CN113122257A - Thin film and preparation method thereof and quantum dot light-emitting diode - Google Patents
Thin film and preparation method thereof and quantum dot light-emitting diode Download PDFInfo
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- H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots
Abstract
The invention discloses a film, a preparation method thereof and a quantum dot light-emitting diode, wherein the film comprises a metal organic frame layer and quantum dots embedded in pores of the metal organic frame layer, and acidic ions or acidic molecules are combined in the metal organic frame layer. The film provided by the invention adopts the metal organic frame layer combined with acidic ions or molecules as a supporting structure, and the acidic groups and the main frame form a dense and strong hydrogen bond network, so that the high-speed conduction of protons is realized, the transmission of hole carriers is facilitated, the injection balance of holes and electrons is improved, and the performance of the quantum dot light-emitting diode is finally improved.
Description
Technical Field
The invention relates to the field of quantum dot light-emitting devices, in particular to a thin film and a preparation method thereof, and a quantum dot light-emitting diode.
Background
Quantum dot light emitting diodes (QLEDs) are of interest due to the attractive properties of quantum dots, such as precise gaussian distribution, tunable emission, and easy to handle solutions. The traditional method for obtaining the quantum dot light-emitting layer by directly depositing the quantum dot solution on the substrate or the functional layer may cause unfavorable results such as quantum dot agglomeration, and the method needs to be optimized.
One of the main intrinsic factors limiting the performance of QLED devices is the quenching of the quantum dot brightness, which is caused by the carrier injection imbalance due to the large hole injection barrier.
The Metal Organic Frameworks (MOFs) are porous polymers and are constructed by metal ions/clusters and organic ligands, and the material has the characteristics of designable structure, adjustable pore channel size, functional modification of pore walls, high crystallization and the like. Especially, the modified MOFs material has good proton conductivity.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a thin film, a preparation method thereof and a quantum dot light-emitting diode, and aims to solve the problem that the current quantum dot light-emitting diode is unbalanced in carrier injection due to a large hole injection barrier, and finally the performance of the device is affected.
The technical scheme of the invention is as follows:
the thin film comprises a metal organic framework layer and quantum dots embedded in pores of the metal organic framework layer, wherein acidic ions or acidic molecules are combined in the metal organic framework layer.
A method for producing a thin film, comprising the steps of:
providing a first feedstock liquid, the first feedstock liquid comprising: the metal organic framework layer raw material and acidic ions or the first raw material solution comprise the metal organic framework layer raw material and acidic molecules;
depositing the first raw material solution on a substrate or a functional layer, and drying to obtain a metal organic framework layer combined with acidic ions or acidic molecules;
providing a second raw material liquid, wherein the second raw material liquid comprises quantum dots;
and depositing the second raw material solution on the metal organic frame layer combined with the acidic ions or acidic molecules, drying, and embedding quantum dots in gaps of the metal organic frame layer to obtain the film.
A method for producing a thin film, comprising the steps of:
providing a first raw material solution, wherein the first raw material solution comprises a metal organic framework layer raw material and acidic ions or the first raw material solution comprises a metal organic framework layer raw material and acidic molecules;
providing a second raw material liquid, wherein the second raw material liquid comprises quantum dots;
and mixing the first raw material solution and the second raw material solution, depositing the mixture on a substrate or a functional layer, and drying to obtain the film.
The quantum dot light-emitting diode comprises an anode, a quantum dot light-emitting layer and a cathode, wherein the quantum dot light-emitting layer is arranged between the anode and the cathode, and the quantum dot light-emitting layer is the film.
A preparation method of a quantum dot light-emitting diode comprises the following steps:
providing an anode;
preparing a thin film on the anode;
preparing a cathode on the quantum dot light-emitting layer to obtain the quantum dot light-emitting diode;
alternatively, a cathode is provided;
preparing a thin film on the cathode;
preparing an anode on the quantum dot light-emitting layer to obtain the quantum dot light-emitting diode;
the film comprises a metal organic framework layer and quantum dots embedded in pores of the metal organic framework layer, wherein acidic ions or acidic molecules are combined in the metal organic framework layer.
Has the advantages that: the film provided by the invention adopts the metal organic frame layer combined with acidic ions or molecules as a supporting structure, and the acidic groups and the main frame form a dense and strong hydrogen bond network, so that the high-speed conduction of protons is realized, the transmission of hole carriers is facilitated, the injection balance of holes and electrons is improved, and the performance of the quantum dot light-emitting diode is finally improved.
Drawings
Fig. 1 is a schematic flow chart of a method for preparing a thin film according to an embodiment of the present invention.
Fig. 2 is a schematic flow chart of a method for manufacturing a thin film according to another embodiment of the present invention.
Fig. 3 is a schematic structural diagram of a quantum dot light emitting diode according to an embodiment of the present invention.
Detailed Description
The invention provides a film, a preparation method thereof and a quantum dot light-emitting diode, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a film, which comprises a metal organic framework layer and quantum dots embedded in pores of the metal organic framework layer, wherein acidic ions or acidic molecules are combined in the metal organic framework layer.
The film provided by the embodiment of the invention adopts the metal organic frame layer combined with acidic ions or molecules as a supporting structure, and the acidic groups and the main frame form a dense and strong hydrogen bond network, so that the high-speed conduction of protons is realized, the transmission of hole carriers is facilitated, the injection balance of holes and electrons is improved, and the performance of the quantum dot light-emitting diode is finally improved.
The film provided by the embodiment of the invention adopts the metal organic frame layer as the supporting structure, the metal organic frame layer has the characteristic of high porosity, the quantum dots are embedded in the pores of the metal organic frame, and the adjacent pores are spaced, so that the agglomeration risk and the fluorescence energy resonance transfer are greatly reduced. In addition, the metal organic framework can be used as a protective shell layer of the quantum dot, so that the defects on the surface of the quantum dot can be modified, and the light intensity of the quantum dot is improved.
According to the film provided by the embodiment of the invention, the quantum dots are embedded in the pore structure of the metal organic frame layer combined with a large amount of acidic ions or molecules, so that on one hand, the proton transmission performance of the large amount of acidic ions or molecules combined in the metal organic frame layer is utilized to improve the injection balance of carriers, and the purpose of improving the performance of a device is achieved; on the other hand, the quantum dots are limited by the gaps of the metal organic framework layer, so that the quantum dots are improved, the self-quenching effect caused by the agglomeration of the quantum dots can be avoided, and the improvement of the luminescence performance of the quantum dots is facilitated.
The combination mode of the acidic ions or molecules and the metal organic framework layer in the embodiment of the invention comprises the following steps: 1. loading the acidic ions or molecules with pores of the metal organic framework layer; 2. bonding acidic ions or molecules on the framework of the metal organic framework layer; 3. the acidic ions are obtained by sulfonating groups (such as sulfhydryl ligand and aromatic ring ligand) on organic ligands of MOFs.
In one embodiment, the acidic ion comprises H4 +、H3O+And HSO4 +And the like are not limited to one or more of these.
In one embodiment, the acidic molecule includes one or more of hexanoic acid, benzenesulfonic acid, trifluoromethanesulfonic acid, sulfuric acid, phosphoric acid, and the like, without limitation.
In one embodiment, the quantum dot is a group II-VI CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdZnS, CdZnSe, CdZnTe, ZnSeS, ZnSeTe, ZnTeS, CdSeS, CdSeTe, CdTeS, CdZnSeS, CdZnSeTe, CdZnSTe, CdSeSTe, ZnSeTe or CdZnSeTe; or InP, InAs or InAsP from group III-V; or group IV-VI PbS, PbSe, PbTe, PbSeS, PbSeTe or PbSTe; or a combination of any one or more of the above.
The metal organic framework layer in the embodiment of the invention is formed by coordination and self-assembly of metal nodes (metal ions or metal clusters including but not limited to magnesium, manganese, iron, cobalt, nickel, zinc and the like) and organic ligands, and the chain length of the organic ligands determines the diameter of pores of the metal organic framework. Generally, the particle size distribution of the quantum dots is 2-20nm, and the diameter of the pores is designed to be 2-30nm according to the size of the quantum dots, so that the quantum dots are all positioned in the pores and are spaced from each other.
According to the embodiment of the invention, the adaptive MOFs is designed according to the particle size of the quantum dots to be embedded, so that the pore size of the MOFs is in a proper range, and the quantum dots are all positioned in the pores and are mutually spaced. Meanwhile, the work function of the MOFs material is coordinated, namely the work function is matched with the energy level of other functional layers of the quantum dot light-emitting diode, so that carriers are injected into a metal organic framework layer and then transferred to quantum dots.
In one embodiment, the material of the metal organic frame layer includes Tb-BDC, MCF-62, MCF-63, MAF-2, SHF-6, MIL-88, HKUST-1, MOF-74, MCF-82, ZIF-8, etc., but is not limited thereto.
In the application process, different metal organic framework layers are obtained by selecting proper metal ions and organic ligands, proper acidic ions or molecules are selected to endow MOFs with good proton conductivity, and finally the acidic MOFs and specific quantum dots are compounded for use to obtain the quantum dot film.
What is desired in the embodiments of the present invention is that pores on the surface of the acidic metal organic frame layer are regularly and uniformly distributed, and a proton conduction network formed by the acidic groups and the main body frame covers the entire MOFs layer, and further, the pores on the surface can be arranged in an array manner to obtain an arrayed quantum dot film.
It should be noted that the quantum dots of this embodiment can be completely embedded in the pores, but it is not excluded that the quantum dots can be partially embedded in the pores, and the rest is formed on the surface of the acidic metal organic frame layer in the form of a quantum dot thin film.
According to the specific structure of the quantum dot light-emitting device to be prepared, the thin film can be selectively formed on the substrate or the functional layer, wherein the functional layer can be a hole transport layer or an electron transport layer.
Fig. 1 is a schematic flow chart of a method for preparing a thin film according to an embodiment of the present invention, as shown in the figure, the method includes the steps of:
s11, providing a first raw material solution, wherein the first raw material solution comprises a metal organic framework layer raw material and acidic ions or comprises a metal organic framework layer raw material and acidic molecules;
s12, depositing the first raw material solution on a substrate or a functional layer, and drying to obtain a metal organic framework layer combined with acidic ions or acidic molecules;
s13, providing a second raw material liquid, wherein the second raw material liquid comprises quantum dots;
and S14, depositing the second raw material solution on the metal organic frame layer combined with the acidic ions or acidic molecules, drying, and embedding quantum dots in gaps of the metal organic frame layer to obtain the film.
It is to be understood that the above-mentioned drying process may also be understood as a process of removing the solvent. The conditions of the drying process, such as whether a vacuum environment is present, whether a reduced pressure environment is present, and the operating temperature, are adjusted according to the actual composition of the raw material solution, and the present invention is not particularly limited to these conditions.
And drying the first raw material solution, and curing to form a film so as to form the metal organic frame layer. Wherein the thickness of the metal organic frame layer can be adjusted by adjusting the thickness at the time of deposition (e.g., coating), or the number of coatings. In the embodiment of the present invention, the thickness of the metal organic frame layer may be 10-500nm, for example, 50nm, 100nm, 150nm, 200nm, 250nm, 300nm, 350nm, 400nm, 450nm, 500nm, and the like.
The second raw material solution is dried and cured to form a film, which can be used to form individual quantum dots or quantum dot thin films, and if a quantum dot thin film is formed, the thickness thereof can be 10 to 200nm, for example, 10nm, 20nm, 50nm, 80nm, 100nm, 140nm, 150nm, 180nm, 200nm, and the like. In other words, the quantum dots may be completely embedded in the pores; but also can be partially embedded into the pores, and the other part is formed on the surface of the metal organic framework layer in the form of a quantum dot thin film, wherein the thickness of the quantum dot thin film is 10-200 nm.
Fig. 2 is a schematic flow chart of a method for manufacturing a thin film according to another embodiment of the present invention, as shown in the figure, including the steps of:
s21, providing a first raw material solution, wherein the first raw material solution comprises a metal organic framework layer raw material and acidic ions or comprises a metal organic framework layer raw material and acidic molecules;
s22, providing a second raw material liquid, wherein the second raw material liquid comprises quantum dots;
and S23, mixing the first raw material solution and the second raw material solution, depositing the mixture on a substrate or a functional layer, and drying to obtain the film. The specific operation of the reaction is adaptively adjusted according to actual raw materials, and the quantum dots can be grown in situ in the pores of the metal organic frame layer.
In the embodiment of the invention, two specific implementation methods for loading acidic ions or acidic molecules by using cavities of MOFs are provided: one is to form a MOFs layer and then form an acidic ion or acidic molecular layer on top of the MOFs layer, which will diffuse into the pore cavities of the MOF to form an acidic metal organic framework layer. And the other method is to mix the original solution capable of forming the MOFs layer with acidic ions or acidic molecules, and the mixture of the metal ions, the connecting agent and the expected guest molecules encapsulates the acidic ions or acidic molecules in the MOFs self-assembly synthesis process to form the acidic metal organic framework layer.
The specific implementation manner of bonding the acidic groups on the MOFs main body framework in the embodiment of the invention is that in the process of selecting appropriate metal ions and organic ligands to obtain the metal organic framework layer, the organic ligands contain the acidic groups required by the invention, and the functionality of the acidic groups cannot be damaged in the self-assembly forming process of the MOFs.
The specific implementation manner of obtaining the acidic metal organic framework layer through sulfonation treatment in the embodiment of the invention is to select appropriate metal ions and organic ligands to obtain the metal organic frameworkIn the process of the layer, the organic ligand contains a sulfhydryl ligand or an aromatic ring ligand, and the sulfhydryl ligand (-SH) is oxidized to form-SO after the self-assembly is finished3H, or sulfuric acid esterification treatment is carried out on the aromatic ring ligand to realize sulfonation, and proton conductivity of the sulfonated MOFs layer can be greatly improved.
Referring to fig. 3, fig. 3 is a schematic structural diagram of a quantum dot light emitting diode according to an embodiment of the present invention, and as shown in the figure, the quantum dot light emitting diode includes an anode 1, a quantum dot light emitting layer 2, and a cathode 3, where the quantum dot light emitting layer 2 is disposed between the anode 1 and the cathode 3, and the quantum dot light emitting layer 2 is a thin film according to an embodiment of the present invention.
In one embodiment, the quantum dot light emitting diode may further include a hole function layer disposed between the anode and the quantum dot light emitting layer. Wherein the hole function layer may be selected from one or both of a hole injection layer and a hole transport layer. When the hole function layer is a hole injection layer or a hole transport layer, the hole transport layer is attached to the quantum dot light emitting layer.
In one embodiment, the quantum dot light emitting diode may further include an electronic function layer disposed between the cathode and the quantum dot light emitting layer. Wherein the electron function layer may be selected from one or both of an electron injection layer and an electron transport layer. When the electronic function layer is an electron injection layer or an electron transmission layer, the electron transmission layer is attached to the quantum dot light-emitting layer.
It should be noted that the quantum dot light emitting diode may further include an interface modification layer, and the interface modification layer may be one or more layers selected from an electron blocking layer, a hole blocking layer, an electron injection layer, an electrode modification layer, and an isolation protection layer.
In this embodiment, the quantum dot light emitting diode may be packaged partially, fully or not.
In this embodiment, each layer deposition method may be a chemical method or a physical method, wherein the chemical method includes, but is not limited to, one or more of a chemical vapor deposition method, a continuous ion layer adsorption and reaction method, an anodic oxidation method, an electrolytic deposition method, and a coprecipitation method; the physical method includes, but is not limited to, one or more of spin coating, printing, knife coating, dip coating, dipping, spraying, roll coating, casting, slit coating, bar coating, thermal evaporation, electron beam evaporation, magnetron sputtering, multi-arc ion coating, physical vapor deposition, atomic layer deposition, and pulsed laser deposition.
The invention is further illustrated by the following specific examples.
Example 1
Preparing the MOFs composite quantum dot luminescent film bonded with the acid groups on the main body framework:
providing an acidic metal organic framework [ (CH)3)2NH2][Y(C2O4)2(H2O)]·3H2Raw material liquid of O: mixing Y (NO)3)3·6H2O (3.83g, 0.01mol) and dimethylamine hydrochloride (2.04g, 0.025mol) were dissolved in 50mL of water, and added dropwise to 50mL of an aqueous solution of oxalic acid (2.52g, 0.02mol) and dimethylamine hydrochloride (2.04g, 0.025mol) with stirring to form an acidic metal-organic framework [ (CH) complex3)2NH2][Y(C2O4)2(H2O)]·3H2A raw material liquid of O.
80 μ l of the above raw material solution was dropped on a substrate, rotated at 3000rpm for 40s, and finally baked at 80 ℃ for 30mins to form a 20 nm-thick acidic metal organic frame layer.
Providing a raw material solution of blue light-emitting quantum dots (CdSe/ZnS) with toluene as a solvent and with the concentration of 30mg/ml, dripping 50 mul of the raw material solution on an acidic metal organic frame layer, rotating at the rotating speed of 4000rpm for 30s, and finally baking at 150 ℃ for 15mins to form-NH bonded on a main body framework2The MOFs composite quantum dot luminescent film.
Example 2
Preparing an MOFs pore-cavity loaded benzenesulfonic acid composite quantum dot luminescent film:
60mg of zinc oxide powder was added to 1ml of a formic acid-water solution (formic acid 0.5ml of the solution), and then 0.5ml of ammonia water was added thereto to obtain a clear solution, to form a metal organic framework raw material solution.
80 μ l of the above raw material solution was dropped on a substrate, rotated at 4000rpm for 40 seconds, and then baked at 80 ℃ for 30mins to form a 20nm thick metal organic frame layer.
And (3) dropwise adding 100 mu l of benzenesulfonic acid on the metal organic frame layer, rotating at the rotating speed of 2000rpm for 80s, and then drying at 50 ℃ for 60mins to form the metal organic frame layer with the pore cavity loaded with benzenesulfonic acid.
Providing a raw material solution of red luminescent quantum dots (CdSe/Zne) with toluene as a solvent and the concentration of 30mg/ml, dropwise adding 50 mu l of the raw material solution on an acidic metal organic frame layer, rotating at the rotating speed of 4000rpm for 30s, and finally baking at 150 ℃ for 15mins to form the MOFs pore-supported benzenesulfonic acid composite quantum dot luminescent film.
In summary, the present invention embeds quantum dots in the pore structure of Metal Organic Frame (MOFs) layers, wherein a large amount of acidic ions or molecules are loaded or modified in the MOFs layers. The MOFs loaded or modified with a large number of acidic ions or molecules have good proton conductivity, and are beneficial to the transmission of hole carriers, and the carrier injection imbalance of the traditional quantum dot device is mainly due to a large hole injection potential barrier, so that the improvement of the transmission of the hole carriers can improve the hole and electron injection balance, and finally the performance of the device is improved. In addition, compared with the traditional method for directly forming the quantum dot film, the method has the following advantages: the porous space structure of the MOFs provides ideal attachment sites for quantum dots, and the risk of agglomeration and fluorescence energy resonance transfer (FRET) are greatly reduced when the quantum dots are separated by the framework of the MOFs.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. The thin film is characterized by comprising a metal organic frame layer and quantum dots embedded in pores of the metal organic frame layer, wherein acidic ions or acidic molecules are combined in the metal organic frame layer.
2. The membrane of claim 1, wherein the acidic ions comprise NH4 +、H3O+And HSO4 +One or more of (a).
3. The membrane of claim 1, wherein the acidic molecules comprise one or more of hexanoic acid, benzenesulfonic acid, trifluoromethanesulfonic acid, sulfuric acid, and phosphoric acid.
4. The film of claim 1, wherein the metal organic frame layer comprises one or more of Tb-BDC, MCF-62, MCF-63, MAF-2, SHF-6, MIL-88, HKUST-1, MOF-74, MCF-82, and ZIF-8.
5. The film of claim 1, wherein the quantum dots have a particle size of 2-20nm and the pores have a diameter of 2-30 nm.
6. The film of claim 1, wherein the pores of the metal organic framework layer are bound with the acidic ions or acidic molecules; alternatively, the first and second electrodes may be,
the acidic ions or acidic molecules are bound to the framework of the metal organic framework layer.
7. A method for preparing a film, comprising the steps of:
providing a first raw material solution, wherein the first raw material solution comprises a metal organic framework layer raw material and acidic ions or the first raw material solution comprises a metal organic framework layer raw material and acidic molecules;
depositing the first raw material solution on a substrate or a functional layer, and drying to obtain a metal organic framework layer combined with acidic ions or acidic molecules;
providing a second raw material liquid, wherein the second raw material liquid comprises quantum dots;
and depositing the second raw material solution on the metal organic frame layer combined with the acidic ions or acidic molecules, drying, and embedding quantum dots in gaps of the metal organic frame layer to obtain the film.
8. A method for preparing a film, comprising the steps of:
providing a first raw material solution, wherein the first raw material solution comprises a metal organic framework layer raw material and acidic ions or the first raw material solution comprises a metal organic framework layer raw material and acidic molecules;
providing a second raw material liquid, wherein the second raw material liquid comprises quantum dots;
and mixing the first raw material solution and the second raw material solution, depositing the mixture on a substrate or a functional layer, and drying to obtain the film.
9. A quantum dot light-emitting diode comprising an anode, a quantum dot light-emitting layer and a cathode, wherein the quantum dot light-emitting layer is disposed between the anode and the cathode, and wherein the quantum dot light-emitting layer is the film of any one of claims 1 to 6.
10. The quantum dot light-emitting diode of claim 9, wherein the thin film has a thickness of 10-500 nm.
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| CN109256476A (en) * | 2018-09-19 | 2019-01-22 | 京东方科技集团股份有限公司 | Quantum dot light emitting layer, quantum dot light emitting device and preparation method |
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Application publication date: 20210716 |