CN114351089A - Composite transparent conductive film and preparation method thereof - Google Patents
Composite transparent conductive film and preparation method thereof Download PDFInfo
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- CN114351089A CN114351089A CN202210000728.9A CN202210000728A CN114351089A CN 114351089 A CN114351089 A CN 114351089A CN 202210000728 A CN202210000728 A CN 202210000728A CN 114351089 A CN114351089 A CN 114351089A
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Abstract
The invention discloses a composite transparent conductive film and a preparation method thereof, wherein the preparation method comprises the following steps: s1, substrate pretreatment: cleaning the surface of the substrate to ensure that the surface of the substrate is clean and free of impurities and drying; s2, preparing a first oxide layer: depositing a first oxide layer on the substrate by using a radio frequency magnetron sputtering method; s3, preparing a metal layer: depositing a metal layer on the first oxide layer by using a direct-current magnetron sputtering method; s4, preparing a second oxide layer: and depositing a second oxide layer on the metal layer by using a radio frequency magnetron sputtering method. The composite transparent conductive film and the preparation method thereof have the characteristics of simple preparation process, excellent photoelectric property, low cost and wide application.
Description
Technical Field
The invention relates to the technical field of photoelectric thin films, in particular to a composite transparent conductive thin film and a preparation method thereof.
Background
The transparent conductive film is a photoelectric device material with high visible light transmittance and good conductivity, and is widely applied to the field of photoelectric devices such as touch screens, displays, light-emitting diodes, solar cells and the like. The major transparent conductive film on the market today is an Indium Tin Oxide (ITO) film. However, the ITO film has the characteristics of high price, containing noble metal element indium, high temperature required in the preparation process, incompatibility with a flexible substrate and the like. The development of a novel high-performance transparent conductive film for replacing ITO has great significance for the development of photoelectric devices. The oxide/metal/oxide sandwich structure composite transparent conductive film has the potential to achieve high transmittance and low resistivity. How to obtain the high-performance oxide/metal/oxide structure composite transparent conductive film by adopting a simple preparation process is a great problem to be solved. .
Disclosure of Invention
The invention aims to provide a composite transparent conductive film and a preparation method thereof, and the composite transparent conductive film has the characteristics of simple preparation process, excellent photoelectric property, low cost and wide application.
The invention can be realized by the following technical scheme:
the invention discloses a preparation method of a composite transparent conductive film, which comprises the following steps:
s1, substrate pretreatment: cleaning the surface of the substrate to ensure that the surface of the substrate is clean and free of impurities and drying;
s2, preparing a first oxide layer: depositing a first oxide layer on the substrate by using a radio frequency magnetron sputtering method;
s3, preparing a metal layer: depositing a metal layer on the first oxide layer by using a direct-current magnetron sputtering method;
s4, preparing a second oxide layer: and depositing a second oxide layer on the metal layer by using a radio frequency magnetron sputtering method.
Further, in step S2 and step S4, the conditions of the rf magnetron sputtering are as follows: the sputtering power is 50-300W, the working gas is argon with the purity of more than 99.999%, and the flow of the working argon is 10-50 sccm.
Further, in step S3, the conditions of the dc magnetron sputtering are: the sputtering power is 40-100W, the working gas is argon and oxygen with the purity of more than 99.999%, and the flow ratio of the argon to the oxygen is 1: 1-100: 1.
Further, the first metal oxide layer is gallium-aluminum co-doped zinc oxide; the thickness of the first metal oxide layer is 5-50 nm.
Further, the metal layer is a silver film; the thickness of the silver film is 5-15 nm.
Further, the second metal oxide layer is GAZO; the thickness of the second metal oxide layer is 5-50 nm.
Further, the substrate is glass, plastic, ceramic or silicon wafer.
The invention also provides a composite transparent conductive film prepared by the preparation method of the composite transparent conductive film.
The composite transparent conductive film and the preparation method thereof have the following beneficial effects:
the preparation method is simple in preparation process, the GAZO is adopted as the oxide layer, the transmissivity is high, the performance is stable, the thickness is only 5-50 nm, and the preparation process is simple and convenient;
secondly, the photoelectric property is excellent, the composite transparent conductive film is prepared by adopting a GAZO/Ag/GAZO structure, and the composite transparent conductive film has the characteristics of high transmissivity and low resistivity;
thirdly, the cost is low, the transparent conductive film is prepared by adopting a multi-source magnetron sputtering system in the preparation method, the operation flow is simple, the repeatability is good, and the preparation cost is effectively saved;
fourthly, the GAZO/Ag/GAZO transparent conductive film prepared by the invention can be widely applied to photoelectric devices, such as: the field of photoelectric devices such as organic solar cells, light-emitting diodes and the like.
Drawings
FIG. 1 is a schematic structural view of a composite transparent conductive film according to embodiment 8 of the present invention;
FIG. 2 is a transmittance spectrum of the composite transparent conductive film according to examples 1 to 4 of the present invention;
FIG. 3 is a transmittance spectrum of the composite transparent conductive film according to examples 5 to 7 of the present invention;
the reference numbers in the drawings include: 100. a substrate; 200. a first oxide layer; 300. a metal layer; 400. A second oxide layer. .
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the following detailed description of the present invention is provided with reference to the accompanying drawings.
The invention discloses a preparation method of a composite transparent conductive film, which comprises the following steps:
s1, substrate pretreatment: cleaning the surface of the substrate to ensure that the surface of the substrate is clean and free of impurities and drying;
s2, preparing a first oxide layer: depositing a first oxide layer on the substrate by using a radio frequency magnetron sputtering method;
s3, preparing a metal layer: depositing a metal layer on the first oxide layer by using a direct-current magnetron sputtering method;
s4, preparing a second oxide layer: and depositing a second oxide layer on the metal layer by using a radio frequency magnetron sputtering method.
Further, in step S2 and step S4, the conditions of the rf magnetron sputtering are as follows: the sputtering power is 50-300W, the working gas is argon with the purity of more than 99.999%, and the flow of the working argon is 10-50 sccm.
Further, in step S3, the conditions of the dc magnetron sputtering are: the sputtering power is 40-100W, the working gas is argon and oxygen with the purity of more than 99.999%, and the flow ratio of the argon to the oxygen is 1: 1-100: 1.
Further, the first metal oxide layer is gallium-aluminum co-doped zinc oxide; the thickness of the first metal oxide layer is 5-50 nm.
Further, the metal layer is a silver film; the thickness of the silver film is 5-15 nm.
Further, the second metal oxide layer is GAZO; the thickness of the second metal oxide layer is 5-50 nm.
Further, the substrate is glass, plastic, ceramic or silicon wafer.
The invention also provides a composite transparent conductive film prepared by the preparation method of the composite transparent conductive film.
Example 1
(1) Cleaning a substrate: placing a 2 cm multiplied by 2 cm soda-lime glass substrate in a film-developing frame and putting the film-developing frame into a beaker, and respectively adding acetone, a detergent, deionized water and absolute ethyl alcohol into the beaker to perform primary ultrasonic cleaning for 15 min;
(2) drying the substrate: and (3) putting the cleaned glass substrate into a vacuum oven, and drying at 70-80 ℃.
(3) Depositing the GAZO film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is GAZO (Ga)2O3:Al2O3ZnO =1:2:97 wt%), setting the radio frequency sputtering power to be 200W, the argon flow to be 20 sccm, and the deposition thickness to be 40 nm;
(4) depositing an Ag film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is Ag, the purity is 99.99%, the direct-current sputtering power is set to be 50W, the argon flow is 15 sccm, the oxygen flow is 0.5 sccm, and the deposition thickness is 12 nm;
(5) and (4) repeating the step (3) to obtain the GAZO/Ag/GAZO composite transparent conductive film.
Example 2
(1) Cleaning a substrate: placing a 2 cm multiplied by 2 cm soda-lime glass substrate in a film-developing frame and putting the film-developing frame into a beaker, and respectively adding acetone, a detergent, deionized water and absolute ethyl alcohol into the beaker to perform primary ultrasonic cleaning for 15 min;
(2) drying the substrate: and (3) putting the cleaned glass substrate into a vacuum oven, and drying at 70-80 ℃.
(3) Depositing the GAZO film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is GAZO (Ga)2O3:Al2O3ZnO =1:2:97 wt%), setting the radio frequency sputtering power to be 200W, the argon flow to be 20 sccm, and the deposition thickness to be 40 nm;
(4) depositing an Ag film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is Ag, the purity is 99.99%, the direct-current sputtering power is set to be 50W, the argon flow is 15 sccm, the oxygen flow is 1.0 sccm, and the deposition thickness is 12 nm;
(5) and (4) repeating the step (3) to obtain the GAZO/Ag/GAZO composite transparent conductive film.
Example 3
(1) Cleaning a substrate: placing a 2 cm multiplied by 2 cm soda-lime glass substrate in a film-developing frame and putting the film-developing frame into a beaker, and respectively adding acetone, a detergent, deionized water and absolute ethyl alcohol into the beaker to perform primary ultrasonic cleaning for 15 min;
(2) drying the substrate: and (3) putting the cleaned glass substrate into a vacuum oven, and drying at 70-80 ℃.
(3) Depositing the GAZO film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is GAZO (Ga)2O3:Al2O3ZnO =1:2:97 wt%), setting the radio frequency sputtering power to be 200W, the argon flow to be 20 sccm, and the deposition thickness to be 40 nm;
(4) depositing an Ag film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is Ag, the purity is 99.99%, the direct-current sputtering power is set to be 50W, the argon flow is 15 sccm, the oxygen flow is 1.5 sccm, and the deposition thickness is 12 nm;
(5) and (4) repeating the step (3) to obtain the GAZO/Ag/GAZO composite transparent conductive film.
Example 4
(1) Cleaning a substrate: placing a 2 cm multiplied by 2 cm soda-lime glass substrate in a film-developing frame and putting the film-developing frame into a beaker, and respectively adding acetone, a detergent, deionized water and absolute ethyl alcohol into the beaker to perform primary ultrasonic cleaning for 15 min;
(2) drying the substrate: and (3) putting the cleaned glass substrate into a vacuum oven, and drying at 70-80 ℃.
(3) Depositing the GAZO film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is GAZO (Ga)2O3:Al2O3ZnO =1:2:97 wt%), setting the radio frequency sputtering power to be 200W, the argon flow to be 20 sccm, and the deposition thickness to be 40 nm;
(4) depositing an Ag film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is Ag, the purity is 99.99%, the direct-current sputtering power is set to be 50W, the argon flow is 15 sccm, the oxygen flow is 3.0 sccm, and the deposition thickness is 12 nm;
(5) and (4) repeating the step (3) to obtain the GAZO/Ag/GAZO composite transparent conductive film.
Example 5
(1) Cleaning a substrate: placing a 2 cm multiplied by 2 cm soda-lime glass substrate in a film-developing frame and putting the film-developing frame into a beaker, and respectively adding acetone, a detergent, deionized water and absolute ethyl alcohol into the beaker to perform primary ultrasonic cleaning for 15 min;
(2) drying the substrate: and (3) putting the cleaned glass substrate into a vacuum oven, and drying at 70-80 ℃.
(3) Depositing the GAZO film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is GAZO (Ga)2O3:Al2O3ZnO =1:2:97 wt%), setting the radio frequency sputtering power to be 200W, the argon flow to be 20 sccm, and the deposition thickness to be 40 nm;
(4) depositing an Ag film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is Ag, the purity is 99.99%, the direct-current sputtering power is set to be 50W, the argon flow is 15 sccm, the oxygen flow is 1.0 sccm, and the deposition thickness is 10 nm;
(5) and (4) repeating the step (3) to obtain the GAZO/Ag/GAZO composite transparent conductive film.
Example 6
(1) Cleaning a substrate: placing a 2 cm multiplied by 2 cm soda-lime glass substrate in a film-developing frame and putting the film-developing frame into a beaker, and respectively adding acetone, a detergent, deionized water and absolute ethyl alcohol into the beaker to perform primary ultrasonic cleaning for 15 min;
(2) drying the substrate: and (3) putting the cleaned glass substrate into a vacuum oven, and drying at 70-80 ℃.
(3) Depositing the GAZO film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is GAZO (Ga)2O3:Al2O3ZnO =1:2:97 wt%), setting the radio frequency sputtering power to be 200W, the argon flow to be 20 sccm, and the deposition thickness to be 40 nm;
(4) depositing an Ag film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is Ag, the purity is 99.99%, the direct-current sputtering power is set to be 50W, the argon flow is 15 sccm, the oxygen flow is 1.0 sccm, and the deposition thickness is 8 nm;
(5) and (4) repeating the step (3) to obtain the GAZO/Ag/GAZO composite transparent conductive film.
Example 7
(1) Cleaning a substrate: placing a 2 cm multiplied by 2 cm soda-lime glass substrate in a film-developing frame and putting the film-developing frame into a beaker, and respectively adding acetone, a detergent, deionized water and absolute ethyl alcohol into the beaker to perform primary ultrasonic cleaning for 15 min;
(2) drying the substrate: and (3) putting the cleaned glass substrate into a vacuum oven, and drying at 70-80 ℃.
(3) Depositing the GAZO film at room temperature by adopting a multi-source magnetron sputtering device, wherein the target material is GAZO (Ga)2O3:Al2O3ZnO =1:2:97 wt%), setting the radio frequency sputtering power to be 200W, the argon flow to be 20 sccm, and the deposition thickness to be 40 nm;
(4) depositing an Ag film by adopting a multi-source magnetron sputtering device at room temperature, wherein the target material is Ag, the purity is 99.99%, the direct-current sputtering power is set to be 50W, the argon flow is 15 sccm, the oxygen flow is 1.0 sccm, and the deposition thickness is 14 nm;
(5) and (4) repeating the step (3) to obtain the GAZO/Ag/GAZO composite transparent conductive film.
Example 8
Another aspect of the present invention is to protect the composite transparent conductive film prepared by the above method for preparing a composite transparent conductive film, which has a structure as shown in fig. 1, and includes a substrate 100, a first oxide layer 200, a metal layer 300, and a second oxide layer 400. The structure deposited on the substrate can be a GAZO/Ag/GAZO transparent conductive film.
In order to evaluate the actual effect of the present invention, the test results of the photoelectric performance test on the transparent conductive film of the embodiment are shown in fig. 2 to 3 and tables 1 to 2. FIG. 2 shows transmittance spectra of GAZO/Ag/GAZO transparent conductive films prepared in examples 1-4. Table 1 shows the photoelectric property parameters of the GAZO/Ag/GAZO transparent conductive films prepared in examples 1-4. The average transmission of examples 1-3 all exceeded 90%, with the average transmission of example 2 being the highest. The sheet resistances of examples 1 to 4 were increased in order, which indicates that the higher the oxygen doping concentration, the higher the sample resistivity. Example 3 has the highest quality factor, indicating that the overall photoelectric properties are superior. FIG. 3 shows transmittance spectra of GAZO/Ag/GAZO transparent conductive films prepared in examples 5-7. Table 2 shows the photoelectric properties of the GAZO/Ag/GAZO transparent conductive films prepared in examples 5-7. Example 6 achieved an average transmission of 95.93%, which is far in excess of examples 5 and 7, indicating that Ag film thickness has a significant effect on the transmission of the sample. An appropriate Ag film thickness can achieve a relatively high quality factor.
TABLE 1 test results of examples 1 to 4
| Examples | Square resistance/(omega/sq) | Carrier concentration/(10)21cm-3) | Mobility/(cm)2V-1s-1) | Average Transmission/(%) | Quality factor/omega-1 |
| 1 | 8.77 | 6.57 | 12.03 | 92.64 | 552 |
| 2 | 10.07 | 7.08 | 9.73 | 96.20 | 957 |
| 3 | 11.3 | 6.82 | 8.96 | 94.11 | 541 |
| 4 | 44.1 | 6.19 | 2.54 | 76.90 | 30 |
Table 2 examples 5-7 test results
| Examples | Square resistance/(omega/sq) | Carrier concentration/(10)21cm-3) | Mobility/(cm)2V-1s-1) | Average Transmission/(%) | Quality factor/omega-1 |
| 5 | 20.82 | 5.07 | 6.72 | 87.58 | 132 |
| 6 | 14.40 | 6.20 | 7.79 | 95.93 | 624 |
| 7 | 7.03 | 7.86 | 12.02 | 84.67 | 309 |
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; either directly or indirectly through intervening media, either internally or in any other relationship. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The above embodiments are only specific embodiments of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications are possible without departing from the inventive concept, and such obvious alternatives fall within the scope of the invention.
Claims (8)
1. A preparation method of a composite transparent conductive film is characterized by comprising the following steps:
s1, substrate pretreatment: cleaning the surface of the substrate to ensure that the surface of the substrate is clean and free of impurities and drying;
s2, preparing a first oxide layer: depositing a first oxide layer on the substrate by using a radio frequency magnetron sputtering method;
s3, preparing a metal layer: depositing a metal layer on the first oxide layer by using a direct-current magnetron sputtering method;
s4, preparing a second oxide layer: and depositing a second oxide layer on the metal layer by using a radio frequency magnetron sputtering method.
2. The method for preparing a composite transparent conductive film according to claim 1, wherein: in step S2 and step S4, the conditions of the rf magnetron sputtering are: the sputtering power is 50-300W, the working gas is argon with the purity of more than 99.999%, and the flow of the working argon is 10-50 sccm.
3. The method for preparing a composite transparent conductive film according to claim 2, wherein: in step S3, the conditions of the dc magnetron sputtering are: the sputtering power is 40-100W, the working gas is argon and oxygen with the purity of more than 99.999%, and the flow ratio of the argon to the oxygen is 1: 1-100: 1.
4. The method for preparing a composite transparent conductive film according to claim 3, wherein: the first metal oxide layer is gallium-aluminum co-doped zinc oxide; the thickness of the first metal oxide layer is 5-50 nm.
5. The method for preparing the composite transparent conductive film according to claim 4, wherein: the metal layer is a silver film; the thickness of the silver film is 5-15 nm.
6. The method for preparing a composite transparent conductive film according to claim 5, wherein: the second metal oxide layer is GAZO; the thickness of the second metal oxide layer is 5-50 nm.
7. The method for preparing a composite transparent conductive film according to claim 6, wherein: the substrate is glass, plastic, ceramic or silicon chip.
8. The composite transparent conductive film prepared by the method for preparing the composite transparent conductive film according to any one of claims 1 to 7.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002025362A (en) * | 2000-07-04 | 2002-01-25 | Nitto Denko Corp | Manufacturing method of silver series transparent conductive thin film and transparent laminate |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002025362A (en) * | 2000-07-04 | 2002-01-25 | Nitto Denko Corp | Manufacturing method of silver series transparent conductive thin film and transparent laminate |
Non-Patent Citations (4)
| Title |
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| HEON KONG.ET.AL.: "High performance flexible transparent conductive electrode based on ZnO/AgOx/ZnO multilayer", 《THIN SOLID FILMS》 * |
| WEI WANG ET.AL.: "Transparent Ultrathin Oxygen-Doped Silver Electrodes for Flexible Organic Solar Cells", 《ADVANCED FUNCTIONAL MATERIALS》 * |
| YU SUP JUNG.ET.AL.: "Properties of GAZO/Ag/GAZO multilayer films prepared by FTS system", 《MICROELECTRONIC ENGINEERING》 * |
| 罗国平等: "射频功率和工作压强对Ga、Al 共掺杂ZnO 薄膜性能的影响", 《材料导报》 * |
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