CN114464368B - High-temperature-resistant transparent conductive shielding structure and preparation method thereof - Google Patents
High-temperature-resistant transparent conductive shielding structure and preparation method thereof Download PDFInfo
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Classifications
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- H—ELECTRICITY
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- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0036—Details
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Surface Treatment Of Glass (AREA)
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Abstract
The invention discloses a high-temperature-resistant transparent conductive shielding structure and a preparation method thereof, wherein the preparation method of the high-temperature-resistant transparent conductive shielding structure comprises the following steps: (1) Preparing glass, forming a plurality of fine grooves on the glass, and connecting the fine grooves to form a hollow network structure; (2) And filling the conductive ink into the fine grooves through the soft scraping strips, and heating and sintering to form the conductive network body. Correspondingly, the invention also provides a high-temperature-resistant transparent conductive shielding structure prepared by the method. The invention has good transparency, shielding effect and heat resistance, ensures the performance stability of the product at high temperature, and avoids the risks of failure, fire and the like.
Description
Technical Field
The invention relates to the technical field of conductive shielding structures, in particular to a high-temperature-resistant transparent conductive shielding structure and a preparation method thereof.
Background
In the past few decades, light transmissive conductive materials have been classified into two categories, continuous and aperture-type in basic operation. The former is mainly a thin film material which is transparent per se, such as Indium Tin Oxide (ITO), ultrathin metal, graphene, transparent conductive polymer and the like; the latter uses the material which is not transparent to form tiny pores to realize the light transmission effect, such as metal pore plates, metal wire meshes, metal nanowires, carbon nanotubes, metal mesh grids and the like. Wherein, the continuous transparent conductive film requires the material to have ideal conductivity and light transmittance. When the index requirements are severe, the range of materials that can be selected will shrink to very few materials and there are severe requirements for the film forming process. Accordingly, the cost of production and manufacture also increases dramatically.
For the aperture type transparent conductive film, the choice of materials is relatively wide because opaque materials can be used. On the other hand, the adjustment of parameters such as the size, the shape and the like of the void distribution can influence the overall performance of the product, so that key influence factors which can be regulated and controlled are more, the selection of optimized materials and processing technology according to the overall performance index is facilitated, and the cost performance of the product is improved. In addition, the transparent conductive structure can adopt nano or micron-sized particles, sheets, wires and other materials, which is beneficial to reducing the raw material loss and the pollutant emission in the manufacturing link through the additive manufacturing technology and further reducing the manufacturing cost of the product. In contrast, conventional aperture type transparent conductive films, such as metal aperture plate or wire mesh structure, have limited light transmission performance and poor visual observation effect because the metal material needs to have a certain strength during the processing, and the average width of the opaque portion thereof is usually more than 50 μm.
Along with the expansion of the application range, the demand of a high-temperature-resistant transparent conductive film is generated;
the potential application fields of high-temperature-resistant transparent conductive films are mainly focused on the following more severe scenes:
1. The shielding device is used under high temperature conditions, such as application requirements of vehicle-mounted, aerospace, shielding under complex working conditions, invisible antennas, transparent hidden circuits and the like.
2. The application requirements of larger electric power, such as shielding of high-power radiation, hidden antennas with larger current, transparent hidden circuits and the like.
3. The application requirement of the microwave oven door can bear the high temperature of at least 150-600 ℃ and has higher shielding effect.
The prior transparent shielding layer can not meet the requirements of better shielding effect and high temperature resistance, and when the transparent shielding layer contains components which are not high temperature resistant, the shielding layer is easy to crack, discolor, smoke and even fire, so that the safety is seriously influenced.
This is because most of the prior art high quality new aperture type transparent conductive products rely on polymeric auxiliary materials. For example, various nano-or micron-sized particles, flakes, wires, etc. of conductive materials require a polymeric component to provide adhesion, scratch resistance, and package protection. For fine metal grid structures obtained by nanoimprint technology, the imprint gum employed is also always retained in the product. However, most of the polymer materials at present undergo serious deterioration at high temperature, and even can cause extreme cases of smoking, ignition and the like.
Research shows that when the hollow network structure is fused at a certain point, chain reaction can occur rapidly, so that the whole transparent conductive network is crashed, and accidents occur.
In summary, conductive powders in conventional products will be damaged/detached at high temperatures (e.g., 150-600 ℃). While certain heat-labile auxiliary materials (e.g. some resin materials) even have a risk of fire. On the other hand, damage to the conductive portion may further cause the product to heat up, thereby forming a vicious circle.
Disclosure of Invention
The invention aims to solve the technical problem of providing a high-temperature-resistant transparent conductive shielding structure and a preparation method thereof, which can have good transparency, shielding effect and heat resistance, ensure the performance stability of products at high temperature and avoid risks of failure, fire and the like.
In order to achieve the technical effects, the invention provides a preparation method of a high-temperature-resistant transparent conductive shielding structure, which comprises the following steps:
(1) Preparing glass, forming a plurality of fine grooves on the glass, and connecting the fine grooves to form a hollow network structure;
(2) And filling the conductive ink into the fine grooves through the soft scraping strips, and heating and sintering to form the conductive network body.
As an improvement of the scheme, the width of the fine groove is 1-100 micrometers, and the depth is 0.5-20 micrometers;
The maximum distance between adjacent fine grooves ranges between 100-1000 microns.
As an improvement of the scheme, the width of the fine groove is 10-50 micrometers, the depth is 5-15 micrometers, and the ratio of the depth to the width of the fine groove is 0.05-1;
the maximum distance between adjacent slots ranges between 260-460 microns.
As an improvement to the above, the maximum distance between adjacent slots is in the range of 310-410 microns.
As a modification of the above, the fine grooves are made by laser or HF acid etching.
As an improvement of the scheme, the conductive ink is filled into the fine groove for 1-5 times through the soft scraping strip;
the conductive ink comprises conductive particles, wherein the conductive particles are metal and/or carbon materials;
the metal is one or more of silver, copper and gold;
the carbon material is one or more of carbon powder, graphene and carbon nano tube.
As an improvement of the above-mentioned aspect, the conductive particles are spherical, plate-like, rod-like, linear or irregular;
The conductive particles range in size from 0.02 to 10 microns.
As an improvement of the scheme, in the step (2), the temperature of the heating sintering is 150-600 ℃;
the heating sintering equipment is selected from a hot air oven, a tunnel furnace, a muffle furnace, photon sintering equipment, microwave sintering equipment or current sintering equipment.
As an improvement of the above solution, the step (2) further includes:
(3) And forming a protective layer on the surface of the glass provided with the conductive network body, wherein the protective layer is a silicon oxide layer or a silicon nitride layer.
As an improvement of the above, the protective layer is prepared by the following means:
The polysilazane ink is uniformly formed on the surface of the glass provided with the conductive network body by using a printing or coating mode, and is converted into a silicon oxide layer or a silicon nitride layer by a high-temperature or ultraviolet irradiation mode.
As an improvement of the above, the protective layer is prepared by the following means:
Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the main component of the protective liquid is polysiloxane or polysilazane;
baking the glass coated with the protective liquid to remove the solvent;
And irradiating the baked glass with ultraviolet light to cause the polysiloxane or polysilazane to undergo a decomposition reaction to generate silicon dioxide, wherein the silicon dioxide covers the surface of the glass and permeates into the conductive network body, so that a transparent protective layer is formed.
As an improvement of the above, the protective layer is prepared by the following means:
Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the main component of the protective liquid is polysiloxane or polysilazane;
And heating the glass coated with the protective liquid to 200-300 ℃ in an environment with oxygen or water vapor, wherein the heating treatment time is 1-5 hours, so that polysiloxane or polysilazane is subjected to decomposition reaction to generate silicon dioxide, and the silicon dioxide covers the surface of the glass and permeates into the conductive network body, thereby forming a transparent protective layer.
As a modification of the above, the wavelength of the ultraviolet light is less than 300nm.
As an improvement of the above scheme, after the step (3), the method further includes:
and carrying out heating annealing treatment on the glass forming the protective layer.
Correspondingly, the invention also provides a high-temperature-resistant transparent conductive shielding structure, which is prepared by the preparation method.
The implementation of the invention has the following beneficial effects:
The invention relates to a preparation method of a high-temperature-resistant transparent conductive shielding structure, which comprises the following steps: forming a plurality of fine grooves on the glass, wherein the fine grooves are connected with each other to form a hollow network structure; filling conductive ink into the fine grooves through soft scraping strips, and heating and sintering to form a conductive network body; and finally forming a protective layer.
First, a plurality of fine grooves are formed on the glass, and by embedding the conductive ink into the fine grooves of the glass, the contact area between the conductive particles in the conductive ink and the glass substrate is increased to improve the adhesion.
Next, a protective liquid containing polysiloxane or polysilazane as a main component is coated on the surface of the glass provided with the conductive network body to form a protective layer with high light transmittance. The polysiloxane or polysilazane has stronger interaction force and ideal penetrability with the glass, and can permeate into the conductive particles while covering the surface, thereby further strengthening the interaction force between the conductive particles and the glass substrate.
Again, the preparation of the protective layer of the present invention is placed after sintering of the conductive network, which is advantageous to ensure that the interconnections between the conductive particles are not affected by the insulating component penetrating into the voids of the conductor during the preparation of the protective layer, so as to avoid negative effects on the conductivity. In addition, after the heat treatment processes such as conductor sintering and the like, the stress between the conductor and the glass can be fully released, and adverse effects such as cracking and stripping of the conductive lines caused by unmatched thermal expansion coefficients in the preparation process of the protective layer are avoided.
In summary, the transparent conductive film mainly composed of glass and conductive components is obtained, and polymer auxiliary materials are not needed in the preparation process, so that the transparent conductive film has good transparency, shielding effect and heat resistance, ensures the performance stability of the product at high temperature, and avoids risks of failure, fire and the like. The invention can normally work at the temperature of 150-600 ℃, and still has the advantages of stability, safety, high transparency, good shielding effect and the like at the high temperature of 150-600 ℃.
Drawings
FIG. 1 is a cross-sectional view of a hollow network structure of a glass surface of the present invention.
Fig. 2 is a schematic structural view of the conductive network body of the present invention.
Fig. 3 is a schematic structural view of the transparent conductive shielding structure of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent.
The prior transparent shielding layer can not meet the requirements of better shielding effect and high temperature resistance, and when the transparent shielding layer contains components which are not high temperature resistant, the shielding layer is easy to crack, discolor, smoke and even fire, so that the safety is seriously influenced.
Therefore, the invention provides a preparation method of a high-temperature-resistant transparent conductive shielding structure, which comprises the following steps:
S101, as shown in FIG. 1, preparing glass 1, forming a plurality of fine grooves 11 on the glass, and connecting the fine grooves 11 to form a hollow network structure;
preferably, the width of the fine groove 11 is 1-100 micrometers, and the depth is 0.5-20 micrometers; the maximum distance between adjacent slots 11 ranges between 100-1000 microns. More preferably, the width of the fine groove 11 is 10-50 micrometers and the depth is 5-15 micrometers; the maximum distance between adjacent slots 11 ranges between 260-460 microns.
The width of the slot 11 is 1-100 micrometers, so as to give consideration to the contradiction between human eyes' feeling and manufacturing cost. When the width is 1-100 micrometers, good visual effect can be obtained, the transparency of the transparent conductive shielding structure is good, good shielding effect can be obtained, and the manufacturing cost is relatively low. If the width of the fine groove is less than 1 μm, the manufacturing cost is high.
The depth of the slot 11 is 0.5-20 microns, which needs to be determined by the width of the slot 11. More preferably, the ratio of the depth to the width of the slot 11 (abbreviated as aspect ratio) is 0.05-1; if the aspect ratio of the slot 11 is less than 0.05, the shielding effect is insufficient, and the transparency is also affected; if the aspect ratio of the fine groove 11 is greater than 1, the strength performance of the glass itself may be affected, and the formation of the conductive network may be easily affected, so that the upper surface of the conductive network cannot be flush with the transparent substrate.
The maximum distance between adjacent fine grooves 11 is between 100 and 1000 microns, and the contradiction between the light transmittance and the shielding effect can be considered. If the maximum distance between the adjacent fine grooves 11 is less than 100 μm, the light transmission effect is poor, the transparency is low, the atomization is high, the visual effect is poor, and if the maximum distance between the adjacent fine grooves 11 is more than 1000 μm, the shielding effect is insufficient. More preferably, the maximum distance between adjacent slots is in the range of 260-460 microns. Even more preferably, the maximum distance between adjacent slots is in the range of 310-410 microns.
The maximum distance between adjacent slots 11 is based on the distance between the slot centerlines.
The plurality of the slots 11 are connected with each other to form a hollow network structure, and the shape of the grid can be implemented in various ways, preferably, the shape of the grid of the hollow network structure is square, hexagonal, octagonal, triangular, diamond or trapezoidal. More preferably, the mesh shape of the hollow network structure is square, rectangular or regular hexagon.
Specifically, the fine grooves may be formed in various ways, for example:
The first method of making the fine grooves on the glass surface is a pulsed laser, which may be nanosecond/picosecond, and ultraviolet/infrared, which directly obtains the fine grooves by the principle of locally melting the glass.
The second method of making fine grooves in the surface of glass is HF acid etching, in which most of the area is covered with resist, only the exposed area is etched, and fine grooves are formed by HF acid etching.
S102, filling conductive ink into the fine grooves 11 through soft scraping strips, and heating and sintering to form a conductive network body 2, as shown in FIG. 2;
the conductive ink is filled into the fine grooves 11 through soft scraping strips, and the conductive network body 2 is formed by heating and sintering, the shape of the conductive network body 2 can be in various embodiments, and preferably, the grid shape of the conductive network body 2 is square, hexagonal, octagonal, triangular, diamond or trapezoidal. More preferably, the mesh shape of the conductive mesh body 2 is square, rectangular or regular hexagon.
Preferably, the number of times that the conductive ink is filled into the fine groove through the soft scraping strip is 1-5 times, and the conductive ink comprises conductive particles, a small amount of auxiliary components such as dispersing agents, surfactants and the like. Wherein the weight of the non-volatilizable auxiliary component is not more than 2% of the weight of the conductive component. The auxiliary component of the invention is less than 2%, and the porosity of the invention can be ensured so that the porosity is not less than 10%.
The conductive particles are metal and/or carbon materials; the metal is one or more of silver, copper and gold; the carbon material is one or more of carbon powder, graphene and carbon nano tube. The auxiliary component is one or more of cellulose, polyvinylpyrrolidone and alkyl sulfate.
Therefore, the conductive component of the conductive ink of the present invention should have sufficient porosity after drying to facilitate penetration of the subsequent protective liquid. This ensures that the conductive layer has the desired firmness in the final product. In addition, the components of the conductive ink which are not resistant to high temperature should be reduced as much as possible, and the components should be carbonized in advance by baking or the like to eliminate unstable factors.
The conductive particles are spherical, plate-like, rod-like, linear or irregular in shape, but are not limited thereto; the conductive particles range in size from 0.02 to 10 microns. The size range of the conductive particles is 0.02-10 microns, so that the dried conductive component can be ensured to have higher void ratio, and the subsequent reinforcing effect of the protective liquid on the product is improved.
If the size range of the conductive particles is > 10 μm, the conductive particles have poor dispersibility and are not well filled in the fine grooves, affecting the formation of the conductive network body 2. If the size range of the conductive particles is less than 0.02 μm, it is easy to be nonconductive and the cost is high. The conductive ink can solve the problem that the conductive component still has higher porosity on the premise of having enough conductivity.
The soft scraping strip is made of rubber, and is structurally characterized by being rectangular with the thickness ranging from 2mm to 3mm, but is not limited to the rectangular.
In the step (2), the temperature of the heating and sintering is preferably 150-500 ℃, and the temperature of the heating and sintering is specifically determined according to the components of the ink.
The heating and sintering equipment is selected from a hot air oven, a tunnel furnace, a muffle furnace, a photon sintering equipment, a microwave sintering equipment or a current sintering equipment, but is not limited to the heating and sintering equipment.
S103, forming a protective layer 3 on the surface of the glass provided with the conductive network body, wherein the protective layer is a silicon oxide layer or a silicon nitride layer, as shown in FIG. 3.
As a preferred embodiment of step S103, the protective layer is made by the following physical means:
The polysilazane ink is uniformly formed on the surface of the glass provided with the conductive network body by using a printing or coating mode, and is converted into a silicon oxide layer or a silicon nitride layer by a high-temperature or ultraviolet irradiation mode.
As another preferred embodiment of step S103, it includes:
Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the main component of the protective liquid is polysiloxane or polysilazane;
baking the glass coated with the protective liquid to remove the solvent;
And irradiating the baked glass with ultraviolet light to cause the polysiloxane or polysilazane to undergo a decomposition reaction to generate silicon dioxide, wherein the silicon dioxide covers the surface of the glass and permeates into the conductive network body, so that a transparent protective layer is formed.
The polysiloxane or polysilazane may be diluted with a solvent or may not be used depending on the viscosity thereof. The application claims that the bulk viscosity of the liquid is not higher than 200cP. In the amount, the wet film thickness ranges from 0.5 to 10 microns.
After the solvent is removed by baking, ultraviolet light is used for irradiating the surface of the sample, so that polysiloxane or polysilazane is subjected to decomposition reaction to generate enough silicon dioxide, thereby forming a transparent and firm protective layer on the surface of the conductive material and having good binding force with glass.
Since the liquid polysiloxane or polysilazane material has desirable permeability, it can penetrate into the inside of the conductive particles while covering the surface, thereby further improving the firmness of the product as shown in fig. 2 below.
Therefore, the protective layer can effectively prevent the conductor component (metal nanoparticles, particularly silver) from being damaged by external force. The protective layer can further improve the firmness of the conductive circuit on the surface of the glass by integrally covering the glass and the conductive circuit. In addition, since such materials can penetrate into the gaps in the conductive particles, an unexpected effect of further improving the firmness can be brought about.
The ultraviolet light has a wavelength of less than 300nm, preferably 150-270nm, more preferably 172nm, 193nm, 222nm, 254nm.
The components of the protective layer are preferably polysiloxane and polysilazane, and silicon dioxide is formed after ultraviolet light with the wavelength of less than 300nm is processed, so that better effects in aspects of heat stability, transparency, adhesive force, surface hardness and the like are obtained. Specific comparison data are as follows:
In terms of thermal stability, epoxy resins of conventional materials can typically withstand no more than 180 ℃ and polyimides can typically withstand no more than 300 ℃. While the fully converted polysiloxane/polysilazane can withstand high temperatures up to 600 ℃. By completely converted polysiloxane/polysilazane is meant that both polysiloxane/polysilazane become silica.
In terms of transparency, even though the appearance of the polymer such as epoxy resin or polyimide is transparent, the transmittance is usually only 75 to 85% (a factor of deducting glass and silver lines). The transmittance of polysiloxane/polysilazane after complete conversion can reach 90-95% (the factors of glass and silver wires are deducted). More preferably, the glass is subjected to anti-reflection treatment, the transmittance of the glass is up to 105%, the anti-reflection treatment is to cover the surface of the glass with a protective layer, and the total transmittance of the whole glass is improved.
In terms of adhesive force, the results of the polymer such as epoxy resin, polyimide and the like tested by the hundred-knife method are 2B-4B; and the adhesion of the fully converted polysiloxane/polysilazane to the glass reached 5B (standard ASTM D3359-08 was used).
In terms of surface hardness, measurements were made with a pencil durometer. The test result of the polymer such as epoxy resin, polyimide and the like is 3H-5H; the hardness of the polysiloxane/polysilazane on the glass after complete conversion can reach 9H (the standard used is GB/T6739-2006, paint film hardness is measured by the method of color paint and varnish pencil).
The components of the protective layer are preferably polysiloxane and polysilazane, and after ultraviolet light treatment with a wavelength of 150-270nm, silicon dioxide is formed, so that the optimal effects in terms of transparency, adhesive force, stability, thermal expansion coefficient, mechanical strength and the like are obtained.
As another preferred embodiment of step S103, it includes:
Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the main component of the protective liquid is polysiloxane or polysilazane;
And heating the glass coated with the protective liquid to 200-300 ℃ in an environment with oxygen or water vapor, wherein the heating treatment time is 1-5 hours, so that polysiloxane or polysilazane is subjected to decomposition reaction to generate silicon dioxide, and the silicon dioxide covers the surface of the glass and permeates into the conductive network body, thereby forming a transparent protective layer.
The components of the protective layer are preferably polysiloxane and polysilazane, and silicon dioxide is formed after moisture curing treatment, so that better effects in aspects of thermal stability, transparency, adhesive force, surface hardness and the like are obtained. Specific comparison data are as follows:
In terms of thermal stability, epoxy resins of conventional materials can typically withstand no more than 180 ℃ and polyimides can typically withstand no more than 300 ℃. While the fully converted polysiloxane/polysilazane can withstand high temperatures up to 600 ℃. By completely converted polysiloxane/polysilazane is meant that both polysiloxane/polysilazane become silica.
In terms of transparency, even though the appearance of the polymer such as epoxy resin or polyimide is transparent, the transmittance is usually only 75 to 85% (a factor of deducting glass and silver lines). The transmittance of polysiloxane/polysilazane after complete conversion can reach 90-95% (the factors of glass and silver wires are deducted). More preferably, the glass is subjected to anti-reflection treatment, the transmittance of the glass is up to 105%, the anti-reflection treatment is to cover the surface of the glass with a protective layer, and the total transmittance of the whole glass is improved.
In terms of adhesive force, the results of the polymer such as epoxy resin, polyimide and the like tested by the hundred-knife method are 2B-4B; and the adhesion of the polysiloxane/polysilazane completely converted on the glass reaches 4B-5B. When the moisture curing conditions are set at 200-250 ℃ and the curing time is set at 2-4 hours, the adhesion of the fully converted polysiloxane/polysilazane to the glass can reach 5B (the adopted standard is ASTM D3359-08).
In terms of surface hardness, measurements were made with a pencil durometer. The test result of the polymer such as epoxy resin, polyimide and the like is 3H-5H; the hardness of the polysiloxane/polysilazane on the glass after complete conversion can reach 9H (the standard used is GB/T6739-2006, paint film hardness is measured by the method of color paint and varnish pencil).
In summary, in the transparent conductive network structure manufactured on the glass substrate, the fixing mode of the conductive powder can bear higher temperature (for example, 200-600 ℃) through brand new structure and material design, so that the performance stability of the product at high temperature is ensured, and risks of failure, fire and the like are avoided.
Compared with the traditional aperture type product, the product has overwhelming advantage in optical effect; compared with the existing novel aperture type transparent conductive product, the novel aperture type transparent conductive product has the advantage of overwhelming stability at high temperature; compared with the common continuous transparent conductive film (such as the traditional ITO), the product realized by the invention has more ideal expansibility and wider application scene.
As a further preferred embodiment of the present invention, after step S103, the method further comprises:
and S104, performing heating annealing treatment on the glass forming the protective layer 3.
The heating annealing operation can ensure that the stress between the protective layer and the conductor and the stress between the protective layer and the glass can be fully released. The thermal annealing process includes, but is not limited to, hot air ovens, tunnel ovens, muffle ovens, photon sintering (continuous or pulsed light), microwave sintering, current sintering, and the like. The temperature of the thermal annealing treatment is preferably 200 to 500 ℃.
Correspondingly, the invention also provides a high-temperature-resistant transparent conductive shielding structure prepared by the preparation method. The transparent conductive shielding structure disclosed by the invention has good transparency, shielding effect and heat resistance, ensures the performance stability of a product at high temperature, and avoids risks such as failure, fire and the like.
The invention is further illustrated by the following examples
Example 1
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 40 microns and the depth of each fine groove is 1 micron; the maximum distance between adjacent fine grooves is in the range of 260 micrometers;
(2) Filling conductive ink into the fine grooves through soft scraping strips for 5 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysiloxane; baking the glass coated with the protective liquid to remove the solvent; and irradiating the baked glass with ultraviolet light with the wavelength less than 300nm, so as to form a transparent protective layer.
Example 2
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 40 microns and the depth of each fine groove is 5 microns; the maximum distance between adjacent fine grooves ranges between 310 microns;
(2) Filling conductive ink into the fine grooves through soft scraping strips, wherein the filling times are 3 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysiloxane; baking the glass coated with the protective liquid to remove the solvent; and irradiating the baked glass with ultraviolet light with the wavelength less than 300nm, so as to form a transparent protective layer.
Example 3
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 40 microns and the depth of each fine groove is 10 microns; the maximum distance between adjacent slots ranges between 360 microns;
(2) Filling conductive ink into the fine grooves through soft scraping strips, wherein the filling times are 2 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysilazane; baking the glass coated with the protective liquid to remove the solvent; and irradiating the baked glass with ultraviolet light with the wavelength less than 300nm, so as to form a transparent protective layer.
Example 4
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 40 microns and the depth of each fine groove is 15 microns; the maximum distance between adjacent fine grooves is between 410 micrometers;
(2) Filling conductive ink into the fine grooves through soft scraping strips, wherein the filling times are 3 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysiloxane; baking the glass coated with the protective liquid to remove the solvent; and irradiating the baked glass with ultraviolet light with the wavelength less than 300nm, so as to form a transparent protective layer.
(4) The glass forming the protective layer was subjected to a thermal annealing treatment at a temperature of 300 ℃.
Example 5
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 40 microns and the depth of each fine groove is 20 microns; the maximum distance between adjacent fine grooves is between 460 micrometers;
(2) Filling conductive ink into the fine grooves through soft scraping strips, wherein the filling times are 2 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysiloxane; the glass coated with the protective liquid was heated to 200 ℃ in the presence of water vapor for 2 hours to form a transparent protective layer.
(4) The glass forming the protective layer was subjected to a thermal annealing treatment at a temperature of 400 ℃.
Example 6
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 5 microns and the depth of each fine groove is 5 microns; the maximum distance between adjacent slots ranges between 360 microns;
(2) Filling conductive ink into the fine grooves through soft scraping strips for 5 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysiloxane; baking the glass coated with the protective liquid to remove the solvent; and irradiating the baked glass with ultraviolet light with the wavelength less than 300nm, so as to form a transparent protective layer.
Example 7
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 10 microns and the depth of each fine groove is 5 microns; the maximum distance between adjacent slots ranges between 360 microns;
(2) Filling conductive ink into the fine grooves through soft scraping strips, wherein the filling times are 3 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysiloxane; baking the glass coated with the protective liquid to remove the solvent; and irradiating the baked glass with ultraviolet light with the wavelength less than 300nm, so as to form a transparent protective layer.
Example 8
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 30 microns and the depth of each fine groove is 10 microns; the maximum distance between adjacent slots ranges between 360 microns;
(2) Filling conductive ink into the fine grooves through soft scraping strips, wherein the filling times are 2 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysilazane; baking the glass coated with the protective liquid to remove the solvent; and irradiating the baked glass with ultraviolet light with the wavelength less than 300nm, so as to form a transparent protective layer.
Example 9
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 50 microns and the depth of each fine groove is 15 microns; the maximum distance between adjacent slots ranges between 360 microns;
(2) Filling conductive ink into the fine grooves through soft scraping strips, wherein the filling times are 3 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysiloxane; baking the glass coated with the protective liquid to remove the solvent; and irradiating the baked glass with ultraviolet light with the wavelength less than 300nm, so as to form a transparent protective layer.
(4) The glass forming the protective layer was subjected to a thermal annealing treatment at a temperature of 300 ℃.
Example 10
(1) Preparing glass, forming a plurality of fine grooves on the glass by pulse laser, wherein the fine grooves are connected with each other to form a hollow network structure, and the width of each fine groove is 100 microns and the depth of each fine groove is 20 microns; the maximum distance between adjacent slots ranges between 360 microns;
(2) Filling conductive ink into the fine grooves through soft scraping strips, wherein the filling times are 2 times, and heating and sintering to form a conductive network body;
(3) Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the protective liquid is polysiloxane; the glass coated with the protective liquid was heated to 200 ℃ in the presence of water vapor for 2 hours to form a transparent protective layer.
(4) The glass forming the protective layer was subjected to a thermal annealing treatment at a temperature of 400 ℃.
The technical tests carried out on examples 1-10 show the results in the following tables one and two:
Table 1-results of the test of examples 1 to 5
Table II results of the tests of examples 6 to 10
The transparency detection standard is GB/T2680-2021, and the detection method comprises the following steps: a spectrophotometer. The @2.4GHz in the shielding effect refers to the shielding effect in a specific electromagnetic band. Regarding heat resistance, related national standards or industry standards are not established at present, and the detection of the heat resistance of the invention refers to GB/T6579-2007.
As is clear from the above table, the transparency of examples 1-10 is high, and the shielding glass window has extremely excellent visual effect, which is far superior to the effect of the existing glass window of the microwave oven;
The shielding effect of the embodiments 1-5 can reach 36dB-45dB under the electromagnetic wave band of 2.4GHz, the intensity of electromagnetic wave can be reduced by about 3000-15000 times under specific conditions, the safety standard of the existing microwave oven can be effectively met, and the shielding requirement under a more severe use environment can be met;
The heat resistance of examples 1-10 reaches 600-650 ℃, and the heat resistance still has shielding performance at the temperature, does not generate fire or smoke, and far exceeds the upper limit of the highest temperature (300 ℃) which the product can contact in application; the service performance at high temperature also meets the shielding effect standard of the product, and can effectively isolate electromagnetic waves in a potential high-temperature application scene, thereby ensuring the safety of users.
Therefore, the invention has good transparency, shielding effect and heat resistance, ensures the performance stability of the product at high temperature, and avoids the risks of failure, fire and the like.
While the foregoing is directed to the preferred embodiments of the present invention, it will be appreciated by those skilled in the art that changes and modifications may be made without departing from the principles of the invention, such changes and modifications are also intended to be within the scope of the invention.
Claims (13)
1. The preparation method of the high-temperature-resistant transparent conductive shielding structure is characterized by comprising the following steps of:
(1) Preparing glass, forming a plurality of fine grooves on the glass, and connecting the fine grooves to form a hollow network structure;
(2) Filling conductive ink into the fine grooves through soft scraping strips, and heating and sintering to form a conductive network body;
The width of the fine groove is 1-100 micrometers, and the depth is 0.5-20 micrometers;
the maximum distance between adjacent fine grooves is between 100 and 1000 micrometers;
the ratio of the depth to the width of the fine groove is 0.05-1;
The conductive ink comprises conductive particles, wherein the conductive particles are metal and/or carbon materials; the conductive particles have a size in the range of 0.02 to 10 microns;
The step (2) further comprises the following steps:
(3) And forming a protective layer on the surface of the glass provided with the conductive network body, wherein the protective layer is a silicon oxide layer or a silicon nitride layer.
2. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein the fine grooves have a width of 10-50 microns and a depth of 5-15 microns;
the maximum distance between adjacent slots ranges between 260-460 microns.
3. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein the maximum distance between adjacent slots is in the range of 310-410 microns.
4. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein the fine grooves are made by laser or HF acid etching.
5. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein the number of times the conductive ink is filled into the fine groove by a soft scratch is 1 to 5 times;
the metal is one or more of silver, copper and gold;
the carbon material is one or more of carbon powder, graphene and carbon nano tube.
6. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein the conductive particles are spherical, plate-like, rod-like, wire-like or irregularly shaped.
7. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein in step (2), the temperature of the heat sintering is 150-600 ℃;
the heating sintering equipment is selected from a hot air oven, a tunnel furnace, a muffle furnace, photon sintering equipment, microwave sintering equipment or current sintering equipment.
8. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein the protective layer is manufactured by:
The polysilazane ink is uniformly formed on the surface of the glass provided with the conductive network body by using a printing or coating mode, and is converted into a silicon oxide layer or a silicon nitride layer by a high-temperature or ultraviolet irradiation mode.
9. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein the protective layer is manufactured by:
Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the main component of the protective liquid is polysiloxane or polysilazane;
baking the glass coated with the protective liquid to remove the solvent;
And irradiating the baked glass with ultraviolet light to cause the polysiloxane or polysilazane to undergo a decomposition reaction to generate silicon dioxide, wherein the silicon dioxide covers the surface of the glass and permeates into the conductive network body, so that a transparent protective layer is formed.
10. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, wherein the protective layer is manufactured by:
Coating a protective liquid on the surface of the glass provided with the conductive network body, wherein the main component of the protective liquid is polysiloxane or polysilazane;
And heating the glass coated with the protective liquid to 200-300 ℃ in an environment with oxygen or water vapor, wherein the heating treatment time is 1-5 hours, so that polysiloxane or polysilazane is subjected to decomposition reaction to generate silicon dioxide, and the silicon dioxide covers the surface of the glass and permeates into the conductive network body, thereby forming a transparent protective layer.
11. The method of claim 9, wherein the ultraviolet light has a wavelength less than 300nm.
12. The method of manufacturing a high temperature resistant transparent conductive shielding structure according to claim 1, further comprising, after step (3):
and carrying out heating annealing treatment on the glass forming the protective layer.
13. A transparent conductive shielding structure resistant to high temperatures, characterized in that it is produced by the production method according to any one of claims 1 to 12.
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