CN111384253B - Quantum dot light-emitting diode and preparation method thereof - Google Patents
Quantum dot light-emitting diode and preparation method thereof Download PDFInfo
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- CN111384253B CN111384253B CN201811610461.5A CN201811610461A CN111384253B CN 111384253 B CN111384253 B CN 111384253B CN 201811610461 A CN201811610461 A CN 201811610461A CN 111384253 B CN111384253 B CN 111384253B
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/16—Electron transporting layers
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- 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 belongs to the technical field of display, and particularly relates to a quantum dot light-emitting diode and a preparation method thereof. A quantum dot light-emitting diode comprises an anode, a cathode and a quantum dot light-emitting layer positioned between the anode and the cathode, wherein an electron transmission layer is also arranged between the cathode and the quantum dot light-emitting layer, and the electron transmission layer is made of graphite fluoride alkyne. The fluorinated graphite alkyne is used for the electron transmission layer of the quantum dot light-emitting diode device, has the advantage of high electron transmission efficiency, is high in matching degree with the quantum dot light-emitting layer, and finally improves the light-emitting performance of the device.
Description
Technical Field
The invention belongs to the technical field of display, and particularly relates to a quantum dot light-emitting diode and a preparation method thereof.
Background
Quantum dot light emitting diodes (QLEDs) are expected to become a new generation of excellent display technology due to their advantages of high light emitting efficiency, high color purity, narrow light emission spectrum, adjustable emission wavelength, and the like, and the technical level of each aspect is also continuously improved. The optimization of the device structure is a large direction for improving the performance of the QLED, and how to improve the luminous efficiency of the light-emitting layer by optimizing the charge transport layer is the most important link.
The graphene has natural direct band gap, conductivity comparable to that of graphene materials, and intrinsic hole mobility (up to 4.29 multiplied by 10) higher than that of graphene at room temperature5cm2·V-1·s-1) The excellent semiconductor carbon material has extremely high application potential in the field of semiconductor materials. At present, materials such as metal oxides and organic polymers are often used for preparing the QLED electron transport layer, but these materials have the disadvantages of low energy level matching degree, low transport efficiency, and the like.
Therefore, the prior art is in need of improvement.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a quantum dot light-emitting diode and a preparation method thereof, and aims to solve the technical problem that the electron transmission efficiency of an electron transmission layer of the conventional device is low.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a quantum dot light-emitting diode which comprises an anode, a cathode and a quantum dot light-emitting layer positioned between the anode and the cathode, wherein an electron transmission layer is also arranged between the cathode and the quantum dot light-emitting layer, and the electron transmission layer is made of fluorinated graphite alkyne.
The electron transport layer in the quantum dot light-emitting diode provided by the invention is composed of graphite fluoride alkyne, the forbidden bandwidth of the graphite alkyne is smaller, the graphite fluoride alkyne is a material with larger forbidden bandwidth (more than 4.0 eV), the Fermi energy of the graphite alkyne and the nearby track are activated by doping fluorine atoms, and the conjugated electron density is changed, so that the forbidden bandwidth is improved in addition to the n-type structure and the conductive property of the intrinsic material of the graphite alkyne, therefore, the graphite fluoride alkyne can be directly used as the electron transport layer material without additional doping, and the graphite fluoride alkyne is used for the electron transport layer of the quantum dot light-emitting diode device, so that the quantum dot light-emitting diode has the advantage of high electron transport efficiency, is high in matching width with a quantum dot light-emitting layer, and finally improves the light-emitting performance of the device.
The invention also provides a preparation method of the quantum dot light-emitting diode, which comprises the following steps:
providing a substrate;
dissolving graphite fluoride alkyne in a solvent to obtain a graphite fluoride alkyne solution;
and depositing the graphite fluoride alkyne solution on a substrate to obtain the electron transport layer.
According to the preparation method of the quantum dot light-emitting diode, the fluorinated graphite alkyne is prepared into the electron transmission layer by a solution method, so that the process is simple, the cost is low, the electron transmission efficiency can be improved, the matching degree with the quantum dot light-emitting layer is high, and the light-emitting performance of the device is finally improved.
Drawings
Fig. 1 is a schematic structural diagram of a quantum dot light-emitting diode according to embodiment 4 of the present invention;
fig. 2 is a flow chart of a manufacturing process of a quantum dot light emitting diode according to an embodiment of the invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
On one hand, the embodiment of the invention provides a quantum dot light-emitting diode, which comprises an anode, a cathode and a quantum dot light-emitting layer positioned between the anode and the cathode, wherein an electron transmission layer is also arranged between the cathode and the quantum dot light-emitting layer, and the electron transmission layer is made of graphite fluoride alkyne.
The electron transport layer in the quantum dot light-emitting diode provided by the embodiment of the invention is composed of graphite fluoride alkyne, the forbidden bandwidth of graphite alkyne is smaller, the graphite fluoride alkyne is a material with larger forbidden bandwidth (more than 4.0 eV), and fluorine atoms are doped to activate the Fermi energy of graphite alkyne and nearby tracks, so that the conjugated electron density is changed, the n-type structure and the conductive property of the intrinsic material of graphite alkyne are reserved, and the forbidden bandwidth is also improved.
The graphene is an n-type semiconductor with approximate conductivity to graphene, has higher charge transport capacity than metal oxides and the like, and is an ideal QLED electron transport layer material. When added to graphdiynes, fluorine is preferentially bonded to sp-hybridized carbon atoms, one of which is first above the plane of the ring and the other below the plane. By doping fluorine, the forbidden band width of the graphite fluoride alkyne can reach more than 4.0 eV: by fluorinating different positions of graphyne, px, py and s orbitals near the Fermi level can be activated, and triple bonds in the graphyne are completely opened to obtain sp3In the hybrid form, the forbidden band width of the graphdine can be adjusted to 4.0eV after a certain doping proportion is achieved. The fluorinated graphdine has no change in configuration, so that the fluorinated graphdine still has high electron transmission efficiency, the forbidden band width can be adjusted to 4.0eV after a proper fluorine element is added, and the proper band gap is favorable for charge transmission between the transmission layer and the quantum dot light-emitting layer, so that the electron transmission performance of the electron transmission layer is improved, and the luminous efficiency of the QLED device is improved.
Furthermore, in the quantum dot light-emitting diode provided by the embodiment of the invention, fluorine is added to an alkyne bond in the graphyne to form the graphyne fluoride, the band gap is adjusted to 3.75-4.0 eV, and the band gap of the graphyne fluoride is adjusted to obtain a better electron transport property.
Further, in the quantum dot light emitting diode provided by the embodiment of the present invention, the fluorinated graphite alkyne is fluorinated (that is, the alkyne bond is sp after completely passing through the fluorine element addition3A bond) is 50 to 100% in the number ratio of the acetylene bonds. Namely, the graphite alkyne has a fluorinated graphite alkyne band gap of 50 to 100 fluorinated alkyne bonds per 100 alkyne bonds, more preferably, 90 to 100% fluorinated alkyne bonds, i.e., carbon atoms on the original alkyne bonds are respectively connected with two fluorine atoms, so that the graphite alkyne has better electron transport performance. Further, the particle size of the fluorinated graphite alkyne is 1-10 nm.
Further, the fluorinated graphite alkyne is selected from at least one of fluorinated graphite alkyne nanospheres, fluorinated graphite alkyne nanowires, fluorinated graphite alkyne nanorods and fluorinated graphite alkyne nanocones, and in one embodiment of the present invention, the fluorinated graphite alkyne nanospheres (including graphite alkyne nanospheres), the graphite alkyne nanowires, the graphite alkyne nanorods and the graphite alkyne nanocones can be obtained by fluorination; or, the fluorinated graphite alkyne is at least one selected from fluorinated alpha-graphite alkyne, fluorinated beta-graphite alkyne, fluorinated gamma-graphite alkyne, fluorinated delta-graphite alkyne and fluorinated 6,6, 12-graphite alkyne, and in an embodiment of the invention, the fluorinated graphite alkyne can be obtained by fluorinating alpha-graphite alkyne (alpha-GY), beta-graphite alkyne (beta-GY), gamma-graphite alkyne (gamma-GY), delta-graphite alkyne (delta-GY), 6,6, 12-graphite alkyne (6,6, 12-GY).
Further, in the quantum dot light emitting diode provided by the embodiment of the invention, the thickness of the electron transport layer is 10-100nm, preferably 30 nm. Furthermore, an electron injection layer is arranged between the cathode and the electron transport layer; and a hole function layer, such as a hole injection layer and a hole transport layer, is arranged between the anode and the quantum dot light-emitting layer.
On the other hand, the embodiment of the invention also provides a preparation method of the quantum dot light-emitting diode, as shown in fig. 2, comprising the following steps:
s01: providing a substrate;
s02: dissolving graphite fluoride alkyne in a solvent to obtain a graphite fluoride alkyne solution;
s03: and depositing the graphite fluoride alkyne solution on a substrate to obtain the electron transport layer.
According to the preparation method of the quantum dot light-emitting diode provided by the embodiment of the invention, the fluorinated graphite alkyne is prepared into the electron transmission layer by a solution method, so that the process is simple, the cost is low, the electron transmission efficiency can be improved, the matching degree with the quantum dot light-emitting layer is high, and the light-emitting performance of the device is finally improved.
Further, in the above step S01: if the surface of the substrate is a cathode (cathode substrate), an electron transmission layer can be directly prepared on the cathode, and then a quantum dot light-emitting layer is prepared; if the surface of the substrate is a quantum dot light-emitting layer (anode substrate), an electron transmission layer is prepared on the surface of the quantum dot light-emitting layer, and then a cathode is prepared.
Further, in the above step S02: the solvent can be polar solvent such as methanol, ethanol, etc., or nonpolar solvent; further, the preparation method of the fluorinated graphite alkyne comprises the following steps: and placing the graphite alkyne in a gaseous fluorine source, and heating to obtain the fluorinated graphite alkyne. Preferably, the temperature of the heating treatment is 50-300 ℃; the time of the heating treatment is 20-40 min. More preferably, the heating treatment is carried out by placing the graphdiyne in an inert gas atmosphere having a volume fraction of 0.5 to 5% of a gaseous fluorine source.
In a specific embodiment, the graphite alkyne powder with a proper particle size is firstly selected and spread on a watch glass, and argon is introduced for a certain time to primarily remove residual air and moisture. Then heating to a certain temperature, and switching to gas with fluorine source at 50-300 deg.C, wherein the temperature is selected according to the kind of fluorine source, and the gas with active chemical activity is F2The temperature of fluorine gas should be selected to be lower, and the temperature of HF gas should be increased if the chemical activity is lower. The concentration of the fluorine source gas is preferably 0.5-5% (volume percentage), and if the concentration of the fluorine source is too high, the two-dimensional carbon structure of the graphite alkyne is easily damaged by the strong oxidizing property of the graphite alkyne; if the concentration is too low, effective gas-solid molecular contact cannot be achieved, and the reaction activity is low. By controlling the temperature, the concentration of the fluorine source and the reaction time, 90-100% of acetylene bonds can be fluorinated, so that the band gap is adjusted to 3.75-4.0 eV.
Preferably, the gaseous fluorine source is selected from F2、SF6And HF; the graphdiyne is selected from at least one of graphdiyne nano-microspheres, graphdiyne nanowires, graphdiyne nano-rods and graphdiyne nanocones; or, the graphoyne is selected from at least one of alpha-graphoyne, beta-graphoyne, gamma-graphoyne, delta-graphoyne, and 6,6, 12-graphoyne.
In an embodiment of the invention, a preparation method of a quantum dot light-emitting diode with a fluorinated graphite alkyne electron transport layer is as follows.
A: firstly, growing a hole transport layer on a substrate;
b: then depositing a quantum dot light-emitting layer on the hole transport layer;
c: and finally, depositing an electron transport layer on the quantum dot light-emitting layer, wherein the electron transport layer is made of the fluorinated graphite alkyne, and evaporating a cathode on the electron transport layer to obtain the light-emitting diode.
According to the preparation method of the quantum dot light-emitting diode, the quantum dot of the quantum dot light-emitting layer is one of red, green and blue. Can be at least one of CdS, CdSe, CdTe, ZnO, ZnS, ZnSe, ZnTe, GaAs, GaP, GaSb, HgS, HgSe, HgTe, InAs, InP, InSb, AlAs, AlP, CuInS, CuInSe and various core-shell structure quantum dots or alloy structure quantum dots. Then the quantum dots can be any one of the three common red, green and blue quantum dots or other yellow light, and the quantum dots can be cadmium-containing or cadmium-free. The quantum dot light emitting layer of the material has the characteristics of wide and continuous excitation spectrum distribution, high emission spectrum stability and the like.
Further, the obtained QLED is subjected to a packaging process, and the packaging process may be performed by a common machine or by a manual method. Preferably, the oxygen content and the water content in the packaging treatment environment are both lower than 0.1ppm so as to ensure the stability of the device.
And depositing the prepared fluorinated graphite alkyne solution on the quantum dot light-emitting layer by using a deposition method which can be but not limited to a spin coating method, a blade coating method, a printing method, a spraying method, a rolling coating method, an electrodeposition method and the like and is not limited to a deposition method which can form a film layer so as to obtain the fluorinated graphite alkyne electron transport layer. Preferably, the thickness of the fluorinated graphite alkyne electron transport layer is 10-100nm, and preferably 30 nm.
The invention is described in further detail with reference to a part of the test results, which are described in detail below with reference to specific examples.
Example 1
Using graphyne nanospheres, 1% fluorine gas F2(99% argon), etc. as examples:
1) spreading 500mg of graphdiyne powder on a watch glass, placing the watch glass in a muffle furnace and continuously introducing argon;
2) heating a muffle furnace to 70 ℃, switching argon into 1% fluorine gas (99% argon), introducing the fluorine gas for 30 minutes, cutting off a fluorine gas source, preserving the temperature for 30 minutes, and cooling to room temperature;
3) and dispersing the fluorinated graphite alkyne in a solvent for preparing a QLED electron transmission layer, and then forming a QLED device with other functional layers.
Example 2
Using graphite alkyne nano-microsphere, 1% SF6(99% argon), etc. as examples:
1) spreading 500mg of graphdiyne powder on a watch glass, placing the watch glass in a muffle furnace and continuously introducing argon;
2) after the muffle furnace is heated to 200 ℃, the argon is switched to 1 percent SF6(99% argon), and 30 minutes after the introduction of the solution, SF was cut off6Air source, keeping the temperature for 30 minutes and then cooling to room temperature;
3) and dispersing the fluorinated graphite alkyne in a solvent for preparing a QLED electron transmission layer, and then forming a QLED device with other functional layers.
Example 3
The details are described by taking the graphdiyne nanorods, 1% HF (99% argon), and the like as examples:
1) spreading 500mg of graphdiyne powder on a watch glass, placing the watch glass in a muffle furnace and continuously introducing argon;
2) heating a muffle furnace to 250 ℃, switching argon into 1% HF (99% argon), introducing the HF for 30 minutes, cutting off an HF gas source, preserving heat for 30 minutes, and cooling to room temperature;
3) and dispersing the fluorinated graphite alkyne in a solvent for preparing a QLED electron transmission layer, and then forming a QLED device with other functional layers.
Example 4
As shown in fig. 1, a schematic structural diagram of a quantum dot light emitting diode, the method for manufacturing the device includes the following steps:
a: firstly, growing a hole transport layer on an ITO substrate;
b: then depositing a quantum dot light-emitting layer on the hole transport layer;
c: and finally, depositing an electron transport layer on the quantum dot light-emitting layer, wherein the electron transport layer is made of the fluorinated graphite alkyne, and evaporating a cathode on the electron transport layer to obtain the light-emitting diode.
Fig. 1 is a schematic structural diagram of a QLED device according to the present invention, and the QLED device sequentially includes a substrate 1, an anode 2, a hole transport layer 3, a quantum dot light emitting layer 4, an electron transport layer 5, and a cathode 6 from bottom to top. The substrate 1 is made of a glass sheet, the anode 2 is made of an ITO (indium tin oxide) base plate, the hole transport layer 3 is made of a metal oxide hole transport layer, the electron transport layer 5 is made of a graphite fluoride alkyne material, and the cathode 6 is made of Al.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A quantum dot light-emitting diode comprises an anode, a cathode and a quantum dot light-emitting layer positioned between the anode and the cathode, wherein an electron transmission layer is also arranged between the cathode and the quantum dot light-emitting layer, and the quantum dot light-emitting diode is characterized in that the electron transmission layer is made of graphite fluoride alkyne, and the number ratio of fluorinated alkyne bonds in the graphite fluoride alkyne is 50-100%.
2. The quantum dot light-emitting diode of claim 1, wherein the fluorinated graphdine has a band gap of 3.75 to 4.0 eV.
3. The quantum dot light-emitting diode of claim 1, wherein the fluorinated graphdiyne has a fluorinated alkyne linkage number ratio of 90-100%.
4. The quantum dot light-emitting diode of claim 1, wherein the particle size of the graphdiyne fluoride is 1-10 nm; and/or the presence of a gas in the gas,
the fluorinated graphite alkyne is selected from at least one of fluorinated graphite alkyne nano-microspheres, fluorinated graphite alkyne nano-wires, fluorinated graphite alkyne nano-rods and fluorinated graphite alkyne nano-cones; and/or the presence of a gas in the gas,
the fluorinated graphoyne is selected from at least one of fluorinated alpha-graphoyne, fluorinated beta-graphoyne, fluorinated gamma-graphoyne, fluorinated delta-graphoyne and fluorinated 6,6, 12-graphoyne.
5. The qd-led of any one of claims 1 to 4, wherein the electron transport layer has a thickness of 10nm to 100 nm.
6. A preparation method of a quantum dot light-emitting diode is characterized by comprising the following steps:
providing a substrate;
dissolving graphite fluoride alkyne in a solvent to obtain a graphite fluoride alkyne solution, wherein the number ratio of alkyne bonds to be fluorinated in the graphite fluoride alkyne is 50-100%;
and depositing the graphite fluoride alkyne solution on a substrate to obtain the electron transport layer.
7. The method of claim 6, wherein the method of preparing the graphite alkyne fluoride comprises: and placing the graphite alkyne in a gaseous fluorine source, and heating to obtain the fluorinated graphite alkyne.
8. The method according to claim 7, wherein the temperature of the heat treatment is 50 to 300 ℃; and/or the presence of a gas in the gas,
the time of the heating treatment is 20-40 min; and/or the presence of a gas in the gas,
and placing the graphdiyne in an inert gas environment with the volume fraction of 0.5-5% of a gaseous fluorine source to carry out the heating treatment.
9. The method of claim 7, wherein the gaseous fluorine source is selected from the group consisting of F2、SF6And HF; and/or the presence of a gas in the gas,
the graphdiyne is selected from at least one of graphdiyne nano-microspheres, graphdiyne nanowires, graphdiyne nano-rods and graphdiyne nanocones; and/or the presence of a gas in the gas,
the graphoyne is selected from at least one of alpha-graphoyne, beta-graphoyne, gamma-graphoyne, delta-graphoyne and 6,6, 12-graphoyne.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811610461.5A CN111384253B (en) | 2018-12-27 | 2018-12-27 | Quantum dot light-emitting diode and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811610461.5A CN111384253B (en) | 2018-12-27 | 2018-12-27 | Quantum dot light-emitting diode and preparation method thereof |
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| KR20150028872A (en) * | 2013-08-27 | 2015-03-17 | 건국대학교 산학협력단 | Graphyne-based materials with a tunable energy band gap using halogenation |
| CN107732015A (en) * | 2017-11-06 | 2018-02-23 | 苏州大学 | Perovskite type solar cell with graphdiyne induced cross-linked fullerene in-plane orientation as electron transport layer and preparation method thereof |
| CN108878663A (en) * | 2017-05-10 | 2018-11-23 | Tcl集团股份有限公司 | QLED device and preparation method thereof |
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| CN102983313A (en) * | 2012-12-05 | 2013-03-20 | 奇瑞汽车股份有限公司 | Silicon-carbon composite material and preparation method thereof, and lithium ion battery |
| KR20150028872A (en) * | 2013-08-27 | 2015-03-17 | 건국대학교 산학협력단 | Graphyne-based materials with a tunable energy band gap using halogenation |
| CN108878663A (en) * | 2017-05-10 | 2018-11-23 | Tcl集团股份有限公司 | QLED device and preparation method thereof |
| CN107732015A (en) * | 2017-11-06 | 2018-02-23 | 苏州大学 | Perovskite type solar cell with graphdiyne induced cross-linked fullerene in-plane orientation as electron transport layer and preparation method thereof |
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