CN109952013B - Spiral electromagnetic shielding material and preparation method thereof - Google Patents
Spiral electromagnetic shielding material and preparation method thereof Download PDFInfo
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- CN109952013B CN109952013B CN201910268779.8A CN201910268779A CN109952013B CN 109952013 B CN109952013 B CN 109952013B CN 201910268779 A CN201910268779 A CN 201910268779A CN 109952013 B CN109952013 B CN 109952013B
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Abstract
The invention discloses a spiral electromagnetic shielding material and a preparation method thereof. The electromagnetic shielding material takes cotton fibers with a similar DNA spiral structure as templates, manganese carbonate is modified on the surfaces of the cotton fibers by means of dopamine, then polyaniline is polymerized and doped in situ on the surfaces of the cotton fibers, and finally ammonia water is used for counter-doping treatment. The invention organically combines the spiral structure similar to DNA, the wave absorbing performance of manganese carbonate and the dielectric loss of doped polyaniline to induce the phenomena of effective multiple relaxation, interface polarization and multiple reflection, so that the spiral electromagnetic shielding material has excellent electromagnetic shielding efficiency. In addition, the counter doping treatment of the ammonia water enables the material and the air to have good impedance matching characteristics, and the electromagnetic energy absorption percentage of the spiral electromagnetic shielding material is further greatly improved. The spiral electromagnetic shielding material provided by the invention has the characteristics of wide shielding range, high shielding efficiency, low price and simple preparation process.
Description
Technical Field
The invention belongs to the technical field of materials with electromagnetic shielding functions, and particularly relates to an electromagnetic shielding material with a spiral structure and a method for preparing the electromagnetic shielding material with the spiral structure by dopamine autopolymerization and in-situ chemical oxidative polymerization.
Background
With the rapid development of modern electronic industry, more and more electronic and electrical devices are widely used in the fields of medical treatment, communication, business and the like. The large amount of electromagnetic waves in the space not only can influence the normal operation of electronic equipment, but also can bring harm to the health of human beings. Electromagnetic pollution has become a fourth category of pollution beyond air, water, noise pollution. The use of electromagnetic shielding materials is one of the effective measures to alleviate the above problems.
The traditional electromagnetic shielding materials, such as metal materials, have the defects of easy corrosion, high density, high price and the like, and limit the application of the traditional electromagnetic shielding materials in some occasions. Compared with other intrinsic organic conductive polymers, doped polyaniline has the advantages of low price of raw materials, convenient synthesis, good thermal stability and chemical stability, excellent microwave loss characteristic and electromagnetic performance and the like, and is considered to be one of electromagnetic shielding materials with development prospects. The doped polyaniline is compounded with other materials, and the prepared material can combine the advantages of different components, has the advantages of light specific gravity, excellent electromagnetic shielding performance, lower cost and the like, and is an important development direction of electromagnetic shielding materials. In addition, most Materials with high electromagnetic shielding efficiency have low electromagnetic energy absorption percentage due to impedance mismatch between the material and air (Acs Applied Materials & Interfaces2017, 9, 809-818), and cause secondary pollution problem of electromagnetic wave to some extent. Therefore, the development of an electromagnetic shielding material with high electromagnetic energy absorption, high shielding efficiency, light weight and low cost has important practical value.
The invention patent CN 103450681A discloses a preparation method of a nickel-plated spiral carbon nanotube/polyaniline composite electromagnetic shielding material. The method comprises the steps of sensitizing and activating a spring-shaped spiral carbon nano tube serving as a template, modifying nickel particles on the surface of the spring-shaped spiral carbon nano tube by using chemical plating, then performing heat treatment on the nickel particles, stirring the nickel particles by using a sodium hydroxide solution, washing the nickel particles to be neutral, coating polyaniline on the surface of the nickel particles by using an in-situ polymerization method, and finally performing secondary doping by using a hydrochloric acid solution to obtain the nickel-plated spiral carbon nano tube/polyaniline ternary composite electromagnetic shielding material. The preparation process of the method is complicated, the spring-shaped structure of the spiral carbon nano tube is not regular, and the electromagnetic shielding performance of the material is reduced to a certain extent.
Disclosure of Invention
The invention aims to provide a spiral electromagnetic shielding material with high shielding efficiency and strong electromagnetic energy absorption and a preparation method thereof.
The spiral electromagnetic shielding material provided by the invention is characterized in that the electromagnetic shielding material has a spiral structure similar to DNA.
The spiral electromagnetic shielding material is characterized in that the electromagnetic shielding material has a multilayer structure; the outermost layer is a doped polyaniline layer, the secondary outer layer is manganese carbonate wrapped with polydopamine, and the middle layer is cotton fiber with a spiral structure.
Further, the length of the spiral cotton fiber used was 3 mm.
Further, the manganese carbonate is flaky, the thickness of a lamella is 20nm, and the particle size is 850 nm.
Further, the thickness of the single layer of the manganese carbonate wrapped with the polydopamine is 2-5 microns, and the thickness of the single layer of the doped polyaniline layer is 3-10 microns.
Further, the electromagnetic shielding material is subjected to ammonia back doping treatment.
Further, the electromagnetic shielding material is subjected to ammonia water back doping treatment, and the concentration of the ammonia water is 1-10 wt.%.
Further, the electromagnetic shielding material is subjected to ammonia water back doping treatment, and the treatment time is 3-20 s.
The preparation method of the spiral electromagnetic shielding material constructs a multilayer structure by means of dopamine autopolymerization and in-situ chemical oxidation polymerization, and specifically comprises the following steps:
(1) preparing a buffer solution with the pH value of 8.5 by using trihydroxymethyl aminomethane and hydrochloric acid; adding spiral cotton fibers, manganese carbonate and dopamine hydrochloride into a buffer solution, and reacting for 1-4 hours at room temperature; the content of the cotton fiber in the buffer solution is 2g/L, the content of manganese carbonate in the buffer solution is 0.5-4 g/L, and the content of dopamine hydrochloride in the buffer solution is 1.5 g/L; after the reaction is finished, filtering and washing the reactant, and marking the product as A;
(2) uniformly dispersing the product A and aniline monomer in 1mol/L sulfuric acid solution, marking as solution α, wherein the content of A in the solution α is 4g/L, and the mass ratio of A to aniline monomer is between 1: 1 and 1: 4;
(3) after the reaction is finished, filtering the reaction product, and soaking the reaction product in ammonia water with the concentration of 1-10 wt.% for 3-20 s; and filtering, drying in vacuum, and grinding and dispersing to obtain the spiral electromagnetic shielding material.
The invention has the beneficial effects that:
the spiral electromagnetic shielding material provided by the invention adopts a multilayer structure: the outermost layer is a doped polyaniline layer, the secondary outer layer is a manganese carbonate layer wrapped with polydopamine, and the middle layer is cotton fiber. Manganese carbonate is modified on the surface of cotton fiber with a similar DNA spiral structure by means of dopamine, and polydopamine coated on the surface of manganese carbonate plays a role of a protective layer, so that decomposition and damage of an acid reaction system to manganese carbonate are avoided when aniline is modified; meanwhile, the groups such as the hydroxyl group, the amino group and the like of the catechol on the surface of the polydopamine increase the adsorption effect with aniline monomers, so that the polyaniline layer has higher grafting density, and finally the electromagnetic shielding material with a spiral structure is obtained. The invention organically combines the spiral structure of the material similar to DNA, the wave absorbing performance of manganese carbonate and the dielectric loss of doped polyaniline; the manganese carbonate plays a role of a polarization center, multiple dielectric relaxation effects can be triggered due to the existence of multiple interfaces among all components in the material, and electromagnetic waves can effectively form multiple reflections in the material by combining the spiral structure of the material, so that the electromagnetic shielding efficiency of the material is improved. In addition, the conductivity of the outermost layer of doped polyaniline is reduced by using an ammonia water counter-doping mode, so that the material has better impedance matching characteristic, electromagnetic waves irradiated to the material can easily enter the material, and the absorption percentage of the material to electromagnetic energy is further enhanced. Because the electromagnetic shielding material provided by the invention has the structural characteristics, the whole material has the advantages of higher electromagnetic shielding efficiency and high electromagnetic energy absorption percentage. The electromagnetic shielding material provided by the invention eliminates technical obstacles for practical engineering application requiring high electromagnetic energy absorption. Meanwhile, the combination of the components of the material is firm, so that the obtained material is not easy to damage and lose efficacy, and has the characteristic of long service life. In addition, the method has the advantages of simple process, low production cost, easy large-scale industrial production and the like, and can be applied to the field of electromagnetic shielding function requiring high electromagnetic energy absorption.
Drawings
Fig. 1 is a schematic structural view of a spiral electromagnetic shielding material prepared according to the present invention.
FIG. 2 is a scanning electron microscope photograph of the spiral electromagnetic shielding material prepared in example 1 of the present invention.
FIG. 3 is a graph of electromagnetic shielding effectiveness of the spiral electromagnetic shielding material prepared in embodiment 1 of the present invention at 8.2 to 12.4 GHz.
Detailed Description
In order to more clearly illustrate the technical solution of the present invention, the following is briefly introduced with reference to the accompanying drawings and embodiments, and it is obvious that other technical solutions can be obtained by those skilled in the art without creative efforts. Any technical solutions equivalent or similar to the present invention are within the protection scope of the present invention.
Example 1:
preparing a buffer solution with the pH value of 8.5 by using trihydroxymethyl aminomethane and hydrochloric acid; adding spiral cotton fibers, manganese carbonate and dopamine hydrochloride into a buffer solution, and reacting for 4 hours at room temperature; the content of the cotton fiber in the buffer solution is 2g/L, the content of the manganese carbonate in the buffer solution is 4g/L, and the content of the dopamine hydrochloride in the buffer solution is 1.5 g/L; after the reaction was complete, the reaction was filtered and washed and the product was designated a.
uniformly dispersing the product A and aniline monomer in 1mol/L sulfuric acid solution, marking as solution α, wherein the content of A in the solution α is 4g/L, the content of aniline monomer in the solution α is 16g/L, dripping 100ml of 1mol/L potassium permanganate sulfuric acid solution into 100ml of the solution α, and carrying out oxidative polymerization reaction at-5 ℃ for 6 hours.
After the reaction is finished, filtering the reaction product, and soaking in 7 wt.% ammonia water for 10 s; and filtering, drying in vacuum, and grinding and dispersing to obtain the spiral electromagnetic shielding material. The schematic structure of the material is shown in fig. 1. A picture of a scanning electron microscope is shown in fig. 2. The material is pressed into a 0.4mm thin sheet, the electromagnetic shielding effectiveness of the tested material under the frequency of 8.2-12.4 GHz is about 97dB (as shown in figure 3), and the electromagnetic energy absorption percentage is about 98%. The electromagnetic shielding material prepared by the method has good electromagnetic shielding efficiency and excellent electromagnetic energy absorption percentage. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 2:
the procedure is as in example 1, changing the ammonia soaking time to 3 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 97dB and the electromagnetic energy absorption percentage is about 94% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 3:
the procedure is as in example 1, changing the ammonia soaking time to 20 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 94dB and the electromagnetic energy absorption percentage is about 95% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 4:
the method was as in example 1, with ammonia concentration changed to 1 wt.%, and ammonia soak time changed to 20 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 96dB and the electromagnetic energy absorption percentage is about 92% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 5:
the method was as in example 1, changing the ammonia concentration to 10 wt.%, and the ammonia soaking time to 20 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 94dB and the electromagnetic energy absorption percentage is about 96% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 6:
the method was as in example 1, with the ammonia concentration changed to 10 wt.%, and the ammonia soak time changed to 10 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 85dB and the electromagnetic energy absorption percentage is about 97 percent under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 7:
the method was as in example 1, changing the ammonia concentration to 1 wt.%, and the ammonia soaking time to 3 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 96dB and the electromagnetic energy absorption percentage is about 82% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 8:
the method is as in example 1, the manganese carbonate content is changed to 0.5 g/L; the ammonia concentration was changed to 1 wt.%, and the ammonia soaking time was changed to 3 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 80dB and the electromagnetic energy absorption percentage is about 83% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 9:
the procedure is as in example 8, changing the reaction time of dopamine at room temperature to 2 h. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 83dB and the electromagnetic energy absorption percentage is about 85% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 10:
the method is as in example 8, changing the reaction time of dopamine at room temperature to 1 h; the aniline content is changed to 4g/L, and the reaction time of polyaniline is changed to 3 h. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 78dB and the electromagnetic energy absorption percentage is about 87 percent under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 11:
the procedure is as in example 10, changing the reaction time of dopamine at room temperature to 2 h. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 94dB and the electromagnetic energy absorption percentage is about 93% when the electromagnetic wave frequency is 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 12:
the method is as in example 10, changing the reaction time of dopamine at room temperature to 2 h; the ammonia concentration was changed to 8 wt.%. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 68dB under the electromagnetic wave frequency of 8.2-12.4 GHz, and the electromagnetic energy absorption percentage is about 90%. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 13:
the procedure is as in example 10, changing the ammonia concentration to 7 wt.%. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 67dB and the electromagnetic energy absorption percentage is about 86% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 14:
the procedure is as in example 10, changing the reaction time of dopamine at room temperature to 2 h. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 69dB under the electromagnetic wave frequency of 8.2-12.4 GHz, and the electromagnetic energy absorption percentage is about 84%. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 15:
the method was as in example 10, with the ammonia concentration being changed to 10 wt.%, and the ammonia soaking time being changed to 7 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 62dB under the electromagnetic wave frequency of 8.2-12.4 GHz, and the electromagnetic energy absorption percentage is about 85%. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 16:
the method is as in example 10, the manganese carbonate content is changed to 2g/L, and the dopamine reaction time at room temperature is changed to 2 h; the reaction time of the polyaniline is changed to 5 h; the ammonia concentration was changed to 8 wt.%, and the ammonia soaking time was changed to 15 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 90dB and the electromagnetic energy absorption percentage is about 87% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 17:
the method is as in example 10, the manganese carbonate content is changed to 2 g/L; the aniline content is changed to 6g/L, and the reaction time is changed to 6 h; the ammonia concentration was changed to 7 wt.%, and the ammonia soaking time was changed to 12 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 87dB and the electromagnetic energy absorption percentage is about 89% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 18:
the procedure is as in example 17, but the aniline content is changed to 4 g/L. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 91dB under the electromagnetic wave frequency of 8.2-12.4 GHz, and the electromagnetic energy absorption percentage is about 90%. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 19:
the method is as in example 17, the reaction time of polyaniline is changed to 5 h; the ammonia soaking time was changed to 15 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 85dB and the electromagnetic energy absorption percentage is about 87 percent under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Example 20:
the method was as in example 17, changing the ammonia concentration to 8 wt.%, and the ammonia soaking time to 15 s. The electromagnetic shielding effectiveness of the spiral electromagnetic shielding material is about 86dB and the electromagnetic energy absorption percentage is about 88% under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Comparative example 1
The method is as in example 1, but the material surface is directly tested after being coated with the doped polyaniline layer without ammonia back doping treatment. The spiral electromagnetic shielding material is tested to have the electromagnetic shielding effectiveness of about 96dB and the electromagnetic energy absorption percentage of about 34 percent under the electromagnetic wave frequency of 8.2-12.4 GHz. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Comparative example 2
The method is as in patent CN 103450681A, the prepared material is pressed into 0.4mm thin sheets to be tested. The electromagnetic shielding effectiveness of the material is about 36dB under the electromagnetic wave frequency of 8.2-12.4 GHz, and the electromagnetic energy absorption percentage is about 28%. The electromagnetic shielding effectiveness and the percentage of electromagnetic energy absorption of the material are listed in table 1.
Through the embodiments 1-20, it can be seen that the spiral electromagnetic shielding material disclosed by the invention has higher electromagnetic shielding effectiveness and electromagnetic energy absorption percentage.
Comparing example 1 with comparative example 1, it can be seen that the electromagnetic shielding effectiveness of the electromagnetic shielding material without ammonia back doping treatment is not significantly changed, but the electromagnetic energy absorption percentage is much lower than that of the spiral electromagnetic shielding material disclosed in the present invention.
By comparing example 1 with comparative example 2, it can be seen that the disclosed DNA helix-like material has much higher electromagnetic shielding effectiveness and percentage of electromagnetic energy absorption than the prior art spring-like helix.
TABLE 1 examples of the invention and comparative examples
Claims (8)
1. A spiral electromagnetic shielding material, characterized by having a multilayer structure; the outermost layer is a doped polyaniline layer, the secondary outer layer is manganese carbonate wrapped with polydopamine, the middle layer is cotton fiber with a spiral structure, and the spiral structure is a DNA-like spiral structure; the particle size of the manganese carbonate is 850nm, and the thickness of a single layer of the manganese carbonate wrapped with polydopamine is 2-5 microns; the manganese carbonate is flaky, the thickness of a lamella is 20nm, and the thickness of a single layer of the doped polyaniline layer is 3-10 mu m.
2. A material as claimed in claim 1 in which the length of the cotton fibres of the helical structure is 3 mm.
3. The material of claim 1, wherein the electromagnetic shielding material is counter-doped with ammonia.
4. The material according to claim 3, wherein the concentration of the ammonia water is 1 to 10 wt.%.
5. The material according to claim 3 or 4, wherein the treatment time is 3 to 20 s.
6. A method for preparing the material of claim 1, comprising the steps of:
(1) preparing a buffer solution with the pH value of 8.5 by using trihydroxymethyl aminomethane and hydrochloric acid; adding cotton fibers with a spiral structure, manganese carbonate and dopamine hydrochloride into the buffer solution, reacting at room temperature for 1-4 hours, filtering and washing reactants after the reaction is finished, and recording a product as A;
(2) uniformly dispersing the product A and aniline monomer in 1mol/L sulfuric acid solution, marking as solution α, dripping 100ml of 1mol/L potassium permanganate sulfuric acid solution into 100ml of solution α, and carrying out oxidative polymerization reaction at-5 ℃ for 3-6 h;
(3) after the reaction is finished, filtering the reaction product, and soaking the reaction product in ammonia water with the concentration of 1-10 wt.% for 3-20 s; and filtering, vacuum drying, grinding and dispersing to obtain the spiral electromagnetic shielding material.
7. The method according to claim 6, wherein the content of the cotton fiber in the buffer solution in the step (1) is 2g/L, the content of the manganese carbonate in the buffer solution is 0.5-4 g/L, and the content of the dopamine hydrochloride in the buffer solution is 1.5 g/L.
8. the method according to claim 6, wherein the content of A in the solution α in the step (2) is 4g/mL, and the mass ratio of A to aniline monomer is between 1: 1 and 1: 4.
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| CN107007845A (en) * | 2017-04-21 | 2017-08-04 | 厦门大学 | A kind of application of manganese carbonate nano composite material in magnetic resonance imaging |
| CN107476069A (en) * | 2017-08-22 | 2017-12-15 | 北京工商大学 | A kind of three-dimensional hollow structure electromagnetic shielding material and preparation method thereof |
| CN106589360B (en) * | 2016-12-08 | 2018-11-16 | 北京工商大学 | A kind of hud typed sugarcane fibre doped polyaniline electromagnetic shielding material and preparation method thereof |
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| US20060213829A1 (en) * | 2005-03-25 | 2006-09-28 | Rutledge Gregory C | Production of submicron diameter fibers by two-fluid electrospinning process |
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| CN106589360B (en) * | 2016-12-08 | 2018-11-16 | 北京工商大学 | A kind of hud typed sugarcane fibre doped polyaniline electromagnetic shielding material and preparation method thereof |
| CN107007845A (en) * | 2017-04-21 | 2017-08-04 | 厦门大学 | A kind of application of manganese carbonate nano composite material in magnetic resonance imaging |
| CN107476069A (en) * | 2017-08-22 | 2017-12-15 | 北京工商大学 | A kind of three-dimensional hollow structure electromagnetic shielding material and preparation method thereof |
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| 《聚苯胺包覆酸处理螺旋碳纤维材料的制备和电化学性能》;史泰龙等;《材料研究学报》;20180131;第32卷(第1期);全文 * |
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