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CN110534656B - Nano material, preparation method and quantum dot light-emitting diode - Google Patents

Nano material, preparation method and quantum dot light-emitting diode Download PDF

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CN110534656B
CN110534656B CN201810518684.2A CN201810518684A CN110534656B CN 110534656 B CN110534656 B CN 110534656B CN 201810518684 A CN201810518684 A CN 201810518684A CN 110534656 B CN110534656 B CN 110534656B
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moo
nano
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nanoparticles
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CN110534656A (en
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何斯纳
吴龙佳
吴劲衡
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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
    • 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]
    • H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
    • H10K50/115—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising active inorganic nanostructures, e.g. luminescent quantum dots

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Abstract

The invention discloses a nano material, a preparation method and a quantum dot light-emitting diode, wherein the nano material comprises the following components: MoO3Nanoparticles and MoS2Nanosheets, said MoS2Nanosheets being bound to the MoO3The surface of the nanoparticles. MoS2Nanosheet and MoO3The nanometer particles have synergistic effect, and can improve the hole transmission efficiency, thereby improving the luminous efficiency and performance of the quantum dot light-emitting diode.

Description

Nano material, preparation method and quantum dot light-emitting diode
Technical Field
The invention relates to the field of quantum dot light-emitting devices, in particular to a nano material, a preparation method and a quantum dot light-emitting diode.
Background
In current quantum dot light emitting diodes, ITO is generally used as a transparent electrode. And PEDOT: PSS is usually used for modifying the ITO surface to be used as an anode buffer layer. But the performance of the quantum dot light emitting diode is reduced due to the acidity of PEDOT (Poly ethylene terephthalate) PSS. To solve this problem, new anode buffer layers have been developed to replace PEDOT: PSS. Wherein the transition metal oxide (WO)3、MoO3、NiO、Cu2O、ReO3And V2O5) The quantum dot light emitting diode is used as an anode buffer layer in many quantum dot light emitting diodes, and achieves good performance. Particularly, molybdenum oxide has a deep electron energy state and efficient hole injection, and some effects are obtained.
Molybdenum disulfide as a transition metal material has attracted attention of researchers at home and abroad due to its unique microstructure, adjustable energy band gap and high carrier mobility. However, a composite material composed of molybdenum oxide and molybdenum disulfide has been reported.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the above-mentioned deficiencies of the prior art, the present invention aims to provide a nano material, a method for preparing the same, and a quantum dot light emitting diode, which aims to solve the problems of the prior MoO3The hole transmission efficiency is not high.
The technical scheme of the invention is as follows:
a nanomaterial, comprising: MoO3Nanoparticles and MoS2Nanosheets, said MoS2Nanosheets being bound to the MoO3The surface of the nanoparticles.
A method for preparing a nano material, comprising the following steps:
providing MoO3A nanoparticle;
mixing the MoO3Mixing the nano particles with a sulfur source, and carrying out hydrothermal reaction on the mixture in MoO3MoS grown on surface of nano-particles2Nanosheets, resulting in the nanomaterial.
A quantum dot light-emitting diode comprises a hole transport layer, wherein the material of the hole transport layer comprises the nano material.
Has the advantages that: the nano material comprises MoO3Nanoparticles and MoS2Nanosheets, MoS2Nanosheet and MoO3The hole transmission efficiency is improved by the synergistic effect of the nano particles, so that the luminous efficiency and the performance of the quantum dot light-emitting diode are improved. The preparation method of the nano material is simple and is suitable for large-area and large-scale preparation.
Drawings
Fig. 1 is a schematic structural diagram of a quantum dot light emitting diode provided by the present invention.
Detailed Description
The invention provides a nano material, a preparation method thereof and a quantum dot light-emitting diode, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a nano material, which comprises the following components: MoO3Nanoparticles and MoS2Nanosheets, said MoS2Nano-bound in said MoO3The surface of the nanoparticles.
The nano material comprises MoO3Nanoparticles bound to said MoO3MoS of nanoparticle surface2Nanosheets, MoS2Nanosheet and MoO3The synergistic effect of the core-shell structure of the nano particles improves the hole transmission efficiency, thereby improving the luminous efficiency and the performance of the quantum dot light-emitting diode.
In a preferred embodiment, a plurality of said MoS' s2Nanosheets being bound to the MoO3Surface of nanoparticles, a plurality of said MoS2Nanosheets being bound to the MoO3Three-dimensional surface of nanoparticles in said MoO3MoS formation on the surface of nanoparticles2A nanosheet shell. In the MoO3MoS formation on the surface of nanoparticles2Nanosheet shell, said MoS2The nano-sheet can protect MoO with relatively high activity to a certain extent3A nanoparticle; simultaneously, MoS of the surface2The nano sheet can be MoO3The nano particles are better dispersed in the solvent, and the dispersibility is improved.
The MoS2Nanosheets being bound to the MoO3The form of the nanoparticle surface is various.
In a preferred embodiment, a plurality of said MoS' s2Nanosheets grown in and bonded to the MoO3On the surface of nanoparticles, in the MoO3MoS formation on the surface of nanoparticles2A nanosheet shell. The nano material obtained by adopting a growth combination mode further reduces MoO3The surface of the nano-particles has defects, and the performance is more stable。
In a preferred embodiment, the nanomaterial has a particle size of 10 to 15 nm.
In a preferred embodiment, the MoO is3The particle size of the nano-particles is 5-10 nm.
In a preferred embodiment, the MoS is a solid-state imaging device2The thickness of the nano-sheet is 2-4 nm.
The invention also provides a preparation method of the nano material, which comprises the following steps:
step S100, providing MoO3A nanoparticle;
step S200, the MoO is processed3Mixing the nano particles with a sulfur source, and carrying out hydrothermal reaction on the mixture in MoO3MoS grown on surface of nano-particles2Nanosheets, resulting in the nanomaterial.
The MoO is prepared by a simple hydrothermal method3Nanoparticles and MoS2Nanosheets, said MoS2Nanosheets grown on the MoO3Nano material on the surface of the nano particles. The preparation method of the nano material is simple and is suitable for large-area and large-scale preparation.
In the step S100, in a preferred embodiment, the MoO3The nano-particles are prepared by the following method: dissolving a molybdenum source in water, adding acid, carrying out hydrothermal reaction under the condition of heat preservation, and sequentially cooling, washing and drying to obtain the MoO3And (3) nanoparticles.
In a more preferred embodiment, the molybdenum source is selected from the group consisting of soluble sodium molybdate, amine molybdate, potassium molybdate, magnesium molybdate, and the like, without limitation to one or more thereof.
In a more preferred embodiment, the acid is selected from the group consisting of concentrated sulfuric acid, concentrated nitric acid, concentrated hydrochloric acid, and the like, without being limited thereto. Adding acid to the solution pH<1 is most preferred. MoO3The formation process can be carried out by the following three chemical reaction equations: (1) MoO4 2- + H+ = HMoO4 -；（2）HMoO4 - + H+ = H2MoO4(aq)；（3）H2MoO4(aq) =MoO3·H2And O. During the hydrothermal reaction, H in the system+More and more favor of H2MoO4To further obtain more MoO3(ii) a If H is+The reaction process tends to be slow, and the reaction time needs to be increased; the reaction time is increased, and large-particle MoO is easily caused3And (5) forming crystals. Thus, the pH<1 is most preferred.
In a more preferred embodiment, the temperature of the hydrothermal reaction is 150-220-oC; the time of the hydrothermal reaction is 18-30 h.
In a more preferred embodiment, the temperature of drying is from 50 to 60 deg.CoC。
In the step S200, in a preferred embodiment, the method specifically includes: mixing the MoO3Dispersing the nano particles in a solvent to obtain MoO3A nanoparticle dispersion; in the MoO3Adding a sulfur source into the nano-particle dispersion liquid, and carrying out a hydrothermal reaction on MoO under the condition of heat preservation3MoS grown on surface of nano-particles2Nanosheets, resulting in the nanomaterial.
In a more preferred embodiment, the MoO is added in a molar ratio of molybdenum to sulfur of 1 (1-1.5)3The nanoparticles are mixed with the sulfur source. Simple MoO3The product is a particle structure with smooth surface, the surface of the product after hydrothermal reaction becomes rough with the addition of sulfur element, and when the molar ratio of molybdenum element to sulfur element is less than 1: (1-1.5) the resulting product surface is predominantly with microscopic MoS2The surface of the nano-sheet becomes rough and uneven; when the molar ratio of molybdenum element to sulfur element is about 1: (1-1.5) in MoO3The surface of the nano-particles grows a large amount of MoS2Nano sheets are uniformly distributed; when the molar ratio of the molybdenum element to the sulfur element is more than 1: (1-1.5) time, MoO3MoS of nanoparticle surface2The number of nano sheets is increased, and the surface even appears flower balls assembled by sheets along with the reaction. The appearance of the flower ball is not well formed with MoO3The nano-particles are core, MoS2Core-shell structure with nanosheet as shellAnd (3) nano materials. Thus, the molar ratio of molybdenum to sulfur is maintained at about 1: (1-1.5) is most preferred.
In a more preferred embodiment, the sulfur source is selected from one or more of thiourea, sodium polysulfide, thioacetamide, and amine sulfide, without limitation.
In a more preferred embodiment, the hydrothermal reaction is carried out in MoO3MoS grown on surface of nano-particles2The temperature of the nano-sheet is 150-220 DEG CoC; the hydrothermal reaction is carried out in MoO3MoS grown on surface of nano-particles2The time of the nano-sheet is 18-30 h.
Further, the pure nano material is obtained through cooling, washing and drying.
In a more preferred embodiment, the temperature of drying is from 50 to 60 deg.CoC。
MoS2As the most representative material in the two-dimensional transition metal sulfide layered nanometer material, due to the unique microstructure, the adjustable energy band gap (1.13-1.87 eV) and the higher carrier mobility, the defect of zero band gap of graphene can be overcome, and the defect of low layered carrier mobility can be overcome, so that the material is an ideal hole transport material. The invention utilizes a hydrothermal method to prepare a nano material, MoO, with a core-shell structure3Nanoparticles as nuclei, grown on MoO3Ultra-thin MoS of nanoparticle surfaces2Nanosheets as shells; the preparation method of the nano material is simple and is suitable for large-area and large-scale preparation. In the nano material of the invention, MoS as a shell material2The nano-sheet can protect MoO with relatively high activity to a certain extent3Nanoparticles, reduction of MoO3A nanoparticle surface defect; simultaneously, MoS grown on the surface2The nano sheet can be MoO3The nano particles are better dispersed in the solvent, so that the dispersibility is improved; compared with MoS2，MoO3The hole transport performance is better, and the fast transfer of holes can be ensured; MoS2Nanosheet and MoO3The synergistic effect of the core-shell structure of the nano particles improves the hole transmission efficiency, thereby improving the quantum dotLight emitting efficiency and performance of the light emitting diode.
The invention also provides a quantum dot light-emitting diode which comprises a hole transport layer, wherein the material of the hole transport layer comprises the nano material. In a preferred embodiment, the hole transport layer has a thickness of 20 to 60 nm.
The quantum dot light emitting diode in the prior art has various forms, and the invention will be mainly described by taking the quantum dot light emitting diode as shown in fig. 1 as an example. Specifically, as shown in fig. 1, the quantum dot light emitting diode includes a substrate 1, an anode 2, a hole transport layer 3, a quantum dot light emitting layer 4, an electron transport layer 5, and a cathode 6, which are stacked from bottom to top. Wherein the material of the hole transport layer 3 comprises the nanomaterial of the present invention.
In a preferred embodiment, the hole transport layer has a thickness of 20 to 60 nm. The quantum dot light-emitting diode has higher luminous efficiency under the thickness.
In a preferred embodiment, the substrate may be selected from glass, PET, PI, etc., without being limited thereto.
In a preferred embodiment, the anode may be selected from one or more of indium doped tin oxide (ITO), fluorine doped tin oxide (FTO), antimony doped tin oxide (ATO), aluminium doped zinc oxide (AZO).
In a preferred embodiment, the material of the quantum dot light-emitting layer may be one or more selected from red quantum dots, green quantum dots, blue quantum dots, and may also be yellow quantum dots. By way of example, the material of the quantum dot light emitting layer may be one or more of CdS, CdSe, CdTe, ZnO, ZnS, ZnSe, ZnTe, GaAs, GaP, GaSb, HgS, HgSe, HgTe, InAs, InP, InSb, AlAs, AlP, CuInS, CuInSe, and various core-shell structured quantum dots or alloy structured quantum dots. The quantum dots may be cadmium-containing or cadmium-free. The quantum dot light-emitting layer of the material has the characteristics of wide and continuous excitation spectrum distribution, high emission spectrum stability and the like.
In a preferred embodimentThe material of the electron transport layer may be selected from materials with good electron transport properties, such as but not limited to n-type ZnO, TiO2、Fe2O3、SnO2、Ta2O3One or more of AlZnO, ZnSnO, InSnO and the like. In a further preferred embodiment, the material of the electron transport layer is selected from the group consisting of n-type ZnO, n-type TiO2One kind of (1).
The invention also provides a preparation method of the quantum dot light-emitting diode, which comprises the following steps:
providing a substrate, and forming an anode on the substrate;
depositing a hole transport layer, a quantum dot light emitting layer and an electron transport layer on the anode in sequence; wherein the material of the hole transport layer comprises the nanomaterial of the present invention;
and (3) evaporating and plating a cathode on the electron transmission layer to prepare the quantum dot light-emitting diode.
In order to obtain a high quality hole transport layer, the substrate containing the anode needs to be subjected to a pretreatment process. Taking an anode-containing substrate as ITO glass as an example, the specific processing steps comprise: cleaning the whole ITO glass with a cleaning agent to primarily remove stains on the surface, then sequentially carrying out ultrasonic cleaning in deionized water, acetone, absolute ethyl alcohol and deionized water for 20 min respectively to remove impurities on the surface, and finally blowing dry with high-purity nitrogen to obtain the treated ITO glass.
Further, the step of depositing the hole transport layer on the surface of the substrate including the anode specifically includes: spin coating a solution of a hole transport layer material with a certain concentration on the pretreated substrate containing the anode, controlling the thickness of the hole transport layer to about 20-60 nm by adjusting the concentration of the solution, the spin coating speed and the spin coating time, and then performing the spin coating on the substrate at 300-350 DEG CoC, annealing to form a film. The step can be annealing in air or in nitrogen atmosphere, and the annealing atmosphere is selected according to actual needs.
Further, the step of preparing the quantum dot light emitting layer on the hole transport layer specifically includes: the prepared substrate with the hole transport layer is placed on a spin coater, the prepared quantum dot luminescent substance solution with a certain concentration is subjected to spin coating to form a film, the thickness of the quantum dot luminescent layer is controlled to be about 20-60 nm by adjusting the concentration of the solution, the spin coating speed and the spin coating time, and then the film is dried at a proper temperature to form the film.
Further, the step of preparing the electron transport layer on the quantum dot light emitting layer specifically includes: the prepared substrate of the quantum dot light emitting layer is placed in a vacuum evaporation chamber, an electron transmission layer with the thickness of about 80 nm is evaporated, the evaporation speed is about 0.01-0.5 nm/s, and annealing is carried out at a proper temperature to form a film.
Further, the step of preparing the cathode on the electron transport layer specifically includes: the substrate deposited with the functional layers is placed in an evaporation bin, a layer of 15-30 nm metal silver or aluminum and the like is thermally evaporated through a mask plate to be used as a cathode, or a nano Ag wire or a Cu wire and the like are used, and the materials have low resistance so that carriers can be smoothly injected.
The invention also comprises the following steps: and carrying out packaging treatment on the obtained quantum dot light-emitting diode, wherein the packaging treatment can adopt common machine packaging or manual packaging. Preferably, in the environment of the packaging treatment, the oxygen content and the water content are both lower than 0.1 ppm so as to ensure the stability of the quantum dot light-emitting diode.
The present invention will be described in detail below with reference to examples.
Example 1: the preparation of the nanomaterial by using ammonium molybdate, concentrated nitric acid and ammonium sulfide is described in detail below.
(1) 1 g of ammonium molybdate was added to 20 mL of water to be completely dissolved, 3 mL of concentrated nitric acid was added, and the mixture was stirred for 30 min. Then transferred to a hydrothermal reaction kettle at 200 DEGoReacting for 24 h under C, then cooling, washing (washing with water for 2 times, washing with absolute ethyl alcohol for 1 time) at 50oDrying under C to obtain MoO3A nanoparticle;
(2) drying the MoO3Ultrasonically dispersing the nano particles in 20 mL of mixed solution of water and ethanol (the volume ratio of the water to the ethanol is 2: 3) to obtain homogeneous MoO3After the nanoparticle dispersion, 0.1 g of ammonium sulfide was added and the dispersion was transferred to a hydrothermal reaction kettle at 200 foReacting for 24 h under C, then cooling, washing (washing with water for 2 times, washing with absolute ethyl alcohol for 1 time) at 50oDrying under C to obtain MoO3The nano-particles are core, MoS2The nano-sheet is a nano material with a shell core-shell structure.
Example 2: the preparation of the nanomaterial by using sodium molybdate, concentrated sulfuric acid and thiourea is described in detail below.
(1) 1 g of sodium molybdate is added into 20 mL of water to be completely dissolved, 3 mL of concentrated sulfuric acid is added, and stirring is carried out for 30 min. Then transferred to a hydrothermal reaction kettle at 200 DEGoReacting for 24 h under C, then cooling, washing (washing with water for 2 times, washing with absolute ethyl alcohol for 1 time) at 50oDrying under C to obtain MoO3A nanoparticle;
(2) drying the MoO3Ultrasonically dispersing the nano particles in 20 mL of mixed solution of water and ethanol (the volume ratio of the water to the ethanol is 2: 3) to obtain homogeneous MoO3After the nanoparticle dispersion, 0.1 g of thiourea was added and the dispersion was transferred to a hydrothermal reaction kettle at 200 foReacting for 24 h under C, then cooling, washing (washing with water for 2 times, washing with absolute ethyl alcohol for 1 time) at 50oDrying under C to obtain MoO3The nano-particles are core, MoS2The nano-sheet is a nano material with a shell core-shell structure.
Example 3: the preparation of the nanomaterial by using potassium molybdate, concentrated hydrochloric acid and thioacetamide is described in detail below.
(1) 1 g of potassium molybdate was added to 20 mL of water to be completely dissolved, 3 mL of concentrated hydrochloric acid was added thereto, and the mixture was stirred for 30 min. Then transferred to a hydrothermal reaction kettle at 200 DEGoReacting for 24 h under C, then cooling, washing (washing with water for 2 times, washing with absolute ethyl alcohol for 1 time) at 50oDrying under C to obtain MoO3A nanoparticle;
(2) drying the MoO3Nanoparticles, ultrasound dispersed in 20 mL of a mixture of water and ethanolMixing the solution (the volume ratio of water to ethanol is 2: 3) to obtain homogeneous MoO3After the nanoparticle dispersion, 0.1 g of thioacetamide was added and the dispersion was transferred to a hydrothermal reaction kettle at 200 foReacting for 24 h under C, then cooling, washing (washing with water for 2 times, washing with absolute ethyl alcohol for 1 time) at 50oDrying under C to obtain MoO3The nano-particles are core, MoS2The nano-sheet is a nano material with a shell core-shell structure.
In summary, the invention provides a nano material, a preparation method thereof and a quantum dot light emitting diode. The nano material comprises MoO3Nanoparticles bound to said MoO3MoS of nanoparticle surface2Nanosheets, comparable to MoS2，MoO3The hole transport performance is better, and the fast transfer of holes can be ensured; MoS2Nanosheet and MoO3The synergistic effect of the core-shell structure of the nano particles improves the hole transmission efficiency, thereby improving the luminous efficiency and the performance of the quantum dot light-emitting diode. The preparation method of the nano material is simple and is suitable for large-area and large-scale preparation.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.

Claims (8)

1. A quantum dot light emitting diode comprising a hole transport layer, wherein the material of the hole transport layer comprises nanomaterials, the nanomaterials comprising: MoO3Nanoparticles and MoS2Nanosheets, said MoS2Nanosheets being bound to the MoO3A nanoparticle surface;
a plurality of the MoS2Nanosheets being bound to the MoO3On the surface of nanoparticles, in the MoO3MoS formation on the surface of nanoparticles2Nanosheet shells to form a core-shell structure.
2. The quantum dot light-emitting diode of claim 1, wherein a plurality of the MoS2Nanosheets grown in and bonded to the MoO3On the surface of nanoparticles, in the MoO3MoS formation on the surface of nanoparticles2A nanosheet shell.
3. The qd-led of any one of claims 1 to 2, wherein the nanomaterial has a particle size of 10-15 nm; and/or the MoO3The particle size of the nano particles is 5-10 nm; and/or the MoS2The thickness of the nano-sheet is 2-4 nm.
4. A preparation method of a quantum dot light-emitting diode comprises a hole transport layer, and is characterized in that the material of the hole transport layer comprises a nano material, and the preparation method of the nano material comprises the following steps:
providing MoO3A nanoparticle;
mixing the MoO3Mixing the nano particles with a sulfur source, and carrying out hydrothermal reaction on the mixture in MoO3MoS grown on surface of nano-particles2Nanosheets, resulting in the nanomaterial.
5. The method of claim 4, wherein the sulfur source is selected from one or more of thiourea, sodium polysulfide, thioacetamide, and amine sulfide.
6. The method according to claim 4, wherein the MoO is added in a molar ratio of molybdenum to sulfur of 1 (1-1.5)3The nanoparticles are mixed with the sulfur source.
7. The method of claim 4, wherein the hydrothermal reaction is carried out in MoO3MoS grown on surface of nano-particles2The temperature of the nano-sheets is 150-220 ℃.
8. The method of claim 4, wherein the hydrothermal reaction is carried out in MoO3MoS grown on surface of nano-particles2The time of the nano-sheet is 18-30 h.
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