CN112701230A - Method for preparing perovskite QLED electronic transmission layer by transferring ZnO nano film - Google Patents
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Abstract
The invention belongs to the technical field of preparation of an electron transmission layer QLED, and particularly relates to a method for preparing a perovskite QLED electron transmission layer by transferring a ZnO nano film by a dry method. Firstly, preparing a layer of ZnO nano film on an auxiliary substrate, then attaching a viscous elastomer PDMS prepared in advance to the ZnO film, adsorbing the ZnO nano film by using the viscosity of the elastomer PDMS, and separating the PDMS/ZnO from the auxiliary substrate. Then annealing is carried out to weaken the viscosity of the PDMS stamp, PDMS/ZnO is attached to the perovskite quantum dot light emitting layer and pressed, ZnO nanoparticles are transferred to the perovskite layer, and finally the PDMS stamp is separated from the ZnO layer. According to the invention, the ZnO nano film is transferred to the perovskite quantum dot light-emitting layer through the PDMS stamp to serve as an electron transmission layer, so that a perfect heterogeneous interface can be constructed, and the damage of the solvent action in the solution addition or the thermal effect of the vacuum process to the perovskite quantum dot light-emitting layer can be avoided.
Description
Technical Field
The invention belongs to the technical field of preparation of an electron transmission layer QLED, and particularly relates to a method for preparing a perovskite QLED electron transmission layer by transferring a ZnO nano film by a dry method.
Background
The zinc oxide is a direct band gap semiconductor with a forbidden band width reaching 3.37eV, the exciton confinement energy of the zinc oxide reaches 60meV at room temperature, and the ZnO crystal structure is generally a hexagonal wurtzite structure and has excellent optical performance and electrical performance. The intrinsic defects of the nano zinc oxide are mainly Zn gaps and O vacancies, and the zinc oxide is an n-type semiconductor material and is generally used for an electron transport layer of a quantum dot light-emitting diode.
The perovskite quantum dots show attractive application prospects in the aspect of perovskite light emitting diodes (PeLEDs) due to excellent photoelectric properties of the perovskite quantum dots. At present, a PeLED device prepared by taking perovskite quantum dots as a light emitting layer has achieved remarkable achievement, and shows great application potential in the fields of illumination, wide color gamut display and the like. Although the perovskite light emitting layer can be prepared by a solution processing method such as spin coating, the charge transport layer is often prepared on the perovskite upper layer by vacuum thermal evaporation. This makes the all-solvent processed perovskite quantum dot devices difficult to implement because processing on the perovskite upper layer using polar solvents results in rapid quenching of the light emitting layer, while using non-polar solvents results in re-dissolution of the quantum dot thin film.
Disclosure of Invention
The invention aims to provide a method for preparing a perovskite QLED electronic transmission layer by transferring a ZnO nano film, which aims to solve the problem that the electronic transmission layer of the perovskite quantum dot light-emitting diode is difficult to realize by a solution method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a perovskite QLED electron transport layer by transferring a ZnO nano film is characterized in that a hole injection layer, a hole transport layer, a perovskite quantum dot film, a ZnO electron transport layer and a metal cathode are sequentially deposited on an ITO layer of a transparent conductive glass substrate.
The ZnO electron transport layer is prepared by a transfer printing method, and the specific process is as follows: depositing a ZnO nano film on an auxiliary substrate, attaching a viscous elastomer prepared in advance on the ZnO nano film, adsorbing the ZnO nano film by the viscosity of the elastomer, transferring the ZnO nano film to the perovskite quantum dot film, and finally separating the viscous elastomer from a ZnO layer.
Further, the auxiliary substrate is any one of a flexible substrate and a rigid substrate.
Further, the flexible substrate comprises any one of polyethylene terephthalate (PET), polyethylene naphthalate (PEN) and Polyimide (PI); wherein the rigid substrate comprises a glass sheet.
Further, the material of the viscous elastomer is polydimethylsiloxane PDMS.
Further, the preparation method of the ZnO nano film is a solution processing method or a vacuum deposition method.
Further, the ZnO nano-film includes a ZnO nano-film doped with metal cations.
Further, the ZnO nanofilm includes a ZnO nanofilm mixed with an organic polymer.
Further, the method specifically comprises the following steps:
step 1: an elastomeric PDMS stamp was prepared in advance.
Step 2: and spin-coating ZnO on polyethylene terephthalate (PET) to prepare a layer of nano ZnO film.
And step 3: and then tearing off a viscous elastomer PDMS stamp prepared in advance and attaching the viscous elastomer PDMS stamp to an auxiliary substrate with ZnO nanoparticles.
And 4, step 4: adsorbing the ZnO nano film to the surface by using the PDMS stamp, separating the elastomer PDMS from the auxiliary substrate, and annealing and heating.
And 5: and attaching the annealed PDMS elastic stamp to the perovskite quantum dot light-emitting layer, pressing with a certain force, separating the PDMS stamp from the perovskite quantum dot light-emitting layer, and transferring the ZnO nano film to the perovskite quantum dot light-emitting layer.
The invention has the advantages that:
(1) the invention utilizes the mechanism that the viscosity and the heating curing viscosity of the viscous elastomer are reduced and the characteristic of the viscous elastomer as an elastomer stamp, can transfer the ZnO nano film to the perovskite quantum dot light emitting layer to be used as an electron transmission layer, and reduces the damage of a solvent or a heat effect to the perovskite quantum dot light emitting layer.
(2) The preparation process adopted by the invention is safe and pollution-free, does not generate byproducts, and has simple process and easy operation;
(3) the tacky elastomers described herein may be further designed to be patterned.
Drawings
FIG. 1 is a schematic flow diagram of the transfer process of the present invention;
fig. 2 is a schematic diagram of transferring a ZnO nano-film by a PDMS stamp according to a first embodiment and a second embodiment of the present invention.
Detailed Description
In order to make the features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail.
Example one
A process flow diagram of a method for preparing a perovskite QLED electron transport layer by transferring ZnO nanoparticles, as shown in fig. 1. The method specifically comprises the following steps:
(1) firstly, preparing an elastomer PDMS stamp: coating and preparing a layer of Polydimethylsiloxane (PDMS) on a glass substrate, wherein the area of a PDMS stamp is 1cm2And 7mm in thickness, and then heated for 20min to be in an incompletely cured state with tackiness, and the annealing temperature was 80 ℃.
The PDMS is prepared by mixing a liquid component and a curing agent in a mass ratio of 10:1, stirring for 10min, putting the mixture into a vacuum drying oven, vacuumizing, standing for 0.5h, taking out, and discharging dissolved air.
(2) The ZnO nano-particle solution is prepared by dissolving 0.59g of zinc acetate in 25ml of methanol, and then heating and stirring in a water bath with the temperature of 63-65 ℃. Simultaneously dissolving 0.3g of potassium hydroxide in 13ml of methanol, heating in water bath at the same temperature for 5min, dripping the potassium hydroxide solution into the zinc acetate solution, and continuously heating and stirring for 2.5 h. Then, the mixture was centrifuged at 2500rpm for 5min by a centrifuge, and the supernatant was decanted. Then washed with 4ml of methanol and the centrifugation process was repeated. After the cleaning, 12ml of n-butanol is poured to prepare the ZnO nanoparticle solution.
(3) As shown in fig. 2, polyethylene terephthalate (PET) is used as the auxiliary substrate. The ZnO nanoparticles were spin-coated on the auxiliary substrate for 20s at 3000rpm using a spin coater to form a film in a semi-dry state. And then, adhering the prepared viscous PDMS elastic stamp to polyethylene terephthalate (PET), pressing to enable the ZnO nano film to be adsorbed on the PDMS stamp, and then separating the PDMS stamp from the auxiliary substrate. At this time, the PDMS stamp was then annealed at 80 ℃ for 2 min.
(4) The perovskite quantum dot light-emitting layer adopts CsPbBr3And (3) carrying out spin coating on the perovskite quantum dots at the rotating speed of 2000rpm for 30 s. And (3) attaching the PDMS stamp adsorbing the ZnO to the perovskite quantum dot light-emitting layer, pressing for about 30s at the pressure of 2000 Pa, and then separating the PDMS stamp from the perovskite quantum dot layer. The ZnO nano film is transferred to the perovskite quantum dot light-emitting layer to be used as an electron transmission layer.
Example two
(1) System for makingPreparing an elastomer PDMS stamp: coating and preparing a layer of Polydimethylsiloxane (PDMS) on polyethylene terephthalate (PET), wherein the area of the PDMS stamp is 1cm2And 7mm in thickness, and then heated for 20min to be in an incompletely cured state with tackiness, and the annealing temperature was 80 ℃.
The PDMS is prepared by mixing a liquid component and a curing agent in a mass ratio of 10:1, stirring for 10min, putting the mixture into a vacuum drying oven, vacuumizing, standing for 0.5h, taking out, and discharging dissolved air.
(2) The ZnO nano-particle solution is prepared by dissolving 0.59g of zinc acetate in 25ml of methanol, and then heating and stirring in a water bath with the temperature of 63-65 ℃. Simultaneously dissolving 0.3g of potassium hydroxide in 13ml of methanol, heating in water bath at the same temperature for 5min, dripping the potassium hydroxide solution into the zinc acetate solution, and continuously heating and stirring for 2.5 h. Then, the mixture was centrifuged at 2500rpm for 5min by a centrifuge, and the supernatant was decanted. Then washed with 4ml of methanol and the centrifugation process was repeated. After the cleaning, 12ml of n-butanol is poured to prepare the ZnO nanoparticle solution. Then, the ZnO nanoparticle solution is selectively mixed with the organic polymer PVP, and the concentration of the mixed solution is 8 mg/ml.
(3) A silicon substrate modified with octadecyltrichlorosilane was used as an auxiliary substrate. And (3) spin-coating the ZnO nanoparticle solution obtained in the step (2) on the auxiliary substrate for 20s at 2000rpm by using a spin coater to form a film in a semi-dry state. And then, attaching the prepared viscous PDMS elastic stamp to a silicon substrate, pressing the viscous PDMS elastic stamp to enable the ZnO nano film to be adsorbed on the PDMS stamp, and then separating the PDMS stamp from the auxiliary substrate. At this time, the PDMS stamp was heated at an annealing temperature of 80 ℃ for 2 min.
(4) The perovskite quantum dot light-emitting layer adopts CsPbI3And (3) carrying out spin coating on the perovskite quantum dots at the rotating speed of 2000rpm for 30 s. And (3) attaching the PDMS stamp adsorbing the ZnO to the perovskite quantum dot light-emitting layer, pressing for 30s at the pressure of 2000 Pa, and then separating the PDMS stamp from the perovskite quantum dot layer. The ZnO nano film is transferred to the perovskite quantum dot light-emitting layer to be used as an electron transmission layer.
In conclusion, the invention has low manufacturing cost and simple preparation process, not only has high preparation speed, but also can be carried out in the atmospheric environment of normal temperature and normal pressure without special requirements for the preparation environment. Moreover, the invention can also prepare the patterned ZnO nano-film according to the actual requirements.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (8)
1. A method for preparing a perovskite QLED electron transmission layer by transferring a ZnO nano film is characterized by comprising the following steps: and a hole injection layer, a hole transport layer, a perovskite quantum dot film, a ZnO electron transport layer and a metal cathode are sequentially deposited on the ITO layer of the transparent conductive glass substrate.
The ZnO electron transport layer is prepared by a transfer printing method, and the specific process is as follows: depositing a ZnO nano film on an auxiliary substrate, attaching a viscous elastomer prepared in advance on the ZnO nano film, adsorbing the ZnO nano film by the viscosity of the elastomer, transferring the ZnO nano film to the perovskite quantum dot film, and finally separating the viscous elastomer from a ZnO layer.
2. The method for preparing the perovskite QLED electron transport layer by transferring the ZnO nano-film according to claim 1, wherein the method comprises the following steps: the auxiliary substrate is any one of a flexible substrate and a rigid substrate.
3. The method for preparing the perovskite QLED electron transport layer by transferring the ZnO nano-film according to claim 2, wherein the method comprises the following steps: the flexible substrate comprises any one of polyethylene terephthalate (PET), polyethylene naphthalate (PEN) and Polyimide (PI).
4. The method for preparing the perovskite QLED electron transport layer by transferring the ZnO nano-film according to claim 2, wherein the method comprises the following steps: wherein the rigid substrate comprises a glass sheet.
5. The method for preparing the perovskite QLED electron transport layer by transferring the ZnO nano-film according to claim 1, wherein the method comprises the following steps: the material of the viscous elastomer is polydimethylsiloxane PDMS.
6. The method for preparing the perovskite QLED electron transport layer by transferring the ZnO nano-film according to claim 1, wherein the method comprises the following steps: the preparation method of the ZnO nano film is a solution processing method or a vacuum deposition method.
7. The method for preparing the perovskite QLED electron transport layer by transferring the ZnO nano-film according to claim 1, wherein the method comprises the following steps: the ZnO nano-film comprises a ZnO nano-film doped with metal cations.
8. The method for preparing the perovskite QLED electron transport layer by transferring the ZnO nano-film according to claim 1, wherein the method comprises the following steps: the ZnO nanofilm includes ZnO nanofilm mixed with an organic polymer.
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| CN113707835A (en) * | 2021-08-24 | 2021-11-26 | 福州大学 | Preparation method of nano-imprinting patterned quantum dot LED |
| CN113937242A (en) * | 2021-08-26 | 2022-01-14 | 福州大学 | Hyperfine quantum dot film and preparation method of high-resolution QLED thereof |
| CN114023896A (en) * | 2021-11-08 | 2022-02-08 | 京东方科技集团股份有限公司 | Manufacturing method of light-emitting device |
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