CN114464368A

CN114464368A - High-temperature-resistant transparent conductive shielding structure and preparation method thereof

Info

Publication number: CN114464368A
Application number: CN202111603752.3A
Authority: CN
Inventors: 龚超; 马昌期; 林剑; 曾超
Original assignee: Guangdong Zhongke Semiconductor Micro Nano Manufacturing Technology Research Institute; Suzhou Institute of Nano Tech and Nano Bionics of CAS
Current assignee: Guangdong Zhongke Semiconductor Micro Nano Manufacturing Technology Research Institute; Suzhou Institute of Nano Tech and Nano Bionics of CAS
Priority date: 2021-12-24
Filing date: 2021-12-24
Publication date: 2022-05-10
Anticipated expiration: 2041-12-24

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 thin grooves on the glass, and connecting the thin 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 a 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

High-temperature-resistant transparent conductive shielding structure and preparation method thereof

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 decades, the light-transmissive conductive material can be classified into a continuous type and an aperture type in a basic operation principle. The former is mainly a self-transparent thin film material, such as Indium Tin Oxide (ITO), ultrathin metal, graphene, transparent conductive polymer and the like; in the latter, the opaque material is used to form fine pores to realize the light transmission effect, such as metal pore plate, metal wire mesh, metal nanowire, carbon nanotube, metal mesh grid, etc. Among them, the continuous transparent conductive film requires the material itself to have both ideal conductivity and transparency. When the specification is severe, the range of available materials shrinks to extremely rare materials and places severe demands on the film forming process. Accordingly, the cost of manufacturing increases dramatically.

For the aperture type light-transmitting conductive film, since an opaque material can be used, the choice of the material is relatively wide. On the other hand, the adjustment of the parameters such as the size and the shape of the gap distribution can affect the overall performance of the product, so that more key influencing factors can be regulated and controlled, the selection of the optimized material and the 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 raw material loss and pollutant discharge in the manufacturing link through an additive manufacturing technology and further reducing the manufacturing cost of products. In contrast, conventional aperture-type transparent conductive films, such as metal aperture plates or metal wire mesh structures, have limited transparency and poor visual observation effects due to the need to ensure a certain strength of the metal material during the processing, and the average width of the opaque portion of the film is usually over 50 μm.

With the expansion of the application range, the requirement of the high-temperature resistant transparent conductive film is met;

the potential application fields of the high-temperature resistant transparent conductive film mainly focus on the following harsh scenes:

1. the high-temperature shielding and shielding integrated circuit can be used under high-temperature conditions, such as vehicle-mounted, aerospace and shielding, invisible antennas and transparent hidden circuits under complex working conditions.

2. The application requirements of larger electric power, such as shielding of high-power radiation, invisible antenna of larger current, transparent hidden circuit, etc.

3. The microwave oven door can bear the high temperature of at least 150-600 ℃ and has higher shielding effect.

The shielding effect and the high temperature resistant demand of preferred can't be satisfied simultaneously to current transparent shielding layer, and when transparent shielding layer contained not high temperature resistant component, the shielding layer cracked very easily, discoloured, smoked or even the fire, seriously influences safety.

This is because most of the high quality new aperture type transparent conductive products of the prior art rely on polymer auxiliary materials. For example, various nano-or micron-sized particles, flakes, wires, and like conductive materials require polymeric components to provide adhesion, scratch resistance, and encapsulation protection. For fine metal mesh structures obtained by nanoimprint technology, the imprint glue used also remains in the product at all times. However, most of the polymer materials are seriously deteriorated at high temperature, and even the extreme conditions of smoking, fire and the like can be caused.

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 broken down, and further accidents occur.

In summary, the conductive powder in the conventional product will be damaged/fall off at high temperature (e.g. 150-. And some thermolabile auxiliary materials (e.g., some resin materials) may even be at risk of fire. On the other hand, the damage of the conductive part may further cause the product to heat up, thereby forming a vicious circle.

Disclosure of Invention

The technical problem to be solved by the invention is to provide a high-temperature-resistant transparent conductive shielding structure and a preparation method thereof, which have good transparency, shielding effect and heat resistance, ensure the performance stability of a product at high temperature, and avoid the 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 thin grooves on the glass, and connecting the thin 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 a conductive network body.

As an improvement of the scheme, the width of the fine groove is 1-100 microns, and the depth is 0.5-20 microns;

the maximum distance between adjacent slots ranges between 100 and 1000 microns.

As an improvement of the above scheme, the width of the fine groove is 10-50 microns, the depth is 5-15 microns, 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 a modification of the above, the maximum distance between adjacent slots ranges between 310 and 410 microns.

As an improvement of the scheme, the fine grooves are formed by laser or HF acid etching.

As an improvement of the above scheme, the number of times the conductive ink is filled into the fine groove through the soft scraping bar is 1-5 times;

the conductive ink comprises conductive particles, and 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 tubes.

As an improvement of the above, the conductive particles are spherical, flaky, 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 equipment for heating and sintering 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.

As an improvement of the above scheme, the step (2) is followed by:

(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 a modification of the above, the protective layer is made in the following manner:

the polysilazane ink is uniformly formed into a film on the surface of the glass provided with the conductive network 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.

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 enable polysiloxane or polysilazane to generate decomposition reaction to generate silicon dioxide, wherein the silicon dioxide covers the surface of the glass and permeates into the conductive network body to form a transparent protective layer.

heating the glass coated with the protective liquid to 200-300 ℃ in the environment of 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 300 nm.

As an improvement of the above scheme, after the step (3), the method further comprises the following steps:

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 preparation method of the high-temperature-resistant transparent conductive shielding structure comprises the following steps: forming a plurality of grooves on the glass, wherein the grooves are mutually connected to form a hollow network structure; then filling the conductive ink into the fine grooves through the soft scraping strips, and heating and sintering to form a conductive network body; and finally forming a protective layer.

Firstly, a plurality of grooves are formed on the glass, and the conductive ink is embedded into the grooves of the glass, so that the contact area between the conductive particles in the conductive ink and the glass substrate is increased, and the adhesive force is improved.

Then, a protective liquid whose main component is polysiloxane or polysilazane is coated on the surface of the glass provided with the conductive network to form a protective layer with high light transmittance. The polysiloxane or polysilazane has strong acting force and ideal permeability with the glass, and can penetrate into the conductive particles while covering the surface, thereby further enhancing the interaction force between the conductive particles and the glass substrate.

And thirdly, the preparation of the protective layer is placed after the conductive network body is sintered, which is beneficial to ensuring that the interconnection among the conductive particles is not influenced by the insulating component which penetrates into the conductor gap in the preparation process of the protective layer, so as to avoid the negative effect on the conductivity. In addition, after the heat treatment process such as conductor sintering, the stress between the conductor and the glass can be fully released, and the adverse effects of cracking, peeling and the like of a conductive line caused by mismatching of thermal expansion coefficients in the preparation process of the protective layer are avoided.

In conclusion, the transparent conductive film mainly composed of glass and conductive components is obtained, a polymer auxiliary material is not needed in the preparation process, and the transparent conductive film 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. 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 temperature of 150-600 ℃.

Drawings

FIG. 1 is a cross-sectional view of a hollow network structure of the surface of the glass of the present invention.

Fig. 2 is a schematic diagram of the structure of the conductive network of the present invention.

Fig. 3 is a schematic structural diagram of the transparent conductive shielding structure of the present invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.

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 figure 1, preparing glass 1, forming a plurality of slots 11 on the glass, and connecting the slots 11 to form a hollow network structure;

preferably, the width of the fine groove 11 is 1 to 100 micrometers, and the depth is 0.5 to 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 to 50 microns, and the depth is 5 to 15 microns; the maximum distance between adjacent slots 11 ranges between 260 and 460 microns.

The width of the fine groove 11 is 1-100 micrometers, so as to take account of the contradiction between the human perception and the manufacturing cost. When the width is 1-100 micrometers, a good visual effect can be obtained, the transparency of the transparent conductive shielding structure is good, a good shielding effect is obtained, and the manufacturing cost is 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 in cooperation with the width of the slot 11. More preferably, the ratio of the depth to the width (simply referred to as aspect ratio) of the fine groove 11 is 0.05 to 1; if the aspect ratio of the fine groove 11 is less than 0.05, the shielding effect is insufficient and the transparency is also affected; if the aspect ratio of the fine grooves 11 is larger than 1, the strength of the glass itself may be affected, and the formation of the conductive network may be affected, so that the upper surface of the conductive network cannot be flush with the transparent substrate.

The maximum distance between the adjacent fine grooves 11 is in the range of 100-1000 μm, which can give consideration to the contradiction between the light transmittance and the shielding effect. If the maximum distance range between the adjacent fine grooves 11 is less than 100 micrometers, the light transmission effect is poor, the transparency is low, the fogging is high, and the visual effect is poor, and if the maximum distance range between the adjacent fine grooves 11 is greater than 1000 micrometers, the shielding effect is insufficient. More preferably, the maximum distance between adjacent slots ranges between 260 and 460 microns. Even more preferably, the maximum distance between adjacent slots ranges between 310 and 410 microns.

The maximum distance between adjacent fine grooves 11 is based on the distance between the center lines of the fine grooves.

The fine grooves 11 are connected with each other to form a hollow network structure, the shape of the network can be various embodiments, and preferably, the network shape of the hollow network structure is square, hexagonal, octagonal, triangular, rhombic or trapezoidal. More preferably, the grid shape of the hollow network structure is square, rectangular or regular hexagon.

Specifically, the fine grooves are formed in various ways, for example:

the first method of making fine grooves in the glass surface is a pulsed laser, which can be nanosecond/picosecond, which can be ultraviolet/infrared, and the fine grooves are obtained directly by the principle of local melting of the glass.

A second method of forming fine grooves in the glass surface 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 the conductive ink into the fine grooves 11 through the 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 a soft scraping bar, and the conductive network 2 is formed by heating and sintering, the shape of the conductive network 2 can be various embodiments, and preferably, the grid shape of the conductive network 2 is square, hexagon, octagon, triangle, diamond or trapezoid. More preferably, the grid shape of the conductive network 2 is square, rectangular or regular hexagon.

Preferably, the number of times of filling the conductive ink into the fine groove through the soft scraping bar is 1 to 5, and the conductive ink includes conductive particles and a small amount of auxiliary components such as a dispersant and a surfactant. Wherein the weight of the non-volatile auxiliary component is not higher than 2% of the weight of the conductive component. The auxiliary component is less than 2 percent, and the porosity of the material can be ensured, so that the porosity is equal to or greater than 10 percent.

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 tubes. 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 permeation of the subsequent protective solution. 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 conductive ink is carbonized in advance through baking and other treatments, so that unstable factors are eliminated.

The conductive particles are spherical, flaky, 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 has high void ratio, and the subsequent reinforcing effect of the protective solution on the product is promoted.

If the size range of the conductive particles is larger than 10 μm, the conductive particles have poor dispersibility and are not easily filled in the fine grooves, which affects the formation of the conductive network 2. If the size range of the conductive particles is less than 0.02 μm, it is easily nonconductive and the cost is high. The conductive ink can solve the problem that the conductive component still has relatively high 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 range of 2-3mm, but not limited to.

In the step (2), the temperature for heating and sintering is preferably 150-.

The equipment for heating and sintering 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 equipment.

And S103, forming a protective layer 3 on the glass surface provided with the conductive network, wherein the protective layer is a silicon oxide layer or a silicon nitride layer, as shown in FIG. 3.

As one preferred embodiment of step S103, the protective layer is made by the following physical means:

As another preferred embodiment of step S103, the method includes:

baking the glass coated with the protective liquid to remove the solvent;

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 200 cP. In amounts, the wet film thickness ranges from 0.5 to 10 microns.

After the solvent is removed by baking, the surface of the sample is irradiated by ultraviolet light, so that polysiloxane or polysilazane is decomposed to generate enough silicon dioxide, and a transparent and firm protective layer is formed on the surface of the conductive material and has good bonding force with glass.

Since the liquid polysiloxane or polysilazane material has a desired permeability, it can penetrate into the interior 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 an external force. Through the whole cover to glass and conducting wire, this protective layer can also further improve the firm degree of conducting wire on the glass surface. Furthermore, since such materials can penetrate into gaps in the conductive particles, there is an unexpected effect of further improving the firmness.

The wavelength of the ultraviolet light is less than 300nm, preferably 150 nm and 270nm, and more preferably 172nm, 193nm, 222nm and 254 nm.

The components of the protective layer are preferably polysiloxane and polysilazane, and silicon dioxide is formed after the ultraviolet light with the wavelength less than 300nm is processed, so that better effects on the aspects of thermal stability, transparency, adhesion, surface hardness and the like are obtained. The specific comparative data are as follows:

in terms of thermal stability, epoxy resins of conventional materials can generally withstand temperatures of not more than 180 ℃ and polyimides can generally withstand temperatures of not more than 300 ℃. While fully converted polysiloxane/polysilazane can withstand high temperatures up to 600 ℃. It should be noted that the polysiloxane/polysilazane with complete conversion means that both polysiloxane/polysilazane are converted to silicon dioxide.

In terms of transparency, polymers such as epoxy resins and polyimides generally have a transmittance of 75 to 85% (excluding factors of glass and silver wires) even if they are transparent in appearance. The transmittance of completely converted polysiloxane/polysilazane can reach 90-95% (excluding the factors of glass and silver wires). Preferably, the anti-reflection treatment is carried out on the glass, the transmittance can reach 105% at most, the anti-reflection treatment is to cover a protective layer on the surface of the glass, and the total transmittance of the whole glass is improved.

In the aspect of adhesion, the result of testing polymers such as epoxy resin, polyimide and the like by a Baige knife method is 2B-4B; while the adhesion of the fully converted polysiloxane/polysilazane on glass reached 5B (ASTM D3359-08).

In terms of surface hardness, measurement was performed with a pencil hardness meter. The test result of polymers such as epoxy resin, polyimide and the like is 3H-5H; the hardness of the completely converted polysiloxane/polysilazane on glass can reach 9H at most (the adopted standard is GB/T6739-2006 paint film hardness determined by a color paint and varnish pencil method).

The components of the protective layer are preferably polysiloxane and polysilazane, and silicon dioxide is formed after the ultraviolet light treatment with the wavelength of 150-270nm, so that the best effect in the aspects of transparency, adhesion, stability, thermal expansion coefficient, mechanical strength and the like is obtained.

As another preferred embodiment of step S103, it includes:

The components of the protective layer are preferably polysiloxane and polysilazane, and silicon dioxide is formed after water vapor curing treatment, so that better effects in the aspects of thermal stability, transparency, adhesion, surface hardness and the like are obtained. The specific comparative data are as follows:

In the aspect of adhesion, the result of testing polymers such as epoxy resin, polyimide and the like by a Baige knife method is 2B-4B; and the adhesion force of the completely converted polysiloxane/polysilazane on the glass reaches 4B-5B. When the moisture curing conditions were set at 200 ℃ and 250 ℃ and the curing time was set at 2-4 hours, the adhesion of the fully converted polysiloxane/polysilazane on glass could reach 5B (using the standard ASTM D3359-08).

In summary, in the transparent conductive network structure fabricated on the glass substrate, the fixing method of the conductive powder can bear higher temperature (e.g. 200-.

Compared with the traditional aperture type product, the product has overwhelming advantages in optical effect; compared with the existing novel aperture type transparent conductive product, the stability of the product at high temperature also has the overwhelming advantage; compared with the common continuous light-transmitting conductive film (such as the conventional ITO), the product realized by the invention has more ideal expansibility and wider application scenes.

As a preferred embodiment of the present invention, after step S103, the method further includes:

s104, carrying out heating annealing treatment on the glass for forming the protective layer 3.

The heating annealing operation can ensure that the stress between the protective layer and the conductor and between the protective layer and the glass can be fully released. The heat annealing treatment includes, but is not limited to, a hot air oven, a tunnel furnace, a muffle furnace, a photonic sintering (continuous or pulsed light), a microwave sintering, an electric current sintering, and the like. The temperature of the heat annealing treatment is preferably 200-500 ℃.

Correspondingly, the invention also provides a high-temperature-resistant transparent conductive shielding structure prepared by the preparation method. The transparent conductive shielding structure 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.

The invention is further illustrated by the following specific examples

Example 1

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 40 micrometers, and the depth of each fine groove is 1 micrometer; the maximum distance between adjacent slots ranges between 260 microns;

(2) filling conductive ink into the fine grooves through the 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 of less than 300nm to form a transparent protective layer.

Example 2

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 40 micrometers, and the depth of each fine groove is 5 micrometers; the maximum distance between adjacent slots ranges between 310 microns;

(2) filling the conductive ink into the fine grooves through the soft scraping strips for 3 times, and heating and sintering to form a conductive network body;

Example 3

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 40 micrometers, and the depth of each fine groove is 10 micrometers; the maximum distance between adjacent slots ranges between 360 microns;

(2) filling conductive ink into the fine grooves through the soft scraping strips for 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 of less than 300nm to form a transparent protective layer.

Example 4

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 40 micrometers, and the depth of each fine groove is 15 micrometers; the maximum distance between adjacent slots ranges between 410 microns;

(2) filling conductive ink into the fine grooves through the soft scraping strips for 3 times, and heating and sintering to form a conductive network body;

(4) And carrying out heating annealing treatment on the glass for forming the protective layer, wherein the heating annealing temperature is 300 ℃.

Example 5

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 40 micrometers, and the depth of each fine groove is 20 micrometers; the maximum distance between adjacent slots ranges between 460 microns;

(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 200c in a water vapor atmosphere for 2 hours to form a transparent protective layer.

(4) And carrying out heating annealing treatment on the glass for forming the protective layer, wherein the heating annealing temperature is 400 ℃.

Example 6

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width and the depth of each fine groove are 5 microns and 5 microns; the maximum distance between adjacent slots ranges between 360 microns;

Example 7

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 10 micrometers, and the depth of each fine groove is 5 micrometers; the maximum distance between adjacent slots ranges between 360 microns;

Example 8

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 30 micrometers, and the depth of each fine groove is 10 micrometers; the maximum distance between adjacent slots ranges between 360 microns;

Example 9

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 50 micrometers, and the depth of each fine groove is 15 micrometers; the maximum distance between adjacent slots ranges between 360 microns;

Example 10

(1) Preparing glass, forming a plurality of fine grooves on the glass through pulse type laser, wherein the fine grooves are mutually connected to form a hollow network structure, and the width of each fine groove is 100 micrometers, and the depth of each fine groove is 20 micrometers; the maximum distance between adjacent slots ranges between 360 microns;

Technical tests were performed on examples 1-10 and the results are shown in tables one and two below:

TABLE test results of examples 1 to 5

TABLE 2 test results of examples 6 to 10

The detection standard of the transparency is GB/T2680-2021, and the detection method comprises the following steps: a spectrophotometer. The @2.4GHz in the shielding effect means a shielding effect at a specific electromagnetic band. Regarding the heat resistance, no relevant national standard or industry standard is established at present, and the detection of the heat resistance is referred to GB/T6579-2007.

As can be seen from the above table, the transparent property of the examples 1-10 is high, and the shielding glass window has extremely excellent visual effect which is far superior to the effect of the glass window of the existing microwave oven;

the shielding effect of the embodiments 1-5 can reach 36dB-45dB at the 2.4GHz electromagnetic wave band, and the intensity of the electromagnetic wave can be reduced by about 3000-15000 times under specific conditions, so that the safety standard of the existing microwave oven can be effectively met, and the shielding requirement under a more severe use environment can also be met;

the heat resistance of the examples 1-10 reaches 600-650 ℃, and the product still has shielding performance at the temperature, does not catch fire or smoke and is far beyond the upper limit (300 ℃) of the highest temperature which the product can contact in application; the service performance at high temperature also meets the shielding effect standard of the product, and represents that the electromagnetic wave can still be effectively isolated in a potential high-temperature application scene, so that the safety of a user is ensured.

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 embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.

Claims

1. A preparation method of a high-temperature-resistant transparent conductive shielding structure is characterized by comprising the following steps:

2. The method of claim 1, wherein the width of the fine groove is 1-100 micrometers and the depth is 0.5-20 micrometers;

the maximum distance between adjacent slots ranges between 100-1000 microns.

3. The method of claim 1, wherein the width of the fine groove is 10-50 microns, the depth is 5-15 microns, 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 and 460 microns.

4. The method as claimed in claim 1, wherein the maximum distance between adjacent slots is within the range of 310-410 μm.

5. The method of claim 1, wherein the fine grooves are formed by laser or HF acid etching.

6. The method of claim 1, wherein the conductive ink is filled into the fine groove 1-5 times by a soft-scratch strip;

the metal is one or more of silver, copper and gold;

7. The method of claim 1, wherein the conductive particles are spherical, flake, rod, wire, or irregular in shape;

the conductive particles range in size from 0.02 to 10 microns.

8. The method for preparing the high temperature resistant transparent conductive shielding structure as claimed in claim 1, wherein in the step (2), the temperature of the heating and sintering is 150-600 ℃;

9. The method of manufacturing a high temperature resistant transparent conductive shielding structure of claim 1, further comprising after step (2):

10. The method of manufacturing a high temperature resistant transparent conductive shielding structure of claim 9, wherein the protective layer is made by:

11. The method of manufacturing a high temperature resistant transparent conductive shielding structure of claim 9, wherein the protective layer is made by:

baking the glass coated with the protective liquid to remove the solvent;

12. The method of manufacturing a high temperature resistant transparent conductive shielding structure of claim 9, wherein the protective layer is made by:

13. The method of claim 11, wherein the ultraviolet light has a wavelength of less than 300 nm.

14. The method for preparing a high temperature resistant transparent conductive shielding structure according to claim 9, further comprising, after step (3):

15. A transparent conductive shielding structure resistant to high temperatures, characterized in that it is obtained by the method of preparation according to any one of claims 1 to 14.