CN113921192A - Preparation method of high-precision patternable micro-nano silver nanowire transparent electrode - Google Patents
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- CN113921192A CN113921192A CN202111106540.4A CN202111106540A CN113921192A CN 113921192 A CN113921192 A CN 113921192A CN 202111106540 A CN202111106540 A CN 202111106540A CN 113921192 A CN113921192 A CN 113921192A
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- 239000002042 Silver nanowire Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 47
- 239000011521 glass Substances 0.000 claims abstract description 46
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229920002120 photoresistant polymer Polymers 0.000 claims abstract description 22
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 11
- 230000001680 brushing effect Effects 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000004528 spin coating Methods 0.000 claims abstract description 7
- 238000005507 spraying Methods 0.000 claims abstract description 7
- 238000000137 annealing Methods 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 238000011161 development Methods 0.000 claims abstract description 4
- 238000000206 photolithography Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 27
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000004677 Nylon Substances 0.000 claims description 5
- 229920001778 nylon Polymers 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000005530 etching Methods 0.000 abstract description 12
- 229910052751 metal Inorganic materials 0.000 abstract description 6
- 239000002184 metal Substances 0.000 abstract description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 6
- 238000001914 filtration Methods 0.000 description 3
- 238000000059 patterning Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000003491 array Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- Nanotechnology (AREA)
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- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing Of Electric Cables (AREA)
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Abstract
The invention discloses a preparation method of a high-precision patternable micro-nano silver nanowire transparent electrode, which comprises (S1) drying a glass substrate after cleaning; (S2) pretreating the glass substrate; (S3) spraying a silver nanowire solution on the glass substrate; (S4) spin-coating photoresist on the silver nanowire conductive film, and performing pre-annealing treatment; (S5) exposing the photoresist film with the aid of a photolithography mask; (S6) immersing the glass substrate in a developing solution for development; (S7) completely removing the silver nanowires exposed outside the photoresist by adopting a physical brushing mode; (S8) completely removing the photoresist remaining on the glass substrate; (S9) drying the glass substrate; (S10) pouring a polyvinyl alcohol solution on the glass substrate to cover the whole electrode pattern, and after the glass substrate is aired, uncovering the PVA film to obtain the micro-nano silver nanowire transparent electrode. The invention solves the problem of rough edge of the conductive channel caused by long metal etching time and incomplete etching.
Description
Technical Field
The invention belongs to the technical field of flexible transparent electrodes, and particularly relates to a preparation method of a high-precision patternable micro-nano silver nanowire transparent electrode.
Background
Flexible transparent electrodes have been widely used in a variety of flexible electronic devices, such as wearable electronics, deformable contact interfaces, flexible integrated circuits, electronic skins, biomedical sensors, and the like. The high performance flexible transparent electrode should have high optical transmittance, low resistance and stable mechanical properties. Indium Tin Oxide (ITO) is widely used as a transparent electrode in both academic and industrial fields. However, ITO does not meet the requirements of flexible devices due to its inherent stiffness (1% post strain fracture) and the high cost of physical vapor deposition. Therefore, metal nanowires, which are novel alternative materials, have attracted much attention in recent years, and among them, silver nanowires (Ag-NWs) have high optical transmittance, high electrical conductivity and good mechanical flexibility, and are ideal materials for preparing transparent flexible electrodes.
However, micropatterning processing of silver nanowire flexible transparent electrodes remains challenging, limiting their application in integrated microsensor arrays and bioelectronics. The existing micro-patterning processing technology of the silver nanowire flexible transparent electrode is high in cost, environment-friendly and long in metal etching time, and particularly when the width of a conductive channel is reduced to be below 50 micrometers, rough burrs caused by incomplete etching can appear on the edge of the channel, so that the electrode is very easy to short circuit. In addition, because the contact characteristic of the silver nanowire and a common flexible substrate such as PDMS is poor, the micro-nano silver nanowire transparent electrode prepared by the prior art needs to be improved in the aspects of conductivity and mechanical property. Therefore, how to solve the problems existing in the prior art is a problem which needs to be solved urgently by the technical personnel in the field.
Disclosure of Invention
The invention aims to provide a method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode, which mainly solves the problems of long metal etching time and rough conductive channel edge caused by incomplete etching in micro-patterning processing of a silver nanowire flexible transparent electrode in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a high-precision patternable micro-nano silver nanowire transparent electrode comprises the following steps:
(S1) cleaning the glass substrate and then drying the glass substrate;
(S2) pretreating the dried glass substrate;
(S3) spraying a silver nanowire solution on the glass substrate;
(S4) spin-coating photoresist on the silver nanowire conductive film, and performing pre-annealing treatment;
(S5) exposing the photoresist film with the aid of a photolithography mask;
(S6) immersing the exposed glass substrate in a developing solution for development;
(S7) completely removing the silver nanowires exposed outside the photoresist by adopting a physical brushing mode;
(S8) completely removing the photoresist remaining on the glass substrate;
(S9) drying the glass substrate;
(S10) pouring a polyvinyl alcohol solution on the glass substrate to cover the whole electrode pattern, and after the glass substrate is aired, uncovering the PVA film to obtain the micro-nano silver nanowire transparent electrode.
Further, the step (S1) of cleaning the glass substrate is to perform ultrasonic cleaning on the glass substrate by sequentially using deionized water, an ethanol solution and an acetone solution.
Further, the pretreatment method in the step (S2) is to perform pretreatment of the glass substrate with O2 Plasma for 10-15 min.
Further, the concentration of the silver nanowire solution in the step (S3) satisfies 2-5mg/ml, the length of the silver nanowire satisfies about 20-30 μm, and the diameter satisfies about 20-30 nm.
Further, the spin coating method in the step (S4) is 500rpm at the front stage for 10S, 3000rpm at the rear stage for 30S, and the pre-annealing time is 5 min.
Further, the exposure time in the step (S5) satisfies 20 to 30S.
Further, in the step (S6), the developing solution is prepared in a ratio of AZ 400K to water of 1:4, wherein the developing time satisfies 20 to 30S.
Further, the physical brushing method in the step (S7) is to repeatedly brush the glass substrate with a nylon long rod brush to completely remove the silver nanowires.
Further, the method of removing the residual photoresist in the step (S8) is to dip the glass substrate into an acetone solution to remove the residual photoresist.
Specifically, the concentration of the polyvinyl alcohol solution in the step (S10) satisfies 8 to 10 wt.%.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method comprises the steps of spraying a silver nanowire solution on a glass substrate in an electrode transfer printing mode, spinning and coating photoresist on a required silver nanowire film, developing by using a developing solution to obtain a required silver nanowire pattern, repeatedly scrubbing and removing redundant silver nanowires by using a nylon long rod brush, and finally removing residual photoresist to obtain a required finished product. The preparation of the high-precision micro-nano electrode is realized by the method, the problem of rough edge of the conductive channel caused by incomplete etching is solved, and meanwhile, the step of etching metal corrosive liquid is replaced by a method of physically brushing the nylon long rod row brush, so that the preparation time and cost are saved, and the pollution of redundant etching waste liquid to the environment is avoided.
(2) The invention utilizes polyvinyl alcohol to uncover the silver nanowire pattern, thereby greatly ensuring the mechanical property of the prepared flexible electrode and effectively improving the mechanical property of the electrode.
Drawings
FIG. 1 is a flow chart of the present invention.
FIG. 2 is a schematic diagram of the transmittance of the visible wavelength band of the silver nanowire transparent electrode prepared by the method of the present invention.
Fig. 3 is a schematic diagram of a mechanical performance test of the silver nanowire transparent electrode prepared by the method under a condition of multiple bending.
Fig. 4(a) is a schematic diagram of the edge roughness of a silver nanowire electrode in the preparation process of the micro-nano silver nanowire electrode.
FIG. 4(b) shows the auxiliary filtration method using wax pattern1Schematic diagram of edge roughness of silver nanowire electrode below.
FIG. 4(c) is a schematic view showing a screen printing method2Schematic diagram of edge roughness of silver nanowire electrode below.
Detailed Description
The present invention is further illustrated by the following figures and examples, which include, but are not limited to, the following examples.
Examples
The invention provides a preparation method of a high-precision patternable micro-nano silver nanowire transparent electrode, and aims to enable the electrode to have good conductivity and mechanical property by an optimal preparation process. The specific preparation process flow of the electrode is as follows, as shown in fig. 1:
(S1) the step of cleaning the glass substrate is to ultrasonically clean the glass substrate by sequentially adopting deionized water, ethanol solution and acetone solution;
(S2) subjecting the dried glass substrate to O2Pre-treating the Plasma for 10-15 min;
(S3) spraying a solution of silver nanowires on a glass substrate, wherein the concentration of the solution of silver nanowires meets 2-5mg/ml, the length of the silver nanowires meets about 20-30 mu m, and the diameter of the silver nanowires meets 20-30nm, and the spraying adopts a paint spraying air gun with the air pressure meeting 15-30 PSI;
(S4) spin-coating a photoresist AZ 4620 on the silver nanowire conductive film, wherein the spin-coating mode of the AZ 4620 is that the front stage is 500rpm, the time is 10S, the rear stage is 3000rpm, the time is 30S, and pre-annealing treatment is carried out on a heating table for 5 min;
(S5) exposing the photoresist film with the assistance of a photolithography mask for an optimal time of 20-30S, thereby avoiding overexposure;
(S6) immersing the exposed glass substrate in an AZ 400K: developing in a developing solution with water of 1:4 for 20-30s, thereby avoiding fine pattern damage caused by over-development;
(S7) repeatedly brushing the glass substrate by using a nylon long rod row brush to completely remove the silver nanowires exposed outside the photoresist;
(S8) immersing the brushed glass substrate in an acetone solution to completely remove the residual photoresist;
(S9) drying the glass substrate;
(S10) pouring a polyvinyl alcohol solution with the concentration of 8-10 wt.% on the glass substrate to cover the whole electrode pattern, and after the whole electrode pattern is dried in the air, uncovering the PVA film to obtain the micro-nano silver nanowire transparent electrode.
The transmittance, conductivity and mechanical properties of the flexible electrode were tested:
fig. 2 shows the visible band transmittance of the prepared silver nanowire transparent electrode; fig. 3 shows the mechanical performance test results of the prepared silver nanowire transparent electrode (200 micrometers long and 30 micrometers wide) under multiple bending conditions. From the test results of fig. 2 and 3, it can be seen that the silver nanowire transparent electrode prepared by the invention has good transmittance and mechanical properties.
The schematic diagram of the edge roughness of the silver nanowire electrode prepared by the invention is shown in fig. 4(a), and as can be seen from fig. 4(a), the edge roughness of the micro-nano silver nanowire electrode prepared by the invention is similar to a smooth micro-nano silver nanowire electrode under the condition that the scale is 100um, so that the problem of rough edge of a conductive channel caused by incomplete etching is well solved. The invention also introduces the prior conventional treatment method (wax mold auxiliary filtration method)1And a screen printing method2) By way of comparison, the wax pattern assisted filtration method can be seen in FIG. 4(b)1The edge roughness of the silver nanowire electrode is very obvious and outstanding in the case of a scale bar of 100um, and it can be seen from fig. 4(c) that the screen printing method is adopted2The silver nanowire electrode edge roughness is also relatively significant with a scale bar of 100 um.
Meanwhile, the present invention compares the existing commonly used processes in a table manner, and the specific conditions are shown in table 1.
TABLE 1 comparison of the Process of the invention with the prior art
It can be clearly seen from table 1 that, compared with the existing common processes, the present invention solves the technical problems to be solved by the present invention, and the comparison of the relevant data in table 1 shows that the etching time of the metal in the micro-patterning process of the silver nanowire flexible transparent electrode is shortest, and the roughness of the edge of the conductive channel caused by incomplete etching is smallest, so that the present invention can be obtained.
The above embodiments are only preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, but all changes that can be made by applying the principles of the present invention and performing non-inventive work on the basis of the principles shall fall within the scope of the present invention.
Claims (10)
1. A preparation method of a high-precision patternable micro-nano silver nanowire transparent electrode is characterized by comprising the following steps:
(S1) cleaning the glass substrate and then drying the glass substrate;
(S2) pretreating the dried glass substrate;
(S3) spraying a silver nanowire solution on the glass substrate;
(S4) spin-coating photoresist on the silver nanowire conductive film, and performing pre-annealing treatment;
(S5) exposing the photoresist film with the aid of a photolithography mask;
(S6) immersing the exposed glass substrate in a developing solution for development;
(S7) completely removing the silver nanowires exposed outside the photoresist by adopting a physical brushing mode;
(S8) completely removing the photoresist remaining on the glass substrate;
(S9) drying the glass substrate;
(S10) pouring a polyvinyl alcohol solution on the glass substrate to cover the whole electrode pattern, and after the glass substrate is aired, uncovering the PVA film to obtain the micro-nano silver nanowire transparent electrode.
2. The method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode according to claim 1, wherein the step (S1) of cleaning the glass substrate is to perform ultrasonic cleaning on the glass substrate by sequentially adopting deionized water, ethanol solution and acetone solution.
3. The method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode as claimed in claim 1, wherein the pretreatment method in the step (S2) is to perform pretreatment on a glass substrate for 10-15min by using O2 Plasma.
4. The method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode according to claim 1, wherein the concentration of the silver nanowire solution in the step (S3) is 2-5mg/ml, the length of the silver nanowire is about 20-30 μm, and the diameter is 20-30 nm.
5. The method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode according to claim 1, wherein the spin coating manner in the step (S4) is 500rpm at the front stage, 10S at the rear stage, 3000rpm at the rear stage, and 30S at the rear stage, and the pre-annealing time is 5 min.
6. The method for preparing the high-precision patternable micro-nano silver nanowire transparent electrode according to claim 1, wherein the exposure time in the step (S5) is 20-30S.
7. The method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode according to claim 1, wherein in the step (S6), a developing solution is prepared according to a ratio of AZ 400K to water of 1:4, wherein the developing time is 20-30S.
8. The method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode according to claim 1, wherein the physical brushing manner in the step (S7) is to repeatedly brush the glass substrate by using a nylon long rod row brush to completely remove the silver nanowires.
9. The method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode according to claim 1, wherein the method for removing the residual photoresist in the step (S8) is to immerse the glass substrate in an acetone solution to remove the residual photoresist.
10. The method for preparing a high-precision patternable micro-nano silver nanowire transparent electrode according to claim 1, wherein the concentration of the polyvinyl alcohol solution in the step (S10) is 8-10 wt.%.
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| WO2013134779A1 (en) * | 2012-03-09 | 2013-09-12 | Ayon, Arturo, A. | Self-aligned tunable metamaterials |
| CN104575869A (en) * | 2015-01-12 | 2015-04-29 | 北京大学 | Patterning etching method of transparent conducting electrode and patterning transparent conducting electrode |
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- 2021-09-22 CN CN202111106540.4A patent/CN113921192B/en active Active
Patent Citations (9)
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| CN102087886A (en) * | 2009-12-08 | 2011-06-08 | 中国科学院福建物质结构研究所 | Silver nanowire-based transparent conductive thin film and preparation method thereof |
| WO2013134779A1 (en) * | 2012-03-09 | 2013-09-12 | Ayon, Arturo, A. | Self-aligned tunable metamaterials |
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