CN110600621A - Electron transport material, preparation method thereof and quantum dot light-emitting diode - Google Patents
Electron transport material, preparation method thereof and quantum dot light-emitting diode Download PDFInfo
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- 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 belongs to the technical field of quantum dots, and particularly relates to an electron transport material, a preparation method thereof and a quantum dot light-emitting diode. The electron transport material is an Al-doped ZnS nano-particle material. The preparation method of the electron transport material comprises the following steps: providing a zinc salt, an aluminum salt, and a sulfur source; dissolving the zinc salt, the aluminum salt and the sulfur source in a solvent to obtain a precursor solution; and depositing the precursor solution on a substrate, and annealing to obtain the Al-doped ZnS nano-particle material. The Al-doped ZnS nano-particle material improves the concentration of free carriers, reduces the resistance of ZnS, increases the conductivity, can move the electronic Fermi level in ZnS to a conduction band by Al doping, enables the electronic Fermi level to be shown as metallic, and reduces the forbidden bandwidth of ZnS from intrinsic 3.62eV to 3.30eV, thereby narrowing the forbidden bandwidth of ZnS.
Description
Technical Field
The invention belongs to the technical field of quantum dots, and particularly relates to an electron transport material, a preparation method thereof and a quantum dot light-emitting diode.
Background
The semiconductor quantum dots have quantum size effect, people can realize the required light emission with specific wavelength by regulating and controlling the size of the quantum dots, and the tuning range of the light emission wavelength of the CdSe QDs can be from blue light to red light. In a conventional inorganic electroluminescent device, electrons and holes are injected from a cathode and an anode, respectively, and then recombined in a light emitting layer to form excitons for light emission. Conduction band electrons in wide bandgap semiconductors can be accelerated under high electric fields to obtain high enough energy to strike QDs to cause it to emit light.
In recent years, inorganic semiconductors have been studied as an electron transport layer in a relatively hot manner. Nanometer ZnO and ZnS are wide bandgap semiconductor materials, and attract the attention of a plurality of researchers due to the advantages of quantum confinement effect, size effect, excellent fluorescence characteristic and the like. Therefore, in the last ten years, ZnO and ZnS nanomaterials have shown great potential for development in the fields of photocatalysis, sensors, transparent electrodes, fluorescent probes, diodes, solar cells, and lasers.
ZnO is an n-type semiconductor material with a direct band gap, has a wide forbidden band of 3.37eV and a low work function of 3.7eV, and the structural characteristics of the energy band determine that ZnO can become a proper electron transport layer material. Meanwhile, ZnS is a II-VI semiconductor material, has two different structures of sphalerite and wurtzite, has forbidden bandwidth (3.62eV), stable chemical property, rich resources and low price. However, zinc sulfide has been reported as an electron transport layer.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides an electron transport material, a preparation method thereof and a quantum dot light-emitting diode, and aims to solve the technical problem that the selection of the electron transport material in the conventional quantum dot light-emitting diode is limited.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an electron transport material, which is an Al-doped ZnS nanoparticle material.
According to the electron transport material provided by the invention, Al element is doped into the ZnS nano-particle material so as to greatly improve the electron transport performance; in the electron transporting material, Al is used as an Al element3+By solid solution of Al3+Occupying Zn in ZnS lattice2+Position of (3), Al3+Two of the three valence electrons form saturated bonds with sulfur, and the third electron is separated from the impurity atom to formThe energy level of the electron is slightly lower than the bottom of the conduction band, enough energy can be obtained at normal temperature and is transferred to the conduction band to be free electron, and the electron moves directionally under the action of an external electric field to conduct electricity, so that net electrons are increased as a result of Al doping, the concentration of free carriers is improved, the resistance of ZnS is reduced, the conductivity is increased, meanwhile, the electron Fermi level in ZnS can be moved to the conduction band by the Al doping, the electronic Fermi level is shown to be metallic, the forbidden bandwidth of ZnS is reduced from intrinsic 3.62eV to 3.30eV, and the forbidden bandwidth of ZnS is narrowed.
The invention also provides a preparation method of the electron transport material, which comprises the following steps:
providing a zinc salt, an aluminum salt, and a sulfur source;
dissolving the zinc salt, the aluminum salt and the sulfur source in a solvent to obtain a precursor solution;
and depositing the precursor solution on a substrate, and annealing to obtain the Al-doped ZnS nano-particle material.
The preparation method of the electron transport material provided by the invention is a simple sol-gel method, the preparation method is simple and easy to implement, and is suitable for large-area and large-scale preparation, the finally obtained electron transport material is the ZnS nano particle material doped with Al, the Al doping in the electron transport material can realize that the forbidden bandwidth of ZnS is reduced by 3.30eV from intrinsic 3.62eV, so that the forbidden bandwidth of ZnS is narrowed, the free carrier concentration of ZnS can be improved, the resistance of ZnS is reduced, the conductivity is increased, and the electron transport capability of the ZnS is improved.
The invention finally provides a quantum dot light-emitting diode which comprises a cathode, an anode and a quantum dot light-emitting layer arranged between the cathode and the anode, wherein an electron transmission layer is also arranged between the cathode and the quantum dot light-emitting layer, and the electron transmission layer is composed of the electron transmission material.
In the quantum dot light-emitting diode provided by the invention, the electron transport layer is composed of the electron transport material, the free carrier concentration of ZnS can be improved by Al doping, so that the conductivity of the material is improved, the forbidden bandwidth of ZnS is narrowed, electrons can be easily transited from an impurity energy level to enter a conduction band, and further, the electrons-holes are promoted to be effectively compounded in the quantum dot light-emitting layer, so that the influence of exciton accumulation on the performance of the device is reduced, and the performance of the device is improved.
Drawings
Fig. 1 is a schematic structural diagram of a QLED device provided in 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 an electron transport material, which is an Al-doped ZnS nanoparticle material.
According to the electron transport material provided by the embodiment of the invention, Al element is doped into the ZnS nano-particle material so as to greatly improve the electron transport performance of the ZnS nano-particle material; in the electron transporting material, Al is used as an Al element3+By solid solution of Al3+Occupying Zn in ZnS lattice2+Position of (3), Al3+Two of the three valence electrons are combined with sulfur to form saturated bonds, the third electron is separated from impurity atoms to form 1 redundant valence electron, the energy level of the electron is positioned in an energy gap and is slightly lower than the bottom of a conduction band, enough energy can be obtained to be transferred onto the conduction band to form free electrons at normal temperature, and the free electrons move directionally under the action of an external electric field to conduct electricity, so that net electrons are increased as a result of Al doping, the concentration of free carriers is improved, the resistance of ZnS is reduced, the conductivity is increased, meanwhile, the Fermi level of the electron in the ZnS can be moved to the conduction band by the Al doping, the Fermi level is shown to be metallic, the band gap of the ZnS is reduced from intrinsic 3.62eV to 3.30eV, and the band gap of the ZnS is narrowed.
Further, in the electron transport material provided in the embodiment of the present invention, a molar ratio of the Zn element to the Al element is 1: (0.01-0.05). Mol of Zn element and Al elementCompared with ZnS film performance, when the doping amount of aluminum reaches a certain value (Zn element: Al element is 1: 0.05), the solid solubility of aluminum in ZnS reaches saturation, and when the doping amount continues to increase, the aluminum is concentrated on the surface of ZnS crystal grains to form a new phase, so that the effective specific surface area of the ZnS nano-particle material is reduced, and the increase of the doping amount can also cause the mutation of crystal lattices to form new crystal lattices and Al2S3And (4) generating. However, when the doping amount of aluminum is too low, aluminum is lost during the reaction process, and thus effective doping cannot be achieved. Therefore, when the molar ratio of the Zn element to the Al element is 1: (0.01-0.05), the doping effect is the best.
Further, the molar ratio of the S element to the metal element is (0.8-1.2): 1; wherein the metal element includes Zn element and Al element. When the ratio of the S element to the sum of the molar amounts of the Zn element and the Al element is less than 0.8: 1, excessive metal elements, and incomplete doping of added Al; and greater than 1.2: when 1, the S element is excessive, and an impurity compound is easily formed and is not easily removed. Optimally, the molar ratio of the S element to the metal element is (0.8-1.2): 1, compact Al-doped ZnS nano-particle material can be obtained, and the prepared electron transport layer film has uniform particle distribution on the surface.
On the other hand, the embodiment of the invention provides a preparation method of an electron transport material, which comprises the following steps:
s01: providing a zinc salt, an aluminum salt, and a sulfur source;
s02: dissolving the zinc salt, the aluminum salt and the sulfur source in a solvent to obtain a precursor solution;
s03: and depositing the precursor solution on a substrate, and annealing to obtain the Al-doped ZnS nano material.
The preparation method of the electron transport material provided by the embodiment of the invention is a simple sol-gel method, the preparation method is simple and easy to implement, and is suitable for large-area and large-scale preparation, the finally obtained electron transport material is the Al-doped ZnS nano particle material, the Al doping in the electron transport material can realize that the forbidden bandwidth of ZnS is reduced by 3.30eV from intrinsic 3.62eV, so that the forbidden bandwidth of ZnS is narrowed, the free carrier concentration of ZnS can be improved, the resistance of ZnS is reduced, the conductivity is increased, and the electron transport capability of the ZnS is improved.
Further, in the step S01, the zinc salt is at least one selected from soluble inorganic zinc salts and organic zinc salts such as zinc acetate, zinc nitrate, zinc chloride, zinc sulfate, zinc acetate dihydrate and the like; the aluminum salt is at least one selected from aluminum nitrate, aluminum chloride, aluminum sulfate and the like; the sulfur source is at least one selected from sodium sulfide, potassium sulfide, thiourea, amine sulfide and the like.
Further, in the above step S02, the solvent is at least one selected from organic solvents such as isopropyl alcohol, ethanol, propanol, butanol, pentanol, hexanol, and the like. In the step of obtaining the precursor solution, the molar ratio of Zn element to Al element is 1: (0.01-0.05), dissolving the zinc salt and the aluminum salt in a solvent to obtain a precursor solution; the molar ratio of the zinc element to the aluminum element in the precursor solution has a large influence on the performance of the ZnS film prepared subsequently, and within the range of the molar ratio, the final electron transport material has the best electron transport performance. Further, the molar ratio of the S element to the metal element is (0.8-1.2): 1, dissolving the zinc salt, the aluminum salt and the sulfur source in a solvent to obtain a precursor solution; wherein the metal element includes Zn element and Al element. Within the range of the molar ratio, compact Al-doped ZnS nano-particle materials can be obtained, and the surface particles of the prepared electron transport layer film are uniformly distributed. Furthermore, the concentration of the metal ions in the precursor solution is 0.2-1M, and the metal ions comprise Zn2+And Al3+。
Further, in the above step S02, the zinc salt, the aluminum salt and the sulfur source are dissolved in a solvent at 60 to 80 ℃; in a specific embodiment, in order to make the precursor solution more uniform, the zinc salt, the aluminum salt and the sulfur source are dissolved in the solvent, and then the mixture is stirred and dissolved for 2 to 4 hours. The precursor solution with uniform dispersion can be quickly obtained in the temperature and time range.
Further, in the step S03, the temperature of the annealing treatment is 200-300 ℃; annealing to form a film in the temperature range, and can better remove the solvent, so that the ZnS nano-particle material film with better crystallinity and Al doping is obtained. The step can be annealing in air or in nitrogen atmosphere, and the annealing atmosphere is selected according to actual needs.
Finally, the embodiment of the invention also provides a quantum dot light-emitting diode, which comprises a cathode, an anode and a quantum dot light-emitting layer arranged between the cathode and the anode, wherein an electron transmission layer is also arranged between the cathode and the quantum dot light-emitting layer, and the electron transmission layer is composed of the electron transmission material provided by the embodiment of the invention, namely the Al-doped ZnS nano-particle material.
In the quantum dot light-emitting diode provided by the embodiment of the invention, the electron transport layer is composed of the electron transport material, the free carrier concentration of ZnS can be improved by Al doping, so that the conductivity of the material is improved, the forbidden bandwidth of ZnS is narrowed, electrons can be easily transited from an impurity level to enter a conduction band, and further, the electrons-holes are promoted to be effectively compounded in the quantum dot light-emitting layer, so that the influence of exciton accumulation on the performance of the device is reduced, and the performance of the device is improved.
Further, a hole transport layer is disposed between the cathode and the quantum dot light emitting layer, and the hole transport layer can be made of a hole transport material conventional in the art, including but not limited to TFB, PVK, Poly-TPD, TCTA, PEDOT: PSS, CBP, etc., or any combination thereof, as well as other high performance hole transport materials. Preparing a hole transport layer: placing the ITO substrate on a spin coater, and spin-coating a prepared solution of a hole transport material to form a film; the film thickness is controlled by adjusting the concentration of the solution, the spin-coating speed and the spin-coating time, and then a thermal annealing process is performed at an appropriate temperature.
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. The preparation method of the quantum dot light-emitting layer comprises the following steps: spin-coating the prepared luminescent material solution with a certain concentration on a spin coater of a substrate with a spin-coated hole transport layer to form a film, controlling the thickness of the luminescent layer to be about 20-60nm by adjusting the concentration of the solution, the spin-coating speed and the spin-coating time, and drying at a proper temperature.
The preparation steps of the electron transport layer are as follows: the substrate which is coated with the quantum dot light-emitting layer by spin coating is placed on a spin coater, Al-doped ZnS precursor solution with a certain concentration is prepared to form a film by spin coating, the thickness of the light-emitting layer is controlled to be about 20-60nm by adjusting the concentration of the solution, the spin coating speed (preferably, the rotating speed is 2000-6000 rpm) and the spin coating time, and then the film is formed by annealing at the temperature of 200-300 ℃ (such as 250 ℃). The step can be annealing in air or in nitrogen atmosphere, and the annealing atmosphere is selected according to actual needs.
The preparation method of the cathode in the quantum dot light-emitting diode comprises the following steps: the substrate deposited with the functional layers is placed in an evaporation bin, a layer of 15-30nm metal silver or aluminum is thermally evaporated through a mask plate to serve as a cathode, or a nano Ag wire or a Cu wire is used, so that a carrier can be smoothly injected due to the small resistance. Further, the obtained quantum dot light emitting diode is subjected to packaging treatment, and the packaging treatment can be carried out by a common machine or by manual packaging. 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.
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 preparation method of the Al-doped ZnS nano-particle material by utilizing zinc chloride, aluminum chloride, ethanol and sodium sulfide comprises the following steps:
1) appropriate amounts of zinc chloride and aluminum chloride were added to 50ml of ethanol to form a solution with a total concentration of 0.5M, wherein the ratio of zinc: the molar ratio of aluminum is 1: 0.03; dissolved at 70 ℃ with stirring.
2) A solution of sodium sulfide dissolved in 10ml of ethanol (molar ratio S) was added2-：Mx+＝1：1，Mx+Which is the sum of zinc ions and aluminum ions), and continuously mixing and stirring the solution in the step 1) at 70 ℃ for 4 hours to obtain a uniform mixed solution.
3) After the mixed solution is cooled, spin-coating the treated ITO by a spin coater, and annealing at 250 ℃.
Example 2
The preparation method of the Al-doped ZnS nano-particle material by utilizing zinc nitrate, aluminum nitrate, propanol and potassium sulfide comprises the following steps:
1) appropriate amounts of zinc nitrate and aluminum nitrate were added to 50ml of propanol to form a solution having a total concentration of 0.5M, wherein the ratio of zinc: the molar ratio of aluminum is 1: 0.04; dissolved at 80 ℃ with stirring.
2) A solution of potassium sulfide dissolved in 10ml of propanol (molar ratio S) was added2-：Mx+＝1.1：1，Mx+Which is the sum of zinc ions and aluminum ions), and continuously mixing and stirring the solution in the step 1) at the temperature of 80 ℃ for 3 hours to obtain a uniform mixed solution.
3) After the mixed solution is cooled, spin-coating the treated ITO by a spin coater, and annealing at 250 ℃.
Example 3
The preparation method of the Al-doped ZnS nano-particle material by using zinc sulfate, aluminum sulfate, methanol and thiourea comprises the following steps:
1) appropriate amounts of zinc sulfate and aluminum sulfate were added to 50ml of methanol to form a solution with a total concentration of 0.5M, wherein the ratio of zinc: the molar ratio of aluminum is 1: 0.05; dissolved at 70 ℃ with stirring.
2) A solution of thiourea in 10ml of methanol (molar ratio S) was added2-：Mx+＝1.2：1，Mx+Which is the sum of zinc ions and aluminum ions), and continuously mixing and stirring the solution in the step 1) at the temperature of 60 ℃ for 4 hours to obtain a uniform mixed solution.
3) After the mixed solution is cooled, spin-coating the treated ITO by a spin coater, and annealing at 250 ℃.
Example 4
A QLED device of a positive type structure, whose structure is shown in fig. 1, 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 in this order from bottom to top. The substrate 1 is made of a glass sheet, the anode 2 is made of an ITO substrate, the hole transport layer 3 is made of TFB, the electron transport layer 5 is made of Al-doped ZnS nanoparticle material (Al-ZnS), and the cathode 6 is made of Al.
The preparation method of the QLED device comprises the following steps:
a: firstly, growing a hole transport layer on a substrate (the substrate is a substrate with an anode arranged on the surface);
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 QLED device.
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 (10)
1. An electron transport material, characterized in that the electron transport material is an Al-doped ZnS nanoparticle material.
2. The electron transport material according to claim 1, wherein a molar ratio of Zn element to Al element in the electron transport material is 1: (0.01-0.05).
3. The electron transport material according to claim 1, wherein the molar ratio of the S element to the metal element in the electron transport material is (0.8 to 1.2): 1; wherein the metal element includes Zn element and Al element.
4. The preparation method of the electron transport material is characterized by comprising the following steps of:
providing a zinc salt, an aluminum salt, and a sulfur source;
dissolving the zinc salt, the aluminum salt and the sulfur source in a solvent to obtain a precursor solution;
and depositing the precursor solution on a substrate, and annealing to obtain the Al-doped ZnS nano-particle material.
5. The method according to claim 4, wherein the zinc salt is at least one selected from the group consisting of zinc acetate, zinc nitrate, zinc chloride, zinc sulfate, zinc acetate dihydrate; and/or
The aluminum salt is selected from at least one of aluminum nitrate, aluminum chloride and aluminum sulfate; and/or
The sulfur source is at least one selected from sodium sulfide, potassium sulfide, thiourea and amine sulfide; and/or
The solvent is at least one selected from isopropanol, ethanol, propanol, butanol, pentanol and hexanol.
6. The production method according to claim 4, wherein the molar ratio of Zn element to Al element is 1: (0.01-0.05), dissolving the zinc salt and the aluminum salt in a solvent; and/or
According to the molar ratio of the S element to the metal element being (0.8-1.2): 1, dissolving the zinc salt, the aluminum salt and the sulfur source in a solvent; wherein the metal element includes Zn element and Al element.
7. The method according to claim 4, wherein the concentration of the metal ion in the precursor solution is 0.2 to 1M; wherein the metal ion comprises Zn2+And Al3+。
8. The method as claimed in claim 4, wherein the temperature of the annealing treatment is 200-300 ℃; and/or
Dissolving the zinc salt, the aluminum salt and the sulfur source in a solvent at the temperature of 60-80 ℃.
9. A quantum dot light-emitting diode comprising a cathode, an anode and a quantum dot light-emitting layer disposed between the cathode and the anode, wherein an electron transport layer is further disposed between the cathode and the quantum dot light-emitting layer, wherein the electron transport layer is composed of the electron transport material according to any one of claims 1 to 3.
10. The quantum dot light-emitting diode of claim 9, wherein the electron transport layer has a thickness of 20 to 60 nm.
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| CN113054118B (en) * | 2019-12-28 | 2022-10-11 | Tcl科技集团股份有限公司 | Composite material, preparation method and application thereof, light-emitting diode and preparation method thereof |
| CN113130791A (en) * | 2019-12-31 | 2021-07-16 | Tcl集团股份有限公司 | Composite material and preparation method thereof, light-emitting diode and preparation method |
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