CN113241408A - Sea urchin-shaped gold nanoparticle-doped flexible photoelectric substrate and preparation method thereof - Google Patents
Sea urchin-shaped gold nanoparticle-doped flexible photoelectric substrate and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
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- H10K77/10—Substrates, e.g. flexible substrates
- H10K77/111—Flexible substrates
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Abstract
The invention discloses a preparation method of a flexible photoelectric substrate doped with echinoid gold nanoparticles, and belongs to the field of preparation of photoelectric devices. The doped flexible substrate provided by the invention adopts an ultraviolet curing material as the substrate, sea urchin-shaped gold nanoparticles with different surface appearances and sizes are used as dopants, and the substrate is covered with a flexible transparent electrode. The echinoid gold nanoparticles are prepared by a solution method by using chloroauric acid as a soluble gold source and utilizing different reducing agents and reaction conditions. Compared with the prior art, the transparent silver nanowire electrode is prepared by adopting a Meyer bar rolling coating method, echinoid gold nanoparticles are dispersed in a substrate precursor solution, the substrate precursor solution is cured by using an ultraviolet curing technology, and the silver nanowires are transferred to the substrate, so that the transparent silver nanowire electrode is used for preparing a photoelectric device, and the optical field enhancement effect and the enhanced spectrum of the flexible substrate can be adjusted by changing the surface appearance and the size of the echinoid gold nanoparticles in the substrate precursor solution.
Description
Technical Field
The invention belongs to the field of photoelectric device preparation, and relates to a preparation method of a flexible photoelectric substrate doped with echinoid gold nanoparticles.
Background
In the electromagnetic response device, the interaction degree of electromagnetic waves and substances fundamentally determines the overall efficiency of the photoelectric conversion device and the signal intensity and detection precision of the detection device. How to construct a micro-nano structure for improving the interaction effect of light and substances by using a physical method is very important, so that the efficiency of a photoelectric conversion device and the performance of a detection device are effectively improved. The echinoid gold nanoparticles are considered to be a new generation of high-performance material suitable for improving the efficiency of a photoelectric conversion device and the response of a detector due to the unique regular 'hot spot' structure. At present, although noble metal nanoparticles have been widely used in various fields, most noble metal nanoparticles have a simple polyhedral or spherical structure, and the application of noble metal nanoparticles having a complex structure such as a sea urchin-like structure is rarely reported. In order to deeply reveal the behavior of light on the surface of a complex noble metal and improve the performance of a photoelectric conversion device and a detection device, the application of echinoid gold nanoparticles with various sizes and shapes in different scenes is very significant, and the echinoid gold nanoparticles play a positive role in the development of electromagnetic response devices.
Disclosure of Invention
The invention aims to: how to provide a preparation method of a flexible substrate with low cost and controllable doping content of echinoid gold nanoparticles, and a preparation method of an organic light-emitting diode device using the substrate, which improves photoelectric conversion efficiency of the device.
The technical scheme adopted by the invention is as follows:
a flexible photoelectric substrate doped with sea urchin-shaped gold nanoparticles adopts a photoinitiator and acrylate as substrate materials, sea urchin-shaped gold nanoparticles prepared by a solution method are used as doped particles, and a flexible transparent electrode is covered on the substrate, wherein the flexible transparent electrode is arranged on the substrate;
the echinoid gold nanoparticles are prepared by chloroauric acid and a reducing agent under different reaction conditions, and the size range of the echinoid gold nanoparticles is 50-600 nm.
Further, the precursor solution of the substrate is prepared from SR499, SR540 and a photoinitiator, and the thickness range is 150-250 um.
Further, SR499, SR540, photoinitiator in the solution, as per 66: 33: 1 mass ratio.
Further, the flexible transparent electrode is a silver nanowire electrode and PEDOT PSS, the thickness of the silver nanowire is 1um, and the thickness of the PEDOT PSS is 50 nm.
The preparation process comprises the following steps;
s1: cleaning and drying a base material with a smooth surface;
s2: rolling and coating the silver nanowire suspension on the smooth surface of the substrate and performing subsequent treatment to prepare the transparent silver nanowire electrode,
s3: dispersing echinoid gold nanoparticles in a precursor solution of a substrate;
s4: covering a precursor solution doped with echinoid gold nanoparticles on the silver nanowire electrode, and curing by using ultraviolet light;
s5: and stripping the cured substrate from the surface of the glass slide, and spin-coating a layer of PEDOT (PSS) with the thickness of 50nm on the surface of the silver nanowire electrode to obtain a finished product of the flexible substrate.
Further, the silver nanowire suspension is roll-coated in S2 by using a meyer rod roll coating method.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. the optical field enhancement effect is realized in the substrate, and for a common photoelectric conversion device, the doped substrate can combine near-field enhancement and far-field scattering, so that the substrate has general potential in application in different types of photoelectric devices, and the structure and performance of the device are not damaged;
2. the size, the shape and the proportion of the echinoid gold nanoparticles in the precursor solution realize the light field enhancement effect and the enhanced spectral response, optimize the spectral response matching degree of the flexible substrate and the photoelectric device, and improve the photoelectric and electro-optical conversion efficiency of the device;
3. the invention adopts a Meyer bar rolling coating method to prepare a transparent silver nanowire electrode, sea urchin-shaped gold nanoparticles are dispersed in a substrate precursor solution, the substrate precursor solution is cured by using an ultraviolet curing technology, and silver nanowires are transferred to a substrate, so that a flexible substrate which is used for preparing a photoelectric device and has a high light field enhancement effect is obtained. The surface appearance and the size of the sea urchin-shaped gold nanoparticles in the substrate precursor solution are changed, the light field enhancement effect and the enhanced spectrum of the flexible substrate can be adjusted, so that the prepared photoelectric device can obtain a better spectrum matching effect, the photoelectric conversion efficiency of the device is improved, the preparation process of the flexible substrate is simple, the composition elements are non-toxic and harmless, the environment is friendly, large-area production is easy to realize, the application potential is large, the ultraviolet curing technology is adopted, the process is simple, the parameters are flexible, large-area and low-cost mold making can be realized, and large-scale application is facilitated.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and that for those skilled in the art, other relevant drawings can be obtained according to the drawings without inventive effort, wherein:
FIG. 1 is a schematic structural view of the present invention;
fig. 2 is a graph comparing luminance of organic light emitting devices prepared in inventive example 11 and inventive example 12;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without making any creative effort, shall fall within the protection scope of the present invention.
It is noted that relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The invention provides a flexible photoelectric substrate doped with echinoid gold nanoparticles, wherein the echinoid gold nanoparticles are prepared by chloroauric acid and a reducing agent under different reaction conditions, and the size range of the echinoid gold nanoparticles is 50-600 nm. Preferably, the flexible substrate precursor solution is prepared from SR499, SR540 and photoinitiator of Saddomar company, USA, the thickness range is 150-250 um, and the SR499, SR540 and photoinitiator in the solution are as follows 66: 33: 1 mass ratio.
The invention also provides a preparation method of the flexible photoelectric substrate doped with the echinoid gold nanoparticles, which comprises the following steps: rolling and coating the silver nanowire suspension on the smooth surface of the base material, performing subsequent treatment to prepare a transparent silver nanowire electrode, dispersing echinoid gold nanoparticles in a base material precursor solution, covering the silver nanowire electrode with the doped base material precursor solution, curing, and taking off the surface of the base material to obtain a finished product of the flexible base material. In the present invention, the sources of all raw materials are not particularly limited, and they may be commercially available. The invention preferably uses a cleaned and dried common glass slide as a substrate to roll-coat the silver nanowire transparent electrode. The cleaning method comprises the steps of sequentially selecting a detergent, deionized water and acetone for cleaning, and drying by adopting a drying oven. According to the invention, the flexible film precursor solution is preferably doped by ultraviolet curing, and the curing power is preferably 60-120W, most preferably 120W. The curing time is preferably 2 to 4 minutes, most preferably 3 minutes. The invention adopts the ultraviolet light curing method to prepare the flexible substrate doped with the controllable sea urchin-shaped gold nanoparticles, improves the photoelectric conversion efficiency of the device, has simple preparation process, is easy to realize large-area production, and has great application potential.
In order to further illustrate the present invention, the following describes in detail a flexible substrate doped based on the content of echinoid gold nanoparticles and a preparation method thereof, which are provided by the present invention, with reference to examples. The reagents used in the following examples are all commercially available; the substrate used in the examples had a thickness of 1mm and a length and width of 76mm and 25mm, respectively.
Example 1 (as blank control group)
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with the echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the echinoid gold nanoparticle doped flexible substrate comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a blank flexible substrate.
Example 2
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 170nm are doped into a precursor solution of the flexible substrate according to the mass ratio of 0.1%; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 3
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 170nm are doped into a precursor solution of the flexible substrate according to the mass ratio of 0.5 percent; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 4
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 170nm are doped into a precursor solution of a flexible substrate according to the mass ratio of 1%; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 5
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 70nm are doped into a precursor solution of the flexible substrate according to the mass ratio of 0.1%; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 6
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 70nm are doped into a precursor solution of the flexible substrate according to the mass ratio of 0.5 percent; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 7
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 70nm are doped into a precursor solution of a flexible substrate according to the mass ratio of 1%; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 7
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 70nm are doped into a precursor solution of a flexible substrate according to the mass ratio of 1%; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 8
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 600nm are doped into a precursor solution of the flexible substrate according to the mass ratio of 0.1%; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 9
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 600nm are doped into a precursor solution of the flexible substrate according to the mass ratio of 0.5 percent; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 10
Cleaning a substrate consisting of ordinary glass with a smooth surface, and drying the substrate after cleaning; preparing a flexible substrate doped with echinoid gold nanoparticles on a transparent and clean substrate, wherein the preparation method of the flexible substrate doped with the echinoid gold nanoparticles comprises the following steps: 1) rolling and coating a commercially available silver nanowire suspension on a substrate, and preparing a transparent silver nanowire electrode after air drying and annealing treatment; 2) sea urchin-shaped gold nanoparticles with the diameter of 600nm are doped into a precursor solution of a flexible substrate according to the mass ratio of 1%; 3) covering the precursor solution of the flexible substrate on the silver nanowire electrode, solidifying by using ultraviolet light, stripping, and spin-coating a layer of PEDOT (PSS) on the surface of the silver nanowire electrode to obtain a sea urchin-shaped gold nanoparticle-doped flexible substrate finished product.
Example 11
An organic light emitting diode device having a structure of AgNWs/PEDOT, PSS/HAT-CN/TAPC/MCP/PO-T2T/LiF/Al was fabricated using the undoped flexible substrate fabricated in example 1. The maximum brightness of the obtained device is 809cd/m2。
Example 12
An organic light emitting diode device having a structure of AgNWs/PEDOT, PSS/HAT-CN/TAPC/MCP/PO-T2T/LiF/Al was fabricated using the undoped flexible substrate fabricated in example 4. The maximum brightness of the obtained device is 1080cd/m2The improvement is about 35% compared with example 11.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and should not be taken as limiting the scope of the present invention, and any modifications, equivalents and improvements made by those skilled in the art within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A sea urchin-shaped gold nanoparticle-doped flexible photoelectric substrate is characterized in that: the substrate adopts a photoinitiator and acrylic ester as substrate materials, sea urchin-shaped gold nanoparticles prepared by a solution method are used as doping particles, and a flexible transparent electrode is covered on the substrate, wherein the flexible transparent electrode is arranged on the substrate;
the echinoid gold nanoparticles are prepared by chloroauric acid and a reducing agent under different reaction conditions, and the size range of the echinoid gold nanoparticles is 50-600 nm.
2. The flexible photoelectric substrate doped with sea urchin-shaped gold nanoparticles as claimed in claim 1, wherein: the precursor solution of the substrate is prepared from SR499, SR540 and a photoinitiator, and the thickness range is 150-250 um.
3. The flexible photoelectric substrate doped with sea urchin-shaped gold nanoparticles as claimed in claim 2, wherein: SR499, SR540, photoinitiator in the solution, as per 66: 33: 1 mass ratio.
4. The flexible photoelectric substrate doped with sea urchin-shaped gold nanoparticles as claimed in claim 1, wherein: the flexible transparent electrode is a silver nanowire electrode and PEDOT PSS, the thickness of the silver nanowire is 1um, and the thickness of the PEDOT PSS is 50 nm.
5. A preparation method of a flexible photoelectric substrate doped with sea urchin-shaped gold nanoparticles is characterized by comprising the following steps: the preparation process comprises the following steps;
s1: cleaning and drying a base material with a smooth surface;
s2: rolling and coating the silver nanowire suspension on the smooth surface of the substrate and performing subsequent treatment to prepare the transparent silver nanowire electrode,
s3: dispersing echinoid gold nanoparticles in a precursor solution of a substrate;
s4: covering a precursor solution doped with echinoid gold nanoparticles on the silver nanowire electrode, and curing by using ultraviolet light;
s5: and stripping the cured substrate from the surface of the glass slide, and spin-coating a layer of PEDOT (PSS) with the thickness of 50nm on the surface of the silver nanowire electrode to obtain a finished product of the flexible substrate.
6. The preparation method of the echinoid gold nanoparticle-doped flexible photoelectric substrate according to claim 5, wherein the preparation method comprises the following steps: and rolling and coating the silver nanowire suspension in the S2 by adopting a Meyer rod rolling coating method.
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