GB2573157A - Method of processing transparent conductor - Google Patents
Method of processing transparent conductor Download PDFInfo
- Publication number
- GB2573157A GB2573157A GB1806890.8A GB201806890A GB2573157A GB 2573157 A GB2573157 A GB 2573157A GB 201806890 A GB201806890 A GB 201806890A GB 2573157 A GB2573157 A GB 2573157A
- Authority
- GB
- United Kingdom
- Prior art keywords
- substrate
- nanowires
- embossing
- plasma
- plasma treatment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 238000000034 method Methods 0.000 title claims abstract description 59
- 239000004020 conductor Substances 0.000 title claims abstract description 22
- 239000000758 substrate Substances 0.000 claims abstract description 79
- 239000002070 nanowire Substances 0.000 claims abstract description 55
- 238000004049 embossing Methods 0.000 claims abstract description 42
- 238000009832 plasma treatment Methods 0.000 claims abstract description 26
- 238000000576 coating method Methods 0.000 claims abstract description 23
- 239000011248 coating agent Substances 0.000 claims abstract description 20
- 238000005245 sintering Methods 0.000 claims abstract description 20
- 229920001169 thermoplastic Polymers 0.000 claims abstract description 14
- 239000004416 thermosoftening plastic Substances 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 8
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 238000003825 pressing Methods 0.000 claims abstract description 6
- 239000011787 zinc oxide Substances 0.000 claims abstract description 6
- 230000005855 radiation Effects 0.000 claims abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- 239000002042 Silver nanowire Substances 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 description 15
- 230000009467 reduction Effects 0.000 description 10
- 230000008569 process Effects 0.000 description 8
- -1 poly(vinylpyrrolidinone) Polymers 0.000 description 5
- 238000004140 cleaning Methods 0.000 description 4
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000011368 organic material Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000007764 slot die coating Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/1884—Manufacture of transparent electrodes, e.g. TCO, ITO
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L29/00—Semiconductor devices adapted for rectifying, amplifying, oscillating or switching, or capacitors or resistors with at least one potential-jump barrier or surface barrier, e.g. PN junction depletion layer or carrier concentration layer; Details of semiconductor bodies or of electrodes thereof ; Multistep manufacturing processes therefor
- H01L29/02—Semiconductor bodies ; Multistep manufacturing processes therefor
- H01L29/06—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions
- H01L29/0657—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body
- H01L29/0665—Semiconductor bodies ; Multistep manufacturing processes therefor characterised by their shape; characterised by the shapes, relative sizes, or dispositions of the semiconductor regions ; characterised by the concentration or distribution of impurities within semiconductor regions characterised by the shape of the body the shape of the body defining a nanostructure
- H01L29/0669—Nanowires or nanotubes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022466—Electrodes made of transparent conductive layers, e.g. TCO, ITO layers
Abstract
Method of processing transparent conductor comprises substrate 12 coated with nanowires 16, wherein the method further comprises a plasma treatment step comprising a treatment of substrate 12 using a plasma, preferably nitrogen plasma, and an embossing step comprising applying pressure to substrate 12 to force nanowires 16 into substrate 12. Embossing step preferably comprises treating substrate 12 to decrease substrate's viscosity to less than 109 Pas. Method may comprise sintering step to heat nanowires 16 using radiation pulses, wherein the sintering step is before embossing step which is before plasma treatment step. Substrate 12 may comprise a thermoplastic and the embossing step may comprise heating substrate 12 while applying pressure. Substrate 12 may comprise a PMMA buffer layer 14 between substrate 12 and nanowires 16. Coating step may comprise coating zinc oxide layer onto the substrate 12, wherein the coating step takes place after the plasma treatment and embossing steps.
Description
Method of Processing Transparent Conductor
The invention relates to a method of producing a transparent conductor.
Transparent conductors are used in many types of electronic devices, including touch panels, touch sensors, solar cells and flexible displays. Often, transparent conductors employ indium tin oxide (ITO) as a conductor. While ITO gives reasonable performance in terms of sheet resistance and surface roughness, its use in flexible displays is limited, as cracks can form when bending an ITO transparent conductor, and the material possesses lower sheet resistance on flexible substrates as high temperature annealing is not possible.
Transparent conductors using metal nanowires provide a more flexible alternative to ITO conductors. However, transparent conductors based on metal nanowires suffer from high surface roughness, which can lead to electrical shorting between electrodes.
According to a first aspect of the invention, there is provided a method of processing a transparent conductor, the method comprising: receiving a substrate coated with nanowires; a plasma treatment step, comprising treatment a surface of the substrate using a plasma; and an embossing step, comprising applying pressure to the substrate to force the nanowires into the substrate.
This method is advantageous, as the plasma treatment step and the embossing step reduce the sheet resistance and the surface roughness of the substrate. The embossing step improves the interconnection between nanowires by mechanically forcing the nanowires together, which improves sheet resistance. Additionally, since the embossing step forces the nanowires into the substrate, this improves the surface roughness. The plasma treatment step modifies the nanowires chemically, removing organic impurities from the nanowires and thereby improving sheet resistance. The synergistic effect of the mechanical improvement of electrical interconnection during embossing and the chemical modification during plasma treatment has been found to give particular reduction in sheet resistance.
In one example, the method further comprises a sintering step, the sintering step comprising heating the nanowires. Heating the nanowires causes them to soften, which causes them to fuse together, thereby reducing sheet resistance.
In one example, in the sintering step, the nanowires are heated using pulses of radiation. The pulses of radiation cause the nanowires to soften and fuse together, while helping to avoid melting of the substrate, which often comprises a thermoplastic.
In one example, the sintering step takes place before the embossing step. Carrying out the steps in this order has been found to be beneficial, as the sintering step, which gives improvements in sheet resistance, can increase the surface roughness of the transparent conductor. The subsequent embossing process can improve the surface roughness to acceptable levels, by forcing the nanowires into the substrate as described above.
In one example, the embossing step occurs before the plasma treatment step. It has been found that removing the organic impurities (using plasma treatment) after embossing is particularly advantageous in terms of reducing surface resistance. Additionally, the plasma treatment step improves the wettability of the substrate, improving the uniformity of subsequent coatings applied to the substrate. This means that it is beneficial to carry out plasma treatment as a final process before a subsequent coating process.
In one example, the plasma is nitrogen plasma. This removes poly(vinylpyrrolidinone) (PVP), which is an organic material present in the nanowires, and consequently gives significant reductions in sheet resistance.
In one example, the embossing step comprises treating the substrate to decrease the substrate’s viscosity to less than 109 Pas. When the substrate has a viscosity of this value or lower, the nanowires can be more easily forced together and into the substrate, thereby reducing surface roughness and sheet resistance.
In one example, the substrate comprises a thermoplastic and the embossing step comprises heating the substrate while the pressure is applied. This allows the substrate’s viscosity to be reduced, preferably below the 109 Pas described above. When the substrate comprises a thermoplastic of a higher density, the substrate must be heated to a higher temperature to provide the same reduction in viscosity.
In one example, the pressure is greater than 10 bar. This pressure helps to ensure that the nanowires are sufficiently compressed together and into the polymer substrate, to give adequate reduction in sheet resistance and surface roughness.
In one example, the substrate comprises a buffer layer between a body of the substrate and the nanowires. The material of the buffer layer can be selected independently of that of the body of the substrate so that the buffer layer can give more favourable performance in the method described here (e.g. low density to give lower viscosity), while the body can be selected to give more favourable performance in use. Additionally, the buffer layer reduces surface roughness and provides a more homogenous surface for the subsequent embossing process.
In one example, the buffer layer is PMMA. PMMA is a low density thermoplastic, which has a lower viscosity at the same temperature as higher density thermoplastics. It is desirable to avoid heating the substrate to too high a temperature, to avoid damage to the substrate.
In one example, the method further comprises a coating step, the coating step comprising coating a zinc oxide layer onto the substrate. This further reduces the surface roughness, acts as barrier to limit water or oxygen ingress and can be integrated directly into some OLED and solar cell production lines
In one example, the coating step takes place after the plasma treatment and embossing steps. The plasma treatment and embossing steps are much more effective if performed when the coating is not present.
In one example, the nanowires are silver nanowires.
According to a second aspect of the invention, there is provided a method of processing a transparent conductor, the method comprising: receiving a substrate coated with nanowires; and a plasma treatment step, comprising treatment with nitrogen plasma. As described above, this removes poly(vinylpyrrolidinone) (PVP), which is an organic material present in the nanowires, and consequently gives significant reductions in sheet resistance This process may be combined with any of the other steps (e.g. embossing and/or sintering) as described above.
According to a third aspect of the invention, there is provided a method of processing a transparent conductor, the method comprising: receiving a substrate coated with nanowires; and an embossing step, comprising applying pressure to the substrate, wherein the embossing step comprises treating the substrate to decrease the substrate’s viscosity to less than 10Λ9 Pas. As described above, when the substrate has a viscosity of this value or lower, the nanowires can be more easily forced together and into the substrate, thereby reducing surface roughness and sheet resistance. This process may be combined with any of the other steps (e.g. plasma treatment and/or sintering) as described above.
For a better understanding of the invention reference is made, by way of example only, to the accompanying figures, in which:
Figure 1 shows a method of processing a transparent conductor; and
Figures 2 to 6 show substrates at various points in the method of Figure 1.
Referring to Figure 1 there is shown a method 1000 of processing a transparent conductor. The method comprises a cleaning step 100. In the cleaning step 100, a substrate 10a (as shown in Figure 2) is received.
The substrate 10a comprises a body 12. The body 12 is substantially planar, and is formed of a thermoplastic. The thermoplastic is polyethylene terephthalate (PET). In other embodiments, the thermoplastic is polyethylene naphthalate (PEN). In the cleaning step 100, the body 12 is cleaned using a solvent.
The method comprises a buffer layer application step 200, subsequent to the cleaning step 100. In the buffer layer application step 200, a buffer layer 14 is coated onto an upper surface the body 12, to form the substrate 10b shown in Figure 3. The buffer layer 14 is planar and covers the entire area of the body 12. The buffer layer 14 is of uniform thickness. The buffer layer 14 is a thermoplastic of lower density than the body 12. The thermoplastic is polymethyl methacrylate (PMMA). Other thermoplastics having similar viscosities and temperature related changes may be used instead of PMMA.
The buffer layer 14 is coated onto an upper surface of the body 12 by spin coating. In other examples, the buffer layer is coated using screen printing, slot die coating, drop casting, doctor blading, bar coating or knife over edge coating.
The method comprises a nanowire coating step 300, subsequent to the buffer layer application step 200. In the nanowire coating step 300, a nanowire layer 16 is coated onto the buffer layer 14 to form the substrate 10c shown in Figure 4. The nanowires in the nanowire layer 16 are silver nanowires. The nanowire layer 16 is on an upper surface of the buffer layer 14.
The nanowire layer 16 is coated onto the buffer layer 14 by spray coating a solution comprising nanowires onto the buffer layer 14. The spray coating is achieved using an air brush (not shown). In other examples, the spray coating may be carried out using an ultrasonic coating process. Alternatively, the nanowire layer may be coated using a drop casting process.
The method comprises a sintering step 400, subsequent to the nanowire coating step 300. In the sintering step, the nanowires are heated, so that the nanowires soften and fuse together. The nanowires are heated using pulses of radiation, which melt the nanowires but avoid melting the body 12 and the buffer layer 14. The sintering step is a photonic curing process.
The method comprises an embossing step 500, subsequent to the nanowire coating step 400. During the embossing step 500, pressure is applied to the substrate 10c to force the nanowires into the substrate 10c, thereby forming the substrate 10d, as shown in Figure 5. In the substrate 10d, the nanowires have been forced into the buffer layer 14, to form an embossed layer 18. The embossed layer 18 comprises the nanowires within the buffer layer 14.
The pressure is applied to the substrate 10c using a compressed air system (not shown). The pressure applied is 10s Pa. However, in other examples, the pressure may be applied by a roller, allowing the embossing step 500 to be carried out on a production line.
During the embossing step 500, the substrate 10c is heated to reduce the viscosity of the buffer layer 14. The substrate is heated to temperature greater than 100degC, but less than 190degC. This reduces the viscosity of the PMMA buffer layer 14 to less than 109 Pas, but avoids melting the substrate 10c.
In another example, the body 12 and/or buffer layer 14 (if present) is made from a UV curable plastic, and the viscosity of the body/buffer layer is reduced by UV light during the embossing step 500.
The method comprises a plasma treatment step 600, subsequent to the embossing step 500. During the plasma treatment step 600, the substrate 10d is exposed to spatial afterglow of nitrogen plasma. This removes PVP, which is an organic material present in the nanowires.
The method comprises a zinc oxide coating step 700, subsequent to the plasma treatment step 600. In the zinc oxide coating step 200, a zinc oxide layer 20 is coated onto an upper surface of the embossed layer 18, to form the substrate 10e shown in Figure 6.
The sequential method of processing described above has been shown to give substantially reduced sheet resistance (reduction of approximately 80%) and surface roughness (reduction of approximately 70%). The method does not affect the transparency of the conductor, and improves the reliability of electrodes formed by the transparent conductor.
In other embodiments, the buffer layer 14 is omitted, and the nanowires are instead coated directly onto the body 12. While this method does not give as much reduction in surface roughness and sheet resistance, it gives some reduction, and is suitable for some lower cost applications.
While the order of the sintering step 400, the embossing step 500 and the plasma treatment step 600 described above is preferred, these steps may be carried out in any order, and will still provide reductions in sheet resistance and surface roughness. However, better results are obtained when the sintering step 400 occurs before the embossing step 500, and/or the embossing step 500 occurs before the plasma treatment step 600.
Additionally, not all of the sintering step 400, the embossing step 500 and the plasma treatment step 600 need to be carried out. When only two steps are performed, the best results (in terms of combined sheet resistance and surface roughness) have been found for a combination of the plasma treatment step 600 and the embossing step 500. The next best results have been found for a combination of the sintering step 400 and the embossing step 500.
Although a few preferred embodiments have been shown and described, it will be appreciated by those skilled in the art that various changes and modifications might be made without departing from the scope of the invention, as defined in the appended claims.
Attention is directed to all papers and documents which are filed concurrently with or previous to this specification in connection with this application and which are open to public inspection with this specification, and the contents of all such papers and documents are incorporated herein by reference.
All of the features disclosed in this specification (including any accompanying claims, abstract and drawings), and/or all of the steps of any method or process so disclosed, may be combined in any combination, except combinations where at least some of such features and/or steps are mutually exclusive.
Each feature disclosed in this specification (including any accompanying claims, abstract and drawings) may be replaced by alternative features serving the same, equivalent or similar purpose, unless expressly stated otherwise. Thus, unless expressly stated otherwise, each feature disclosed is one example only of a generic series of equivalent or similar features.
The invention is not restricted to the details of the foregoing embodiment(s). The invention extends to any novel one, or any novel combination, of the features disclosed in this specification (including any accompanying claims, abstract and drawings), or to any novel one, or any novel combination, of the steps of any method or process so disclosed.
Claims (17)
1. A method of processing a transparent conductor, the method comprising: receiving a substrate coated with nanowires; a plasma treatment step, comprising treatment of a surface of the substrate using a plasma; and an embossing step, comprising applying pressure to the substrate to force the nanowires into the substrate.
2. A method according to claim 1, further comprising a sintering step, the sintering step comprising heating the nanowires.
3. A method according to claim 2, wherein in the sintering step, the nanowires are heated using pulses of radiation.
4. A method according to claim 2 or 3, wherein the sintering step takes place before the embossing step.
5. A method according to any of claims 2 to 4, wherein the embossing step occurs before the plasma treatment step.
6. A method according to any preceding claim, wherein the plasma is nitrogen plasma.
7. A method according to any preceding claim, wherein the embossing step comprises treating the substrate to decrease the substrate’s viscosity to less than 109 Pas.
8. A method according to any preceding claim, wherein the substrate comprises a thermoplastic and the embossing step comprises heating the substrate while the pressure is applied.
9. A method according to any preceding claim, wherein the pressure is greater than 10s Pa.
10. A method according to any preceding claim, wherein the substrate comprises a buffer layer between a body of the substrate and the nanowires.
11. A method according to claim 10, wherein the buffer layer is PMMA.
12. A method according to any preceding claim further comprising a coating step, the coating step comprising coating a zinc oxide layer onto the substrate.
13. A method according to claim 12, wherein the coating step takes place after the plasma treatment and embossing steps.
14. A method according to any preceding claim, wherein the nanowires are silver nanowires.
15. A method of processing a transparent conductor, the method comprising: receiving a substrate coated with nanowires; and a plasma treatment step, comprising treatment with a nitrogen plasma.
16. A method of processing a transparent conductor, the method comprising: receiving a substrate coated with nanowires; and an embossing step, comprising applying pressure to the substrate, wherein the embossing step comprises treating the substrate to decrease the substrate’s viscosity to less than 109 Pas.
17. A method according to claim 16, wherein the substrate comprises a thermoplastic and treating the substrate to decrease the substrate’s viscosity comprises heating the substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB1806890.8A GB2573157A (en) | 2018-04-27 | 2018-04-27 | Method of processing transparent conductor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB1806890.8A GB2573157A (en) | 2018-04-27 | 2018-04-27 | Method of processing transparent conductor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB201806890D0 GB201806890D0 (en) | 2018-06-13 |
| GB2573157A true GB2573157A (en) | 2019-10-30 |
Family
ID=62494912
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB1806890.8A Withdrawn GB2573157A (en) | 2018-04-27 | 2018-04-27 | Method of processing transparent conductor |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB2573157A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100243295A1 (en) * | 2006-10-12 | 2010-09-30 | Cambrios Technologies Corporation | Nanowire-based transparent conductors and applications thereof |
| US20110094651A1 (en) * | 2009-10-22 | 2011-04-28 | Fujifilm Corporation | Method for producing transparent conductor |
-
2018
- 2018-04-27 GB GB1806890.8A patent/GB2573157A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100243295A1 (en) * | 2006-10-12 | 2010-09-30 | Cambrios Technologies Corporation | Nanowire-based transparent conductors and applications thereof |
| US20110094651A1 (en) * | 2009-10-22 | 2011-04-28 | Fujifilm Corporation | Method for producing transparent conductor |
Also Published As
| Publication number | Publication date |
|---|---|
| GB201806890D0 (en) | 2018-06-13 |
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| Date | Code | Title | Description |
|---|---|---|---|
| WAP | Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1) |