CN109950366B - Method for preparing transparent conductive nanowire grid film on surface of three-dimensional microstructure - Google Patents
Method for preparing transparent conductive nanowire grid film on surface of three-dimensional microstructure Download PDFInfo
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- CN109950366B CN109950366B CN201910276109.0A CN201910276109A CN109950366B CN 109950366 B CN109950366 B CN 109950366B CN 201910276109 A CN201910276109 A CN 201910276109A CN 109950366 B CN109950366 B CN 109950366B
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Abstract
The invention discloses a method for preparing a transparent conductive nanowire grid film on the surface of a three-dimensional microstructure, which comprises the steps of firstly manufacturing a rigid substrate with the three-dimensional microstructure on the upper surface, then manufacturing a flexible pressing plate matched with the rigid substrate by taking the rigid substrate as a template in an imprinting mode, coating a conductive nanowire mixed solution on the three-dimensional microstructure of the rigid substrate, downwards extruding the rigid substrate and the flexible pressing plate until a certain gap is reserved between the rigid substrate and the flexible pressing plate, drying the conductive nanowire mixed solution reserved in the gap to obtain the nano grid film attached to the surface of the three-dimensional microstructure of the rigid substrate, realizing circuit conduction by conductive nanowires mutually overlapped in grids, and realizing transparency by meshes between the nanowires, namely realizing the preparation of the transparent conductive nanowire grid film on the surface of the three; before the rigid substrate is coated with the conductive nanowire mixed liquid, a micro-step is formed by adopting a method of corrosion after oxidation, and the size of a gap can be controlled by matching the rigid substrate with the flexible pressing plate; the obtained transparent conductive nanowire grid film has high quality, high preparation efficiency and low cost.
Description
Technical Field
The invention belongs to the technical field of photoelectric detection, and particularly relates to a method for preparing a transparent conductive nanowire grid film on the surface of a three-dimensional microstructure.
Background
The photoelectric detector is used for converting an optical signal into an electrical signal, and the basic principle is that a sensitive material generates a photon-generated carrier under the action of light waves, and the generated photon-generated carrier is collected by an electrode and flows out of an external circuit to form a photocurrent. Photodetectors have a wide range of uses such as imaging, detection, industrial automation, and photometry. In the photodetector, an electrode is an indispensable element. At present, the electrodes in most of the widely used photodetectors are manufactured on a planar structure, which is a mature technology. However, with the development of the photoelectric detection device, it is an important requirement to fabricate a transparent electrode on the surface of the three-dimensional microstructure, which needs to solve the two problems of continuous coverage of a complex curved surface and electrode transparency. The common methods such as sputtering, evaporation and the like can realize the preparation of the three-dimensional microstructure surface metal film electrode such as step coverage and the like in a certain range. However, if the thickness of the metal film is too small, a reliable continuous electrical path is difficult to form, the resistance is increased sharply, and if the thickness is large, the light transmittance is reduced significantly, so that it is difficult to achieve both good light transmittance and a reliable electrical path.
Disclosure of Invention
In order to solve the problems, the invention provides a method for preparing a transparent conductive nanowire grid film on the surface of a three-dimensional microstructure, the method can be used for preparing transparent conductive films continuously covered on the surfaces of various three-dimensional microstructures, and the obtained transparent conductive films are high in quality, high in preparation efficiency and low in cost.
In order to achieve the above purpose, the invention adopts the following scheme:
a method for preparing a transparent conductive nanowire grid film on the surface of a three-dimensional microstructure comprises the following steps:
firstly, selecting rigid materials such as silicon wafers and the like, preparing a three-dimensional microstructure on the upper surface of the rigid materials to obtain a rigid substrate 1 with the three-dimensional microstructure on the upper surface, and then transferring the three-dimensional structure shape of the surface layer of the rigid substrate 1 to the lower surface of a flexible material by using the rigid substrate 1 as a template and adopting an imprinting method to obtain a flexible pressing plate 2 with the three-dimensional microstructure on the lower surface;
then placing the rigid substrate 1 with the three-dimensional microstructure on the surface into a high-temperature oxidation furnace for oxidation, so that the surface material of the rigid substrate forms an oxide layer;
and placing the oxidized rigid substrate 1 into corrosive liquid to remove a surface oxide layer of the oxidized rigid substrate, wherein the corroded rigid substrate 1 and the flexible pressing plate 2 are matched to form a gap, and the size of the gap is consistent with the thickness of the oxide layer corroded and removed by the rigid substrate.
Further, before etching the rigid substrate 1, a small-area dry film is covered on several positions of the upper surface of the rigid substrate to protect the covered area, and an oxide layer in the protected area is not removed in the etching process, so that a micro-step 3 is formed for gap control of a subsequent process.
Coating a conductive nanowire mixed solution on a three-dimensional microstructure on the surface layer of a rigid substrate 1, then placing a flexible pressing plate 2 above the rigid substrate 1 to align the three-dimensional microstructure on the lower surface of the flexible pressing plate 2 with the three-dimensional microstructure on the upper surface of the rigid substrate 1, and slowly moving the flexible pressing plate 2 downwards until the flexible pressing plate 2 contacts a micro-step 3 on the surface of the rigid substrate 1; the gap between the flexible pressing plate 2 and the rigid substrate 1 is filled with the conductive nanowire mixed solution; and after the conductive nanowire mixed solution is dried, taking down the flexible pressing plate 2 to obtain the transparent conductive nanowire mesh film which is attached to the three-dimensional microstructure surface on the upper surface of the rigid substrate and is formed by the conductive nanowires.
The grid film is formed by lapping conductive nanowires to form a conductive grid, and meshes between the nanowires can transmit light, so that the transparency of the grid film is realized.
Further, the upper surface of the rigid substrate 1 is pretreated before being coated with the conductive nano mixed solution, so that the capability of adsorbing the conductive nano wires is enhanced.
Further, in the process that the flexible pressing plate 2 is close to the rigid substrate 1 but not in contact with the rigid substrate, the redundant conductive nanowire mixed liquid is squeezed to overflow the gap between the flexible pressing plate and the rigid substrate until the flexible pressing plate and the rigid substrate are in contact with each other.
Furthermore, the flexible press plate 2 and the rigid substrate 1 are placed by adopting an optical alignment platform to operate, so that the three-dimensional microstructure on the lower surface of the flexible press plate 2 is aligned with the three-dimensional microstructure on the upper surface of the rigid substrate 1, and the three-dimensional microstructures can be mutually nested.
Further, the rigid substrate 1 is made of a material capable of oxidizing to form an oxide layer and etching to remove the oxide layer, such as single crystal silicon, polysilicon, etc.
Further, the flexible pressing plate 2 is made of a flexible material capable of being molded by imprinting, such as PDMS, imprinting glue, and the like.
Further, the cross-sectional size of the micro-step 3 is determined by the size of the dry film covering, and the height thereof is determined by the oxidation time and the etching time of the rigid substrate 1; the height of the micro-step 3 controls the size of a gap between the lower surface of the flexible pressing plate 2 and the upper surface of the rigid substrate 1, so that the thickness of the finally obtained conductive nanowire grid film is controlled, and the height of the micro-step 3 is selected according to specific requirements.
Compared with the prior art, the invention has the following advantages:
1. the film which can ensure the light transmission and the electric conductivity is prepared on the surface of the three-dimensional microstructure.
2. The prepared transparent conductive film has good continuous covering effect on the surface of the three-dimensional microstructure.
3. The prepared transparent conductive film has uniform thickness and can be accurately controlled.
Drawings
FIG. 1 is a schematic diagram of a rigid substrate having a three-dimensional microstructure on its upper surface and a flexible platen having a three-dimensional microstructure on its lower surface.
FIG. 2 is a schematic diagram of the combination of the oxide layer formed on the upper surface of the rigid substrate after oxidation and the flexible platen.
FIG. 3 is a schematic diagram of the flexible platen after the oxide layer on the surface of the rigid substrate is removed by etching.
Fig. 4 is a schematic diagram of a conductive nanowire mesh film formed on the surface of a rigid substrate by pressing the rigid substrate through a flexible pressing plate.
Example of the implementation
The following describes a high-efficiency visible light detection structure and a manufacturing method thereof with reference to the accompanying drawings and embodiments.
The invention discloses a method for preparing a transparent conductive nanowire grid film on the surface of a three-dimensional microstructure, which comprises the following steps: the material of the rigid substrate 1 is a material that can be oxidized at a high temperature and the oxide layer is removed by etching, and the present embodiment is preferably monocrystalline silicon. The material of the flexible platen 2 is a material that can be molded by stamping, and the embodiment is preferably PDMS.
As shown in fig. 1, a three-dimensional microstructure is first fabricated on the upper surface of a single crystal silicon wafer, and the single crystal silicon wafer with the three-dimensional microstructure on the surface is a rigid substrate 1. And then taking the rigid substrate 1 with the three-dimensional microstructure on the upper surface as a template, coating PDMS on the surface of the template, applying certain pressure, and taking down the PDMS from the template after the PDMS is cured to form the flexible pressing plate 2 with the three-dimensional microstructure on the lower surface. The three-dimensional microstructure on the upper surface of the rigid substrate 1 and the three-dimensional microstructure on the lower surface of the flexible press plate 2 can be nested with each other, and the surfaces of the respective microstructures are attached to each other without a gap.
Further, the three-dimensional microstructure on the surface of the rigid substrate 1 shown in the figure is a rectangular step, which is only an example, and in practical application, three-dimensional microstructures with other shapes, such as black silicon, pyramid, cylindrical frustum, etc., can be made as required.
As shown in fig. 2, the rigid substrate 1 is put into a high temperature furnace to be oxidized, and an oxide layer is formed on the surface thereof. The figure only shows a part of the structure of the area near the upper surface of the rigid substrate, but not the whole substrate.
As shown in fig. 3, the oxide layer on the upper surface of the rigid substrate 1 is etched away. The rigid substrate 1 after the surface oxide layer is removed is matched with the flexible pressing plate 2, and a gap is formed between the two microstructures.
Furthermore, before removing the oxide layer on the upper surface of the rigid substrate 1 by etching, a small-area dry film is attached to a plurality of positions of the oxide layer for protection, so that the oxide layer in the area covered by the dry film is reserved in the etching of the rigid substrate 1 to form the micro-step 3. The lower surface of the flexible pressing plate 2 is contacted with the micro-step 3, and a gap is formed between the flexible pressing plate 2 and the rigid substrate 1.
As shown in fig. 4, a conductive nanowire mixed solution 4 is coated on the upper surface of the rigid substrate 1, then the lower surface of the flexible pressing plate 2 is placed opposite to the upper surface of the rigid substrate 1, and the flexible pressing plate 2 and the rigid substrate 1 are slowly approached to each other until the lower surface of the flexible pressing plate 2 contacts with the micro-step 3 on the upper surface of the rigid substrate 1, and the conductive nanowire mixed solution 4 is filled in a gap between the flexible pressing plate 2 and the micro-step 3. And after the mixed liquid is dried, the flexible pressing plate 2 is taken down, and the transparent conductive nanowire grid film formed by the conductive nanowires and attached to the surface of the three-dimensional microstructure on the upper surface of the rigid substrate can be obtained.
The grid film is formed by lapping conductive nanowires to form a conductive grid, and meshes between the nanowires can transmit light, so that the transparency of the grid film is realized.
Further, the upper surface of the rigid substrate 1 is pretreated before being coated with the conductive nano mixed solution, so that the capability of adsorbing the conductive nano wires is enhanced.
Further, in the process that the flexible pressing plate 2 is close to the rigid substrate 1 but not in contact with the rigid substrate, the redundant conductive nanowire mixed liquid is squeezed to overflow the gap between the flexible pressing plate and the rigid substrate until the flexible pressing plate and the rigid substrate are in contact with each other.
Furthermore, the flexible press plate 2 and the rigid substrate 1 are placed by adopting an optical alignment platform to operate, so that the three-dimensional microstructure on the lower surface of the flexible press plate 2 is aligned with the three-dimensional microstructure on the upper surface of the rigid substrate 1, and the three-dimensional microstructures can be mutually nested.
Claims (8)
1. A method for preparing a transparent conductive nanowire grid film on the surface of a three-dimensional microstructure is characterized by comprising the following steps: the method comprises the following steps:
manufacturing a three-dimensional microstructure on the upper surface of a rigid material matrix to obtain a rigid substrate (1);
transferring the three-dimensional microstructure shape of the upper surface of a rigid substrate (1) to the lower surface of a flexible material substrate by adopting an imprinting method to obtain a flexible pressing plate (2);
oxidizing the rigid substrate (1) to form an oxide layer on the surface of the rigid substrate;
corroding and removing an oxide layer on the upper surface of the rigid substrate (1); before the rigid substrate is corroded, covering a dry film at a plurality of positions on the upper surface of the rigid substrate for protection, reserving an oxide layer at the position covered by the dry film in the corrosion, and forming a micro step (3) on the upper surface of the rigid substrate (1);
coating a conductive nanowire mixed solution on a three-dimensional microstructure on the upper surface of a rigid substrate (1), then placing the lower surface of a flexible pressing plate (2) opposite to the upper surface of the rigid substrate (1), slowly moving the flexible pressing plate (2) to be close to the rigid substrate (1) until the lower surface of the flexible pressing plate (2) is contacted with a micro-step (3), forming a gap between the flexible pressing plate (2) and the rigid substrate (1) due to the existence of the micro-step (3), and reserving the conductive nanowire mixed solution in the gap; and (3) after the conductive nanowire mixed liquid is dried, taking down the flexible pressing plate (2) to obtain the transparent conductive nanowire grid film attached to the three-dimensional microstructure surface on the upper surface of the rigid substrate (1).
2. The method for preparing the transparent conductive nanowire mesh film on the surface of the three-dimensional microstructure according to claim 1, wherein the method comprises the following steps: the rigid substrate (1) is used for treating the surface of the three-dimensional microstructure of the upper surface of the rigid substrate before being coated with the conductive nanowire mixed solution so as to enhance the capacity of adsorbing the conductive nanowires.
3. The method for preparing the transparent conductive nanowire mesh film on the surface of the three-dimensional microstructure according to claim 1, wherein the method comprises the following steps: the flexible pressing plate (2) and the rigid substrate (1) are placed by adopting an optical alignment platform to operate, so that the three-dimensional microstructures on the lower surface of the flexible pressing plate (2) and the three-dimensional microstructures on the upper surface of the rigid substrate (1) are aligned and mutually nested.
4. The method for preparing the transparent conductive nanowire mesh film on the surface of the three-dimensional microstructure according to claim 1, wherein the method comprises the following steps: the rigid substrate (1) is made of a material which can be oxidized to generate an oxide layer and can be corroded to remove the oxide layer.
5. The method for preparing the transparent conductive nanowire mesh film on the surface of the three-dimensional microstructure according to claim 4, wherein the method comprises the following steps: the rigid substrate (1) is made of monocrystalline silicon or polycrystalline silicon.
6. The method for preparing the transparent conductive nanowire mesh film on the surface of the three-dimensional microstructure according to claim 1, wherein the method comprises the following steps: the flexible pressing plate (2) is made of a flexible material capable of being formed by stamping.
7. The method for preparing the transparent conductive nanowire mesh film on the surface of the three-dimensional microstructure according to claim 6, wherein the method comprises the following steps: the flexible material is PDMS or stamping glue.
8. The method for preparing the transparent conductive nanowire mesh film on the surface of the three-dimensional microstructure according to claim 1, wherein the method comprises the following steps: the cross section size of the micro-step (3) is determined by the size of the covering dry film, and the height of the micro-step is determined by the oxidation time and the corrosion time of the rigid substrate (1); the height of the micro-step (3) controls the size of a gap between the lower surface of the flexible pressing plate (2) and the upper surface of the rigid substrate (1), so that the thickness of the finally obtained conductive nanowire grid film is controlled, and the height of the micro-step (3) is selected according to specific requirements.
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| CN100517584C (en) * | 2003-12-19 | 2009-07-22 | 北卡罗来纳大学查珀尔希尔分校 | Methods for fabricating isolated micro- and nano- structures using soft or imprint lithography |
| CN101414119B (en) * | 2008-10-28 | 2011-06-22 | 吉林大学 | Method for building sub-micron or nano-scale formwork by micrometre scale formwork |
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| WO2017044421A1 (en) * | 2015-09-08 | 2017-03-16 | Canon Kabushiki Kaisha | Substrate pretreatment and etch uniformity in nanoimprint lithography |
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