CN111740023A - Novel quantum dot light-emitting diode device and preparation method thereof - Google Patents
Novel quantum dot light-emitting diode device and preparation method thereof Download PDFInfo
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- CN111740023A CN111740023A CN202010690255.0A CN202010690255A CN111740023A CN 111740023 A CN111740023 A CN 111740023A CN 202010690255 A CN202010690255 A CN 202010690255A CN 111740023 A CN111740023 A CN 111740023A
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- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
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Abstract
The invention relates to a novel quantum dot light-emitting diode device and a preparation method thereof, wherein the preparation method comprises the following steps: preparing a substrate, wherein the substrate is used as an anode electrode layer; spin coating a hole injection layer on the substrate; spin coating a TFB/Au NPS/TFB stack on the hole injection layer; spin-coating a quantum dot light emitting layer on the TFB/Au NPS/TFB laminated structure; spin coating an electron transport layer over the quantum dot light emitting layer; and manufacturing a cathode electrode on the electron transport layer. The invention introduces a novel laminated structure TFB/Au NPs/TFB, accelerates the radiation recombination rate of QDs by utilizing the plasma interaction of Au NPs and quantum dots, enhances the fluorescence emission of the quantum dots, and improves the external quantum efficiency of the device.
Description
Technical Field
The invention relates to the field of quantum dot light-emitting diodes, in particular to a novel quantum dot light-emitting diode device and a preparation method thereof.
Background
Colloidal quantum dots have received extensive attention and research due to their advantages of wide absorption, narrow emission, high color purity and quantum efficiency, etc. At present, the research of quantum dots on the structural level has advanced greatly, but factors hindering the application of quantum dots in devices are still more. The electron-hole injection in the device is unbalanced, so that excessive electrons are accumulated in the luminescent layer, the proportion of non-radiative recombination of excitons is increased, and the fluorescence attenuation of the quantum dot layer is further caused; in addition, interface defects exist in the device, excitons generated by electrode injection are influenced by interface defect states during recombination, fluorescence quenching of non-radiative recombination of quantum dots is caused, and fluorescence attenuation of a quantum dot layer is further caused. In summary, the fluorescence attenuation caused by these problems is a main factor affecting the performance of QLED (Quantum Dot Light Emitting Diodes).
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a novel quantum dot light-emitting diode device and a preparation method thereof, which can enhance the fluorescence emission of quantum dots and improve the external quantum efficiency of the device.
In order to achieve the purpose, the invention provides the following scheme:
a preparation method of a novel quantum dot light-emitting diode device comprises the following steps:
preparing a substrate, wherein the substrate is used as an anode electrode layer;
spin coating a hole injection layer on the substrate;
spin coating a TFB/Au NPS (gold nanoparticles)/TFB stack on the hole injection layer;
spin-coating a quantum dot light emitting layer on the TFB/AuNPS/TFB laminated structure;
spin coating an electron transport layer over the quantum dot light emitting layer;
and manufacturing a cathode electrode on the electron transport layer.
Preferably, the spin coating of the hole injection layer on the substrate specifically includes:
and (3) hanging and dropping a PEDOT (PSS) solution on the substrate, and spin-coating the solution to form a film so as to form the hole injection layer.
Preferably, after the forming the hole injection layer, the method further includes:
and exposing the electrode at the edge of the substrate formed by the hole injection layer and the substrate to form a first auxiliary electrode.
Preferably, the spin coating of the TFB/AuNPS/TFB stacked structure on the hole injection layer specifically includes:
suspending a TFB solution on the hole injection layer, and spin-coating the TFB solution until the solution forms a film to form a hole transport layer;
spin-coating AuNPS on the hole transport layer to form a metal nanoparticle layer;
hanging and dripping TFB solution on the metal nanoparticle layer again, and spin-coating the solution to form a film to form a spacing layer;
the hole transport layer, the metal nanoparticle layer and the spacing layer form the TFB/Au NPS/TFB laminated structure.
Preferably, the spin coating of the AuNPS forms the metal nanoparticle layer at a rotation speed of 2000 rpm.
Preferably, the rotation speed for forming the spacer layer is 3000 rpm.
Preferably, the electronic transmission layer is spin-coated on the quantum dot light-emitting layer, specifically:
and dropwise adding a ZnO NPs (zinc oxide nanoparticles) solution on the quantum dot light-emitting layer to form the electron transmission layer.
Preferably, after the forming the electron transport layer, the method further includes:
and exposing the electrode at the edge of the sample to form a second auxiliary electrode.
Preferably, the substrate is an ITO (Indium tin oxide) glass substrate.
A novel quantum light emitting diode, comprising: the light emitting diode comprises a substrate, a hole injection layer arranged on the substrate, a TFB/AuNPS/TFB laminated structure arranged on the hole injection layer, a quantum dot light emitting layer arranged on the TFB/AuNPS/TFB laminated structure, an electron transport layer arranged on the quantum dot light emitting layer, and a cathode electrode arranged on the electron transport layer, wherein the substrate is used as an anode electrode layer.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects: the invention discloses a novel quantum dot light-emitting diode device and a preparation method thereof.A novel laminated structure TFB/Au NPs/TFB is introduced, and the radiation recombination rate of QDs (quantum dots) is accelerated by utilizing the plasma interaction of AuNPs and quantum dots, so that the fluorescence emission of the quantum dots is enhanced, and the external quantum efficiency of the device is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
Fig. 1 is a diagram of a novel structure of a quantum dot light emitting diode device according to the present invention;
FIG. 2 is a flow chart of a method for fabricating a novel quantum dot light emitting diode of the present invention;
FIG. 3 is a graph showing the absorption spectra of AuNPs and the fluorescence spectra of QDs according to the present invention;
FIG. 4 is an electromagnetic field profile of AuNPs in the present invention and its use
Fig. 5 is a TEM (Transmission electron microscope) sectional view of the plasma device under the optimum conditions.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a novel quantum dot light-emitting diode device and a preparation method thereof, which can enhance the fluorescence emission of quantum dots and improve the external quantum efficiency of the device.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Fig. 1 is a structural diagram of the novel quantum dot light emitting diode device of the present invention, and as shown in fig. 1, the novel quantum dot light emitting diode device of the present invention includes: the LED comprises an ITO substrate, a PEDOT (polymer ethylene terephthalate) hole injection layer arranged on the substrate, a TFB/Au NPS/TFB laminated structure arranged on the hole injection layer, a QDs (quantum dot light emitting) layer arranged on the TFB/Au NPS/TFB laminated structure, a ZnO NPs (N-phosphor) electron transport layer arranged on the quantum dot light emitting layer and an Al cathode electrode arranged on the electron transport layer, wherein the substrate is used as an anode electrode layer.
Specifically, the functional layers are all constructed by a spin coating method except that ITO and Al are deposited by vacuum thermal evaporation.
The invention also discloses a preparation method of the novel quantum dot light-emitting diode, which can enhance the fluorescence emission of the quantum dots and improve the external quantum efficiency of the device.
Fig. 2 is a flowchart of a method for manufacturing a novel quantum dot light emitting diode, and as shown in fig. 1, the method for manufacturing a novel quantum dot light emitting diode according to the present invention includes:
step 100: preparing a substrate, wherein the substrate is used as an anode electrode layer;
step 200: spin coating a hole injection layer on the substrate;
step 300: spin coating a TFB/Au NPS (gold nanoparticles)/TFB stack on the hole injection layer;
step 400: spin-coating a quantum dot light emitting layer on the TFB/AuNPS/TFB laminated structure;
step 500: spin coating an electron transport layer over the quantum dot light emitting layer;
step 600: and manufacturing a cathode electrode on the electron transport layer.
Preferably, the substrate is an ITO substrate.
Specifically, in step 100, the specific steps of preparing the substrate include:
firstly, putting an ITO substrate to be cleaned into dust-free cloth wetted by a detergent for repeated wiping; then, cleaning large particle dust remained on the surface of the ITO substrate after wiping by using a nitrogen gun, and then placing the ITO substrate into a dyeing tank filled with a detergent for ultrasonic treatment for 20min at 80 ℃; then, sequentially putting the mixture into deionized water, acetone and isopropanol to carry out ultrasonic treatment for 15min at normal temperature; the ITO after ultrasonic treatment is dried by a nitrogen gun and is put into UV-O3 for treatment for 15 min. Ozone treatment not only can clean the ITO surface, but also can improve the ITO work function.
Preferably, the specific steps of step 200 are: taking out the rested PEDOT, namely PSS solution, and filtering by using a 0.45 mu m filter head; and then sucking 150 mu L of the filtered PEDOT/PSS solution by using a pipette gun, dripping the PEDOT/PSS solution on an ITO substrate, and spin-coating the ITO substrate for 60s at the rotating speed of 5000rpm by using a spin coater until the solution is formed into a film. And (3) wiping the edge of the ITO/PEDOT (PSS) substrate by using a cotton swab dipped with deionized water to expose the electrode at the edge of the substrate. It was then placed on an annealing plate and heated to 150 ℃ for 15min, and the sample was removed and transferred to a nitrogen glove box insulated from water and oxygen for cooling.
Optionally, the specific steps of step 300 are:
the TFB was spin-coated by dissolving a certain amount of TFB powder in chlorobenzene (8 mg/ml) which is an organic solvent, measured with a scale, and stirring the solution on a stirrer until the powder was dissolved. Filtering the prepared TFB chlorobenzene solution by using a 0.2 mu m filter head to remove impurities, then adsorbing a sample on an objective table by using a spin coater, dropwise adding 60 mu L of TFB solution taken out by using a liquid-transferring gun at a constant speed in the middle of an ITO/PEDOT: PSS substrate with the rotating speed of 5000rpm, placing the ITO/PEDOT: PSS/TFB substrate on an annealing plate, heating to 150 ℃ and maintaining for 30 mm after the solution is subjected to spin coating for 45s to form a film, and placing and cooling after the annealing is finished.
Spin coating Au NPs, spin coating Au NPs with the particle size of 20nm on an ITO/PEDOT: PSS/TFB/AuNPs/TFB substrate at the rotating speed of 2000rpm, and annealing for 10min at 120 ℃. Then, TFB as a spacer layer was spin-coated on the AuNPs layer at 3000rpm and annealed at 150 ℃ for 30 min.
Preferably, the specific steps of step 400 are:
spin coating QDs: filtering the 18mg/mL QDs solution by using a 0.2 mu m PTFE filter head, then adsorbing a sample on a stage by using a spin coater, taking out 60 mu L of the filtered QDs solution by using a pipette gun, dripping the filtered QDs solution into the middle of a substrate with the rotating speed of 2500rpm at a constant speed, and spin-coating for 45s to form a film by the solution.
As an optional implementation manner, the specific steps of step 500 are:
and (3) spin coating ZnO: taking an appropriate amount of ethanol solution of ZnONPs with the concentration of 30mg/ml, filtering impurities by using a 0.2 mu m filter head, taking out 60 mu L of filtered solution by using a pipette, dripping the filtered solution in the middle of an ITO/PEDOT (PSS (AuNPs)/TFB/QDs substrate, and spin-coating for 45s at the rotating speed of 3000rpm by using a spin coater until the solution is formed into a film. The edges of the samples were then wiped with a cotton swab dipped with a small amount of chlorobenzene or toluene solution to expose the electrodes at the edges of the samples, which were then transferred to an annealing plate and heated to 60 ℃ for 30 min.
Optionally, the specific steps of step 600 are:
al electrode deposition, namely moving the constructed sample into a high vacuum deposition chamber (the vacuum degree is less than or equal to 1 × 10-6mbar) to perform
Is used to thermally deposit an aluminum cathode to 100nm, wherein a mask is used to define the top Al contact and form an effective device light emitting area of 0.04cm 2.
Preferably, after the step of fabricating the cathode electrode on the electron transport layer, the method further includes:
packaging the device: dripping 1-2 drops of ultraviolet curing glue into the center of the constructed device, covering a cover glass, and irradiating for 2-3 min by using an ultraviolet lamp for curing.
Alternatively, in the structure of the device, besides the ITO and Al are deposited by vacuum thermal evaporation, other functional layers are constructed by a spin coating method. Wherein the TFB is used as a hole transport layer and a spacer layer of quantum dots and AuNPs.
FIG. 3 is an absorption spectrum diagram of gold nanoparticles and a fluorescence spectrum diagram of QDs, as shown in FIG. 3, the matching of the absorption peak (522nm) of gold nanoparticles and the fluorescence peak (526nm) of quantum dots is good, and the superposition of the two spectra indicates that resonance may occur between the radiation light generated by QDs and the local plasmon resonance effect excited by AuNPs, which results in effective energy transfer, thereby enhancing the emission intensity.
According to the invention, the Au NPs solution is constructed in a spin coating mode, the device is optimized by changing the rotating speed of the AuNPs, and the result shows that the device effect is best when the rotating speed is 2000 rpm. Meanwhile, the distance between the metal nanoparticles and the excitons depends on a strong coupling relationship, so that the rotation speed of the TFB serving as an isolation layer between the QDs and the AuNPs is adjusted to realize the regulation of the distance between the QDs and the AuNPs, and the result shows that the maximum brightness and the current efficiency of the device are optimal when the rotation speed of the TFB is 3000 rpm. Compared with a device without AuNPs, the maximum brightness of the device with the plasma resonance structure is improved by 17.8%; the external quantum efficiency is improved by 29.34 percent.
In order to explore the effect of AuNPs on fluorescence of QDs (quantum dots) layers, stable and transient fluorescence spectrum tests are carried out on quantum dot films at different TFB (tunneling fluorescence spectroscopy) rotating speeds, and the structure of the film is as follows: PSS/TFB/AuNPs/TFB (different rotation speeds)/QDs, and test results show that the introduction of AuNPs shortens the service life of excitons, and meanwhile, the PL intensity of QDs is increased and then reduced along with the reduction of the distance from the Au NPs to a light-emitting layer, because when quantum dots and the AuNPs are too close to each other, the excitons are easy to generate non-radiative recombination in metals, so that fluorescence quenching is caused. Correspondingly, when the distance between the QDs and the AuNPs is proper, the AuNPs and the quantum dot film generate a strong coupling effect, the radiation recombination rate of excitons is favorably improved, and the photoluminescence performance of the QDs film is enhanced. To verify this, the interaction of AuNPs with QDs was simulated in the device environment (thickness and dielectric constant of each layer) by Finite-difference time-Domain (FDTD), as shown in fig. 4, where the LSPR intensity is distributed on the axis (x ═ 0) and the vertical axis Z represents the intensity value of the LSPR. The time domain finite difference time domain simulation of LSPR intensity distribution showed an effective distance of LSPR of about 20nm when AuNPs have a particle size of 20nm, and meanwhile, as shown in fig. 5, it was found from the TEM test that the thickness of TFB was 20nm, which indicates that AuNPs are less than 20nm apart from QDs. In summary, the electromagnetic field distribution of the gold nanoparticles has a certain range, and when the distance between the gold nanoparticles and the luminescent layer is proper, the QDs is in the maximum field intensity generated by AuNPs, so that the resonance coupling strength is maximized, and the device performance is optimal.
The LSPR effect of the metal nano-particles can further improve the problem of low luminous efficiency of the device by enhancing the fluorescence of the quantum dots. The LSPR characteristic of metal nanoparticles is an important attribute different from bulk phase materials, and in recent years, researchers have conducted intensive research on the fields of photonics, catalysis, optical sensing, and the like, wherein fluorescence enhancement of luminescent materials near the metal nanoparticles attracts more and more attention. Research shows that the fluorescence intensity of the metal surface is influenced by the distance from the metal surface to the fluorescent molecules, when the distance between the metal and the fluorescent molecules is smaller, although the excited electromagnetic field intensity is stronger, more energy is transmitted to the metal in a non-radiation form, so that the negative influence caused by non-radiation loss is stronger than the enhancement effect of the excitation electromagnetic field, fluorescence quenching is caused, and when the distance between the QDs and the AuNPs is proper, the AuNPs and the quantum dot film generate stronger coupling effect, thereby being beneficial to improving the radiation recombination rate of excitons and enhancing the photoluminescence performance of the QDs film. Therefore, it is important to enhance the quantum dot light emitting diode by using the plasma effect of AuNPs and QDs.
The invention has the following beneficial effects:
the invention introduces a novel laminated structure TFB/AuNPs/TFB and is used for constructing a QLED device with a plasma resonance structure. The radiation recombination rate of QDs is accelerated by utilizing the plasma interaction of Au NPs and quantum dots, the fluorescence emission of the quantum dots is enhanced, and the external quantum efficiency of the device is improved.
The distribution density of the Au NPs is optimized by adjusting the rotating speed of the AuNPs, and when the rotating speed is 2000rpm, the performance of a device is optimal; the distance between Au NPs and QDs is regulated and controlled by adjusting the thickness of the spacer layer TFB, and the device performance is optimal when the rotating speed is 3000 rpm; compared with a non-AuNPs device, the maximum brightness of the device is improved to 183900cd/m2 from 156300cd/m2 due to the introduction of AuNPs, and the improvement amplitude is 17.8%; the external quantum efficiency is improved from 16.08% to 22.76%, and the improvement of 29.34% under the condition of higher external quantum efficiency is realized.
The invention discovers that excitons are easy to generate non-radiative recombination in metal to cause fluorescence quenching when the distances between the quantum dots and AuNPs are too close by analyzing transient and steady fluorescence spectrums of the quantum dot film under different TFB rotating speeds. Correspondingly, when the distance between the QDs and the Au NPs is proper, the Au NPs and the quantum dot film generate a strong coupling effect, which is beneficial to improving the radiative recombination rate of excitons and enhancing the photoluminescence performance of the QDs film.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. For the system disclosed by the embodiment, the description is relatively simple because the system corresponds to the method disclosed by the embodiment, and the relevant points can be referred to the method part for description.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. A preparation method of a novel quantum dot light-emitting diode device is characterized by comprising the following steps:
preparing a substrate, wherein the substrate is used as an anode electrode layer;
spin coating a hole injection layer on the substrate;
spin coating a TFB/AuNPS/TFB stack on the hole injection layer;
spin-coating a quantum dot light emitting layer on the TFB/AuNPS/TFB laminated structure;
spin coating an electron transport layer over the quantum dot light emitting layer;
and manufacturing a cathode electrode on the electron transport layer.
2. The method for manufacturing a novel quantum dot light-emitting diode device according to claim 1, wherein the spin coating of the hole injection layer on the substrate specifically comprises:
and (3) hanging and dropping a PEDOT (PSS) solution on the substrate, and spin-coating the solution to form a film so as to form the hole injection layer.
3. The method for preparing the novel quantum dot light-emitting diode device according to claim 2, wherein in the step of forming the hole injection layer, the method further comprises:
and exposing the electrode at the edge of the substrate formed by the hole injection layer and the substrate to form a first auxiliary electrode.
4. The method according to claim 1, wherein the step of spin-coating a TFB/AuNPS/TFB stack on the hole injection layer comprises:
suspending a TFB solution on the hole injection layer, and spin-coating the TFB solution until the solution forms a film to form a hole transport layer;
spin-coating AuNPS on the hole transport layer to form a metal nanoparticle layer;
hanging and dripping TFB solution on the metal nanoparticle layer again, and spin-coating the solution to form a film to form a spacing layer;
the hole transport layer, the metal nanoparticle layer and the spacing layer form the TFB/Au NPS/TFB laminated structure.
5. The method for preparing the novel quantum dot light-emitting diode device according to claim 4, wherein the spin coating of AuNPS to form the metal nanoparticle layer is performed at 2000 rpm.
6. The method for preparing a novel quantum dot light-emitting diode device according to claim 4, wherein the rotation speed for forming the spacer layer is 3000 rpm.
7. The method for preparing a novel quantum dot light-emitting diode device according to claim 1, wherein an electron transport layer is spin-coated on the quantum dot light-emitting layer, specifically:
and dropwise adding a ZnO NPs solution on the quantum dot light-emitting layer to form the electron transmission layer.
8. The method for preparing the novel quantum dot light-emitting diode device according to claim 5, wherein in the step of forming the electron transport layer, the method further comprises:
and exposing the electrode at the edge of the sample to form a second auxiliary electrode.
9. The method of claim 1, wherein the substrate is an ITO glass substrate.
10. A novel quantum light emitting diode, comprising: the light emitting diode comprises a substrate serving as an anode electrode layer, a hole injection layer arranged on the substrate, a TFB/Au NPS/TFB laminated structure arranged on the hole injection layer, a quantum dot light emitting layer arranged on the TFB/Au NPS/TFB laminated structure, an electron transport layer arranged on the quantum dot light emitting layer, and a cathode electrode arranged on the electron transport layer.
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| CN105140412A (en) * | 2015-09-01 | 2015-12-09 | Tcl集团股份有限公司 | QLED device with high light-emitting efficiency and preparation method thereof |
| US20190288230A1 (en) * | 2018-03-14 | 2019-09-19 | Samsung Electronics Co., Ltd. | Electroluminescent device, and display device comprising thereof |
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Application publication date: 20201002 |