CN110648783A - ITO thin film and transparent conductive thin film - Google Patents
ITO thin film and transparent conductive thin film Download PDFInfo
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Abstract
Provided are an ITO film and a transparent conductive film, wherein the ITO film improves the stability of an amorphous ITO film without annealing treatment, the resistance value does not change with time, the moisture resistance and the gas barrier property are improved, and cracks caused by bending are overcome; the transparent conductive film has excellent conductivity, transparency and durability. The ITO thin film of the present invention is characterized in that an amorphous ITO film is formed on the surface of a flexible substrate in a state of not being annealed, the film thickness of the amorphous ITO film is within a range of 30nm to 320nm, and the surface resistance of the amorphous ITO film is within a range of 9 to 105 (omega/□).
Description
Technical Field
The present invention particularly relates to an ITO thin film and a transparent conductive thin film which are suitable for illumination using a solar cell, an organic EL display, and an organic EL.
Background
Transparent conductive films are used for touch panels, solar cells, electromagnetic wave/electrostatic shielding, and ultraviolet/infrared shielding, and particularly in illumination using solar cells, organic EL displays, and organic EL, performances of total light transmittance of 90% and surface resistance of 5 to 10(Ω/□) have been demanded.
However, patent document 1 discloses that an amorphous ITO film is used without annealing (example 5 and comparative example 4).
Documents of the prior art
Patent document
Patent document 1: japanese patent No. 6106756
Disclosure of Invention
Technical problem to be solved by the invention
Therefore, although example 5 has high transparency when silica is formed on the ITO film, comparative example 4 has low transparency and scratch resistance because silica is not formed on the ITO film.
In patent document 1, in order to reduce the resistance of the ITO film, the thickness of the ITO film is increased to 90nm, and SnO is added to improve the stability of the ITO film2The content was 10 wt%.
The object of the present invention is to provide an ITO film which improves the stability of an amorphous ITO film without annealing treatment, has no change in resistance value with time, improves moisture resistance and gas barrier properties, and overcomes cracks caused by bending; also provided is a transparent conductive film having excellent conductivity, transparency and durability.
Solution for solving the above technical problem
The ITO thin film of the present invention according to claim 1, which is characterized in that an amorphous ITO film is formed on a surface of a flexible substrate without being annealed, wherein the amorphous ITO film has a film thickness in the range of 30nm to 320nm, and the surface resistance of the amorphous ITO film is in the range of 9 to 105(Ω/□).
The invention described in claim 2 is characterized in that the ITO film described in claim 1 uses polyethylene terephthalate as the base material.
The invention described in claim 3 is characterized in that, in the ITO thin film described in claim 1 or 2, the film density of the amorphous ITO film is 65% or more.
The invention described in claim 4 is characterized in that, in the ITO thin film described in any one of claims 1 to 3, the surface average roughness of the amorphous ITO film is 9nm or less.
The invention described in claim 5 is characterized in that, in the ITO thin film described in any one of claims 1 to 4, SnO contained in the amorphous ITO film2In the range of 2 to 7 wt%.
The transparent conductive thin film according to claim 6 of the present invention is a transparent conductive thin film in which a first ITO film is formed on a surface of a flexible base material, a thin film metal layer is formed on a surface of the first ITO film, and a second ITO film is formed on a surface of the thin film metal layer, wherein the first ITO film is an amorphous ITO film in a state of not being annealed; the second ITO film is an amorphous ITO film which is not subjected to the annealing treatment, the film thickness of the second ITO film is within a range of 30nm to 320nm, and the surface resistance of the amorphous ITO film is within a range of 9 to 105 (omega/□).
The invention described in claim 7 is the transparent conductive film described in claim 6, wherein the film metal layer is an Ag layer having a thickness of 10nm to 20 nm.
The invention described in claim 8 is the transparent conductive film described in claim 6 or 7, wherein polyethylene terephthalate is used as the base material.
The invention described in claim 9 is the transparent conductive thin film according to any one of claims 6 to 8, wherein the second ITO film has a film density of 65% or more.
The invention described in claim 10 is the transparent conductive thin film according to any one of claims 6 to 9, wherein the second ITO film has a surface average roughness of 9nm or less.
Technical scheme 11 the present inventionFurthermore, in the transparent conductive thin film according to any one of claims 6 to 10, SnO contained in the second ITO film2In the range of 2 to 7 wt%.
Effects of the invention
According to the present invention, an ITO thin film which has an unchanged resistance value with time, is improved in moisture resistance and gas barrier properties, and is free from cracks caused by bending can be provided.
Further, according to the present invention, a transparent conductive film having excellent conductivity, transparency, and durability can be provided.
Drawings
Fig. 1 is a table showing the measurement results of the hall numbers using example 1 and comparative example 1.
FIG. 2 is a graph showing the results of a bending test using example 2 and comparative example 1 with a diameter of 1.0 mm.
Fig. 3 is a graph showing the results of the no-load bending test using example 2 and comparative example 1.
FIG. 4 is a graph showing the results of storage characteristics at 80 ℃ in example 2.
FIG. 5 is a graph showing the results of storage characteristics at 60 ℃ and 90% RH using example 2.
FIG. 6 is a graph showing the results of thermal cycling tests at-30 ℃ and 80 ℃ using example 2.
FIG. 7 is a table showing the results of heat resistance of the composition obtained in example 3, comparative example 2 and comparative example 3.
FIG. 8 is a table showing the results of a depth test using 50 ℃ hot water in example 3, comparative example 2 and comparative example 3.
FIG. 9 is a table showing the results of a depth test using 60 to 80 ℃ hot water in example 3, comparative example 2, and comparative example 3.
FIG. 10 is a table showing the results of the test conducted by allowing the test pieces of example 3, comparative example 2 and comparative example 3 to stand at room temperature in the atmosphere.
Fig. 11 is a graph showing the results of the no-load bending test using example 3 and comparative example 3.
FIG. 12 is a microphotograph of the surfaces of the ITO thin films of example 1 and comparative example 1.
Fig. 13 is a graph showing the results of measuring the surface roughness of the test piece shown in fig. 12.
Detailed Description
According to the ITO thin film of embodiment 1 of the present invention, the thickness of the amorphous ITO film is in the range of 30nm to 320nm, and the surface resistance of the amorphous ITO film is in the range of 9 to 105(Ω/□). According to the present embodiment, by providing an amorphous ITO film with a high density, stability can be improved, and an ITO film that has no change in resistance over time, has improved moisture resistance and gas barrier properties, and is resistant to cracking due to bending can be provided.
Embodiment 4 of the present invention is the ITO thin film according to embodiments 1 to 3, wherein the surface average roughness of the amorphous ITO film is 9nm or less. According to this embodiment, by setting the surface average roughness of the amorphous ITO film to 9nm or less, the film density of the amorphous ITO film can be set to 65% or more, and the stability can be improved.
In the transparent conductive thin film according to embodiment 6 of the present invention, the first ITO film is an amorphous ITO film in a state where annealing is not performed, the second ITO film is an amorphous ITO film in a state where annealing is not performed, the film thickness is in a range of 30nm to 320nm, and the surface resistance of the amorphous ITO film is in a range of 9 to 105(Ω/□). According to the present embodiment, a transparent conductive film having excellent conductivity, transparency, and durability can be provided.
In embodiment 7 of the present invention, in the transparent conductive film according to embodiment 6, the thin film metal layer is an Ag layer having a thickness of 10nm to 20 nm. According to this embodiment, Ag having poor durability can be protected by the second ITO film to improve durability, and the total light transmittance of Ag of about 50% can be improved to about 90% by the second ITO film.
Embodiment 9 of the present invention is the transparent conductive thin film according to embodiments 6 to 8, wherein the film density of the second ITO film is 65% or more. According to this embodiment, stability can be improved by setting the film density of the amorphous ITO film to 65% or more.
In embodiment 10 of the present invention, in the transparent conductive thin film according to embodiments 6 to 9, the surface average roughness of the second ITO film is 9nm or less. According to this embodiment, by setting the surface average roughness of the amorphous ITO film to 9nm or less, the film density of the amorphous ITO film can be set to 65% or more, and the stability can be improved.
Embodiment 11 of the present invention is the transparent conductive thin film according to embodiments 6 to 10, wherein SnO contained in the second ITO film is used2In the range of 2 to 7 wt%. According to this embodiment, SnO is used2The transparency can be improved within the range of 2 to 7 wt%.
(example 1)
Both surfaces of PET (polyethylene terephthalate) having a thickness of 125 μm were subjected to hard coating treatment to form a base material using a catalyst containing 5 wt% SnO2The ITO target of (1) is formed on one surface of the substrate by sputtering in an argon atmosphere containing about 1% oxygen gas and under a vacuum degree of 0.1 to 0.9Pa (about 0.6Pa)An ITO film (thickness of about 35nm) having a surface resistance R of 75 to 83 (omega/□).
The total light transmittance of the ITO (indium oxide containing tin oxide) thin film of example 1 was 84%. In addition, the total light transmittance was measured using HGM-2DP from Bethes testing machine.
(example 2)
An ITO film (thickness of about 30nm) having a surface resistance R of 100 to 105(Ω/□) was formed in the same manner as in example 1.
In this way, examples 1 and 2 are ITO thin films in which an amorphous ITO film was formed on the surface of a flexible substrate without annealing treatment.
Various plastic films (sheets) having transparency can be used for a substrate having flexibility. As the plastic film, for example, a plastic film containing polyester, polycarbonate, polyamide, polyimide, polyolefin, polyvinyl chloride, polyvinylidene chloride, polystyrene, polyvinyl alcohol, polyacrylate, polyarylate, or polyphenylene sulfide can be used as a resin component. Among these, polyester is particularly preferable, and among the polyesters, polyethylene terephthalate is particularly preferable. Polyethylene terephthalate has excellent flexibility and transparency, and is suitable for forming an amorphous ITO film. The total light transmittance of the PET film substrate treated with the double-sided hardcoat layer was about 91%. The film base material temperature during the sputtering plating was normal temperature. In the sputtering method, a general magnetron electrode method is used.
Comparative example 1
Both surfaces of PET (polyethylene terephthalate) having a thickness of 125 μm were subjected to hard coating treatment to form a base material using a catalyst containing 5 wt% SnO2The ITO target of (1%) was subjected to sputtering plating in an argon atmosphere containing an oxygen gas of about 1% under a vacuum degree of 0.1 to 0.9Pa (about 0.6Pa), to form an ITO film (thickness of about d 25nm) having a surface resistance R of 170(Ω/□) on one surface of the substrate. Then, the film was heated in the atmosphere at about 150 ℃ for about 50 minutes to form a thin-film crystallized ITO thin film having a surface resistance R of 142(Ω/□). In addition, to prevent annealing to PET film substrateHaze was increased using a double-sided hardcoat PET film substrate.
(evaluation method 1)
Fig. 1 is a table showing the measurement results of the hall numbers using example 1 and comparative example 1.
ResiTest 8330 manufactured by Toyo Technika was used for the measurement.
As can be seen from the results shown in fig. 1, example 1 is a high density film because of having higher mobility compared to comparative example 1.
(evaluation method 2)
FIG. 2 is a graph showing the results of a bending test of 1.0mm in diameter using example 2 and comparative example 1.
Fig. 2a is a conceptual diagram of the test, fig. 2b is a photograph showing the membrane surface after the test, and fig. 2c is a table showing the measurement results.
As shown in fig. 2b and 2c, no cracks occurred in example 2, compared to the cracks occurred in comparative example 1.
(evaluation method 3)
FIG. 3 is a graph showing the results of a no-load bending test using example 2 and comparative example 1
Fig. 3a is a conceptual diagram of the test, and fig. 3b is a table showing the measurement results.
As can be seen from the no-load bending test results, example 2 also withstood repeated bending relative to comparative example 1.
The transparent conductive thin film is an amorphous ITO film in which a first ITO film is not annealed, and a second ITO film is not annealed, and has a film thickness in the range of 30nm to 320nm and a surface resistance in the range of 9 to 105 (omega/□).
(evaluation method 4)
FIG. 4 is a graph showing the results of storage characteristics at 80 ℃ in example 2.
As shown in fig. 4, the resistance value does not change with time even after 1000 hours have elapsed.
(evaluation method 5)
FIG. 5 is a graph showing the results of storage characteristics at 60 ℃ and 90% RH using example 2.
As shown in fig. 5, the resistance value did not change with time even after 1000 hours had elapsed.
(evaluation method 6)
FIG. 6 is a graph showing the results of thermal cycling tests at-30 ℃ and 80 ℃ using example 2.
As shown in fig. 6, the resistance value did not change with time even after 1000 hours had elapsed.
(example 3)
An Ag layer having a thickness of about 10nm to 20nm was formed on the surface of the ITO thin film of example 1 by sputtering using an Ag target under a vacuum of 0.1 to 0.9Pa (about 0.6 Pa). Further, a catalyst containing 5 wt% of SnO2The ITO target of (1) is formed by sputtering in an argon atmosphere containing about 1% oxygen gas under a vacuum of 0.1 to 0.9Pa (about 0.6Pa) to form an ITO film (having a thickness of about 50nm) having a surface resistance R of 55 to 75(Ω/□) on the surface of the Ag layer.
In this manner, example 3 is a transparent conductive thin film, in which a first ITO film is formed on the surface of a flexible substrate, a thin film metal layer is formed on the surface of the first ITO film, and a second ITO film is formed on the surface of the thin film metal layer.
The transparent conductive film of example 3 had a surface resistance R of 5.0(Ω/□) and a total light transmittance of 89%. The total light transmittance of the Ag layer with a thickness of about 10nm to 20nm was 50%.
Comparative example 2
Both surfaces of PET (polyethylene terephthalate) having a thickness of 125 μm were subjected to hard coating treatment to form a base material using a catalyst containing 5 wt% SnO2The ITO target of (1) is formed by sputtering in an argon atmosphere containing about 1% oxygen gas under a vacuum degree of 0.1 to 0.9Pa (about 0.6Pa) to form an ITO film (thickness of about 25nm) having a surface resistance R of 170(Ω/□) on one surface of the substrate. Then, an Ag layer having a thickness of about 10nm to 20nm is formed on the surface of the ITO film by sputtering using an Ag target under a vacuum of 0.1 to 0.9Pa (about 0.6 Pa). Further, an ITO target was used in an argon atmosphere containing about 1% of oxygen gasIn the method, an ITO film having a thickness of about 50nm is formed on the surface of the Ag layer by sputtering plating under a vacuum of 0.1 to 0.9Pa (about 0.6 Pa). Immediately after plating, the surface resistance was 5.5(Ω/□) and the total light transmittance was 85%. Then, in the atmosphere, under a heating atmosphere of about 150 ℃, for about 50 minutes, 2 ITO films (having thicknesses of about 25nm and about 50nm, respectively) were crystallized. After crystallization, the surface resistance was 5.0(Ω/□) and the total light transmittance was 89%.
Comparative example 3
A substrate is formed by hard coating both surfaces of PET (polyethylene terephthalate) having a thickness of 125 μm, and an Ag layer having a thickness of about 10 to 20nm is formed on one surface of the substrate by sputtering using an Ag target under a vacuum of 0.1 to 0.9Pa (about 0.6 Pa). After the Ag layer was formed, the surface resistance R was 5.0(Ω/□), and the total light transmittance was 50%.
(evaluation method 7)
FIG. 7 is a table showing the results of heat resistance of the composition obtained in example 3, comparative example 2 and comparative example 3.
The heat resistance test was conducted by leaving it in an atmosphere of 150 ℃.
As shown in fig. 7, although example 3 gave good results even after 22 hours had elapsed, comparative example 2 showed a change in heat resistance with time after 22 hours had elapsed. Comparative example 3 had lost the heat-resistant function at the time point of 2 hours.
(evaluation method 8)
FIG. 8 is a table showing the results of the 50 ℃ temperature depth test using example 3, comparative example 2 and comparative example 3.
As shown in fig. 8, although example 3 gave good results even after 60 minutes had elapsed, comparative example 2 started to be affected after 20 minutes had elapsed. Comparative example 3 the Ag layer deteriorated and discolored and peeled off at the time point of 5 minutes.
(evaluation method 9)
FIG. 9 is a table showing the results of the 60 to 80 ℃ hot water depth test using example 3, comparative example 2, and comparative example 3.
As shown in fig. 9, although example 3 gave good results even after 60 minutes had elapsed, comparative example 2 started to be affected after 40 minutes had elapsed. Comparative example 3 the Ag layer deteriorated and discolored and peeled off before 5 minutes elapsed.
(evaluation method 10)
Fig. 10 is a table showing the results of the room temperature standing test in the atmosphere using example 3, comparative example 2, and comparative example 3.
As shown in fig. 10, although example 3 gave good results even after 9 months, comparative example 2 started to be affected after 3 months and the Ag layer partially discolored after 9 months. Comparative example 3 before 2 months had elapsed, the Ag layer deteriorated, discolored and peeled off.
(evaluation method 11)
Fig. 11 is a graph showing the results of the no-load bending test using example 3 and comparative example 3. The test method was the same as evaluation method 3.
In example 3 and comparative example 3, the resistance change rate and the total light transmittance were good results after 5000 bending tests.
FIG. 12 is a microphotograph of the surfaces of the ITO thin films of example 1 and comparative example 1.
FIG. 12a shows the ITO film of example 1, FIG. 12b shows the ITO film of comparative example 1, and the test pieces are all 10. mu. m.times.2.5. mu.m.
Fig. 13 is a graph showing the results of measuring the surface roughness of the test piece shown in fig. 12.
FIG. 13a is an ITO thin film of example 1, and FIG. 13b is an ITO thin film of comparative example 1. For the measurement of the surface roughness, an ET200 type fine shape measuring apparatus manufactured by Xiaozhu, K.K. was used. In addition, for the photomicrograph of the surface indentation and the measurement, a scanning probe microscope (Dimension Icon SPM) manufactured by bruker corporation was used.
The ITO thin film of example 1 had a surface average roughness ra (nm) of 4.1, and the ITO thin film of comparative example 1 had a surface average roughness ra (nm) of 9.5. Further, the surface average roughness ra (nm) of the double-sided hard coat film substrate used in example 1 was 5.
In the case of using an ITO film and requiring a low surface resistance value, there is generally a method of increasing the thickness of the ITO film layer.
(example 4)
The amorphous ITO film was formed to a film thickness of about 320nm by the same method as in example 1.
The total light transmittance of the ITO film at this time was about 82%, and the surface resistance R was about 9 (. omega./□).
In addition, it was confirmed that the average hole diameter and the hole ratio of the ITO film were the same as those of the amorphous high-density film in example 1, and the resistance value did not change with time.
Comparative example 4
Comparative example 4 an ITO film (having a thickness of about 300nm) having a surface resistance R of 15(Ω/□) was formed by sputtering plating in the same manner as in comparative example 1.
In order to prevent the resistance value from changing with time, the ITO film was heated in the atmosphere at about 150 ℃ for about 50 minutes to form a thin film crystallized ITO film.
As a result, curling with the ITO film surface as the upper surface occurs on the transparent conductive film, cracks (fissures) occur in a part of the ITO film, and the surface resistance value becomes R10 to infinity (fissured portion) (Ω/□), and a stable resistance value cannot be obtained.
The film density will be described below.
The film density is derived from the void fraction per unit area. The void fraction is defined as the ratio of the total length of the hole diameter of the measured recess to the measured length. Then, the recess having a depth of 22nm or more was regarded as a hole, and the diameter at the position of the recess depth 1/2 was regarded as the size of the hole (hole diameter).
As a result of measurement, the ITO thin film of example 1 had an average hole diameter of 0.32 μm and a hole rate of 9.5%, and the ITO thin film of comparative example 1 had an average hole diameter of 0.46 μm and a hole rate of 36.5%.
The ITO thin film of example 1 had a hole rate of 9.5% and thus a film density of 90.5%, and the ITO thin film of comparative example 1 had a hole rate of 36.5% and thus a film density of 63.5%.
In this way, the ITO thin film of the present invention has a high-density film as the amorphous ITO film by setting the film thickness of the amorphous ITO film to be in the range of 30nm to 320nm and the surface resistance of the amorphous ITO film to be in the range of 9 to 105(Ω/□), and thus can provide an ITO thin film which is improved in stability, has a resistance value which does not change with time, is improved in moisture resistance and gas barrier properties, and is free from cracks due to bending.
The surface average roughness of the amorphous ITO film is preferably 9nm or less, more preferably 4.1nm or less, and by setting the surface average roughness of the amorphous ITO film to 9nm or less, the film density of the amorphous ITO film can be set to 65% or more, and the stability can be improved.
The film density of the amorphous ITO film is preferably 65% or more, more preferably 90% or more, and the stability can be improved by making the film density of the amorphous ITO film 65% or more.
SnO contained in amorphous ITO film2Preferably, the content is in the range of 2 to 7 wt%, and more preferably 5 wt% as in example 1 and example 2. By adding SnO2Setting in the range of 2 wt% to 7 wt% can enhance transparency.
Further, as shown in example 3, it is preferable that the first ITO film as well as the second ITO film has a film thickness in the range of 30nm to 320nm and a surface resistance of the amorphous ITO film is in the range of 9 to 105(Ω/□). By changing the first ITO film or the second ITO film into such an ITO thin film, a transparent conductive thin film excellent in conductivity, transparency, and durability can be provided.
Further, the second ITO film was set to an amorphous ITO film as follows: the thickness of the film is in the range of 30nm to 320nm, the surface resistance of the amorphous ITO film is in the range of 9 to 105 (omega/□), the thin film metal layer is an Ag layer with the thickness of 10nm to 20nm, so that Ag with poor durability can be protected by the second ITO film to improve the durability, and the total light transmittance of about 50% of Ag can be improved to about 90% by the second ITO film.
In example 3, Ag is used as the thin-film metal layer, but is not particularly limited to Ag, and Cu, Al, Au, Ni/Cr, Ti, Sn, or the like may be used alone or an alloy consisting of two or more of them may be used.
Claims (11)
1. An ITO thin film comprising an amorphous ITO film formed on the surface of a flexible substrate without being annealed, wherein the amorphous ITO film has a film thickness in the range of 30nm to 320nm and a surface resistance in the range of 9 to 105(Ω/□).
2. The ITO film according to claim 1, wherein polyethylene terephthalate is used as the substrate.
3. The ITO thin film according to claim 1 or 2, wherein the amorphous ITO film has a film density of 65% or more.
4. The ITO thin film according to any one of claims 1 to 3, wherein the amorphous ITO film has a surface average roughness of 9nm or less.
5. The ITO thin film according to any one of claims 1 to 4, wherein the amorphous ITO film contains SnO2In the range of 2 to 7 wt%.
6. A transparent conductive thin film comprising a flexible substrate, a first ITO film formed on the surface of the substrate, a thin metal layer formed on the surface of the first ITO film, and a second ITO film formed on the surface of the thin metal layer,
the first ITO film is an amorphous ITO film which is not subjected to the annealing treatment; the second ITO film is an amorphous ITO film which is not subjected to the annealing treatment, the film thickness of the second ITO film is within a range of 30nm to 320nm, and the surface resistance of the amorphous ITO film is within a range of 9 to 105 (omega/□).
7. The transparent conductive film according to claim 6, wherein the film metal layer is an Ag layer having a thickness of 10nm to 20 nm.
8. The transparent conductive film according to claim 6 or 7, wherein polyethylene terephthalate is used as the substrate.
9. The transparent conductive film according to any one of claims 6 to 8, wherein the film density of the second ITO film is 65% or more.
10. The transparent conductive film according to any one of claims 6 to 9, wherein the surface average roughness of the amorphous second ITO film is 9nm or less.
11. The transparent conductive film according to any one of claims 6 to 10, wherein SnO contained in the second ITO film2In the range of 2 to 7 wt%.
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| CN105556618A (en) * | 2013-09-10 | 2016-05-04 | 洛克技研工业株式会社 | Transparent conductive substrate and method for manufacturing transparent conductive substrate |
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| CN112908517A (en) * | 2021-01-19 | 2021-06-04 | 大正(江苏)微纳科技有限公司 | Transparent conductive film and preparation method thereof |
| CN112908517B (en) * | 2021-01-19 | 2022-08-05 | 大正(江苏)微纳科技有限公司 | Transparent conductive film and preparation method thereof |
Also Published As
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| KR102336155B1 (en) | 2021-12-06 |
| TWI683017B (en) | 2020-01-21 |
| KR20200001441A (en) | 2020-01-06 |
| CN116189964A (en) | 2023-05-30 |
| JP7116994B2 (en) | 2022-08-12 |
| JP2020001232A (en) | 2020-01-09 |
| TW202000950A (en) | 2020-01-01 |
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