CN113270234A - Universal preparation method of coffee ring-shaped metal nanowire conductive electrode - Google Patents
Universal preparation method of coffee ring-shaped metal nanowire conductive electrode Download PDFInfo
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- CN113270234A CN113270234A CN202110511273.2A CN202110511273A CN113270234A CN 113270234 A CN113270234 A CN 113270234A CN 202110511273 A CN202110511273 A CN 202110511273A CN 113270234 A CN113270234 A CN 113270234A
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- 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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- H—ELECTRICITY
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- 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
Abstract
The invention belongs to the technical field of conductive electrodes, and provides a universal preparation method of a coffee ring-shaped metal nanowire conductive electrode. The preparation method of the conductive electrode comprises the steps of regulating and controlling the contact angle of the surface of any substrate to 60-180 degrees in a physical or chemical mode, and then spraying a metal nanowire solution on the surface of the substrate; under the action of capillary flow, the metal nanowires in the solution are driven from the central position to the edge position to form the metal nanowire conductive electrode with an ordered grid structure (also called a coffee ring structure).
Description
Technical Field
The invention belongs to the technical field of conductive electrodes, and relates to a universal preparation method of a coffee annular metal nanowire conductive electrode.
Background
The statements in this section merely provide background information related to the present disclosure and may not necessarily constitute prior art.
In the process of changing from industrialization to information-oriented society, the electronic manufacturing industry is rapidly developing, and the conductive electrode plays an indispensable and important role in the modern electronic manufacturing industry, and the application range of the conductive electrode covers many fields. For example, various electronic devices such as a touch panel, a solar cell, an organic light emitting diode, an electromagnetic shielding device, and a heater. In addition, the method also has very wide application value in the aspects of emerging health care, such as epidermal electrodes, electroencephalogram monitoring, intelligent contact lenses and the like.
The most widely used conductive electrode at present is tin-doped Indium Tin Oxide (ITO). Although the technology is mature, the ITO conductive electrode needs to be prepared at high temperature, which greatly limits the choice of substrate. There are three common ITO electrode substrates currently on the market, one is glass, one is Polyimide (PI), and the other is reinforced polyethylene terephthalate (PET). This is mainly due to the relatively high temperature resistance of these substrates. And others, such as: substrates with relatively low temperature resistance, such as Polyethylene (PE), polylactic acid (PLA), polyvinyl chloride (PVC), paper sheets, wood and the like, cannot be doped at high temperature to prepare the ITO conductive electrode. In the current research, various methods for preparing the conductive electrode have certain requirements on the selection of a substrate, and the universality is poor.
In view of the above research, the inventors believe that although the above solution can expand the choice of the conductive electrode substrate to some extent, the universality is still relatively limited, which greatly limits the application of the conductive electrode.
Disclosure of Invention
In order to solve the technical problems in the background art, the invention provides a method for regulating and controlling a contact angle of a substrate surface (including but not limited to a physical method of micro-nano processing and a chemical method of using a hydrophobic solution for processing), and realizes a conductive electrode of a coffee ring-shaped (also called as an ordered grid shape) metal nanowire (including but not limited to a gold nanowire, a silver nanowire, a copper nanowire, a nickel nanowire, a platinum nanowire and the like) prepared on the surface of any substrate (including but not limited to glass, a silicon wafer, paper, ceramics, metal, plastics, wood materials, flexible high polymer substrates and the like), wherein the silver nanowire (Ag NWs) is taken as a representative of the metal nanowire, the preparation process is simple, the requirement on equipment is low, and the prepared conductive electrode is universal and suitable for large-area batch production.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first aspect of the present invention provides a universal preparation method of a coffee ring-shaped metal nanowire (including but not limited to gold nanowire, silver nanowire, copper nanowire, nickel nanowire, platinum nanowire, etc.) conductive electrode, thereby obtaining a conductive thin film with uniform resistance, which comprises:
the contact angle regulation is carried out on any substrate surface (including but not limited to glass, silicon wafers, paper, ceramics, metal, plastics, wood materials, flexible high polymer substrates and the like) through physical or chemical aspects, and then
Spraying a metal nanowire solution (taking an Ag NWs solution as an example) on the surface of the base material;
under the action of capillary flow, AgNWs in the Ag NWs solution are driven from the central position to the edge position to form an AgNWs ordered grid-like structure (also called a 'coffee ring structure'), thereby obtaining the conductive electrode.
Further, the contact angle is regulated to be 50-180 degrees.
Further, the diameter of the metal nanowire (such as Ag NWs) is 10-200 nm.
Further, the length of the metal nanowire (such as Ag NWs) is 1-500 um.
Further, the metal nanowire solution is an aqueous solution, an organic solution or a mixed solution of water and an organic solution of the metal nanowire.
Further, the organic solution is isopropanol, ethanol or methanol solution.
Further, the concentration of the metal nanowire solution (such as Ag NWs) is 0.001-10 mg/ml.
Further, the metal nanowire solution is sprayed on the surface of the base material subjected to contact angle regulation and control through spraying equipment.
The invention provides a universal preparation method of the coffee ring-shaped metal nanowire conductive electrode, which is used for preparing the ordered latticed AgNWs conductive electrode on different substrates (including but not limited to glass, silicon wafers, paper, ceramics, metals, plastics, wood materials, flexible high polymer substrates and the like), and is suitable for various flexible and non-flexible electronic devices and equipment.
The invention has the beneficial effects that:
in the preparation process of the conductive electrode provided by the invention, the contact angle of the surface of the substrate is regulated to 50-180 degrees by a physical or chemical method, and then Ag NWs solution is sprayed on the surface of the substrate; under the action of capillary flow, AgNWs in the solution are driven from the central position to the edge position to form an ordered latticed AgNWs structure, which can also be called as a coffee ring structure. Therefore, in practical application, the conductive electrodes with different substrates can be prepared according to different requirements, and the application range of the metal nanowire electrode is greatly expanded.
Advantages of additional aspects of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 is a schematic reference flow chart of a method for manufacturing a conductive electrode according to the present invention;
FIG. 2(a) is an optical microscope image of the surface topography obtained by spraying the gold thin film as a substrate according to example 1 of the present invention, wherein the contact angle of the substrate surface is not controlled;
FIG. 2(b) is an optical microscope photograph of the surface topography obtained by spraying the gold thin film as a substrate according to example 1 of the present invention after the contact angle of the substrate surface is adjusted;
FIG. 3(a) is an optical microscope photograph of the surface topography obtained by spraying the glass slide as a substrate with an unregulated contact angle of the substrate surface according to example 2 of the present invention;
FIG. 3(b) is an optical microscope photograph of the surface topography obtained by spraying the glass slide as a substrate after the contact angle of the substrate surface is adjusted according to the embodiment 2 of the present invention;
FIG. 4(a) is an optical microscope image of the surface topography obtained by spraying the nylon film as a substrate according to example 3 of the present invention, wherein the contact angle of the substrate surface is not controlled;
FIG. 4(b) is an optical microscope image of the surface morphology obtained by spraying the nylon film as a substrate in example 3 of the present invention after the contact angle of the substrate surface is adjusted;
FIG. 5(a) is an optical microscope image of the surface topography obtained by spraying the paper sheet (A4 paper) as a substrate and the contact angle of the substrate surface is not adjusted according to the invention in example 4;
FIG. 5(b) is an optical microscope photograph of the surface topography obtained by spraying the substrate with a paper sheet (A4 paper) according to example 4 of the present invention after the contact angle of the substrate surface is adjusted.
Detailed Description
The invention is further described with reference to the following figures and examples.
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
In the present invention, terms such as "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "side", "bottom", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only terms of relationships determined for convenience of describing structural relationships of the parts or elements of the present invention, and are not intended to refer to any parts or elements of the present invention, and are not to be construed as limiting the present invention.
In the present invention, terms such as "fixedly connected", "connected", and the like are to be understood in a broad sense, and mean either a fixed connection or an integrally connected or detachable connection; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be determined according to specific situations by persons skilled in the relevant scientific or technical field, and are not to be construed as limiting the present invention.
In order to solve the defects of poor universality of conductive electrode substrate selection and complex preparation method in the prior art mentioned in the background art, the invention provides a universal preparation method of a metal nanowire conductive electrode in the shape of a coffee ring, which prepares the metal nanowire conductive electrode in an ordered grid structure by regulating and controlling a contact angle of the surface of the substrate, takes metal Ag NWs as an example for description, and the specific process is shown in figure 1 and comprises the following steps:
step 1: the contact angle of any substrate surface is regulated to 50-180 degrees by a chemical or physical method.
In this embodiment, the substrate includes, but is not limited to, a Polyimide (PI) film, a Colorless Polyimide (CPI) film, a Polyester (PET) film, a metal film (gold, silver, copper, etc.), a glass slide, a paper sheet, a Nylon film (Nylon), Polytetrafluoroethylene (PTFE), polyvinyl chloride (PVC), etc.
Step 2: and spraying an Ag NWs solution on the surface of the base material after the contact angle regulation of the surface of the base is finished.
In this embodiment, the diameter of the Ag NWs in the Ag NWs solution is 10-200 nm. The length of the nano silver in the nano silver solution is 1-500 um. The Ag NWs solution is an aqueous solution, an organic solution or a mixed solution of water and the organic solution of Ag NWs.
Specifically, the organic solution is isopropanol, ethanol or methanol solution. The concentration of the nano silver solution is 0.001-10 mg/ml. And the Ag NWs solution is sprayed on the surface of the base material regulated and controlled by the contact angle in a spraying and covering mode. The carrier gas used for spraying includes, but is not limited to, high purity air, nitrogen, argon, and the like.
The size of the ordered grid-like (also referred to as coffee ring) structure can be adjusted by the pressure of the carrier gas, the nozzle size, and the viscosity of the fluid. The higher the pressure of the carrier gas is, the smaller the nozzle size is, the more easily AgNWs solution is dispersed into small droplets, so that the small droplets are sprayed on a substrate, and the grid-shaped size obtained after the solvent is volatilized and dried is smaller; similarly, when the concentration of the metal Ag NWs solution is small, i.e. the viscosity of the fluid is small, the carrier gas can disperse the solution into small droplets more easily, resulting in an ordered grid structure with small size.
And step 3: under the action of capillary flow, AgNWs in the Ag NWs solution is driven from the central position to the edge position to form an AgNWs ordered grid structure, and then the conductive electrode with relatively uniform resistance is obtained.
Compared with the prior art, the invention utilizes the coffee ring effect, namely when metal nanowire solution with certain concentration is sprayed on the surface of the substrate, sprayed small droplets are pinned on the surface of the substrate, because the evaporation speed in the middle of the droplets is lower than that of the edge area, capillary flow is generated, so that the metal nanowires in the solution are driven from the central position to the edge position, and the coffee ring is generated. The method has the advantages of low cost, simple preparation, low requirements on experimental equipment, materials and environment, capability of remarkably reducing the contact resistance of the metal nanowires and convenience for large-scale batch production, and in addition, the size of the ordered latticed structure can be regulated and controlled according to actual requirements, so that reasonable sheet resistance and transparency can be selected according to the requirements of actual application.
Through the targeted regulation and control of the contact angle of the surface of the substrate, the metal nanowire structure with the ordered grid structure can be obtained on the surfaces of various substrates through a spraying method, and then the high-performance conductive electrode with uniform resistance is prepared on any substrate.
Four different examples are given below based on different AgNWs sizes and solution concentrations and different spray parameters:
example 1
The method for preparing the metal AgNWs coffee ring conductive electrode with the ordered grid structure on the surface of the gold film comprises the following steps:
and (3) adding nano silver with the diameter and the length of 30nm and 20um into IPA to prepare an AgNWs solution with the concentration of 0.5mg/ml, adding the AgNWs solution into spraying equipment, and spraying the AgNWs solution on the surface of a gold film regulated and controlled by a contact angle to obtain the AgNWs coffee ring conductive electrode with the ordered grid structure (figure 2 b).
Wherein, the gold thin film is used as the substrate, but the surface is not controlled by the contact angle, and the surface morphology obtained by spraying is a disordered structure as shown in figure 2 (a).
Example 2
The method for preparing the metal AgNWs coffee ring conductive electrode with the ordered grid structure on the surface of the glass slide substrate comprises the following steps:
ag NWs with the diameter of 10nm and the length of 20 microns are selected and added into IPA to prepare AgNWs solution with the concentration of 5mg/ml, the AgNWs solution is added into spraying equipment, and then the AgNWs solution is sprayed on the surface of a glass slide regulated and controlled by a contact angle, so that the metal AgNWs coffee ring conductive electrode with an ordered latticed (also called 'coffee ring shape') structure is obtained (figure 3 b).
In which the glass slide is used as a substrate, but the surface thereof is not controlled by a contact angle, and the surface morphology obtained by spraying is a disordered structure as shown in fig. 3 (a).
Example 3
The method for preparing the metal AgNWs coffee ring conductive electrode with the ordered grid structure on the surface of the nylon film comprises the following steps:
and (3) adding nano silver with the diameter of 80nm and the length of 60 micrometers into IPA to prepare AgNWs solution with the concentration of 2mg/ml, adding the AgNWs solution into spraying equipment, and spraying the AgNWs solution on the surface of a nylon film regulated and controlled by a contact angle to obtain the metal AgNWs coffee ring conductive electrode with the ordered grid structure (figure 4 b).
Wherein, the nylon film is used as a base material, but the surface of the nylon film is not controlled by a contact angle, and the surface appearance obtained by spraying is a disordered structure as shown in figure 4 (a).
Example 4
The method for preparing the metal AgNWs coffee ring conductive electrode with the ordered grid structure on the surface of the paper sheet (A4 paper) is as follows:
adding 0.5mg/ml AgNWs solution into spraying equipment, and then spraying the AgNWs solution on the surface of the paper sheet modified by the contact angle, thereby obtaining the AgNWs coffee ring conductive electrode with the ordered grid structure (figure 5 b).
Wherein, the paper sheet is used as a base material, but the surface contact angle is not regulated, and the surface topography obtained by spraying is shown in figure 5(a) and is a disordered structure.
The method for preparing the metal AgNWs coffee ring conductive electrode with the ordered latticed structure through substrate surface contact angle regulation has the advantages of simple process, low requirement on equipment, universality, suitability for large-area batch production and suitability for various substrate surfaces including but not limited to glass, silicon wafers, wood, paper, metal, ceramics, materials, all organic matter flexible substrates and the like.
The preparation process provided by the embodiment is simple, is friendly to industrial expanded production, and can easily realize the adjustment of the ordered latticed size by adjusting the spraying parameters, so that the targeted regulation and control can be performed according to different applications.
The method for preparing the coffee ring-shaped metal nanowire conductive electrode can be popularized to the field of electronic devices.
For example: the application of the AgNWs coffee ring conductive electrode with the ordered grid structure based on surface contact angle modification in the fields of information, energy, medical treatment and national defense;
applications in information include, without limitation, use in the manufacture of electronic displays, electronic storage materials, touch-sensitive materials, printing devices, and the like.
Applications in the medical field include, but are not limited to, use in the manufacture of flexible wearable medical devices.
Applications in the energy field include, but are not limited to, thin film solar cells, metallurgical equipment, thermal processing equipment, and the like.
Applications in the defense area include, but are not limited to, applications in the aerospace area.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A universal preparation method of a coffee ring-shaped metal nanowire conductive electrode is characterized by comprising the following steps:
regulating and controlling a contact angle of any substrate surface by a physical or chemical method, and then spraying a metal nanowire solution on the substrate surface;
under the action of capillary flow, the metal nanowires in the solution are driven from the central position to the edge position to form an ordered grid-shaped structure, and then the conductive electrode is obtained.
2. The universal preparation method of the coffee ring-shaped metal nanowire conductive electrode as claimed in claim 1, wherein the contact angle of the substrate surface is regulated to be 50-180 °.
3. The universal preparation method of the coffee ring-shaped metal nanowire conductive electrode as claimed in claim 1, wherein the diameter of the metal nanowires in the solution is 10-200 nm.
4. The universal preparation method of the coffee ring-shaped metal nanowire conductive electrode as claimed in claim 1, wherein the length of the metal nanowire in the solution is 1-500 um.
5. The universal preparation method of the coffee ring-shaped metal nanowire conductive electrode as claimed in claim 1, wherein the metal nanowire solution is an aqueous solution, an organic solution or a mixture of water and an organic solution.
6. The universal preparation method of the coffee ring morphology metal nanowire conducting electrode as claimed in claim 1, wherein the organic solution is isopropanol, ethanol or methanol solution.
7. The universal preparation method of the coffee ring-shaped metal nanowire conductive electrode as claimed in claim 1, wherein the concentration of the nano silver solution is 0.001-10 mg/ml.
8. The universal preparation method of the coffee ring-shaped metal nanowire conductive electrode as claimed in claim 1, wherein the metal nanowire solution is sprayed on the surface of the substrate by a spraying method.
9. The universal preparation method of the coffee ring-shaped metal nanowire conductive electrode as claimed in claim 1, wherein the coffee ring-shaped metal nanowire is transferred by an organic polymer substrate material by a reverse mold method to prepare the embedded conductive electrode with the ordered grid structure.
10. The coffee ring-shaped metal nanowire conductive electrode prepared by the universal preparation method of the coffee ring-shaped metal nanowire conductive electrode as claimed in any one of claims 1 to 9, which is suitable for various flexible and non-flexible electronic devices and equipment.
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Citations (5)
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| CN105271110A (en) * | 2015-09-18 | 2016-01-27 | 北京工业大学 | Method of manufacturing dense nano granular film and ordered nanowire film by using coffee-ring effects |
| CN106648259A (en) * | 2017-01-09 | 2017-05-10 | 京东方科技集团股份有限公司 | Touch screen manufacturing method, touch screen and displaying device |
| CN112053800A (en) * | 2020-07-31 | 2020-12-08 | 山东大学 | Embedded high-temperature-resistant transparent conductive film, and preparation method and application thereof |
| US20210016349A1 (en) * | 2018-03-08 | 2021-01-21 | Nanyang Technological University | Scalable electrically conductive nanowires bundle-ring-network for deformable transparent conductor |
| CN112670411A (en) * | 2020-12-11 | 2021-04-16 | 华南理工大学 | Full-solution flexible organic thin film transistor array and preparation method and application thereof |
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- 2021-05-11 CN CN202110511273.2A patent/CN113270234A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271110A (en) * | 2015-09-18 | 2016-01-27 | 北京工业大学 | Method of manufacturing dense nano granular film and ordered nanowire film by using coffee-ring effects |
| CN106648259A (en) * | 2017-01-09 | 2017-05-10 | 京东方科技集团股份有限公司 | Touch screen manufacturing method, touch screen and displaying device |
| US20210016349A1 (en) * | 2018-03-08 | 2021-01-21 | Nanyang Technological University | Scalable electrically conductive nanowires bundle-ring-network for deformable transparent conductor |
| CN112053800A (en) * | 2020-07-31 | 2020-12-08 | 山东大学 | Embedded high-temperature-resistant transparent conductive film, and preparation method and application thereof |
| CN112670411A (en) * | 2020-12-11 | 2021-04-16 | 华南理工大学 | Full-solution flexible organic thin film transistor array and preparation method and application thereof |
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