Amorphous ITO conductive film and preparation method thereof

Abstract

The invention discloses an amorphous ITO conductive film and a preparation method thereof, and the preparation method of the amorphous ITO conductive film comprises the following steps: taking a substrate, preparing a first resin layer on one surface of the substrate, and preparing a second resin layer on the other surface of the substrate; preparing a barrier connecting layer on the second resin layer; carrying out magnetron sputtering on the barrier connecting layer by using an ITO target material to prepare an amorphous ITO layer; in the magnetron sputtering process, first gas and second gas are introduced, the first gas comprises argon and hydrogen with the volume ratio being (97-99): (3-1), the second gas is oxygen, and the volume ratio of the first gas to the second gas is 100: (3-5); the vacuum degree is 3 * 10 <-4 > Pa to 1 * 10 <-4 > Pa. The argon-hydrogen mixed gas is used as the sputtering gas to prepare the amorphous ITO conductive film, the requirement for the vacuum degree of equipment is low, the process steps are simple, and the high-temperature-resistant amorphous ITO conductive film can be prepared.

Description

Technical Field

[0001] This invention belongs to the field of conductive film technology, specifically relating to an amorphous ITO conductive film and its preparation method. Background Technology

[0002] A dimming film is a novel type of electronic light-controlling product. The electro-controlled intelligent dimming film device consists of a liquid crystal / polymer hybrid material injected between two transparent conductive films. In the absence of an electric field, the film is opaque. When an alternating current is applied, the liquid crystal molecules align in an orderly manner, causing the electro-dimming film to transition from an opaque (OFF) state to a transparent (ON) state. Through the application of an electric field, it can achieve rapid transitions between the ON and OFF states, and between OFF and ON states. It is commonly used in automotive sunroofs, side windows, or in office building conference room glass.

[0003] ITO conductive film is a widely used conductive film in dimming films. It has high light transmittance and high electrical conductivity, and is easy to deposit into thin films. In actual production, ITO conductive film is generally obtained by magnetron sputtering, which sputters an indium tin oxide coating onto the material and then performs high-temperature annealing treatment, resulting in a crystalline ITO conductive film.

[0004] Although crystalline ITO conductive films possess excellent conductivity and light transmittance, the deposition equipment for crystalline ITO conductive films requires high vacuum deposition capabilities, with an optimal vacuum level of at least 10. -5 Pa-10 -6 The high pressure (Pa) requires high vacuum and cooling capabilities from the equipment, resulting in high costs. Furthermore, when using crystalline ITO conductive films to fabricate dimming glass at the back end, a prolonged period of high-temperature static cooling is required during the lamination process, necessitating further improvement in the high-temperature resistance of the crystalline ITO conductive film. Summary of the Invention

[0005] The purpose of this invention is to provide an amorphous ITO conductive film and its preparation method. This preparation method has low requirements for equipment vacuum degree and simple process steps, and can prepare a high-temperature resistant amorphous ITO conductive film.

[0006] To achieve the above objectives, a specific embodiment of the present invention provides the following technical solution:

[0007] A method for preparing an amorphous ITO conductive film, the method comprising the following steps:

[0008] Take a substrate, prepare a first resin layer on one side of the substrate, and prepare a second resin layer on the other side of the substrate;

[0009] A barrier bonding layer is prepared on the second resin layer;

[0010] An amorphous ITO layer was prepared by magnetron sputtering on a barrier bonding layer using an ITO target. During the magnetron sputtering process, a first gas and a second gas were introduced. The first gas consisted of argon and hydrogen in a volume ratio of (97-99):(3-1), and the second gas was oxygen. The volume ratio of the first gas to the second gas was 100:(3-5). The vacuum level was 3×10⁻⁶. -4 Pa-1×10 -4 Pa.

[0011] In one or more embodiments of the present invention, the flow rate of the first gas is 390 sccm-400 sccm, and the flow rate of the second gas is 12 sccm-20 sccm.

[0012] In one or more embodiments of the present invention, the mass percentage of indium oxide and tin oxide in the ITO target is 90:10-97:3.

[0013] In one or more embodiments of the present invention, during the magnetron sputtering process, the ITO target is transported at a speed of 3m / min-4m / min and the power output is 17kW-19kW.

[0014] In one or more embodiments of the present invention, a barrier bonding layer is prepared by magnetron sputtering on a second resin layer using a silicon target. During the magnetron sputtering process, the silicon target is transported at a speed of 3 m / min to 5 m / min, the power output is 0.5 kW to 2 kW, and the Ar gas flow rate is 1000 sccm to 1200 sccm.

[0015] Another specific embodiment of the present invention provides the following technical solution:

[0016] An amorphous ITO conductive film, wherein the amorphous ITO conductive film is prepared by the above-described preparation method.

[0017] In one or more embodiments of the present invention, the thickness of the amorphous ITO layer is 20 nm to 150 nm.

[0018] In one or more embodiments of the present invention, the barrier connection layer is a silicon plating layer with a thickness of 1.0 nm to 1.5 nm.

[0019] In one or more embodiments of the present invention, the first resin layer is an acrylic resin layer containing silica particles, with a thickness of 800nm-1000nm and a refractive index of 1.50-1.55; and / or,

[0020] The second resin layer is an acrylic resin layer containing silica particles, with a thickness of 550nm-700nm and a refractive index of 1.50-1.55.

[0021] In one or more embodiments of the present invention, the substrate is a PET substrate with a thickness of 23μm-250μm.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] 1. This invention uses an argon-hydrogen mixed gas as the sputtering gas to prepare an amorphous ITO conductive film, requiring a vacuum of 10... -4 With a vacuum level of around Pa, the vacuum requirement is not high. The vacuuming and cooling capacity requirements of the equipment are lower than those of crystalline ITO conductive film, which reduces the equipment's vacuuming and cooling capacity, as well as the vacuuming time, thus saving equipment costs.

[0024] 2. The non-crystalline conductive film in this invention does not require aging at the back end, reducing back-end process steps and lowering labor costs.

[0025] 3. The non-crystalline ITO conductive film in this invention has excellent high temperature resistance. When placed at high temperature (130℃ / 10 days), the sheet resistance fluctuation is small, which can reduce the risk of the high temperature static process affecting the sheet resistance and thus causing product abnormalities during the back-end lamination process. Attached Figure Description

[0026] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0027] Figure 1 This is a schematic diagram of the structure of an amorphous ITO conductive film in one embodiment of the present invention.

[0028] Explanation of key figure labels:

[0029] 1. Substrate; 2. First resin layer; 3. Second resin layer; 4. Barrier bonding layer; 5. Amorphous ITO layer. Detailed Implementation

[0030] To enable those skilled in the art to better understand the technical solutions in this disclosure, the technical solutions in the embodiments of this disclosure will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this disclosure, and not all embodiments. Based on the embodiments in this disclosure, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of this disclosure.

[0031] A specific embodiment of the present invention provides a method for preparing an amorphous ITO conductive film, comprising the following steps:

[0032] Step 1, prepare the substrate.

[0033] Specifically, the substrate is PET substrate with a thickness of 23μm-250μm, specifically 23μm, 100μm, 150μm, 200μm, and 250μm.

[0034] Step 2: Prepare a first resin layer on one side of the substrate and a second resin layer on the other side of the substrate.

[0035] Specifically, a first resin layer and a second resin layer are formed on both sides of the substrate by a precision coating process. The first resin uses an acrylic resin coating liquid, specifically GU2600K acrylic resin from Guojing Chemical, and is mixed with at least silica nanoparticles and a solvent (such as methyl ethyl ketone) to make the refractive index of the first resin layer 1.50-1.55 and the thickness 800nm-1000nm.

[0036] The second resin layer also uses an acrylic resin coating liquid, specifically Guojing Chemical GU2600K acrylic resin, and at least mixes silica nanoparticles and solvents (such as methyl ethyl ketone) to make the refractive index of the first resin layer 1.50-1.55 and the thickness 550nm-700nm.

[0037] Step 3: Prepare a barrier bonding layer on the second resin layer.

[0038] Specifically, before preparing the barrier bonding layer, the second resin layer is pretreated. An Al or Ti target can be used for pretreatment. The substrate is placed in the pretreatment chamber of a magnetron sputtering equipment for glow discharge cleaning. The heating and ionization power supplies are turned on, and Ar ions are introduced for argon ion bombardment. Argon ion bombardment increases the surface roughness of the substrate, improving the film-substrate adhesion and the film deposition structure. The treatment time is 20-30 seconds to obtain a cleaner surface and improve the adhesion between the second resin layer and the barrier bonding layer.

[0039] The barrier bonding layer is formed using a silicon target sputtering process, with a thickness of 1.0 nm-1.5 nm and a refractive index of 3.3. During magnetron sputtering, the silicon target is transported at a speed of 3 m / min-5 m / min, the Ar gas flow rate is 1000 sccm-1200 sccm, and an MF intermediate frequency power supply is used for sputtering with an output power of 0.5 kW-2 kW.

[0040] Step 4: Use an ITO target to perform magnetron sputtering on the barrier bonding layer to prepare an amorphous ITO layer.

[0041] Specifically, the mass percentage of indium oxide and tin oxide in the ITO target used is 90:10-97:3. During sputtering, the ITO target transport speed is 3-4 m / min, and a DC power supply with an output power of 17-19 kW is used. A first gas and a second gas are introduced during sputtering. The first gas consists of argon and hydrogen in a volume ratio of (97-99):(3-1), and the second gas is oxygen. The volume ratio of the first gas to the second gas is 100:(3-5). The vacuum level of the equipment during sputtering is 3 × 10⁻⁶. -4 Pa-1×10 -4 Pa.

[0042] In this step, an amorphous ITO layer is formed on the barrier bonding layer. The required vacuum level of the equipment during preparation is relatively low, and the conductive film prepared does not require aging in the later stage. This reduces the number of subsequent process steps and lowers labor costs. Moreover, the conductive film has excellent high temperature resistance, and temperature does not affect the performance of the amorphous ITO conductive film. The sheet resistance and optical properties remain good, which can effectively solve the impact of the high-temperature static process required in the later lamination process on the performance of the conductive film.

[0043] Furthermore, the use of an argon-hydrogen mixture during sputtering has the advantage of reducing oxygen vacancy defects: H2 reacts with O on the target surface or in the plasma (e.g., H2 + O → H2O), reducing the O content in the sputtered particles and suppressing the formation of oxygen vacancies in the film. Oxygen vacancies are scattering centers for charge carriers; reducing them can improve electron mobility while avoiding the disordered increase in charge carrier concentration caused by excessive oxygen vacancies (which actually reduces mobility), ultimately resulting in better electrical conductivity. Pure Ar sputtering requires an ultra-high vacuum (e.g., 10⁻⁶ ppm). -5 (Pa level) to reduce the influence of oxidizing impurities such as O2 and H2O; while H2 in Ar / H2 can actively consume these impurities (converting them into H2O), even with a background vacuum of only 10 Pa. -3 Even at the Pa level, low impurity partial pressure can be maintained, reducing equipment costs. The Ar / H2 mixed gas, through the reducing and reactive properties of H2, effectively inhibits target surface oxidation, removes background impurities, improves plasma stability, and reduces target outgassing, thereby lowering the stringent requirements for background vacuum and dynamic vacuum. In contrast, pure Ar sputtering relies more heavily on a high vacuum environment to eliminate oxidizing impurities and reduce interference, ensuring sputtering efficiency and film quality.

[0044] Furthermore, the thickness of the amorphous ITO layer is 20nm-150nm, specifically 20nm, 80nm, 100nm, 120nm, and 150nm. The specific thickness can be matched according to different resistance values.

[0045] Another specific embodiment of the present invention provides an amorphous ITO conductive film, which is obtained by the above preparation method, such as... Figure 1 As shown, its structure specifically includes a substrate 1, a first resin layer 2 is provided on one side of the substrate 1, and a second resin layer 3, a barrier bonding layer 4, and an amorphous ITO layer 5 are sequentially stacked on the other side of the substrate 1.

[0046] The present invention will be further described in detail below with reference to specific embodiments.

[0047] Example 1

[0048] The preparation method of the amorphous ITO conductive film in this embodiment is as follows:

[0049] A 125μm thick PET substrate is coated with an acrylic resin coating solution to form a first resin layer. The acrylic resin coating solution is a mixture of acrylic resin and nano-silica. The thickness of the first resin layer is 800nm, and the refractive index is 1.55. An acrylic resin coating solution is then coated on the other side of the PET substrate to form a second resin layer. The acrylic resin coating solution is a mixture of acrylic resin and nano-silica. The thickness of the second resin layer is 600nm, and the refractive index is 1.55.

[0050] The second resin layer is pretreated and glow-cleaned.

[0051] A barrier bonding layer was formed on the surface of the second resin layer by magnetron sputtering using a silicon target at a speed of 4.0 m / min. Sputtering was performed using an MF intermediate frequency power supply with an output power of 1.0 kW and an Ar gas flow rate of 1200 sccm. The barrier bonding layer had a thickness of 1.5 nm and a refractive index of 3.3.

[0052] Magnetron sputtering was performed on the barrier bonding layer surface using a 93:7 ITO target with a target feed rate of 4 m / min. An industrial argon-hydrogen mixture (argon to hydrogen ratio 99:1) and oxygen were introduced, with an argon-hydrogen mixture and oxygen ratio of 100:3.75. The actual sputtering speed was 400 sccm for the argon-hydrogen mixture and 15 sccm for the oxygen. Sputtering was performed using a DC power supply with an output power of 18.0 kW, resulting in an amorphous ITO layer with a thickness of 30 nm and a refractive index of 1.9.

[0053] In this embodiment, the vacuum level of the equipment during magnetron sputtering is 3×10⁻⁶. -4 Pa, the purity of the target materials used is 99.99%, and the magnetic field strength of all sputtering target sites is 400GS-700GS.

[0054] Example 2

[0055] The preparation method of the amorphous ITO conductive film in this embodiment is as follows:

[0056] A 125μm thick PET substrate is coated with an acrylic resin coating solution to form a first resin layer. The acrylic resin coating solution is a mixture of acrylic resin and nano-silica. The thickness of the first resin layer is 800nm, and the refractive index is 1.55. An acrylic resin coating solution is then coated on the other side of the PET substrate to form a second resin layer. The acrylic resin coating solution is a mixture of acrylic resin and nano-silica. The thickness of the second resin layer is 600nm, and the refractive index is 1.55.

[0057] The second resin layer is pretreated and glow-cleaned.

[0058] A barrier bonding layer was formed on the surface of the second resin layer by magnetron sputtering using a silicon target at a speed of 4.0 m / min. Sputtering was performed using an MF intermediate frequency power supply with an output power of 1.0 kW and an Ar gas flow rate of 1200 sccm. The barrier bonding layer had a thickness of 1.5 nm and a refractive index of 3.3.

[0059] Magnetron sputtering was performed on the barrier bonding layer surface using a 93:7 ITO target with a target feed rate of 4 m / min. An industrial argon-hydrogen mixture (argon to hydrogen ratio 98:2) and oxygen were introduced, with a argon-hydrogen mixture to oxygen ratio of 100:3.75. The actual sputtering speed was 400 sccm for the argon-hydrogen mixture and 15 sccm for the oxygen. Sputtering was performed using a DC power supply with an output power of 18.0 kW, resulting in an amorphous ITO layer with a thickness of 30 nm and a refractive index of 1.9.

[0060] In this embodiment, the vacuum level of the equipment during magnetron sputtering is 2×10⁻⁶. -4 Pa, the purity of the target materials used is 99.99%, and the magnetic field strength of all sputtering target sites is 400GS-700GS.

[0061] Example 3

[0062] The preparation method of the amorphous ITO conductive film in this embodiment is as follows:

[0063] A 125μm thick PET substrate is coated with an acrylic resin coating solution to form a first resin layer. The acrylic resin coating solution is a mixture of acrylic resin and nano-silica. The thickness of the first resin layer is 800nm, and the refractive index is 1.55. An acrylic resin coating solution is then coated on the other side of the PET substrate to form a second resin layer. The acrylic resin coating solution is a mixture of acrylic resin and nano-silica. The thickness of the second resin layer is 600nm, and the refractive index is 1.55.

[0064] The second resin layer is pretreated and glow-cleaned.

[0065] A barrier bonding layer was formed on the surface of the second resin layer by magnetron sputtering using a silicon target at a speed of 4.0 m / min. Sputtering was performed using an MF intermediate frequency power supply with an output power of 1.0 kW and an Ar gas flow rate of 1200 sccm. The barrier bonding layer had a thickness of 1.5 nm and a refractive index of 3.3.

[0066] Magnetron sputtering was performed on the barrier bonding layer surface using a 93:7 ITO target with a target feed rate of 4 m / min. An industrial argon-hydrogen mixture (argon to hydrogen ratio 97:3) and oxygen were introduced, with a argon-hydrogen mixture to oxygen ratio of 100:3.75. The actual sputtering speed was 400 sccm for the argon-hydrogen mixture and 15 sccm for the oxygen. Sputtering was performed using a DC power supply with an output power of 18.0 kW, resulting in an amorphous ITO layer with a thickness of 30 nm and a refractive index of 1.9.

[0067] In this embodiment, the vacuum level of the equipment during magnetron sputtering is 1×10⁻⁶. -4 Pa, the purity of the target materials used is 99.99%, and the magnetic field strength of all sputtering target sites is 400GS-700GS.

[0068] Comparative Example 1

[0069] The preparation method of the amorphous ITO conductive film in this comparative example is basically the same as that in Example 1. The difference is that when the amorphous ITO layer is prepared by magnetron sputtering, the ratio of argon to hydrogen in the argon-hydrogen mixture is 96:4.

[0070] Magnetron sputtering was performed on the barrier bonding layer surface using an ITO target with a 93:7 ratio and a target feed rate of 4 m / min. An industrial argon-hydrogen mixture (argon to hydrogen ratio 96:4) and oxygen were introduced, with an argon-hydrogen mixture and oxygen ratio of 100:3.75. The actual sputtering speed was 400 sccm for the argon-hydrogen mixture and 15 sccm for the oxygen. Sputtering was performed using a DC power supply with an output power of 18.0 kW, resulting in an amorphous ITO layer with a thickness of 30 nm and a refractive index of 1.9.

[0071] Comparative Example 2

[0072] The preparation method of the amorphous ITO conductive film in this comparative example is basically the same as that in Example 1. The difference is that when the amorphous ITO layer is prepared by magnetron sputtering, the ratio of argon-hydrogen mixture to oxygen is 100:6.

[0073] Magnetron sputtering was performed on the barrier bonding layer surface using a 93:7 ITO target with a target feed rate of 4 m / min. An industrial argon-hydrogen mixture (argon to hydrogen ratio 99:1) and oxygen were introduced, with a argon-hydrogen mixture to oxygen ratio of 100:6. The actual sputtering speed was 400 sccm for the argon-hydrogen mixture and 24 sccm for the oxygen. Sputtering was performed using a DC power supply with an output power of 18.0 kW, resulting in an amorphous ITO layer with a thickness of 30 nm and a refractive index of 1.9.

[0074] Comparative Example 3

[0075] The preparation method of the amorphous ITO conductive film in this comparative example is basically the same as that in Example 1. The difference is that when preparing the amorphous ITO layer by magnetron sputtering, the argon-hydrogen mixture is replaced with argon gas.

[0076] Magnetron sputtering was performed on the barrier bonding layer surface using a 93:7 ITO target with a target feed rate of 4 m / min. Industrial gases argon and oxygen were introduced in a 100:3.75 ratio, with 400 sccm of argon and 15 sccm of oxygen used. Sputtering was performed using a DC power supply with an output power of 18.0 kW, resulting in an amorphous ITO layer with a thickness of 30 nm and a refractive index of 1.9.

[0077] Comparative Example 4

[0078] The preparation method of the amorphous ITO conductive film in this comparative example is basically the same as that in Example 1, except that the vacuum degree of the equipment during magnetron sputtering is 1×10⁻⁶. -4 Below Pa, specifically 1×10 -5 Pa.

[0079] Comparative Example 5

[0080] The preparation method of the crystalline ITO conductive film in this comparative example is as follows:

[0081] A 125μm thick PET substrate is coated with an acrylic resin coating solution to form a first resin layer. The acrylic resin coating solution is a mixture of acrylic resin and nano-silica. The thickness of the first resin layer is 800nm, and the refractive index is 1.55. An acrylic resin coating solution is then coated on the other side of the PET substrate to form a second resin layer. The acrylic resin coating solution is a mixture of acrylic resin and nano-silica. The thickness of the second resin layer is 600nm, and the refractive index is 1.55.

[0082] The second resin layer is pretreated and glow-cleaned.

[0083] A barrier bonding layer was formed on the surface of the second resin layer by magnetron sputtering using a silicon target at a speed of 4.0 m / min. Sputtering was performed using an MF intermediate frequency power supply with an output power of 1.0 kW and an Ar gas flow rate of 1200 sccm. The barrier bonding layer had a thickness of 1.5 nm and a refractive index of 3.3.

[0084] Magnetron sputtering was performed on the barrier bonding layer surface using a 93:7 ITO target with a target feed rate of 4 m / min. Industrial gases argon and oxygen were introduced in a 100:1.35 ratio, with 400 sccm of argon and 5.4 sccm of oxygen actually used. Sputtering was performed using a DC power supply with an output power of 10.5 kW, resulting in a crystalline ITO layer with a thickness of 18 nm and a refractive index of 1.9. The layer was then aged at 150 °C for 1 hour.

[0085] In this comparative example, the vacuum level of the equipment during magnetron sputtering is 3×10⁻⁶. -4 Pa, the purity of the target materials used is 99.99%, and the magnetic field strength of all sputtering target sites is 400GS-700GS.

[0086] Comparative Example 6

[0087] The preparation method of the crystalline ITO conductive film in this comparative example is basically the same as that in Comparative Example 5. The difference is that the vacuum degree of the equipment during magnetron sputtering is 1×10⁻⁶. -4 Below Pa, specifically 1×10 -5 Pa.

[0088] Performance tests were conducted on the conductive films in each embodiment and comparative example, and the test results are shown in Table 1:

[0089] Table 1. Sheet resistance of conductive films (target range 140-160 ohms)

[0090] Group Point 1 Point 2 Point 3 Point 4 5 points Point 6 7 points 8 9 10 Maximum sheet resistance Minimum sheet resistance mean sheet resistance Example 1 141 142 142 142 142 142 143 142 141 143 143 141 142 Example 2 147 148 149 148 148 147 148 149 148 148 149 147 148 Example 3 156 155 157 156 155 156 156 157 157 157 157 155 156 Comparative Example 1 175 177 176 175 175 176 175 175 175 175 177 175 175 Comparative Example 2 135 133 133 135 134 134 135 134 135 134 135 133 134 Comparative Example 3 189 189 188 189 190 191 189 189 188 189 191 188 189 Comparative Example 4 144 144 143 145 145 145 145 143 145 144 145 143 144 Comparative Example 5 220 230 245 233 235 236 244 241 235 236 245 220 236 Comparative Example 6 145 141 142 143 143 145 145 143 142 143 145 141 143

[0091] The conductive film from Example 2 was placed in an oven at 130°C for different times, and the sheet resistance of the conductive film was then tested. The results are shown in Table 2.

[0092] Table 2 Sheet resistance of conductive films (ohms)

[0093] Placement time Point 1 Point 2 Point 3 Point 4 5 points 6 o'clock 7 points 8 9 10 Maximum sheet resistance Minimum sheet resistance mean sheet resistance Original square resistance 147 148 149 148 148 147 148 149 148 148 149 147 148 1 day 146 145 145 146 145 145 149 148 147 147 149 145 146 3 days 145 145 147 145 145 145 148 147 147 148 148 145 146 5 days 148 147 150 150 151 148 149 149 148 149 151 147 149 7 days 147 149 149 148 148 149 148 148 149 151 151 147 149 10 days 148 149 148 148 149 149 147 148 150 149 150 147 149

[0094] As shown in Table 1, the argon-hydrogen mixture ratio in Examples 1-3 was within the range of (97-99):(3-1), and the average sheet resistance of the resulting conductive films was 142 ohms, 148 ohms, and 156 ohms, respectively, with the sheet resistance all within the range of 140-160 ohms, which met the requirements. Among them, the conductive film in Example 2 had better performance.

[0095] In Comparative Example 1, the ratio of argon to hydrogen was 96:4, which was too high. As a result, the sheet resistance of the conductive film was too high, with an average value of 175 ohms, which was not in the range of 140-160 ohms.

[0096] Compared to Example 1, the sputtering gas for ITO was a 99:1 argon-hydrogen mixture. The ratio of argon-hydrogen mixture to oxygen was changed from 100:3.75 to 100:6. Example 1 actually used 400 sccm of argon-hydrogen mixture and 15 sccm of oxygen, while Comparative Example 2 actually used 400 sccm of argon-hydrogen mixture and 24 sccm of oxygen. From the experimental results, the argon-hydrogen mixture to oxygen ratio in Comparative Example 2 is too high. When it is greater than 100:5, the sheet resistance is too low, with an average value of 134 ohms, which is not within the required sheet resistance range of 140-160 ohms.

[0097] Comparative Example 3 was compared with Example 1 under the same process conditions. The only difference was that the sputtering gas for ITO was changed from an argon-hydrogen mixture to argon. The experimental results showed that the average sheet resistance of Comparative Example 3 was 189 ohms, which is outside the required sheet resistance range of 140-160 ohms.

[0098] Comparative Example 3 and Comparative Example 4 were performed under the same process conditions, the only difference being the vacuum level of the magnetron sputtering machine. Comparative Example 3 had a vacuum level of 3 × 10⁻⁶. -4 Pa-1×10 -4 Between Pa, the vacuum degree of Comparative Example 4 is 1×10 -4 Below Pa, the average sheet resistance of Comparative Example 3 is 189 ohms, which is outside the required range of 140-160 ohms. The average sheet resistance of Comparative Example 4 is 144 ohms, which is within the required range of 140-160 ohms. This shows that the vacuum level of the magnetron sputtering machine is within 1×10⁻⁶ Pa. -4 For sputtering gases below Pa, argon gas can also be used to achieve sheet resistances within the range of 140-160 ohms. Pure argon sputtering requires ultra-high vacuum (e.g., 10 ohms). -5 To reduce the influence of oxidizing impurities such as O2 and H2O, the process conditions for using the argon-hydrogen mixture as the sputtering gas for non-crystalline ITO in Example 1 were demonstrated to be achievable under low vacuum conditions (vacuum degree 3 × 10⁻⁶). -4 Pa-1×10 -4 (between Pa), and can obtain a sheet resistance between 140-160 ohms.

[0099] Comparative Example 5 uses a crystalline ITO process. The preceding coating structures are the same as in Comparative Example 1, but the final ITO layer uses crystalline ITO, applied at a vacuum degree of 3×10⁻⁶. -4 Pa-1×10 -4 Between Pa, the average sheet resistance of Comparative Example 5 is 236 ohms, which is outside the required sheet resistance range of 140-160 ohms.

[0100] Comparative Example 6 and Comparative Example 5 had the same process conditions, the only difference being the vacuum level of the magnetron sputtering machine; Comparative Example 5.1 had a vacuum level of 3 × 10⁻⁶. -4 Pa-1×10 -4 Between Pa, Comparative Example 6 has a vacuum degree of 1×10 -4 Below Pa, the average sheet resistance of Comparative Example 6 is 143 ohms, which is within the sheet resistance range of 140-160 ohms. This shows that the vacuum level of the magnetron sputtering machine is within 1×10⁻⁶ ohms. -4 Below Pa, Comparative Example 6 can also achieve a sheet resistance range of 140-160 ohms, which shows that crystalline ITO also requires ultra-high vacuum (1×10⁻⁶ Pa). -4 Conductive films with a sheet resistance range of 140-160 ohms can only be prepared at a pressure below Pa. However, crystalline ITO requires an extremely high vacuum and aging at the back end, which increases the number of back-end process steps, so it is not used.

[0101] As shown in Table 2, when the conductive film samples from Example 2 were placed in an oven at 130°C to observe the change in sheet resistance, the initial average sheet resistance was 148 ohms. After 1 day, the average sheet resistance was 146 ohms, after 3 days, after 5 days, after 7 days, and after 10 days, the average sheet resistance was 149 ohms. All of these values ​​were within the sheet resistance range of 140-160 ohms, demonstrating that the sheet resistance of the conductive film in Example 2 was very stable under high temperature conditions of 130°C, with very small fluctuations and stable high temperature resistance.

[0102] It will be apparent to those skilled in the art that this disclosure is not limited to the details of the exemplary embodiments described above, and that this disclosure can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of this disclosure is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within this disclosure. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0103] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A method for preparing an amorphous ITO conductive film, characterized in that, The preparation method of the amorphous ITO conductive film includes the following steps: Take a substrate, prepare a first resin layer on one side of the substrate, and prepare a second resin layer on the other side of the substrate; A barrier bonding layer is prepared on the second resin layer; An amorphous ITO layer was prepared by magnetron sputtering on a barrier bonding layer using an ITO target. During the magnetron sputtering process, a first gas and a second gas were introduced. The first gas consisted of argon and hydrogen in a volume ratio of (97-99):(3-1), and the second gas was oxygen. The volume ratio of the first gas to the second gas was 100:(3-5). The vacuum level was 3×10⁻⁶. - 4 Pa-1×10 -4 Pa.

2. The method for preparing the amorphous ITO conductive film according to claim 1, characterized in that, The flow rate of the first gas is 390 sccm-400 sccm, and the flow rate of the second gas is 12 sccm-20 sccm.

3. The method for preparing the amorphous ITO conductive film according to claim 1, characterized in that, The mass percentage of indium oxide and tin oxide in the ITO target is 90:10-97:

3.

4. The method for preparing the amorphous ITO conductive film according to claim 1, characterized in that, During the magnetron sputtering process, the ITO target is transported at a speed of 3m / min-4m / min, and the power output is 17kW-19kW.

5. The method for preparing the amorphous ITO conductive film according to claim 1, characterized in that, A barrier bonding layer was prepared on the second resin layer by magnetron sputtering using a silicon target. During the magnetron sputtering process, the silicon target was transported at a speed of 3 m / min to 5 m / min, the power output was 0.5 kW to 2 kW, and the Ar gas flow rate was 1000 sccm to 1200 sccm.

6. A non-crystalline ITO conductive film, characterized in that, The amorphous ITO conductive film is prepared by the preparation method described in claim 1.

7. The amorphous ITO conductive film according to claim 6, characterized in that, The thickness of the amorphous ITO layer is 20nm-150nm.

8. The amorphous ITO conductive film according to claim 6, characterized in that, The barrier connection layer is a silicon-plated layer with a thickness of 1.0 nm to 1.5 nm.

9. The amorphous ITO conductive film according to claim 6, characterized in that, The first resin layer is an acrylic resin layer containing silica particles, with a thickness of 800nm-1000nm and a refractive index of 1.50-1.55; and / or, The second resin layer is an acrylic resin layer containing silica particles, with a thickness of 550nm-700nm and a refractive index of 1.50-1.

55.

10. The amorphous ITO conductive film according to claim 6, characterized in that, The substrate is a PET substrate with a thickness of 23μm-250μm.

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