CN116437691A - Composite material, film, electroluminescent device and display device - Google Patents

Composite material, film, electroluminescent device and display device Download PDF

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CN116437691A
CN116437691A CN202111658491.5A CN202111658491A CN116437691A CN 116437691 A CN116437691 A CN 116437691A CN 202111658491 A CN202111658491 A CN 202111658491A CN 116437691 A CN116437691 A CN 116437691A
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ligand
composite material
metal oxide
nanoparticles
amino
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马兴远
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TCL Technology Group Co Ltd
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TCL Technology Group Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The application discloses a composite material, which comprises metal oxide nano particles, and a first ligand and a second ligand which are connected to the surfaces of the metal oxide nano particles, wherein the first ligand is an organic ligand with a main chain carbon number of more than or equal to 2, and the second ligand is an inorganic ligand. The first ligand can passivate surface defects of the metal oxide nanoparticles, adjust the solubility of the metal oxide nanoparticles and ensure the stability of a metal oxide nanoparticle solution; the second ligand can passivate the defects of the surface of the metal oxide nano-particles, which are not passivated by the first ligand, so that the dangling bonds of the surface of the metal oxide nano-particles are further reduced, the surface defects of the metal oxide nano-particles are further passivated, and the electrical property stability of the metal oxide nano-particles is further improved. The application also discloses a film, an electroluminescent device and a display device comprising the composite material.

Description

Composite material, film, electroluminescent device and display device
Technical Field
The application relates to the technical field of display, in particular to a composite material, a film comprising the composite material, an electroluminescent device comprising the film and a display device comprising the electroluminescent device.
Background
The quantum dot electroluminescent device (QLED device) has the advantages of adjustable wavelength, high color saturation, high material stability, low preparation cost and the like, and becomes the best candidate of the next generation display technology. Through development of approximately twenty years, the external quantum efficiency of the QLED device has been improved from 0.01% to more than 20%.
The QLED device mainly comprises an anode, a hole injection layer, a hole transport layer, a light emitting layer, an electron transport layer, an electron injection layer and a cathode. Under the action of an electric field, holes generated by an anode and electrons generated by a cathode of the QLED device move, are respectively injected into the hole transmission layer and the electron transmission layer and finally migrate to the light-emitting layer, and when the hole transmission layer and the electron transmission layer meet at the light-emitting layer, energy excitons are generated, so that light-emitting molecules are excited to finally generate visible light.
In a QLED device, the electron transport layer generally uses metal oxide nanoparticles, mainly because the electron mobility of the metal oxide nanoparticles is higher, the metal oxide nanoparticles are wide-bandgap inorganic semiconductor materials in the deep ultraviolet region, and can play a good role in blocking holes while ensuring electron transport, limit excitons to the light emitting layer, and improve the light emitting efficiency of the device. However, the stability of the metal oxide nanoparticles themselves is poor, resulting in poor stability of the QLED device.
Disclosure of Invention
In view of this, the present application provides a composite material, which aims to solve the problem that the existing composite material for an electron transport layer of an electroluminescent device is poor in stability.
The embodiment of the application is realized in such a way that the composite material comprises metal oxide nano particles, and a first ligand and a second ligand which are connected to the surfaces of the metal oxide nano particles, wherein the first ligand is an organic ligand with a main chain carbon number of more than or equal to 2, and the second ligand is an inorganic ligand.
Alternatively, in some embodiments of the present application, the molar amount of the first ligand is 50 to 80% of the total molar amount of the first ligand and the second ligand.
Alternatively, in some embodiments of the present application, the metal oxide nanoparticles are selected from the group consisting of ZnO nanoparticles, mg-dopedZinc oxide nanoparticles, al-doped zinc oxide nanoparticles, in-doped zinc oxide nanoparticles, mg-doped and Li-doped zinc oxide nanoparticles, mg-doped and Al-doped zinc oxide nanoparticles, mg-doped and In-doped zinc oxide nanoparticles, ga-doped and In-doped zinc oxide nanoparticles, tiO 2 Nanoparticles, snO 2 Nanoparticles and In 2 O 3 At least one of the nanoparticles.
Alternatively, in some embodiments of the present application, the metal oxide nanoparticles have a particle size in the range of 2 to 10nm.
Optionally, in some embodiments of the present application, the number of backbone carbon atoms of the first ligand is 3 or more and 18 or less.
Optionally, in some embodiments of the present application, the first ligand is selected from at least one of a thiol, an amino alcohol, and an alkylamine.
Alternatively, in some embodiments of the present application, the mercaptoalcohol is selected from at least one of mercaptobutanol, mercaptoethanol, mercaptopropanol, mercaptopentanol, mercaptohexanol, mercaptoheptanol, and mercaptododecanol;
the mercaptan is at least one selected from ethanethiol, propanethiol, butanethiol, pentanethiol, hexanethiol, dodecanethiol and octadecanethiol;
the amino alcohol is at least one selected from amino butanol, amino ethanol, amino propanol, amino pentanol, amino hexanol, amino heptanol and amino octanol;
the alkylamine is at least one selected from ethylamine, propylamine, butylamine, pentylamine, hexylamine, heptylamine, octylamine, dodecylamine and octadecylamine.
Alternatively, in some embodiments of the present application, the second ligand is a halogen ligand selected from Cl - 、Br - 、I - F (F) - At least one of them.
Alternatively, in some embodiments of the present application, the first ligand is selected from at least one of a thiol or a thiol, and the second ligand is selected from Cl - 、Br - I - At least one of (a)。
Alternatively, in some embodiments of the present application, the first ligand is selected from at least one of an amino alcohol or an alkylamine, and the second ligand is selected from F - 。
Alternatively, in some embodiments of the present application, the first ligand is selected from at least one of an amino alcohol or an alkylamine, and the second ligand is selected from Cl - 、Br - I - At least one of them.
Optionally, in some embodiments of the present application, the first ligand to second ligand molar ratio ranges from (1:1) to (2:1).
Correspondingly, the embodiment of the application also provides a film, wherein the film comprises the composite material.
Correspondingly, the embodiment of the application also provides an electroluminescent device, which comprises an anode, a luminescent layer, an electron transport layer and a cathode which are arranged in a stacked manner, wherein the electron transport layer comprises the composite material.
Optionally, in some embodiments of the present application, the light-emitting layer is a quantum dot light-emitting layer, a material of the quantum dot light-emitting layer is at least one of a single-structure quantum dot and a core-shell structure quantum dot, a material of a core of the single-structure quantum dot, a material of a core of the core-shell structure quantum dot, and a material of a shell of the core-shell structure quantum dot are at least one of a group II-VI compound, a group III-V compound, and a group I-III-VI compound, and the group II-VI compound is at least one of CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeTe and CdZnSTe; the III-V compound is at least one selected from InP, inXs, gxP, gxXs, gxSb, xlN, xlP, inXsP, inNP, inNSb, gxXlNP and InXlnP; the I-III-VI compound is selected from CuInS 2 、CuInSe 2 AgInS 2 At least one of them.
Correspondingly, the embodiment of the application also provides a display device, which comprises the electroluminescent device.
The composite material comprises metal oxide nanoparticles, and a first ligand and a second ligand which are connected to the surfaces of the metal oxide nanoparticles, wherein the first ligand is an organic ligand with a main chain carbon number of more than or equal to 2, and has a long-chain structure relative to the second ligand, so that surface defects of the metal oxide nanoparticles can be passivated, the solubility of the metal oxide nanoparticles can be regulated, the stability of a metal oxide nanoparticle solution is ensured, the second ligand has a short-chain structure relative to the first ligand, and defects of the surfaces of the metal oxide nanoparticles, which are not passivated by the first ligand, can be passivated, so that dangling bonds of the surfaces of the metal oxide nanoparticles are further reduced, the surface defects of the metal oxide nanoparticles are further passivated, and the electrical performance stability of the metal oxide nanoparticles is further improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic structural diagram of an electroluminescent device according to an embodiment of the present application;
fig. 2 is a schematic structural diagram of another electroluminescent device according to an embodiment of the present application.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all, of the embodiments of the present application. All other embodiments, based on the embodiments herein, which are obtained by a person skilled in the art without making any inventive effort, are intended to be within the scope of the present application. Furthermore, it should be understood that the detailed description is presented herein for purposes of illustration and explanation only and is not intended to limit the present application.
In this application, unless otherwise indicated, terms of orientation such as "upper" and "lower" are used to generally refer to the upper and lower positions of the device in actual use or operation, and specifically the orientation of the drawing figures; while "inner" and "outer" are for the outline of the device. In addition, in the description of the present application, the term "comprising" means "including but not limited to", and the term "selected from" means "selected from but not limited to". The terms first, second, third and the like are used merely as labels, and do not impose numerical requirements or on the order of construction. The term "plurality" means "two or more".
Various embodiments of the present application may exist in a range format; it should be understood that the description in a range format is merely for convenience and brevity and should not be interpreted as a rigid limitation on the scope of the application. It is therefore to be understood that the range description has specifically disclosed all possible sub-ranges and individual values within that range. For example, it should be considered that a description of a range from 1 to 6 has specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5, and 6, wherever applicable. In addition, whenever a numerical range is referred to herein, it is meant to include any reference number (fractional or integer) within the indicated range.
The embodiment of the application provides a composite material which is mainly used for preparing an electron transport layer of an electroluminescent device, wherein the composite material comprises metal oxide nano particles, and a first ligand and a second ligand which are connected to the surfaces of the metal oxide nano particles. The first ligand is an organic ligand with the main chain carbon number being more than or equal to 2, in other words, the first ligand is a long-chain ligand; the second ligand is an inorganic ligand, in other words, the second ligand is a short chain ligand.
The first ligand is a long-chain ligand, has a long-chain structure relative to the second ligand, can passivate surface defects of the metal oxide nanoparticles, adjust the solubility of the metal oxide nanoparticles, and ensure the stability of the metal oxide nanoparticle solution. The second ligand is a short-chain ligand, has a short-chain structure relative to the first ligand, and can passivate the defects of the surface of the metal oxide nanoparticles, which are not passivated by the first ligand, so that the dangling bonds of the surface of the metal oxide nanoparticles are further reduced, the surface defects of the metal oxide nanoparticles are further passivated, and the electrical property stability of the metal oxide nanoparticles is further improved.
In the composite material, the molar quantity of the first ligand is 50-80% of the total molar quantity of the first ligand and the second ligand, and correspondingly, the molar quantity of the second ligand is 20-50% of the total molar quantity of the first ligand and the second ligand. Within the range, the defects on the surfaces of the metal oxide particles can be sufficiently passivated by the first ligand and the second ligand, so that the metal oxide particles have fewer surface defects; but also can avoid the problem of poor solubility of the composite material in the solvent caused by excessive content of the second ligand.
The metal oxide nanoparticles may be selected from, but not limited to, znO nanoparticles, MZO (Mg-doped zinc oxide) nanoparticles, AZO (Al-doped zinc oxide) nanoparticles, IZO (In-doped zinc oxide) nanoparticles, MLZO (Mg-doped, li zinc oxide) nanoparticles, MAZO (Mg-doped, al-doped zinc oxide) nanoparticles, MIZO (Mg-doped, in-doped zinc oxide) nanoparticles, GZO (Ga-doped zinc oxide) nanoparticles, IGZO (Ga-doped, in-doped zinc oxide) nanoparticles, tiO 2 Nanoparticles, snO 2 Nanoparticles, in 2 O 3 At least one of the nanoparticles.
The metal oxide nanoparticles may have a particle size range of 2 to 20nm. In some embodiments, the metal oxide nanoparticles may have a particle size in the range of 2 to 10nm. In the particle size range, the metal oxide nanoparticles have good solubility, conductivity and stability.
In some embodiments, the first ligand has a backbone carbon number of 2 or more and 20 or less. Further, in some embodiments, the first ligand has a backbone carbon number of 3 or more and 18 or less. As an example, the number of main chain carbon atoms of the first ligand may be 3, 4, 5, 6, 7, 8, etc.
The first part is provided withThe body may be selected from, but is not limited to, at least one of thiol, amino alcohol, alkylamine. Wherein the thiol alcohol refers to a substance containing both thiol (-SH) and hydroxyl (-OH), and the amino alcohol refers to a substance containing both amino (-NH) 2 ) And an alcoholic hydroxyl group. Thiol groups are respectively arranged in thiol and mercaptan, amino groups are respectively arranged in amino alcohol and alkylamine, and the thiol groups and amino groups have strong binding force with the metal oxide nano particles, are not easy to fall off, are favorable for improving the stability of the metal oxide nano particles, and enable the metal oxide nano particles to have good solubility in an organic solvent.
The thiol may be selected from, but is not limited to, at least one of thiol butanol, thiol ethanol, thiol propanol, thiol pentanol, thiol hexanol, thiol heptanol, and thiol dodecanol.
The thiol may be at least one selected from, but not limited to, ethanethiol, propanethiol, butanethiol, pentanethiol, hexanethiol, dodecanethiol, and octadecanethiol.
The amino alcohol may be selected from at least one of, but not limited to, amino butanol, amino ethanol, amino propanol, amino pentanol, amino hexanol, amino heptanol, and amino octanol.
The alkylamine may be at least one selected from, but not limited to, ethylamine, propylamine, butylamine, pentylamine, hexylamine, heptylamine, octylamine, dodecylamine, and octadecylamine.
In some embodiments, the second ligand may be a halogen ligand, which may be selected from, but is not limited to, cl - 、Br - 、I - F (F) - At least one of them. The halogen ligand and the metal oxide nano-particles have stronger binding force and are not easy to fall off, so that the metal oxide nano-particles have better stability.
In one embodiment, the first ligand in the composite material is selected from at least one of thiol or thiol, and the second ligand is selected from Cl - 、Br - I - At least one of them. Second ligand Cl - 、Br - I - The method has stronger electron withdrawing capability, can effectively reduce the energy level of the metal oxide nano-particles, and the first ligand mercapto alcohol and the mercaptan can not greatly influence the energy level of the metal oxide nano-particles. In this way, the metal oxide nanoparticles in the composite material of the present embodiment may have a lower energy level, that is, the energy level of the metal oxide nanoparticles in the composite material of the present embodiment may be lower than the energy level of the metal oxide nanoparticles not including the first ligand and the second ligand, in other words, the binding of the first ligand and the second ligand in the present embodiment may cause the energy level of the composite material of the present embodiment to be lower than the energy level of the metal oxide nanoparticles not including the first ligand and the second ligand in the present embodiment. When the composite material of the embodiment is used for an electron transport layer of a quantum dot electroluminescent device, electrons are advantageously injected into the electron transport layer from a cathode. In addition, when the light-emitting layer of the electroluminescent device comprises quantum dots with lower energy levels, the composite material is contained in the electron transport layer, so that energy level matching between the electron transport layer and the light-emitting layer is facilitated, holes can be effectively prevented from being injected into the electron transport layer from the light-emitting layer, electrons are conveniently injected into the electron transport layer from the cathode, and the electroluminescent device has higher luminous efficiency and longer service life. In at least one embodiment, the lower energy quantum dots are InP-based quantum dots.
In one embodiment, the first ligand in the composite material is selected from at least one of amino alcohol or alkylamine, and the second ligand is selected from F - . The amino group in the first ligand has stronger electron donating ability, so that the energy level of the metal oxide nano particles can be effectively improved; and the second ligand F - The atomic volume is small, the negative dipole moment is small, and the energy level of the metal oxide nano particles cannot be greatly influenced. In this way, the metal oxide nanoparticles in the composite material according to the present embodiment can have a higher energy level, i.e., the energy level of the metal oxide nanoparticles in the composite material according to the present embodiment can be made to be higher than that of the metal oxide nanoparticles not including the first metal oxide nanoparticles according to the present embodimentThe energy levels of the metal oxide nanoparticles of the ligand and the second ligand are higher, in other words, the binding of the first ligand and the second ligand in this embodiment may make the energy level of the composite material in this embodiment higher than the energy level of the metal oxide nanoparticles not including the first ligand and the second ligand in this embodiment. When the light-emitting layer of the electroluminescent device comprises quantum dots with higher energy levels, the electron transport layer is made of the composite material disclosed by the embodiment, so that energy level matching between the electron transport layer and the light-emitting layer is facilitated, electrons are facilitated to be injected into the light-emitting layer from the electron transport layer, holes can be effectively prevented from being injected into the electron transport layer from the light-emitting layer, and the electroluminescent device has higher luminous efficiency and longer service life. In at least one embodiment, the quantum dot with higher energy level is a CdZnSe single quantum dot or a core-shell structure quantum dot with CdZnSe as a core.
In one embodiment, the first ligand in the composite material is selected from at least one of amino alcohol or alkylamine, and the second ligand is selected from Cl - 、Br - I - At least one of them. The amino group in the first ligand can effectively improve the energy level of the metal oxide nano-particles, and the second ligand Cl - 、Br - I - The energy level of the metal oxide nanoparticles can be effectively reduced. Thus, by adjusting the ratio of the first ligand to the second ligand, the level of the composite can be adjusted, for example, when the fermi level of the composite is low, the fermi level of the composite can be increased by increasing the molar ratio of the first ligand amino alcohol and/or the alkylamine relative to the second ligand in the composite; when the fermi level of the composite is higher, then the second ligand Cl in the composite can be increased - 、Br - And/or I - The fermi level of the composite is reduced relative to the molar ratio of the first ligand. For example, in some embodiments, the molar ratio of the first ligand to the second ligand in the composite material ranges from (1:1) to (2:1), such that the absolute value of the difference in fermi level between the fermi level of the quantum dot light emitting layer and the electron transporting layer may be made equal to or less And 0.3eV, so that the light-emitting layer and the electron transport layer have higher energy level matching degree, and the electroluminescent device has higher light-emitting efficiency and longer service life.
The embodiment of the application also provides a preparation method of the composite material, which comprises the following steps:
step S01: providing the metal oxide nano particles and an organic solvent, and mixing to obtain a metal oxide nano particle dispersion liquid;
step S02: and adding the first ligand and the compound containing the second ligand into the dispersion liquid, and mixing to obtain the composite material.
In the step S01:
the organic solvent is a solvent conventionally used for dispersing the metal nanoparticles, and may be, for example, at least one selected from, but not limited to, ethanol, propanol, butanol, n-octane, n-heptane, and ethylene glycol monomethyl ether.
It is understood that the addition amount of the organic solvent is not limited as long as the metal oxide nanoparticles can be sufficiently dispersed. In at least one embodiment, the concentration of the metal oxide nanoparticles in the metal oxide nanoparticle dispersion is in the range of 10 to 100mg/ml. Within the range, the metal oxide nanoparticles can be ensured not to be agglomerated, and ligand modification reaction after the first ligand and the compound containing the second ligand are added can be fully reacted.
In the step S02:
the compound including the second ligand may be a halogen compound, which may be selected from, but not limited to, at least one of NaF, naCl, naBr, naI, znCl, znBr, znF and ZnI.
The addition amount of the first ligand is as follows: the molar amount of the first ligand is 1.5-50% of the molar amount of the metal oxide nanoparticles.
The addition amount of the second ligand is as follows: the molar amount of the second ligand is 0.02-10% of the molar amount of the metal oxide nanoparticle.
In at least one embodiment, the first ligand and the compound containing the second ligand are added in the order of adding the first ligand and then adding the second ligand, so that the first ligand and the metal oxide nanoparticles can react, the solubility of the metal oxide nanoparticles is effectively improved, and agglomeration and precipitation of the metal oxide nanoparticles are prevented.
It will be appreciated that the compound comprising the second ligand may be dispersed in an organic solvent to provide a dispersion of the compound comprising the second ligand, and then added to the metal oxide nanoparticle dispersion.
It is understood that in the step S02, the step of washing and drying is further included after the mixing. It will be appreciated that the wash drying may be a method conventionally used for wash drying nanoparticles. In some embodiments, the solvents used in the washing are ethanol and ethyl acetate.
The embodiment of the application also provides a film, wherein the film comprises the composite material.
In some embodiments, the composite is used for an electron transport layer material, and correspondingly, the thin film is an electron transport layer.
The embodiment of the application also provides a preparation method of the film, which comprises the following steps:
step S11: providing the composite material;
step S12: and arranging the composite material on a substrate to obtain the film.
It is understood that the kind of the substrate is not limited. In one embodiment, the substrate is a cathode substrate, which may be a conventionally used substrate such as glass, and the composite material is disposed on the cathode substrate. In yet another embodiment, the substrate includes a stacked anode and a light emitting layer, the metal oxide material being disposed on a surface of the light emitting layer remote from the anode.
In the step S12, the method of disposing the composite material on the substrate may be a chemical method or a physical method. The chemical method can be chemical vapor deposition, continuous ion layer adsorption and reaction, anodic oxidation, electrolytic deposition, coprecipitation, etc. The physical method can be a physical plating method or a solution processing method, and the physical plating method can be a thermal evaporation plating method CVD, an electron beam evaporation plating method, a magnetron sputtering method, a multi-arc ion plating method, a physical vapor deposition method PVD, an atomic layer deposition method, a pulse laser deposition method and the like; the solution processing method may be spin coating, printing, inkjet printing, knife coating, printing, dip-coating, dipping, spraying, roll coating, casting, slit coating, bar coating, or the like.
In at least one embodiment, the method of disposing the composite material on the substrate is a solution method, in which the composite material is dispersed with a dispersing agent to obtain a composite material dispersion, and then the composite material dispersion is disposed on the substrate by a solution method.
The dispersant may be selected from but not limited to cyclohexane, t-butanol, methanol, ethanol, butanol, pentanol, 2- (trifluoromethyl) -3-2 ethoxy dodecafluorohexane (C) 9 H 5 F 15 O), methoxy-nonafluorobutane (C) 4 F 9 OCH 3 ) 1-chloro-4-methoxybutane (C) 5 H 11 ClO) and 2-bromo-1, 1-diethoxyethane (C) 6 H 13 BrO 2 ) At least one of them.
Referring to fig. 1, an embodiment of the present application further provides an electroluminescent device 100, which includes an anode 10, a light emitting layer 20, an electron transport layer 30, and a cathode 40 that are stacked. The electron transport layer 30 includes the composite material therein, or the electron transport layer 30 is the thin film.
It will be appreciated that the electroluminescent device 100 may further include a hole injection layer, a hole transport layer, an electron blocking layer, a hole blocking layer, an electron injection layer, an interface modification layer, and the like, which are functional layers conventionally used in electroluminescent devices to help improve the performance of the electroluminescent device.
Referring to fig. 2, in an embodiment, the electroluminescent device 100 includes an anode 10, a hole injection layer 50, a hole transport layer 60, a light emitting layer 20, an electron transport layer 30, and a cathode 40, which are stacked. The electron transport layer 30 includes the composite material therein, or the electron transport layer 30 is the thin film.
The material of the anode 10 is a material known in the art for anodes, and may be selected from, for example, but not limited to, doped metal oxide electrodes, composite electrodes, and the like. The material of the doped metal oxide electrode may be selected from at least one of indium doped tin oxide (ITO), fluorine doped tin oxide (FTO), antimony doped tin oxide (XTO), aluminum doped zinc oxide (XZO), gallium doped zinc oxide (GZO), indium doped zinc oxide (IZO), magnesium doped zinc oxide (MZO), and aluminum doped magnesium oxide (XMO), but is not limited thereto. The composite electrode is a composite electrode comprising doped or undoped transparent metal oxide and metal sandwiched therebetween, such as XZO/Ag/XZO, XZO/Xl/XZO, ITO/Ag/ITO, ITO/Xl/ITO, znO/Ag/ZnO, znO/Xl/ZnO, and TiO 2 /Ag/TiO 2 、TiO 2 /Xl/TiO 2 ZnS/Ag/ZnS, znS/XL/ZnS, etc.
The light emitting layer 20 may be an organic light emitting layer or a quantum dot light emitting layer. When the light emitting layer 20 is an organic light emitting layer, the electroluminescent device 100 may be an organic electroluminescent device; when the light emitting layer 20 is a quantum dot light emitting layer, the electroluminescent device 100 may be an electroluminescent device.
The material of the organic light emitting layer is a material known in the art for an organic light emitting layer of an electroluminescent device, for example, may be selected from, but not limited to, CBP: ir (mppy) 3 (4, 4' -bis (N-carbazole) -1,1' -biphenyl: tris [2- (p-tolyl) pyridin-C2, N) iridium (III)), TCTX: ir (mmpy) (4, 4' -tris (carbazol-9-yl) triphenylamine: tris [2- (p-tolyl) pyridine-C2, N) iridium), a diarylanthracene derivative, a stilbene aromatic derivative, a pyrene derivative, a fluorene derivative, a blue-emitting TBPe fluorescent material, a green-emitting TTPX fluorescent material, an orange-emitting TBRb fluorescent material, and a red-emitting DBP fluorescent material.
The material of the quantum dot light emitting layer is a quantum dot material known in the art for a quantum dot light emitting layer of an electroluminescent device, and for example, may be at least one selected from, but not limited to, single structure quantum dots and core-shell structure quantum dots. The material and the core shell of the quantum dot with the single structureThe material of the core of the structure quantum dot, and the material of the shell of the core-shell structure quantum dot may be selected from, but not limited to, at least one of group II-VI compounds, group III-V compounds, and group I-III-VI compounds. By way of example, the group II-VI compound may be selected from, but not limited to, at least one of CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeTe and CdZnSTe; the III-V compound may be selected from at least one of, but not limited to InP, inXs, gxP, gxXs, gxSb, xlN, xlP, inXsP, inNP, inNSb, gxXlNP and InXLNP; the I-III-VI compound may be selected from, but is not limited to, cuInS 2 、CuInSe 2 AgInS 2 At least one of them.
As an example, the quantum dot of the core-shell structure may be selected from at least one of CdSe/CdSeS/CdS, inP/ZnSeS/ZnS, cdZnSe/ZnSe/ZnS, cdSeS/ZnSeS/ZnS, cdSe/ZnSe/ZnS, znSeTe/ZnS, cdSe/CdZnSeS/ZnS, and InP/ZnSe/ZnS.
The cathode 40 is a cathode known in the art for an electroluminescent device, and may be, for example, at least one selected from, but not limited to, an Ag electrode, an Xl electrode, an Xu electrode, a Pt electrode, an Ag/IZO electrode, an IZO electrode, and an alloy electrode.
The material of the hole injection layer 50 is a material known in the art for a hole injection layer, and may be selected from, for example, but not limited to, 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-hexaazabenzophenanthrene (HXT-CN), PEDOT: PSS, and s-MoO doped therewith 3 Derivatives of (PEDOT: PSS: s-MoO) 3 ) At least one of them.
The material of the hole transport layer 60 may be a material known in the art for a hole transport layer, and may be, for example, at least one selected from Poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine ] (PTXX), 2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9 '-spirobifluorene (spiro-omeTXD), 4' -cyclohexylbis [ N, N-bis (4-methylphenyl) aniline ] (TXPC), N '-bis (1-naphthyl) -N, N' -diphenyl-1, 1 '-diphenyl-4, 4' -diamine (NPB), 4 '-bis (N-carbazole) -1,1' -biphenyl (CBP), poly [ (9, 9-dioctylfluorenyl-2, 7-diyl) -co- (4, 4'- (N- (p-butylphenyl)) diphenylamine) ] (b), poly (9-vinyl carbazole) (PVK), poly (tfd), poly (3, 4' -ethylenethiophene) -triphenylamine (tcp-4, 4 '-ethylenethiophene) (tcp), and Poly (tcp-triphenylamine) (4', 4-triphenylamine).
It will be appreciated that the materials of the various layers of the electroluminescent device 100 may be tailored to the lighting requirements of the electroluminescent device 100.
It is understood that the electroluminescent device 100 may be a front-mounted electroluminescent device or an inverted electroluminescent device.
The embodiment of the application also provides a display device, which comprises the electroluminescent device 100.
The present application is specifically illustrated by the following examples, which are only some of the examples of the present application and are not limiting of the present application.
Example 1
Providing an ITO anode 10 having a thickness of 40 nm;
depositing a PEDOT material on the anode 10 in air, and then performing heat treatment at 150 ℃ for 15min to obtain a hole injection layer 50 with the thickness of 20 nm;
in N 2 In a glove box, a TFB material is deposited on the hole injection layer 50, and then heat treatment is carried out for 30min at 150 ℃ to obtain a hole transport layer 60 with the thickness of 30 nm;
in N 2 Depositing CdSe/CdSeS/CdS quantum dot material on the hole transport layer 60 in a glove box, and then performing heat treatment at 100 ℃ for 5min to obtain a light-emitting layer 20 with the thickness of 20 nm;
in N 2 In a glove box, 10mmol of mercaptobutanol is added into 50ml of butanol solution of ZnO nano-particles with the concentration of 40mg/ml, and the mixture is stirred for 60min at room temperature; then adding 1ml of NaF ethanol solution with the concentration of 0.1M, and continuously stirring for 30min; then washing with ethanol and ethyl acetate, and drying to obtain a composite material; the composite material comprises ZnO nano particles, and a first ligand thiobutanol and a second ligand F which are connected to the surfaces of the ZnO nano particles - In the composite material, mercaptobutanol and F - The molar ratio of (2) was 7:3.
Dispersing the composite material in ethanol to obtain an ethanol solution of the composite material; spin-coating the ethanol solution of the composite material on the surface of the luminescent layer 20, and then performing heat treatment at 100 ℃ for 30min to obtain an electron transport layer 30 with the thickness of 50 nm;
in N 2 In a glove box, ag is evaporated on the electron transport layer 30 to obtain a cathode 40 with the thickness of 100 nm;
in N 2 In the glove box, the electroluminescent device 100 was obtained by encapsulation with an epoxy resin.
Example 2
This example is essentially the same as example 1, except that the NaF in example 1 is replaced with NaCl and the CdSe/CdSeS/CdS quantum dot material in example 1 is replaced with InP/ZnSeS/ZnS quantum dot material.
The composite material of the embodiment comprises ZnO nano particles, and a first ligand thiobutanol and a second ligand Cl which are connected to the surfaces of the ZnO nano particles - And in the composite material, mercaptobutanol and Cl - The molar ratio of (2) is 8:2.
Example 3
This example is essentially the same as example 1 except that the thiobutanol in example 1 is replaced with an amino butanol and the CdSe/CdSeS/CdS quantum dot material in example 1 is replaced with a CdZnSe/ZnSe/ZnS quantum dot material.
The composite material of the embodiment comprises ZnO nano-particles, and a first ligand amino butanol and a second ligand F which are connected to the surfaces of the ZnO nano-particles - And in the composite material, the amino butanol and F - The molar ratio of (2) was 6:4.
Example 4
This example is essentially the same as example 1, except that mercaptobutanol in example 1 is replaced with aminobutanol, naF in example 1 is replaced with NaCl, and CdSe/CdSeS/CdS quantum dot material in example 1 is replaced with CdSeS/ZnS quantum dot material.
The composite material of the embodiment comprises ZnO nano-particles, and a first ligand aminobutanol and a second ligand Cl connected to the surfaces of the ZnO nano-particles - And in the composite material, the amino butanol and the Cl - The molar ratio of (2) is 5:5.
Example 5
This example is essentially the same as example 1, except that the thiobutanol of example 1 is replaced with propanethiol.
The composite material of the embodiment comprises ZnO nano-particles, and a first ligand propanethiol and a second ligand F which are connected to the surfaces of the ZnO nano-particles - And in the composite material, mercaptan and F - The molar ratio of (2) is 8:2.
Example 6
This example is essentially the same as example 1, except that the thiobutanol of example 1 is replaced with octanamine.
The composite material of the embodiment comprises ZnO nano-particles, and a first ligand octanamine and a second ligand F which are connected to the surfaces of the ZnO nano-particles - And in the composite material, octane amine and F - The molar ratio of (2) was 7:3.
Example 7
This example is essentially the same as example 1, except that 10mmol of thiobutanol in example 1 is replaced with 5mmol of aminobutanol and 10mmol of heptanamine.
The composite material of the embodiment comprises ZnO nano-particles, and a first ligand amino butanol, heptane amine and a second ligand F which are connected to the surfaces of the ZnO nano-particles - And in the composite material, amino butanol, heptane amine and F - The molar ratio of (2) is 5:3:2.
Example 8
This example is substantially the same as example 1 except that 1ml of NaF having a concentration of 0.1M in example 1 is replaced with 0.5ml of NaCl having a concentration of 0.1M, 0.5ml of NaBr having a concentration of 0.1M and 0.5ml of NaI having a concentration of 0.1M.
The composite material of the embodiment comprises ZnO nano particles, and a first ligand thiobutanol and a second ligand Cl which are connected to the surfaces of the ZnO nano particles - 、Br - 、I - And in the composite material, the thiobutanol and Cl - 、Br - 、I - Molar ratio of 7:1:1:1。
Example 9
This example is essentially the same as example 1 except that 10mmol of thiobutanol in example 1 is replaced with 0.5mmol of thiobutanol and 0.5mmol of heptanamine, and 1ml of NaF having a concentration of 0.1M is replaced with 0.5ml of NaF having a concentration of 0.1M, 0.5ml of NaBr having a concentration of 0.1M and 0.5ml of NaI having a concentration of 0.1M.
The composite material of the embodiment comprises ZnO nano-particles, and a first ligand thiobutanol, heptane amine and a second ligand F which are connected to the surfaces of the ZnO nano-particles - 、Br - 、I - And in the composite material, thiobutanol, heptane amine, F - 、Br - 、I - The molar ratio of (2) to (1) is 3:3:2:1:1.
Example 10
This example is essentially the same as example 1 except that 13mmol of thiobutanol is added to 50ml of a butanol solution of ZnO nanoparticles having a concentration of 40mg/ml, and stirred at room temperature for 60min; then, 2.5ml of NaF ethanol solution with a concentration of 0.1M was added thereto, and stirring was continued for 30 minutes.
In the composite material of this example, thiobutanol and F - The molar ratio of (2) is 5:5.
Example 11
This example is essentially the same as example 1 except that 1.3mmol of thiobutanol is added to 50ml of a butanol solution of ZnO nanoparticles having a concentration of 40mg/ml, and stirred at room temperature for 60min; then, 0.125ml of NaF ethanol solution with the concentration of 0.1M was added, and stirring was continued for 30min.
In the composite material of this example, thiobutanol and F - The molar ratio of (2) was 6:4.
Example 12
This example is essentially the same as example 1, except that the example replaces ZnO nanoparticles with TiO 2 And (3) nanoparticles.
In the composite material of this example, mercaptobutanol and F - The molar ratio of (2) was 6:4.
Example 13
This embodiment is substantially the same as embodiment 1,the difference is that the present example replaces 50ml of ZnO nanoparticles with a concentration of 40mg/ml with 30ml of MZO nanoparticles with a concentration of 40mg/ml and 40ml of SnO with a concentration of 20mg/ml 2 And (3) nanoparticles.
In the composite material of this example, mercaptobutanol and F - The molar ratio of (2) was 7:3.
Example 14
This example is essentially the same as example 4, except that the amount of aminobutanol used in this example is 8mmol and the amount of NaCl used is 1ml of a 0.1M solution in NaCl ethanol.
In the composite material of the embodiment, the aminobutanol and the Cl - The molar ratio of (2) to (1).
Example 15
This example is essentially the same as example 4 except that the aminobutanol is used in an amount of 1mmol and NaCl is used in an amount of 3ml of 0.1M NaCl ethanol solution.
In the composite material of the embodiment, the aminobutanol and the Cl - The molar ratio of (2) was 0.5:1.
Example 16
This example is essentially the same as example 4, except that the amount of aminobutanol used in this example is 15mmol and the amount of NaCl used is 0.2ml of a 0.1M solution in NaCl ethanol.
In the composite material of the embodiment, the aminobutanol and the Cl - The molar ratio of (2) is 2.5:1.
Comparative example 1
This comparative example is substantially the same as example 1 except that the electron transport layer material of this comparative example is ZnO nanoparticles having-OH ligands attached to the surface.
Comparative example 2
This comparative example is substantially the same as example 2 except that the electron transport layer material of this comparative example is ZnO nanoparticles having-OH ligands attached to the surface.
Comparative example 3
This comparative example is substantially the same as example 3 except that the electron transport layer material of this comparative example is ZnO nanoparticles having-OH ligands attached to the surface.
The fermi levels of the electron transport layers (composite materials) and the light emitting layers (quantum dot materials) of examples 1 to 16 and comparative examples 1 to 3 were tested. The test method is to spin-coat the material into a film and then test the fermi level with a kelvin probe microscope. The test results are shown in the table one.
The electroluminescent devices prepared from the composite materials of examples 1 to 16 and comparative examples 1 to 3 were tested for external quantum efficiency and lifetime on day 1 after completion of the preparation and 60 days in air, respectively. The external quantum efficiency and the EQE optical test instrument are adopted for measurement, the service life T95@1000nit is tested by a 128-path service life test system customized by Guangzhou New FOV, the system architecture is that a constant voltage and constant current source drive an electroluminescent device, the test voltage or current changes, a photodiode detector and the test system test the brightness (photocurrent) change of the electroluminescent device, and the luminance meter tests and calibrates the brightness (photocurrent) of the electroluminescent device to obtain the time for the initial brightness of the electroluminescent device to decay to 95%. The test results are shown in the table one.
The composite materials of examples 1-16 and comparative examples 1-3 were tested for stability in ethanol solutions. The test method is to place the ethanol solutions of the composites of examples 1 to 16 and comparative examples 1 to 3 in air for 30 days, respectively, and visually observe the clarity of the solutions. And then the ethanol solution of the composite material placed for 30 days is respectively used for preparing an electroluminescent device by adopting the preparation method of the device in the embodiment 1, and the external quantum efficiency and the service life T95@1000nit of the electroluminescent device are tested. The detection results are shown in the table I.
Table one:
Figure BDA0003449040440000161
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Figure BDA0003449040440000171
from Table one can see:
the electroluminescent devices of examples 1 to 16 have higher luminous efficiency and longer lifetime than those of comparative examples 1 to 3;
the electroluminescent devices of examples 2 to 4 have higher luminous efficiency and longer lifetime than those of examples 1 and 5 to 16, and it can be seen that the surfaces of the ZnO nanoparticles are combined with the first ligand thiobutanol and the second ligand Cl - The luminous efficiency and the service life of the electroluminescent device can be effectively improved by matching with the InP system quantum dots; the surface of ZnO nano-particle is combined with first ligand amino butanol and second ligand F - The light-emitting efficiency and the service life of the electroluminescent device can be effectively improved by matching with CdZnSe/ZnSe/ZnS quantum dots; the surface of ZnO nano-particle is combined with first ligand amino butanol and second ligand Cl - The luminous efficiency and the service life of the electroluminescent device can be effectively improved;
the electroluminescent devices of examples 1 to 16 showed close luminous efficiency and lifetime on days 1 and 60, compared to the electroluminescent devices of comparative examples 1 to 3, and it was found that the electroluminescent devices of examples 1 to 16 had better stability in luminous efficiency and lifetime;
the ethanol solutions of the composites of examples 1-16 were significantly better in clarity after 30 days of placement, and the electroluminescent devices produced had higher luminous efficiency and longer lifetime, compared to the ethanol solutions of the composites of comparative examples 1-3.
The electroluminescent devices of examples 4 and 14 have higher luminous efficacy and longer life and better stability than those of examples 15 to 16, and it can be seen that when the first ligand in the composite material is selected from at least one of aminoalcohols or alkylamines, the second ligand is selected from Cl - 、Br - I - In the case of at least one of (1) to (2) of the above, the molar ratio of the first ligand to the second ligand in the composite material is in the range of (1:1) to (2:1), so that the luminous efficiency, the service life and the stability of the electroluminescent device can be effectively improved.
The above describes the composite materials and the electroluminescent device provided in the embodiments of the present application in detail, and specific examples are applied herein to illustrate the principles and embodiments of the present application, and the above examples are only used to help understand the method and core ideas of the present application; meanwhile, those skilled in the art will have variations in the specific embodiments and application scope in light of the ideas of the present application, and the present description should not be construed as limiting the present application in view of the above.

Claims (16)

1. A composite material characterized by: the composite material comprises metal oxide nanoparticles, and a first ligand and a second ligand which are connected to the surfaces of the metal oxide nanoparticles, wherein the first ligand is an organic ligand with a main chain carbon number of more than or equal to 2, and the second ligand is an inorganic ligand.
2. The composite material of claim 1, wherein: the molar quantity of the first ligand is 50-80% of the total molar quantity of the first ligand and the second ligand.
3. The composite material of claim 1, wherein: the metal oxide nanoparticles are selected from ZnO nanoparticles, mg-doped zinc oxide nanoparticles, al-doped zinc oxide nanoparticles, in-doped zinc oxide nanoparticles, mg-doped and Li-doped zinc oxide nanoparticles, mg-doped and Al-doped zinc oxide nanoparticles, mg-doped and In-doped zinc oxide nanoparticles, ga-doped and In-doped zinc oxide nanoparticles, tiO 2 Nanoparticles, snO 2 Nanoparticles and In 2 O 3 At least one of the nanoparticles.
4. The composite material of claim 1, wherein: the particle size range of the metal oxide nano particles is 2-10 nm.
5. The composite material of claim 1, wherein: the number of carbon atoms of the main chain of the first ligand is more than or equal to 3 and less than or equal to 18.
6. The composite material of claim 1, wherein: the first ligand is selected from at least one of mercapto alcohol, mercaptan, amino alcohol and alkylamine.
7. The composite material of claim 6, wherein: the mercapto alcohol is at least one selected from mercapto butanol, mercapto ethanol, mercapto propanol, mercapto pentanol, mercapto hexanol, mercapto heptanol and mercapto dodecanol;
the mercaptan is at least one selected from ethanethiol, propanethiol, butanethiol, pentanethiol, hexanethiol, dodecanethiol and octadecanethiol;
the amino alcohol is at least one selected from amino butanol, amino ethanol, amino propanol, amino pentanol, amino hexanol, amino heptanol and amino octanol;
the alkylamine is at least one selected from ethylamine, propylamine, butylamine, pentylamine, hexylamine, heptylamine, octylamine, dodecylamine and octadecylamine.
8. The composite material of claim 1, wherein: the second ligand is a halogen ligand selected from Cl - 、Br - 、I - F (F) - At least one of them.
9. The composite material of claim 1, wherein: the first ligand is selected from at least one of mercapto alcohol or mercaptan, and the second ligand is selected from Cl - 、Br - I - At least one of them.
10. The composite material of claim 1, wherein: the first ligand is selected from at least one of amino alcohol or alkylamine, and the second ligand is selected from F - 。
11. The composite material of claim 1, wherein: the first ligand is selected from at least one of amino alcohol or alkylamine, and the second ligand is selected from Cl - 、Br - I - At least one of them.
12. The composite material of claim 11, wherein: the molar ratio of the first ligand to the second ligand ranges from (1:1) to (2:1).
13. A film, characterized in that: the film comprising the composite of any one of claims 1-12.
14. An electroluminescent device comprising an anode, a light emitting layer, an electron transport layer and a cathode which are stacked, wherein: the electron transport layer comprising the composite material of any of claims 1-12.
15. An electroluminescent device as claimed in claim 14, wherein: the luminescent layer is a quantum dot luminescent layer, the material of the quantum dot luminescent layer is at least one of single-structure quantum dots and core-shell structure quantum dots, the material of the single-structure quantum dots, the material of the cores of the core-shell structure quantum dots and the material of the shells of the core-shell structure quantum dots are at least one of II-VI group compounds, III-V group compounds and I-III-VI group compounds, and the II-VI group compounds are at least one of CdSe, cdS, cdTe, znSe, znS, cdTe, znTe, cdZnS, cdZnSe, cdZnTe, znSeS, znSeTe, znTeS, cdSeS, cdSeTe, cdTeS, cdZnSeTe and CdZnSte; the III-V compound is at least one selected from InP, inXs, gxP, gxXs, gxSb, xlN, xlP, inXsP, inNP, inNSb, gxXlNP and InXlnP; the I-III-VI compound is selected from CuInS 2 、CuInSe 2 AgInS 2 At least one of them.
16. A display device, characterized in that: the display device comprising an electroluminescent device as claimed in any one of claims 14 to 15.
CN202111658491.5A 2021-12-30 2021-12-30 Composite material, film, electroluminescent device and display device Pending CN116437691A (en)

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