CN111384249B - Composite material, preparation method thereof and quantum dot light-emitting diode - Google Patents
Composite material, preparation method thereof and quantum dot light-emitting diode Download PDFInfo
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Abstract
The invention belongs to the technical field of materials, and particularly relates to a composite material, a preparation method thereof and a quantum dot light-emitting diode. The composite material includes p-type metal oxide nanoparticles and nitrogen-doped graphdine dispersed in the p-type metal oxide nanoparticles. The nitrogen-doped graphdiyne is dispersed in the p-type metal oxide nano particles, and the formed composite material is used for a hole transport material, so that the hole transport efficiency can be improved, and the luminous efficiency of a device is improved.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a composite material, a preparation method thereof and a quantum dot light-emitting diode.
Background
Quantum dot light emitting diodes (QLEDs) are a new generation of excellent display technology due to their advantages of high light emitting efficiency, high color purity, narrow light emitting spectrum, tunable emission wavelength, etc., and the major problems that currently limit the large-scale commercial application of QLEDs are their short device lifetime and poor stability, among which the most important problem is that the efficiency of the hole injection layer and the hole transport layer in the device structure is too low to balance with the electron transport efficiency.
At present, the transmission performance of a hole transport layer material is generally far lower than that of an electron transport layer, charge transport of a device is difficult to balance, electrons are easy to accumulate in the electron layer and even pass through a quantum dot light emitting layer to directly reach the hole layer for compounding, and therefore the light emitting efficiency is low. PEDOT: PSS (poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid) is an excellent conductive material with high light transmittance and high work function, and is the most commonly used QLED hole injection layer material at present, however, a great deal of research shows that the PEDOT: PSS has the characteristics of acidity, easiness in water absorption and the like, and is easy to corrode an electrode and destroy the stability of a device. The metal oxide hole transport material has more stable property and service life, but the hole transport efficiency is generally lower.
The graphene has natural direct band gap, conductivity comparable to that of graphene materials, and intrinsic hole mobility (up to 4.29 multiplied by 10) higher than that of graphene at room temperature5cm2·V-1·s-1) The excellent semiconductor carbon material has extremely high application potential in the field of semiconductor materials, and can be used for improving the performance of hole transport materials after being modified.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides a composite material, a preparation method thereof and a quantum dot light-emitting diode, and aims to solve the technical problem that the hole transmission effect of the existing hole transmission material is not ideal.
In order to achieve the purpose, the invention adopts the following technical scheme:
in one aspect, the invention provides a composite material comprising p-type metal oxide nanoparticles and nitrogen-doped graphdine dispersed in the p-type metal oxide nanoparticles.
The composite material provided by the invention comprises p-type metal oxide nanoparticles and nitrogen-doped grapyne dispersed in the p-type metal oxide nanoparticles, wherein nitrogen atoms can be doped into a grapyne structure in a form of substituting sp-N for carbon atoms of acetylene bonds, and after nitrogen doping modification, the nitrogen atom radius is smaller than that of the carbon atoms, so that the plane interval of the nitrogen-doped grapyne is reduced compared with that of the grapyne, and the charge transmission performance between planes of the grapyne can be further improved; the nitrogen-doped graphdiyne is dispersed in the p-type metal oxide nano particles, and the formed composite material is used for a hole transport material, so that the hole transport efficiency can be improved, and the luminous efficiency of a device is improved.
The invention also provides a preparation method of the composite material, which comprises the following steps:
providing nitrogen-doped graphdiyne and a p-type metal oxide;
dissolving the nitrogen-doped graphdiyne and the p-type metal oxide in a solvent to obtain a precursor solution;
and depositing the precursor solution on a substrate to obtain the composite material.
The preparation method of the composite material provided by the invention directly dissolves the nitrogen-doped graphdiyne and the p-type metal oxide in a solvent, and then deposits the nitrogen-doped graphdiyne and the p-type metal oxide on a substrate for annealing to obtain the composite material. The preparation method has simple process and low cost, the finally obtained composite material can obviously improve the charge transmission performance, and when the composite material is used for a hole transmission material, the hole transmission efficiency can be improved, so that the luminous efficiency of a device is improved.
Finally, the invention provides a quantum dot light-emitting diode, which comprises an anode, a cathode and a quantum dot light-emitting layer positioned between the anode and the cathode, wherein a hole transport layer is also arranged between the anode and the quantum dot light-emitting layer, and the material of the hole transport layer is the composite material.
The hole transport layer in the quantum dot light-emitting diode consists of the special composite material, so that the device can improve the hole transport efficiency and has good luminous efficiency.
Drawings
FIG. 1 is a flow chart of a method for preparing a composite material according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a quantum dot light-emitting diode according to embodiment 4 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In one aspect, embodiments of the present invention provide a composite material comprising p-type metal oxide nanoparticles and nitrogen-doped graphdine dispersed in the p-type metal oxide nanoparticles.
The composite material provided by the embodiment of the invention comprises p-type metal oxide nanoparticles and nitrogen-doped grapyne dispersed in the p-type metal oxide nanoparticles, wherein nitrogen atoms can be doped into a grapyne structure in a manner that sp-N replaces carbon atoms of acetylene bonds, and after nitrogen doping modification, the nitrogen atom radius is smaller than that of the carbon atoms, so that compared with the grapyne, the plane interval of the nitrogen-doped grapyne is reduced, and the charge transmission performance between planes of the grapyne can be further improved; the nitrogen-doped graphdiyne is dispersed in the p-type metal oxide nano particles, and the formed composite material is used for a hole transport material, so that the hole transport efficiency can be improved, and the luminous efficiency of a device is improved.
The Graphoyne (GDY) has very high intrinsic hole mobility (up to 4.29X 10) at room temperature5cm2·V-1·s-1) The carbon material is an excellent semiconductor carbon material and has great application potential. And sp-N is doped with the graphdine, so that the charge transmission performance between planes of the graphdine can be further improved. The composite material provided by the embodiment of the invention is used as a hole transport material, the main material of the composite material is a metal oxide material with the forbidden band width of about 4.0eV and good hole transport performance, and the charge transport performance of the composite material can be obviously improved by adding the nitrogen-doped graphdiyne, so that the effect of improving the luminous efficiency of a QLED device is achieved.
In an effective embodiment of the invention, the nitrogen atoms in the nitrogen-doped graphdiyne are bonded to the p-type metal oxide nanoparticles. The doping of nitrogen atoms generates a large amount of heteroatom defects and active centers, and a coordination site can be formed when the nitrogen atoms are subsequently mixed with p-type metal oxide particles, namely, N atoms and metal oxides form coordination bonds, so that the effect of connecting metal particles and charge transmission among the particles is achieved, and the hole transmission efficiency of the nitrogen-doped graphite alkyne-metal oxide mixed material can be further improved after film forming.
Further, in the composite material provided by the embodiment of the invention, the number ratio of the alkyne bonds (namely sp-N bonds) substituted by nitrogen in the nitrogen-doped graphdiyne is 10-50%; namely 10-50 acetylene bonds in 100 acetylene bonds are replaced by nitrogen, the nitrogen-doped graphyne with the proportion is most stable, and the N atoms can be ensured to replace acetylene bond C atoms by sp-N. Preferably, the particle size of the nitrogen-doped graphdine is 1-10 nm.
Further, the nitrogen-doped graphdiyne is selected from at least one of nitrogen-doped graphdiyne nano-microspheres, nitrogen-doped graphdiyne nano-wires, nitrogen-doped graphdiyne nano-rods and nitrogen-doped graphdiyne nanocones; in an embodiment of the present invention, the material may be obtained by doping graphite alkyne nanospheres (including graphite alkyne nanospheres), graphite alkyne nanowires, graphite alkyne nanorods, and graphite alkyne nanocones with nitrogen. Or, the nitrogen-doped graphyne is selected from at least one of nitrogen-doped alpha-graphyne, nitrogen-doped beta-graphyne, nitrogen-doped gamma-graphyne, nitrogen-doped delta-graphyne and nitrogen-doped 6,6, 12-graphyne, and in an embodiment of the invention, the nitrogen-doped graphyne can be obtained by nitrogen-doping alpha-graphyne (alpha-GY), beta-graphyne (beta-GY), gamma-graphyne (gamma-GY), delta-graphyne (delta-GY), 6,6, 12-graphyne (6,6, 12-GY).
Further, the mass ratio of the p-type metal oxide nanoparticles to the nitrogen-doped graphdine is 100: (2-10). Still further, the p-type metal oxide nanoparticles are selected from at least one of nickel oxide nanoparticles, molybdenum oxide nanoparticles, vanadium oxide nanoparticles, and tungsten oxide nanoparticles.
On the other hand, the embodiment of the invention also provides a preparation method of the composite material, as shown in fig. 1, comprising the following steps:
s01: providing nitrogen-doped graphdiyne and a p-type metal oxide;
s02: dissolving the nitrogen-doped graphdiyne and the p-type metal oxide in a solvent to obtain a precursor solution;
s03: and depositing the precursor solution on a substrate to obtain the composite material.
According to the preparation method of the composite material provided by the embodiment of the invention, the nitrogen-doped graphdiyne and the p-type metal oxide are directly dissolved in the solvent and then deposited on the substrate for annealing, so that the composite material is obtained. The preparation method has simple process and low cost, the finally obtained composite material can obviously improve the charge transmission performance, and when the composite material is used for a hole transmission material, the hole transmission efficiency can be improved, so that the luminous efficiency of a device is improved.
Further, in the above step S01, the p-type metal oxide is at least one selected from the group consisting of nickel oxide, molybdenum oxide, vanadium oxide, and tungsten oxide. The preparation method of the nitrogen-doped graphdiyne comprises the following steps: and placing the graphdiyne in an inert atmosphere environment containing ammonia gas, and heating to obtain the nitrogen-doped graphdiyne.
Preferably, the temperature of the heating treatment is 250-300 ℃; the time of the heating treatment is 20-40 min. More optionally, the heating treatment is carried out by placing the graphdiyne in an inert atmosphere with the volume fraction of ammonia gas being 1-5%. Within the range, the quantity ratio of alkyne bonds substituted by nitrogen formed by the graphathpane after the graphathpane is fully reacted is 10-50%, the nitrogen-doped graphathpane is most stable in the ratio, and the N atoms can be ensured to substitute the C atoms of the alkyne bonds by sp-N; if the ammonia gas concentration is too high, excessive nitridation is easily caused, other pi bonds and conjugate bonds in the graphyne structure are damaged, so that the graphyne intrinsic structure is decomposed, and if the ammonia gas concentration is too low, the nitrogen doping degree is low, and the modification effect is not obvious. The reaction temperature is preferably 250-300 ℃, and N atoms in ammonia gas have enough reactivity to replace acetylene bond C atoms in the temperature range; if the reaction temperature is too high, the graphite alkyne structure is easily damaged.
Further, the graphite alkyne can be one or more of graphite alkyne nano microspheres, graphite alkyne nanowires, graphite alkyne nano rods, graphite alkyne nano cones, graphite alkyne nano hollow spheres and the like with the particle size of 1-10nm, and can be graphite alkyne with various configurations such as alpha-graphite alkyne (alpha-GY), beta-graphite alkyne (beta-GY), gamma-graphite alkyne (gamma-GY), delta-graphite alkyne (delta-GY), 6,6, 12-graphite alkyne (6,6,12-GY) and the like;
further, in the above step S02, the solvent may be polar or non-polar, specifically selected from at least one of isopropyl alcohol, ethanol, propanol, butanol, pentanol and hexanol;
finally, the invention provides a quantum dot light-emitting diode, which comprises an anode, a cathode and a quantum dot light-emitting layer positioned between the anode and the cathode, wherein a hole transport layer is also arranged between the anode and the quantum dot light-emitting layer, and the material of the hole transport layer is the composite material.
The hole transport layer in the quantum dot light-emitting diode provided by the embodiment of the invention is made of the special composite material, so that the device can improve the hole transport efficiency and has good luminous efficiency.
In a specific embodiment, the preparation method of the quantum dot light emitting diode comprises the following steps:
a: firstly, growing a hole transport layer on a substrate; wherein the material of the hole transport layer is a nitrogen-doped graphyne hybridized metal oxide as described above;
b: then depositing a quantum dot light-emitting layer on the hole transport layer;
c: and finally, depositing an electron transmission layer on the quantum dot light-emitting layer, and evaporating a cathode on the electron transmission layer to obtain the light-emitting diode.
The preparation method of the light-emitting diode is characterized in that the quantum dots of the quantum dot light-emitting layer are one of red, green and blue. Can be at least one 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 structure quantum dots or alloy structure quantum dots. Then the quantum dots can be any one of the three common red, green and blue quantum dots or other yellow light, and the quantum dots can 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.
Further, the obtained QLED is subjected to a packaging process, and the packaging process may be performed by a common machine or by a manual method. Preferably, the oxygen content and the water content in the packaging treatment environment are both lower than 0.1ppm so as to ensure the stability of the device.
And depositing the prepared nitrogen-doped graphyne-hybridized metal oxide mixed solution on an anode substrate by a deposition method which can be but not limited to a spin coating method, a blade coating method, a printing method, a spraying method, a roll coating method, an electrodeposition method and the like and is not limited to a deposition method which can form a film layer so as to prepare the nitrogen-doped graphyne-hybridized metal oxide hole transport layer. Preferably, the thickness of the nitrogen-doped graphyne hybrid metal oxide hole injection layer is 10-100 nm.
The invention is described in further detail with reference to a part of the test results, which are described in detail below with reference to specific examples.
Example 1
The details are described below by taking α -graphyne (α -GY) nanoparticle powder, n-butanol solvent, and nickel oxide nanoparticles as examples:
1) uniformly spreading alpha-graphite alkyne powder on a watch glass, and heating to a certain temperature of 250 ℃ in an argon atmosphere;
2) slowly introducing 5% ammonia (balanced by 95% argon gas) into the graphite alkyne powder, and continuously heating and introducing the ammonia gas for 30 minutes to obtain a nitrogen-doped graphite alkyne material;
3) dispersing nitrogen-doped graphdiyne and nickel oxide particles in n-butanol solvent and stirring for a certain time to obtain a mixed colloidal solution of the hole transport material;
4) and depositing the mixed solution of the nitrogen-doped graphite alkyne hybridized nickel oxide hole transport material on an anode substrate to prepare a hole transport material layer.
5) And depositing a quantum dot light-emitting layer, an electron transport layer and a cathode on the hole transport layer in sequence to obtain the QLED device.
Example 2
The details are described below by taking delta-graphyne (delta-GY) nanoparticle powder, ethanol solvent, and molybdenum oxide nanoparticles as examples:
1) uniformly spreading delta-graphdine powder on a watch glass, and heating to a certain temperature of 250 ℃ in an argon atmosphere;
2) slowly introducing 5% ammonia (balanced by 95% argon gas) into the graphite alkyne powder, and continuously heating and introducing the ammonia gas for 30 minutes to obtain a nitrogen-doped graphite alkyne material;
3) dispersing nitrogen-doped graphdiyne and molybdenum oxide particles in an ethanol solvent and stirring for a certain time to obtain a mixed colloidal solution of the hole transport material;
4) and depositing the mixed solution of the nitrogen-doped graphite alkyne hybridized molybdenum oxide hole transport material on an anode substrate to prepare a hole transport material layer.
5) And depositing a quantum dot light-emitting layer, an electron transport layer and a cathode on the hole transport layer in sequence to obtain the QLED device.
Example 3
The details are described below by taking gamma-graphite alkyne (gamma-GY) nano microsphere powder, ethanol solvent and tungsten oxide nano particles as examples:
1) uniformly spreading gamma-graphite alkyne powder on a watch glass, and heating to a certain temperature of 250 ℃ in an argon atmosphere;
2) slowly introducing 5% ammonia (balanced by 95% argon gas) into the graphite alkyne powder, and continuously heating and introducing the ammonia gas for 30 minutes to obtain a nitrogen-doped graphite alkyne material;
3) dispersing nitrogen-doped graphdiyne and tungsten oxide particles in an ethanol solvent and stirring for a certain time to obtain a mixed colloidal solution of the hole transport material;
4) and depositing the mixed solution of the nitrogen-doped graphdine hybridized tungsten oxide hole transport material on an anode substrate to prepare a hole transport material layer.
5) And depositing a quantum dot light-emitting layer, an electron transport layer and a cathode on the hole transport layer in sequence to obtain the QLED device.
Example 4
As shown in fig. 2, a schematic structural diagram of a quantum dot light emitting diode, the preparation method comprises the following steps:
a: firstly, growing a hole injection layer on a substrate;
b: then depositing a hole transport layer on the hole injection layer; wherein the material of the hole transport layer is a mixture of nitrogen-doped graphdine and p-type metal oxide nanoparticles.
C: then depositing a quantum dot light-emitting layer on the hole transport layer;
d: and finally, depositing an electron transmission layer on the quantum dot light-emitting layer, and evaporating a cathode on the electron transmission layer to obtain the light-emitting diode.
Fig. 1 is a schematic structural diagram of a QLED device in this embodiment, and the device includes, in order from bottom to top, a substrate 1, an anode 2, a hole injection layer 3, a hole transport layer 4, a quantum dot light-emitting layer 5, an electron transport layer 6, and a cathode 7. PSS, a hole injection layer 3, a hole transport layer 4, ZnO, an electron transport layer 6 and a cathode 7, wherein the substrate 1 is made of a glass sheet, the anode 2 is made of an ITO substrate, the hole injection layer 3 is made of PEDOT, the nitrogen-doped graphdine and p-type metal oxide nanoparticle mixture is made of the hole transport layer 4, the electron transport layer 6 is made of ZnO, and the cathode 7 is made of Al.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. A composite material comprising p-type metal oxide nanoparticles and nitrogen-doped graphdine dispersed in the p-type metal oxide nanoparticles, wherein nitrogen atoms in the nitrogen-doped graphdine are bonded to the p-type metal oxide nanoparticles.
2. The composite material of claim 1, wherein the nitrogen atoms in the nitrogen-doped graphdiyne are doped into the graphdiyne structure in the form of sp-N bonds instead of alkyne-bonded carbon atoms.
3. The composite material of claim 1, wherein the nitrogen-doped graphdiyne has a ratio of the number of alkyne bonds substituted by nitrogen of 10-50%; and/or the presence of a gas in the gas,
the mass ratio of the p-type metal oxide nanoparticles to the nitrogen-doped graphdiyne is 100: (2-10).
4. The composite material of claim 1, wherein the nitrogen-doped graphdine has a particle size of 1-10 nm; and/or the presence of a gas in the gas,
the nitrogen-doped graphdiyne is selected from at least one of nitrogen-doped graphdiyne nano-microspheres, nitrogen-doped graphdiyne nano-wires, nitrogen-doped graphdiyne nano-rods and nitrogen-doped graphdiyne nano-cones; and/or the presence of a gas in the gas,
the nitrogen-doped graphdiyne is selected from at least one of nitrogen-doped alpha-graphdiyne, nitrogen-doped beta-graphdiyne, nitrogen-doped gamma-graphdiyne, nitrogen-doped delta-graphdiyne and nitrogen-doped 6,6, 12-graphdiyne; and/or the presence of a gas in the gas,
the p-type metal oxide nanoparticles are selected from at least one of nickel oxide nanoparticles, molybdenum oxide nanoparticles, vanadium oxide nanoparticles, and tungsten oxide nanoparticles.
5. A method for preparing a composite material according to any one of claims 1 to 4, comprising the steps of:
providing nitrogen-doped graphdiyne and a p-type metal oxide;
dissolving the nitrogen-doped graphdiyne and the p-type metal oxide in a solvent to obtain a precursor solution;
and depositing the precursor solution on a substrate to obtain the composite material.
6. The method of claim 5, wherein the method of preparing the nitrogen-doped graphdiyne comprises: and placing the graphdiyne in an inert atmosphere environment containing ammonia gas, and heating to obtain the nitrogen-doped graphdiyne.
7. The method as claimed in claim 6, wherein the temperature of the heat treatment is 250-300 ℃; and/or the presence of a gas in the gas,
the heating treatment time is 20-40 min; and/or the presence of a gas in the gas,
and placing the graphdiyne in an inert atmosphere environment with the volume fraction of ammonia gas being 1-5%, and carrying out the heating treatment.
8. The method according to claim 5, wherein the solvent is at least one selected from the group consisting of isopropyl alcohol, ethyl alcohol, propyl alcohol, butyl alcohol, amyl alcohol and hexyl alcohol; and/or
The p-type metal oxide is at least one selected from nickel oxide, molybdenum oxide, vanadium oxide and tungsten oxide; and/or the presence of a gas in the gas,
the graphdiyne is selected from at least one of graphdiyne nano-microspheres, graphdiyne nanowires, graphdiyne nano-rods and graphdiyne nanocones; and/or the presence of a gas in the gas,
the graphoyne is selected from at least one of alpha-graphoyne, beta-graphoyne, gamma-graphoyne, delta-graphoyne and 6,6, 12-graphoyne.
9. A quantum dot light-emitting diode, comprising an anode, a cathode and a quantum dot light-emitting layer positioned between the anode and the cathode, wherein a hole transport layer is further arranged between the anode and the quantum dot light-emitting layer, and the material of the hole transport layer is the composite material of any one of claims 1 to 4.
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| CN104377304A (en) * | 2014-09-12 | 2015-02-25 | 中国科学院物理研究所 | Perovskite-based thin film solar cell and preparing method thereof |
| CN204243085U (en) * | 2014-09-12 | 2015-04-01 | 中国科学院物理研究所 | Perovskite-based thin-film solar cells |
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