High-adhesion weldable conductive copper film electrode and preparation method and application thereof

By using a Hall ion source for pre-plating cleaning and copper film deposition in the preparation of thin film electrodes, combined with vacuum heating and specific gas assistance, the problems of poor adhesion and difficult welding of copper film electrodes were solved, achieving high adhesion and reproducibility. Preparation of soldered conductive copper film electrodes.

CN119332202APending Publication Date: 2025-01-21CHINA BUILDING MATERIALS ACADEMY CO LTD
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Patent Information

Application Number
CN202411193515.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-08-28
Publication Date
2025-01-21

AI Technical Summary

Technical Problem

It is difficult to prepare copper film electrodes with good conductivity, high film-based adhesion and can be directly welded, especially in the application of thin film electrodes, with problems of welding difficulties and poor adhesion.

Method used

A Hall ion source is used for pre-plating cleaning and copper film deposition. The copper film is improved by heating and controlling deposition parameters under vacuum conditions, including using Ar/H2 mixed gas for pre-plating cleaning and O2 as an auxiliary gas for copper film deposition. adhesion and conductive properties.

Benefits of technology

A high-adhesion, weldable conductive copper film electrode is achieved, which simplifies the preparation process, reduces the cost, and improves the conductivity and adhesion of the copper film electrode.

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Abstract

The invention relates to a high-adhesion weldable conductive copper film electrode and a preparation method and application thereof. The method comprises the following steps: S1, clamping a cleaned conductive substrate to expose an electrode deposition area, and heating under a vacuum condition; and S2, the conductive substrate obtained in the step S1 is subjected to pre-plating cleaning through a Hall ion source, then copper film deposition is conducted, meanwhile, the Hall ion source is adopted for assistance, and after the vacuum chamber is cooled, the substrate is taken out. By means of the method, the copper film electrode which is good in electric conductivity, high in film base adhesive force and capable of being directly welded can be prepared, the preparation technology of the metal heating electrode is greatly simplified, and the manufacturing cost is low.
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Description

Technical Field

[0001] The invention belongs to the field of materials and films, and specifically relates to a high-adhesion, weldable conductive copper film electrode and a preparation method and application thereof. Background Art

[0002] Conductive glass is a glass with a transparent conductive film such as ITO coated on the surface. When it is used as a heating backplane to heat the LCD screen, electrodes need to be made. At present, electrodes are mostly made by coating a certain width of conductive silver paste on the edge and sintering it. The conductive silver paste is made of conductive materials such as organic polymers, silver, and copper powder. When leading out the wire on the conductive silver paste, conventional welding methods have welding difficulties and poor adhesion of the solder joints. In order to ensure the firmness of the wire, the backplane and other glass are often pressed together or coated with a layer of glue. The entire production process is relatively complicated.

[0003] "Soldering" is commonly used in the electronics industry. It is to connect metal wires and other metal materials by soldering using hot melt. It has the advantages of simple process, fewer steps, and low cost, but it is usually used for welding bulk materials. Compared with bulk materials, the metal copper film prepared by conventional vacuum method has a thin film layer and poor adhesion to the film base. When "soldering" is used, due to the large difference in thermal expansion coefficient between the copper film and the base material, the copper film expands due to heat during welding, causing the film layer to fall off directly from the base, resulting in welding failure.

[0004] The prior art discloses the welding of a transparent conductive film and a wire and the preparation of a metal electrode on the film. Through a multi-step process, a SnO2 film is prepared and then a Ni film is chemically deposited to complete the production. However, the production process is complicated. Summary of the invention

[0005] In view of this, the main purpose of the present invention is to provide a high-adhesion, weldable conductive copper film electrode and its preparation method and application. The technical problem to be solved is how to prepare a copper film electrode with good conductivity, high film-base adhesion and direct weldability.

[0006] The purpose of the present invention and the technical problem to be solved are achieved by adopting the following technical solutions. The present invention proposes a method for preparing a conductive copper film electrode with high adhesion and weldability, comprising the following steps:

[0007] S1 clamps the cleaned conductive substrate, leaving the electrode deposition area, and heats it under vacuum conditions;

[0008] S2: the conductive substrate obtained in step S1 is cleaned before plating using a Hall ion source, and then a copper film is deposited while being assisted by a Hall ion source. After the vacuum chamber is cooled, the substrate is taken out to obtain the conductive copper film electrode.

[0009] Preferably, in the aforementioned method for preparing a highly adhesive, weldable conductive copper film electrode, the cleaning of the conductive substrate in step S1 comprises: firstly ultrasonically cleaning with acetone for 10-15 min, and then ultrasonically cleaning with anhydrous ethanol for 10-15 min.

[0010] Preferably, in the above-mentioned method for preparing a conductive copper film electrode with high adhesion and weldability, the vacuum degree in step S1 is ≤3.0×10 -3 Pa.

[0011] Preferably, in the aforementioned method for preparing a high-adhesion, weldable conductive copper film electrode, the heating temperature in step S1 is 200-250° C., the temperature control accuracy is ±5° C., and the insulation time is 40-60 min.

[0012] Preferably, in the aforementioned method for preparing a high-adhesion, weldable conductive copper film electrode, the parameters for pre-plating cleaning using a Hall ion source in step S2 are set as follows: the gas is an Ar / H2 mixed gas, the total flow rate is 35-50SCCM, Ar:H2≥5, the anode voltage is 100-150v, the anode current is 2-4A, and the cleaning time is 10-15 minutes.

[0013] Preferably, in the aforementioned method for preparing a high-adhesion, weldable conductive copper film electrode, the parameters for copper film deposition in step S2 are set as follows: the purity of the copper material is 99.9%, the rate is 0.2-0.4nm / s, and the copper film thickness is 400-600nm.

[0014] Preferably, in the aforementioned method for preparing a high-adhesion, weldable conductive copper film electrode, the parameters for assisting with a Hall ion source in step S2 are set as follows: the auxiliary gas is O2, the flow rate is 30-40SCCM, the anode voltage is 150V-200V, and the anode current is 3-5A.

[0015] The purpose of the present invention and the solution to its technical problems can be further achieved by adopting the following technical measures. The present invention proposes a high-adhesion, weldable conductive copper film electrode, which is prepared by the following steps:

[0016] S1 clamps the cleaned conductive substrate, leaving the electrode deposition area, and heats it under vacuum conditions;

[0017] S2: the conductive substrate obtained in step S1 is cleaned before plating using a Hall ion source, and then a copper film is deposited while being assisted by a Hall ion source. After the vacuum chamber is cooled, the substrate is taken out to obtain the conductive copper film electrode.

[0018] Preferably, the aforementioned high-adhesion, weldable conductive copper film electrode, wherein the surface resistance of the conductive copper film electrode is 0.5-0.9Ω, and the adhesion is level 0.

[0019] The purpose of the present invention and the solution to its technical problems can be further achieved by adopting the following technical measures. The present invention proposes a transparent heated backplane glass, the transparent heated backplane glass comprises a highly adhesive and weldable conductive copper film electrode; the conductive copper film electrode is prepared by the following steps:

[0020] S1 clamps the cleaned conductive substrate, leaving the electrode deposition area, and heats it under vacuum conditions;

[0021] S2: the conductive substrate obtained in step S1 is cleaned before plating using a Hall ion source, and then a copper film is deposited while being assisted by a Hall ion source. After the vacuum chamber is cooled, the substrate is taken out to obtain the conductive copper film electrode.

[0022] By means of the above technical solution, the present invention provides a high-adhesion, weldable conductive copper film electrode and a preparation method and application thereof, which have at least the following advantages:

[0023] The method provided by the present invention can prepare copper film electrodes with good conductivity, high film-base adhesion and direct welding, which greatly simplifies the preparation process of metal heating electrodes and has low cost.

[0024] The method provided by the present invention can prepare copper film electrodes with good conductivity, high film-base adhesion, and direct solderability. Compared with the traditional silver paste coating method, it greatly simplifies the preparation process of metal heating electrodes, has fewer steps, less material used, and low cost.

[0025] The surface resistance of the conductive copper film electrode prepared by the present invention is 0.5-0.9Ω, and the adhesion is level 0.

[0026] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the preferred embodiments of the present invention are described in detail as follows. DETAILED DESCRIPTION

[0027] In order to further explain the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the following is a detailed description of the high adhesion, weldable conductive copper film electrode and its preparation method and its specific implementation method, structure, characteristics and effects proposed by the present invention in combination with the preferred embodiments. In the following description, different "one embodiment" or "embodiment" does not necessarily refer to the same embodiment. In addition, specific features, structures or characteristics in one or more embodiments may be combined in any suitable form.

[0028] The following materials or reagents, unless otherwise specified, were commercially available.

[0029] Some embodiments of the present invention provide a method for preparing a high-adhesion, weldable conductive copper film electrode proposed by the present invention, comprising the following steps:

[0030] 1) Conductive substrate cleaning: The glass substrate with the ITO conductive film on the surface is cleaned, firstly acetone is used as a cleaning agent to perform ultrasonic cleaning for 10-15 minutes to remove stains such as oil stains and fingerprints on the surface of the glass substrate, and then anhydrous ethanol is used as a cleaning agent to perform ultrasonic cleaning for 10-15 minutes to remove moisture from the surface of the glass substrate; the glass substrate with the ITO conductive film on the surface is a conventional conductive glass in the art, and the thickness of the ITO conductive film is nanometer level.

[0031] 2) The glass substrate obtained in step 1) is mounted in a card, excluding the electrode deposition area, and placed in a substrate holder in a vacuum chamber, and vacuum is drawn until the vacuum degree is ≤3.0×10 -3 Pa, the vacuum degree within this range can avoid the adverse effect of residual gas on the subsequent film preparation, turn on the resistance wire heater; the heating temperature of the resistance wire heater is 200-250℃, the temperature control accuracy is ±5℃, and the insulation time is 40-60min; selecting a heating temperature of 200-250℃ can increase the adhesion of the subsequent film layer; selecting a insulation time of 40-60min can achieve uniformity of the temperature field in the entire vacuum chamber;

[0032] 3) Using a Hall ion source to clean the glass substrate obtained in step 2) before plating, the gas is Ar / H2 mixed gas, the total flow rate is 30-50SCCM, the flow ratio Ar:H2≥5, the anode voltage is 100-150V, and the anode current is 2-4A. Under this process condition, the normal ignition and operation of the ion source can be guaranteed, and the cleaning time is 10-15 minutes;

[0033] 5) Using an electron gun to evaporate copper material with a purity of 99.9%, a crystal oscillator controls the deposition rate at a rate of 0.2-0.4 nm / s to avoid film material splashing caused by too fast a rate. The copper film thickness is 400-600 nm to ensure that a copper film with good conductivity is obtained;

[0034] 6) While depositing the copper film, a Hall ion source is used for assistance, and the auxiliary parameters are: auxiliary gas is O2, flow rate is 30-40SCCM, anode voltage is 150V-200V, and anode current is 3-5A; under this process condition, the normal ignition and operation of the ion source can be guaranteed, and the oxygen ions required for copper oxidation can be provided;

[0035] 7) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0036] In the above technical scheme, the present invention pre-cleans and fills the argon / hydrogen mixed gas, utilizes the high energy of hydrogen atoms to activate the conductive film on the conductive glass, and improves the bonding strength with the subsequent copper film. During deposition, oxygen is filled as an auxiliary, and the product is a mixture of copper and copper oxide, which overcomes the disadvantage of poor adhesion of pure copper. At the same time, by controlling the amount of oxygen filled, the copper oxide content is kept at a low level, which basically does not affect the conductivity. The present invention does not need to roughen the conductive glass, add a transition layer, etc. The manufactured electrode also has good conductivity and can be directly welded, and the steps are simpler. The thickness of the copper film electrode is at the nanometer level.

[0037] Some embodiments of the present invention also provide a high-adhesion, weldable conductive copper film electrode, which is prepared by the above method. According to tests, the conductive copper film electrode has a surface resistance of 0.5-0.9Ω and an adhesion of level 0.

[0038] Some embodiments of the present invention further provide a transparent heated backplane glass, wherein the transparent heated backplane glass comprises the above-mentioned high-adhesion, weldable conductive copper film electrode. The copper film surface resistance is tested using a contact or non-contact square resistance tester, and the adhesion is tested according to the GB / T9286-2021 standard.

[0039] The present invention is further described below in conjunction with specific embodiments.

[0040] Embodiment 1:

[0041] This embodiment provides a method for preparing a conductive copper film electrode with high adhesion and weldability, comprising the following steps:

[0042] (1) Cleaning the conductive substrate: using acetone for ultrasonic cleaning for 15 minutes, and then using anhydrous ethanol for ultrasonic cleaning for 15 minutes; the conductive substrate is a glass substrate having a nano-scale ITO conductive film on the surface;

[0043] (2) The conductive substrate is placed in the substrate holder and the vacuum degree is 3.0×10 -3 When Pa, the resistance wire heater is turned on; the heating temperature is 200℃, the temperature control accuracy is ±5℃, and the insulation time is 40min;

[0044] (3) Using a Hall ion source to clean the conductive substrate before plating, the gas is an Ar / H2 mixture, where the Ar flow rate is 30 SCCM, the H2 flow rate is 5 SCCM, and the specific cleaning parameters are as follows: the anode voltage is 100 V, the anode current is 2 A, and the cleaning time is 15 minutes;

[0045] (4) using an electron gun to evaporate copper material with a purity of 99.9%, and using a crystal oscillator to control the deposition rate at a rate of 0.2 nm / s, the copper film thickness was 600 nm;

[0046] (5) While depositing the copper film, a Hall ion source was used for assistance, and the auxiliary parameters were as follows: the auxiliary gas was O2, the flow rate was 30 SCCM, the anode voltage was 150 V, and the anode current was 3 A;

[0047] (6) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0048] The surface resistance of the conductive copper film electrode prepared in the above embodiment is 0.5Ω, and the adhesion is level 0.

[0049] Embodiment 2:

[0050] This embodiment provides a method for preparing a conductive copper film electrode with high adhesion and weldability, comprising the following steps:

[0051] (1) Cleaning the conductive substrate by ultrasonic cleaning with acetone for 15 minutes and then ultrasonic cleaning with anhydrous ethanol for 15 minutes; the conductive substrate is a glass substrate having a nano-scale ITO conductive film on the surface;

[0052] (2) The conductive substrate is placed in the substrate holder and the vacuum degree is 3.0×10 -3 When Pa, the resistance wire heater is turned on; the heating temperature is 200℃, the temperature control accuracy is ±5℃, and the insulation time is 40min;

[0053] (3) Using a Hall ion source to clean the conductive substrate before plating, the gas is an Ar / H2 mixture, where the Ar flow rate is 40 SCCM, the H2 flow rate is 5 SCCM, and the specific cleaning parameters are as follows: the anode voltage is 100 V, the anode current is 2 A, and the cleaning time is 15 minutes;

[0054] (4) using an electron gun to evaporate copper material with a purity of 99.9%, and using a crystal oscillator to control the deposition rate at a rate of 0.2 nm / s, the copper film thickness was 600 nm;

[0055] (5) While depositing the copper film, a Hall ion source was used for assistance, and the auxiliary parameters were as follows: the auxiliary gas was O2, the flow rate was 30 SCCM, the anode voltage was 150 V, and the anode current was 3 A;

[0056] (6) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0057] The surface resistance of the conductive copper film electrode prepared in the above embodiment is 0.5Ω, and the adhesion is level 0.

[0058] Embodiment 3:

[0059] This embodiment provides a method for preparing a conductive copper film electrode with high adhesion and weldability, comprising the following steps:

[0060] (1) Cleaning the conductive substrate by ultrasonic cleaning with acetone for 15 minutes and then ultrasonic cleaning with anhydrous ethanol for 15 minutes; the conductive substrate is a glass substrate having a nano-scale ITO conductive film on the surface;

[0061] (2) The conductive substrate is placed in the substrate holder and the vacuum degree is 3.0×10 -3 When Pa, the resistance wire heater is turned on; the heating temperature is 200℃, the temperature control accuracy is ±5℃, and the insulation time is 40min;

[0062] (3) Using a Hall ion source to clean the conductive substrate before plating, the gas is an Ar / H2 mixture, where the Ar flow rate is 40 SCCM, the H2 flow rate is 5 SCCM, and the specific cleaning parameters are as follows: the anode voltage is 100 V, the anode current is 2 A, and the cleaning time is 15 minutes;

[0063] (4) using an electron gun to evaporate copper material with a purity of 99.9%, and using a crystal oscillator to control the deposition rate at a rate of 0.3 nm / s, the copper film thickness was 600 nm;

[0064] (5) While depositing the copper film, a Hall ion source was used for assistance, and the auxiliary parameters were as follows: the auxiliary gas was O2, the flow rate was 30 SCCM, the anode voltage was 150 V, and the anode current was 3 A;

[0065] (6) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0066] The surface resistance of the conductive copper film electrode prepared in the above embodiment is 0.8Ω, and the adhesion is level 0.

[0067] Embodiment 4:

[0068] This embodiment provides a method for preparing a conductive copper film electrode with high adhesion and weldability, comprising the following steps:

[0069] (1) Cleaning the conductive substrate by ultrasonic cleaning with acetone for 15 minutes and then ultrasonic cleaning with anhydrous ethanol for 15 minutes; the conductive substrate is a glass substrate having a nano-scale ITO conductive film on the surface;

[0070] (2) The conductive substrate is placed in the substrate holder and the vacuum degree is 3.0×10 -3When Pa, the resistance wire heater is turned on; the heating temperature is 200℃, the temperature control accuracy is ±5℃, and the insulation time is 40min;

[0071] (3) Using a Hall ion source to clean the conductive substrate before plating, the gas is an Ar / H2 mixture, where the Ar flow rate is 40 SCCM, the H2 flow rate is 5 SCCM, and the specific cleaning parameters are as follows: the anode voltage is 100 V, the anode current is 2 A, and the cleaning time is 15 minutes;

[0072] (4) using an electron gun to evaporate copper material with a purity of 99.9%, and using a crystal oscillator to control the deposition rate at a rate of 0.2 nm / s, the copper film thickness was 600 nm;

[0073] (5) While depositing the copper film, a Hall ion source was used for assistance, and the auxiliary parameters were as follows: the auxiliary gas was O2, the flow rate was 35 SCCM, the anode voltage was 150 V, and the anode current was 3 A;

[0074] (6) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0075] The surface resistance of the conductive copper film electrode prepared in the above embodiment is 0.8Ω, and the adhesion is level 0.

[0076] Embodiment 5:

[0077] This embodiment provides a method for preparing a conductive copper film electrode with high adhesion and weldability, comprising the following steps:

[0078] (1) Cleaning the conductive substrate by ultrasonic cleaning with acetone for 15 minutes and then ultrasonic cleaning with anhydrous ethanol for 15 minutes; the conductive substrate is a glass substrate having a nano-scale ITO conductive film on the surface;

[0079] (2) The conductive substrate is placed in the substrate holder and the vacuum degree is 3.0×10 -3 When Pa, the resistance wire heater is turned on; the heating temperature is 200℃, the temperature control accuracy is ±5℃, and the insulation time is 40min;

[0080] (3) Using a Hall ion source to clean the conductive substrate before plating, the gas is an Ar / H2 mixture, where the Ar flow rate is 40 SCCM, the H2 flow rate is 5 SCCM, and the specific cleaning parameters are as follows: the anode voltage is 100 V, the anode current is 2 A, and the cleaning time is 15 minutes;

[0081] (4) using an electron gun to evaporate copper material with a purity of 99.9%, and using a crystal oscillator to control the deposition rate at a rate of 0.2 nm / s, the copper film thickness was 600 nm;

[0082] (5) While depositing the copper film, a Hall ion source was used for assistance, and the auxiliary parameters were as follows: the auxiliary gas was O2, the flow rate was 30 SCCM, the anode voltage was 200 V, and the anode current was 3 A;

[0083] (6) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0084] The surface resistance of the conductive copper film electrode prepared in the above embodiment is 0.5Ω, and the adhesion is level 0.

[0085] Embodiment 6:

[0086] This embodiment provides a method for preparing a conductive copper film electrode with high adhesion and weldability, comprising the following steps:

[0087] (1) Cleaning the conductive substrate by ultrasonic cleaning with acetone for 15 minutes and then ultrasonic cleaning with anhydrous ethanol for 15 minutes; the conductive substrate is a glass substrate having a nano-scale ITO conductive film on the surface;

[0088] (2) The conductive substrate is placed in the substrate holder and the vacuum degree is 3.0×10 -3 When Pa, the resistance wire heater is turned on; the heating temperature is 200℃, the temperature control accuracy is ±5℃, and the insulation time is 40min;

[0089] (3) Using a Hall ion source to clean the conductive substrate before plating, the gas is an Ar / H2 mixture, where the Ar flow rate is 40 SCCM, the H2 flow rate is 5 SCCM, and the specific cleaning parameters are as follows: the anode voltage is 100 V, the anode current is 2 A, and the cleaning time is 15 minutes;

[0090] (4) using an electron gun to evaporate copper material with a purity of 99.9%, and using a crystal oscillator to control the deposition rate at a rate of 0.2 nm / s, the copper film thickness was 600 nm;

[0091] (5) While depositing the copper film, a Hall ion source was used for assistance, and the auxiliary parameters were as follows: the auxiliary gas was O2, the flow rate was 30 SCCM, the anode voltage was 150 V, and the anode current was 4 A;

[0092] (6) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0093] The surface resistance of the conductive copper film electrode prepared in the above embodiment is 0.9Ω, and the adhesion is level 0.

[0094] Comparative Example 1:

[0095] This comparative example provides a method for preparing a conductive copper film electrode, comprising the following steps:

[0096] (1) Cleaning the conductive substrate by ultrasonic cleaning with acetone for 15 minutes and then ultrasonic cleaning with anhydrous ethanol for 15 minutes; the conductive substrate is a glass substrate having a nano-scale ITO conductive film on the surface;

[0097] (2) The conductive substrate is placed in the substrate holder and the vacuum degree is 3.0×10 -3 When Pa, the resistance wire heater is turned on; the heating temperature is 200℃, the temperature control accuracy is ±5℃, and the insulation time is 40min;

[0098] (3) Using a Hall ion source to clean the conductive substrate before plating, the gas is an Ar / H2 mixture, where the Ar flow rate is 40 SCCM, the H2 flow rate is 5 SCCM, and the specific cleaning parameters are as follows: the anode voltage is 100 V, the anode current is 2 A, and the cleaning time is 15 minutes;

[0099] (4) using an electron gun to evaporate copper material with a purity of 99.9%, and using a crystal oscillator to control the deposition rate at a rate of 0.2 nm / s, the copper film thickness was 600 nm;

[0100] (5) While depositing the copper film, a Hall ion source was used for assistance, and the auxiliary parameters were as follows: the auxiliary gas was Ar, the flow rate was 30 SCCM, the anode voltage was 150 V, and the anode current was 3 A;

[0101] (6) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0102] The conductive copper film electrode prepared in the above comparative example has a surface resistance of 0.2Ω and an adhesion of level 5.

[0103] Comparative Example 2:

[0104] This comparative example provides a method for preparing a conductive copper film electrode, comprising the following steps:

[0105] (1) Cleaning a conductive substrate by ultrasonic cleaning with acetone for 15 minutes and then ultrasonic cleaning with anhydrous ethanol for 15 minutes; the substrate is a glass substrate having a nano-scale ITO conductive film on the surface;

[0106] (2) The conductive substrate is placed in the substrate holder and the vacuum degree is 3.0×10 -3 When Pa, the resistance wire heater is turned on; the heating temperature is 200℃, the temperature control accuracy is ±5℃, and the insulation time is 40min;

[0107] (3) Using a Hall ion source to clean the conductive substrate before plating, the gas is an Ar / H2 mixture, where the Ar flow rate is 40 SCCM, the H2 flow rate is 5 SCCM, and the specific cleaning parameters are as follows: the anode voltage is 100 V, the anode current is 2 A, and the cleaning time is 15 minutes;

[0108] (4) using an electron gun to evaporate copper material with a purity of 99.9%, and using a crystal oscillator to control the deposition rate at a rate of 0.2 nm / s, the copper film thickness was 600 nm;

[0109] (5) While depositing the copper film, a Hall ion source was used for assistance, and the auxiliary parameters were as follows: the auxiliary gas was O2, the flow rate was 30 SCCM, the anode voltage was 150 V, and the anode current was 1 A;

[0110] (6) Turn off the evaporation source, ion source, heating and vacuum system, and after the vacuum chamber cools down, take out the substrate to obtain the conductive copper film electrode.

[0111] The surface resistance of the conductive copper film electrode prepared in the above comparative example is 0.4Ω, and the adhesion is level 3.

[0112] By comparing Examples 1-6 and Comparative Examples 1-2, it can be seen that when auxiliary deposition is performed, only Ar gas is filled, and the plated film layer is a pure copper film. Although a low surface resistance can be obtained, the adhesion is very poor and can only reach level 5. This is because the bonding force between the deposited copper film and the ITO glass is only the van der Waals force, and the bonding force is low; in addition, when O2 is filled during auxiliary deposition, but the ion source anode current is low, the adhesion of the prepared copper film is still insufficient. This is because after O2 is filled, a mixture of copper oxide and copper is generated on the surface of the ITO glass. In addition to the van der Waals force, there is also some chemical bonding force, and the adhesion is stronger than that of pure copper, but the lower ion source anode current provides insufficient energy to the deposited particles, resulting in the film layer adhesion still not reaching level 0.

[0113] In the above embodiments, the description of each embodiment has its own emphasis. For parts that are not described in detail in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

[0114] The numerical range described in the present invention includes all the numerical values ​​within the range, and includes the range value formed by any two numerical values ​​within the range. Different numerical values ​​of the same indicator appearing in all embodiments of the present invention can be arbitrarily combined to form a range value.

[0115] The technical features in the claims and / or the specification of the present invention may be combined, and the combination is not limited to the combination obtained by reference in the claims. The technical solution obtained by combining the technical features in the claims and / or the specification is also within the protection scope of the present invention.

[0116] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any form. Any simple modification, equivalent change and modification made to the above embodiment according to the technical essence of the present invention still falls within the scope of the technical solution of the present invention.

Claims

1. A method for preparing a high-adhesion, weldable conductive copper film electrode, characterized in that: The following steps are involved: S1 clamps the cleaned conductive substrate, leaving the electrode deposition area, and heats it under vacuum conditions; S2: the conductive substrate obtained in step S1 is cleaned before plating using a Hall ion source, and then a copper film is deposited while being assisted by a Hall ion source. After the vacuum chamber is cooled, the substrate is taken out to obtain the conductive copper film electrode.

2. The method for preparing a conductive copper film electrode having high adhesion and being weldable according to claim 1, characterized in that: The cleaning of the conductive substrate in step S1 includes: firstly using acetone for ultrasonic cleaning for 10-15 minutes, and then using anhydrous ethanol for ultrasonic cleaning for 10-15 minutes.

3. The method for preparing a conductive copper film electrode having high adhesion and being weldable as claimed in claim 1, characterized in that: The vacuum degree in step S1 is ≤3.0×10 -3 Pa.

4. The method for preparing a high-adhesion, weldable conductive copper film electrode according to claim 1, characterized in that: The heating temperature in step S1 is 200-250°C, the temperature control accuracy is ±5°C, and the insulation time is 40-60min.

5. The method for preparing a high-adhesion, weldable conductive copper film electrode according to claim 1, characterized in that: The parameters for pre-plating cleaning using the Hall ion source described in step S2 are set as follows: the gas is Ar / H2 mixed gas, the total flow rate is 35-50SCCM, Ar:H2≥5, the anode voltage is 100-150v, the anode current is 2-4A, and the cleaning time is 10-15 minutes.

6. The method for preparing a conductive copper film electrode having high adhesion and being weldable according to claim 1, characterized in that: The parameters of the copper film deposition in step S2 are set as follows: the purity of the copper material is 99.9%, the rate is 0.2-0.4 nm / s, and the thickness of the copper film is 400-600 nm.

7. The method for preparing a conductive copper film electrode having high adhesion and being weldable as claimed in claim 1, characterized in that: The parameters of the Hall ion source for assisting in step S2 are set as follows: the assisting gas is O2, the flow rate is 30-40 SCCM, the anode voltage is 150V-200V, and the anode current is 3-5A.

8. A high-adhesion, weldable conductive copper film electrode, characterized in that: The conductive copper film electrode is prepared by the following steps: S1 clamps the cleaned conductive substrate, leaving the electrode deposition area, and heats it under vacuum conditions; S2: the conductive substrate obtained in step S1 is cleaned before plating using a Hall ion source, and then a copper film is deposited while being assisted by a Hall ion source. After the vacuum chamber is cooled, the substrate is taken out to obtain the conductive copper film electrode.

9. The high-adhesion, weldable conductive copper film electrode according to claim 8, characterized in that: The surface resistance of the conductive copper film electrode is 0.5-0.9Ω, and the adhesion is level 0.

10. A transparent heated back panel glass, characterized in that: The transparent heated back plate glass comprises a conductive copper film electrode with high adhesion and weldability; the conductive copper film electrode is prepared by the following steps: S1 clamps the cleaned conductive substrate, leaving the electrode deposition area, and heats it under vacuum conditions; S2: the conductive substrate obtained in step S1 is cleaned before plating using a Hall ion source, and then a copper film is deposited while being assisted by a Hall ion source. After the vacuum chamber is cooled, the substrate is taken out to obtain the conductive copper film electrode.