CN115893495A - Tungsten oxide nano material and preparation method thereof, hole functional film and photoelectric device - Google Patents

Tungsten oxide nano material and preparation method thereof, hole functional film and photoelectric device Download PDF

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CN115893495A
CN115893495A CN202111160505.0A CN202111160505A CN115893495A CN 115893495 A CN115893495 A CN 115893495A CN 202111160505 A CN202111160505 A CN 202111160505A CN 115893495 A CN115893495 A CN 115893495A
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tungsten oxide
oxide nano
halogenated
acid
hole
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徐威
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C01G41/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C31/00—Saturated compounds having hydroxy or O-metal groups bound to acyclic carbon atoms
    • C07C31/34—Halogenated alcohols
    • C07C31/36—Halogenated alcohols the halogen not being fluorine
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41—Preparation of salts of carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C53/00—Saturated compounds having only one carboxyl group bound to an acyclic carbon atom or hydrogen
    • C07C53/15—Saturated compounds having only one carboxyl group bound to an acyclic carbon atom or hydrogen containing halogen
    • C07C53/16—Halogenated acetic acids
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/14—Carrier transporting layers
    • H10K50/15—Hole transporting layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K50/00—Organic light-emitting devices
    • H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
    • H10K50/17—Carrier injection layers
    • 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
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    • 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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    • Y02E10/549—Organic PV cells

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Abstract

The application discloses a tungsten oxide nano material and a preparation method thereof, wherein the preparation method comprises the following steps: providing tungstic acid; mixing tungstic acid with halogenated acid and/or halogenated alcohol, and heating for reaction to obtain the tungsten oxide nano material. The tungsten oxide nano material prepared by the preparation method of the tungsten oxide nano material comprises tungsten oxide nano particles and halogenated acid ligands and/or halogenated alcohol ligands connected to the surfaces of the tungsten oxide nano particles. The halogenated acid ligand and/or the halogenated alcohol ligand can effectively passivate defect state luminescence of the tungsten oxide nanoparticles, improve the dispersibility and stability of the tungsten oxide nanoparticles in a solvent, improve the hole mobility of a hole functional layer comprising the tungsten oxide nanoparticles, and improve the hole injection and transmission capacity of a photoelectric device, so that the charge balance in the photoelectric device is improved, and further the external quantum efficiency and the service life of the photoelectric device are improved. In addition, the application also discloses a hole functional film and a photoelectric device.

Description

Tungsten oxide nano material and preparation method thereof, hole functional film and photoelectric device
Technical Field
The application relates to the technical field of display, in particular to a preparation method of a tungsten oxide nano material, the tungsten oxide nano material prepared by the preparation method, a hole functional film comprising the tungsten oxide nano material and a photoelectric device comprising the hole functional film.
Background
The photoelectric device is a device manufactured according to a photoelectric effect, and has wide application in the fields of new energy, sensing, communication, display, illumination and the like, such as a solar cell, a photoelectric detector, an electroluminescent device and the like.
At present, the light emitting elements of display panels of electronic products such as computers, mobile phones and the like are mainly electroluminescent devices. The existing widely used electroluminescent devices are mainly organic electroluminescent devices (OLEDs) and quantum dot electroluminescent devices (QLEDs). The structure of a conventional electroluminescent device mainly comprises an anode, a hole injection layer, a hole transport layer, a luminescent layer, an electron transport layer, an electron injection layer and a cathode. Under the action of an electric field, holes generated by an anode of the electroluminescent device and electrons generated by a cathode move, are respectively injected into the hole transport layer and the electron transport layer and finally migrate to the light emitting layer, and when the holes and the electrons meet at the light emitting layer, energy excitons are generated, so that light emitting molecules are excited to finally generate visible light.
It is known that the electron-hole injection balance of the electroluminescent device can effectively improve the efficiency, the service life and other properties of the electroluminescent device. However, the conventional electroluminescent device has poor hole injection and/or transport capability for various reasons, so that the electron-hole injection of the electroluminescent device is unbalanced. For example, in order to increase the aperture ratio of a display panel, a top emission electroluminescent device is generally employed. In the optical design of a top-emitting electroluminescent device, the cavity length of the device is usually optimized by increasing the thickness of a hole injection layer of the electroluminescent device, and the increase of the thickness of the hole injection layer of the electroluminescent device can reduce the hole injection capability of the electroluminescent device, so that the electron-hole injection in the electroluminescent device is unbalanced, and the efficiency and the service life of the electroluminescent device are low.
In recent years, inorganic semiconductor materials are used as hole injection materials and hole transport materials, and thus, the inorganic materials become one of the more popular research contents in the preparation technology of electroluminescent devices. Among them, tungsten oxide (WO) 3 ) The energy gap is 2.6-2.8eV, the blue light in sunlight can be absorbed, and the material has the advantages of good chemical stability, adjustable W/O stoichiometry, adjustable energy level structure, high carrier mobility, low price and the like, and can be used as a hole injection material or a hole transmission material. However, WO 3 The hole injection and hole transport properties of (a) are poor, so that electron-hole injection in the electroluminescent device is unbalanced, resulting in low efficiency and short lifetime of the electroluminescent device.
Disclosure of Invention
In view of this, the present application provides a tungsten oxide nano material and a preparation method thereof, aiming to solve the problem of low efficiency and life of a photoelectric device caused when the existing tungsten oxide nano material is used in the photoelectric device.
The embodiment of the application is realized in such a way that the preparation method of the tungsten oxide nano material comprises the following steps:
providing tungstic acid;
mixing tungstic acid and halogenated acid and/or halogenated alcohol, and heating to react to obtain the tungsten oxide nano material, wherein the tungsten oxide nano material comprises tungsten oxide nano particles and halogenated acid ligands and/or halogenated alcohol ligands connected to the surfaces of the tungsten oxide nano particles.
Optionally, in some embodiments of the present application, the heating temperature ranges from 40 to 80 ℃; and/or
The reaction time is 48-72h.
Alternatively, in some embodiments herein, the mass ratio of the tungstic acid to the haloacid and/or halohydrin is in the range of (1.0.
Optionally, in some embodiments of the present application, the preparation method of the tungstic acid comprises: mixing tungstate with acid, and reacting to obtain tungstic acid, wherein the tungstate is at least one of sodium tungstate, titanium tungstate, nickel tungstate and magnesium tungstate.
Optionally, in some embodiments of the present application, the tungstic acid is mixed with a halogenated acid and/or a halogenated alcohol, and then a step of adding a weak base is further included.
Optionally, in some embodiments of the present application, the weak base is selected from K 2 CO 3 、KHCO 3 、Na 2 CO 3 And NaHCO 3 At least one of (a).
Alternatively, in some embodiments herein, the molar ratio of the tungstic acid to the weak base is in the range of (1.
Alternatively, in some embodiments herein, the halogenated acid is a halogenated acetic acid and the halogenated alcohol is a halogenated ethanol.
Correspondingly, the embodiment of the application also provides the tungsten oxide nano material prepared by the preparation method, and the tungsten oxide nano material comprises tungsten oxide nano particles and halogenated acid ligands and/or halogenated alcohol ligands connected to the surfaces of the tungsten oxide nano particles.
Optionally, in some embodiments of the present application, the tungsten oxide nanomaterial includes a halogenated acid ligand and/or a halogenated alcohol ligand in an amount ranging from 10 to 50wt%.
Optionally, in some embodiments of the present application, the tungsten oxide nanoparticles are doped with a doping metal element.
Optionally, in some embodiments of the present application, the doping metal element is selected from at least one of Ti, ni, and Mg; and/or
The molar weight of the doped metal element is 1-20% of the molar weight of the tungsten oxide.
Correspondingly, the embodiment of the application also provides a hole functional film, wherein the hole functional film is a hole injection film or a hole transmission film, and the hole functional film comprises the tungsten oxide nano material prepared by the preparation method, or the hole functional film comprises the tungsten oxide nano material.
Correspondingly, the embodiment of the application further provides a photoelectric device which comprises an anode, a hole functional layer, a light emitting layer and a cathode which are stacked, wherein the hole functional layer comprises the tungsten oxide nano material prepared by the preparation method, or the hole functional layer comprises the tungsten oxide nano material.
The tungsten oxide nano material prepared by the preparation method of the tungsten oxide nano material comprises tungsten oxide nano particles and a halogenated acid ligand and/or a halogenated alcohol ligand connected to the surfaces of the tungsten oxide nano particles. The halogenated acid ligand and/or the halogenated alcohol ligand can effectively passivate defect state luminescence of the tungsten oxide nanoparticles, improve the dispersity and stability of the tungsten oxide nanoparticles in a solvent, improve the hole mobility of a hole functional layer comprising the tungsten oxide nanoparticles, and improve the hole injection and transmission capacity of a photoelectric device, so that the charge balance in the photoelectric device is improved, and the external quantum efficiency and the service life of the photoelectric device are improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
Fig. 1 is a flowchart of a method for preparing a tungsten oxide nano material according to an embodiment of the present disclosure;
fig. 2 is a schematic structural diagram of an optoelectronic device provided in an embodiment of the present application;
FIG. 3 is a schematic structural diagram of another optoelectronic device provided by an embodiment of the present application;
fig. 4 is a schematic structural diagram of another optoelectronic device provided in the embodiments of the present application.
Detailed Description
The technical solutions in the embodiments of the present application will be described clearly and completely with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only some embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any inventive step, shall fall within the scope of protection of the present application. Furthermore, it should be understood that the detailed description and specific examples, while indicating exemplary embodiments of the invention, are given by way of illustration and explanation only, and are not intended to limit the scope of the invention. In the present application, unless otherwise specified, the use of directional words such as "upper" and "lower" specifically refer to the orientation of the figures in the drawings. In addition, in the description of the present application, the term "including" means "including but not limited to". Various embodiments of the invention may exist in a range of forms; it is to be understood that the description in range format is merely for convenience and brevity and should not be construed as an inflexible limitation on the scope of the invention; accordingly, the described range descriptions should be considered to have specifically disclosed all the possible sub-ranges as well as individual numerical values within that range. For example, it is contemplated that the 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 individual numbers within the stated range, such as 1, 2,3, 4,5, and 6, for example, as applicable regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any number (fractional or integer) recited within the indicated range.
Referring to fig. 1, an embodiment of the present application provides a method for preparing a tungsten oxide nano material, including the following steps:
step S11: providing tungstic acid;
step S12: mixing tungstic acid and halogenated acid and/or halogenated alcohol, and heating to react to obtain the tungsten oxide nano material, wherein the tungsten oxide nano material comprises tungsten oxide nano particles and halogenated acid ligands and/or halogenated alcohol ligands connected to the surfaces of the tungsten oxide nano particles.
In the step S11:
the tungstic acid may be selected from, but not limited to, at least one of white tungstic acid, yellow tungstic acid and metatungstic acid.
In one embodiment, the tungstic acid is prepared by the following method: mixing tungstate with acid, and reacting to obtain tungstic acid.
The tungstate may be selected from, but not limited to, sodium tungstate (Na) 2 WO 4 ) Titanium Tungstate (TiW) 2 O 5 ) Nickel tungstate (NiW) 2 O 5 ) And magnesium tungstate (MgWO) 4 ) At least one of (1). The sodium tungstate may be sodium tungstate dihydrate (Na) 2 WO 4 ·2H 2 O), the titanium tungstate can be titanium tungstate hexahydrate (TiW) 2 O 5 ·2H 2 O), the nickel tungstate can be nickel tungstate hexahydrate (NiW) 2 O 5 ·2H 2 O), the magnesium tungstate may be magnesium tungstate dihydrate (MgWO) 4 ·2H 2 O)。
When the tungstate comprises at least one of titanium tungstate, nickel tungstate and magnesium tungstate, the prepared tungstic acid contains at least one of metal elements such as Ti, ni and Mg. Correspondingly, the tungsten oxide nanoparticles in the tungsten oxide nanoparticles prepared in step S14 are metal element-doped tungsten oxide nanoparticles, and the tungsten oxide nanoparticles include metal element-doped tungsten oxide nanoparticles and a halogenated acid ligand and/or a halogenated alcohol ligand connected to the surface of the tungsten oxide nanoparticles. The doped metal element includes, but is not limited to, at least one of Ti, ni, and Mg.
The acid is an acid conventionally used for preparing tungstic acid, and for example, may be selected from, but not limited to, at least one of nitric acid and hydrochloric acid. In one embodiment, the acid is a 10% aqueous solution of nitric acid.
In some embodiments, the method of preparing the tungstic acid further comprises the step of cleaning the tungstic acid with a cleaning agent. It is understood that the cleaning agent may be isopropanol, cyclohexane, ethanol, etc. conventionally used for cleaning tungstic acid.
In the step S12:
the halogenated acid is a compound containing a halogen atom and a carboxyl group in a molecule. The halogen atom may be selected from, but not limited to, at least one of fluorine (F), chlorine (Cl), bromine (Br), and iodine (I). In some embodiments, the halogenated acid is the halogenated acetic acid, illustratively, the halogenated acid is selected fromMonochloroacetic acid (CH) 2 ClCOOH), dichloroacetic acid (CHCl) 2 COOH) and trichloroacetic acid (CCl) 3 COOH).
The halohydrin contains halogen atoms and-CH in molecules 2 -OH groups. The halogen atom may be selected from, but not limited to, at least one of fluorine (F), chlorine (Cl), bromine (Br), and iodine (I). In some embodiments, the halohydrin is the haloethanol, which is illustratively selected from monochloroethanol (CH) 2 ClCH 2 OH), ethanol dichloride (CHCl) 2 CH 2 OH) and trichloroethanol (CCl) 3 CH 2 OH).
In some embodiments, the mass ratio of the tungstic acid to the haloacid and/or halohydrin is in the range of (1.0.
In some embodiments, the method of mixing tungstic acid with a halogenated acid and/or a halogenated alcohol is sonication to disperse tungstic acid uniformly in the halogenated acid and/or the halogenated alcohol.
In some embodiments, after the tungstic acid is mixed with the halogenated acid and/or the halogenated alcohol, a weak base is added to adjust the pH value of the solution to 6-8 so as to promote the formation of coordination bonds between the tungstic acid and the halogenated acid and/or the halogenated alcohol. The weak base may be selected from but not limited to K 2 CO 3 、KHCO 3 、Na 2 CO 3 And NaHCO 3 At least one of (1). In one embodiment, the weak base is an aqueous solution of a weak base, and the content of the weak base in the aqueous solution of the weak base is in the range of 10 to 30wt%.
In some embodiments, the molar ratio of the tungstic acid to the weak base ranges from (1.
In some embodiments, the heating is at a temperature in the range of 40-80 ℃. The reaction time is 48-72h. It is understood that the reaction may be carried out under stirring in order to allow the reaction to proceed rapidly and sufficiently.
In some embodiments, the tungsten oxide nanomaterial includes a haloacid ligand and/or a halohydrin ligand in an amount in a range from 10 to 50wt%. If the content of the ligand is too low, the defect state luminescence of the tungsten oxide nanoparticles cannot be effectively passivated, and if the content of the ligand is too high, the conductivity of the tungsten oxide nanoparticles is too low.
The particle size range of the tungsten oxide nano particles is 8-15nm. The tungsten oxide nanoparticles have too small particle size, poor conductivity and instability; the tungsten oxide nanoparticles have too large particle size, and the energy level of a hole energy-space layer prepared from the tungsten oxide nanoparticles is not matched with that of a light-emitting layer of a photoelectric device, so that the difficulty in injecting carriers can be caused.
In some embodiments, the tungsten oxide nanoparticles may be doped with a metal element, in other words, the tungsten oxide nanoparticles are metal element-doped tungsten oxide nanoparticles. The doping metal element may be selected from, but not limited to, at least one of Ti, ni, and Mg. The doped metal element can effectively improve the hole concentration and the hole mobility of the tungsten oxide nano material.
In the tungsten oxide nano material, the molar weight of the doped metal element is 1-20% of that of tungsten oxide. If the content of the doped metal element is too low, no doping effect is achieved, and if the content of the doped metal element is too high, the doped metal element is crystallized and separated out independently.
The tungsten oxide nano material prepared by the preparation method of the tungsten oxide nano material comprises tungsten oxide nano particles and a halogenated acid ligand and/or a halogenated alcohol ligand connected to the surfaces of the tungsten oxide nano particles. The halogenated acid ligand and/or the halogenated alcohol ligand can effectively passivate defect state luminescence of the tungsten oxide nanoparticles, improve the dispersity and stability of the tungsten oxide nanoparticles in a solvent, improve the hole mobility of a hole functional layer comprising the tungsten oxide nanoparticles, and improve the hole injection and transmission capacity of a photoelectric device, so that the charge balance in the photoelectric device is improved, and the external quantum efficiency and the service life of the photoelectric device are improved.
The embodiment of the present application further provides a hole functional film, which may be a hole injection film or a hole transport film. The hole functional film comprises the tungsten oxide nano material.
The embodiment of the present application further provides a method for preparing the hole functional thin film, which includes the following steps:
step S21: providing the tungsten oxide nano material;
step S22: and arranging the tungsten oxide nano material on a substrate to form a tungsten oxide nano material film, namely obtaining the cavity hollow energy film.
It is understood that the kind of the substrate is not limited. In an embodiment, the substrate is an anode substrate, the substrate may be a conventionally used substrate such as glass, and the tungsten oxide nano material is disposed on the anode. In yet another embodiment, the substrate includes a cathode and a light emitting layer stacked, and the tungsten oxide nano-material is disposed on the light emitting layer.
In the step S22, a method of disposing the tungsten oxide nano 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 coating method or a solution processing method, and the physical coating method can be a thermal evaporation coating method CVD, an electron beam evaporation coating method, a magnetron sputtering method, a multi-arc ion coating 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, ink jet printing, blade coating, printing, dip-coating, dipping, spray coating, roll coating, casting, slit coating, stripe coating, or the like.
In an embodiment, the method for disposing the tungsten oxide nanomaterial on the substrate is a solution method, in which case, the tungsten oxide nanomaterial is dispersed by using a dispersant to obtain a tungsten oxide nanomaterial dispersion solution, and then the tungsten oxide nanomaterial dispersion solution is disposed on the substrate by a solution method. The dispersant may be selected from, but not limited to, at least one of methanol, ethanol, butanol, and pentanol. In one embodiment, the concentration of the dispersion is in the range of 5-40mg/mL.
Referring to fig. 2 to 4, embodiments of the present application further provide an optoelectronic device 100, where the optoelectronic device 100 may be a solar cell, a photodetector, an organic optoelectronic device (OLED), or a quantum dot optoelectronic device (QLED). The photovoltaic device 100 includes an anode 10, a hole functional layer 20, a light emitting layer 30, and a cathode 40, which are sequentially stacked. The hole function layer 20 includes at least one of a hole injection layer 21 and a hole transport layer 22. The hole injection layer 21 and/or the hole transport layer 22 are the hole energy film, in other words, the tungsten oxide nanomaterial is included in the hole injection layer 21 and/or the hole transport layer 22.
Referring to fig. 2, in an embodiment, the optoelectronic device 100 includes an anode 10, a hole injection layer 21, a light emitting layer 30, and a cathode 40, which are sequentially stacked. The hole injection layer 21 comprises the tungsten oxide nano-material.
Referring to fig. 3, in another embodiment, the optoelectronic device 100 includes an anode 10, a hole transport layer 22, a light emitting layer 30 and a cathode 40, which are sequentially stacked. The hole transport layer 22 comprises the tungsten oxide nanomaterial.
Referring to fig. 4, in another embodiment, the optoelectronic device 100 includes an anode 10, a hole injection layer 21, a hole transport layer 22, a light emitting layer 30 and a cathode 40, which are sequentially stacked. The hole injection layer 21 and/or the hole transport layer 22 comprise the tungsten oxide nanomaterial.
The material of the anode 10 is a material known in the art for anodes, and for example, may be selected from, but not limited to, a doped metal oxide electrode, a composite electrode, and the like. The doped metal oxide electrode may be selected from, but not limited to, at least one of indium-doped tin oxide (ITO), fluorine-doped tin oxide (FTO), antimony-doped tin oxide (ATO), aluminum-doped zinc oxide (AZO), gallium-doped zinc oxide (GZO), indium-doped zinc oxide (IZO), magnesium-doped zinc oxide (MZO), and aluminum-doped magnesium oxide (AMO). The composite electrode is a composite electrode formed by sandwiching metal between doped or undoped transparent metal oxides, such as AZO/Ag/AZO, AZO/Al/AZO, ITO/Ag/ITO, ITO/Al/ITO, znO/Ag/ZnO, znO/Al/ZnO, tiO 2 /Ag/TiO 2 、TiO 2 /Al/TiO 2 ZnS/Ag/ZnS, znS/Al/ZnS and the like.
The light emitting layer 30 may be an organic light emitting layer or a quantum dot light emitting layer. When the light emitting layer 30 is an organic light emitting layer, the optoelectronic device 100 may be an organic optoelectronic device. When the light emitting layer 30 is a quantum dot light emitting layer, the optoelectronic device 100 may be a quantum dot optoelectronic device.
The material of the organic light emitting layer is a material known in the art for an organic light emitting layer of an optoelectronic device, and may be selected from, for example, but not limited to, CBP Ir (mppy) 3 (4, 4' -bis (N-carbazole) -1,1' -biphenyl tris [2- (p-tolyl) pyridine-C2, N) -iridium (III)), TCTA Ir (mmpy) (4, 4',4 ″ -tris (carbazol-9-yl) triphenylamine: at least one of tris [2- (p-tolyl) pyridine-C2, N) iridium (III)), diarylanthracene derivatives, stilbene aromatic derivatives, pyrene derivatives or fluorene derivatives, blue-emitting TBPe fluorescent materials, green-emitting TTPA fluorescent materials, orange-emitting TBRb fluorescent materials, and red-emitting DBP fluorescent materials.
The material of the quantum dot light-emitting layer is a quantum dot material known in the art for quantum dot light-emitting layers of optoelectronic devices, and for example, may be selected from, but not limited to, at least one of single-structure quantum dots and core-shell structure quantum dots. For example, the single structure quantum dots 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, cdznsse, cdZnSeTe, zneses, znSeTe, znste, znSeTe, cdSeTe, cdTeS, cdZnSeTe, and CdZnSeTe; the III-V compound may be selected from, but not limited to, at least one of InP, inAs, gaP, gaAs, gaSb, alN, alP, inAsP, inNP, inNSb, gaAlNP, and InAlNP; the group I-III-VI compound may be selected from, but is not limited to, cuInS 2 、CuInSe 2 And AgInS 2 At least one of (1). The quantum dots of the core-shell structure may be selected from, but not limited to, at least one of CdSe/ZnS, cdSe/ZnSe/ZnS, znCdSe/ZnSe/ZnS, znSeTe/ZnS, cdSe/CdZnSeS/ZnS, inP/ZnSe/ZnS, and InP/ZnSeS/ZnS.
The cathode 40 is a cathode known in the art for a photovoltaic device, and for example, may be selected from at least one of Ag electrode, al electrode, au electrode, pt electrode, ag/IZO electrode, IZO electrode or alloy electrode.
In one embodiment, the optoelectronic device 100 further comprises an electron transport layer connected between the light emitting layer 30 and the cathode 40.
The material of the electron transport layer is a material known in the art for electron transport layers, and for example, may be selected from, but not limited to, znO, tiO 2 、ZrO 2 、HfO 2 、Ca、Ba、CsF、LiF、CsCO 3 At least one of ZnMgO, PBD (2- (4-biphenyl) -5-phenyl oxadiazole), 8-hydroxyquinoline aluminum (Alq 3) and graphene.
When the optoelectronic device 100 includes both the hole injection layer 21 and the hole transport layer 22, and only the hole injection layer 21 includes the tungsten oxide nanomaterial, the material of the hole transport layer 22 may be a material known in the art for a hole transport layer, for example, at least one selected from, but not limited to, poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine ] (PTAA), 2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9 '-spirobifluorene (spiro-omeTAD), 4' -cyclohexylbis [ N, N-bis (4-methylphenyl) aniline ] (TAPC), 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) ] (TFB), poly (9-vinylcarbazole) (PVK), polytriphenylamine (Poly-TPD), poly (3, 4-ethylenedioxythiophene) -Poly (styrenesulfonic acid) (PSS) and 4,4' -triphenylamine (tcot) carbazole (TCTA).
When the optoelectronic device 100 includes both the hole injection layer 21 and the hole transport layer 22 and only the hole transport layer 22 includes the tungsten oxide nanomaterial, the material of the hole injection layer 21 is a material known in the art for use in hole injection layers, and may be selected from, for example, but not limited to, 2,3,6,7,10, 11-hexacyano-1, 4,5,8,9, 12-hexaazatriphenylene (HAT-CN), PEDOT: PSS, and s-MoO doped thereof 3 (PEDOT: PSS: s-MoO) 3 ) At least one of (a).
It is understood that, in addition to the above functional layers, the optoelectronic device 100 may further add some functional layers that are conventionally used in optoelectronic devices and contribute to improving the performance of optoelectronic devices, such as an electron blocking layer, a hole blocking layer, an electron injection layer, and an interface modification layer.
It is understood that the materials of the various layers of the optoelectronic device 100 can be tailored to the lighting requirements of the optoelectronic device 100.
It is understood that the optoelectronic device 100 can be an upright optoelectronic device or an inverted optoelectronic device.
The embodiment of the present application further provides a method for manufacturing the optoelectronic device 100, including the following steps:
step S31: providing an anode 10;
step S32: providing the tungsten oxide nano material, and arranging the tungsten oxide nano material on the anode 10 to obtain a hole functional layer 20;
step S33: a light-emitting layer 30 and a cathode 40 are sequentially formed on the hole function layer 20.
It is understood that, when the optoelectronic device 100 further includes an electron transport layer, the step S33 is: a light-emitting layer 30, an electron transport layer, and a cathode 40 are sequentially formed on the hole function layer 20.
The embodiment of the present application further provides another method for manufacturing the optoelectronic device 100, including the following steps:
step S41: providing a cathode 40, and forming a light-emitting layer 30 on the cathode 40;
step S42: providing the tungsten oxide nano material, and arranging the tungsten oxide nano material on the light-emitting layer 30 to obtain a hole functional layer 20;
step S43: an anode 10 is formed on the hole function layer 20.
It is understood that, when the optoelectronic device 100 further includes an electron transport layer, the step S41 is: a cathode 40 is provided, and an electron transport layer and a light-emitting layer 30 are sequentially formed on the cathode 40.
In the above two preparation methods:
the method for forming the anode 10, the light-emitting layer 30, the electron transport layer and the cathode 40 can be implemented by a conventional technique in the art, and can be, for example, a chemical method or a physical method. The chemical or physical methods are as described above and will not be described herein.
It is understood that, when the optoelectronic device 100 further includes other functional layers such as an electron blocking layer, a hole blocking layer, an electron injection layer and/or an interface modification layer, the method for manufacturing the optoelectronic device 100 further includes a step of forming each functional layer.
The present application will be specifically described below with reference to specific examples, which are only some examples of the present application and are not intended to limit the present application.
Example 1
Providing an ITO/Ag/ITO composite anode 10, wherein the thicknesses of an ITO layer, an Ag layer and an ITO layer stacked in the ITO/Ag/ITO composite anode 10 are respectively 10nm, 100nm and 10nm;
spin-coating a PEDOT (PSS (model AI 4083)) material on the anode 10, and then performing heat treatment at 150 ℃ for 15min to obtain a hole injection layer 21 with the thickness of 24 nm;
adding 10mmol of Na 2 WO 4 ·2H 2 Dissolving O in 100ml deionized water, adding 10% HNO 3 The aqueous solution is stirred vigorously to obtain off-white H 2 WO 4 Precipitating and then washing the H with isopropanol 2 WO 4 Precipitating; subjecting the H to 2 WO 4 Dissolving the precipitate in 150mL of monochloroacetic acid, ultrasonically dispersing, and adding 10mL of K with the mass concentration of 10wt% 2 CO 3 Violently stirring the aqueous solution for 60min, stirring the aqueous solution for 2 days at 50 ℃, and then centrifugally cleaning the aqueous solution by using deionized water and ethanol to obtain a tungsten oxide nano material, wherein the tungsten oxide nano material comprises tungsten oxide nano particles and monochloroacetic acid ligand connected to the surfaces of the tungsten oxide nano particles, and the content of the monochloroacetic acid ligand is 20wt%;
dispersing the tungsten oxide nano material in cyclohexane to obtain tungsten oxide nano material dispersion liquid with the concentration of 20mg/mL, spin-coating the tungsten oxide nano material dispersion liquid on the hole injection layer 21, and then carrying out heat treatment at 100 ℃ for 30min to obtain a hole transport layer 22 with the thickness of 24 nm;
spin-coating CdSe/CdZnSeS/ZnS quantum dot luminescent material on the hole transport layer 22 to obtain a luminescent layer 30 with the thickness of 29 nm;
coating a ZnMgO material on the luminescent layer 30 in a spinning way, wherein the content of Mg in the ZnMgO material is 15wt%, and carrying out heat treatment for 20min under the nitrogen atmosphere and at the temperature of 100 ℃ to obtain an electron transport layer with the thickness of 50 nm;
performing vapor plating on the electron transport layer with Ag to obtain a cathode 40 with the thickness of 40 nm;
and evaporating an NPB material on the cathode 40 to obtain a covering layer with the thickness of 60nm, so as to obtain the photoelectric device 100. The optoelectronic device 100 of the present embodiment is a quantum dot optoelectronic device.
Example 2
This example is essentially the same as example 1, except that 8mmol of Na 2 WO 4 ·2H 2 O and 1mmol of TiW 2 O 5 ·6H 2 Dissolving O in 100ml of deionized water, and correspondingly, obtaining the tungsten oxide nano material which comprises Ti-doped tungsten oxide nano particles and monochloroacetic acid ligand connected to the surfaces of the tungsten oxide nano particles. Wherein the molar amount of Ti is 10% of the molar amount of W.
Example 3
This example is essentially the same as example 1, except that 8mmol of Na 2 WO 4 ·2H 2 O and 1mmol of NiW 2 O 5 ·6H 2 Dissolving O in 100ml of deionized water, and correspondingly, obtaining the tungsten oxide nano material which comprises Ni-doped tungsten oxide nano particles and monochloroacetic acid ligand connected to the surfaces of the tungsten oxide nano particles. Wherein the molar amount of Ni is 10% of the molar amount of W.
Example 4
This example is essentially the same as example 1, except that 8mmol of Na 2 WO 4 ·2H 2 O and 2mmol MgWO 4 ·2H 2 Dissolving O in 100ml of deionized water, and correspondingly, obtaining the tungsten oxide nano material which comprises Mg-doped tungsten oxide nano particles and monochloroacetic acid ligand connected to the surfaces of the tungsten oxide nano particles. Wherein, mg isThe molar amount was 20% of the molar amount of W.
Example 5
This example is essentially the same as example 1, except that this example uses 8.5mmol of Na 2 WO 4 ·2H 2 O、0.5mmol NiW 2 O 5 ·6H 2 O and 0.5mmol MgWO 4 ·2H 2 Dissolving O in 100ml of deionized water, and correspondingly, obtaining the tungsten oxide nano material which comprises Ni and Mg doped tungsten oxide nano particles and monochloroacetic acid ligand connected to the surfaces of the tungsten oxide nano particles. Wherein the molar amount of Ni is 5% of the molar amount of W, and the molar amount of Mg is 5% of the molar amount of W.
Example 6
This example is essentially the same as example 1, except that this example uses 8.5mmol of Na 2 WO 4 ·2H 2 O、0.5mmol TiW 2 O 5 ·6H 2 O and 0.5mmol MgWO 4 ·2H 2 Dissolving O in 100ml of deionized water, and correspondingly, obtaining the tungsten oxide nano material which comprises Ti and Mg doped tungsten oxide nano particles and monochloroacetic acid ligand connected to the surfaces of the tungsten oxide nano particles. Wherein the molar amount of Ti is 5% of the molar amount of W, and the molar amount of Mg is 5% of the molar amount of W.
Example 7
This example is essentially the same as example 1, except that H is as defined above 2 WO 4 And dissolving the precipitate in 150mL of ethanol dichloride, wherein the obtained tungsten oxide nano material correspondingly comprises tungsten oxide nano particles and ethanol dichloride ligands connected to the surfaces of the tungsten oxide nano particles.
Example 8
Providing an ITO/Ag/ITO composite anode 10, wherein the thicknesses of an ITO layer, an Ag layer and an ITO layer stacked in the ITO/Ag/ITO composite anode 10 are respectively 10nm, 100nm and 10nm;
adding 10mmol of Na 2 WO 4 ·2H 2 Dissolving O in 100ml deionized water, adding 10% HNO 3 The aqueous solution is stirred vigorously to obtain off-white H 2 WO 4 Precipitating and then washing the H with isopropanol 2 WO 4 Precipitating; subjecting said H to 2 WO 4 Dissolving the precipitate in 150mL trichloroacetic acid, ultrasonically dispersing, adding 10mL K with mass concentration of 10wt% 2 CO 3 Violently stirring the aqueous solution for 60min, stirring the aqueous solution for 2 days at 50 ℃, and then centrifugally cleaning the aqueous solution by using deionized water and ethanol to obtain a tungsten oxide nano material, wherein the tungsten oxide nano material comprises tungsten oxide nano particles and trichloroacetic acid ligands connected to the surfaces of the tungsten oxide nano particles, and the content of the trichloroacetic acid ligands is 60wt%;
dispersing the tungsten oxide nano material in cyclohexane to obtain tungsten oxide nano material dispersion liquid with the concentration of 20mg/mL, spin-coating the tungsten oxide nano material dispersion liquid on the anode 10, and then carrying out heat treatment at 100 ℃ for 30min to obtain a hole injection layer 21 with the thickness of 24 nm;
spin-coating a TFB material on the hole injection layer 21 to obtain a hole transport layer 22 with a thickness of 24 nm;
spin-coating CBP-Ir (mppy) 3 material on the hole transport layer 22 to obtain a light emitting layer 30 with the thickness of 29 nm;
spin coating a PBD material on the light-emitting layer 30, and carrying out heat treatment at 150 ℃ for 30min in a nitrogen atmosphere to obtain an electron transport layer with the thickness of 50 nm;
sequentially evaporating Ag and IZO on the electron transport layer to obtain an Ag/IZO cathode 40 with the thickness of 40 nm;
and evaporating an NPB material on the cathode 40 to obtain a covering layer with the thickness of 60nm, so as to obtain the photoelectric device 100. The optoelectronic device 100 of the present embodiment is an organic optoelectronic device.
Comparative example 1
This comparative example is substantially the same as example 1 except that the material of the hole transport layer 22 of this comparative example is TFB.
Comparative example 2
This comparative example is substantially the same as example 8 except that the material of the hole injection layer 21 of this comparative example is PEDOT: PSS (model: AI 4083).
The photovoltaic devices of examples 1 to 8 and comparative examples 1 to 2 were subjected to external quantum efficiency EQE and lifetime T95 — 1knit tests. The external quantum efficiency EQE is measured by adopting an EQE optical testing instrument, the service life test is carried out by a service life testing box, and the service life T95_1knit refers to the time that the brightness of the quantum dot light-emitting diode is attenuated to 95% at the initial brightness of 1 knit. The detection results are shown in the following table I.
Table one:
Figure BDA0003289989290000141
Figure BDA0003289989290000151
as can be seen from table one, the external quantum efficiency and lifetime of the quantum dot optoelectronic devices of examples 1 to 7 are significantly higher than those of the quantum dot optoelectronic device of comparative example 1, and the external quantum efficiency and lifetime of the organic optoelectronic device of example 8 are significantly higher than those of the organic optoelectronic device of comparative example 2.
The tungsten oxide nanomaterial and the preparation method thereof, the hole functional thin film and the photoelectric device provided by the embodiment of the application are described in detail above, a specific example is applied in the description to explain the principle and the implementation mode of the application, and the description of the embodiment is only used for helping to understand the method and the core concept of the application; meanwhile, for those skilled in the art, according to the idea of the present application, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present application.

Claims (14)

1. The preparation method of the tungsten oxide nano material is characterized by comprising the following steps of:
providing tungstic acid;
mixing the tungstic acid with halogenated acid and/or halogenated alcohol, and heating to react to obtain the tungsten oxide nano material, wherein the tungsten oxide nano material comprises tungsten oxide nano particles and halogenated acid ligands and/or halogenated alcohol ligands connected to the surfaces of the tungsten oxide nano particles.
2. The method of claim 1, wherein: the heating temperature range is 40-80 ℃; and/or
The reaction time is 48-72h.
3. The method of claim 1, wherein: the mass ratio of the tungstic acid to the halogenated acid and/or halogenated alcohol is in the range of (1.0.
4. The method of claim 3, wherein: the preparation method of the tungstic acid comprises the following steps: mixing tungstate with acid, and reacting to obtain tungstic acid, wherein the tungstate is at least one of sodium tungstate, titanium tungstate, nickel tungstate and magnesium tungstate.
5. The method of claim 1, wherein: the tungstic acid is mixed with halogenated acid and/or halogenated alcohol, and then a step of adding weak base is included.
6. The method of claim 5, wherein: the weak base is selected from K 2 CO 3 、KHCO 3 、Na 2 CO 3 And NaHCO 3 At least one of; alternatively, the molar ratio of the tungstic acid to the weak base ranges from (1.
7. The method of claim 1, wherein: the halogenated acid is halogenated acetic acid, and the halogenated alcohol is halogenated ethanol.
8. A tungsten oxide nano-material is characterized in that: the tungsten oxide nano material comprises tungsten oxide nano particles and halogenated acid ligands and/or halogenated alcohol ligands connected to the surfaces of the tungsten oxide nano particles.
9. The tungsten oxide nanomaterial of claim 8, wherein: in the tungsten oxide nano material, the content range of the halogenated acid ligand and/or the halogenated alcohol ligand is 10-50wt%.
10. The tungsten oxide nanomaterial of claim 8, wherein: the tungsten oxide nanoparticles are doped with doped metal elements.
11. The tungsten oxide nanomaterial of claim 10, wherein: the doped metal element is selected from at least one of Ti, ni and Mg; and/or
The molar weight of the doped metal element is 1-20% of the molar weight of the tungsten oxide.
12. The tungsten oxide nanomaterial of claim 8, wherein: the tungsten oxide nano material is prepared by the preparation method of any one of claims 1 to 7.
13. A hole-functional film, which is a hole-injecting film or a hole-transporting film, characterized in that: the hole function film comprises tungsten oxide nano-materials prepared by the preparation method of any one of claims 1 to 7, or the hole function film comprises tungsten oxide nano-materials of any one of claims 8 to 12.
14. An optoelectronic device comprising a stacked anode, a hole functional layer, a light emitting layer and a cathode, wherein: the hole function layer comprises tungsten oxide nano-materials prepared by the preparation method of any one of claims 1 to 7, or the hole function layer comprises tungsten oxide nano-materials of any one of claims 8 to 12.
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