CN112786798B - Luminescent material composition and application thereof - Google Patents

Luminescent material composition and application thereof Download PDF

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CN112786798B
CN112786798B CN202011642717.8A CN202011642717A CN112786798B CN 112786798 B CN112786798 B CN 112786798B CN 202011642717 A CN202011642717 A CN 202011642717A CN 112786798 B CN112786798 B CN 112786798B
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luminescent material
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electron acceptor
acceptor dopant
material composition
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CN112786798A (en
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蒋杰
庄锦勇
李雪
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Guangdong Juhua Printing Display Technology Co Ltd
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Guangdong Juhua Printing Display Technology Co Ltd
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
    • 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]
    • H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] 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]
    • H10K50/14—Carrier transporting layers
    • H10K50/15—Hole transporting layers
    • H10K50/155—Hole transporting layers comprising dopants
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K2101/00—Properties of the organic materials covered by group H10K85/00
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Abstract

The invention discloses a luminescent material composition and application thereof, wherein the luminescent material composition comprises a luminescent material, an electron acceptor dopant, a first organic solvent and a second organic solvent, wherein the first organic solvent is used for dispersing the luminescent material, and the second organic solvent is used for dispersing the electron acceptor dopant. According to the invention, by doping the electron acceptor dopant in the luminescent material, on one hand, the energy band of the luminescent layer can be bent, and the injection barrier of holes can be reduced, and on the other hand, the hole transmission capability and the hole transmission rate of the luminescent layer can be improved, so that the problem of unbalanced injection of electrons and holes is solved.

Description

Luminescent material composition and application thereof
Technical Field
The invention relates to the technical field of display devices, in particular to the technical field of light-emitting diodes, and specifically relates to a luminescent material composition and application thereof.
Background
In a conventional display device, a light emitting diode is generally used as a light source, and a sandwich structure of an Electron Transport Layer (ETL)/an emission layer (EML)/a Hole Transport Layer (HTL) is generally used in a conventional light emitting diode, where the ETL transports electrons injected from a cathode to the EML, and holes are injected from an anode and transported to the EML through the HTL, and the electrons and the holes generate recombination radiation at the EML to realize light emission.
The ETL is generally zinc oxide (ZnO) or titanium oxide (TiO) 2 ) Tin oxide (SnO) 2 ) Isoinorganic semiconductor oxides, having higher electron mobility and matched conduction band energy levels; the HTL is generally selected from organic compounds such as Polyvinylimidazole (PVK), poly [ bis (4-phenyl) (4-butylphenyl) amine](poly-TPD), poly [ (9, 9-di-N-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (N- (4-N-butyl) phenyl) -diphenylamine)](TFB), etc., but these organic compounds are far less charge-transporting than inorganic oxides; in addition, most of the commonly used hole transport materials have a HOMO energy level of about 5.2eV, and a large potential barrier exists between the HOMO energy level and a valence band energy level of the light emitting layer, so that holes are difficult to inject into the light emitting layer, and therefore the problem of unbalanced injection of electrons and holes is caused, and further the problems of low light emitting efficiency, short service life and the like of the light emitting diode are caused, and the commercial development of the light emitting diode is severely restricted.
Disclosure of Invention
The invention mainly aims to provide a luminescent material composition and application thereof, and aims to solve the problem of unbalanced injection of electrons and holes in the conventional light-emitting diode structure.
In order to achieve the above object, the present invention provides a light emitting material composition including a light emitting material, an electron acceptor dopant, a first organic solvent, and a second organic solvent, wherein the first organic solvent is used to disperse the light emitting material, and the second organic solvent is used to disperse the electron acceptor dopant.
Optionally, the luminescent material comprises quantum dots; and/or the presence of a gas in the gas,
the electron acceptor dopant is a p-type organic molecule (particularly, a p-type small organic molecule); and/or the presence of a gas in the gas,
the first organic solvent includes at least one of tetrahydrofuran, anisole, morpholine, n-octane, n-hexane, dichloromethane, chloroform, 1, 4-dioxane, tetrahydronaphthalene, tetradecane, hexadecane, n-octylbenzene, isopropyl myristate, decycyclohexane, decahydronaphthalene, hexadecene, bicyclohexane, undecylcyclohexane, longifolene, cyclododecene, n-octylcyclohexane, dodecylcyclohexane, dodecylbenzene, undecylcyclohexane, n-octylphenyl ether, and isobornyl methacrylate; and/or the presence of a gas in the gas,
the second organic solvent comprises at least one of toluene, xylene, o-xylene, m-xylene, trimethylbenzene, chlorobenzene and o-dichlorobenzene; and/or the presence of a gas in the atmosphere,
the mass of the electron acceptor dopant is 0.1-10% of that of the luminescent material; and/or the presence of a gas in the atmosphere,
the concentration of the luminescent material in the luminescent material composition is 5-15 mg/mL.
Optionally, the electron acceptor dopant has a LUMO energy level in the range of-5.25 to-5.45 eV.
Optionally, the electron acceptor dopant includes at least one of 2,3,5, 6-tetrafluoro-7, 7', 8' -tetracyanoquinodimethane and 1,3,4,5,7, 8-hexafluorotetracyanonaphthoquinodimethane.
The invention also provides a preparation method of the luminescent material composition, which comprises the following steps:
dispersing a luminescent material in a first organic solvent to obtain a luminescent material dispersion liquid;
dispersing the electron acceptor dopant in a second organic solvent to obtain an electron acceptor dopant dispersion liquid;
and uniformly mixing the luminescent material dispersion liquid and the electron acceptor dopant dispersion liquid to obtain the luminescent material composition.
Optionally, the step of uniformly mixing the luminescent material dispersion liquid and the electron acceptor dopant dispersion liquid to obtain a luminescent material composition includes:
and dropwise adding the electron acceptor dopant dispersion liquid into the luminescent material dispersion liquid, and uniformly mixing the mixture in a shaking way after each drop of the electron acceptor dopant dispersion liquid is added until the electron acceptor dopant dispersion liquid is added, so as to obtain the luminescent material composition.
The invention also provides a light-emitting diode, wherein the material of a light-emitting layer of the light-emitting diode comprises the light-emitting material composition or the light-emitting material composition prepared by the preparation method.
The invention also provides a preparation method of the light-emitting diode, which comprises the following steps:
the luminescent material composition is taken as a raw material, and is sequentially subjected to film coating, vacuum pumping treatment and heat treatment to prepare and form a luminescent layer.
Optionally, the treatment temperature of the heat treatment is 110-130 ℃, and the treatment time is 10-40 min.
The invention also provides a display device comprising the light-emitting diode or the light-emitting diode prepared by the preparation method.
In the technical scheme provided by the invention, the luminescent material composition comprises a luminescent material, an electron acceptor dopant, a first organic solvent and a second organic solvent, and the electron acceptor dopant is doped in the luminescent material, so that on one hand, the energy band of a luminescent layer can be bent, the injection barrier of a hole is reduced, on the other hand, the hole transmission capability and the hole transmission rate of the luminescent layer can be improved, and the problem of unbalanced injection of the electron and the hole is solved; meanwhile, the luminescent material and the electron acceptor dopant are dispersed by respectively adopting the first organic solvent and the second organic solvent, so that the luminescent material and the electron acceptor dopant have good solubility, and the luminescent layer prepared from the luminescent material has good film-forming property and is not easy to precipitate.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art descriptions will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other relevant drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a schematic structural diagram of a light emitting diode device provided in the prior art;
fig. 2 is a schematic energy level diagram of a light emitting diode device provided in the prior art;
fig. 3 is a schematic view illustrating a doping principle of a light-emitting material composition according to an embodiment of the present invention applied to a light-emitting layer of a light-emitting diode device;
fig. 4 is a schematic illustration of a doping principle of another embodiment of the light-emitting material composition provided by the present invention applied to a light-emitting layer of a light-emitting diode device;
fig. 5 is a schematic structural diagram of an embodiment of a light emitting diode provided in the present invention;
FIG. 6 is a schematic diagram of the energy levels of the LED provided in FIG. 5;
fig. 7 is a schematic view of carrier injection of the light emitting diode provided in fig. 5.
The reference numbers illustrate:
reference numerals Name(s) Reference numerals Name (R)
10 Substrate 50a A first hole transport layer
20 A first electrode 50b Second hole transport layer
30 Electron transport layer 60 A second electrode
40 Luminescent layer
The implementation, functional features and advantages of the objects of the present invention will be further explained with reference to the accompanying drawings.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available. In addition, the meaning of "and/or" appearing throughout includes three juxtapositions, exemplified by "A and/or B" including either A or B or both A and B. In addition, technical solutions between various embodiments may be combined with each other, but must be realized by a person skilled in the art, and when the technical solutions are contradictory or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In a conventional display device, a light emitting diode is generally used as a light source, and a sandwich structure of an Electron Transport Layer (ETL)/an emission layer (EML)/a Hole Transport Layer (HTL) is generally adopted in a conventional light emitting diode, the ETL transports electrons injected from a cathode to the EML, holes are injected from an anode and transported to the EML through the HTL, and the electrons and the holes generate recombination radiation in the EML to realize light emission, and a specific structure of the conventional light emitting diode is, for example, an inverted device, and as shown in fig. 1, the conventional light emitting diode includes a first electrode 10, an electron transport layer 20, an emission layer 40, a hole transport layer (in fig. 1, the hole transport layer includes a first hole transport layer 50a and a second hole transport layer 50 b), and a second electrode 60, which are sequentially disposed.
The ETL is generally zinc oxide (ZnO) or titanium oxide (TiO) 2 ) Tin oxide (SnO) 2 ) Isoinorganic semiconductor oxides, having higher electron mobility and matched conduction band energy levels; the HTL is generally selected from organic compounds, such as Polyvinylimidazole (PVK), poly [ bis (4-phenyl) (4-butylphenyl) amine](poly-TPD), poly [ (9, 9-di-N-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (N- (4-N-butyl) phenyl) -diphenylamine)](TFB), etc., but these organic compounds are far less charge-transporting than inorganic oxides; most of the commonly used hole transport materials have a HOMO level of about 5.2eV (as shown in fig. 2, the first electrode is Indium Tin Oxide (ITO), and electron transport is performedThe layer is zinc oxide (ZnO), the luminescent layer is quantum dot luminescent layer (QDs), the first hole transport layer is N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine (NPB), the second hole transport layer is molybdenum trioxide (MoO) 3 ) The second electrode is Al), a large potential barrier exists between the second electrode and the valence band energy level of the light-emitting layer, so that holes are difficult to inject into the light-emitting layer, and thus the problem of unbalanced injection of electrons and holes is caused, and further the problems of low light-emitting efficiency, short service life and the like of the light-emitting diode are caused, and the commercial development of the light-emitting diode is severely restricted.
In order to solve the problem of unbalanced injection of electrons and holes, the invention provides a luminescent material composition which is used for preparing a luminescent layer of a luminescent device. Specifically, in a specific embodiment of the light emitting material composition provided by the present invention, the light emitting material composition includes a light emitting material, an electron acceptor dopant, a first organic solvent, and a second organic solvent, wherein the first organic solvent is used to disperse the light emitting material, and the second organic solvent is used to disperse the electron acceptor dopant.
Thus, the luminescent material composition comprises a luminescent material, an electron acceptor dopant, a first organic solvent and a second organic solvent, and the electron acceptor dopant is doped in the luminescent material of the luminescent layer, so that on one hand, the energy band of the luminescent layer can be bent, the injection barrier of holes can be reduced, on the other hand, the hole transport capability and the speed of the luminescent layer can be improved, and the injection problem of the holes at the interface of the luminescent layer and the hole transport layer can be improved, so that the problem of unbalanced injection of the electrons and the holes can be improved; meanwhile, the luminescent material and the electron acceptor dopant are dispersed by the first organic solvent and the second organic solvent respectively, so that the luminescent material and the electron acceptor dopant have good solubility, and the luminescent layer prepared from the luminescent material and the electron acceptor dopant has good film forming property and is not easy to precipitate, and the problems of difficult dissolution, easy precipitation and poor film forming quality when the luminescent material and the electron acceptor dopant are dispersed simultaneously by a single solvent are solved.
The light emitting device includes, but is not limited to, a quantum dot light emitting diode (QLED) or an Organic Light Emitting Diode (OLED), and when the light emitting material of the light emitting layer is a quantum dot material, the light emitting device is the QLED, and when the light emitting material of the light emitting layer is an organic light emitting material, the light emitting device is the OLED. In the embodiment provided by the invention, the light emitting device is preferably a QLED, correspondingly, the light emitting material comprises quantum dots, and the formed light emitting layer is referred to as a quantum dot light emitting layer. By doping the electron acceptor dopant into the quantum dot light-emitting layer, electrons in a valence band of the quantum dot can be captured by a deeper HOMO energy level, so that the hole concentration of the quantum dot layer is improved, p-type doping is realized, and the hole mobility is improved; meanwhile, the Fermi level of the quantum dots doped with p-type molecules is shifted downwards, so that an upward energy band bending is formed on a contact interface of the quantum dot layer and the hole transport layer, the injection barrier of holes is reduced, and the injection efficiency of the holes is improved.
In the embodiment of the present invention, the electron acceptor dopant is preferably a p-type small organic molecule, specifically at least one of 2,3,5, 6-tetrafluoro-7, 7', 8' -tetracyanoquinodimethane (F4-TCNQ) and 1,3,4,5,7, 8-hexafluorotetracyanonaphthoquinodimethane (F6-TCNNQ), and may be any one of the above two substances or a mixture of the two substances. The structures of the F4-TCNQ and the F6-TCNNQ are as follows:
Figure BDA0002874467070000061
in an embodiment of the light emitting material composition provided by the present invention, the electron acceptor dopant is F4-TCNQ, and a doping schematic diagram when the electron acceptor dopant is applied to a light emitting layer of a light emitting diode is shown in fig. 3. In another embodiment of the light emitting material composition provided by the present invention, the electron acceptor dopant is F6-TCNNQ, and a doping scheme when the electron acceptor dopant is applied to a light emitting layer of a light emitting diode is shown in fig. 4. The F4-TCNQ and the F6-TCNNQ are strong electron acceptor dopants, and the deeper LUMO energy level (-5.25 eV/-5.45 eV) can capture electrons in the HOMO energy level of a host so as to realize p-type doping.
When the electron acceptor dopant is doped into the light-emitting material, the doping amount is too low, the improvement effect on the problem of unbalanced injection of electrons and holes is not ideal, the doping amount is too large, and the light-emitting performance and the like of the light-emitting layer are easily affected, so in a specific embodiment provided by the invention, the doping amount of the electron acceptor dopant is preferably set as follows: the mass of the electron acceptor dopant is 0.1-10% of the mass of the luminescent material. Therefore, the doping amount of the electron acceptor dopant is moderate, the problem of unbalanced injection of electrons and holes can be well solved, and the luminous performance of the luminous layer can be ensured.
When specifically selected, the first organic solvent includes, but is not limited to, at least one selected from tetrahydrofuran, anisole, morpholine, n-octane, n-hexane, dichloromethane, chloroform, 1, 4-dioxane, tetrahydronaphthalene, tetradecane, hexadecane, n-octylbenzene, isopropyl myristate, decylcyclohexane, decahydronaphthalene, hexadecene, bicyclohexane, undecylcyclohexane, longifolene, cyclododecene, n-octylcyclohexane, dodecylcyclohexane, dodecylbenzene, undecylcyclohexane, n-octylphenyl ether, and isobornyl methacrylate, and may be any one of the above organic solvents or a mixed solvent of two or more thereof, and all of them fall within the scope of the present invention. In a specific embodiment of the present invention, the first organic solvent is preferably any one of the organic solvents described above, which is beneficial to simplify the formulation of the luminescent material composition and simplify the formulation process of the luminescent material composition.
When specifically selected, the second organic solvent includes, but is not limited to, at least one selected from toluene, xylene, o-xylene, m-xylene, trimethylbenzene, chlorobenzene, and o-dichlorobenzene, and may be any one of the above organic solvents, or a mixed solvent of two or more of the organic solvents, which falls within the scope of the present invention. Similarly, in an embodiment of the present invention, the second organic solvent is preferably any one of the organic solvents, which is beneficial to simplify the formulation of the luminescent material composition and simplify the formulation process of the luminescent material composition.
Based on the above-mentioned mass ratio relationship between the luminescent material and the electron acceptor dopant, the concentration of the luminescent material in the luminescent material composition is further defined, specifically, the concentration of the luminescent material in the luminescent material composition is preferably 5 to 15mg/mL. In this manner, it is advantageous to ensure sufficient dispersion of the luminescent material and electron acceptor dopant in the luminescent material composition. In addition, when the mass ratio of the luminescent material to the electron acceptor dopant and the concentration of the luminescent material in the composition are determined, the volume ratio of the first organic solvent to the second organic solvent in the luminescent material composition can be calculated, which is not described herein again. In some embodiments provided herein, the volume ratio of the first organic solvent to the second organic solvent is preferably 1.
Based on the luminescent material composition provided above, the present invention further provides a method for preparing the luminescent material composition, in a specific embodiment, the method may be performed by mixing the first organic solvent and the second organic solvent to form a mixed solvent, and then adding the luminescent material and the electron acceptor dopant into the mixed solvent, and mixing them thoroughly and uniformly. Or preparing the luminescent material into a luminescent material solution by using the first organic solvent, preparing the electron acceptor dopant into an electron acceptor dopant solution by using the second organic solvent, and then uniformly mixing the two solutions. In an embodiment of the method for preparing the luminescent material composition provided by the present invention, a step method is preferably used, and specifically, the method for preparing the luminescent material composition comprises the following steps:
s10, dispersing a luminescent material in a first organic solvent to obtain a luminescent material dispersion liquid;
s20, dispersing the electron acceptor dopant in a second organic solvent to obtain an electron acceptor dopant dispersion liquid;
and S30, uniformly mixing the luminescent material dispersion liquid and the electron acceptor dopant dispersion liquid to obtain the luminescent material composition.
The luminescent material is added into the first organic solvent in proportion, and the rapid and uniform dispersion of the luminescent material can be accelerated by means of vibration, ultrasound, stirring and the like, so that the luminescent material dispersion liquid is prepared. The electron acceptor dopant is added into the second organic solvent in proportion, and the rapid and uniform dispersion of the electron acceptor dopant can be accelerated by means of vibration, ultrasound, stirring and the like, so that the electron acceptor dopant dispersion liquid is prepared.
It is understood that the sequence of step S10 and step S20 is not limited, and may be performed before step S10 and after step S20, or after step S10 and before step S20, or simultaneously, which all fall within the protection scope of the present invention, and it is only necessary to complete the preparation of the luminescent material dispersion and the preparation of the electron acceptor dopant dispersion before step S30. And after the preparation of the two dispersions is respectively completed, fully and uniformly mixing the two dispersions to obtain the luminescent material composition. By means of stepwise formulation, fast and uniform dispersion of the luminescent material and the electron acceptor dopant, respectively, is facilitated, as well as uniform dispersion of the luminescent material and the electron acceptor dopant in the luminescent material composition.
Preferably, in order to ensure a sufficiently homogeneous mixing of the luminescent material and the electron acceptor dopant, in the embodiment of the present invention, it is preferable that step S30 is performed in the following manner: and dropwise adding the electron acceptor dopant dispersion liquid into the luminescent material dispersion liquid, and uniformly mixing the mixture in a shaking way after each drop of the electron acceptor dopant dispersion liquid is added until the electron acceptor dopant dispersion liquid is added, so as to obtain the luminescent material composition. In this way, after each drop of the electron acceptor dopant dispersion liquid is added, the luminescent material dispersion liquid and the electron acceptor dopant dispersion liquid are fully and uniformly mixed by shaking, so that the luminescent material and the electron acceptor dopant are fully and uniformly dispersed in the prepared luminescent material composition.
Fig. 5 to 7 show an embodiment of a light emitting diode according to the present invention. The material of the luminescent layer of the light-emitting diode provided by the invention comprises a luminescent material and an electron acceptor dopant. By doping the electron acceptor dopant in the light emitting layer, the problem of unbalanced injection of electrons and holes existing in the light emitting diode is improved. The light emitting diode includes but is not limited to a QLED or an OLED, preferably a QLED, and has the advantages of adjustable light emitting wavelength, high light emitting quantum efficiency, good color purity, long service life, and the like. By doping the electron acceptor dopant into the quantum dot light-emitting layer, the deeper HOMO energy level can capture electrons in a valence band of the quantum dot, so that the hole concentration of the quantum dot layer is improved, p-type doping is realized, and the hole mobility is improved; meanwhile, the Fermi level of the quantum dots doped with p-type molecules is shifted downwards, so that an upward energy band bending is formed on a contact interface of the quantum dot layer and the hole transport layer, the injection barrier of holes is reduced, and the injection efficiency of the holes is improved.
Specifically, the light emitting diode may be an upright device or an inverted device, and in the embodiment of the present invention, an inverted device is preferred, and a specific structure of the light emitting diode is similar to that shown in fig. 1, and the light emitting diode includes a first electrode, an electron transport layer, a quantum dot light emitting layer, a hole transport layer, and a second electrode, which are sequentially disposed, where a material of the light emitting layer includes quantum dots and an electron acceptor dopant. The number of the arranged layers of the electron transport layer, the quantum dot light-emitting layer and the hole transport layer is not limited, and the electron transport layer, the quantum dot light-emitting layer and the hole transport layer can be arranged into one layer or multiple layers, and the number of the arranged layers is independent. In addition, when the electron doping acceptor dopant is doped into the quantum dot light-emitting layer, the doping position of the electron doping acceptor dopant is not limited, and the doping position is determined by the adopted preparation method, for example, the electron doping acceptor dopant is doped into the quantum dot light-emitting layer, that is, the electron doping acceptor dopant and the quantum dot are uniformly mixed and dispersed; more preferably, the electron acceptor dopant is doped at one side of the quantum dot light-emitting layer close to the hole transport layer, so that the improvement effect of the doping of the electron acceptor dopant on the imbalance problem of electron and hole transport is more favorably improved.
The first electrode (cathode) is one of transparent Indium Tin Oxide (ITO), indium Zinc Oxide (IZO), zinc aluminum oxide (AZO) and Indium Gallium Zinc Oxide (IGZO). The electron transport layer is made of zinc oxide (ZnO) and titanium oxide (TiO) 2 ) Tin oxide (SnO) 2 ) And magnesium-doped zinc oxide (ZnMgO). The quantum dots in the quantum dot light-emitting layer are selected from at least one of semiconductor compounds consisting of II-VI groups, III-V groups or IV-VI groups and core-shell structures thereof, and are preferably cadmium-based quantum dots. The electron acceptor dopant doped by the quantum dot light emitting layer includes at least one of F4-TCNQ and F6-TCNNQ. The hole transport layer is made of polyvinyl imidazole (PVK) and molybdenum trioxide (MoO) 3 ) Poly [ bis (4-phenyl) (4-butylphenyl) amine](poly-TPD), poly [ (9, 9-di-N-octylfluorenyl-2, 7-diyl) -alt- (4, 4' - (N- (4-N-butyl) phenyl) -diphenylamine)](TFB) and N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine (NPB). The second electrode (anode) is at least one of metal aluminum (Al), silver (Ag), gold (Au), calcium (Ga), barium (Ba), magnesium (Mg) and the like and alloys thereof. In addition, the light emitting diode also comprises a substrate which can be a rigid substrate or a flexible substrate.
Specifically, in an embodiment of the light emitting diode provided by the present invention, the light emitting diode has a structure as shown in fig. 5, and includes a cathode (ITO), an electron transport layer (ZnO), a Quantum Dot (QDs) doped F4-TCNQ light emitting layer, a first hole transport layer (NPB), and a second hole transport layer (MoO) sequentially disposed in this order 3 ) And an anode (Al); the energy level of the charge carrier is schematically shown in FIG. 6, and the charge carrier injection is schematically shown in FIG. 7. As can be seen from comparing fig. 2 and fig. 5 to fig. 7, compared with the prior art, in the embodiment of the present invention, the electron acceptor dopant is doped in the quantum dot light emitting layer, so that the injection barrier of the hole is reduced, and thus the problem of unbalanced injection of the electron and the hole can be improved, and further the problems of low light emitting efficiency and short lifetime of the light emitting diode can be improved.
Further, the invention also provides a preparation method of the light emitting diode, which comprises the following steps: taking the luminescent material composition as a raw material, and sequentially performing film coating, vacuum pumping treatment and heat treatment to prepare and form a luminescent layer; wherein the luminescent material composition is prepared according to the preparation method of the luminescent material composition. According to the fact that the light emitting diode is an upright device or an inverted device, the preparation method thereof is different, and specifically, referring to the prior art, as long as the light emitting material composition is used as a raw material for preparing a light emitting layer, the light emitting diode is taken as an inverted device as an example, and the preparation method of the light emitting diode comprises the following steps:
step S100, providing a substrate, and preparing a cathode layer on the substrate;
step S200, preparing an electron transport layer on the cathode layer;
step S300, coating the luminescent material composition on the electron transport layer to form a liquid film, then vacuumizing, removing a solvent in the luminescent material composition, and then performing heat treatment to prepare a quantum dot luminescent layer doped with an electron acceptor dopant;
and S400, sequentially preparing a hole transport layer and an anode layer on the quantum dot light-emitting layer.
Furthermore, in step S400, the vacuum degree of the vacuum pumping treatment is 200 to 400pa, and the treatment time is 5 to 20min, under which condition, the solvent in the luminescent material composition can be removed quickly and effectively. The treatment temperature of the heat treatment is 110-130 ℃, and the treatment time is 10-40 min.
The present invention also provides a display device, including but not limited to a display screen of a mobile phone, a computer, a television, etc., the display device includes a light emitting diode, and the specific structure of the light emitting diode refers to the above embodiments. Since the light emitting diode of the present invention adopts all the technical solutions of all the embodiments, at least all the beneficial effects brought by the technical solutions of the embodiments are achieved, and no further description is given here.
The technical solutions of the present invention are further described in detail below with reference to specific examples and drawings, it should be understood that the following examples are merely illustrative of the present invention and are not intended to limit the present invention.
Example 1
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F4-TCNQ, n-octylbenzene and toluene; wherein the concentration of the cadmium-based quantum dots is 10mg/mL, the concentration of the F4-TCNQ is 0.5mg/mL, and the volume ratio of the n-octylbenzene to the toluene is 9.
Example 2
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F4-TCNQ, dicyclohexyl and toluene; wherein the concentration of the cadmium-based quantum dots is 10mg/mL, the concentration of the F4-TCNQ is 0.5mg/mL, and the volume ratio of the bicyclohexane to the toluene is 9.
Example 3
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F4-TCNQ, isopropyl myristate and toluene; wherein the concentration of the cadmium-based quantum dots is 10mg/mL, the concentration of the F4-TCNQ is 0.5mg/mL, and the volume ratio of isopropyl myristate to toluene is 9.
Example 4
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F4-TCNQ, longifolene and toluene; wherein the concentration of the cadmium-based quantum dots is 10mg/mL, the concentration of the F4-TCNQ is 0.5mg/mL, and the volume ratio of the longifolene to the toluene is 9.
Example 5
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F6-TCNNQ, tetrahydrofuran and xylene; wherein the concentration of the cadmium-based quantum dots is 10mg/mL, the concentration of the F6-TCNQ is 1mg/mL, and the volume ratio of tetrahydrofuran to xylene is 9.
Example 6
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F6-TCNNQ, n-octyl cyclohexane and m-xylene; wherein the concentration of the cadmium-based quantum dots is 10mg/mL, the concentration of the F4-TCNQ is 0.01mg/mL, and the volume ratio of n-octyl cyclohexane to m-xylene is 1.
Example 7
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F4-TCNQ, F6-TCNNQ, n-octyl cyclohexane and m-xylene; wherein the concentration of the cadmium-based quantum dots is 5mg/mL, the total concentration of the F4-TCNQ and the F6-TCNNQ is 0.01mg/mL, and the volume ratio of n-octyl cyclohexane to m-xylene is 1.
Example 8
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F4-TCNQ, n-octane and trimethylbenzene; wherein the concentration of the cadmium-based quantum dots is 5mg/mL, the concentration of the F4-TCNQ is 0.05mg/mL, and the volume ratio of n-octane to trimethylbenzene is 5.
Example 9
The luminescent material composition comprises quantum dots (red CdSe/ZnSe/ZnS), F4-TCNQ, tetradecane and chlorobenzene; wherein the concentration of the cadmium-based quantum dots is 15mg/mL, the concentration of the F4-TCNQ is 0.75mg/mL, and the volume ratio of the tetradecane to the chlorobenzene is 1.
Example 10
The composition of the luminescent material composition was the same as in example 1, and the preparation method was:
(1) Dispersing the quantum dots in n-octylbenzene to prepare quantum dot dispersion liquid;
(2) Dispersing F4-TCNQ in toluene to prepare F4-TCNQ dispersion liquid;
(3) And (3) dropwise adding the prepared F4-TCNQ dispersion liquid into the quantum dot dispersion liquid, shaking and shaking uniformly after 1 drop is added, and obtaining the luminescent material composition until the F4-TCNQ dispersion liquid is added.
Example 11
The composition of the luminescent material composition is the same as that of example 2, and the preparation method comprises the following steps:
(1) Dispersing the quantum dots in dicyclohexyl to prepare a quantum dot dispersion liquid;
(2) Dispersing F4-TCNQ in toluene to prepare F4-TCNQ dispersion liquid;
(3) And (3) dropwise adding the prepared F4-TCNQ dispersion liquid into the quantum dot dispersion liquid, shaking and shaking uniformly after 1 drop is added, and obtaining the luminescent material composition until the F4-TCNQ dispersion liquid is added.
Example 12
The composition of the luminescent material composition was the same as in example 3, and the preparation method was:
(1) Dispersing the quantum dots in isopropyl myristate to prepare a quantum dot dispersion liquid;
(2) Dispersing F4-TCNQ in toluene to prepare F4-TCNQ dispersion liquid;
(3) And dropwise adding the prepared F4-TCNQ dispersion liquid into the quantum dot dispersion liquid, shaking and shaking uniformly after 1 drop until the F4-TCNQ dispersion liquid is added, and thus obtaining the luminescent material composition.
Example 13
The composition of the luminescent material composition was the same as in example 4, and the preparation method was:
(1) Dispersing the quantum dots in longifolene to prepare quantum dot dispersion liquid;
(2) Dispersing F4-TCNQ in toluene to prepare F4-TCNQ dispersion liquid;
(3) And dropwise adding the prepared F4-TCNQ dispersion liquid into the quantum dot dispersion liquid, shaking and shaking uniformly after 1 drop until the F4-TCNQ dispersion liquid is added, and thus obtaining the luminescent material composition.
Example 14
The preparation method of the light-emitting diode comprises the following steps:
(1) Taking a transparent conductive film ITO as an anode, wherein the thickness is 50nm;
(2) Depositing MgZnO on the anode by a solution method to form an electron transport layer (wherein the doping proportion of Mg is 5%, the concentration of MgZnO is 30Mg/ml, the rotating speed is 3000rpm 30s, and after a liquid film is formed, carrying out heat treatment at 100 ℃ for 10 min), wherein the final thickness is 50nm;
(3) Taking the luminescent material composition of example 1 as a raw material, depositing a composite quantum dot luminescent layer on an electron transport layer by a solution method (rotating speed of 1500rpm 30s, forming a liquid film, vacuumizing to 300pa in a vacuum chamber for 10min, and then performing heat treatment at 120 ℃ for 10 min), wherein the final thickness is 12nm;
(4) Depositing NPB on the composite quantum dot light-emitting layer by an evaporation method to serve as a first hole transport layer, wherein the thickness of the first hole transport layer is 30nm;
(5) Vapor deposition of MoO on the first hole transport layer 3 As a second hole transport layer, 20nm thick;
(6) Al is deposited on the second hole transport layer as a cathode by an evaporation method, and the thickness is 100nm.
Example 15
The preparation method of the light-emitting diode comprises the following steps:
(1) Taking a transparent conductive film ITO as an anode, wherein the thickness is 50nm;
(2) Depositing MgZnO on the anode by a solution method to form an electron transport layer (wherein the doping proportion of Mg is 5%, the concentration of MgZnO is 30Mg/ml, the rotating speed is 3000rpm 30s, and after a liquid film is formed, carrying out heat treatment at 100 ℃ for 10 min), wherein the final thickness is 50nm;
(3) Taking the luminescent material composition of the embodiment 2 as a raw material, depositing a composite quantum dot luminescent layer on an electron transport layer by a solution method (rotating speed of 1500rpm 30s, forming a liquid film, vacuumizing to 300pa in a vacuum chamber for 10min, and then performing heat treatment at 120 ℃ for 10 min), wherein the final thickness is 12nm;
(4) Depositing NPB on the composite quantum dot light-emitting layer by an evaporation method to serve as a first hole transport layer, wherein the thickness of the first hole transport layer is 30nm;
(5) Vapor deposition of MoO on the first hole transport layer 3 As a second hole transport layer, 20nm thick;
(6) Al is deposited on the second hole transport layer as a cathode by an evaporation method, and the thickness is 100nm.
Example 16
The preparation method of the light-emitting diode comprises the following steps:
(1) Taking a transparent conductive film ITO as an anode, wherein the thickness is 50nm;
(2) Depositing MgZnO on the anode by a solution method to form an electron transport layer (wherein the doping proportion of Mg is 5%, the concentration of MgZnO is 30Mg/ml, the rotating speed is 3000rpm 30s, and after a liquid film is formed, carrying out heat treatment at 100 ℃ for 10 min), wherein the final thickness is 50nm;
(3) Taking the luminescent material composition of the embodiment 3 as a raw material, depositing a composite quantum dot luminescent layer on an electron transport layer by a solution method (the rotation speed is 1500rpm 30s, after a liquid film is formed, vacuumizing to 300pa in a vacuum chamber for 10min, and then carrying out heat treatment at 120 ℃ for 10 min), wherein the final thickness is 12nm;
(4) Depositing NPB on the composite quantum dot luminescent layer by an evaporation method to be used as a first hole transport layer, wherein the thickness of the first hole transport layer is 30nm;
(5) Vapor deposition of MoO on the first hole transport layer 3 As a second hole transport layer, 20nm thick;
(6) Al is deposited on the second hole transport layer as a cathode by an evaporation method, and the thickness is 100nm.
Example 17
The preparation method of the light-emitting diode comprises the following steps:
(1) Taking a transparent conductive film ITO as an anode, wherein the thickness is 50nm;
(2) MgZnO is deposited on the anode as an electron transport layer by a solution method (wherein the doping proportion of Mg is 5%, the concentration of MgZnO is 30Mg/ml, the rotating speed is 3000rpm 30s, a liquid film is formed, and then heat treatment is carried out for 10min at the temperature of 100 ℃), and the final thickness is 50nm;
(3) Taking the luminescent material composition of the embodiment 4 as a raw material, depositing a composite quantum dot luminescent layer on an electron transport layer by a solution method (the rotation speed is 1500rpm 30s, after a liquid film is formed, vacuumizing to 300pa in a vacuum chamber for 10min, and then carrying out heat treatment at 120 ℃ for 10 min), wherein the final thickness is 12nm;
(4) Depositing NPB on the composite quantum dot light-emitting layer by an evaporation method to serve as a first hole transport layer, wherein the thickness of the first hole transport layer is 30nm;
(5) Vapor deposition of MoO on the first hole transport layer 3 As a second hole transport layer, 20nm thick;
(6) Al is deposited on the second hole transport layer as a cathode by an evaporation method, and the thickness is 100nm.
Example 18
The preparation method of the light-emitting diode comprises the following steps:
(1) Taking a transparent conductive film ITO as an anode, wherein the thickness is 50nm;
(2) Depositing MgZnO on the anode by a solution method to form an electron transport layer (wherein the doping proportion of Mg is 5%, the concentration of MgZnO is 30Mg/ml, the rotating speed is 3000rpm 30s, and after a liquid film is formed, carrying out heat treatment at 100 ℃ for 10 min), wherein the final thickness is 50nm;
(3) Taking the luminescent material composition of example 1 as a raw material, depositing a composite quantum dot luminescent layer on an electron transport layer by a solution method (rotating speed of 1500rpm 30s, forming a liquid film, vacuumizing to 200pa in a vacuum chamber for processing for 15min, and then performing heat treatment at 110 ℃ for 20 min), wherein the final thickness is 12nm;
(4) Depositing NPB on the composite quantum dot luminescent layer by an evaporation method to be used as a first hole transport layer, wherein the thickness of the first hole transport layer is 30nm;
(5) Vapor deposition of MoO on the first hole transport layer 3 As a second hole transport layer, 20nm thick;
(6) Al is deposited on the second hole transport layer as a cathode by an evaporation method, and the thickness is 100nm.
Example 19
The preparation method of the light-emitting diode comprises the following steps:
(1) Taking a transparent conductive film ITO as an anode, wherein the thickness is 50nm;
(2) Depositing MgZnO on the anode by a solution method to form an electron transport layer (wherein the doping proportion of Mg is 5%, the concentration of MgZnO is 30Mg/ml, the rotating speed is 3000rpm 30s, and after a liquid film is formed, carrying out heat treatment at 100 ℃ for 10 min), wherein the final thickness is 50nm;
(3) Taking the luminescent material composition of example 1 as a raw material, depositing a composite quantum dot luminescent layer on an electron transport layer by a solution method (rotating speed of 1500rpm 30s, forming a liquid film, vacuumizing to 400pa in a vacuum chamber for processing for 5min, and then performing heat treatment at 130 ℃ for 40 min), wherein the final thickness is 12nm;
(4) Depositing NPB on the composite quantum dot luminescent layer by an evaporation method to be used as a first hole transport layer, wherein the thickness of the first hole transport layer is 30nm;
(5) Depositing MoO on the first hole transport layer by evaporation 3 As a second hole transport layer, the thickness was 20nm;
(6) Al was deposited as a cathode on the second hole transport layer by evaporation to a thickness of 100nm.
Example 20
The preparation method of the light-emitting diode comprises the following steps:
(1) Taking a transparent conductive film ITO as an anode, wherein the thickness is 50nm;
(2) MgZnO is deposited on the anode as an electron transport layer by a solution method (wherein the doping proportion of Mg is 5%, the concentration of MgZnO is 30Mg/ml, the rotating speed is 3000rpm 30s, a liquid film is formed, and then heat treatment is carried out for 10min at the temperature of 100 ℃), and the final thickness is 50nm;
(3) Taking the luminescent material composition of example 1 as a raw material, depositing a composite quantum dot luminescent layer on an electron transport layer by a solution method (rotating speed of 1500rpm 30s, forming a liquid film, vacuumizing to 300pa in a vacuum chamber for 10min, and then performing heat treatment at 120 ℃ for 30 min), wherein the final thickness is 12nm;
(4) Depositing NPB on the composite quantum dot luminescent layer by an evaporation method to be used as a first hole transport layer, wherein the thickness of the first hole transport layer is 30nm;
(5) Depositing MoO on the first hole transport layer by evaporation 3 As a second hole transport layer, the thickness was 20nm;
(6) Al is deposited on the second hole transport layer as a cathode by an evaporation method, and the thickness is 100nm.
Comparative example
A light emitting diode was fabricated in the same manner as in example 14, except that the electron acceptor dopant was not doped in the quantum dot light emitting layer.
The results of the performance test on the light emitting diodes prepared in examples 14 to 20 are shown in table 1 below. In Table 1, V @10mA/cm 2 Indicates a current density of 10mA/cm 2 A corresponding driving voltage; EQE @10mA/cm 2 Indicates a current density of 10mA/cm 2 The corresponding EQE; t95 (h) @1000cd/m 2 Indicating that the device had an initial luminance of 1000cd/m 2 The next continuous lighting, when the luminance decays to 95% of the initial luminance (here, 950 cd/m) 2 ) Time of flight
Table 1 results of performance test of light emitting diodes prepared in each example
V(v)@10mA/cm 2 EQE(％)@10mA/cm 2 T95(h)@1000cd/m 2
Example 14 3.6 7.1 2012
Example 15 3.4 7.88 2064
Example 16 3.4 7.0 1793
Example 17 3.2 6.3 1238
Example 18 3.3 7.2 2004
Example 19 3.4 7.3 1986
Example 20 3.2 7.1 1845
Comparative example 1.8 4.9 947
As can be seen from the test data in table 1, when the luminescent material composition provided by the embodiment of the invention is used for preparing a luminescent layer in a quantum dot light emitting diode, the prepared QLED has higher luminescent efficiency and service life by doping an electron acceptor dopant in the quantum dot luminescent layer.
The above is only a preferred embodiment of the present invention, and it is not intended to limit the scope of the invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall be included in the scope of the present invention.

Claims (8)

1. A light-emitting material composition, comprising a light-emitting material, an electron acceptor dopant, a first organic solvent, and a second organic solvent, wherein the first organic solvent is used to disperse the light-emitting material, and the second organic solvent is used to disperse the electron acceptor dopant;
the electron acceptor dopant is a p-type organic molecule, and the LUMO energy level of the electron acceptor dopant is-5.25 to-5.45 eV; wherein the electron acceptor dopant includes at least one of 2,3,5, 6-tetrafluoro-7, 7', 8' -tetracyanoquinodimethane and 1,3,4,5,7, 8-hexafluorotetracyanonaphthoquinodimethane.
2. The luminescent material composition according to claim 1, wherein the luminescent material comprises quantum dots; and/or the presence of a gas in the atmosphere,
the first organic solvent comprises at least one of tetrahydrofuran, anisole, morpholine, n-octane, n-hexane, dichloromethane, chloroform, 1, 4-dioxane, tetrahydronaphthalene, tetradecane, hexadecane, n-octylbenzene, isopropyl myristate, decylcyclohexane, decahydronaphthalene, hexadecene, bicyclohexane, undecylcyclohexane, longifolene, cyclododecene, n-octylcyclohexane, dodecylcyclohexane, dodecylbenzene, undecylcyclohexane, n-octylphenyl ether, and isobornyl methacrylate; and/or the presence of a gas in the atmosphere,
the second organic solvent comprises at least one of toluene, xylene, o-xylene, m-xylene, trimethylbenzene, chlorobenzene and o-dichlorobenzene; and/or the presence of a gas in the gas,
the mass of the electron acceptor dopant is 0.1 to 10 percent of the mass of the luminescent material; and/or the presence of a gas in the gas,
the concentration of the luminescent material in the luminescent material composition is 5-15mg/mL.
3. A method for preparing a luminescent material composition according to any one of claims 1 to 2, comprising the steps of:
dispersing a luminescent material in a first organic solvent to obtain a luminescent material dispersion liquid;
dispersing the electron acceptor dopant in a second organic solvent to obtain an electron acceptor dopant dispersion liquid;
and uniformly mixing the luminescent material dispersion liquid and the electron acceptor dopant dispersion liquid to obtain the luminescent material composition.
4. The method for producing a light-emitting material composition according to claim 3, wherein the step of uniformly mixing the light-emitting material dispersion liquid and the electron acceptor dopant dispersion liquid to obtain the light-emitting material composition comprises:
and dropwise adding the electron acceptor dopant dispersion liquid into the luminescent material dispersion liquid, and uniformly mixing the mixture in a shaking way after each drop of the electron acceptor dopant dispersion liquid is added until the electron acceptor dopant dispersion liquid is added, so as to obtain the luminescent material composition.
5. A light-emitting diode, wherein the material of the light-emitting layer of the light-emitting diode comprises the light-emitting material composition according to any one of claims 1 to 2, or the light-emitting material composition prepared by the preparation method according to claim 3 or 4.
6. A preparation method of a light-emitting diode is characterized by comprising the following steps:
the luminescent material composition according to any one of claims 1 to 2 is used as a raw material, and a luminescent layer is formed by sequentially performing coating, vacuuming and heat treatment.
7. The method for manufacturing the light-emitting diode according to claim 6, wherein the heat treatment temperature is 110 to 130 ℃ and the treatment time is 10 to 40min.
8. A display device comprising the light-emitting diode according to claim 5 or the light-emitting diode manufactured by the manufacturing method according to claim 6 or 7.
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