CN116096197A - Quantum dot light emitting structure, photoinduced patterning method and application thereof - Google Patents
Quantum dot light emitting structure, photoinduced patterning method and application thereof Download PDFInfo
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Abstract
The invention discloses a quantum dot light-emitting structure, a photoinduced patterning method and application thereof. The photo-patterning method comprises the following steps: providing a coating liquid, wherein the coating liquid comprises quantum dots and a photosensitive additive, and the surface of the quantum dots is provided with a ligand; forming a precursor film by forming a film of the coating liquid; and carrying out patterned illumination on the precursor film in a protective atmosphere, and removing part of the precursor film through a development step to obtain the patterned quantum dot light-emitting structure. The photoinduced patterning method provided by the invention can realize direct photoetching formation of the quantum dot material, is convenient for obtaining the pixel array of the high-resolution quantum dot light-emitting structure, and can reduce the influence on the performance of the quantum dot to obtain a better photoetching effect due to the adoption of ultraviolet irradiation under protective atmosphere, so that the optical performance of the quantum dot is better reserved, and further the quantum dot light-emitting device with higher precision and better light-emitting performance is obtained.
Description
Technical Field
The invention relates to the technical field of semiconductor processing, in particular to the field of semiconductor illumination display, and particularly relates to a quantum dot light-emitting structure, a photoinduced patterning method and application thereof.
Background
The prior art light emission technologies can be broadly divided into two categories, one being passive display, such as liquid crystal, photoluminescent devices; the other is active display, such as Organic Light Emitting Diode (OLED), quantum dot light emitting diode (QLED). The QLED technology has wide color gamut, high color purity and continuously adjustable luminescence peak position, so that the QLED technology is widely focused by scientific research and enterprises.
Quantum Dot (QD) is a semiconductor nanomaterial with three-dimensional Quantum confinement effect. When it is excited by energy (optical or electrical), it will emit light of a specific wavelength depending on its own characteristics. As a light emitting layer in a quantum dot light emitting diode (QLED) display technology, the current quantum dot pixelation technology is mainly based on nanoimprint, inkjet printing, transfer printing, or electrophoretic deposition. However, the above solution has technical problems such as material residue, coffee ring effect, boundary damage or complex process, and is difficult to meet the commercialization requirements of high-resolution QLED devices. In contrast, as shown in fig. 1, photolithography is better able to achieve the desired pixel size, but requires the use of photoresist to complete the designed pattern.
The traditional photoetching process has complicated steps, and particularly when pixel points with various colors are required to be prepared, photoresist is required to be coated for multiple times, so that the performance of the device is adversely affected.
The prior art also provides some direct photolithography methods, such as a quantum dot direct photolithography scheme based on photoacid generator, in which the replacement or modification of the ligand on the surface of the quantum dot is generated, which results in a great decrease in various properties of the light emitting layer, and especially the lifetime of the prepared device is far from expectancy.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a quantum dot light emitting structure, a photoinduced patterning method and application thereof.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention comprises the following steps:
in a first aspect, the present invention provides a method for photopatterning a quantum dot light emitting structure, comprising:
providing a coating liquid, wherein the coating liquid comprises quantum dots and a photosensitive additive, and the surface of the quantum dots is provided with a ligand;
coating the coating liquid into a film to form a precursor film;
and carrying out patterning illumination on the precursor film in a protective atmosphere, and then cleaning and removing part of the precursor film by a solvent to obtain the patterned quantum dot light-emitting structure.
In a second aspect, the invention further provides a quantum dot light-emitting structure prepared by the photoinduced patterning method.
In a third aspect, the present invention also provides an application of the above-mentioned photopatterning method in the preparation of a quantum dot light-emitting device.
Based on the technical scheme, compared with the prior art, the invention has the beneficial effects that:
the photoinduced patterning method provided by the invention can realize direct photoetching formation of the quantum dot material, is convenient for obtaining the pixel array of the high-resolution quantum dot light-emitting structure, and can reduce the influence on the performance of the quantum dot to obtain a better photoetching effect due to the adoption of ultraviolet irradiation under protective atmosphere, so that the optical performance of the quantum dot is better reserved, and further the quantum dot light-emitting device with higher precision and better light-emitting performance is obtained.
The above description is only an overview of the technical solutions of the present invention, and in order to enable those skilled in the art to more clearly understand the technical means of the present application, the present invention may be implemented according to the content of the specification, the following description is given of the preferred embodiments of the present invention with reference to the accompanying drawings.
Drawings
FIG. 1 is a flow chart of a prior art photoresist patterning method provided in the background of the invention;
FIG. 2 is a flow chart of a photo-patterning method according to an exemplary embodiment of the invention;
FIG. 3 is a photograph showing a patterning accuracy test of a photo-patterning method according to an exemplary embodiment of the present invention;
FIG. 4 is a photomicrograph of a quantum dot light emitting structure/device made by a photo-patterning process according to an exemplary embodiment of the present invention;
fig. 5 is a photomicrograph of another quantum dot light emitting structure/device made by the photopatterning method according to an exemplary embodiment of the present invention.
Detailed Description
In view of the shortcomings in the prior art, the inventor of the present invention has long studied and practiced in a large number of ways to propose the technical scheme of the present invention.
The invention aims to design a novel quantum dot direct photoetching technology to obtain a quantum dot luminescent layer with ultra-high resolution, and simultaneously solve the problem of reduced fluorescence quantum yield of quantum dots caused by the addition of a photosensitive additive and ultraviolet exposure treatment. The technical scheme, the implementation process, the principle and the like are further explained as follows.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced otherwise than as described herein, and therefore the scope of the present invention is not limited to the specific embodiments disclosed below.
The embodiment of the invention provides a photoinduced patterning method of a quantum dot luminous structure, which comprises the following steps of:
providing a coating liquid, wherein the coating liquid comprises quantum dots and a photosensitive additive, and the surface of the quantum dots is provided with a ligand;
coating the coating liquid into a film to form a precursor film;
and carrying out patterning illumination on the precursor film in a protective atmosphere, and then cleaning and removing part of the precursor film by a solvent to obtain the patterned quantum dot light-emitting structure.
Specifically, in the technical scheme, the photoinduced patterning method disclosed by the invention, namely a quantum dot direct photoetching technology, can be uniformly mixed with the prepared original quantum dot solution by adopting a small amount (less than or equal to 5 weight percent) of photosensitive additive. Wherein the ligand of the original quantum dot can be mercaptan, alkyl phosphonic acid, alkyl sulfonic acid, alkyl carboxylic acid, oleylamine, etc., and the solvent is selected from non-polar solvents such as toluene, n-hexane, n-octane, etc.
More specifically, a material containing carbon-carbon unsaturated bonds, an isocyanate material or a thiol-ene or bis-azide material can be used as a photosensitive additive, and is connected or self-crosslinked with quantum dot ligands under specific exposure treatment to form a grid structure, so that the exposed part is cured to obtain the cured and formed pattern of the required pattern.
After exposure is completed, the sample is developed with a raw solvent, or other solvents of similar properties, and then the desired patterned quantum dot light emitting structure can be obtained.
The principle of the quantum dot light-emitting structure can be electrochemiluminescence or fluorescence light-emitting.
In addition, the inventor of the present invention found that the direct photolithography in the prior art often has adverse effects on the luminescence performance of the quantum dots under ultraviolet light and during the reaction process of the photosensitive additive, and the problem of reduced fluorescence efficiency of the quantum dots generated during the implementation process can be solved by adjusting and improving the environmental atmosphere in the photolithography process to protect, for example, by adopting inert gases such as nitrogen, argon and the like.
Specifically, the atmosphere protection can effectively avoid ultraviolet bleaching effect, namely, in an inert atmosphere, the oxidation-reduction reaction between oxygen and the quantum dots and between the oxygen and the surface ligands under the ultraviolet condition is eliminated, and meanwhile, the shedding probability of the surface ligands is greatly reduced, so that the quantum dots maintain better fluorescence efficiency and service life.
In some embodiments, the ligand includes any one or a combination of two or more of thiol, alkylphosphonic acid, alkylsulfonic acid, alkylcarboxylic acid (e.g., oleic acid), and oleylamine, etc., but is not limited thereto.
In some embodiments, the photoactive additive includes any one or a combination of two or more of a material containing carbon-carbon unsaturation, an isocyanate-based material, a bis-azide-based material, and the like.
In some embodiments, the material containing carbon-carbon unsaturation includes oleic acid and olefinic materials complexed with oleic acid. Specifically, for example, oleyl mercaptan is mixed with oleic acid, linoleic acid and alpha-linolenic acid.
In some embodiments, the solvent in the coating liquid and/or the solvent used to clean a portion of the precursor film is selected from a nonpolar solvent, and more preferably any one or a combination of two or more of toluene, n-hexane, and n-octane.
In some embodiments, the material containing carbon-carbon unsaturation comprises any one or a combination of two or more of divinylbenzene, ethyl cinnamate, triallyl isocyanurate, diphenylmethane diisocyanate.
In some embodiments, the bis-azido based materials include 1, 11-diazide-3, 6, 9-oxaundecane, 1, 8-diazide-3, 6-dioxaoctaoctane, 1-azido-2- (2-azidoethoxy) ethane, 4' -azidobiphenyl, 2, 6-bis- (4-azidobenzene) cyclohexanone, and the like. Specifically, the bis-azide material provided by the technical scheme is short-chain molecules with smaller steric hindrance, is easy to obtain, and is convenient for preparing high-performance QLED devices.
In some embodiments, the wavelength of the patterned illumination is 260nm or less, preferably 172-254nm, when the photoactive additive is selected from the group consisting of bis-azide-based materials. As some typical application examples of the above technical solution, when the biazide material in the above embodiment is preferred, the uv exposure wavelength may be selected to be 254nm, and a wavelength of 172nm may also be used, which helps to achieve efficient crosslinking, but the biazide material provided in the prior art cannot match the wavelength range.
In particular, shorter wavelengths provide less diffraction effects and are useful for improving boundary sharpness in small-size pixels. In addition, the photosensitive wave bands of different photosensitive groups are different, and the azide group is generally in the deep ultraviolet region, which is more beneficial to improving the photoetching precision.
In some embodiments, theThe photosensitive additive further comprises a photosensitive additive comprising two or more N-BF components 2 Materials of the groups.
In some embodiments, the compositions contain more than two N-BF 2 Materials of groups, e.g. 5, 11, 11, 17, 17-hexafluorophosphoric acid-6, 12, 18-trihexylamine-5, 6, 11, 12, 17, 18-hexahydropyridine-4 b λ4 ，6，10b λ4 ，12，16b λ4 18-Hexagon-5 λ4 ，11 λ4 ，17 λ4 -a triboro-tribenzo-trinaphthylene; and the wavelength of the patterned lithography is 365nm or more, preferably 405nm.
The molecular formula of the material is shown as follows:
the photosensitive additive can realize photo-induced crosslinking under longer ultraviolet wavelength (such as 405 nm), and expands the process selection range of the quantum dot direct photoetching technology. Meanwhile, photons with longer ultraviolet wavelength have smaller energy, and damage to the quantum dot material is smaller, so that the optical performance of the quantum dot can be maintained to a greater extent. The photoactive additives provided in the prior art do not match this wavelength.
In some embodiments, the coating liquid has a mass fraction of photoactive additive of less than 5wt%.
In some embodiments, the mass concentration of quantum dots in the coating liquid is 15-30mg/ml, preferably 20mg/ml
In some embodiments, the patterned photolithography has an exposure intensity of 50-500mJ/cm 2 Preferably 120mJ/cm 2 。
In some embodiments, the exposure time of the patterned lithography is 1-60min, preferably 15min. Of course, the exposure time is adaptively set in order to satisfy the above exposure intensity, and is not limited to the ranges exemplarily listed herein.
As some typical application examples of the above technical solution, the above photo patterning method may be implemented by the following steps: the quantum dot stock solution of the ligands such as mercaptan, oleic acid, oleylamine and the like is uniformly mixed with the photosensitive agent containing unsaturated bonds or bis-azides, and after the quantum dot stock solution is coated into a film, the film is irradiated in an ultraviolet band through a mask with a preset pattern, and then the film is cleaned by a proper solvent to obtain a corresponding patterned quantum dot luminous structure.
The embodiment of the invention also provides a quantum dot light-emitting structure prepared by the photoinduced patterning method provided by any one of the embodiments.
In some embodiments, the quantum dot light emitting structure has a dimensional accuracy of less than 2 μm, and the photo-induced fluorescence efficiency of the exposed film is substantially the same as that of the original quantum dot film.
The embodiment of the invention also provides an application of the photoinduced patterning method provided by any of the embodiments in preparation of a quantum dot light-emitting device.
The technical scheme of the invention is further described in detail below through a plurality of embodiments and with reference to the accompanying drawings. However, the examples are chosen to illustrate the invention only and are not intended to limit the scope of the invention.
Example 1
The preparation process of the quantum dot light-emitting structure is illustrated in this embodiment, and specifically is as follows:
preparing a coating liquid: adding 4,4 '-bis-azido biphenyl into quantum dot stock solution, stirring uniformly to prepare coating solution, wherein the solvent of the quantum dot stock solution is toluene, the dissolved quantum dots are 20mg/ml, the ligands thereof are oleic acid and oleylamine, and the mass fraction of the quantum dots in the prepared coating solution is 98wt%, and the mass fraction of the 4,4' -bis-azido biphenyl is 2wt%.
Coating of precursor film: and (3) coating to form a liquid film by adopting a spin coating method, and then drying to obtain a precursor film.
Patterning lithography: ultraviolet lithography is carried out on the precursor film, and the illumination intensity is 120mJ/cm 2 The wavelength of the ultraviolet light is 254nm, the illumination time is 15min, and in the photoetching process, argon protection is continuously carried out.
And (3) patterning and developing: and (3) adopting toluene solvent to clean the precursor film of the ultraviolet light non-irradiated part in the patterning photoetching, so that the precursor film is dissolved and removed, and finally, the quantum dot luminous structure with the patterning structure is obtained.
Based on the embodiment, a plurality of samples are fabricated by using different lithography masks, one of which is shown in fig. 3, and is a lithography precision test sample for the above preparation method, it can be seen that the photo-patterning process of the embodiment has high patterning precision, and can obtain higher resolution and structural integrity.
By adopting different photoetching masks, the quantum dot light-emitting device is prepared, and two devices with different sizes and resolutions are respectively shown in fig. 4 and 5, and it can be seen that the preparation of the quantum dot light-emitting device with high resolution and high precision can be realized by adopting the method of the embodiment.
Example 2
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 1, except that:
in the preparation of the coating liquid, 1, 11-diaza-3, 6, 9-oxaundecane was used instead of 4,4' -bis-azidobiphenyl.
In patterned lithography, the wavelength of ultraviolet light was set to 196nm for 5min.
The remaining steps and parameters were the same as in example 1.
The quantum dot light-emitting device prepared by the embodiment has lower illumination wavelength, so that edge diffraction generated by short wavelength is smaller, the formed light-emitting structure is favorable for obtaining sharper boundaries, meanwhile, the specific short-chain molecules are adopted, the steric hindrance is small, the crosslinking reaction is favorable, the efficiency is improved, and the high-performance light-emitting device is easy to prepare.
Example 3
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 1, except that:
in the preparation of the coating liquid, 1-azido-2- (2-azidoethoxy) ethane is used for replacing 4,4' -bis-azidobiphenyl.
In patterned lithography, the wavelength of ultraviolet light is set to 172nm.
The remaining steps and parameters were the same as in example 1.
The quantum dot light-emitting device prepared by the embodiment has lower illumination wavelength, so that the photoetching precision of the formed light-emitting structure is higher, meanwhile, the specific short-chain molecules are adopted, the steric hindrance is small, the efficient crosslinking is realized, and the high-performance light-emitting device is easy to prepare.
Example 4
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 1, except that:
in the preparation of the coating liquid, 5, 11, 11, 17, 17-hexafluorophosphoric acid-6, 12, 18-trihexylamine-5, 6, 11, 12, 17, 18-piperidine-4 b λ4 ，6，10b λ4 ，12，16b λ4 18-Hexagon-5 λ4 ，11 λ4 ，17 λ4 -triboro-trinaphthylene replaces 4,4' -bis-azido-biphenyl.
In patterned lithography, the wavelength of ultraviolet light is set to 405nm.
The remaining steps and parameters were the same as in example 1.
The quantum dot light-emitting device prepared by the embodiment can be matched with longer illumination wavelength due to the provision of the specific photosensitive additive, so that the damage to the light-emitting performance of the quantum dot is small on the basis of keeping the photoetching precision, and the high-performance light-emitting device is easy to prepare.
Example 5
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 1, except that:
in the preparation of the coating liquid, alkyl terminal alkynoic acid is used as a part of surface ligand, and 1, 6-hexanedithiol replaces 4,4' -bis-azido biphenyl.
The remaining steps and parameters were the same as in example 1.
The quantum dot light emitting device prepared in this embodiment, because the photosensitive additive is the coordination of thiol and alkene, the reaction belongs to click chemistry, and mainly the rate of the reaction crosslinking reaction of thiol and alkene (alkene) or alkyne (alkyne) under the induction of ultraviolet light is higher.
Example 6
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 2, except that:
when the coating liquid is prepared, the solvent is n-octane, the mass fraction of the quantum dots and the solvent is 98wt%, and the corresponding mass concentration is 15mg/ml; the mass fraction of the photoactive additive was 2wt%.
In patterning lithography, the exposure intensity was 120mJ/cm 2 The exposure time was 15min.
Example 7
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 2, except that:
photosensitive crosslinking and a 1:1 mass ratio blend of methacrylate and polyethylene cinnamate, wherein the mass ratio of the blend to the solute is 5wt%. The irradiation wavelength used was 254nm, and the exposure time was 20min. The exposure dose was 160mJ/cm 2 。
Comparative example 1
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 1, except that:
in patterning lithography, it is performed directly in air, but not under the protection of inert gas.
Due to the lack of the protection effect of inert gas, the ultraviolet bleaching phenomenon is easy to occur, namely, the surface ligand is dropped off, and the fluorescence performance and stability are reduced.
Comparative example 2
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 2, except that:
in patterning lithography, the illumination wavelength in example 1 was followed without being adapted to 254nm for a specific photosensitive group.
Since the wavelength is not perfectly matched to the photoactive additive and the wavelength is relatively long, the rate of the crosslinking reaction is affected and a substantial extension of the reaction time is required.
Comparative example 3
This example illustrates a quantum dot light emitting structure, which is substantially the same as that of example 4, except that:
in patterning lithography, the illumination wavelength in example 1 was used without adaptation to 405nm.
Since the wavelength is not exactly matched to the photoactive additive, the rate of the crosslinking reaction is affected and the reaction time needs to be adjusted. In addition, the longer wavelength can reduce the influence on the performance of the quantum dot, and the requirements on the reaction atmosphere are more relaxed.
Based on the above embodiments and comparative examples, it can be clear that the photo-induced patterning method provided by the embodiment of the invention can realize direct photolithography forming of the quantum dot material and is convenient for obtaining a pixel array of a high-resolution quantum dot light emitting structure, and because ultraviolet irradiation under protective atmosphere is adopted, the influence on the performance of the quantum dot can be reduced, a better photolithography effect can be obtained, the optical performance of the quantum dot is better maintained, and further, the quantum dot light emitting device with higher precision and better light emitting performance can be obtained.
It should be understood that the above embodiments are merely for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and implement the same according to the present invention without limiting the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.
Claims (10)
1. A method of photopatterning a quantum dot light emitting structure, comprising:
providing a coating liquid, wherein the coating liquid comprises quantum dots and a photosensitive additive, and the surface of the quantum dots is provided with a ligand;
coating the coating liquid into a film to form a precursor film;
and carrying out patterning illumination on the precursor film in a protective atmosphere, and then cleaning and removing part of the precursor film by a solvent to obtain the patterned quantum dot light-emitting structure.
2. The method of claim 1, wherein the ligand comprises any one or a combination of two or more of thiol, alkylphosphonic acid, alkylsulfonic acid, alkylcarboxylic acid, and oleylamine;
and/or the photosensitive additive comprises any one or more than two of materials containing carbon-carbon unsaturated bonds, isocyanate materials, aza-fluorine boron materials and bis-azide materials;
preferably, the material containing carbon-carbon unsaturated bonds comprises oleic acid and an alkene material capable of being mixed and compounded with the oleic acid;
preferably, the solvent in the coating liquid and/or the solvent used for cleaning part of the precursor film is selected from a nonpolar solvent, and more preferably, any one or a combination of two or more of toluene, n-hexane and n-octane.
3. The method of claim 2, wherein the material containing carbon-carbon unsaturation comprises any one or a combination of two or more of divinylbenzene, ethyl cinnamate, triallylisocyanurate, diphenylmethane diisocyanate;
and/or the vinyl material capable of being compounded with the oleic acid comprises any one or the combination of more than two of acrylic ester, methacrylic ester and vinylbenzene;
and/or the bis-azido material comprises any one or combination of two of 1, 11-diaza-3, 6, 9-oxaundecane and 1-azido-2- (2-azidoethoxy) ethane.
4. A photo-patterning process according to claim 3, wherein the wavelength of the patterned light is 260nm or less, preferably 172-254nm, when the photoactive additive is selected from the group of bis-azido materials.
5. The method of claim 2, wherein the photoactive additive further comprises a photoresist composition comprising two or more N-BF 2 Materials of the groups.
6. The method of claim 5, wherein the photoresist comprises more than two N-BF 2 The material of the group is selected from 5, 11, 11, 17, 17-hexafluorophosphoric acid-6, 12, 18-trihexylamine-5, 6, 11, 12, 17, 18-hexahydropyridine-4 b λ4 ，6，10b λ4 ，12，16b λ4 18-Hexagon-5 λ4 ，11 λ4 ，17 λ4 -a triboro-tribenzo-trinaphthylene;
and the wavelength of the patterning lithography is ultraviolet band above 365 nm.
7. The method of claim 1, wherein the mass fraction of photosensitive additive in the coating solution is below 5 wt%;
and/or the mass concentration of the quantum dots in the coating liquid is 15-30mg/ml.
8. The method of claim 1, wherein the patterned lithography has an exposure intensity of 50-500mJ/cm 2 ；
And/or the exposure time of the patterning photoetching is 5-60min.
9. A quantum dot light emitting structure made by the photopatterning method of any one of claims 1-8.
10. Use of the photopatterning method of any of claims 1-8 for the preparation of a quantum dot light emitting device.
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