CN109817510B - Preparation method and application of thin film, and QLED device - Google Patents
Preparation method and application of thin film, and QLED device Download PDFInfo
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Abstract
The invention discloses a preparation method of a film, application of the film and a QLED device, wherein the preparation method comprises the following steps: mixing a first metal salt solution and a second metal salt solution, adding a first fuel, uniformly mixing to obtain a mixed solution, depositing the mixed solution to form a film, heating to decompose the first fuel and release heat, and promoting the first metal salt and the second metal salt to react to obtain the film; the first fuel is fuel which can generate decomposition reaction when the temperature in the reaction system is above 120 ℃, the first metal is one or more of bivalent metal elements and trivalent metal elements, and the second metal is one or more of trivalent metal elements and tetravalent metal elements. The method utilizes the characteristic that the first fuel can be decomposed at a lower temperature to release a large amount of heat, and promotes the reaction of the metal first metal salt and the metal second metal salt in a solution state at the lower temperature to form the metal oxide film, the film has high compactness and good uniformity, and the problems that the perovskite type metal oxide prepared by the existing method has poor quality and the application of the perovskite type metal oxide in a QLED device is influenced are solved.
Description
Technical Field
The invention relates to the technical field of perovskite type metal oxides, in particular to a preparation method of a thin film, application of the thin film and a QLED device.
Background
The perovskite type metal oxide is a perovskite type material, has extremely stable performance, is applied to a photovoltaic device or a sensor, is an n-type wide band gap semiconductor material, has the characteristic of electron transmission with the band gap of about 3.2 ev, and can be applied to a QLED as an electron transmission layer. However, the current methods for synthesizing the material are high-temperature synthesis or magnetron sputtering methods, which may cause damage to the QD layer, and limit the application of the material in QLED devices.
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 preparation method of a thin film, application of the thin film and a QLED device, and aims to solve the problem that the perovskite type metal oxide prepared by the conventional method is poor in quality and affects the application of the perovskite type metal oxide in the QLED device.
The technical scheme of the invention is as follows:
a method for producing a thin film, comprising the steps of: mixing a first metal salt solution and a second metal salt solution, adding a first fuel, uniformly mixing to obtain a mixed solution, depositing the mixed solution to form a film, heating to decompose the first fuel and release heat, and promoting the first metal salt and the second metal salt to react to obtain the film;
wherein the first fuel is fuel which can generate decomposition reaction when the temperature in the reaction system is above 120 ℃, the first metal is one or more of bivalent metallic elements and trivalent metallic elements, and the second metal is one or more of trivalent metallic elements and tetravalent metallic elements.
The film preparation method is characterized in that the molar ratio of the first metal element of all the first metal salts to the second metal element of all the second metal salts is 1: 1.
The preparation method of the film, wherein the first fuel is acetylacetone.
The preparation method of the film comprises the step of enabling the molar ratio of acetylacetone to the first metal element to be 2: 1-7: 1.
The preparation method of the film comprises the step of heating the film at the temperature of 120-140 ℃.
The preparation method of the thin film comprises the step of adding a second fuel into the mixed solution before the mixed solution is formed into the film, wherein the second fuel is a fuel which can generate decomposition reaction when the temperature in a reaction system is more than 150 ℃.
The preparation method of the film comprises the step of mixing the first fuel and the second fuel, wherein the first fuel is one or more of urea, glycine, cane sugar, glucose and citric acid.
The preparation method of the perovskite metal oxide comprises the step of enabling the molar ratio of the second fuel to the first metal element to be 0.8: 1-1.2: 1.
The preparation method of the thin film comprises the following steps of preparing a first metal, preparing a second metal, and preparing a thin film, wherein the first metal is one or more of Ca, Sr, Ba, La and Sc, and the second metal is one or more of Ti, Zr, Sn, Fe, Al and Ga.
The application of the film preparation method is to provide a substrate, and deposit the film prepared by the method on the substrate to form an electron transport layer.
A QLED device comprising a first electrode, an electron transport layer, a light emitting layer and a second electrode, wherein the electron transport layer is made of a thin film prepared as described above.
Has the advantages that: the invention utilizes the first fuel to decompose and release a large amount of heat at a lower temperature, promotes the first metal salt and the second metal salt to react to generate the metal oxide film, has high compactness and good uniformity, can be widely applied to an electron transmission layer in a QLED device, provides the electron transmission stability of the device, and solves the problems that the perovskite type metal oxide prepared by the existing method has poor quality and influences the application of the perovskite type metal oxide in the QLED device.
Drawings
FIG. 1 is a flow chart of a preferred embodiment of the method for preparing a thin film according to the present invention.
Fig. 2 is a schematic structural diagram of a forward-mounted QLED device without a hole injection layer and a hole transport layer according to the present invention.
Fig. 3 is a schematic structural diagram of a flip-chip QLED device without a hole injection layer and a hole transport layer according to the present invention.
Fig. 4 is a schematic structural diagram of a forward-mounted QLED device including a hole injection layer and a hole transport layer according to the present invention.
Fig. 5 is a schematic structural diagram of a flip-chip QLED device including a hole injection layer and a hole transport layer according to the present invention.
Fig. 6 is a schematic structural diagram of a QLED device in embodiment 6 of the present invention.
Detailed Description
The invention provides a preparation method of a film, application of the film and a QLED device, 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 preparation method of the film disclosed by the invention is shown in figure 1 and comprises the following steps:
s1, mixing the first metal salt solution and the second metal salt solution, adding the first fuel, and uniformly mixing to obtain a mixed solution;
and S2, depositing the mixed solution to form a film, heating to decompose the first fuel and release heat, and promoting the reaction of the first metal salt and the second metal salt to obtain the film.
The first fuel is fuel which can generate decomposition reaction when the temperature in the reaction system is above 120 ℃, the first metal is one or more of bivalent metal elements and trivalent metal elements, and the second metal is one or more of trivalent metal elements and tetravalent metal elements. For example, the first metal is one or more of Ca, Sr, Ba, La and Sc, and the second metal is one or more of Ti, Zr, Sn, Fe, Al and Ga.
According to the invention, a first metal salt of a metal element and a second metal salt of the metal element are mixed together in a solution form, then a first fuel is added to form a mixed solution, the mixed solution is preheated after being formed into a film until the first fuel is decomposed to release heat, the partial surface of the mixed solution is uniformly heated by utilizing the characteristic that the first fuel can be combusted and decomposed at a lower temperature to generate a large amount of heat, the solvent of the mixed solution is evaporated, then the first metal salt of the metal element and the second metal salt of the metal element are promoted to carry out an oxidation reaction, and finally a metal oxide film is generated.
The first metal salt solution is a 2-methoxyethanol solution of a first metal salt or a first metal salt aqueous solution, the second metal salt solution can also be a 2-methoxyethanol solution of a second metal salt or a second metal salt aqueous solution, and the first metal salt and the second metal salt in a solution state participate in a reaction so as to form a sufficiently uniformly dispersed state.
Preferably, the molar ratio of the first metal element in all of the first metal salts to the second metal element in all of the second metal salts is 1:1, such that the first metal salts to the second metal saltsAfter the oxidation of the bimetallic salt, the perovskite-type metal oxide can be just obtained, no matter whether the first metal salt or the second metal salt is a metal element salt or a plurality of metal element salts, no matter whether the first metal element exists in the first metal salt in a positive divalent state or a positive trivalent state, and whether the second metal element exists in the second metal salt in a positive trivalent state or a positive tetravalent state, the molar ratio of the first metal element to the second metal element is 1: and (1) sufficiently reacting the two salts to form the perovskite-structured oxide, and not generating other metal compound impurities, for example, when the first metal salt and the second metal salt are both the two salts, the first metal a salt, the first metal b salt, the second metal a salt and the second metal b salt are respectively, wherein the molar ratio of (the first metal a salt + the first metal b salt) to (the second metal a salt + the second metal b salt) is 1: 1. The metal oxide obtained at this time is a perovskite-type metal oxide ABOxWherein A is the first metal element, B is the second metal element, and x is 2.5-3.5.
The first fuel is fuel which can generate decomposition reaction when the temperature in the reaction system is above 120 ℃, and the first fuel is heated to above 120 ℃, such as 120 ℃, 125 ℃, 140 ℃ and 180 ℃, so that the first fuel is decomposed to release heat, and a large amount of heat is released by decomposition, and the first metal salt and the second metal salt are promoted to react to generate the metal oxide film. Preferably, the heating temperature is 120-140 ℃, because the first fuel is mixed with the first metal salt and the second metal salt in solution, the reaction of the first metal salt and the second metal salt is directly carried out on a molecular layer, the reaction can be carried out only at a relatively low exothermic temperature, and the preparation of the metal oxide can be realized in a relatively low temperature environment, which can avoid the problem of damage to devices caused by high-temperature annealing film formation and the like in practical application.
The first fuel can be acetylacetone, and when the temperature in the reaction system reaches 125 ℃, the acetylacetone can be decomposed to release heat, preferably, the molar ratio of the acetylacetone to the first metal salt is 2: 1-7: 1, a small amount of acetylacetone cannot generate enough heat, and excessive acetylacetone can cause a large amount of gas to influence the uniform distribution of the generated metal oxide, and finally, the compactness uniformity of a film prepared by the metal oxide is influenced, and the quality of the product is influenced.
Preferably, the method further comprises a step of adding a second fuel into the mixed solution before the mixed solution is formed into a membrane, wherein the second fuel is a fuel which can generate a decomposition reaction when the temperature in the reaction system is more than 150 ℃. The second fuel is used as auxiliary fuel, the auxiliary fuel has high heat release condition, can absorb part of heat released by the first fuel such as acetylacetone and the like, after reaching a certain temperature, the auxiliary fuel releases heat (the auxiliary fuel releases heat more than the first fuel such as acetylacetone and the like), the first fuel is ignited through a lower temperature, the heat released by the first fuel can promote the reaction to occur, and the second fuel can be ignited, the second fuel absorbs part of heat released by the first fuel, and the gas formed by the sudden heat release of the first fuel can be prevented from influencing the uniformity and the compactness of the final film; after the second fuel absorbs heat and reaches the temperature at which the decomposition reaction can occur, the second fuel can generate the decomposition reaction and continuously emit more heat, thereby providing a longer heat release interval. The heat given off by the mixed fuel promotes the precursor film of the metal oxide to react to form a film.
The second fuel can be a compound mainly containing C/H/O/N or containing C/H/O, wherein the compound can be dissolved in aqueous solution or 2-MEA solution, the pyrolysis temperature of the compound is lower than 350 ℃, and the compound is heated to decompose and generate CO2Or H2O or N2Or other oxides of nitrogen, and these compounds are easy to use and store at normal temperature, and the reaction is not explosive. For example, the second fuel is one or more of urea, glycine, sucrose, glucose, and citric acid. Wherein, in the reaction system, the temperature for starting the decomposition reaction of urea is 150 ℃, the temperature for starting the decomposition reaction of glycine is 150 ℃, the temperature for starting the decomposition reaction of sucrose is 200 ℃, the temperature for starting the decomposition reaction of glucose is 300 ℃, and the temperature for starting the decomposition reaction of citric acid is 175 ℃. When the temperature in the reaction system reaches or exceeds the second fuelAt the decomposition reaction temperature, the second fuel undergoes a decomposition reaction, releasing heat and promoting the reaction of the first metal salt and the second metal salt.
Further, the molar ratio of the second fuel to the first metal element in the first metal salt is 0.8: 1-1.2: 1. Too little second fuel cannot be matched with first fuel such as acetylacetone to relieve the decomposition heat release of the first fuel, a longer heat release temperature interval cannot be formed, the metal salts of the first metal and the second metal cannot be promoted to be converted into oxides, and too much second fuel still can cause a large amount of gas to be released, and finally the compactness uniformity of the film is influenced.
In the preparation method of the film, the first metal salt can be nitrate, acetate or chloride of the first metal, and similarly, the second metal salt can be nitrate, acetate or chloride of the second metal. It should be noted that, when the first metal salt or the second metal salt is a chloride salt, the step S2 needs to be performed in an aerobic environment to ensure that the first metal element and the second metal element are sufficiently oxidized to form a metal oxide.
The invention also provides application of the film preparation method, wherein a substrate is provided, the film prepared by the method is deposited on the substrate, namely an electron transport layer is formed, then a light-emitting layer is deposited on the electron transport layer, and then a second electrode is deposited on the light-emitting layer. Specifically, the mixed solution prepared by the method is deposited on a substrate, aged for 4-48h, prepared into a film by a solution method, and then annealed (140-.
The invention also provides a QLED device, and the QLED device can be divided into a QLED device with a forward mounting structure and a QLED device with an inverted mounting structure according to different light-emitting types of the QLED device.
As a specific example, when the QLED device is a QLED device of a forward mounting structure, as shown in fig. 2, the QLED device includes an anode 100, a light emitting layer 400 deposited on the anode 100, an electron transport layer 500 deposited on the light emitting layer 400, and a cathode 600 deposited on the electron transport layer 500, wherein the electron transport layer 500 is made of a thin film prepared by the above-mentioned method, the stability of the QLED device can be effectively improved, and the electrical properties of the QLED device can be ensured.
As another embodiment, when the QLED device is a flip-chip QLED device, as shown in fig. 3, the QLED device includes a cathode 600, an electron transport layer 500, a light emitting layer 400, and an anode 100, which are sequentially stacked from bottom to top.
As a preferred embodiment, when the QLED device is a QLED device of a forward-mounted structure, as shown in fig. 4, the QLED device may include an anode 100, a hole injection layer 200 deposited on the anode 100, a hole transport layer 300 deposited on the hole injection layer 200, a light emitting layer 400 deposited on the hole transport layer 300, an electron transport layer 500 deposited on the light emitting layer 400, and a cathode 600 deposited on the electron transport layer 500, wherein: the light emitting layer 400 may be a common quantum dot QD, such as at least one of common red, green, blue and yellow light quantum dots and infrared and ultraviolet light quantum dots; the hole transport layer 300 may be, but is not limited to, Poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine) (TFB), Polyvinylcarbazole (PVK), Poly (N, N ' bis (4-butylphenyl) -N, N ' -bis (phenyl) benzidine) (Poly-TPD), Poly (9, 9-dioctylfluorene-CO-bis-N, N-phenyl-1, 4-Phenylenediamine) (PFB), 4', 4 "-tris (carbazol-9-yl) triphenylamine (TCTA), 4' -bis (9-Carbazol) Biphenyl (CBP), N ' -diphenyl-N, N ' -bis (3-methylphenyl) -1,1 ' -biphenyl-4, one or more of 4' -diamine (TPD), N ' -diphenyl-N, N ' - (1-naphthyl) -1,1 ' -biphenyl-4, 4' -diamine (NPB), preferably CBP; the hole injection layer 200 may be made of molybdenum oxide, tungsten oxide, vanadium oxide, copper oxide, or 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-Hexaazatriphenylene (HATCN), poly (3, 4-ethylenedioxythiophene) -polystyrenesulfonic acid (PEDOT: PSS), etc., preferably using MoO 3; the anode can be Ag, Al, Cu, Au or alloy electrode, and is preferably Ag electrode.
As another preferred embodiment, when the QLED device is a flip-chip-structured QLED device, as shown in fig. 5, the QLED device may include a cathode 600, an electron transport layer 500 deposited on the cathode 600, an emission layer 400 deposited on the electron transport layer 500, a hole transport layer 300 deposited on the emission layer 400, a hole injection layer 200 deposited on the hole transport layer 300, and an anode 100 deposited on the hole injection layer 200, wherein: the light emitting layer 400 may be a common quantum dot QD, such as at least one of common red, green, blue and yellow light quantum dots and infrared and ultraviolet light quantum dots; the hole transport layer 300 may be, but is not limited to, Poly (9, 9-dioctylfluorene-CO-N- (4-butylphenyl) diphenylamine) (TFB), Polyvinylcarbazole (PVK), Poly (N, N ' bis (4-butylphenyl) -N, N ' -bis (phenyl) benzidine) (Poly-TPD), Poly (9, 9-dioctylfluorene-CO-bis-N, N-phenyl-1, 4-Phenylenediamine) (PFB), 4', 4 "-tris (carbazol-9-yl) triphenylamine (TCTA), 4' -bis (9-Carbazol) Biphenyl (CBP), N ' -diphenyl-N, N ' -bis (3-methylphenyl) -1,1 ' -biphenyl-4, one or more of 4' -diamine (TPD), N ' -diphenyl-N, N ' - (1-naphthyl) -1,1 ' -biphenyl-4, 4' -diamine (NPB), preferably CBP; the hole injection layer 200 may be made of molybdenum oxide, tungsten oxide, vanadium oxide, copper oxide, or 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-Hexaazatriphenylene (HATCN), poly (3, 4-ethylenedioxythiophene) -polystyrenesulfonic acid (PEDOT: PSS), etc., preferably using MoO 3; the anode can be Ag, Al, Cu, Au or alloy electrode, and is preferably Ag electrode.
It should be noted that the invention is not limited to the QLED device with the above structure, and may further include an interface functional layer or an interface modification layer, including but not limited to one or more of an electron blocking layer, a hole blocking layer, an electrode modification layer, and an isolation protection layer. The QLED devices described herein may be partially encapsulated, fully encapsulated, or unpackaged.
The present invention will be described in detail below with reference to examples.
Example 1
1mmol of Ba (NO)3)2With 1mmol of SnCl4·5H2O was dissolved in 2-methyl ethanol solution (5 ml), and after mixing, 3mmol of acetylacetone and 1mmol of acetylacetone were addedGlycine is evenly stirred and then aged for 4 hours to obtain BaSnO3Then forming a film by using the precursor solution, and annealing at 130 ℃ for 30min to obtain BaSnO3A film.
Example 2
Adding 1mmol of La (NO)3)3And 1mmol Ga (NO)3)3Dissolving in 5ml water solution, mixing, adding 4mmol acetylacetone and 1.2mmol glycine, stirring, aging for 8 hr to obtain LaGaO3Then forming a film of the precursor solution, and annealing at 150 ℃ for 60min to obtain LaGaO3A film.
Example 3
Adding 1mmol Sr (NO)3)2With 1mmol of SnCl4·5H2Dissolving O in 5ml of 2-methyl ethanol solution, mixing, adding 3mmol of acetylacetone and 1mmol of urea, stirring uniformly, and aging for 8h to obtain SrSnO3Then forming a film, and annealing at 170 ℃ for 45min to obtain SrSnO3A film.
Example 4
0.05 mmol of La (NO)3)3With 0.95 mmol of Ba (NO)3)2And 1mmol of SnCl4·5H2Dissolving O in 5ml of 2-methyl ethanol solution, mixing, adding 4mmol of acetylacetone and 1.2mmol of sucrose, stirring uniformly, and aging for 8h to obtain La0.05Ba0.95SnO3.025Then forming a film of the precursor solution, and annealing at 200 ℃ for 45min to obtain La0.05Ba0.95SnO3.025A film.
Example 5
Adding 0.5 mmol of Sc (NO)3)3With 0.5 mmol of Ba (NO)3)2And 1mmol TiCl4·5H2Dissolving O in 5ml of 2-methyl ethanol solution, mixing, adding 7mmol of acetylacetone, stirring uniformly, and aging for 8h to obtain Sc0.5Ba0.5SnO3.25Then forming a film of the precursor solution, and annealing at 140 ℃ for 45min to obtain Sc0.5Ba0.5SnO3.25A film.
Example 6
This example provides a QLED device, as shown in FIG. 6, by depositing a layer of BaSnO prepared in example 1 on a Substrate (Substrate) containing a bottom electrode ITO3Annealing the precursor solution for 1h at the rotating speed of 3000rpm and the temperature of 150 ℃ to form an electron transport layer ETL with the thickness of 20 nm; then transferring the material to a glove box, and then depositing a luminescent layer with the thickness of 20 nm;
then transferring the light emitting layer to a glove box, and then depositing a hole transport layer on the light emitting layer, wherein the hole transport layer is CBP, and the thickness of the hole transport layer is 30 nm;
subsequently depositing a hole injection layer on the hole transport layer, the layer using MoO3The thickness is 10 nm;
and finally, depositing a top electrode on the hole injection layer, wherein the top electrode is an Ag electrode, the thickness of the layer is 100nm, and then simply packaging the device. The obtained QLED device has stable electron transmission performance and excellent light emitting effect.
In summary, the invention provides a preparation method of a thin film, an application of the thin film and a QLED device. The invention utilizes the characteristic that the first fuel can release a large amount of heat at a lower temperature, and simultaneously is matched with the second fuel, so that a longer heat release interval is formed in the reaction process, and the influence of gas formed by sudden heat release of the first fuel on the uniformity and compactness of the final film can be prevented; the mixed fuel formed by the first fuel and the second fuel can promote the precursor film of the metal oxide to react to form a film under the action of heat emitted by the mixed fuel at a lower temperature, the formed film has high compactness and good uniformity, can be widely applied to an electron transport layer in a QLED device, provides the electron transport stability of the device, and solves the problems that the perovskite type metal oxide prepared by the existing method has poor quality and influences the application of the perovskite type metal oxide in the QLED device.
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. A preparation method of a thin film applied to a QLED device, wherein the QLED device comprises a first electrode, an electron transport layer, a luminescent layer and a second electrode, the electron transport layer is made of the thin film, and the preparation method of the thin film comprises the following steps:
mixing a first metal salt solution and a second metal salt solution, adding a first fuel, uniformly mixing to obtain a mixed solution, depositing the mixed solution to form a film, heating to decompose the first fuel and release heat, and promoting the first metal salt and the second metal salt to react to obtain the film;
the first fuel is fuel which can generate decomposition reaction at the temperature of more than 120 ℃ in the reaction system, the first metal is one or more of bivalent metal elements and trivalent metal elements, and the second metal is one or more of trivalent metal elements and tetravalent metal elements.
2. The method for producing a thin film according to claim 1, wherein a molar ratio of the first metal element of all the first metal salts to the second metal element of all the second metal salts is 1: 1.
3. The method of claim 1, wherein the first fuel is acetylacetone.
4. The method of claim 3, wherein the molar ratio of acetylacetone to the first metal element is 2:1 to 7: 1.
5. The method as claimed in claim 1, wherein the heating temperature is 120-140 ℃.
6. The method of claim 1, further comprising a step of adding a second fuel to the mixed solution before the mixed solution is formed into a film, wherein the second fuel is a fuel that can undergo a decomposition reaction at a temperature of 150 ℃ or higher in the reaction system.
7. The method for preparing a membrane according to claim 6, wherein the second fuel is one or more of urea, glycine, sucrose, glucose and citric acid.
8. The method of claim 7, wherein the molar ratio of the second fuel to the first metal element is 0.8:1 to 1.2: 1.
9. The method of claim 1, wherein the first metal is one or more of Ca, Sr, Ba, La, and Sc, and the second metal is one or more of Ti, Zr, Sn, Fe, Al, and Ga.
10. A QLED device comprising a first electrode, an electron transport layer, a light emitting layer and a second electrode, wherein the electron transport layer is made from a thin film prepared by the method of any one of claims 1 to 9.
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