Preparation Method of ITO Conductive Glass and ITO Conductive Glass

Abstract

This application relates to a preparation method of ITO conductive glass and ITO conductive glass. The preparation method includes the following steps: preparing an ITO thin film on the surface of a glass substrate, and preparing a thermal protection layer on the surface of the ITO thin film to obtain a pre-product; performing heat treatment on the pre-product, and the temperature of the heat treatment is 660°C to 710°C. In the preparation method, after preparing the ITO thin film on the surface of the glass substrate, a thermal protection layer is prepared on the surface of the ITO thin film to obtain a pre-product. Then the pre-product is heat-treated at a temperature of 660°C to 710°C. During the heat treatment process, the thermal protection layer can prevent the ITO thin film from being damaged at high temperature, and the heat treatment can promote the recrystallization of ITO, improve the crystallinity of ITO, and thus can improve the conductivity of the ITO thin film.

Description

Technical Field

[0001] The present application relates to the technical field of glass, and particularly to a method for preparing ITO conductive glass and the ITO conductive glass. Background Art

[0002] Forming an ITO thin film on a glass substrate can obtain corresponding conductive glass. Improving the conductivity of the ITO thin film is of great significance for improving the performance of the conductive glass. However, in traditional ITO conductive glass, the conductivity of the ITO thin film is poor. Summary of the Invention

[0003] Based on this, it is necessary to provide a method for preparing ITO conductive glass and the ITO conductive glass. The preparation method can improve the conductivity of the ITO thin film and promote the improvement of the performance of the conductive glass.

[0004] A method for preparing ITO conductive glass includes the following steps: preparing an ITO thin film on the surface of a glass substrate, and preparing a thermal protection layer on the surface of the ITO thin film to obtain a pre-product; performing heat treatment on the pre-product, and the temperature of the heat treatment is 660°C to 710°C.

[0005] In the above method for preparing ITO conductive glass, after preparing the ITO thin film on the surface of the glass substrate, a thermal protection layer is prepared on the surface of the ITO thin film to obtain a pre-product. Then the pre-product is heat-treated at a temperature of 660°C to 710°C. During the heat treatment process, the thermal protection layer can prevent the ITO thin film from being damaged at high temperature, and the heat treatment can promote the recrystallization of ITO, improve the crystallinity of ITO, and further improve the conductivity of the ITO thin film.

[0006] Furthermore, the above method for preparing ITO conductive glass can reduce the emissivity of the ITO conductive glass, and at the same time can also improve the visible light transmittance of the ITO conductive glass, thereby improving the comprehensive performance of the ITO conductive glass.

[0007] In some embodiments, the thermal protection layer includes one or more of silicon oxide, silicon nitride, silicon oxynitride, zirconium oxide, zirconium silicon nitride, and zirconium silicon oxide.

[0008] In some embodiments, the thickness of the thermal protection layer is 20 nm to 40 nm.

[0009] In some embodiments, the time of the heat treatment is 5 min to 15 min.

[0010] In some embodiments, at room temperature, the ITO thin film is prepared on the surface of the glass substrate by the first magnetron sputtering method.

[0011] In some embodiments, the first magnetron sputtering includes the following steps: sputtering the glass substrate under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of the argon is 1000 sccm to 1500 sccm, and the flow rate of the oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 -3 mbar to 8×10 -3 mbar.

[0012] In some embodiments, before preparing the ITO thin film on the surface of the glass substrate, it further includes: preparing a barrier layer on the surface of the glass substrate, and the barrier layer includes one or more of silicon oxide, silicon nitride, and silicon oxynitride.

[0013] In some embodiments, at room temperature, the barrier layer is prepared on the surface of the glass substrate by the second magnetron sputtering method.

[0014] In some embodiments, the second magnetron sputtering includes the following steps: sputtering the glass substrate under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of the argon is 1000 sccm to 1500 sccm, and the flow rate of the oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 -3 mbar to 8×10 -3 mbar.

[0015] In some embodiments, the thickness of the barrier layer is 30 nm to 50 nm.

[0016] An ITO conductive glass is prepared by the above preparation method. Detailed embodiments

[0017] To make the above objects, features, and advantages of the present application more obvious and understandable, the detailed embodiments of the present application will be described below. Many specific details are set forth in the following description in order to fully understand the present application. However, the present application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the connotation of the present application. Therefore, the present application is not limited by the specific embodiments disclosed below.

[0018] In this application, unless otherwise clearly defined and limited, terms such as "installation", "connection", "linkage", "fixation", etc. shall be understood in a broad sense. For example, it may be a fixed connection, a detachable connection, or an integral one; it may be a mechanical connection or an electrical connection; it may be a direct connection or an indirect connection through an intermediate medium, and it may be the communication inside two components or the interaction relationship between two components, unless otherwise clearly limited. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0019] In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one of such features. In the description of this application, the meaning of "a plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically limited.

[0020] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which this application belongs. The terms used in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The term "and / or" used herein includes any and all combinations of one or more of the related listed items.

[0021] An embodiment of this application provides a method for preparing ITO conductive glass. The method for preparing ITO conductive glass includes the following steps: preparing an ITO thin film on the surface of a glass substrate, and preparing a thermal protection layer on the surface of the ITO thin film to obtain a pre-product; performing heat treatment on the pre-product, and the temperature of the heat treatment is 660°C to 710°C.

[0022] In the method for preparing ITO conductive glass of this embodiment, after preparing the ITO thin film on the surface of the glass substrate, a thermal protection layer is prepared on the surface of the ITO thin film to obtain a pre-product. Then the pre-product is heat-treated at a temperature of 660°C to 710°C. During the heat treatment process, the thermal protection layer can prevent the ITO thin film from being damaged at high temperatures, and the heat treatment can promote the recrystallization of ITO and improve the crystallinity of ITO, thereby improving the conductivity of the ITO thin film.

[0023] Furthermore, the method for preparing ITO conductive glass of this embodiment can reduce the emissivity of the ITO conductive glass, and at the same time can also improve the visible light transmittance of the ITO conductive glass, thereby improving the comprehensive performance of the ITO conductive glass.

[0024] As some optional examples of the temperature of the heat treatment, the temperature of the heat treatment can be 660 °C, 662 °C, 665 °C, 668 °C, 670 °C, 672 °C, 675 °C, 678 °C, 680 °C, 682 °C, 685 °C, 688 °C, 690 °C, 692 °C, 695 °C, 698 °C, 700 °C, 702 °C, 705 °C, 708 °C, 710 °C, etc. It can be understood that other selections can also be made for the temperature of the heat treatment within the range of 660 °C to 710 °C.

[0025] In some embodiments, the thermal protection layer includes one or more of silicon oxide (SiOx), silicon nitride (SiNx), silicon oxynitride (SiNxOy), zirconium oxide (ZrOx), silicon zirconium nitride (SiZrNx), and silicon zirconium oxide (SiZrOx).

[0026] In some embodiments, the thickness of the thermal protection layer is 20 nm to 40 nm. When the thickness of the thermal protection layer is too small, it is difficult to fully exert the thermal protection effect of the thermal protection layer. When the thickness of the thermal protection layer is too large, the preparation cost of the ITO conductive glass will increase. Optionally, the thickness of the thermal protection layer can be 20 nm, 21 nm, 22 nm, 23 nm, 24 nm, 25 nm, 26 nm, 27 nm, 28 nm, 29 nm, 30 nm, 31 nm, 32 nm, 33 nm, 34 nm, 35 nm, 36 nm, 37 nm, 38 nm, 39 nm, 40 nm, etc. It can be understood that other selections can also be made for the thickness of the thermal protection layer within the range of 20 nm to 40 nm.

[0027] In some embodiments, the time of the heat treatment is 5 min to 15 min. When the time of the heat treatment is too short, it is difficult to fully exert the effect of the heat treatment. When the time of the heat treatment is too long, the preparation cost of the ITO conductive glass will increase. Optionally, the time of the heat treatment can be 5 min, 6 min, 7 min, 8 min, 9 min, 10 min, 11 min, 12 min, 13 min, 14 min, 15 min, etc. It can be understood that other selections can also be made for the time of the heat treatment within the range of 5 min to 15 min. In these embodiments, the conductivity of the ITO thin film can be effectively improved through a shorter time.

[0028] In some embodiments, in the preparation method of the ITO conductive glass, an appropriate heat treatment time can be adopted according to the thickness of the glass substrate. When the thickness of the glass substrate is small, a shorter heat treatment time can be adopted. When the thickness of the glass substrate is large, a longer heat treatment time can be adopted.

[0029] In some embodiments, the thickness of the glass substrate is 2 mm to 20 mm. Optionally, the thickness of the glass substrate can be 2 mm, 3 mm, 4 mm, 5 mm, 6 mm, 7 mm, 8 mm, 9 mm, 10 mm, 11 mm, 12 mm, 13 mm, 14 mm, 15 mm, 16 mm, 17 mm, 18 mm, 19 mm, 20 mm, etc. It can be understood that other selections can also be made for the thickness of the glass substrate within the range of 2 mm to 20 mm.

[0030] In some embodiments, the thickness of the ITO film is 40 nm to 180 nm. Optionally, the thickness of the ITO film can be 40 nm, 50 nm, 60 nm, 70 nm, 80 nm, 90 nm, 100 nm, 110 nm, 120 nm, 130 nm, 140 nm, 150 nm, 160 nm, 170 nm, 180 nm, etc. It can be understood that other selections can also be made for the thickness of the ITO film within the range of 40 nm to 180 nm.

[0031] In some embodiments, under normal temperature conditions, an ITO film is prepared on the surface of the glass substrate by first magnetron sputtering. Preparing the ITO film by first magnetron sputtering under normal temperature conditions can reduce the manufacturing cost of the ITO conductive glass.

[0032] It can be understood that the normal temperature in this application can be 10°C to 30°C. Optionally, the normal temperature can be 10°C, 12°C, 15°C, 18°C, 20°C, 22°C, 25°C, 28°C, 30°C, etc. It can also be understood that the normal temperature can also be other temperature values within the range of 10°C to 30°C.

[0033] In some embodiments, the first magnetron sputtering includes the following steps: sputtering the glass substrate under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of argon is 1000 sccm to 1500 sccm, and the flow rate of oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 -3 mbar to 8×10 -3 mbar.

[0034] Optionally, in the first magnetron sputtering, the flow rate of argon can be 1000 sccm, 1050 sccm, 1100 sccm, 1150 sccm, 1200 sccm, 1250 sccm, 1300 sccm, 1350 sccm, 1400 sccm, 1450 sccm, 1500 sccm, etc. It can be understood that other selections can also be made for the flow rate of argon within the range of 1000 sccm to 1500 sccm.

[0035] Optionally, in the first magnetron sputtering, the flow rate of oxygen can be 10 sccm, 12 sccm, 15 sccm, 18 sccm, 20 sccm, 22 sccm, 25 sccm, 28 sccm, 30 sccm, 32 sccm, 35 sccm, 38 sccm, 40 sccm, etc. It can be understood that other selections of the oxygen flow rate can also be made within the range of 10 sccm to 40 sccm.

[0036] Optionally, in the first magnetron sputtering, the pressure of the process atmosphere can be 3×10 -3 mbar, 3.5×10 -3 mbar, 4×10 -3 mbar, 4.5×10 -3 mbar, 5×10 -3 mbar, 5.5×10 -3 mbar, 6×10 -3 mbar, 6.5×10 -3 mbar, 7×10 -3 mbar, 7.5×10 -3 mbar, 8×10 -3 mbar, etc. It can be understood that other selections of the pressure of the process atmosphere can also be made within the range of 3×10 - 3 mbar to 8×10 -3 mbar.

[0037] In some embodiments, before preparing the ITO thin film on the surface of the glass substrate, it further includes: preparing a barrier layer on the surface of the glass substrate, and the barrier layer includes one or more of silicon oxide (SiOx), silicon nitride (SiNx), and silicon oxynitride (SiNxOy). By preparing a barrier layer on the surface of the glass substrate, the precipitation of alkali metals in the glass substrate into the ITO thin film can be blocked, and the risk of adverse effects of alkali metals on the performance of ITO can be reduced. It can be understood that the ITO thin film is prepared on the surface of the barrier layer.

[0038] In some embodiments, at room temperature, the barrier layer is prepared on the surface of the glass substrate by the second magnetron sputtering method. At room temperature, preparing the barrier layer by the second magnetron sputtering method can reduce the preparation cost of the ITO conductive glass.

[0039] In some embodiments, the second magnetron sputtering includes the following steps: sputtering the glass substrate under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of argon is 1000 sccm to 1500 sccm, and the flow rate of oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 -3mbar ~ 8×10 -3 mbar.

[0040] Optionally, in the second magnetron sputtering, the flow rate of argon gas can be 1000 sccm, 1050 sccm, 1100 sccm, 1150 sccm, 1200 sccm, 1250 sccm, 1300 sccm, 1350 sccm, 1400 sccm, 1450 sccm, 1500 sccm, etc. It can be understood that other selections of the flow rate of argon gas can also be made within the range of 1000 sccm to 1500 sccm.

[0041] Optionally, in the second magnetron sputtering, the flow rate of oxygen gas can be 10 sccm, 12 sccm, 15 sccm, 18 sccm, 20 sccm, 22 sccm, 25 sccm, 28 sccm, 30 sccm, 32 sccm, 35 sccm, 38 sccm, 40 sccm, etc. It can be understood that other selections of the flow rate of oxygen gas can also be made within the range of 10 sccm to 40 sccm.

[0042] Optionally, in the second magnetron sputtering, the pressure of the process atmosphere can be 3×10 -3 mbar, 3.5×10 -3 mbar, 4×10 -3 mbar, 4.5×10 -3 mbar, 5×10 -3 mbar, 5.5×10 -3 mbar, 6×10 -3 mbar, 6.5×10 -3 mbar, 7×10 -3 mbar, 7.5×10 -3 mbar, 8×10 -3 mbar, etc. It can be understood that the pressure of the process atmosphere can also be other selections within the range of 3×10 - 3 mbar ~ 8×10 -3 mbar.

[0043] In some embodiments, the thickness of the barrier layer is 30 nm to 50 nm. When the thickness of the barrier layer is too small, it is difficult to fully exert the barrier function. When the thickness of the barrier layer is too large, the manufacturing cost of the ITO conductive glass will increase. Optionally, the thickness of the barrier layer can be 30 nm, 31 nm, 32 nm, 33 nm, 34 nm, 35 nm, 36 nm, 37 nm, 38 nm, 39 nm, 40 nm, 41 nm, 42 nm, 43 nm, 44 nm, 45 nm, 46 nm, 47 nm, 48 nm, 49 nm, 50 nm, etc. It can be understood that other selections can also be made for the thickness of the barrier layer within the range of 30 nm to 50 nm.

[0044] In some embodiments, preparing the thermal protection layer on the surface of the ITO thin film includes: preparing the thermal protection layer on the surface of the ITO thin film by means of the third sputtering under normal temperature conditions. Preparing the thermal protection layer under normal temperature conditions can reduce the manufacturing cost of the ITO conductive glass.

[0045] In some embodiments, the third magnetron sputtering includes the following steps: sputtering a glass substrate with an ITO thin film under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of argon is 1000 sccm to 1500 sccm, and the flow rate of oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 -3 mbar to 8×10 -3 mbar.

[0046] Optionally, in the third magnetron sputtering, the flow rate of argon can be 1000 sccm, 1050 sccm, 1100 sccm, 1150 sccm, 1200 sccm, 1250 sccm, 1300 sccm, 1350 sccm, 1400 sccm, 1450 sccm, 1500 sccm, etc. It can be understood that other selections can also be made for the flow rate of argon within the range of 1000 sccm to 1500 sccm.

[0047] Optionally, in the third magnetron sputtering, the flow rate of oxygen can be 10 sccm, 12 sccm, 15 sccm, 18 sccm, 20 sccm, 22 sccm, 25 sccm, 28 sccm, 30 sccm, 32 sccm, 35 sccm, 38 sccm, 40 sccm, etc. It can be understood that other selections can also be made for the flow rate of oxygen within the range of 10 sccm to 40 sccm.

[0048] Optionally, in the third magnetron sputtering, the pressure of the process atmosphere can be 3×10 -3 mbar, 3.5×10 -3 mbar, 4×10 -3mbar, 4.5×10 -3 mbar, 5×10 -3 mbar, 5.5×10 -3 mbar, 6×10 -3 mbar, 6.5×10 -3 mbar, 7×10 -3 mbar, 7.5×10 -3 mbar, 8×10 -3 mbar, etc. It can be understood that the air pressure of the process atmosphere can also be other selections within the range of 3×10 - 3 mbar to 8×10 -3 mbar.

[0049] In some embodiments, before preparing the ITO thin film on the surface of the glass substrate, it further includes: cleaning the glass substrate, and the resistivity of the water used for the cleaning treatment is 12 MΩ·cm or more. By cleaning the glass substrate, the glass substrate is cleaned, which is convenient for fabricating the ITO thin film on the surface of the glass substrate. Optionally, the cleaning treatment is carried out by a cleaning machine with an air knife, so that the glass substrate can be dried by the air knife of the cleaning machine. Then, the dried glass substrate can be sent into the coating chamber of the magnetron sputtering equipment through a transfer table.

[0050] In some embodiments, the preparation method of the ITO conductive glass includes the following steps:

[0051] S01: Clean the glass substrate to clean the surface of the glass substrate and dry the cleaned glass substrate. Optionally, the cleaning treatment is carried out by washing with water. Further optionally, the resistivity of the water is 12 MΩ·cm or more.

[0052] S02: Under normal temperature conditions, perform magnetron sputtering on the dried glass substrate to prepare a barrier layer on the surface of the glass substrate. Optionally, the magnetron sputtering includes: performing magnetron sputtering on the glass substrate under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of argon is 1000 sccm to 1500 sccm, and the flow rate of oxygen is 10 sccm to 40 sccm; the air pressure of the process atmosphere is 3×10 -3 mbar to 8×10 -3 mbar. Optionally, the barrier layer includes one or more of silicon oxide (SiOx), silicon nitride (SiNx), and silicon oxynitride (SiNxOy). The thickness of the barrier layer is 30 nm to 50 nm.

[0053] S03: Under normal temperature conditions, an ITO thin film is prepared on the surface of the barrier layer by magnetron sputtering. Optionally, magnetron sputtering includes: magnetron sputtering a glass substrate under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of argon is 1000 sccm to 1500 sccm, and the flow rate of oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 - 3 mbar to 8×10 -3 mbar. Optionally, the thickness of the ITO thin film is 40 nm to 180 nm.

[0054] S04: Under normal temperature conditions, a thermal protection layer is prepared on the surface of the ITO thin film by magnetron sputtering to obtain a pre-product. Optionally, magnetron sputtering includes: magnetron sputtering a glass substrate with an ITO thin film under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of argon is 1000 sccm to 1500 sccm, and the flow rate of oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 -3 mbar to 8×10 -3 mbar. Optionally, the thermal protection layer includes one or more of silicon oxide (SiOx), silicon nitride (SiNx), silicon oxynitride (SiNxOy), zirconium oxide (ZrOx), silicon zirconium nitride (SiZrNx), and silicon zirconium oxide (SiZrOx). Optionally, the thickness of the thermal protection layer is 20 nm to 40 nm.

[0055] S05: Heat-treat the pre-product. The heat treatment temperature is 660 °C to 710 °C. The heat treatment time is 5 min to 15 min.

[0056] Another embodiment of the present application provides an ITO conductive glass. The ITO conductive glass is prepared by the above preparation method. The ITO conductive glass has good comprehensive performance. For example, the ITO thin film has high conductivity, and the ITO conductive glass has a low emissivity and a high visible light transmittance.

[0057] Example 1

[0058] The preparation method of the ITO conductive glass in this example is as follows:

[0059] S101: In a cleaning machine with an air knife, clean the glass substrate with water having a resistivity of 12 MΩ·cm, clean the surface of the glass substrate, and dry the cleaned glass substrate. The thickness of the glass substrate is 6 mm, and the length and width dimensions are 2440 mm × 3660 mm.

[0060] S102: Under normal temperature conditions, perform magnetron sputtering on the dried glass substrate to prepare a barrier layer on the surface of the glass substrate. The material of the barrier layer is silicon oxide (SiOx). The thickness of the barrier layer is 30 nm.

[0061] S103: Under normal temperature conditions, prepare an ITO thin film on the surface of the barrier layer by magnetron sputtering. The thickness of the ITO thin film is 46 nm.

[0062] S104: Under normal temperature conditions, prepare a thermal protection layer on the surface of the ITO thin film by magnetron sputtering to obtain a pre-product. The material of the thermal protection layer is silicon nitride (SiNx). The thickness of the thermal protection layer is 30 nm.

[0063] S105: Perform heat treatment on the pre-product. The temperature of the heat treatment is 660 °C. The time of the heat treatment is 5 min.

[0064] Example 2

[0065] The preparation method of the ITO conductive glass in this example is as follows:

[0066] S101: In a cleaning machine with an air knife, clean the glass substrate with water having a resistivity of 12 MΩ·cm, clean the surface of the glass substrate, and dry the cleaned glass substrate. The thickness of the glass substrate is 6 mm, and the length and width dimensions are 2440 mm × 3660 mm.

[0067] S102: Under normal temperature conditions, perform magnetron sputtering on the dried glass substrate to prepare a barrier layer on the surface of the glass substrate. The material of the barrier layer is silicon nitride (SiNx). The thickness of the barrier layer is 38 nm.

[0068] S103: Under normal temperature conditions, prepare an ITO thin film on the surface of the barrier layer by magnetron sputtering. The thickness of the ITO thin film is 57 nm.

[0069] S104: Under normal temperature conditions, prepare a thermal protection layer on the surface of the ITO thin film by magnetron sputtering to obtain a pre-product. The thermal protection layer is a composite layer composed of a silicon oxide (SiOx) layer with a thickness of 30 nm and a silicon zirconium oxide (SiZrOx) layer with a thickness of 10 nm.

[0070] S105: Perform heat treatment on the pre-product. The temperature of the heat treatment is 690 °C. The time of the heat treatment is 6 min.

[0071] Example 3

[0072] The preparation method of the ITO conductive glass in this example is as follows:

[0073] S101: In a cleaning machine equipped with an air knife, clean the glass substrate with water having a resistivity of 12 MΩ·cm, thoroughly clean the surface of the glass substrate, and dry the cleaned glass substrate. The thickness of the glass substrate is 6 mm, and the length and width dimensions are 2440 mm × 3660 mm..

[0074] S102: Under normal temperature conditions, perform magnetron sputtering on the dried glass substrate to prepare a barrier layer on the surface of the glass substrate. The material of the barrier layer is silicon oxynitride (SiNxOy). The thickness of the barrier layer is 49.5 nm.

[0075] S103: Under normal temperature conditions, prepare an ITO thin film on the surface of the barrier layer by magnetron sputtering. The thickness of the ITO thin film is 93.6 nm.

[0076] S104: Under normal temperature conditions, prepare a thermal protection layer on the surface of the ITO thin film by magnetron sputtering to obtain a pre-product. The thermal protection layer is a composite layer composed of a silicon nitride (SiNx) layer with a thickness of 18 nm and a zirconium oxide (ZrOx) layer with a thickness of 2 nm.

[0077] S105: Perform heat treatment on the pre-product. The temperature of the heat treatment is 700 °C. The time of the heat treatment is 10 min.

[0078] Example 4

[0079] The preparation method of the ITO conductive glass in this example is as follows:

[0080] S101: In a cleaning machine equipped with an air knife, clean the glass substrate with water having a resistivity of 12 MΩ·cm, thoroughly clean the surface of the glass substrate, and dry the cleaned glass substrate. The thickness of the glass substrate is 6 mm, and the length and width dimensions are 2440 mm × 3660 mm..

[0081] S102: Under normal temperature conditions, perform magnetron sputtering on the dried glass substrate to prepare a barrier layer on the surface of the glass substrate. The material of the barrier layer is silicon oxynitride (SiNxOy). The thickness of the barrier layer is 49.5 nm.

[0082] S103: Under normal temperature conditions, prepare an ITO thin film on the surface of the barrier layer by magnetron sputtering. The thickness of the ITO thin film is 156.5 nm.

[0083] S104: Under normal temperature conditions, prepare a thermal protection layer on the surface of the ITO thin film by magnetron sputtering to obtain a pre-product. The material of the thermal protection layer is silicon zirconium nitride (SiZrNx). The thickness of the thermal protection layer is 32.8 nm.

[0084] S105: Heat-treat the pre-product. The heat treatment temperature is 710 °C, and the heat treatment time is 15 min.

[0085] Comparative Example 1

[0086] The preparation method of ITO conductive glass in this comparative example is as follows:

[0087] S101: In a cleaning machine with an air knife, clean the glass substrate with water having a resistivity of 12 MΩ·cm, clean the surface of the glass substrate, and dry the cleaned glass substrate. The thickness of the glass substrate is 6 mm, and the length and width dimensions are 2440 mm × 3660 mm.

[0088] S102: Under normal temperature conditions, magnetron sputter the dried glass substrate to prepare a barrier layer on the surface of the glass substrate. The material of the barrier layer is silicon nitride (SiNx), and the thickness of the barrier layer is 38 nm.

[0089] S103: Under normal temperature conditions, prepare an ITO thin film on the surface of the barrier layer by magnetron sputtering. The thickness of the ITO thin film is 57 nm.

[0090] S104: Heat-treat the product obtained in S103. The heat treatment temperature is 690 °C, and the heat treatment time is 6 min.

[0091] Comparative Example 2

[0092] The preparation method of ITO conductive glass in this comparative example is as follows:

[0093] S101: In a cleaning machine with an air knife, clean the glass substrate with water having a resistivity of 12 MΩ·cm, clean the surface of the glass substrate, and dry the cleaned glass substrate. The thickness of the glass substrate is 6 mm, and the length and width dimensions are 2440 mm × 3660 mm.

[0094] S102: Under normal temperature conditions, prepare an ITO thin film on the surface of the glass substrate by magnetron sputtering. The thickness of the ITO thin film is 156.5 nm.

[0095] S103: Heat-treat the product obtained in S102. The heat treatment temperature is 710 °C, and the heat treatment time is 15 min.

[0096] Test Example

[0097] Test the surface resistance, emissivity, and visible light transmittance of the glass obtained in the examples and comparative examples. The results are shown in Table 1.

[0098] Table 1

[0099]

[0100] It is understood that the glass substrates in the examples and comparative examples are the same float glass original sheets.

[0101] It is understood that the film layer cracking in Table 1 indicates the damage of the film layer on the surface of the glass substrate, and the corresponding surface resistance is infinite.

[0102] As can be seen from Table 1, compared with Comparative Examples 1-2, in the preparation methods of Examples 1-4, before and after heat treatment, the glass has a greater reduction in surface resistance, a greater reduction in emissivity, and a greater increase in visible light transmittance.

[0103] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of description, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, it should be considered as the scope described in this specification.

[0104] The above-described embodiments merely represent several implementation manners of the present application. The description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the patent application. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present application, several modifications and improvements can still be made, and these all belong to the protection scope of the present application.

Claims

1. A preparation method of ITO conductive glass, characterized in that, It includes the following steps: preparing an ITO thin film on the surface of a glass substrate, and preparing a thermal protection layer on the surface of the ITO thin film by means of third magnetron sputtering under the condition of 10°C to 30°C to obtain a pre-product; performing heat treatment on the pre-product, wherein the temperature of the heat treatment is 692°C to 710°C; the time of the heat treatment is 10 min to 15 min; the thermal protection layer is a composite layer composed of a silicon nitride layer and a zirconia layer, or the thermal protection layer is a zirconium silicon nitride layer; The third magnetron sputtering includes the following steps: sputtering a glass substrate with an ITO thin film under a process atmosphere; the air pressure of the process atmosphere is 3.5×10 -3 mbar~8×10 -3 mbar.

2. The preparation method of the ITO conductive glass according to claim 1, characterized in that, the thickness of the thermal protection layer is 20 nm to 40 nm.

3. The preparation method of the ITO conductive glass according to claim 1, wherein, Under normal temperature conditions, the ITO thin film is prepared on the surface of the glass substrate by means of first magnetron sputtering.

4. The preparation method of the ITO conductive glass according to claim 3, wherein, The first magnetron sputtering includes the following steps: sputtering the glass substrate under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of the argon is 1000 sccm to 1500 sccm, and the flow rate of the oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 -3 mbar to 8×10 -3 mbar.

5. The preparation method of the ITO conductive glass according to any one of claims 1 to 4, characterized in that, Before preparing the ITO thin film on the surface of the glass substrate, it further includes: preparing a barrier layer on the surface of the glass substrate, and the barrier layer includes one or more of silicon oxide, silicon nitride, and silicon oxynitride.

6. The preparation method of the ITO conductive glass according to claim 5, wherein, Under normal temperature conditions, the barrier layer is prepared on the surface of the glass substrate by means of second magnetron sputtering.

7. The preparation method of the ITO conductive glass according to claim 6, characterized in that, The second magnetron sputtering includes the following steps: sputtering the glass substrate under a process atmosphere; the process atmosphere includes argon and oxygen, the flow rate of the argon is 1000 sccm to 1500 sccm, and the flow rate of the oxygen is 10 sccm to 40 sccm; the pressure of the process atmosphere is 3×10 -3 mbar to 8×10 -3 mbar.

8. The preparation method of the ITO conductive glass according to claim 6, characterized in that, The thickness of the barrier layer is 30 nm to 50 nm.

9. An ITO conductive glass, characterized in that, Prepared by the preparation method according to any one of claims 1 to 8.

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