CN112908520A - Etching method of silver nanowire, transparent conductive electrode and preparation method of transparent conductive electrode - Google Patents
Etching method of silver nanowire, transparent conductive electrode and preparation method of transparent conductive electrode Download PDFInfo
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Abstract
The invention provides a nano silver etching method, a transparent conductive electrode and a preparation method thereof. The etching method of the silver nanowires comprises the following steps: etching the silver nanowire into a plurality of line segments by laser etching, wherein the laser wavelength of the laser etching is 380 nm-1 mm, and the laser power is 0.1W/cm2～20W/cm2. The etching method enables the silver nanowires before and after the moment to have large electrical difference and small optical property difference, the visual difference on the appearance is very small, and the appearances of display screens prepared by the etching method are basically consistent.
Description
Technical Field
The invention relates to the field of preparation of transparent conductive electrodes, in particular to a nano silver etching method with shallow etching traces, a transparent conductive electrode and a preparation method thereof.
Background
In the fields of touch screens, optoelectronics, display screens, and the like, metal oxides, such as Indium Tin Oxide (ITO), are mainly used as transparent conductive films. However, the ITO conductive film needs to be prepared by vacuum physical deposition and high temperature annealing process, so that the conductive film using the polymer film as the substrate has the disadvantage of high sheet resistance. In addition, the ITO material is difficult to be applied to flexible devices because it is easily broken and damaged by bending and external force.
At present, a product capable of replacing an ITO film as a transparent conductive electrode material is a silver nanowire conductive film, the silver nanowire conductive film can be prepared in a coating mode, expensive vacuum equipment is not used in the preparation process, and therefore the product has advantages in cost compared with an ITO product. In addition, the silver nanowire serving as the nano material can be bent, and the application of the silver nanowire on a flexible device is also superior. Therefore, in the market prospect, the silver nanowire film has the potential of replacing an ITO film as a main transparent conductive film product.
However, in the practical application field, the silver nanowire conductive film needs to be patterned, and the current silver nanowire thin film has the defect of deep etching trace. The main reason for the deep etching mark is that silver, which is a metal material, scatters and reflects light. When the silver nanowire thin film is etched, the difference of light scattering and reflection between the etched area and the non-etched area can be different. This optical difference is probably due to the chemical reaction, such as oxidation and sulfidation, occurring on the surface of the silver nanowire after etching, and then the optical properties of the surface of the silver nanowire are changed. It is also possible that the silver nanowires are directly oxidized to silver ions, resulting in a decrease in the density of the silver nanowires or a thinning of the wires.
In view of the above, there is a need to provide an improved nano silver etching method, a transparent conductive electrode and a method for preparing the same, so as to solve the above problems.
Disclosure of Invention
The invention aims to provide a nano silver etching method with shallow etching traces, a transparent conductive electrode and a preparation method thereof.
In order to realize one of the above purposes, the invention adopts the following technical scheme;
the silver nanowire etching method adopts laser etching to etch the silver nanowire into a plurality of line segments, the laser wavelength of the laser etching is 380 nm-1 mm, and the laser power is 0.1W/cm2～20W/cm2。
A silver nanowire etching method adopts illumination etching to etch a silver nanowire into a plurality of line segments, the illumination wavelength of the illumination etching is between 380nm and 1mm, and the illumination time is between 1 minute and 30 minutes.
The silver nanowire etching method adopts high-temperature baking to etch the silver nanowire into a plurality of line segments, wherein the high-temperature baking temperature is 100-170 ℃, and the processing time is 10-60 minutes.
Further, the distance between two adjacent sections of silver nanowires is not more than 200 nm.
Further, the distance between two adjacent sections of silver nanowires is not more than 20 nm.
A preparation method of a transparent conductive electrode is characterized by comprising the following steps:
coating silver nanowires on a substrate to form a silver nanowire conductive film;
placing a mask plate with a through hole above the silver nanowire conductive film;
the silver nanowires covered by the mask plate form a first area;
and etching the silver nanowires exposed outwards through the through holes into a plurality of line segments to form a second area by adopting the etching method of the silver nanowires.
Further, the change of the number of silver nanowires before and after etching is not more than 10%;
or, the length change of the silver nanowires before and after being etched is not more than 5%;
or, the diameter change of the silver nanowires before and after being etched is not more than 5%;
or the electrical difference value of the silver nanowire conductive film in the second area before and after being etched is not less than 10^3 omega/□;
or the haze difference of the silver nanowire conductive film in the second area before and after being etched is delta H < + > -1%; or the transmittance difference of the silver nanowire conductive film in the second area before and after being etched is Delta T < + > 1%; or the chromaticity b of the silver nanowire conductive film in the second area before and after being etched is different from delta b < + > 1%.
Further, in the second region, the silver nanowires have a plurality of cutting positions, and the distances between different cutting positions are the same or different.
Further, the method also comprises the step of preparing a matrix for protecting the electrode layer on the side of the silver nanowire conductive film, which faces away from the substrate, wherein the matrix covers the silver nanowires or semi-covers the silver nanowires.
A transparent conductive electrode is prepared by the preparation method of the transparent conductive electrode.
The etching method of the silver nanowires enables the silver nanowires before and after the moment to have large electrical difference and small optical property difference, visual difference on appearance is very small, and the appearances of display screens prepared by the etching method are basically consistent.
Drawings
FIG. 1 is a schematic diagram of a conductive film with etched silver nanowires in accordance with a preferred embodiment of the present invention;
fig. 2 is an SEM image of a conductive film formed of silver nanowires before etching or a first region in an embodiment of the invention;
fig. 3 is an SEM image of a conductive film formed of silver nanowires after etching or a second region in an embodiment of the present invention;
FIG. 4 is a schematic diagram of a substrate coated with a conductive film according to a preferred embodiment of the present invention;
FIG. 5 is a schematic illustration of the first region and the second region of FIG. 4 in a preferred embodiment;
FIG. 6 is a schematic view of a preferred embodiment of the substrate added in FIG. 1;
FIG. 7 is a schematic view of another preferred embodiment of adding a matrix in FIG. 1.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in detail below with reference to specific embodiments.
In general, as shown in fig. 1 to 3, a silver nanowire conductive film 20 is formed by coating a silver nanowire 10 on a substrate, and then the silver nanowire conductive film 20 is etched.
According to the etching method of the silver nanowire 10, the silver nanowire 10 is cut into a plurality of line segments, as shown in fig. 1 or fig. 3, the cut silver nanowire 10 cannot form an effective conductive network, and the electrical difference before and after etching is large; and the cut silver nanowires 10 remain substantially intact, so that the difference in optical properties of the silver nanowire conductive film 20 before and after etching is small, and the silver nanowire conductive film can be used for preparing a transparent electrode with excellent quality.
In the present invention, the physical etching method includes, but is not limited to, the following:
and cutting off the silver nanowires 10 by adopting a laser etching method. In this embodiment, the laser wavelength of the laser etching is in the infrared and visible region, i.e. 380 nm-1 mm, and the laser power is 0.1W/cm2～20W/cm2。
Or cutting off the silver nanowires 10 by adopting a light etching method. In this embodiment, the illumination wavelength of the illumination etching is in the infrared and visible light regions, i.e. 380nm to 1mm, and the illumination time is 1 minute to 30 minutes.
Or cutting off the silver nanowires 10 by adopting a high-temperature baking method. In the embodiment, the high-temperature baking temperature is 100-170 ℃, and the processing time is 10-60 minutes.
In the above physical method, a point on the silver nanowire 10 having a higher activation state and a lower oxidation-reduction potential is preferably selected as the cut point. The silver nanowire 10 is wrapped by a protective layer to improve the chemical stability of silver during synthesis, and meanwhile, a certain area is exposed or silver dots with a lower oxidation potential remain, so that the silver nanowire has the function of activating a silver reaction no matter laser etching, illumination etching or high-temperature baking, and the silver dots with lower oxidation potential preferentially react at a certain critical point.
In addition, the distance between two adjacent segments of nanowires can be controlled to a certain extent by controlling etching conditions such as etching strength, temperature, time and the like. The larger the etching strength is, the higher the etching temperature is, and the longer the etching time is, the larger the distance between two adjacent segments of nanowires is.
It will be understood by those skilled in the art that "cutting" refers to randomly etching the entire nanowire into a plurality of segments, or randomly etching away part of the segments on the nanowire to divide the nanowire into a plurality of segments, as shown in fig. 1 or fig. 3, but the etched silver nanowire 10 is still regarded as one silver nanowire 10; that is, the density of the silver nanowires 10 in the statistical sense, the length of the silver nanowires 10 in the statistical sense, and the diameter of the silver nanowires 10 in the statistical sense are not changed after etching.
As shown in fig. 1 or fig. 3, one silver nanowire 10 may have a plurality of cutting positions, and the pitches of the different cutting positions are the same or different. The more the cut portions, the worse the conductivity of the silver nanowire conductive film 20 after cutting, and the larger the difference in conductivity of the silver nanowire conductive film 20 before and after cutting.
The distance between two adjacent sections of silver nanowires is not more than 20nm, or not more than 200nm, or not more than 1000nm, the etching trace of the silver nanowire 10 is shallow, the difference of the optical properties of the silver nanowire conductive film 20 before and after etching is small, and the silver nanowire conductive film can be used for preparing a transparent electrode with excellent quality. And the smaller the distance between two adjacent sections of silver nanowires is, the smaller the difference of optical properties is.
Before and after the silver nanowire 10 is cut, the density of the silver nanowire 10 statistically varies as follows: the number of silver nanowires 10 varies by no more than 5%, or by no more than 10%, in a unit area. The area of the unit area can be referred to as: about 10 x 10um2Or about 100 x 100um2Or about 1000 x 1000um2。
As will be appreciated by those skilled in the art: the density here means a ratio of a coverage area of the silver nanowires 10 per unit area; after the etching and cutting, since a portion of the silver nanowires 10 is etched away, the coverage area of the silver nanowires 10 may be reduced to some extent.
Before and after the silver nanowire 10 is cut, the length of the silver nanowire 10 statistically varies as follows: the length of the silver nanowire 10 varies by not more than 1%, or not more than 5%, in a unit area. The area of the unit area can be referred to as: about 10 x 10um2Or about 100 x 100um2Or about 1000 x 1000um2。
As will be appreciated by those skilled in the art: the length here means: the total length of all the silver nanowires 10 covered per unit area is changed before and after etching.
Before and after the silver nanowire 10 is cut, the diameter of the silver nanowire 10 statistically changes to: the diameter of the silver nanowire 10 varies by not more than 1%, or not more than 5%, in a unit area. The area of the unit area can be referred to as: about 10 x 10um2Or about 100 x 100um2Or about 1000 x 1000um2。
As will be appreciated by those skilled in the art: the total length is the area covered, which corresponds to the corresponding optical feature, and when the optical feature changes, it appears as an etching mark. The diameter here means: the silver nanowires 10 have a statistically average diameter per unit area before etching, and if etching does not appear as cutting, the diameter changes greatly, and etching traces are obvious.
The electrical difference of the conductive film is typically not less than 10^8 Ω/□, or not less than 10^6 Ω/□, or not less than 10^3 Ω/□ before and after the silver nanowires 10 constituting the conductive film are cut.
The difference in haze of the conductive film before and after the silver nanowires 10 of the conductive film were cut was: delta H < + -. 0.1%, or Delta H < + -. 0.5%, or Delta H < + -. 1%; the difference in transmittance of the conductive film is: delta T < + -. 0.1%, or delta T < + -. 0.5%, or delta T < + -. 1%; the chromaticity b x difference of the conductive film is: Δ b < ± 0.1%, or Δ b < ± 0.5%, or Δ b < ± 1%.
Based on the above etching methods of the silver nanowires 10, the preparation method of the transparent conductive electrode of the present invention comprises the following steps: as shown in fig. 4, a silver nanowire 10 is coated on a substrate 30 to constitute a silver nanowire conductive film 20; placing a mask plate with through holes above the silver nanowire conductive film 20; as shown in fig. 5, the silver nanowire conductive film 20 covered by the mask plate constitutes a first region 41; the silver nanowires 10 exposed to the outside through the through holes are etched into a plurality of line segments, and the distance between two adjacent segments of silver nanowires 10 is not greater than 1000nm, thereby forming a second region 42.
In the present invention, the substrate 30 is made of glass, polyester such as polyethylene terephthalate (PET), polyethylene naphthalate, and polycarbonate, polyimide, synthetic rubber such as EPR, SBR, and EPDM, or a silicon-containing compound such as polydimethylsiloxane.
The mask can be various masks used in the prior art, for example: a mask made of a metal material or a mask formed of a photoresist, etc., which will not be described herein.
The method of etching the silver nanowires 10 exposed to the outside through the through holes into a plurality of line segments adopts any one of the above-mentioned etching methods of nano silver, the silver nanowires 10 in the formed second region 42 are cut off, an effective conductive network cannot be formed, and the electrical difference between the first region 41 and the second region 42 is large; and the distance between two adjacent sections of silver nanowires is not more than 1000nm, the etching mark of the silver nanowire 10 is shallow, the difference between the optical properties of the first region 41 and the second region 42 is small, the visual difference in appearance is very small, and the appearances of the display screens prepared from the silver nanowires are basically consistent.
The present invention also provides a transparent conductive electrode 100 comprising: the silver nanowire array comprises a substrate 30 and an electrode layer 40 positioned on the substrate 30, wherein the electrode layer 40 comprises a first region 41 and a second region 42 which are designed in a patterning mode, the first region 41 is provided with a plurality of interconnected silver nanowires 10, and a conductive network can be formed; the second region 42 has silver nanowires 10 that are cut off and do not constitute an effective conductive network.
The boundary between the first region 41 and the second region 42 is not limited to a straight line, and may be a polygonal line or a curved line.
In the second region 42, the cut silver nanowire 10 is formed by etching the same silver nanowire 10 as the first region 41, "cutting" means that the entire nanowire is randomly etched into a plurality of line segments, or a part of the line segments on the nanowire are randomly etched to be cut into a plurality of line segments, but the etched silver nanowire 10 is still regarded as one silver nanowire 10; that is, the density of the silver nanowires 10 in the second region 42 in the statistical sense, the length of the silver nanowires 10 in the statistical sense, and the diameter of the silver nanowires 10 in the statistical sense are not changed after etching.
Specifically, the distance between two adjacent silver nanowires in the cut silver nanowire 10 is not greater than 20nm, or not greater than 200nm, or not greater than 1000 nm. And one silver nanowire 10 may have a plurality of cutting positions, and the pitches of the different cutting positions are the same or different.
Therefore, the silver nanowires 10 in the second region 42 are cut off, an effective conductive network cannot be formed, and the electrical difference between the first region 41 and the second region 42 is large; and the distance between two adjacent sections of silver nanowires is not more than 1000nm, the etching mark of the silver nanowire 10 is shallow, the difference between the optical properties of the first region 41 and the second region 42 is small, the visual difference in appearance is very small, and the appearances of the display screens prepared from the silver nanowires are basically consistent.
Before and after the silver nanowires 10 of the second region 42 are cut, the density of the silver nanowires 10 statistically varies as: the number of silver nanowires 10 varies by no more than 5%, or by no more than 10%, in a unit area. The area of the unit area can be referred to as: about 10 x 10um2Or about 100 x 100um2Or about 1000 x 1000um2. Namely: the number of silver nanowires 10 per unit area of the first region 41 and the number of silver nanowires 10 per unit area of the second region 42 are varied by not more than 5%, or not more than 10%.
Before and after the silver nanowire 10 of the second region 42 is cut, the length of the silver nanowire 10 statistically varies as follows: the length of the silver nanowire 10 varies by not more than 1%, or not more than 5%, in a unit area. The area of the unit area can be referred to as: about 10 x 10um2Or about 100 x 100um2Or about 1000 x 1000um2. It can also be understood that: the length and length of the silver nanowire 10 per unit area of the first region 41The variation in length of the silver nanowires 10 per unit area of the second region 42 is no more than 1%, or no more than 5%.
Before and after the silver nanowires 10 of the second region 42 are cut, the diameter of the silver nanowires 10 statistically changes to: the diameter of the silver nanowire 10 varies by not more than 1%, or not more than 5%, in a unit area. The area of the unit area can be referred to as: about 10 x 10um2Or about 100 x 100um2Or about 1000 x 1000um2. It can also be understood that: the diameter of the silver nanowire 10 per unit area of the first region 41 and the diameter of the silver nanowire 10 per unit area of the second region 42 are not changed by more than 1%, or not more than 5%.
The electrical contrast of the first region 41 with the second region 42 is typically no less than 10 < Lambda > 8 </Lambda >/□, or no less than 10 < Lambda > 6 </Lambda >/□, or no less than 10 < Lambda > 3 </Lambda >/□.
The difference in haze between the first region 41 and the second region 42 is: delta H < + -0.1%, or Delta H < + -0.5%, or Delta H < + -1%. The difference in transmittance between the first region 41 and the second region 42 is: delta T < + -0.1%, or Delta T < + -0.5%, or Delta T < + -1%. The difference b between the chromaticities of the first region 41 and the second region 42 is: Δ b < ± 0.1%, or Δ b < ± 0.5%, or Δ b < ± 1%.
Further, the transparent conductive electrode 100 further includes a matrix 50 for protecting or holding the silver nanowires 10 of the electrode layer 40, as shown in fig. 6, the matrix 50 completely covers the silver nanowires 10; or as shown in fig. 7, the matrix covers the silver nanowires 10, i.e. a part of the silver nanowires 10 is exposed outside the matrixes 50.
The matrix is primarily an optically clear polymer, as is well known in the art. Examples of suitable polymer matrices include, but are not limited to: polymethacrylates (e.g., polymethylmethacrylate), polyacrylates and polyacrylates of polyacrylonitrile, polyvinyl alcohols, polyesters (e.g., polyethylene terephthalate (PET), polynaphthalene, and polycarbonates), polymers with high aromaticity such as phenolics or cresol-formaldehyde, polystyrene, polyvinyltoluene, polyvinylxylene, polyimides, polyamides, polyamide-imides, polyetherimides, polysulfides, polysulfones, polyphenylenes, polyphenylene ethers, Polyurethanes (PU), epoxies, polyolefins (e.g., polypropylene, polymethylpentene, and cycloolefins), acrylonitrile-butadiene-styrene copolymers (ABS), cellulose, silicones, and other silicon-containing polymers (e.g., polysilsesquioxanes and polysilanes), polyvinyl chloride (PVC), polyacetates, polyacrylonitriles, and polysilsesquioxanes), polyvinyl alcohol, polyesters (e.g., polyethylene terephthalate (PET), polynaphthalene, and polycarbonates), polymers with high aromaticity such as phenolics or, Polynorbornene, synthetic rubbers (e.g., EPR, SBR, EPDM), fluoropolymers (e.g., polyvinylidene fluoride, polytetrafluoroethylene (TFE), or polyhexafluoropropylene).
In summary, in the etching method of the silver nanowire 10 of the present invention, the silver nanowire 10 is cut off, so that an effective conductive network cannot be formed, and the electrical difference before and after etching is large; and the distance between two adjacent sections of silver nanowires is not more than 1000nm, the etching trace of the silver nanowire 10 is shallow, the optical property difference before and after etching is small, and the silver nanowire can be used for preparing a transparent electrode with excellent quality.
In the transparent conductive electrode 100 of the present invention, the silver nanowires 10 in the second region 42 are cut off, and an effective conductive network cannot be formed, and the electrical difference between the first region 41 and the second region 42 is large; and the distance between two adjacent sections of silver nanowires is not more than 1000nm, the etching mark of the silver nanowire 10 is shallow, the difference between the optical properties of the first region 41 and the second region 42 is small, the visual difference in appearance is very small, and the appearances of the display screens prepared from the silver nanowires are basically consistent.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the spirit and scope of the present invention.
Claims (10)
1. A method for etching silver nanowires, characterized by: etching the silver nanowire into a plurality of line segments by laser etching, wherein the laser wavelength of the laser etching is 380 nm-1 mm, and the laser power is 0.1W/cm2～20W/cm2。
2. A method for etching silver nanowires, characterized by: and etching the silver nanowires into a plurality of line segments by adopting illumination etching, wherein the illumination wavelength of the illumination etching is between 380nm and 1mm, and the illumination time is between 1 minute and 30 minutes.
3. A method for etching silver nanowires, characterized by: and etching the silver nanowires into a plurality of line segments by adopting high-temperature baking, wherein the high-temperature baking temperature is 100-170 ℃, and the processing time is 10-60 minutes.
4. The method for etching silver nanowires according to any one of claims 1 to 3, characterized in that: the distance between two adjacent sections of silver nanowires is not more than 200 nm.
5. The method for etching silver nanowires of claim 4, wherein: the distance between two adjacent sections of silver nanowires is not more than 20 nm.
6. A preparation method of a transparent conductive electrode is characterized by comprising the following steps:
coating silver nanowires on a substrate to form a silver nanowire conductive film;
placing a mask plate with a through hole above the silver nanowire conductive film;
the silver nanowires covered by the mask plate form a first area;
the method for etching silver nanowires according to any one of claims 1 to 5, wherein the silver nanowires exposed through the through holes are etched into a plurality of line segments to form the second region.
7. The method for preparing a transparent conductive electrode according to claim 6,
the quantity change of the silver nanowires before and after being etched is not more than 10 percent;
or, the length change of the silver nanowires before and after being etched is not more than 5%;
or, the diameter change of the silver nanowires before and after being etched is not more than 5%;
or the electrical difference value of the silver nanowire conductive film in the second area before and after being etched is not less than 10^3 omega/□;
or the haze difference of the silver nanowire conductive film in the second area before and after being etched is delta H < + > -1%; or the transmittance difference of the silver nanowire conductive film in the second area before and after being etched is Delta T < + > 1%; or the chromaticity b of the silver nanowire conductive film in the second area before and after being etched is different from delta b < + > 1%.
8. The method for preparing a transparent conductive electrode according to claim 6, wherein the silver nanowires in the second region have a plurality of cut-off portions, and the pitches of the different cut-off portions are the same or different.
9. The method for producing a transparent conductive electrode according to claim 6, further comprising producing a matrix for protecting the electrode layer on a side of the silver nanowire conductive film facing away from the substrate, the matrix covering or half-covering the silver nanowires.
10. A transparent conductive electrode, characterized by: the transparent conductive electrode prepared by the method of any one of claims 6 to 9.
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Also Published As
| Publication number | Publication date |
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| CN109686496A (en) | 2019-04-26 |
| CN112908518A (en) | 2021-06-04 |
| CN109686496B (en) | 2021-02-09 |
| CN112908520B (en) | 2023-01-24 |
| CN112908518B (en) | 2022-11-08 |
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