CN105720205A - PEI (polyethyleneimine) based high-efficiency perovskite quantum dot light-emitting thin film and preparation method thereof - Google Patents
PEI (polyethyleneimine) based high-efficiency perovskite quantum dot light-emitting thin film and preparation method thereof Download PDFInfo
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Abstract
The invention mainly relates to a novel light-emitting thin film, and particularly relates to a PEI (polyethyleneimine) based high-efficiency perovskite quantum dot light-emitting thin film and a preparation method thereof. PEI and ZnO are used as electron transporting layers; and the perovskite quantum dot light-emitting thin film is used as a fluorescent layer. The PEI based high-efficiency perovskite quantum dot light-emitting thin film structurally comprises a substrate (1) formed by an ITO (indium tin oxide) thin film, a ZnO layer (2) deposited on the substrate, a PEI layer (3) spin-coated on a ZnO nanocrystalline thin film, and perovskite quantum dots (4) spin-coated on the ZnO nanocrystalline thin film coated with PEI, wherein the ZnO layer and the PEI layer are combined into an electron migration layer together; and the inorganic cesium lead halide perovskite quantum dots are used as a light-emitting layer (4). Compared with fluorescence quantum yield of a perovskite quantum dot light-emitting thin film prepared by an existing process, fluorescence quantum yield of the perovskite quantum dot light-emitting thin film prepared by the preparation method disclosed by the invention can be improved by 2 to 3 times.
Description
Technical field
The present invention relates to the application at light-emitting film of a kind of new material.The invention mainly relates to a kind of novel light-emitting thin film, particularly relate to efficient calcium titanium ore quantum dot light emitting thin film based on PEI and preparation method thereof.
Technical background
Perovskite quantum dot, has the outstanding features such as solwution method is prepared, is easily worked, Color tunable, quantum yield are high, is with a wide range of applications at field of photoelectric devices such as light emitting diode, laser, display, solaodes.As novel luminescent material, the feature that glow peak is narrow, fluorescence conversion ratio is high so that it is there is good application prospect in light-emitting film field.
Now in preparation technology, after perovskite quantum dot solution is prepared into perovskite quantum dot light emitting thin film, there is the problem that fluorescence efficiency sharply declines.Meanwhile, when using perovskite quantum dot light emitting film preparation electronic device (solaode, laser instrument, light emitting diode), there is also the problem that fluorescence quantum efficiency is low.Commonly used technique be: one is be deposited in ITO-substrate of glass as fluorescence coating using perovskite quantum dot；Two is with glass for substrate, perovskite quantum dot is deposited in electron transfer layer (such as zinc oxide (ZnO) nano-crystal film) as fluorescence coating.Due to problem described above, limit the application at electronic device of the perovskite quantum dot.How to improve the fluorescence efficiency of perovskite quantum dot light emitting thin film, become urgent need to solve the problem.And study the high molecular weight water soluble polymer being found that a kind of crystal property strengthening quantum dot and fluorescence quantum yield recently, i.e. polymine (C2H5N, Polyethylenimine, be called for short PEI), it has high tack, high adsorption, contributes to the advantages such as electronics injection simultaneously.
Based on the above, the present invention proposes a kind of novel light-emitting film, adopts PEI and ZnO nano brilliant in electron transport layer, and halogenide perovskite quantum dot is as fluorescence coating so that it is fluorescence quantum yield has and is obviously improved.Through searching, based on the efficient calcium titanium ore quantum dot light emitting thin film and preparation method thereof of PEI, both at home and abroad there are no relevant report.
Summary of the invention
In order to solve the problem that in prior art, perovskite quantum dot light emitting film fluorescence quantum yield is low, the preparation method of the perovskite quantum dot light emitting thin film of a kind of high-fluorescence quantum yield that the present invention proposes, devise a kind of novel structure simultaneously.
The present invention adopts the following technical scheme that realization, and accompanying drawings is as follows:
A kind of efficient calcium titanium ore quantum dot light emitting thin film based on PEI, adopt PEI and ZnO as electron transport layer, perovskite quantum dot light emitting thin film is as fluorescence coating, and its structure includes: the substrate 1 of ito thin film, the ZnO layer 2 being deposited on substrate, be spin-coated on ZnO nano brilliant thin do not go up PEI layer 3, the perovskite quantum dot 4 that is spin-coated on the ZnO nano crystalline substance thin film being coated with by PEI；Described ZnO layer and PEI layer are together to form electron transfer layer；Described inorganic caesium lead halogenide perovskite quantum dot is as luminescent layer 4.
The preparation method of a kind of efficient calcium titanium ore quantum dot light emitting thin film based on PEI, specifically comprises the following steps that
The first step, prepare halogenide perovskite quantum dot, first synthesize the oleate solution of corresponding halogen element, then reaction solution is heated in a nitrogen environment to clarification；Octadecane alkene and corresponding halogenide add oleic acid and oleyl amine, the oleate solution of synthesis is injected rapidly after solution is clear, it is centrifuged through supercooling, after the series of processes that redispersion is centrifuged again, discard the supernatant, and by precipitate redispersion, namely obtain the inorganic halides perovskite quantum dot of preparation；
Second step, prepare ZnO nano crystalline substance thin film, the mixed solution of zinc acetate with ethanol is stirred through nitrogen stream post-heating, inject the alcoholic solution containing sodium hydroxide after being cooled to room temperature and stir, after purification run, zinc oxide nanocrystalline solution centrifugal will be obtained and add hexane, then the precipitate obtained is purified again, finally give the ZnO nano crystalline substance thin film of preparation；
3rd step, electro-conductive glass (ITO) is successively cleaned with chemical reagent, then process under ultraviolet-ozone environment；
4th step, the ZnO nano crystalline substance thin film that will prepare, be spun in ITO substrate；
5th step, in glove box, PEI solution is spin-coated on ZnO nano crystal layer prepared by previous step；
6th step, by the method for spin coating, halogenide perovskite quantum dot solution is deposited on the ZnO nano crystalline substance thin film being coated with by PEI.
Chemical agent described in 3rd step includes: soap, deionized water, ethanol, chloroform, acetone or isopropanol.
Perovskite quantum dot light emitting thin film prepared by the present invention compared to existing technique prepare perovskite quantum dot light emitting thin film, its fluorescence quantum yield can improve 2～3 times.
Compared with prior art, the invention has the beneficial effects as follows:
1, the efficient calcium titanium ore quantum dot light emitting thin film based on PEI of the present invention, the material adopted makes the fluorescence quantum yield of light-emitting film promote；
2, the efficient calcium titanium ore quantum dot light emitting thin film based on PEI of the present invention, the material adopted makes the light-emitting film crystal property of formation strengthen.
3, the efficient calcium titanium ore quantum dot light emitting thin film based on PEI of the present invention, the material adopted makes the fluorescence lifetime of light-emitting film extend.
Accompanying drawing explanation
The schematic diagram of Fig. 1 present invention；
The overall construction drawing of Fig. 2 present invention；
The preparation method flow chart of Fig. 3 present invention；
The inorganic calcium titanium ore CsPbBrI of Fig. 4 present invention2The electron microscope picture of quantum dot；
The electron microscope picture that the ZnO nano of Fig. 5 present invention is brilliant；
Fig. 6 a, Fig. 6 b are respectively not or have the electron microscope picture of perovskite quantum dot film of PEI；
Fig. 7 is with or without the X-ray diffractogram of the perovskite quantum dot film of PEI；
The fluorescence decay curve of perovskite quantum dot light emitting thin film in tri-kinds of different structures of Fig. 8.
Fig. 9 is with and without the absorption of the perovskite quantum dot film of PEI and luminescent spectrum.
Detailed description of the invention
The embodiment further illustrating the efficient calcium titanium ore quantum dot light emitting thin film based on PEI of the present invention and preparation method thereof below in conjunction with accompanying drawing gives implementation process and test and assay, but protection scope of the present invention is not limited to following embodiment.
Embodiment
1, the preparation scheme based on the efficient calcium titanium ore quantum dot light emitting thin film of PEI is:
Step one, 10nm HONGGUANG inorganic calcium titanium ore CsPbBrI2The preparation of quantum dot.Prepared inorganic calcium titanium ore CsPbBrI2The peak value of quantum dot is at about 650nm.The method that building-up process is crossed according to prior disclosure is implemented.In order to synthesize the oleate solution of caesium, by cesium carbonate (0.8g), oleic acid, (Oleicacid is called for short OA, 2.5ml), octadecane alkene (Octadecene, it is called for short ODE, 30ml) join in the three-neck flask of 100ml, and at the temperature of 120 DEG C vacuum outgas and dry 1 hour.Reaction solution is heated to 150 DEG C under the environment of nitrogen, until solution clarification.By 10ml octadecane alkene (Octadecene is called for short ODE), 0.115g lead iodide (PbI2) and 0.046g lead bromide (PbBr2)) load in the three-necked bottle of 50 milliliters, dry and degassed 1 hour in 120 DEG C of vacuum, 1ml oleic acid (Oleicacid is called for short OA) after dried and 1ml oleyl amine (Oleylamine, abbreviation OLA) are expelled in flask at this temperature.After solution is apparent from, temperature is increased to 180 DEG C, injects rapidly the oleate solution (0.8ml, concentration 0.1mol/L in octadecane alkene solvent are preheated to 100 DEG C before injection) of caesium.After five seconds, by ice-water bath, reactant mixture is cooled to room temperature.Reactant mixture is centrifugal 10min when 5000 turns per minute.After centrifugal, by precipitate in 2ml toluene solution redispersion and when 12000 turns per minute recentrifuge.Repeat such step again, discard the supernatant, by precipitate redispersion in 2 milliliters of toluene solutions, obtain 10nm inorganic calcium titanium ore CsPbBrI2Quantum dot.
Step 2, prepare ZnO nano crystalline substance thin film.0.4403g zinc acetate and 30ml alcohol mixed solution are loaded 250ml three-necked bottle.After 10 minutes nitrogen stream, by three-necked bottle heated and stirred, mixed solution is made to seethe with excitement.After 30 minutes, acetic acid zinc powder is wholly absent, and solution becomes colorless transparent.Then, three-necked bottle naturally cooling to room temperature, solution becomes a white turbid solution.10ml alcoholic solution containing 0.2g sodium hydroxide is injected in flask rapidly, and continues stirring 4 hours.Then a series of purification run is carried out.Under normal circumstances, the zinc oxide nanocrystalline solution of 5ml is loaded in a 50ml centrifuge tube and fully adds hexane.Precipitate after centrifugal is dissolved in the ethanol of 3ml.Purify again, in finally giving the ZnO nano crystalline substance thin film being dissolved in 3ml ethanol and leaving the glove box of full nitrogen in.Ethanol makes the absolute methanol of 5% into according to volume ratio, the ethyl acetate of 1%, the pentane of 1% and the methyl-pentanol of 1%.
Step 3, by the glass substrate priority soap with ito thin film, deionized water, ethanol, chloroform, acetone, isopropanol cleans, and then processes 15 minutes at ultraviolet-ozone.
Step 4, by preparation ZnO nano crystalline substance thin film deposition on a glass substrate.The ZnO nano crystalline substance solution of synthesis is spin-coated on when 1000 turns per minute ITO electro-conductive glass upper 1 minute, and annealing 10 minutes under the temperature conditions of 150 DEG C in atmosphere.
Step 5, product previous step prepared are put in glove box.Being spun on ZnO nano crystalline substance thin film with the speed of 3000 turns per minute by PEI solution (being dissolved in the methyl cellosolve that mass fraction is 0.4%), and anneal 10 minutes at 100 DEG C of temperature, as electron transfer layer, thickness is 50nm.
Step 6, the inorganic calcium titanium ore CsPbBrI that will have prepared2Quantum dot is spun on the ZnO nano crystalline substance thin film being coated with PEI, and thickness is 60nm.
2, test and test result:
In order to verify the performance of perovskite quantum dot light emitting thin film of the present invention, the present invention has carried out following test:
(1) the present invention is directed to the sign of the perovskite quantum dot light emitting thin film in two kinds of structures to test: all with glass-ITO for substrate, one is deposited on the perovskite quantum dot light emitting thin film in electron transfer layer (ZnO nano is brilliant), two is first be spin-coated in electron transfer layer by PEI solution, then perovskite quantum dot is deposited on the light-emitting film in electron transfer layer.Consult Fig. 6, the latter's perovskite quantum dot film than former structure evenly, compact, it was shown that it is a kind of high-quality light-emitting film.
(2) in order to verify the advantage of the perovskite quantum dot light emitting thin film of the present invention further, the lattice structure situation of the perovskite quantum dot light emitting thin film in following two structure is analyzed by present invention X-ray diffraction analysis (XRD) technology: all with glass-ITO for substrate, one is deposited on the perovskite quantum dot light emitting thin film in electron transfer layer (ZnO nano is brilliant), two is first be spin-coated in electron transfer layer by PEI solution, then perovskite quantum dot is deposited on the light-emitting film in electron transfer layer:.The diffraction maximum consulting Fig. 7 perovskite quantum dot film that the latter and present invention proposition be can be observed increases to some extent, it was shown that PEI can improve the degree of crystallinity of quantum dot film, can improve its crystal structure.
(3) fluorescence quantum yield and the fluorescence lifetime of following three kinds of structures have been carried out contrast test by the present invention: perovskite quantum dot/ITO, perovskite quantum dot/ZnO/ITO, perovskite quantum dot/PEI/ZnO/ITO.Consulting Fig. 8, result shows that perovskite quantum dot slightly increases as the not only fluorescence lifetime of the light-emitting film in the structure of fluorescence coating, and its fluorescence quantum yield is also obviously improved using PEI and ZnO as electron transfer layer.
(4) in order to verify the raising of the fluorescence quantum yield of the present invention better, the absorption spectrum of perovskite quantum dot light emitting thin film in two kinds of structures and luminescent spectrum have been carried out relative analysis by the present invention.Consult Fig. 9, it is shown in the perovskite quantum dot being spin-coated on PEI layer higher than the fluorescence quantum yield value being directly spin-coated on electron transfer layer (ZnO nano is brilliant) upper perovskite quantum dot, it is obviously improved 88% by 20%, and does not change the luminescent spectrum of itself.
In sum, it was shown that the perovskite quantum dot light emitting thin film prepared by the present invention is compared to the perovskite quantum dot prepared by prior art, and its quantum fluorescence efficiency, performance are obviously improved, and given preparation method is attainable.
Claims (3)
1. the efficient calcium titanium ore quantum dot light emitting thin film based on PEI, it is characterised in that:
Adopt PEI and ZnO as electron transport layer, perovskite quantum dot light emitting thin film is as fluorescence coating, and its structure includes: the substrate (1) of ito thin film, the ZnO layer (2) being deposited on substrate, be spin-coated on ZnO nano brilliant thin do not go up PEI layer (3), the perovskite quantum dot (4) that is spin-coated on the ZnO nano crystalline substance thin film being coated with by PEI；Described ZnO layer and PEI layer are together to form electron transfer layer；Described inorganic caesium lead halogenide perovskite quantum dot is as luminescent layer (4).
2., based on a preparation method for the efficient calcium titanium ore quantum dot light emitting thin film of PEI, specifically comprise the following steps that
The first step, prepare halogenide perovskite quantum dot, first synthesize the oleate solution of corresponding halogen element, then reaction solution is heated in a nitrogen environment to clarification；Octadecane alkene and corresponding halogenide add oleic acid and oleyl amine, the oleate solution of synthesis is injected rapidly after solution is clear, it is centrifuged through supercooling, after the series of processes that redispersion is centrifuged again, discard the supernatant, and by precipitate redispersion, namely obtain the inorganic halides perovskite quantum dot of preparation；
Second step, prepare ZnO nano crystalline substance thin film, the mixed solution of zinc acetate with ethanol is stirred through nitrogen stream post-heating, inject the alcoholic solution containing sodium hydroxide after being cooled to room temperature and stir, after purification run, zinc oxide nanocrystalline solution centrifugal will be obtained and add hexane, then the precipitate obtained is purified again, finally give the ZnO nano crystalline substance thin film of preparation；
3rd step, electro-conductive glass (ITO) is successively cleaned with chemical reagent, then process under ultraviolet-ozone environment；
4th step, the ZnO nano crystalline substance thin film that will prepare, be spun in ITO substrate；
5th step, in glove box, PEI solution is spin-coated on ZnO nano crystal layer prepared by previous step；
6th step, by the method for spin coating, halogenide perovskite quantum dot solution is deposited on the ZnO nano crystalline substance thin film being coated with by PEI.
3. the preparation method of a kind of efficient calcium titanium ore quantum dot light emitting thin film based on PEI according to claim 2, the chemical agent described in the 3rd step includes: soap, deionized water, ethanol, chloroform, acetone or isopropanol.
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| CN106634987A (en) * | 2016-12-19 | 2017-05-10 | Tcl集团股份有限公司 | Metal halide perovskite quantum dot CsSnX3 and preparation method thereof |
| CN106938854A (en) * | 2017-03-14 | 2017-07-11 | 电子科技大学 | A kind of preparation method of large scale lead halide caesium perovskite crystal |
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| US11965124B2 (en) | 2018-12-29 | 2024-04-23 | Tcl Technology Group Corporation | QLED and manufacturing method thereof |
| CN109768169A (en) * | 2019-01-15 | 2019-05-17 | 新疆交通建设集团股份有限公司 | Iron carbonyl quantum dot perovskite light-absorption layer and preparation method thereof |
| CN111009613A (en) * | 2019-11-29 | 2020-04-14 | 武汉大学苏州研究院 | Perovskite quantum dot doped organic ultraviolet detector and preparation method thereof |
| CN113604220A (en) * | 2021-08-17 | 2021-11-05 | 东北电力大学 | Perovskite quantum dot material and preparation method and application thereof |
| CN113604220B (en) * | 2021-08-17 | 2023-06-13 | 东北电力大学 | Perovskite quantum dot material, and preparation method and application thereof |
| CN113956517A (en) * | 2021-10-13 | 2022-01-21 | 淮阴工学院 | Preparation method of multifunctional passive radiation cooling film |
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