3A glass cover plate with electric heating function and preparation method thereof

Abstract

The invention relates to the technical field of display, and particularly discloses a 3A glass cover plate with an electric heating function and a preparation method thereof.The glass cover plate comprises a substrate, and an AG layer, an AR layer composed of a first high-refractive-index layer, a first low-refractive-index layer, a second high-refractive-index layer and a second low-refractive-index layer and an AF layer are sequentially arranged on the substrate in a stacked mode; wherein the first high-refractive-index layer and the second high-refractive-index layer are crystal indium tin oxide layers; the first low-refractive-index layer and the second low-refractive-index layer are microcrystal indium tin oxide layers. According to the 3A glass cover plate, the high-refractive-index insulating film layer and the low-refractive-index insulating film layer in the AR layer are set to be transparent crystalline and microcrystalline conductive film layers with the same refractive index, the good electric heating function is achieved, the farthest-end layer of the AR layer is set to be the transparent microcrystalline conductive film layer with the high surface roughness, the surface abrasion resistance of the prepared 3A glass cover plate is high, and the service life of the 3A glass cover plate is prolonged. And thus, the product experience and competitiveness are improved.

Description

Technical Field

[0001] The present invention relates to the field of display technology, and in particular to a 3A glass cover plate with an electric heating function and a preparation method thereof. Background Art

[0002] At present, the central control or instrument panel in the car is equipped with a protective cover, which generally uses a 3A glass cover with AG (anti-glare), AR (anti-reflection) and AF (anti-fingerprint) functions. The surface of the glass cover is prone to fogging on rainy or foggy days; in some scene areas with low temperatures, the response speed of the display module will slow down, resulting in display problems in the application and a poor product experience.

[0003] In order to solve the problem of fogging on the cover plate surface and slow response speed of the display module at low temperature, it is necessary to add an additional electric heating component to realize the electric heating function. The solution for the electric heating function is often realized by setting a separate electric heating conductive layer or electric heating component, such as directly attaching an independent ITO conductive layer to heat the glass on the display module (such as CN221378440 U), and directly providing a resistance wire to heat the display module (such as CN 117233998 A). The existing electric heating products have a complex structure, which adds new processes and costs on the one hand, and the conductive materials are often not effectively protected on the other hand, resulting in a serious attenuation of the electric heating effect.

[0004] In addition, the existing 3A glass cover AF layer is generally made by spraying, and a layer of nanochemical material is coated on the surface of the AR layer to make it have strong hydrophobicity, oil resistance, anti-fingerprint and other functions. When the existing 3A glass is rubbed about 1500 times, there will be friction marks on the surface, the surface water drop angle will be reduced from 110° to 100°, and the anti-fingerprint performance will deteriorate. Summary of the invention

[0005] The present invention provides a 3A glass cover plate with electric heating function and a preparation method thereof. The 3A glass cover plate has the electric heating function and can also improve the wear resistance of the 3A glass cover plate.

[0006] The technical solution of the present invention is to provide a 3A glass cover plate with an electric heating function, comprising a substrate, on which an AG layer, an AR layer consisting of a first high refractive index layer, a first low refractive index layer, a second high refractive index layer and a second low refractive index layer are sequentially stacked; wherein the first high refractive index layer and the second high refractive index layer are both crystalline indium tin oxide layers; and the first low refractive index layer and the second low refractive index layer are both microcrystalline indium tin oxide layers.

[0007] Optionally, the refractive index of the first high refractive index layer and the second high refractive index layer is between 1.8 and 2.5.

[0008] Optionally, the first low refractive index layer and the second low refractive index layer are both microcrystalline indium tin oxide layers with a refractive index of 1.35-1.65.

[0009] Optionally, the thicknesses of the first high refractive index layer, the first low refractive index layer, the second high refractive index layer and the second low refractive index layer are 8-12 nm, 35-45 nm, 100-140 nm and 70-90 nm, respectively.

[0010] The present invention also relates to a method for preparing the 3A glass cover plate with electric heating function, comprising the following steps: S1. Grind and clean the glass substrate, protect the side not subjected to AG treatment, and then chemically etch it. After that, remove the protection and clean it again to complete the AG treatment. S2. The glass treated with AG is chemically tempered and then cleaned. A light-shielding ink layer is screen-printed on the untreated side of the glass substrate. The glass substrate is placed in a magnetron sputtering device cavity. An argon-oxygen mixed gas is introduced into the cavity under vacuum conditions. Indium tin oxide is used as a target material. The temperature of the substrate is controlled at 150° C. to 200° C. A pre-crystallized indium tin oxide film is formed on the substrate by magnetron sputtering deposition. S3, introducing a hydrogen, argon and oxygen mixed gas into the cavity, using indium tin oxide as a target material, controlling the temperature of the substrate to be 100° C. to 150° C., and performing magnetron sputtering deposition on the pre-crystallized indium tin oxide film obtained in S4 to form a pre-microcrystalline indium tin oxide film; S5, repeating the magnetron sputtering operation in S2 and the magnetron sputtering operation in S3 in sequence; S6, the obtained glass is annealed to complete AR treatment; S7, screen print strips of peelable adhesive on both ends of the glass substrate near the AG and AR sides, spray AF oil on the outer surface of the AR layer after cleaning, and finally tear off the peelable adhesive to expose the long strips of binding positions of the indium tin oxide layer for electrical connection between the FPC and the AR; The 3A glass cover is obtained.

[0011] Optionally, S1 is protected by applying an acid-resistant film or screen-printing acid-resistant ink.

[0012] Optionally, the tempering treatment in S2 is KNO 3 The molten steel was tempered at 390°C for 2 hours.

[0013] Optionally, the volume percentage of oxygen in the argon-oxygen mixed gas in S2 is 1.5% to 3%; the mass percentage of indium oxide in the indium tin oxide target is 95% to 98%.

[0014] Optionally, the volume percentage of hydrogen in the hydrogen-argon-oxygen mixed gas in S3 is 0.5% to 1.2%, and the volume percentage of oxygen is 1.5% to 2.5%; the mass percentage of indium oxide in the indium tin oxide target is 88% to 92%.

[0015] Optionally, the S6 annealing treatment temperature is 150°C.

[0016] The present invention has the following beneficial effects: The present invention provides a 3A glass cover plate with an electric heating function, wherein the AR layer is provided with multiple layers of high and low refractive index transparent conductive films in sequence from near to far near the glass substrate, wherein the transparent crystalline conductive film layer is used as the high refractive index layer, and the transparent microcrystalline conductive film layer is used as the low refractive index layer. The windows at both ends of the transparent conductive film layer are provided with binding positions, which can be used to bind with the FPC to achieve electrical connection and play an electric heating function. By setting the high and low refractive index insulating film layers in the AR layer as transparent crystalline and microcrystalline conductive film layers with equivalent refractive index, the conductive film layer has a good electric heating function to increase the temperature of the liquid crystal, thereby increasing the response speed of the display module and achieving the defogging effect on the cover plate surface, and at the same time, it has an optical performance that matches the equivalent refractive index layer and can achieve the AR layer's anti-reflection, and because the most distal layer of the AR is set as a transparent microcrystalline conductive film layer with a relatively high surface roughness, the surface of the prepared 3A glass cover plate has a relatively high wear resistance, thereby improving the product experience and competitiveness.

[0017] The AR layer of the present invention integrates electric heating and optical anti-reflection functions, which on the one hand reduces the production process and reduces the production cost. On the other hand, the microcrystalline conductive film layer placed on the far side of the AR layer has a relatively rough surface due to the disorder of the crystal structure. The rough surface increases the actual contact area of ​​the AF layer, thereby enhancing the contact force and adhesion between the AF layer and the substrate, and the wear resistance is significantly improved. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 This is a schematic diagram of the structure of the 3A glass cover plate in Comparative Example 1 of the present invention.

[0019] Figure 2 This is a schematic diagram of the structure of the 3A glass cover plate of the present invention.

[0020] Figure 3 Schematic diagram of the distribution of binding sites in the 3A glass cover plate of the present invention.

[0021] Figure 4 XRD patterns of microcrystalline, crystalline and amorphous indium tin oxide. DETAILED DESCRIPTION

[0022] The experimental methods in the following examples are conventional methods unless otherwise specified. The raw materials, reagents, etc. used in the following examples are commercially available products unless otherwise specified.

[0023] The present invention provides a 3A glass cover plate with electric heating function, such as Figure 2~Figure 3 As shown, it includes a substrate, on which an AG layer, an AR layer consisting of a first high refractive index layer H1, a first low refractive index layer L1, a second high refractive index layer H1 and a second low refractive index layer L1 are sequentially stacked; wherein the first high refractive index layer and the second high refractive index layer are both crystalline indium tin oxide layers; and the first low refractive index layer and the second low refractive index layer are both microcrystalline indium tin oxide layers. The refractive index of the first high refractive index layer and the second high refractive index layer is between 1.8 and 2.5. The refractive index of the first low refractive index layer and the second low refractive index layer, both of which are microcrystalline indium tin oxide layers, is between 1.35 and 1.65. The thicknesses of the first high refractive index layer, the first low refractive index layer, the second high refractive index layer and the second low refractive index layer are 8 to 12 nm, 35 to 45 nm, 100 to 140 nm and 70 to 90 nm, respectively.

[0024] The main process flow for preparing 3A glass cover is: glass substrate → AG → tempered → silk screen printing light-shielding ink → AR → AF → binding FPC → bonding display module.

[0025] The specific preparation includes the following steps: S1. Grind and clean the glass substrate. The first side to be treated with AG is not protected. The second side is covered with an acid-resistant film or screen-printed with acid-resistant ink for full-surface protection. The glass is chemically etched, and then the acid-resistant film or acid-resistant ink is torn off and cleaned again to complete the AG layer. The glass treated with S2 and AG is chemically tempered and then cleaned. The tempering liquid is KNO 3 The molten solution was tempered at 390°C for 2 hours; S3. After cleaning, screen-print light-shielding ink with a thickness of 20 μm on the second side of the substrate, and then dry and solidify at 150° C. for 30 minutes.

[0026] S4. Place the tempered glass substrate in the cavity of the magnetron sputtering equipment. Under vacuum conditions, introduce argon-oxygen mixed gas (oxygen volume percentage is 1.5% to 3%) into the cavity. Use indium tin oxide (indium oxide mass percentage is 95% to 98%) as the target material. Control the temperature of the substrate to 150°C to 200°C, and form a pre-crystallized indium tin oxide film on the substrate by magnetron sputtering deposition.

[0027] S5. A hydrogen, argon and oxygen mixed gas (hydrogen volume percentage of 0.5% to 1.2%, oxygen volume percentage of 1.5% to 2.5%) is introduced into the cavity, and indium tin oxide (indium oxide mass percentage of 88% to 92%) is used as a target. The temperature of the substrate is controlled to be 100°C to 150°C, and a pre-microcrystalline indium tin oxide film is formed by magnetron sputtering deposition on the pre-crystallized indium tin oxide film obtained in S4. The hydrogen in the hydrogen, argon and oxygen mixed gas can cause a large amount of oxygen deficiency in the indium tin oxide film, thereby causing a large number of lattice defects. After annealing, the indium tin oxide film forms an intermediate state between crystalline and amorphous indium tin oxide. The appropriate proportion of oxygen in the hydrogen, argon and oxygen mixed gas helps to adjust the resistivity of the indium tin oxide film.

[0028] S6. Repeat the preparation step S4 to form a pre-crystallized indium tin oxide film by magnetron sputtering deposition on the pre-microcrystalline indium tin oxide film obtained in S5.

[0029] S7, repeating the preparation step S5 to form a pre-microcrystalline indium tin oxide film by magnetron sputtering deposition on the pre-crystallized indium tin oxide film obtained in S6.

[0030] S8. Annealing at 150°C allows the pre-crystallized indium tin oxide films obtained in S4 and S6 to form a crystalline indium tin oxide layer H1, and the pre-microcrystalline indium tin oxide films obtained in S5 and S7 to form a microcrystalline indium tin oxide layer L1, to obtain an AR layer stacked by H1 / L1 / H1 / L1, with an AR layer resistance of 4~17Ω / □, and thicknesses of each layer of H1 / L1 / H1 / L1 of 8~12nm / 35~45nm / 100~140nm / 70~90nm.

[0031] XRD patterns of microcrystalline, crystalline and amorphous indium tin oxide are shown in Figure 4 As shown, the microcrystalline indium tin oxide layer is in a state between amorphous and crystalline. By XRD (X-ray diffraction test), the amorphous indium tin oxide has no diffraction peak at (222), while the crystalline indium tin oxide layer prepared by the above method has a relatively obvious diffraction peak at (222). The diffraction peak intensity of the microcrystalline indium tin oxide layer at (222) is weak and relatively mild, indicating that its degree of crystallization is very low, between amorphous and crystalline. It can also be characterized by acid etching resistance. The amorphous indium tin oxide can be etched by oxalic acid, while the crystalline indium tin oxide cannot be etched by oxalic acid.

[0032] S9. Use screen printing technology to screen print two long strips of peelable adhesive symmetrically at both ends of the first side of the substrate. After cleaning, spray AF oil on the first side of the substrate. The AF thickness is 25nm.

[0033] S9, tear off the long strip of peelable glue to expose the long strip binding position of the indium tin oxide layer, which is used to bind the FPC and the indium tin oxide film to achieve electrical heating effect ( Figure 3 ), the electric heating temperature is 30~50℃, and a 3A glass cover is obtained.

[0034] S10, bonding the 3A glass cover plate obtained in S9 to the display screen using OCA optical adhesive to obtain an electric heating display module.

[0035] The present invention is described in detail below in conjunction with specific embodiments. This embodiment is implemented based on the technical solution of the present invention, and provides a detailed implementation method and a specific operation process, but the protection scope of the present invention is not limited to the following embodiments.

[0036] The main preparation parameters of Example 1 to Example 7 and Comparative Example 8 are shown in Table 1 below, and the other conditions are the same. The obtained products were tested, and the performance data are shown in Table 1. The friction-resistant water drop angle test method is as follows: 0000# steel wool, 20mm*20mm grinding head, stroke: 1.5inch, speed: 60cycle / min, load weight: 1000g, the surface of the 3A glass cover plate of the present application is rubbed, and when rubbed to 1500 times or 2000 times, the water drop angle of the test surface is taken out.

[0037] Comparative Example 8 3A glass cover structure Figure 1 As shown, the difference is that the AR structure is different from that in the embodiment of the present invention, in H / L / H / L, H is niobium oxide, and L is silicon oxide. The specific parameters and performance data are shown in Table 1.

[0038] Table 1

[0039] It can be seen from the data in Table 1 that by reasonably adjusting the magnetron sputtering parameters of each transparent conductive layer in the AR layer in Examples 1 to 7, the transmittance can reach 93% or more, the haze is 8%, the water drop angle before friction is ≥115°, the water drop angle after friction 1500 times is ≥107°, the water drop angle after friction 2000 times is ≥105°, and the electric heating temperature can reach 32°C or more; a 3A glass cover plate with electric heating, AR anti-reflection and high wear resistance is achieved.

[0040] The AR layer of Comparative Example 8 is matched with conventional niobium oxide and silicon oxide insulating layers, with a transmittance of more than 93%, a haze of 8%, a water drop angle of ≥115° before friction, a water drop angle of 101° after 1500 frictions, and a water drop angle of 98° after 2000 frictions, and the electric heating function cannot be realized; the 3A glass cover plate comparative embodiment does not have an electric heating function and the surface wear resistance is poor.

[0041] The above embodiments describe the preferred implementation of the present invention, but the present invention is not limited thereto. Within the technical concept of the present invention, the technical solution of the present invention can be subjected to a variety of simple modifications, including the combination of various technical features in any other manner, and these simple modifications and combinations should also be regarded as the contents disclosed by the present invention and belong to the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention shall be subject to the attached claims.

Claims

1. A 3A glass cover with electric heating function, characterized in that: The invention comprises a substrate, on which an AG layer, an AR layer consisting of a first high refractive index layer, a first low refractive index layer, a second high refractive index layer and a second low refractive index layer and an AF layer are sequentially stacked; wherein the first high refractive index layer and the second high refractive index layer are both crystalline indium tin oxide layers; and the first low refractive index layer and the second low refractive index layer are both microcrystalline indium tin oxide layers.

2. The 3A glass cover plate according to claim 1, characterized in that: The refractive index of the first high refractive index layer and the second high refractive index layer is between 1.8 and 2.

5.

3. The 3A glass cover plate according to claim 1, characterized in that: The first low refractive index layer and the second low refractive index layer are both microcrystalline indium tin oxide layers, and the refractive index is 1.35-1.

65.

4. The 3A glass cover plate according to claim 1, characterized in that: The thicknesses of the first high refractive index layer, the first low refractive index layer, the second high refractive index layer and the second low refractive index layer are 8-12 nm, 35-45 nm, 100-140 nm and 70-90 nm, respectively.

5. The method for preparing a 3A glass cover plate with electric heating function according to any one of claims 1 to 4, characterized in that: The following steps are involved: S1. Grind and clean the glass substrate, protect the side not subjected to AG treatment, and then chemically etch it. After that, remove the protection and clean it again to complete the AG treatment. S2. The glass treated with AG is chemically tempered and then cleaned. A light-shielding ink layer is screen-printed on the untreated side of the glass substrate. The glass substrate is placed in a magnetron sputtering device cavity. An argon-oxygen mixed gas is introduced into the cavity under vacuum conditions. Indium tin oxide is used as a target material. The temperature of the substrate is controlled at 150° C. to 200° C. A pre-crystallized indium tin oxide film is formed on the substrate by magnetron sputtering deposition. S3, introducing a hydrogen, argon and oxygen mixed gas into the cavity, using indium tin oxide as a target material, controlling the temperature of the substrate to be 100° C. to 150° C., and performing magnetron sputtering deposition on the pre-crystallized indium tin oxide film obtained in S4 to form a pre-microcrystalline indium tin oxide film; S5, repeating the magnetron sputtering operation in S2 and the magnetron sputtering operation in S3 in sequence; S6, the obtained glass is annealed to complete AR treatment; S7, screen print strips of peelable adhesive on both ends of the glass substrate near the AG and AR sides, spray AF oil on the outer surface of the AR layer after cleaning, and finally tear off the peelable adhesive to expose the long strips of binding positions of the indium tin oxide layer for electrical connection between the FPC and the AR; The 3A glass cover is obtained.

6. The preparation method according to claim 5, characterized in that: In S1, acid-resistant film or screen-printed acid-resistant ink is used for protection.

7. The preparation method according to claim 5, characterized in that: In S2, KNO3 molten liquid was used for tempering at 390°C for 2 hours.

8. The preparation method according to any one of claims 5 to 7, characterized in that: The volume percentage of oxygen in the argon-oxygen mixed gas in S2 is 1.5% to 3%; the mass percentage of indium oxide in the indium tin oxide target is 95% to 98%.

9. The preparation method according to any one of claims 5 to 7, characterized in that: The volume percentage of hydrogen in the hydrogen-argon-oxygen mixed gas in S3 is 0.5% to 1.2%, and the volume percentage of oxygen is 1.5% to 2.5%; the mass percentage of indium oxide in the indium tin oxide target is 88% to 92%.

10. The preparation method according to any one of claims 5 to 7, characterized in that: The S6 annealing treatment temperature is 150°C±10°C.

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