer, and secondary outer layer is the manganese carbonate for being enclosed with poly-dopamine, and middle layer has helical structure
Cotton fiber.
Further, the length of used spiral shape cotton fiber is 3mm.
Further, the manganese carbonate is sheet, lamellar spacing 20nm, partial size 850nm.
Further, the thickness in monolayer of the manganese carbonate for being enclosed with poly-dopamine is 2~5 μm, the doped polyaniline layer
Thickness in monolayer be 3~10 μm.
Further, the electromagnetic shielding material is handled by ammonium hydroxide contra-doping.
Further, the electromagnetic shielding material is handled by ammonium hydroxide contra-doping, and the concentration of the ammonium hydroxide is 1~
10wt.%.
Further, the electromagnetic shielding material is handled by ammonium hydroxide contra-doping, and the processing time is 3~20s.
The preparation method of above-mentioned spiral shape electromagnetic shielding material, by means of dopamine auto polymerization and in situ chemical oxidative polymerization
Method constructs multilayered structure, specifically comprises the following steps:
(1) buffer solution for the use of trishydroxymethylaminomethane and hydrochloric acid configuration pH value being 8.5；Spiral cotton is fine
Buffer solution is added in dimension, manganese carbonate and Dopamine hydrochloride, reacts 1~4h at room temperature；Cotton fiber containing in buffer solution
Amount is 2g/L, and content of the manganese carbonate in buffer solution is 0.5~4g/L, and content of the Dopamine hydrochloride in buffer solution is
1.5g/L；After completion of the reaction, reactant is filtered and washed, product is denoted as A；
(2) product A and aniline monomer are dispersed in the sulfuric acid solution of 1mol/L, are denoted as solution α, A is in solution α
Content be 4g/L, A and aniline monomer mass ratio are between 1:1 and 1:4；The potassium permanganate sulfuric acid of the 1mol/L of 100ml is molten
Drop enters in the solution α of 100ml, and polymerization reaction occurs at -5 DEG C, and the reaction time is 3~6h；
(3) after completion of the reaction, reaction product is filtered, 3~20s is impregnated in the ammonium hydroxide that concentration is 1~10wt.%；It crosses
It after filter, is dried in vacuo, spiral shape electromagnetic shielding material is obtained after grinding distribution.
Beneficial effects of the present invention:
Spiral shape electromagnetic shielding material provided by the present invention uses multilayered structure: outermost layer is doped polyaniline layer, secondary
Outer layer is the manganese carbonate layer for being enclosed with poly-dopamine, and middle layer is cotton fiber.The present invention is first by dopamine by manganese carbonate
On the one hand modification is played in the cotton fiber surface with similar DNA helical structure, the poly-dopamine for being coated on manganese carbonate surface
The effect of protective layer, when avoiding modification aniline, acid reaction system destroys the decomposition of manganese carbonate；Poly-dopamine surface simultaneously
Two phenolic hydroxyl group of neighbour, amino groups increase the suction-operated between aniline monomer, make polyaniline grafting with higher
Density, it is final to obtain the electromagnetic shielding material with helical structure.The present invention is by the spiral structure of the similar DNA of material, carbonic acid
The dielectric loss of the absorbing property of manganese, doped polyaniline organically combines；Manganese carbonate plays the role of polarization center, and material internal is each
The presence at multiple interface between component, can trigger multiple dielectric relaxation effect, and the helical structure of bond material makes electromagnetic wave in material
Material is internal to be effectively formed multipath reflection, improves the electromagnet shield effect of material.In addition, being dropped using the mode of ammonium hydroxide contra-doping
The low-doped outermost conductivity of polyaniline makes material have better impedance matching property, and irradiation is made to arrive the electromagnetic wave of material
It is easier to enter material internal, and then enhances material to the percent absorption of electromagnetic energy.Due to electromagnetic screen provided by the invention
Covering material has the characteristics that above structure, material integrally electromagnet shield effect with higher and high electromagnetic energy absorption percentage
Advantage.Electromagnetic shielding material provided by the invention is to eliminate in the practical engineering application for need high electromagnetic energy absorption technically
Obstacle.Meanwhile the material for being firmly combined between material component of the invention, thus being obtained is hardly damaged failure, has and uses the longevity
Order long feature.In addition, method of the invention has, simple process, that production cost is low, is easy to large-scale industrial production etc. is excellent
Point can be applied to the electro-magnetic screen function field for requiring high electromagnetic energy absorption.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of spiral shape electromagnetic shielding material prepared by the present invention.
The scanning electron microscope diagram piece of spiral shape electromagnetic shielding material prepared by Fig. 2 embodiment of the present invention 1.
The electromagnet shield effect of spiral shape electromagnetic shielding material prepared by Fig. 3 embodiment of the present invention 1 in 8.2~12.4GHz
Figure.
Specific embodiment
In order to illustrate more clearly of technical solution of the present invention, be briefly described with reference to the accompanying drawings and examples, show and
Easy insight, drawings discussed below and embodiment, for those of ordinary skill in the art, what is do not made the creative labor
Under the premise of, other technical solutions can also be obtained.But it is any to be equal or similar technical solution belongs to this with of the invention
Invent the range of protection.
Embodiment 1:
The buffer solution for the use of trishydroxymethylaminomethane and hydrochloric acid configuration pH value being 8.5；By spiral cotton fiber,
Buffer solution is added in manganese carbonate and Dopamine hydrochloride, reacts 4h at room temperature；Content of the cotton fiber in buffer solution is 2g/
L, content of the manganese carbonate in buffer solution are 4g/L, and content of the Dopamine hydrochloride in buffer solution is 1.5g/L；It has reacted
Reactant is filtered and washed by Bi Hou, and product is denoted as A.
Product A and aniline monomer are dispersed in the sulfuric acid solution of 1mol/L, are denoted as solution α, A is in solution α
Content is 4g/L, and content of the aniline monomer in solution α is 16g/L；The potassium permanganate sulfuric acid solution of the 1mol/L of 100ml is dripped
Enter in the solution α of 100ml, oxidative polymerization, reaction time 6h occur at -5 DEG C.
After completion of the reaction, it after reaction product being filtered, is immersed in the ammonium hydroxide that concentration is 7wt.% and impregnates 10s；After filtering, very
Sky is dry, and spiral shape electromagnetic shielding material is obtained after grinding distribution.The structural schematic diagram of material is as shown in Figure 1.Scanning electron
Microscopical picture is as shown in Figure 2.Material is pressed into the thin slice of 0.4mm, test material is in the case where frequency is 8.2~12.4GHz
Electromagnet shield effect be 97dB or so (as shown in Figure 3), electromagnetic energy absorption percentage is 98% or so.Show this kind of method
The electromagnetic shielding material of preparation has good electromagnet shield effect and excellent electromagnetic energy absorption percentage.By the electricity of material
Magnetic screen efficiency and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 2:
Method such as embodiment 1, is changed to 3s for ammonium hydroxide soaking time.Such spiral shape electromagnetic shielding material is tested in electromagnetic wave
Electromagnet shield effect under frequency is 8.2~12.4GHz is 97dB or so, and electromagnetic energy absorption percentage is 94% or so.It will
The electromagnet shield effect and electromagnetic energy absorption percentage of material are listed in Table 1 below.
Embodiment 3:
Method such as embodiment 1, is changed to 20s for ammonium hydroxide soaking time.Such spiral shape electromagnetic shielding material is tested in electromagnetism
Electromagnet shield effect under wave frequency rate is 8.2~12.4GHz is 94dB or so, and electromagnetic energy absorption percentage is 95% or so.
The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 4:
Ammonia concn is changed to 1wt.% by method such as embodiment 1, and ammonium hydroxide soaking time is changed to 20s.Test such spiral shape
Electromagnet shield effect of the electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is 96dB or so, electromagnetic energy absorption
Percentage is 92% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 5:
Ammonia concn is changed to 10wt.% by method such as embodiment 1, and ammonium hydroxide soaking time is changed to 20s.Test such spiral
Electromagnet shield effect of the shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is 94dB or so, and electromagnetic energy is inhaled
Receiving percentage is 96% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 6:
Ammonia concn is changed to 10wt.% by method such as embodiment 1, and ammonium hydroxide soaking time is changed to 10s.Test such spiral
Electromagnet shield effect of the shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is 85dB or so, and electromagnetic energy is inhaled
Receiving percentage is 97% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 7:
Ammonia concn is changed to 1wt.% by method such as embodiment 1, and ammonium hydroxide soaking time is changed to 3s.Test such spiral shape
Electromagnet shield effect of the electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is 96dB or so, electromagnetic energy absorption
Percentage is 82% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 8:
Method such as embodiment 1, is changed to 0.5g/L for carbonic acid manganese content；Ammonia concn is changed to 1wt.%, ammonium hydroxide soaking time
It is changed to 3s.Testing electromagnet shield effect of such spiral shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is
80dB or so, electromagnetic energy absorption percentage are 83% or so.By the electromagnet shield effect of material and electromagnetic energy absorption percentage
Than being listed in Table 1 below.
Embodiment 9:
Method such as embodiment 8, is changed to 2h for the reaction time of dopamine at room temperature.Test such spiral shape electromagnetic shielding material
Expect that the electromagnet shield effect in the case where wave frequency is 8.2~12.4GHz is 83dB or so, electromagnetic energy absorption percentage is
85% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 10:
Method such as embodiment 8, is changed to 1h for the reaction time of dopamine at room temperature；Aniline content is changed to 4g/L, polyaniline
Reaction time be changed to 3h.Test electromagnetism of such spiral shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz
Shield effectiveness is 78dB or so, and electromagnetic energy absorption percentage is 87% or so.By the electromagnet shield effect and electromagnetic energy of material
Amount percent absorption is listed in Table 1 below.
Embodiment 11:
Method such as embodiment 10, is changed to 2h for the reaction time of dopamine at room temperature.Test such spiral shape electromagnetic shielding
Electromagnet shield effect of the material in the case where wave frequency is 8.2~12.4GHz is 94dB or so, and electromagnetic energy absorption percentage is
93% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 12:
Method such as embodiment 10, is changed to 2h for the reaction time of dopamine at room temperature；Ammonia concn is changed to 8wt.%.Test
Electromagnet shield effect of such spiral shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is 68dB or so, electricity
Magnetic energy percent absorption is 90% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 13:
Method such as embodiment 10, is changed to 7wt.% for ammonia concn.Such spiral shape electromagnetic shielding material is tested in electromagnetism
Electromagnet shield effect under wave frequency rate is 8.2~12.4GHz is 67dB or so, and electromagnetic energy absorption percentage is 86% or so.
The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 14:
Method such as embodiment 10, is changed to 2h for the reaction time of dopamine at room temperature.Test such spiral shape electromagnetic shielding
Electromagnet shield effect of the material in the case where wave frequency is 8.2~12.4GHz is 69dB or so, and electromagnetic energy absorption percentage is
84% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 15:
Ammonia concn is changed to 10wt.% by method such as embodiment 10, and ammonium hydroxide soaking time is changed to 7s.Test such spiral
Electromagnet shield effect of the shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is 62dB or so, and electromagnetic energy is inhaled
Receiving percentage is 85% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 16:
Method such as embodiment 10, is changed to 2g/L for carbonic acid manganese content, the reaction time of dopamine is changed to 2h at room temperature；Polyphenyl
The reaction time of amine is changed to 5h；Ammonia concn is changed to 8wt.%, and ammonium hydroxide soaking time is changed to 15s.Test such spiral shape electromagnetism
Electromagnet shield effect of the shielding material in the case where wave frequency is 8.2~12.4GHz is 90dB or so, electromagnetic energy absorption percentage
Than being 87% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 17:
Method such as embodiment 10, is changed to 2g/L for carbonic acid manganese content；Aniline content is changed to 6g/L, and the reaction time is changed to 6h；
Ammonia concn is changed to 7wt.%, and ammonium hydroxide soaking time is changed to 12s.Such spiral shape electromagnetic shielding material is tested in wave frequency
It is 87dB or so for the electromagnet shield effect under 8.2~12.4GHz, electromagnetic energy absorption percentage is 89% or so.By material
Electromagnet shield effect and electromagnetic energy absorption percentage be listed in Table 1 below.
Embodiment 18:
Method such as embodiment 17, is changed to 4g/L for aniline content.Such spiral shape electromagnetic shielding material is tested in electromagnetic wave
Electromagnet shield effect under frequency is 8.2~12.4GHz is 91dB or so, and electromagnetic energy absorption percentage is 90% or so.It will
The electromagnet shield effect and electromagnetic energy absorption percentage of material are listed in Table 1 below.
Embodiment 19:
Method such as embodiment 17, is changed to 5h for the reaction time of polyaniline；Ammonium hydroxide soaking time is changed to 15s.It tests such
Electromagnet shield effect of the spiral shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is 85dB or so, electromagnetic energy
Measuring percent absorption is 87% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Embodiment 20:
Ammonia concn is changed to 8wt.% by method such as embodiment 17, and ammonium hydroxide soaking time is changed to 15s.Test such spiral
Electromagnet shield effect of the shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz is 86dB or so, and electromagnetic energy is inhaled
Receiving percentage is 88% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Comparative example 1
Method such as embodiment 1, but directly it is tested, is not used after coating-doping polyaniline on the surface of the material
The processing of ammonium hydroxide contra-doping.Test electromagnetic screen of such spiral shape electromagnetic shielding material in the case where wave frequency is 8.2~12.4GHz
Efficiency 96dB or so is covered, electromagnetic energy absorption percentage is 34% or so.The electromagnet shield effect of material and electromagnetic energy are inhaled
Percentage is received to be listed in Table 1 below.
Comparative example 2
The material of preparation, is pressed into the thin slice of 0.4mm, is tested by method such as patent of invention CN 103450681A.It surveys
Try electromagnet shield effect 36dB or so of such material in the case where wave frequency is 8.2~12.4GHz, electromagnetic energy absorption percentage
Than being 28% or so.The electromagnet shield effect of material and electromagnetic energy absorption percentage are listed in Table 1 below.
Pass through Examples 1 to 20, it can be seen that spiral shape electromagnetic shielding material electromagnetism with higher disclosed by the invention
Shield effectiveness and electromagnetic energy absorption percentage.
Through embodiment 1 compared with comparative example 1, it can be seen that the electromagnetic shielding material of ammonium hydroxide contra-doping processing is not used
Though electromagnet shield effect do not have significant change, electromagnetic energy absorption percentage is far below spiral shape electromagnetism disclosed by the invention
The electromagnetic energy absorption percentage of shielding material.
Through embodiment 1 compared with comparative example 2, it can be seen that the material of similar DNA helical structure disclosed by the invention
With the electromagnet shield effect and electromagnetic energy absorption percentage for being much higher than prior art spring like helical structure.
1 the embodiment of the present invention of table and comparative example
Claims (10)
1. a kind of spiral shape electromagnetic shielding material, which is characterized in that have multilayered structure；Outermost layer is doped polyaniline layer, secondary
Outer layer is the manganese carbonate for being enclosed with poly-dopamine, and middle layer is the cotton fiber with helical structure, and the spiral shape is similar
The helical structure of DNA.
2. material according to claim 1, which is characterized in that the length of the spiral shape cotton fiber is 3mm.
3. material according to claim 1, which is characterized in that the manganese carbonate is sheet, lamellar spacing 20nm, partial size
For 850nm.
4. material according to claim 1, which is characterized in that the thickness in monolayer of the manganese carbonate for being enclosed with poly-dopamine
It is 2~5 μm, the thickness in monolayer of the doped polyaniline layer is 3~10 μm.
5. material according to claim 1, which is characterized in that the electromagnetic shielding material is by ammonium hydroxide contra-doping
Reason.
6. material according to claim 5, which is characterized in that the concentration of the ammonium hydroxide is 1~10wt.%.
7. material according to claim 5 or 6, which is characterized in that the processing time is 3~20s.
8. the preparation method of material described in claim 1, which comprises the steps of:
(1) buffer solution for the use of trishydroxymethylaminomethane and hydrochloric acid configuration pH value being 8.5；By spiral cotton fiber,
The buffer solution is added in manganese carbonate and Dopamine hydrochloride, reacts 1~4h at room temperature and after completion of the reaction carries out reactant
Filtering and washing, are denoted as A for product；
(2) product A and aniline monomer are dispersed in the sulfuric acid solution of 1mol/L, solution α are denoted as, by the 1mol/ of 100ml
The potassium permanganate sulfuric acid solution of L instills in the solution α of 100ml, occurs oxidative polymerization at -5 DEG C, and the reaction time is 3~
6h；
(3) after completion of the reaction, reaction product is filtered, 3~20s is impregnated in the ammonium hydroxide that concentration is 1~10wt.%；Filtering, very
Sky is dry, and grinding distribution is to get the spiral shape electromagnetic shielding material.
9. according to the method described in claim 8, it is characterized in that, cotton fiber described in step (1) is in buffer solution
Content is 2g/L, and content of the manganese carbonate in buffer solution is 0.5~4g/L, and the Dopamine hydrochloride is in buffer solution
Content be 1.5g/L.
10. according to the method described in claim 8, it is characterized in that, content of the A in solution α described in step (2) is 4g/
ML, A and aniline monomer mass ratio are between 1:1 and 1:4.
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