CN111952467A - Preparation method of perovskite thin film and light-emitting diode device based on graphene oxide passivation - Google Patents
Preparation method of perovskite thin film and light-emitting diode device based on graphene oxide passivation Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 63
- 239000010409 thin film Substances 0.000 title claims abstract description 33
- 238000002161 passivation Methods 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000004528 spin coating Methods 0.000 claims abstract description 47
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- 239000010931 gold Substances 0.000 claims abstract description 12
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052737 gold Inorganic materials 0.000 claims abstract description 9
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- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 230000008020 evaporation Effects 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 195
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 66
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 51
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 26
- 239000000758 substrate Substances 0.000 claims description 26
- 238000000137 annealing Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- 239000011521 glass Substances 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 20
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000004140 cleaning Methods 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
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- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- 239000012286 potassium permanganate Substances 0.000 claims description 13
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims description 13
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 12
- 238000007865 diluting Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 8
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- 239000004246 zinc acetate Substances 0.000 claims description 8
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- 239000012467 final product Substances 0.000 claims description 6
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 6
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 6
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- OJIFYBKFIOKLGR-UHFFFAOYSA-N methoxymethane;hydroiodide Chemical compound I.COC OJIFYBKFIOKLGR-UHFFFAOYSA-N 0.000 claims description 3
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- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- QHJPGANWSLEMTI-UHFFFAOYSA-N aminomethylideneazanium;iodide Chemical compound I.NC=N QHJPGANWSLEMTI-UHFFFAOYSA-N 0.000 description 3
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- 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
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K50/00—Organic light-emitting devices
- H10K50/10—OLEDs or polymer light-emitting diodes [PLED]
- H10K50/14—Carrier transporting layers
- H10K50/15—Hole transporting layers
- H10K50/155—Hole transporting layers comprising dopants
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- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
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- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/10—Organic polymers or oligomers
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Abstract
The invention provides a preparation method of a perovskite thin film and a light-emitting diode device based on graphene oxide passivation. The perovskite thin film light-emitting diode device based on graphene oxide passivation is formed by the steps of firstly preparing a ZnO thin film and a PEIE thin film on an ITO thin film by using a spin coating process, then forming a perovskite precursor solution mixed with graphene oxide on the formed ZnO/PEIE thin film by spin coating, preparing a hole transport layer on the perovskite thin film by using the spin coating process, and thermally evaporating molybdenum oxide and gold by using an evaporation technology to finally form the perovskite thin film light-emitting diode device based on graphene oxide passivation. The film passes through the graphene oxide pair FApBI3The doping mixture of the perovskite passivates the surface defects of the perovskite and prevents the perovskite from phase transition to a certain extent, so that the light-emitting diode of the type has the advantages of high brightness and high external quantum efficiency.
Description
Technical Field
The invention belongs to the field of photoelectric materials and devices, and particularly relates to a preparation method of a perovskite thin film and a light-emitting diode device based on graphene oxide passivation.
Background
With the development of science and technology and the advancement of society, information exchange and transmission become an indispensable part in daily life. The quantum dot photoluminescent optical thin film device, as a display device most likely to be put into practical use, plays an important role in the fields of information exchange, transmission and the like. The perovskite light emitting diode device is a display device most likely to be put into practical use, and has become the most popular research object at present because of its excellent advantages such as photoluminescence, wide color gamut, and adjustable light color. Currently, most perovskite light emitting diodes adopt a method of preparing a perovskite precursor solution and then preparing the solution into a device through spin coating. In order to improve the light emitting performance of the device and improve the light emitting stability and the service life, the stability of the perovskite material or the perovskite light emitting film layer needs to be improved by controlling the water and oxygen corrosion resistance of the perovskite material or the perovskite light emitting film layer.
Disclosure of Invention
The invention aims to provide a perovskite thin film based on graphene oxide passivation and a preparation method of a light-emitting diode device, aiming at the defects and defects of the prior art.
The invention specifically adopts the following technical scheme:
a preparation method of a perovskite thin film and a light-emitting diode device based on graphene oxide passivation is characterized by comprising the following steps:
step S1: sequentially spin-coating a ZnO solution and a PEIE solution on the surface of the ITO glass substrate by using a spin-coating process, and annealing to form a ZnO/PEIE film;
step S2: spin-coating a perovskite precursor solution on the surface of the ZnO/PEIE film by using a spin-coating process, and annealing and drying to form a perovskite film based on graphene oxide passivation;
step S3: spin-coating a hole transport layer precursor solution on the surface of the perovskite thin film based on graphene oxide passivation, and drying to form a hole transport layer;
step S4: and evaporating the molybdenum oxide and the gold thin film to the sample wafer prepared in the step S3 by using an evaporation technology to obtain the perovskite light-emitting diode device based on graphene oxide passivation.
Preferably, in step S1, the ZnO solution is obtained by:
step S11: mixing zinc acetate dihydrate with a DMSO solution, heating and stirring to prepare a DMSO solution of zinc acetate;
step S12: mixing TMAH and ethanol, and stirring until the mixture is clear and transparent to obtain an ethanol solution of TMAH;
step S13: dropwise adding an ethanol solution of TMAH into a zinc acetate solution, heating and stirring until the reaction is finished, precipitating the reaction solution by using ethyl acetate, and obtaining a ZnO precipitate by a centrifugal filtration method;
step S14: dissolving the ZnO precipitate by using a butanol solution, and filtering to obtain a ZnO solution;
the PEIE solution is obtained by diluting a PEIE mother solution with the molecular weight of 70000g/ml by methoxy ethanol.
Preferably, the perovskite precursor solution is prepared by the following steps:
step S21: preparing a DMF solution of graphene oxide, and taking the DMF solution of graphene oxide as a solvent for dissolving perovskite;
step S22: a perovskite precursor solution was prepared using a DMF solution of graphene oxide.
Preferably, step S21 specifically includes the following steps:
step S211: stirring concentrated sulfuric acid, natural graphite powder and potassium permanganate respectively under an ice bath condition and an oil bath heating condition in sequence, then diluting the solution by using deionized water under the condition of ensuring the solution temperature to be certain, and continuing stirring after the dilution is finished;
step S212: after stirring, reducing potassium permanganate and manganese dioxide by using high-concentration hydrogen peroxide to obtain a clear solution, filtering, respectively cleaning by using hydrochloric acid and acetone, and placing the final product in a screw bottle for storage;
step S213: dissolving graphene oxide by using DMF to obtain a DMF solution of graphene oxide;
step S22 specifically includes the following steps:
dissolving lead iodide and methyl ether iodide in the DMF solution of graphene oxide in the step S21, and heating to form FAPBI3A perovskite precursor solution.
Preferably, the hole transport layer precursor solution is prepared by dissolving TFB in chlorobenzene.
Preferably, in the preparation of the ZnO solution, the mass ratio of zinc acetate dihydrate to TMAH is 1: 1.4-2, stirring the zinc acetate dihydrate and the DMSO solution at the temperature of 50 ℃ and the rotation speed of 450 rpm; the concentration of the DMSO solution is analytically pure, the ethanol solution of TMAH is dripped into the zinc acetate solution at a constant speed when used, and the stirring speed and the stirring time are respectively 500rpm and 1 h. The ratio of ethyl acetate to the reaction solution was 1: 1, the rotating speed and the time of centrifugation are 3000-6000rpm and 3min respectively;
the concentration of the prepared PEIE solution was 0.4 wt%;
the spin coating parameters of ZnO and PEIE are respectively 2000-5000rpm for 45s and 5000rpm for 60s, and the annealing parameters are respectively 130-160 ℃ annealing for 20min and 90-120 ℃ annealing for 10 min.
Preferably, in step S21, the concentrated sulfuric acid concentration is 98%, and the potassium permanganate concentration is analytically pure; the ratio of graphite powder to potassium permanganate is 1: 5, keeping the ice bath temperature not higher than 10 ℃, and stirring for 1 h; stirring in an oil bath at 35 deg.C for 20 hr, diluting with deionized water while maintaining the solution at about 90 deg.C, and stirring for 2 hr; the ratio of graphite powder to concentrated sulfuric acid is 1: 60, the ratio of the concentrated sulfuric acid solution to the deionized water is 1: 2;
the concentration of hydrogen peroxide is 30%, the concentration of hydrochloric acid is 37%, and the ratio of hydrogen peroxide to concentrated sulfuric acid is about 1: 20; washing with hydrochloric acid for 2 or 3 times, wherein the amount of washing is 4000ml each time, washing with acetone for 3 or 4 times, wherein the amount of washing is 1000ml each time, and centrifuging at 6000rpm for 30 s;
the concentration range of the DMF solution of the graphene oxide is 1 mg/ml-10 g/ml.
Preferably, the FAPBI3The heating temperature of the perovskite precursor solution is 50-70 ℃, the heating time is 2-4h, the rotation speed of the solution spin coating process in the step S2 is 1000-.
Preferably, in step S3, the concentration of TFB in the hole transport layer precursor solution is 8mg/ml, the rotation speed of the spin coating process is 1000-5000rpm, the annealing time is 10-30min, and the annealing temperature is 110-130 ℃.
Preferably, the thickness of the molybdenum oxide is 5-15nm, and the thickness of the gold film is 50-70 nm.
Preferably, the ITO glass used has an area of 2cm by 2 cm.
Compared with the prior art, the invention and the optimized scheme thereof utilize a simple spin-coating film-forming process technology, the DMF solution of graphene oxide is prepared on the ITO glass substrate, then the solution is used as a solvent to dissolve the perovskite material, the perovskite precursor solution is spin-coated on the surface of the substrate through spin-coating, finally a corresponding perovskite film layer is formed on the prepared ZnO/PEIE film, then TFB is dissolved in chlorobenzene to be prepared into a certain concentration, a hole transmission layer is formed through spin-coating till drying, drying is carried out at room temperature, and finally a layer of MoOx/Au electrode is formed through thermal deposition, so that the corresponding FAPBI is formed3Perovskite light emitting diode, due to the thin film passing through graphene oxide to FAPBI3The doping and mixing of the perovskite improves the concentration of electron holes in the light-emitting layer, so that the light-emitting diode of the type has the advantages of high brightness and high external quantum efficiency.
Drawings
The invention is described in further detail below with reference to the following figures and detailed description:
FIG. 1 is a schematic structural diagram of an ITO glass substrate according to an embodiment of the invention;
FIG. 2 is a schematic structural diagram of an ITO glass substrate with ZnO formed according to an embodiment of the invention;
FIG. 3 is a schematic structural diagram of an ITO glass substrate for forming a PEIE film according to an embodiment of the present invention;
FIG. 4 is a schematic structural view of an ITO glass substrate after spin coating of perovskite according to an embodiment of the invention;
FIG. 5 is a schematic structural diagram of an ITO glass substrate with a TFB film layer formed thereon according to an embodiment of the present invention;
FIG. 6 is a schematic diagram of a final LED structure according to an embodiment of the present invention;
in the figure: 1-a glass substrate; 2-an ITO layer; 3-ZnO film; 4-PEIE film; 5-perovskite particles; GO (graphene oxide) in 6-perovskite gaps; 7-a hole transport layer; 8-MoOx/Au electrodes.
Detailed Description
In order to make the features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail as follows:
as shown in fig. 1 to fig. 6, the present embodiment provides a specific scheme of a method for preparing a perovskite thin film and a light emitting diode device based on graphene oxide passivation, which includes the following steps:
step S1: sequentially spin-coating a ZnO solution and a PEIE solution on the surface of a glass substrate 1 with an ITO layer 2 by using a spin-coating process, and annealing to form a ZnO film 3 and a PEIE film 4;
step S2: spin-coating perovskite precursor solution on the surfaces of the ZnO film 3 and the PEIE film 4 by using a spin-coating process, annealing and drying to form a perovskite film based on graphene oxide passivation, wherein the film layer contains a large number of perovskite particles 5 and GO6 particles in perovskite gaps;
step S3: spin-coating a hole transport layer precursor solution on the surface of the perovskite thin film based on graphene oxide passivation, and drying to form a hole transport layer 7;
step S4: and evaporating the molybdenum oxide and the gold thin film onto the sample wafer prepared in the step S3 by using an evaporation technology to form a MoOx/Au electrode 8, so as to obtain the perovskite light-emitting diode device based on graphene oxide passivation.
Wherein, in step S1, the ZnO solution is obtained by:
step S11: mixing zinc acetate dihydrate with a DMSO solution, heating and stirring to prepare a DMSO solution of zinc acetate;
step S12: mixing TMAH and ethanol, and stirring until the mixture is clear and transparent to obtain an ethanol solution of TMAH;
step S13: dropwise adding an ethanol solution of TMAH into a zinc acetate solution, heating and stirring until the reaction is finished, precipitating the reaction solution by using ethyl acetate, and obtaining a ZnO precipitate by a centrifugal filtration method;
step S14: dissolving the ZnO precipitate by using a butanol solution, and filtering to obtain a ZnO solution;
the PEIE solution is obtained by diluting a PEIE mother solution with the molecular weight of 70000g/ml by methoxy ethanol.
The perovskite precursor solution is prepared by the following steps:
step S21: preparing a DMF solution of graphene oxide, and taking the DMF solution of graphene oxide as a solvent for dissolving perovskite;
step S22: a perovskite precursor solution was prepared using a DMF solution of graphene oxide.
Step S21 specifically includes the following steps:
step S211: stirring concentrated sulfuric acid, natural graphite powder and potassium permanganate respectively under an ice bath condition and an oil bath heating condition in sequence, then diluting the solution by using deionized water under the condition of ensuring the solution temperature to be certain, and continuing stirring after the dilution is finished;
step S212: after stirring, reducing potassium permanganate and manganese dioxide by using high-concentration hydrogen peroxide to obtain a clear solution, filtering, respectively cleaning by using hydrochloric acid and acetone, and placing the final product in a screw bottle for storage;
step S213: dissolving graphene oxide by using DMF to obtain a DMF solution of graphene oxide;
step S22 specifically includes the following steps:
dissolving lead iodide and methyl ether iodide in the DMF solution of graphene oxide in the step S21, and heating to form FAPBI3A perovskite precursor solution.
The precursor solution of the hole transport layer is prepared by dissolving TFB in chlorobenzene.
Based on the above scheme, the following three specific examples are provided to further supplement the scheme of the present invention:
example one
(1) Weighing 0.6585g of zinc acetate dihydrate medicine, placing the medicine in a clean reagent bottle with a clean magneton and a capacity of 100 ml, then using a pipette to extract 30ml of DMSO solution, dropwise adding the DMSO solution into the reagent bottle, placing the reagent bottle on a heating and stirring table, setting the temperature at 50 ℃ and the rotating speed at 450rpm, and dissolving the zinc acetate dihydrate into the DMSO solvent through violent stirring; and secondly, 0.9062 g of TMAH medicament is weighed, placed in a small reagent bottle, 10ml of ethanol solution is extracted by a liquid transfer gun, added into the reagent bottle, and stirred until the mixture is clear and transparent. And then dripping the prepared TMAH solution into the DMSO precursor at a constant speed within 8 min, and keeping the rotation speed at 500rpm for 1 h. After the reaction was completed, the reaction solution was subjected to a precipitation operation with ethyl acetate in an equal ratio. Respectively extracting reaction liquid and ethyl acetate solution with the same amount (5 ml) by using a rubber-tipped dropper, placing the reaction liquid and the ethyl acetate solution into a centrifugal tube, centrifuging for 3min at the rotating speed of 3000rpm, taking out the centrifugal tube after the centrifugation is finished, and pouring and discarding supernatant liquid to dissolve the reaction liquid and the ethyl acetate solution;
(2) PEIE with Mw =70000g/ml is selected, diluted to 0.4wt% by methoxy ethanol and placed in a clean small bottle with the volume of 5ml for standby;
(3) 600ml of 98% sulfuric acid was placed in a 2L round bottom flask and cooled to below 10 ℃ in an ice water bath. Then, slowly adding 10g of natural graphite powder into cooled concentrated sulfuric acid while stirring within 10min, then slowly adding 50g of potassium permanganate into the solution within 30min, and continuously stirring for 1h under the ice bath condition; after stirring, transferring the solution into an oil bath environment, keeping the temperature at 35 ℃, stirring for 20 hours, then diluting the mixture with 1200ml of deionized water under the condition of keeping the temperature of the mixture at 90 ℃, and continuing stirring for 2 hours after the completion; extracting 30ml of 30% hydrogen peroxide by using a liquid transfer gun, slowly and dropwise adding the hydrogen peroxide into the reaction liquid, when the color of the solution is changed into brilliant yellow, cleaning the solution by using hydrochloric acid three times, wherein each time is 4000ml, and then cleaning the solution by using acetone four times, wherein each time is 1000ml, and the centrifugal parameter is 6000rpm and lasts for 30min during cleaning. The final product is stored in a silk-mouth bottle and sealed. 50mg of graphene oxide product was weighed out and prepared into a DMF solution with a concentration of 5 mg/ml graphene oxide using a 10 DMF solution.
(4) 0.0461g of lead iodide and 0.0413g of formamidine iodide are dissolved in 1.44mL of DMF solution of graphene oxide, and the mixture is heated and stirred at 60 ℃ for 3h to prepare FAPBI3A perovskite precursor solution.
(5) Selecting an ITO conductive glass sheet, firstly respectively ultrasonically cleaning ITO for 15min by using deionized water and glass water, then wiping the ITO clean by using dust-free cloth, then respectively ultrasonically cleaning the ITO for 15min by using acetone and ethanol, and finally drying in an oven. Before spin-coating the film, carrying out plasma ozone treatment on the ITO for 20-30 min;
(6) filtering ZnO butanol solution with 0.2 μm filter head, applying 110 μ l ZnO solution on ITO glass surface with a pipette during spin coating, adjusting the rotation speed of spin coater to 3000rpm for 45s, and annealing at 160 deg.C for 20 min. After which the substrate was transferred to a glove box for spin coating of the PEIE layer.
(7) The spin speed of the spin coater was adjusted to 5000rpm, the spin was maintained for 30 seconds, and 110. mu.l of the diluted PEIE solution was selected by a pipette at the start of the spin coating, and the solution was spin-coated. Then annealed at 90 ℃ for 10 min. The substrate was washed twice with DMF solution leaving an ultrathin PEIE film on top.
(8) Placing a substrate on a spin coater, adjusting the rotation speed of the spin coater to 3000rpm, keeping the rotation speed for 45s, selecting 85 mul of prepared perovskite precursor solution by using a liquid-transferring gun, quickly dripping the precursor solution at the center of the surface of the substrate while pressing a start button of the spin coater, placing the substrate on a heating table after the spin coating is finished, and keeping the temperature at 150 ℃ for annealing for 20 min.
(9) Dissolving TFB in chlorobenzene solution to obtain solution with concentration of 8mg/ml, filtering with 0.2 μm filter head, adjusting uniform glue machine parameter to 3000rpm, and maintaining for 30 s. And (3) pressing a start button of a spin coater, simultaneously taking 65 mu l of solution by using a pipette, quickly dripping the solution on the surface of the device, spin-coating, and then placing the device on an electric hot plate for annealing at 110 ℃ for 20 min.
(10) Under the vacuum condition, the thickness of the deposited molybdenum oxide is 7 nm, the deposition rate is 0.04nm/s, the deposition rate is 0.3 nm/s, the thickness of the gold is 60 nm, and the molybdenum oxide is dried for 1h at room temperature to obtain the light-emitting diode.
Example two
(1) Weighing 0.6585g of zinc acetate dihydrate medicine, placing the medicine in a clean reagent bottle with a clean magneton and a capacity of 100 ml, then using a pipette to extract 30ml of DMSO solution, dropwise adding the DMSO solution into the reagent bottle, placing the reagent bottle on a heating and stirring table, setting the temperature at 50 ℃ and the rotating speed at 450rpm, and dissolving the zinc acetate dihydrate into the DMSO solvent through violent stirring; secondly, 1.317g of TMAH medicament is weighed and placed in a small reagent bottle, 10ml of ethanol solution is extracted by a pipette, added into the reagent bottle and stirred until the mixture is clear and transparent. And then dripping the prepared TMAH solution into the DMSO precursor at a constant speed within 8 min, and keeping the rotation speed at 500rpm for 1 h. After the reaction was completed, the reaction solution was subjected to a precipitation operation with ethyl acetate in an equal ratio. Respectively extracting reaction liquid and ethyl acetate solution with the same amount (5 ml) by using a rubber-tipped dropper, placing the reaction liquid and the ethyl acetate solution into a centrifugal tube, centrifuging for 3min at the rotating speed of 4000rpm, taking out the centrifugal tube after the centrifugation is finished, and pouring and discarding supernatant liquid to dissolve the reaction liquid and the ethyl acetate solution;
(2) PEIE with Mw =70000g/ml is selected, diluted to 0.4wt% by methoxy ethanol and placed in a clean small bottle with the volume of 5ml for standby;
(3) 600ml of 98% sulfuric acid was placed in a 2L round bottom flask and cooled to below 10 ℃ in an ice water bath. Then, slowly adding 10g of natural graphite powder into cooled concentrated sulfuric acid while stirring within 10min, then slowly adding 50g of potassium permanganate into the solution within 30min, and continuously stirring for 1h under the ice bath condition; after stirring, transferring the solution into an oil bath environment, keeping the temperature at 35 ℃, stirring for 20 hours, then diluting the mixture with 1200ml of deionized water under the condition of keeping the temperature of the mixture at 90 ℃, and continuing stirring for 2 hours after the completion; extracting 30ml of 30% hydrogen peroxide by using a liquid transfer gun, slowly and dropwise adding the hydrogen peroxide into the reaction liquid, when the color of the solution is changed into brilliant yellow, cleaning the solution by using hydrochloric acid three times, wherein each time is 4000ml, and then cleaning the solution by using acetone four times, wherein each time is 1000ml, and the centrifugal parameter is 6000rpm and lasts for 30min during cleaning. The final product is stored in a silk-mouth bottle and sealed. 10mg of graphene oxide product was weighed out and prepared into a DMF solution with a concentration of 1mg/ml graphene oxide using 10ml DMF solution.
(4) 0.0461g of lead iodide and 0.0344g of formamidine iodide were dissolved in 1.44mL of graphene oxide in DMF and stirred at 50 ℃ for 4h to prepare FAPBI3A perovskite precursor solution.
(5) Selecting an ITO conductive glass sheet, firstly respectively ultrasonically cleaning ITO for 15min by using deionized water and glass water, then wiping the ITO clean by using dust-free cloth, then respectively ultrasonically cleaning the ITO for 15min by using acetone and ethanol, and finally drying in an oven. Before spin-coating the film, carrying out plasma ozone treatment on the ITO for 20-30 min;
(6) filtering ZnO butanol solution with 0.2 μm filter head, applying 110 μ l ZnO solution on ITO glass surface with a pipette in spin coating process, adjusting rotation speed of spin coater to 4000rpm for 45s, and annealing at 150 deg.C for 20 min. After which the substrate was transferred to a glove box for spin coating of the PEIE layer.
(7) The spin speed of the spin coater was adjusted to 5000rpm, the spin was maintained for 30 seconds, and 110. mu.l of the diluted PEIE solution was selected by a pipette at the start of the spin coating, and the solution was spin-coated. Then annealing at 110 deg.C for 10 min. The substrate was washed twice with DMF solution leaving an ultrathin PEIE film on top.
(8) Placing a substrate on a spin coater, adjusting the rotation speed of the spin coater to 4000rpm, keeping the rotation speed for 45s, selecting 85 mul of prepared perovskite precursor solution by using a liquid-transferring gun, quickly dripping the precursor solution at the center of the surface of the substrate while pressing a start button of the spin coater, placing the substrate on a heating table after the spin coating is finished, and keeping the temperature at 140 ℃ for annealing for 20 min.
(9) Dissolving TFB in chlorobenzene solution to prepare solution with concentration of 8mg/ml, filtering the TFB chlorobenzene solution by using a 0.2-micron filter head, adjusting parameters of a spin coater to 4000rpm, and keeping for 30 s. And (3) pressing a start button of the spin coater, simultaneously taking 65 mu l of solution by using a pipette, quickly dripping the solution on the surface of the device, spin-coating, and then placing the device on an electric hot plate for annealing at 120 ℃ for 20 min.
(10) Under the vacuum condition, the thickness of the deposited molybdenum oxide is 7 nm, the deposition rate is 0.04nm/s, the deposition rate is 0.3 nm/s, the thickness of the gold is 60 nm, and the molybdenum oxide is dried for 1h at room temperature to obtain the light-emitting diode.
EXAMPLE III
(1) Weighing 0.6585g of zinc acetate dihydrate medicine, placing the medicine in a clean reagent bottle with a clean magneton and a capacity of 100 ml, then using a pipette to extract 30ml of DMSO solution, dropwise adding the DMSO solution into the reagent bottle, placing the reagent bottle on a heating and stirring table, setting the temperature at 50 ℃ and the rotating speed at 450rpm, and dissolving the zinc acetate dihydrate into the DMSO solvent through violent stirring; 1.1194g of TMAH medicament is weighed, placed in a small reagent bottle, 10ml of ethanol solution is extracted by a pipette, added into the reagent bottle and stirred until the solution is clear and transparent. And then dripping the prepared TMAH solution into the DMSO precursor at a constant speed within 8 min, and keeping the rotation speed at 500rpm for 1 h. After the reaction was completed, the reaction solution was subjected to a precipitation operation with ethyl acetate in an equal ratio. Respectively extracting reaction liquid and ethyl acetate solution with the same amount (5 ml) by using a rubber-tipped dropper, placing the reaction liquid and the ethyl acetate solution into a centrifugal tube, centrifuging for 3min at the rotating speed of 6000rpm, taking out the centrifugal tube after the centrifugation is finished, and pouring and discarding supernatant liquid to dissolve the reaction liquid and the ethyl acetate solution;
(2) PEIE with Mw =70000g/ml is selected, diluted to 0.4wt% by methoxy ethanol and placed in a clean small bottle with the volume of 5ml for standby;
(3) 600ml of 98% sulfuric acid was placed in a 2L round bottom flask and cooled to below 10 ℃ in an ice water bath. Then, slowly adding 10g of natural graphite powder into cooled concentrated sulfuric acid while stirring within 10min, then slowly adding 50g of potassium permanganate into the solution within 30min, and continuously stirring for 1h under the ice bath condition; after stirring, transferring the solution into an oil bath environment, keeping the temperature at 35 ℃, stirring for 20 hours, then diluting the mixture with 1200ml of deionized water under the condition of keeping the temperature of the mixture at 90 ℃, and continuing stirring for 2 hours after the completion; extracting 30ml of 30% hydrogen peroxide by using a liquid transfer gun, slowly and dropwise adding the hydrogen peroxide into the reaction liquid, when the color of the solution is changed into brilliant yellow, cleaning the solution by using hydrochloric acid three times, wherein each time is 4000ml, and then cleaning the solution by using acetone four times, wherein each time is 1000ml, and the centrifugal parameter is 6000rpm and lasts for 30min during cleaning. The final product is stored in a silk-mouth bottle and sealed. 100 mg of graphene oxide product was weighed out and prepared into a DMF solution with a concentration of 10mg/ml graphene oxide using 10ml DMF solution.
(4) 0.0461g of lead iodide and 0.0258g of formamidine iodide are dissolved in 1.44mL of DMF solution of graphene oxide, and the mixture is heated and stirred for 2h at 70 ℃ to prepare FAPBI3A perovskite precursor solution.
(5) Selecting an ITO conductive glass sheet, firstly respectively ultrasonically cleaning ITO for 15min by using deionized water and glass water, then wiping the ITO clean by using dust-free cloth, then respectively ultrasonically cleaning the ITO for 15min by using acetone and ethanol, and finally drying in an oven. Before spin-coating the film, carrying out plasma ozone treatment on the ITO for 20-30 min;
(6) filtering ZnO butanol solution with 0.2 μm filter head, applying 110 μ l ZnO solution on ITO glass surface with a pipette during spin coating, adjusting the rotation speed of spin coater to 5000rpm for 45s, and annealing at 130 deg.C for 20 min. After which the substrate was transferred to a glove box for spin coating of the PEIE layer.
(7) The spin speed of the spin coater was adjusted to 5000rpm, the spin was maintained for 30 seconds, and 110. mu.l of the diluted PEIE solution was selected by a pipette at the start of the spin coating, and the solution was spin-coated. Then annealing at 100 deg.C for 10 min. The substrate was washed twice with DMF solution leaving an ultrathin PEIE film on top.
(8) Placing a substrate on a spin coater, adjusting the rotation speed of the spin coater to 5000rpm, keeping the rotation speed for 45s, selecting 85 mul of prepared perovskite precursor solution by using a liquid-transferring gun, quickly dripping the precursor solution at the center of the surface of the substrate while pressing a start button of the spin coater, placing the substrate on a heating table after the spin coating is finished, and keeping the temperature at 160 ℃ for annealing for 10 min.
(9) Dissolving TFB in chlorobenzene solution to prepare solution with concentration of 8mg/ml, filtering the TFB chlorobenzene solution by using a 0.2-micron filter head, adjusting the parameter of a spin coater to 5000rpm, and keeping for 30 s. And (3) pressing a start button of the spin coater, simultaneously taking 65 mu l of solution by using a pipette, quickly dripping the solution on the surface of the device, spin-coating, and then placing the device on an electric hot plate for annealing at 130 ℃ for 15 min.
(10) Under the vacuum condition, the thickness of the deposited molybdenum oxide is 7 nm, the deposition rate is 0.04nm/s, the deposition rate is 0.3 nm/s, the thickness of the gold is 60 nm, and the molybdenum oxide is dried for 1h at room temperature to obtain the light-emitting diode.
The present invention is not limited to the above preferred embodiments, and other various methods for manufacturing the perovskite thin film and the light emitting diode device based on graphene oxide passivation can be obtained by anyone who can obtain the same results according to the teaching of the present invention.
Claims (10)
1. A preparation method of a perovskite thin film and a light-emitting diode device based on graphene oxide passivation is characterized by comprising the following steps:
step S1: sequentially spin-coating a ZnO solution and a PEIE solution on the surface of the ITO glass substrate by using a spin-coating process, and annealing to form a ZnO/PEIE film;
step S2: spin-coating a perovskite precursor solution on the surface of the ZnO/PEIE film by using a spin-coating process, and annealing and drying to form a perovskite film based on graphene oxide passivation;
step S3: spin-coating a hole transport layer precursor solution on the surface of the perovskite thin film based on graphene oxide passivation, and drying to form a hole transport layer;
step S4: and evaporating the molybdenum oxide and the gold thin film to the sample wafer prepared in the step S3 by using an evaporation technology to obtain the perovskite light-emitting diode device based on graphene oxide passivation.
2. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation according to claim 1, wherein:
in step S1, the ZnO solution is obtained by:
step S11: mixing zinc acetate dihydrate with a DMSO solution, heating and stirring to prepare a DMSO solution of zinc acetate;
step S12: mixing TMAH and ethanol, and stirring until the mixture is clear and transparent to obtain an ethanol solution of TMAH;
step S13: dropwise adding an ethanol solution of TMAH into a zinc acetate solution, heating and stirring until the reaction is finished, precipitating the reaction solution by using ethyl acetate, and obtaining a ZnO precipitate by a centrifugal filtration method;
step S14: dissolving the ZnO precipitate by using a butanol solution, and filtering to obtain a ZnO solution;
the PEIE solution is obtained by diluting a PEIE mother solution with the molecular weight of 70000g/ml by methoxy ethanol.
3. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation according to claim 1, wherein:
the perovskite precursor solution is prepared by the following steps:
step S21: preparing a DMF solution of graphene oxide, and taking the DMF solution of graphene oxide as a solvent for dissolving perovskite;
step S22: a perovskite precursor solution was prepared using a DMF solution of graphene oxide.
4. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation according to claim 3, wherein:
step S21 specifically includes the following steps:
step S211: stirring concentrated sulfuric acid, natural graphite powder and potassium permanganate respectively under an ice bath condition and an oil bath heating condition in sequence, then diluting the solution by using deionized water under the condition of ensuring the solution temperature to be certain, and continuing stirring after the dilution is finished;
step S212: after stirring, reducing potassium permanganate and manganese dioxide by using high-concentration hydrogen peroxide to obtain a clear solution, filtering, respectively cleaning by using hydrochloric acid and acetone, and placing the final product in a screw bottle for storage;
step S213: dissolving graphene oxide by using DMF to obtain a DMF solution of graphene oxide;
step S22 specifically includes the following steps:
dissolving lead iodide and methyl ether iodide in the DMF solution of graphene oxide in the step S21, and heating to form FAPBI3A perovskite precursor solution.
5. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation according to claim 1, wherein: the cavity transport layer precursor solution is prepared by dissolving TFB in chlorobenzene.
6. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation of claim 2, wherein:
in the preparation of the ZnO solution, the mass ratio of zinc acetate dihydrate to TMAH is 1: 1.4-2, stirring the zinc acetate dihydrate and the DMSO solution at the temperature of 50 ℃ and the rotation speed of 450 rpm; the concentration of the used DMSO solution is analytically pure, the ethanol solution of TMAH is dripped into the zinc acetate solution at a constant speed when used, and the stirring speed and the stirring time are respectively 500rpm and 1 h;
the ratio of ethyl acetate to the reaction solution was 1: 1, the rotating speed and the time of centrifugation are 3000-6000rpm and 3min respectively;
the concentration of the prepared PEIE solution was 0.4 wt%;
the spin coating parameters of ZnO and PEIE are respectively 2000-5000rpm for 45s and 5000rpm for 60s, and the annealing parameters are respectively 130-160 ℃ annealing for 20min and 90-120 ℃ annealing for 10 min.
7. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation according to claim 4, wherein:
in step S21, the concentrated sulfuric acid concentration is 98%, and the potassium permanganate concentration is analytically pure; the ratio of graphite powder to potassium permanganate is 1: 5, keeping the ice bath temperature not higher than 10 ℃, and stirring for 1 h; stirring in an oil bath at 35 deg.C for 20 hr, diluting with deionized water while maintaining the solution at about 90 deg.C, and stirring for 2 hr; the ratio of graphite powder to concentrated sulfuric acid is 1: 60, the ratio of the concentrated sulfuric acid solution to the deionized water is 1: 2;
the concentration of hydrogen peroxide is 30%, the concentration of hydrochloric acid is 37%, and the ratio of hydrogen peroxide to concentrated sulfuric acid is about 1: 20; washing with hydrochloric acid for 2 or 3 times, wherein the amount of washing is 4000ml each time, washing with acetone for 3 or 4 times, wherein the amount of washing is 1000ml each time, and centrifuging at 6000rpm for 30 s;
the concentration range of the DMF solution of the graphene oxide is 1 mg/ml-10 g/ml.
8. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation according to claim 4, wherein:
the FAPBI3Perovskite precursor solution additionThe heat temperature is 50-70 ℃, the heating time is 2-4h, the rotation number of the solution spin coating process in the step S2 is 1000-.
9. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation of claim 5, wherein:
in step S3, the concentration of TFB in the hole transport layer precursor solution is 8mg/ml, the rotation speed of the spin coating process is 1000-.
10. The method of preparing a perovskite thin film and light emitting diode device based on graphene oxide passivation according to claim 1, wherein: the thickness of the molybdenum oxide is 5-15nm, and the thickness of the gold film is 50-70 nm.
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