CN112863766A - Method for preparing coffee ring conductive film based on silicon substrate and application - Google Patents
Method for preparing coffee ring conductive film based on silicon substrate and application Download PDFInfo
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Abstract
The invention provides a method for preparing a coffee ring conductive film based on a silicon substrate and application thereof. The defects of poor sheet resistance uniformity and large roughness of the flexible conductive film in the prior art are overcome. The invention aims to provide a conductive thin film material which is simple in preparation process, uniform in sheet resistance and low in roughness. Based on the purpose, the invention provides a method for preparing a coffee ring conductive film based on a silicon substrate, which comprises the steps of applying a metal precursor solution to the surface of the silicon substrate to obtain a coffee ring conductive grid, coating a flexible liquid flexible substrate on the conductive grid, curing the liquid flexible substrate to form a film, and peeling the conductive film from the silicon substrate to obtain the conductive film. The invention verifies that the conductive film has uniform sheet resistance and low root mean square roughness, and is suitable for various electronic equipment.
Description
Technical Field
The invention belongs to the technical field of flexible conductive films, and particularly relates to a silicon-based substrate (comprising Si and SiO)2Substrate), a method for preparing a coffee ring conductive film, a conductive film prepared by the preparation method and application.
Background
The information in this background section is only for enhancement of understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
With the development of the times, the living needs of people are continuously improved. The proportion of the flexible transparent conductive film in the market is also getting bigger and bigger, and the application is also getting wider and wider, and the flexible transparent conductive film comprises various electronic devices such as a flexible touch screen, a curved screen, a sports bracelet, a flexible solar cell and a flexible OLED. The method has a very wide application prospect in the field of flexible intelligent electronic devices.
Most of the flexible transparent conductive films on the market at present are mainly made of traditional tin-doped Indium Tin Oxide (ITO)/PET materials. The reason is mainly from the excellent photoelectric property, more uniform sheet resistance and relatively low roughness, but due to the shortage of indium resources and the fact that the ITO is a brittle material, the long-term development of the ITO transparent conductive film in the field of flexible electronics is greatly limited. Among alternative materials such as silver nanowires (AgNWs), carbon nanotubes, graphene, metal meshes, etc., AgNWs attracts more attention by virtue of its superior photoelectric properties, excellent flexibility, and lower cost. However, the AgNWs conductive thin film also has some disadvantages in practical applications, such as non-uniform sheet resistance, large roughness, etc.
In the current research, the research on the sheet resistance uniformity of the conductive film is less, the sheet resistance uniformity effect is not ideal, the preparation process is more complex, and the cost is higher.
Disclosure of Invention
Based on the above research background, the present invention aims to provide a conductive thin film material with simple preparation process, uniform sheet resistance and low roughness, aiming at the problems of large surface roughness and non-uniform sheet resistance of the AgNWs conductive thin film.
Aiming at the research purpose, the invention provides the following technical scheme:
in a first aspect of the present invention, a method for preparing a coffee ring conductive film based on a silicon substrate is provided, the preparation method comprising the steps of: and applying the metal precursor solution to the surface of the silicon substrate to obtain a coffee annular conductive grid, coating a flexible liquid flexible substrate on the conductive grid, curing the liquid flexible substrate into a film, and stripping the conductive film from the silicon substrate to obtain the conductive film.
In previous studies by the inventors, an embedded flexible transparent high temperature resistant conductive film of AgNWs coffee ring and Polyimide (PI) was provided. Researches show that the 'coffee ring' structure can effectively reduce the contact resistance of AgNWs, and the embedded structure can improve the stability, particularly the heat resistance, of the conductive film. Based on the research result, the inventor thinks that the preparation process of the transparent high-temperature-resistant conductive film is further optimized, and the conductive film which has the low resistance and high stability, can reduce the roughness and improve the sheet resistance uniformity is obtained. Based on the design thought, the invention adopts silicon as a substrate material, and researches on how to prepare a coffee ring structure on the silicon surface. The conductive film prepared based on the method has good sheet resistance uniformity and can be used as a good substitute product of ITO/PET.
In a second aspect of the invention, a conductive film prepared by the method for preparing the coffee ring conductive film based on the silicon substrate in the first aspect is provided.
In a third aspect of the present invention, there is provided the use of the conductive film of the second aspect in the fields of information, energy, medical treatment, and defense.
The beneficial effects of one or more technical schemes are as follows:
the conductive film provided by the invention has the advantages of low cost, simple preparation, low requirements on experimental equipment, materials and environment, strong adjustability and large-scale batch production. And the conductive film has good sheet resistance uniformity and low roughness, and the comprehensive performance is superior to that of the commercial ITO/PET flexible conductive film.
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 shows that the Si and SiO-based material of the present invention2A reference flow schematic diagram of a preparation method of the flexible transparent conductive film of the/Si substrate coffee ring;
FIG. 2 is an optical microscopy image of a Si-based coffee ring according to example 1 of the present invention;
FIG. 3 is SiO according to example 1 of the present invention2Si-based coffee ring lightA microscope map is learned;
FIG. 4 is an atomic force microscope atlas of a flexible conductive film as described in example 1 of the invention;
FIG. 5 is a graph of sheet resistance uniformity of the flexible conductive film according to example 1 of the present invention;
fig. 6 is an optical microscopy image of gunws coated on a hard glass substrate.
Detailed Description
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.
Interpretation of terms:
and (3) coffee ring: when AgNWs solution with a certain concentration is sprayed on a substrate, small sprayed droplets are pinned on the surface of the substrate, because the evaporation speed in the middle of the droplets is lower than that in the edge region, the capillary flow generated in the way can inhibit the Maligoni effect, so that AgNWs in the solution is driven from the central position to the edge position to generate a 'coffee ring', and the 'coffee ring' and the 'coffee ring structure' in the application document refer to a continuous annular structure formed by AgNWs on the surface of the substrate material.
SiO2Si substrate: one of the surfaces has SiO2Silicon wafer of layer, said SiO2The thickness of the/Si substrate is 100-1000 um, wherein SiO2The layer thickness is 50-1000 nm.
As introduced by the background art, aiming at the technical problem of high roughness of the AgNWs conductive film in the prior art, the invention provides a method for preparing a coffee ring conductive film based on a silicon substrate.
In a first aspect of the present invention, a method for preparing a coffee ring conductive film based on a silicon substrate is provided, the preparation method comprising the steps of: and applying the metal precursor solution to the surface of the silicon substrate to obtain a coffee annular conductive grid, coating a flexible liquid flexible substrate on the conductive grid, curing the liquid flexible substrate into a film, and stripping the conductive film from the silicon substrate to obtain the conductive film.
Preferably, the metal precursor solution includes, but is not limited to, nano silver, nano gold, and/or nano copper.
Further, the metal precursor is nano silver, and further, is a nano silver aqueous solution, an organic solution or a mixed solution of water and an organic solution.
In some embodiments of the above preferred technical solution, the organic solution of nano silver is IPA, ethanol or methanol solution of nano silver.
In some embodiments, the nanosilver is present at a concentration of 0.001 to 10 mg/ml.
In some embodiments, the nanosilver has a diameter of 10 to 100 nm; or the length of the nano silver is 10-500 um.
Preferably, the silicon substrate is Si or SiO2A substrate.
The silicon substrate is Si or SiO2The substrate of the contact surface, i.e. the surface in contact with the metal precursor solution, is Si or SiO2。
In a specific implementation manner of the above preferred technical scheme, the Si substrate is a bare silicon wafer, and the thickness is 100-1000 um.
In one embodiment of the above preferred embodiment, the SiO is2The substrate is made of SiO2Silicon wafer of layer, said SiO2A substrate of 100-1000 um thickness and SiO2The layer thickness is 50-1000 nm.
The above Si and SiO2The main function of the/Si substrate is to provide certain tension for the formation of the nano-silver coffee ring structureAnd lower surface energy surfaces, in Si, SiO2the/Si substrate can also obtain a relatively ideal ring forming effect.
Preferably, the application method includes but is not limited to smearing, dripping or spraying. In an embodiment of the present invention with a good effect, the application method is spraying.
Further, the spraying manner is to spray the metal precursor solution on the surface of the silicon substrate by using a spray gun.
In some specific embodiments of the present invention, the specific parameters of the spraying are as follows: the diameter of the nozzle of the spray gun is 0.1-10mm, the distance from the nozzle to the polymer film is 1-100cm, and the carrier gas is inert gas, wherein the inert gas comprises high-purity air, nitrogen, argon and the like.
The size of the coffee annulus can be adjusted by the pressure of the carrier gas, the size of the nozzle, and the viscosity of the fluid. The higher the pressure of the carrier gas, the smaller the nozzle size, the more easily the AgNWs solution is dispersed into small droplets, so that the small droplets are sprayed on the substrate, and the size of the coffee ring obtained after the solvent is volatilized and dried is smaller; similarly, when the concentration of the nano-silver solution is small, i.e. the viscosity of the fluid is small, the carrier gas can disperse the solution into small droplets more easily, and a coffee ring with a smaller size is obtained.
Preferably, the flexible substrate includes, but is not limited to, a Polyimide (PI) film, a Colorless Polyimide (CPI) film, a Polyester (PET) film, a Polydimethylsiloxane (PDMS) film, a styrene rubber (SEBS) film, Polytetrafluoroethylene (PTFE), polyvinyl chloride (PVC), and the like.
Further preferably, the flexible substrate is a polyimide film; further, the thickness of the polyimide film is 10-1000 um.
According to the research result of the invention, Si and SiO are adopted2the/Si substrate coffee ring transparent conductive film can obtain uniform sheet resistance and lower surface roughness. The thickness of the flexible transparent film can be conveniently adjusted by adopting a spin-coating method. Those skilled in the art can select a suitable thickness according to the purpose of useWhen the degree is larger, the glue spreading can be realized in a mode of spreading glue for many times.
Preferably, the solid content in the liquid flexible substrate is 5-50%.
Preferably, the liquid flexible substrate is cured by heating, the curing heating temperature is 60-350 ℃, and the heating time is 20-120 min.
Further preferably, the heating is performed in a drying manner; in a specific embodiment, the spin-coated film material is placed in an oven to cure the liquid flexible substrate.
In a second aspect of the invention, a conductive film prepared by the method for preparing the coffee ring conductive film based on the silicon substrate in the first aspect is provided.
In a third aspect of the present invention, there is provided the use of the conductive film of the second aspect in the fields of information, energy, medical treatment, and defense.
Preferably, the information aspect is applied to the preparation of electronic displays, electronic storage materials, touch materials, printing equipment and the like.
Preferably, applications in the medical field include, but are not limited to, use in the manufacture of flexible wearable medical devices.
Preferably, the applications in the energy field include but are not limited to thin film solar cells, metallurgical equipment, thermal treatment equipment and the like.
Preferably, applications in the defense area include, but are not limited to, applications in the aerospace area.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1
In the present embodiment, a Si-based or SiO-based material is provided2The preparation method of the conductive film comprises the following steps: selecting nano silver with the diameter and the length of 30nm and the length of 20um, adding the nano silver into IPA to prepare AgNWs solution with the concentration of 0.5mg/ml, adding the AgNWs solution into a spray gun, wherein the diameter of the spray nozzle is 0.3mm, the spraying distance is 20cm, dissolving the AgNWs solutionSpraying on Si, SiO2On the Si substrate, the solution is volatilized to form a coffee ring.
Si, SiO to form a coffee ring2Placing the/Si substrate on a spin coater, and spin-coating the liquid polyimide solution on the Si and SiO sprayed with AgNWs coffee ring at the rotation speed of 500rpm2On a/Si substrate. Mixing the liquid polyimide with Si and SiO coated with AgNWs coffee ring2Putting the/Si substrate into an oven, heating at 100 ℃ for 60min, forming a cured flexible conductive film by the film to be cured, and spraying the AgNWs coffee ring coated Si and SiO2And after the/Si substrate film and the solidified flexible conductive film are cooled, peeling off the flexible conductive film.
Example 2
In the present embodiment, a Si-based or SiO-based material is provided2The preparation method of the conductive film comprises the following steps: adding nano silver with the diameter of 10nm and the length of 20 mu m into IPA to prepare AgNWs solution with the concentration of 5mg/ml, adding the AgNWs solution into a spray gun, wherein the diameter of the spray nozzle is 0.1mm, the spraying distance is 30cm, and spraying the AgNWs solution on Si and SiO2On the Si substrate, the solution is volatilized to form a coffee ring.
Si, SiO to form a coffee ring2Placing the/Si substrate on a spin coater, and spin-coating the liquid polyimide solution on the Si and SiO sprayed with AgNWs coffee ring at the rotation speed of 600rpm2On a/Si substrate. Mixing the liquid polyimide with Si and SiO coated with AgNWs coffee ring2Putting the/Si substrate into an oven, heating at 120 ℃ for 30min, forming a cured flexible conductive film by the film to be cured, and spraying Si and SiO on the AgNWs coffee ring2And after the/Si substrate and the solidified flexible conductive film are cooled, peeling off the flexible conductive film.
Example 3
In the present embodiment, a Si-based or SiO-based material is provided2The preparation method of the conductive film comprises the following steps: selecting nano silver with the diameter of 80nm and the length of 60 mu m respectively, adding the nano silver into IPA to prepare the nano silver with the concentration of2mg/ml of AgNWs solution, adding the AgNWs solution into a spray gun, spraying the AgNWs solution on Si and SiO, wherein the diameter of the spray nozzle is 3mm, and the spraying distance is 70cm2On the Si substrate, the solution is volatilized to form a coffee ring.
Si, SiO to form a coffee ring2Placing the/Si substrate on a spin coater, and spin-coating the liquid polyimide solution on the Si and SiO sprayed with AgNWs coffee ring at the rotation speed of 500rpm2On a/Si substrate. Mixing the liquid polyimide with Si and SiO coated with AgNWs coffee ring2Putting the/Si substrate into an oven, heating for 50min at 130 ℃, forming a cured flexible conductive film by the film to be cured, and spraying Si and SiO on the AgNWs coffee ring2And after the/Si substrate and the solidified flexible conductive film are cooled, peeling off the flexible conductive film.
In this example, the surface roughness of the conductive thin film described in example 1 was measured, and the results are shown in fig. 4, and as can be seen from fig. 4, the conductive thin film described in example 1 is based on Si, SiO2The root mean square roughness RMS of the flexible conductive film of the/Si substrate was 4.57 nm. This is mainly due to Si, SiO2Roughness of the Si substrate itself at atomic level.
In addition, the present example also verifies the electrical properties of the sheet resistance uniformity of the conductive film described in example 1, and the sheet resistance uniformity is better, and the maximum variation of the sheet resistance is about 5%, which is comparable to the ITO/PET with high quality.
As can be seen from FIGS. 2 and 3, the conductive film prepared by the method of the present invention has a uniform coffee ring size.
Comparative example 1
In this embodiment, a conductive film prepared on a surface of a glass substrate is provided. It is well known in the art that glass is a non-metallic material of silicates formed after melting silica with other chemicals, in contrast to SiO2The surface has a greater surface tension. In this example, glass was used as a base material, and other preparation methods were the same as those in example 1, and the obtained conductive film was as shown in fig. 6, and the solidified nano silver was only linearly stacked, and the coffee was not obtainedThe conductive performance of the ring structure is obviously reduced.
In the research process of the invention, a plurality of other similar materials or substrate materials with low surface tension are tried, and Si and SiO can not be realized2This effect of stable repetition.
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 method for preparing a coffee ring conductive film based on a silicon substrate is characterized by comprising the following steps: and applying the metal precursor solution to the surface of the silicon substrate to obtain a coffee annular conductive grid, coating a flexible liquid flexible substrate on the conductive grid, curing the liquid flexible substrate into a film, and stripping the conductive film from the silicon substrate to obtain the conductive film.
2. The silicon-based substrate-based method for preparing a coffee ring conductive film of claim 1, wherein the metal precursor solution includes but is not limited to nano silver, nano gold and/or nano copper;
preferably, the metal precursor is nano silver, and further, is a nano silver aqueous solution, an organic solution or a mixed solution of water and an organic solution; further, the nano silver organic solution is a nano silver IPA, ethanol or methanol solution;
preferably, the concentration of the nano silver is 0.001-10 mg/ml; or the diameter of the nano silver is 10-100 nm; or the length of the nano silver is 10-500 um.
3. The method for preparing a coffee ring conductive film on the basis of a silicon substrate as claimed in claim 1, wherein the silicon substrate is Si or SiO2A substrate;
preferably, the Si substrate is a bare silicon wafer with the thickness of 100-1000 um; the SiO2The substrate is made of SiO2Silicon wafer of layer, said SiO2A substrate of 100-1000 um thickness and SiO2The layer thickness is 50-1000 nm.
4. The method for preparing the coffee ring conductive film on the basis of the silicon substrate as claimed in claim 1, wherein the application manner includes but is not limited to a smearing, dropping or spraying manner;
preferably, the application mode is spraying;
further, the spraying manner is that a spray gun is adopted to spray the metal precursor solution on the surface of the silicon substrate;
specifically, the specific parameters of the spraying are as follows: the diameter of the nozzle of the spray gun is 0.1-10mm, the distance from the nozzle to the polymer film is 1-100cm, and the carrier gas is inert gas, wherein the inert gas comprises high-purity air, nitrogen and argon.
5. The silicon-based substrate-based method for preparing a coffee ring conductive film of claim 1, wherein the flexible substrate includes but is not limited to polyimide film, colorless polyimide film, polyester film, polydimethylsiloxane film, styrene rubber film, polytetrafluoroethylene, polyvinyl chloride;
preferably, the flexible substrate is a polyimide film; further, the thickness of the polyimide film is 10-1000 um.
6. The method for preparing the coffee ring conductive film based on the silicon substrate as claimed in claim 1, wherein the solid content in the liquid flexible substrate is 5-50%.
7. The method for preparing the coffee ring conductive film on the basis of the silicon substrate as claimed in claim 1, wherein the liquid flexible substrate is cured by heating, the curing heating temperature is 60-350 ℃, and the heating time is 20-120 min;
preferably, the heating is performed in a drying manner; further, the spin-coated film material is placed in an oven to be cured by the liquid flexible substrate.
8. A conductive film prepared by the method for preparing a coffee ring conductive film based on a silicon substrate according to any one of claims 1 to 7.
9. Use of the conductive film according to claim 8 in the fields of information, energy, medical treatment and defense.
10. The use of the conductive film of claim 9 in the fields of information, energy, medical and defense, wherein the information applications include but are not limited to the preparation of electronic displays, electronic storage materials, touch control materials, printing devices;
or, applications in the medical field include, but are not limited to, use in the manufacture of flexible wearable medical devices;
or, the applications in the energy field include but are not limited to thin film solar cells, metallurgical equipment, thermal treatment equipment and the like;
or, applications in the defense area include, but are not limited to, applications in the aerospace area.
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