CN111952470B - CdSe quantum dot doped with silicon dioxide and manufacturing method of light-emitting diode device - Google Patents
CdSe quantum dot doped with silicon dioxide and manufacturing method of light-emitting diode device Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 239000002096 quantum dot Substances 0.000 title claims abstract description 68
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 57
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 41
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
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- 238000000034 method Methods 0.000 claims abstract description 23
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 13
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- 230000008569 process Effects 0.000 claims abstract description 11
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 48
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 46
- 238000003756 stirring Methods 0.000 claims description 44
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 39
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 32
- 239000000758 substrate Substances 0.000 claims description 31
- 238000000137 annealing Methods 0.000 claims description 29
- 239000002243 precursor Substances 0.000 claims description 28
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 23
- 239000011787 zinc oxide Substances 0.000 claims description 23
- 235000019441 ethanol Nutrition 0.000 claims description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 16
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 16
- 229910052711 selenium Inorganic materials 0.000 claims description 16
- 239000011669 selenium Substances 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000004246 zinc acetate Substances 0.000 claims description 13
- 230000005525 hole transport Effects 0.000 claims description 12
- 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 12
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 7
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 claims description 7
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 claims description 7
- 239000003921 oil Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
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- OUEFENYULDYAFC-UHFFFAOYSA-N dioxosilane hexane Chemical compound CCCCCC.[Si](=O)=O OUEFENYULDYAFC-UHFFFAOYSA-N 0.000 claims description 2
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- 239000007788 liquid Substances 0.000 claims description 2
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- 230000003301 hydrolyzing effect Effects 0.000 claims 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 abstract description 4
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 abstract 1
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
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- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
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- 239000003814 drug Substances 0.000 description 3
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- 239000002904 solvent Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- 229920000144 PEDOT:PSS Polymers 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 239000002346 layers by function Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
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- 229910052905 tridymite Inorganic materials 0.000 description 1
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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]
- H10K50/11—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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- 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]
- H10K50/11—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers
- H10K50/12—OLEDs or polymer light-emitting diodes [PLED] characterised by the electroluminescent [EL] layers comprising dopants
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
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- Optics & Photonics (AREA)
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- Nanotechnology (AREA)
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Abstract
The invention relates to a method for manufacturing CdSe quantum dots doped with silicon dioxide and a light-emitting diode device, which comprises the steps of firstly preparing PEDOT on an ITO (indium tin oxide) film by a spin coating process after cleaning and ozone treatment of ITO conductive glass on the ITO glass: and the PSS layer is sequentially spin-coated to obtain a TFB layer, a CdSe quantum dot luminescent layer, a ZnO electron transport layer and a silicon dioxide electrode, wherein silicon dioxide nano particles modified by a silane coupling agent KH550 and stearic acid are particularly used for doping in the quantum dot layer, and finally the CdSe quantum dot doped with silicon dioxide and a light-emitting diode device are formed. The CdSe is doped by the silicon dioxide nano particles, so that the gap between the quantum dots is ensured to be filled, the possibility that electron holes are compounded through the gap is reduced, and the performance of the device is improved under the condition of ensuring the carrier concentration.
Description
Technical Field
The invention belongs to the field of photoelectric materials and devices, and particularly relates to a method for manufacturing CdSe quantum dots doped with silicon dioxide and a light-emitting diode device.
Background
With the development of technology and the advancement of society, information communication and delivery become an indispensable part of daily life. The quantum dot photoluminescence optical thin film device, which is the most practical display device, plays a vital role in the fields of information communication, transmission and the like. The quantum dot luminescent optical thin film device is the most practical display device, and has become the most popular research object at present because of the advantages of excellent photoluminescence, wide color gamut, adjustable light color and the like. In the present day, most quantum dot light emitting diodes choose to prepare a quantum dot precursor solution first, which is then spin coated to form a device. In order to improve the luminescence performance of the device and improve the luminescence stability and service life, the particle size of the quantum dot material or the improvement of each functional layer of the quantum dot device needs to be controlled to improve the performance of the device and the like. Through a great deal of experiments, the quantum dot light emitting diode device with better light emitting performance is obtained by doping or modifying different functional layers of the quantum dot light emitting diode device by using some substances.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for manufacturing a CdSe quantum dot doped with silicon dioxide and a light emitting diode device, which can improve the performance of the device while ensuring the concentration of electron holes.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a method for manufacturing CdSe quantum dots doped with silicon dioxide and a light-emitting diode device comprises the following steps:
step S1: selecting an ITO glass as a substrate of a light-emitting diode, wherein the ITO glass comprises a glass substrate and an ITO film covered on the surface of the glass substrate;
step S2: spin coating PEDOT on ITO conductive glass: PSS solution and forming a film by annealing and drying;
step S3: a hole transport layer solution was prepared and spin-coated on PEDOT: annealing and drying the PSS film layer to form a hole transport layer;
step S4: modifying the silicon dioxide nano-particles by using a silane coupling agent KH550 and stearic acid, and dissolving the nano-particles by using n-hexane to prepare an n-hexane solution of the silicon dioxide nano-particles;
step S5: preparing CdSe quantum dots, preparing a mixed solution of the CdSe quantum dots and silicon dioxide nano particles, and spin-coating the solution on the hole transport layer to form a CdSe quantum dot light-emitting central layer;
step S6: preparing ZnO solution, and spin-coating the solution on the quantum dot film layer to form an electron transport layer of zinc oxide;
step S7: and (3) evaporating silver on the sample wafer prepared in the step (S6) by utilizing an evaporation technology to form a silver electrode, so as to prepare the CdSe quantum dot light-emitting diode doped with silicon dioxide.
Further, the step S3 specifically includes:
step S31, TFB is dissolved in chlorobenzene to prepare a hole transport layer solution;
step S32, spin-coating the solution to the solution which is spin-coated with PEDOT: and forming a hole transport layer on the ITO conductive glass substrate of the PSS film by annealing and drying.
Further, the specific step S4 is:
step S41: weighing a proper amount of silica nano particles, adding the silica nano particles into the stirred and hydrolyzed absolute ethyl alcohol/water mixed solution containing the silane coupling agent KH550, stirring vigorously to uniformly disperse the silica, stirring for a period of time under the condition of an oil bath, centrifuging, washing for a plurality of times by using ethanol, and drying to obtain silica particles modified by the silane coupling agent;
step S42: weighing a certain amount of stearic acid to dissolve in dimethylbenzene, uniformly dispersing silicon dioxide particles modified by a silane coupling agent under the stirring condition, reacting for a period of time at constant temperature, centrifugally washing and drying, and dissolving by using a proper amount of normal hexane to prepare a normal hexane solution of modified silicon dioxide nano particles.
Further, the step S5 specifically includes:
step S51, stirring and dissolving selenium powder, sulfur powder and TOP solution at a preset temperature to prepare a precursor solution of selenium;
step S52, stirring cadmium oxide, zinc acetate and oleic acid for a preset time, then injecting a small amount of ODE solution, and raising the temperature of the solution;
step S53, taking a selenium precursor solution, rapidly injecting the selenium precursor solution into the solution when the solution temperature reaches a preset value, and keeping the solution for a period of time, and simultaneously, exciting by using an ultraviolet lamp; finally, rapidly cooling the quantum dot solution in a water bath mode, and diluting with n-hexane to obtain the quantum dot solution;
step S54: taking out the supernatant of the quantum dot solution after partial standing, dissolving oleic acid by using a proper amount of methanol, adding a proper amount of normal hexane solution for dissolving, taking out an upper layer solution, adding a proper amount of absolute ethyl alcohol for centrifuging, and finally dissolving precipitate by using a normal hexane solution of silica nano particles to obtain a purified quantum dot solution;
and S55, taking out the purified quantum dot solution, and preparing the CdSe quantum dot film on the ITO glass substrate with the hole transport layer by a spin coating mode.
Further, the step S6 specifically includes:
step S61: mixing zinc acetate dihydrate with a DMSO solution, and heating and stirring at a preset temperature to prepare the DMSO solution of zinc acetate;
step S62, mixing TMAH and ethanol, and stirring until the mixture is clear and transparent to obtain an ethanol solution of TMAH;
step 63, dropwise adding an ethanol solution of TMAH into a zinc acetate solution, and heating and stirring for a period of time at a preset temperature; precipitating the reaction solution by using a proper amount of ethyl acetate after the reaction is finished, obtaining ZnO precipitate by a centrifugal filtration method, dissolving by using a proper amount of butanol solution, and filtering to obtain ZnO solution;
step S64: and spin-coating the ZnO solution on the ITO glass substrate with the quantum dot film by using a spin-coating process, and annealing and drying to obtain the ZnO film.
Further, the PEDOT: the use level of PSS is 70-90 mu l, the rotating speed of the spin coating process is 1000-5000rpm, the annealing time is 10-30min, and the annealing temperature is 110-130 ℃.
Further, the concentration of the TFB is 8mg/ml, the revolution of the spin coating process is 1000-5000rpm, the annealing time is 10-30min, and the annealing temperature is 110-130 ℃.
Further, the oil bath temperature is 60-100 ℃ and the holding time is 2-4 hours when the silicon dioxide particles modified by the silane coupling agent are prepared; the centrifugal speed and the centrifugal time are respectively 3000-6000rpm and 5min; the temperature is 50-80 ℃ and the time is 2-4h when the stearic acid is used for further modification; the centrifugal speed and time are 6000-8000rpm and 5min respectively, and the finally prepared normal hexane solution of the silicon dioxide nano particles is prepared by weighing a proper amount of silicon dioxide nano particle powder according to the concentration range of 0.1 mg/ml-1 g/ml and dissolving by using a corresponding amount of normal hexane solution.
Further, in the precursor solution of selenium, the ratio of selenium powder to sulfur powder is 1:0.8, stirring temperature is 140-160 ℃; the ratio of cadmium oxide to zinc acetate is 1:3, the stirring temperature is 140-160 ℃, ODE solution is injected when the stirring time reaches 30min, meanwhile, the rising temperature is 290-310 ℃, the precursor solution of selenium is rapidly injected, the holding time is 10min, the precursor solution is excited by an ultraviolet lamp, in the quantum dot cleaning process, the ratio of the supernatant liquid of the quantum dot to methanol is 1:1, absolute ethyl alcohol needs more than upper solution, and finally, the prepared silicon dioxide n-hexane solution is used for dissolving, in the spin coating process of the quantum dot layer, the rotating speed is 2000-4000rpm, the annealing temperature is 80-120 ℃, and the time is 60s.
Further, in the preparation of the ZnO solution, the mass ratio of zinc acetate dihydrate to TMAH is 1:1.4-2, the stirring temperature of the zinc acetate dihydrate and the DMSO solution is 50 ℃, and the rotating speed is 450rpm; the concentration of the DMSO solution is analytically pure, and the ethanol solution of TMAH is dripped into the zinc acetate solution at a constant speed, and the stirring speed and the stirring time are respectively 500rpm and 1 h; the ratio of ethyl acetate to the reaction liquid is 1:1, the rotating speed and the time of centrifugation are 3000-6000rpm and 3min respectively; the spin-coating parameters of ZnO are 2000-4000rpm and kept for 45s, and the annealing parameters are 130-150 ℃ and annealed for 10-30min respectively.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method is novel, the preparation cost is low, the preparation process is simple, the modified silicon dioxide particles can be well combined with the quantum dots by doping the CdSe quantum dot layer with the silicon dioxide doped material, the pores among the quantum dots are filled to a certain extent, the compactness of the quantum dot luminescent layer is improved, and therefore the performance of the quantum dot light-emitting diode device in brightness and the like is improved.
Drawings
FIG. 1 is a schematic diagram of an ITO glass substrate according to an embodiment of the present invention
FIG. 2 is a schematic illustration of an embodiment of the invention plated with a layer of PEDOT: ITO glass substrate structure schematic diagram of PSS film
FIG. 3 is a schematic diagram showing the structure of an ITO glass substrate with TFB thin film according to an embodiment of the invention
FIG. 4 is a schematic diagram of the structure of an ITO glass substrate after spin-coating quantum dots according to an embodiment of the present invention
FIG. 5 is a schematic view showing the structure of an ITO glass substrate on which ZnO is formed in one 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-glass substrate, 2-ITO layer, 3-PEDOT: PSS film, 4-TFB film, 5-CdSe quantum dot, 6-SiO2 nanoparticle, 7-electron transport layer, 8-Ag electrode.
Detailed Description
The invention will be further described with reference to the accompanying drawings and examples.
Example 1
(1) Absolute ethanol/water 9:1, adding 25wt.% of silane coupling agent into the mixed solution, and stirring for 30min to hydrolyze. A certain amount of silicon dioxide powder is weighed and added into the solution, the solution is reacted for 3 hours at a constant temperature of 80 ℃ by using an oil bath, then the product is centrifuged at 6000rpm and washed for a plurality of times by using ethanol, and finally the product is placed into a vacuum oven at 60 ℃ and dried for 12 hours, thus obtaining the silicon dioxide powder modified by the silane coupling agent. 1ml of stearic acid was mixed with 9ml of xylene, 50mg of silica powder modified with a silane coupling agent was added, reacted at 60℃for 3 hours, centrifuged at 6000rpm for 5 minutes, washed with ethanol several times, and dried at 60℃for 12 hours. 5mg of silicon dioxide powder modified by a silane coupling agent and stearic acid is weighed and dissolved in 50ml of normal hexane solution to obtain normal hexane solution of silicon dioxide nano particles with concentration of 0.1 mg/ml.
(2) 0.6585g of zinc acetate dihydrate medicine is weighed and placed in a clean reagent bottle with clean magneton and capacity of 100 ml, 30 ml of DMSO solution is extracted by a pipette and is dripped into the reagent bottle, the reagent bottle is placed on a heating stirring table, the temperature is set to be 50 ℃, the rotating speed is 450rpm, and the zinc acetate dihydrate is dissolved in DMSO solvent by intense stirring; next, 0.9062 g of TMAH agent was weighed and placed in a small reagent bottle, and 10 ml ethanol solution was extracted with a pipette, added to the reagent bottle, and stirred until clear and transparent. And then dripping the prepared TMAH solution into the DMSO precursor at a constant speed within 8 min, and keeping the rotating speed at 500rpm for 1h. After the completion of the reaction, the reaction solution was subjected to a precipitation operation with an equal ratio of ethyl acetate. Respectively extracting the reaction solution and ethyl acetate solution with equal amounts (5 ml) by using a rubber head dropper, placing the reaction solution and the ethyl acetate solution into a centrifuge tube, centrifuging for 3min at a rotating speed of 3000rpm, taking out the centrifuge tube after centrifuging, pouring out supernatant, and dissolving by using butanol solution;
(3) Taking 0.0158g of selenium powder and 0.128g of sulfur powder, placing into a three-neck flask, adding 2ml of TOP solution, and stirring at 150 ℃ to dissolve to prepare a precursor solution of selenium; 0.0257g of cadmium oxide and 0.878g of zinc acetate are weighed into a three-neck flask, 5ml of OA solution is added, stirring is carried out for 30min at 150 ℃, then 15ml of ODE solution is injected, the temperature of the solution is increased to 300 ℃, the precursor solution of selenium is rapidly injected and kept for 10min, excitation is carried out at 2min by using an ultraviolet lamp, finally the quantum dot solution is cooled by using a water bath mode, and the quantum dot solution is dissolved by using n-hexane and kept stand at low temperature. Dissolving the supernatant of the quantum dot solution by using methanol before spin coating, then adding n-hexane, extracting an upper layer solution, adding excessive absolute ethyl alcohol, centrifuging for 10min at 6000 revolutions, and then dissolving the quantum dots by using the n-hexane of the prepared silicon dioxide nano particles;
(4) Selecting an ITO conductive glass sheet, firstly ultrasonically cleaning ITO for 15min by using deionized water and glass respectively, then wiping the ITO clean by using dust-free cloth, then ultrasonically cleaning the ITO for 15min by using acetone and ethanol respectively, and finally drying in an oven. Before spin coating the film, carrying out plasma ozone treatment on the ITO for 20-30 min;
(5) Placing the substrate on a spin coater, setting the rotating speed to 4000rpm, keeping for 40s, and selecting PEDOT: 80 μl of PSS, rapidly dripping the solution on the surface of the substrate while pressing a starting button of a spin coater, and annealing at 120deg.C for 20min after spin coating;
(6) TFB was dissolved in chlorobenzene solution to prepare a solution having a concentration of 8mg/ml, and the TFB chlorobenzene solution was filtered by using a 0.2 μm filter head, and the spin coater parameters were adjusted to 3000rpm and maintained for 30 seconds. While pressing the start button of the spin coater, 65 μl of the solution was quickly dropped onto the surface of the device with a pipette, spin coated, and then annealed at 120deg.C for 20min on a hotplate.
(7) Placing the substrate on a spin coater, adjusting the rotating speed of the spin coater to 4000rpm, keeping the rotating speed for 45 seconds, selecting 85 mu l of prepared quantum dot precursor solution by using a pipetting gun, rapidly 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 spin coating, and keeping the temperature of 120 ℃ for annealing for 20 minutes.
(8) The ZnO butanol solution was filtered using a 0.2 μm filter head, and 110. Mu.l of the ZnO solution was applied to the ITO glass surface by a pipette during spin coating, and the spin speed of the spin coater was adjusted to 4000rpm for 45s, followed by annealing at 150℃for 20min.
(9) And under the vacuum condition, the deposition rate of the deposited silver with the thickness of 60 nm is 0.3 nm/s, and the silver is dried for 1h at room temperature, so that the light-emitting diode is obtained.
Example two
(1) Absolute ethanol/water 9:1, adding 25wt.% of silane coupling agent into the mixed solution, and stirring for 30min to hydrolyze. A certain amount of silicon dioxide powder is weighed and added into the solution, the solution is reacted for 3 hours at a constant temperature of 80 ℃ by using an oil bath, then the product is centrifuged at 6000rpm and washed for a plurality of times by using ethanol, and finally the product is placed into a vacuum oven at 60 ℃ and dried for 12 hours, thus obtaining the silicon dioxide powder modified by the silane coupling agent. 1ml of stearic acid was mixed with 9ml of xylene, 50mg of silica powder modified with a silane coupling agent was added, reacted at 60℃for 3 hours, centrifuged at 6000rpm for 5 minutes, washed with ethanol several times, and dried at 60℃for 12 hours. 25mg of silica powder modified with a silane coupling agent and stearic acid was weighed and dissolved with 50ml of n-hexane to obtain an n-hexane solution of silica nanoparticles at a concentration of 0.5 mg/ml.
(2) 0.6585g of zinc acetate dihydrate medicine is weighed and placed in a clean reagent bottle with clean magneton and capacity of 100 ml, 30 ml of DMSO solution is extracted by a pipette and is dripped into the reagent bottle, the reagent bottle is placed on a heating stirring table, the temperature is set to be 50 ℃, the rotating speed is 450rpm, and the zinc acetate dihydrate is dissolved in DMSO solvent by intense stirring; then 1.317 g TMAH reagent is weighed and placed in a small reagent bottle, 10 ml ethanol solution is extracted by a pipette, added into the reagent bottle and stirred until the reagent bottle 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 rotating speed at 500rpm for 1h. After the completion of the reaction, the reaction solution was subjected to a precipitation operation with an equal ratio of ethyl acetate. Respectively extracting the reaction solution and ethyl acetate solution with equal amounts (5 ml) by using a rubber head dropper, placing the reaction solution and the ethyl acetate solution into a centrifuge tube, centrifuging for 3min at a rotating speed of 3000rpm, taking out the centrifuge tube after centrifuging, pouring out supernatant, and dissolving by using butanol solution;
(3) Taking 0.0158g of selenium powder and 0.128g of sulfur powder, placing into a three-neck flask, adding 2ml of TOP solution, and stirring at 150 ℃ to dissolve to prepare a precursor solution of selenium; 0.0257g of cadmium oxide and 0.878g of zinc acetate are weighed into a three-neck flask, 5ml of OA solution is added, stirring is carried out for 30min at 150 ℃, then 15ml of ODE solution is injected, the temperature of the solution is increased to 300 ℃, the precursor solution of selenium is rapidly injected and kept for 10min, excitation is carried out at 2min by using an ultraviolet lamp, finally the quantum dot solution is cooled by using a water bath mode, and the quantum dot solution is dissolved by using n-hexane and kept stand at low temperature. Before spin coating, methanol is used for dissolving the supernatant of the quantum dot solution, then n-hexane is added, the upper layer solution is extracted, excessive absolute ethyl alcohol is added, and the solution is centrifuged for 10min at 6000 revolutions, and then the prepared silicon dioxide nano particles are used for dissolving the quantum dots.
(4) Selecting an ITO conductive glass sheet, firstly ultrasonically cleaning ITO for 15min by using deionized water and glass respectively, then wiping the ITO clean by using dust-free cloth, then ultrasonically cleaning the ITO for 15min by using acetone and ethanol respectively, and finally drying in an oven. Before spin coating the film, carrying out plasma ozone treatment on the ITO for 20-30 min;
(5) Placing the substrate on a spin coater, setting the rotating speed to 3000rpm, keeping for 40s, and selecting PEDOT: 80 μl of PSS, rapidly dripping the solution on the surface of the substrate while pressing a starting button of a spin coater, and annealing at 110deg.C for 20min after spin coating;
(6) TFB was dissolved in chlorobenzene solution to prepare a solution having a concentration of 8mg/ml, and the TFB chlorobenzene solution was filtered by using a 0.2 μm filter head, and the spin coater parameters were adjusted to 4000rpm and maintained for 30 seconds. While pressing the start button of the spin coater, 65 μl of the solution was quickly dropped onto the surface of the device with a pipette, spin coated, and then annealed at 110deg.C for 20min on a hotplate.
(7) Placing the substrate on a spin coater, adjusting the rotating speed of the spin coater to 3000rpm, keeping the rotating speed for 45s, selecting 85 mu l of prepared quantum dot precursor solution by using a pipetting gun, rapidly 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 spin coating, and keeping the temperature of 110 ℃ for annealing for 20min.
(8) The ZnO butanol solution was filtered using a 0.2 μm filter head, and 110. Mu.l of the ZnO solution was applied to the ITO glass surface by a pipette during spin coating, and the spin speed of the spin coater was adjusted to 4000rpm for 45s, followed by annealing at 150℃for 20min.
(9) And under the vacuum condition, the deposition rate of the deposited silicon dioxide with the thickness of 60 and nm is 0.3 nm/s, and the silicon dioxide is dried for 1h at room temperature, so that the light-emitting diode is obtained.
Example III
(1) Absolute ethanol/water 9:1, adding 25wt.% of silane coupling agent into the mixed solution, and stirring for 30min to hydrolyze. A certain amount of silicon dioxide powder is weighed and added into the solution, the solution is reacted for 3 hours at a constant temperature of 80 ℃ by using an oil bath, then the product is centrifuged at 6000rpm and washed for a plurality of times by using ethanol, and finally the product is placed into a vacuum oven at 60 ℃ and dried for 12 hours, thus obtaining the silicon dioxide powder modified by the silane coupling agent. 1ml of stearic acid was mixed with 9ml of xylene, 50mg of silica powder modified with a silane coupling agent was added, reacted at 60℃for 3 hours, centrifuged at 6000rpm for 5 minutes, washed with ethanol several times, and dried at 60℃for 12 hours. 50mg of silica powder modified by a silane coupling agent and stearic acid was weighed and dissolved with 50ml of n-hexane to obtain an n-hexane solution of silica nanoparticles having a concentration of 1 mg/ml.
(2) 0.6585g of zinc acetate dihydrate medicine is weighed and placed in a clean reagent bottle with clean magneton and capacity of 100 ml, 30 ml of DMSO solution is extracted by a pipette and is dripped into the reagent bottle, the reagent bottle is placed on a heating stirring table, the temperature is set to be 50 ℃, the rotating speed is 450rpm, and the zinc acetate dihydrate is dissolved in DMSO solvent by intense stirring; next, 1.1194 g of TMAH agent was weighed and placed in a small reagent bottle, and 10 ml ethanol solution was extracted with a pipette, added to the reagent bottle, and stirred until clear and transparent. And then dripping the prepared TMAH solution into the DMSO precursor at a constant speed within 8 min, and keeping the rotating speed at 500rpm for 1h. After the completion of the reaction, the reaction solution was subjected to a precipitation operation with an equal ratio of ethyl acetate. Respectively extracting the reaction solution and ethyl acetate solution with equal amounts (5 ml) by using a rubber head dropper, placing the reaction solution and the ethyl acetate solution into a centrifuge tube, centrifuging for 3min at a rotating speed of 3000rpm, taking out the centrifuge tube after centrifuging, pouring out supernatant, and dissolving by using butanol solution;
(3) Taking 0.0158g of selenium powder and 0.128g of sulfur powder, placing into a three-neck flask, adding 2ml of TOP solution, and stirring at 150 ℃ to dissolve to prepare a precursor solution of selenium; 0.0257g of cadmium oxide and 0.878g of zinc acetate are weighed into a three-neck flask, 5ml of OA solution is added, stirring is carried out for 30min at 150 ℃, then 15ml of ODE solution is injected, the temperature of the solution is increased to 300 ℃, the precursor solution of selenium is rapidly injected and kept for 10min, excitation is carried out at 2min by using an ultraviolet lamp, finally the quantum dot solution is cooled by using a water bath mode, and the quantum dot solution is dissolved by using n-hexane and kept stand at low temperature. Before spin coating, methanol is used for dissolving the supernatant of the quantum dot solution, then n-hexane is added, the upper layer solution is extracted, excessive absolute ethyl alcohol is added, and the solution is centrifuged for 10min at 6000 revolutions, and then the prepared silicon dioxide nano particles are used for dissolving the quantum dots.
(4) Selecting an ITO conductive glass sheet, firstly ultrasonically cleaning ITO for 15min by using deionized water and glass respectively, then wiping the ITO clean by using dust-free cloth, then ultrasonically cleaning the ITO for 15min by using acetone and ethanol respectively, and finally drying in an oven. Before spin coating the film, carrying out plasma ozone treatment on the ITO for 20-30 min;
(5) Placing the substrate on a spin coater, setting the rotation speed to 5000rpm, maintaining for 40s, and selecting PEDOT: PSS 90 μl, rapidly dripping the solution on the surface of the substrate while pressing a starting button of a spin coater, and annealing at 120deg.C for 20min after spin coating;
(6) TFB was dissolved in chlorobenzene solution to prepare a solution with a concentration of 8mg/ml, and the TFB chlorobenzene solution was filtered with a 0.2 μm filter head, and the spin coater parameters were adjusted to 5000rpm and maintained for 30s. While pressing the start button of the spin coater, 65 μl of the solution was quickly dropped onto the surface of the device with a pipette, spin coated, and then annealed at 130deg.C for 20min on a hotplate.
(7) Placing the substrate on a spin coater, adjusting the rotating speed of the spin coater to 2000rpm, keeping the rotating speed for 45s, selecting 110 mu l of prepared quantum dot precursor solution by using a pipetting gun, rapidly 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 spin coating, and keeping the temperature of 130 ℃ for annealing for 20min.
(8) The ZnO butanol solution was filtered using a 0.2 μm filter head, and 110. Mu.l of the ZnO solution was applied to the ITO glass surface by a pipette during spin coating, and the spin speed of the spin coater was adjusted to 4000rpm for 45s, followed by annealing at 150℃for 20min.
(9) And under the vacuum condition, the deposition rate of the deposited silver with the thickness of 60 nm is 0.3 nm/s, and the silver is dried for 1h at room temperature, so that the light-emitting diode is obtained.
The foregoing description is only of the preferred embodiments of the invention, and all changes and modifications that come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (8)
1. The manufacturing method of the CdSe quantum dot doped with the silicon dioxide and the light-emitting diode device is characterized by comprising the following steps:
step S1: selecting ITO conductive glass as a substrate of the light-emitting diode;
step S2: spin coating PEDOT on ITO conductive glass: PSS solution and forming a film by annealing and drying;
step S3: a hole transport layer solution was prepared and spin-coated on PEDOT: annealing and drying the PSS film layer to form a hole transport layer;
step S4: modifying the silicon dioxide nano-particles by using a silane coupling agent KH550 and stearic acid, and dissolving the nano-particles by using n-hexane to prepare an n-hexane solution of the silicon dioxide nano-particles;
step S5: preparing CdSe quantum dots, preparing a mixed solution of the CdSe quantum dots and silicon dioxide nano particles, and spin-coating the mixed solution on the hole transport layer to form a CdSe quantum dot light-emitting central layer;
step S6: preparing ZnO solution, and spin-coating the solution on the quantum dot film layer to form an electron transport layer of zinc oxide;
step S7: evaporating silver on the sample wafer prepared in the step S6 by utilizing an evaporation technology to form a silver electrode, so as to prepare the CdSe quantum dot light-emitting diode doped with silicon dioxide;
the specific steps of the step S4 are as follows:
step S41: weighing a certain amount of silica nano particles, adding the silica nano particles into the anhydrous ethanol/water mixed solution containing the silane coupling agent KH550 after stirring and hydrolyzing, vigorously stirring to uniformly disperse the silica, stirring for a period of time under the condition of an oil bath, centrifuging, washing for a plurality of times by using ethanol, and drying to obtain silica particles modified by the silane coupling agent;
step S42: weighing a certain amount of stearic acid to dissolve in dimethylbenzene, uniformly dispersing silicon dioxide particles modified by a silane coupling agent under the stirring condition, reacting for a period of time at constant temperature, centrifugally washing and drying, and dissolving by using a proper amount of normal hexane to prepare a normal hexane solution of modified silicon dioxide nano particles;
the step S5 specifically comprises the following steps:
step S51, stirring and dissolving selenium powder, sulfur powder and TOP solution at a preset temperature to prepare a precursor solution of selenium;
step S52, stirring cadmium oxide, zinc acetate and oleic acid for a preset time, then injecting a small amount of ODE solution, and raising the temperature of the solution;
step S53, taking a selenium precursor solution, rapidly injecting the selenium precursor solution into the solution when the solution temperature reaches a preset value, and keeping the solution for a period of time, and simultaneously, exciting by using an ultraviolet lamp; finally, rapidly cooling the quantum dot solution in a water bath mode, and diluting with n-hexane to obtain the quantum dot solution;
step S54: taking out the supernatant of the quantum dot solution after partial standing, dissolving oleic acid by using a proper amount of methanol, adding a proper amount of normal hexane solution for dissolving, taking out an upper layer solution, adding a proper amount of absolute ethyl alcohol for centrifuging, and finally dissolving precipitate by using a normal hexane solution of silica nano particles to obtain a purified quantum dot solution;
and S55, taking out the purified quantum dot solution, and preparing the CdSe quantum dot film on the ITO glass substrate with the hole transport layer by a spin coating mode.
2. The method for manufacturing the CdSe quantum dot and the light emitting diode device doped with silicon dioxide according to claim 1, wherein the step S3 is specifically:
step S31, TFB is dissolved in chlorobenzene to prepare a hole transport layer solution;
step S32, spin-coating the solution to the solution which is spin-coated with PEDOT: and forming a hole transport layer on the ITO conductive glass substrate of the PSS film by annealing and drying.
3. The method for manufacturing the CdSe quantum dot and the light emitting diode device doped with silicon dioxide according to claim 1, wherein the step S6 is specifically:
step S61: mixing zinc acetate dihydrate with a DMSO solution, and heating and stirring at a preset temperature to prepare the DMSO solution of zinc acetate;
step S62, mixing TMAH and ethanol, and stirring until the mixture is clear and transparent to obtain an ethanol solution of TMAH;
step 63, dropwise adding an ethanol solution of TMAH into a zinc acetate solution, and heating and stirring for a period of time at a preset temperature; precipitating the reaction solution by using a proper amount of ethyl acetate after the reaction is finished, obtaining ZnO precipitate by a centrifugal filtration method, dissolving by using a proper amount of butanol solution, and filtering to obtain ZnO solution;
step S64: and spin-coating the ZnO solution on the ITO glass substrate with the quantum dot film by using a spin-coating process, and annealing and drying to obtain the ZnO film.
4. The method for manufacturing the CdSe quantum dot doped with silicon dioxide and the light emitting diode device according to claim 1, wherein the method comprises the following steps: the PEDOT: the use level of PSS is 70-90 mu l, the rotating speed of the spin coating process is 1000-5000rpm, the annealing time is 10-30min, and the annealing temperature is 110-130 ℃.
5. The method for manufacturing CdSe quantum dots and light-emitting diode devices doped with silicon dioxide according to claim 2, wherein the concentration of TFB is 8mg/ml, the spin-coating process revolution is 1000-5000rpm, the annealing time is 10-30min, and the annealing temperature is 110-130 ℃.
6. The method for manufacturing CdSe quantum dots and light-emitting diode devices doped with silicon dioxide according to claim 1, wherein the oil bath temperature is 60-100deg.C and the holding time is 2-4h when preparing silicon dioxide particles modified by silane coupling agent; the centrifugal speed and the centrifugal time are respectively 3000-6000rpm and 5min; the temperature is 50-80 ℃ and the time is 2-4h when the stearic acid is used for further modification; the centrifugal speed and time are 6000-8000rpm and 5min respectively, and the finally prepared normal hexane solution of the silicon dioxide nano particles is prepared by weighing a proper amount of silicon dioxide nano particle powder according to the concentration range of 0.1 mg/ml-1 g/ml and dissolving by using a corresponding amount of normal hexane solution.
7. The method for manufacturing CdSe quantum dots and light-emitting diode devices doped with silicon dioxide according to claim 1, wherein the ratio of selenium powder to sulfur powder in the precursor solution of selenium is 1:0.8, stirring temperature is 140-160 ℃; the ratio of cadmium oxide to zinc acetate is 1:3, the stirring temperature is 140-160 ℃, ODE solution is injected when the stirring time reaches 30min, meanwhile, the rising temperature is 290-310 ℃, the precursor solution of selenium is rapidly injected, the holding time is 10min, the precursor solution is excited by an ultraviolet lamp, in the quantum dot cleaning process, the ratio of the supernatant liquid of the quantum dot to methanol is 1:1, absolute ethyl alcohol needs more than upper solution, and finally, the prepared silicon dioxide n-hexane solution is used for dissolving, in the spin coating process of the quantum dot layer, the rotating speed is 2000-4000rpm, the annealing temperature is 80-120 ℃, and the time is 60s.
8. The method for manufacturing CdSe quantum dot and light-emitting diode device doped with silicon dioxide according to claim 3, wherein in the preparation of ZnO solution, the mass ratio of zinc acetate dihydrate to TMAH is 1:1.4-2, the stirring temperature of the zinc acetate dihydrate and the DMSO solution is 50 ℃, and the rotating speed is 450rpm; the concentration of the DMSO solution is analytically pure, and the ethanol solution of TMAH is dripped into the zinc acetate solution at a constant speed, and the stirring speed and the stirring time are respectively 500rpm and 1 h; the ratio of ethyl acetate to the reaction liquid is 1:1, the rotating speed and the time of centrifugation are 3000-6000rpm and 3min respectively; the spin-coating parameters of ZnO are 2000-4000rpm and kept for 45s, and the annealing parameters are 130-150 ℃ and annealed for 10-30min respectively.
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