CN109890190B - Transparent electromagnetic shielding film and preparation method thereof - Google Patents
Transparent electromagnetic shielding film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a transparent electromagnetic shielding film and a preparation method thereof. The invention increases the absorption of the whole material to electromagnetic waves by introducing ferromagnetic particles for modification, and further increases the shielding capability of the material to the electromagnetic waves.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding, and particularly relates to a transparent electromagnetic shielding film and a preparation method thereof.
Background
With the development of human electronic communication and electrical control, mutual interference between electromagnetic signals increasingly becomes a key problem threatening the normal operation of electronic equipment, and the pursuit of efficient electromagnetic shielding materials by human society is more urgent. The traditional electromagnetic shielding material is mainly made of block metal, electromagnetic waves are prevented from entering the traditional electromagnetic shielding material by utilizing the high conductive capacity of the block metal, and although the block metal has a good shielding effect on the electromagnetic waves, the block metal has large mass, is not easy to prepare a flexible shielding material, and cannot meet the development requirements of miniaturization, light weight and flexibility of electronic equipment. In addition, the traditional electromagnetic shielding material has low light transmission in a visible light wave band, and is difficult to meet the electromagnetic shielding requirement of increasingly wide photoelectric coupling systems. In general, the next generation electromagnetic shielding suitable for the optical-electrical coupling system needs to have not only good shielding capability, but also good transmission capability and good flexibility in the visible light band, which are difficult to achieve by the conventional shielding material.
The development of the one-dimensional metal nano material provides a new opportunity for the development of the transparent electromagnetic shielding material, the metal material has excellent electric conductivity and the one-dimensional nano material has special optical characteristics due to the nanometer small-size effect, so that the conductive metal grid formed on the basis of the metal material has very high optical transmittance and very high electric conductivity, the high electric conductivity can prevent electromagnetic waves from entering the material, and the reflection of the material to the electromagnetic waves is enhanced. The transparent electromagnetic shielding film prepared by the metal silver nanowires is widely concerned by academia and industry. The silver nanowire transparent electromagnetic shielding film is a preferred technology for replacing a tin-doped indium oxide (ITO) transparent conductive glass shielding material which is generally applied at present due to the advantages of high light transmittance, good conductivity, flexibility and the like.
With the development of silver nanowire synthesis technology, thin film deposition technology, and optical welding and chemical welding technology of silver nanowires, the conductivity and light transmittance of silver nanowires have reached high levels, for example, the inventor team has realized an ultra-flexible transparent conductive electrode with a sheet resistance of 10 Ω/□ and a light transmittance of 90% in a visible light band. The level can be compared with the mature conductive glass at the present stage, and has great potential in the field of electromagnetic shielding, but the transparent electromagnetic shielding film prepared by pure silver nanowires has some defects.
First, the stability of water and oxygen. Because of the nanoscale size characteristics, the specific surface area of the silver nanowire transparent electromagnetic shielding film is large, and the reactivity of silver atoms on the surface of the silver nanowire is obviously enhanced compared with that of a bulk silver material, so that the water-oxygen corrosion speed of the silver nanowire is much higher than that of the bulk silver material. The sheet resistance of the silver nanowire transparent electromagnetic shielding film is rapidly increased or even failed in the storage process, and the reflection capability of the silver nanowire transparent electromagnetic shielding film to electromagnetic waves is rapidly reduced;
secondly, in the aspect of mechanical stability, the interaction force between the silver nanowire mesh prepared by the solution method and the substrate is very weak, so that the silver nanowires are easy to peel off after the film is bent for many times, the connectivity of the film is poor, and the conductivity and the reflection capability of the corresponding film to electromagnetic waves are rapidly reduced;
and in the aspect of shielding effectiveness, the electromagnetic shielding mode of the network formed by simply connecting the silver nanowires serving as the shielding layer is mainly reflection, and the shielding mode based on the reflection is not enough to generate enough shielding effectiveness, so that the network needs to be further compounded with other materials to enhance the absorption capacity of the network on electromagnetic waves.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a transparent electromagnetic shielding film and a preparation method thereof, aiming at the defects in the prior art, by introducing a magnetic and high-conductivity ferroferric oxide metal oxide nanoparticle modification layer on the surface of a silver nanowire network and covering a metal oxide nanoparticle protector on the surface of the silver nanowire, the corrosion of water and oxygen in the atmosphere to the metal silver nanowire is prevented, and the stability of the silver nanowire in the atmosphere is improved.
The invention adopts the following technical scheme:
a transparent electromagnetic shielding film sequentially comprises a modification layer, a metal conductive grid and a substrate from top to bottom, wherein the modification layer is a mixture of metal oxide nanoparticles and a polymer.
Specifically, the metal oxide is ferroferric oxide, the polymer is polyvinylpyrrolidone, and the mass ratio of the ferroferric oxide to the polyvinylpyrrolidone is 1 (1-5).
Specifically, the metal conductive grid adopts a silver nanowire mesh structure formed by randomly coating silver nanowire ink, the sheet resistance of the metal conductive grid is 10-200 ohm/square, and the light transmittance is 80-95%.
Furthermore, the diameter of the silver nanowire is 20-100 nm, and the length of the silver nanowire is 10-100 mu m.
Specifically, the substrate is glass, a polyethylene terephthalate film, a polyimide film, a polyvinyl alcohol PVA film, a polystyrene film or a polydimethylsiloxane film.
Another technical solution of the present invention is a method for preparing a transparent electromagnetic shielding film, comprising the steps of:
s1, cleaning the substrate by using acetone, ethanol and deionized water;
s2, coating the silver nanowire dispersion liquid on the surface of the substrate to prepare a film;
s3, annealing the film prepared in the step S2 to prepare a semi-finished product;
s4, mixing the metal oxide nano particles and the polymer to prepare a dispersion liquid, and coating the dispersion liquid on the surface of the semi-finished product prepared in the step S3;
s5, annealing the semi-finished product prepared in the step S4 to obtain the transparent electromagnetic shielding film.
Specifically, in the step S2, the concentration of the silver nanowires is 0.5-10 mg/ml.
Specifically, in step S3, the annealing temperature is 50 to 100 ℃ and the annealing time is 0.2 to 1 hour.
Specifically, in step S5, the annealing temperature is 50 to 100 ℃ and the annealing time is 0.2 to 1 hour.
Specifically, the coating method is spin coating, electrostatic spraying, slit coating or blade coating.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a transparent electromagnetic shielding film, which introduces magnetic and high-conductivity Fe on the surface of a silver nanowire network3O4The metal oxide nano particle modification layer reduces the surface roughness of the transparent electromagnetic shielding film through the combined action of the ferroferric oxide nano particles and the polyvinylpyrrolidone additive, the metal oxide nano particle protector is covered on the surface of the metal conductive grid to prevent the corrosion of water and oxygen in the atmosphere to the metal conductive grid, the stability of the metal conductive grid in the atmosphere is improved, and the ferroferric oxide nano particles with good conductivity form connection at the contact position of the metal conductive grid, so that the contact resistance among the metal conductive grids can be further reduced, the connectivity of the metal conductive grid network is optimized, the whole conductivity of the metal conductive grid network is optimized, the reflection capacity of the whole material to electromagnetic waves can be optimized, and the Fe-based electromagnetic wave shielding film is made of the metal oxide nano particle modification layer3O4The material is a ferromagnetic material, has a good absorption effect on electromagnetic wave magnetic field components, and thus the absorption capacity of the whole material on electromagnetic waves is increased, and the shielding effect of the whole material on the electromagnetic waves is greatly improved.
Furthermore, the silver nanowire mesh structure is formed by randomly coating the silver nanowire ink, so that the interaction between the silver nanowires and the substrate is enhanced, the adhesive force of the silver nanowires is improved, and the mechanical stability is improved.
Furthermore, the interconnection among the silver nanowires is enhanced, the contact resistance of the silver nano conductive network is reduced, the conductive performance of the transparent film is improved, the reflection capability of electromagnetic waves is improved, the nanoparticles are attached to the silver nanowires, and the silver nanowires are prevented from contacting atmospheric water oxygen and the environment, so that the environmental stability is improved.
The invention also discloses a preparation method of the transparent electromagnetic shielding film, which reduces the contact resistance of the silver nano conductive network, improves the conductive performance of the transparent film and improves the reflection capability to electromagnetic waves by enhancing the mutual connection among the silver nano wires; ferromagnetic particles are introduced for modification, so that the absorption of the whole material to electromagnetic waves is increased, and the shielding capability of the material to the electromagnetic waves is further increased; the interaction between the silver nanowires and the substrate is enhanced, the adhesive force of the silver nanowires is improved, and the mechanical stability is increased; the surface roughness of the transparent electromagnetic shielding film is reduced through the combined action of the ferroferric oxide nano particles and the polyvinylpyrrolidone additive.
Further, in step S4, the metal oxide nanoparticle suspension is composed of metal oxide nanoparticles and a polymer dispersant, and the polymer dispersant is used to increase the dispersing ability of the metal oxide nanoparticles and prevent the metal oxide nanoparticles from agglomerating to form a stable dispersion system.
In conclusion, the ferromagnetic particles are introduced for modification, so that the absorption of the whole material to electromagnetic waves is increased, and the shielding capability of the material to the electromagnetic waves is further increased.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is a schematic view of a transparent electromagnetic shielding film according to the present invention;
fig. 2 is a diagram of analyzing the performance of the transparent electromagnetic shielding thin film according to the present invention, wherein (a) is the comparison of the electromagnetic shielding performance of the present invention with a pure silver nanowire mesh, (b) is the comparison of the electromagnetic absorption performance of the present invention with a pure silver nanowire mesh, (c) is the comparison of the electromagnetic reflection performance of the present invention with a pure silver nanowire mesh, and (d) is the comparison of the optical transmittance of the present invention with a pure silver nanowire mesh;
fig. 3 is a comparison graph of the number of times of bending of the transparent electromagnetic shielding film of the present invention, wherein (a) is a comparison of the electromagnetic shielding effectiveness of the present invention and a pure silver nanowire mesh as a function of the number of times of bending, and (b) is a comparison of the sheet resistance of the present invention and a pure silver nanowire mesh as a function of the number of times of 3M tape pasting;
fig. 4 is a graph of the transparent electromagnetic shielding thin film of the present invention, wherein (a) is the shielding effectiveness of the electromagnetic shielding thin film prepared by the electrostatic spraying method of the present invention; (b) the electromagnetic shielding film prepared by the electrostatic spraying method has the transmittance in a visible light wave band.
Wherein: 1. a substrate; 2. a metal conductive mesh; 3. and a finishing layer.
Detailed Description
In the description of the present invention, it is to be understood that the terms "upper", "lower", and the like, indicate orientations or positional relationships based on those shown in the drawings, are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Referring to fig. 1, the present invention provides a transparent electromagnetic shielding film, which includes a substrate 1, a metal conductive grid 2 and a modification layer 3, which are sequentially disposed from bottom to top, wherein the metal conductive grid 2 is a silver nanowire grid structure formed by coating silver nanowire ink, and the modification layer 3 is a composite composed of ferroferric oxide metal oxide nanoparticles and polyvinylpyrrolidone.
Wherein the mass ratio of the ferroferric oxide to the polyvinylpyrrolidone is 1 (1-5).
Wherein the diameter of the silver nanowire is 20-100 nm, and the length of the silver nanowire is 10-100 mu m.
Wherein the sheet resistance of the metal conductive grid 2 is 10-200 ohm/square, and the light transmittance is 80-95%.
The substrate 1 is any one of glass, a polyethylene terephthalate (PET) film, a polyimide PI film, a polyvinyl alcohol PVA film, a Polystyrene (PS) film, or a Polydimethylsiloxane (PDMS) film. The invention relates to a preparation method of a transparent electromagnetic shielding film, which comprises the following steps:
s1, cleaning the substrate by using acetone, ethanol and deionized water;
s2, coating the silver nanowire dispersion liquid with the concentration of 0.5-10 mg/ml on the surface of the substrate;
s3, annealing the substrate prepared in the step S2 at the temperature of 50-100 ℃ for 0.2-1 hour to prepare a semi-finished product;
s4, coating the dispersion liquid formed by the ferroferric oxide nano particles and the polyvinylpyrrolidone on the surface of the semi-finished product prepared in the step S3;
s5, annealing the semi-finished product prepared in the step S4 at the temperature of 50-100 ℃ for 0.2-1 hour to obtain the transparent electromagnetic shielding film.
Preferably, the coating methods in step S2 and step S3 are spin coating, spray coating, slit coating, and blade coating.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Transparent conductive film prepared by spin coating method
Preparing ferroferric oxide metal oxide nano particles and polyvinylpyrrolidone dispersion liquid:
first 100mg of Fe3O4Adding the nanoparticles into 20ml of ethanol, carrying out ultrasonic treatment at room temperature for 15 minutes, adding 300mg of polyvinylpyrrolidone, carrying out ultrasonic crushing on the mixture for 1 hour under 600kw of power, and then obtaining stable Fe3O4Metal oxide nanoparticles and polyvinylpyrrolidone suspension.
Preparation of the substrate:
the volume ratio of the glass substrate to the glass substrate is 1: 1 for 5 minutes, then carrying out ultrasonic treatment in deionized water for 10 minutes, then taking out, drying by using nitrogen, and then treating in an ultraviolet ozone device for 10 minutes for later use.
Preparing a transparent conductive film:
silver nanowires dispersed in IPA at a concentration of 3.5mg/ml were dropped onto the substrate, spin coated at 4000 revolutions per minute for 60 seconds, and then annealed on a 60 degree celsius hot plate for 10 minutes.
And then dropwise adding the precursor suspension of the modification layer to the surface of the conductive grid, spin-coating for 60 seconds at the rotating speed of 4000 revolutions per minute, and annealing for 10 minutes on a hot table at the temperature of 100 ℃ to obtain the transparent electromagnetic shielding film.
The modification layer can remarkably improve the environmental and mechanical stability of the silver nanowire.
The electromagnetic shielding effectiveness of the prepared transparent electromagnetic shielding film and the pure silver nanowire mesh was tested by the waveguide method, and the obtained result is shown in fig. 2 (a). The electromagnetic absorption efficiency of the transparent electromagnetic shielding film and the pure silver nanowire mesh is calculated by using the energy of the transmitted and reflected electromagnetic waves, and the result is shown in fig. 2(b), and the electromagnetic absorption efficiency of the transparent electromagnetic shielding film and the pure silver nanowire mesh is calculated by using the energy of the reflected electromagnetic waves, and the result is shown in fig. 2 (c).
The electromagnetic shielding effectiveness of the invented transparent electromagnetic shielding film is significantly decreased with the increase of the number of bending times, as shown in fig. 3(a), and the electromagnetic shielding effectiveness of the invented transparent electromagnetic shielding film is significantly decreased with the increase of the number of 3M tape-attaching times, as shown in fig. 3 (b).
Example 2 a transparent electromagnetic shielding film prepared by an ultrasonic spraying method
Preparing ferroferric oxide metal oxide nano particles and polyvinylpyrrolidone dispersion liquid: firstly, 50mg of Fe3O4 nano particles are added into 20ml of ethanol, 200mg of polyvinylpyrrolidone is added after ultrasonic treatment is carried out for 15 minutes at room temperature, then the mixture is subjected to ultrasonic crushing for 1 hour under 600kw of power, and then stable ferroferric oxide metal oxide nano particles and polyvinylpyrrolidone suspension are obtained.
Preparation of the substrate: a Polyimide (PI) film substrate was formed in a volume ratio of 1: 1, performing ultrasonic treatment in an acetone-ethanol blending solution for 5 minutes, performing ultrasonic treatment in deionized water for 10 minutes, taking out, drying by using nitrogen, and treating in an ultraviolet ozone device for 10 minutes for later use;
preparing a transparent conductive film: adding silver nanowires with the concentration of 3mg/ml dispersed in IPA into an electrostatic spraying device for spraying;
the working parameters are as follows: atomizing at 20KV, wherein the height of a nozzle from a substrate is 15 cm, the heating temperature of the substrate is 80 ℃, the spraying time is 10 minutes, and then the modifying layer precursor liquid is injected into an electrostatic spraying device for spraying;
the working parameters are as follows: the atomization voltage is 25KV, the height of the nozzle from the substrate is 15 cm, the heating temperature of the substrate is 80 ℃, and the spraying time is 15 minutes;
a transparent electromagnetic shielding film is obtained. As shown in FIG. 4(a), the electromagnetic shielding effectiveness of the thin film can reach-23 dB. As shown in fig. 4(b), the film exhibits excellent transmittance in the visible light range, and the light transmittance at 550nm may reach 80%.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (2)
1. A method of preparing a transparent electromagnetic shielding film, comprising the steps of:
s1, cleaning the substrate by using acetone, ethanol and deionized water;
s2, coating the silver nanowire dispersion liquid with the concentration of 0.5-10 mg/ml on the surface of the substrate to prepare a film;
s3, annealing the film prepared in the step S2 to prepare a semi-finished product, wherein the annealing temperature is 50-100 ℃, and the annealing time is 0.2-1 hour;
s4, mixing the metal oxide nano particles and the polymer to prepare a dispersion liquid, and coating the dispersion liquid on the surface of the semi-finished product prepared in the step S3;
s5, annealing the semi-finished product prepared in the step S4 to obtain a transparent electromagnetic shielding film, wherein the annealing temperature is 50-100 ℃, the annealing time is 0.2-1 hour, the transparent electromagnetic shielding film sequentially comprises a modification layer (3), a metal conductive grid (2) and a substrate (1) from top to bottom, the metal conductive grid (2) is coated with silver nanowire ink with the diameter of 20-100 nm and the length of 10-100 mu m to form a silver nanowire grid structure, the sheet resistance of the metal conductive grid (2) is 10-200 ohm/square, the light transmittance is 80-95%, the substrate (1) is glass, a polyethylene terephthalate film, a polyimide film, a polyvinyl alcohol (PVA) film, a polystyrene film or a polydimethylsiloxane film, the modification layer (3) is a mixture of metal oxide nanoparticles and a polymer, and the metal oxide is ferroferric oxide, the polymer is polyvinylpyrrolidone, and the mass ratio of ferroferric oxide to polyvinylpyrrolidone is 1 (1-5).
2. The method of claim 1, wherein the coating method is spin coating, electrostatic spraying, slot coating, or knife coating.
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| CN110504068A (en) * | 2019-08-11 | 2019-11-26 | 东北师范大学 | A kind of high conductivity and the transparent silver nanowires electrode preparation method having good stability |
| CN113936844B (en) * | 2020-07-13 | 2023-02-03 | 华为技术有限公司 | Transparent conductive electrode, preparation method thereof and electronic device |
| CN112793269B (en) * | 2020-12-30 | 2022-11-01 | 中国科学院长春应用化学研究所 | Electromagnetic shielding composite material with multilayer structure and preparation method and application thereof |
| CN112839502B (en) * | 2021-02-07 | 2022-09-30 | 深圳市华科创智技术有限公司 | Electromagnetic shielding layer |
| CN115341386B (en) * | 2022-08-15 | 2024-03-26 | 四川华造宏材科技有限公司 | Flexible conductive composite nanofiber film and preparation method thereof |
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| CN109413972B (en) * | 2018-09-25 | 2021-04-27 | 重庆大学 | Flexible transparent conductive composite material film for electromagnetic shielding and preparation method thereof |
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