CN105514238A - Electroluminescent device based on carbon quantum dots and preparation method thereof - Google Patents
Electroluminescent device based on carbon quantum dots and preparation method thereof Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 40
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 24
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011521 glass Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001338 self-assembly Methods 0.000 claims abstract description 15
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical group [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 claims abstract description 9
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 19
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 14
- 239000013049 sediment Substances 0.000 claims description 12
- 239000012279 sodium borohydride Substances 0.000 claims description 12
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 9
- -1 octadecylene Chemical group 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 125000003368 amide group Chemical group 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 claims description 3
- 238000005260 corrosion Methods 0.000 claims description 3
- 239000003599 detergent Substances 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 230000000717 retained effect Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000010409 thin film Substances 0.000 abstract description 5
- 238000000151 deposition Methods 0.000 abstract description 4
- 238000001771 vacuum deposition Methods 0.000 abstract description 2
- 238000002347 injection Methods 0.000 abstract 3
- 239000007924 injection Substances 0.000 abstract 3
- 238000005576 amination reaction Methods 0.000 abstract 1
- 230000021523 carboxylation Effects 0.000 abstract 1
- 238000006473 carboxylation reaction Methods 0.000 abstract 1
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000010408 film Substances 0.000 description 24
- 238000012360 testing method Methods 0.000 description 11
- 238000004020 luminiscence type Methods 0.000 description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 238000000280 densification Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical class [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
- H01L33/04—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction
- H01L33/06—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a quantum effect structure or superlattice, e.g. tunnel junction within the light emitting region, e.g. quantum confinement structure or tunnel barrier
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/005—Processes
- H01L33/0054—Processes for devices with an active region comprising only group IV elements
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
An electroluminescent device based on carbon quantum dots comprises a top electrode, a bottom electrode, an electron injection layer and a light-emitting layer, wherein the electron injection layer and the light-emitting layer are sequentially located between the top electrode and the bottom electrode; the electron injection layer is a lithium fluoride thin film; the top electrode is made from Al; the bottom electrode is made from ITO conductive glass; the light-emitting layer is carbon quantum dot thin films which are self-assembled layer by layer. According to a preparation method, carbon quantum dots are prepared according to the steps that citric acid and octadecene react in an oil phase at high temperature; the surfaces of the carbon quantum dots are modified in the mode that the surfaces of the carbon quantum dots are subjected to amination and carboxylation through dimethylformamide and acrylic acid; the layer-by-layer self-assembly method of the carbon quantum dot thin films includes the step that ITO conductive glass alternately deposits in two carbon quantum dot solutions for 15 min. The electroluminescent device has the advantages that the light-emitting layer of the device is obtained through the layer-by-layer self-assembly method, complex technologies of a vacuum evaporation method and a meteorological deposition method and high cost are avoided, the large-area thin film can be obtained easily, and the device has a good rectification characteristic and a stable electroluminescent phenomenon.
Description
Technical field
The present invention relates to the preparation of carbon quantum dot electroluminescent device, particularly a kind of electroluminescent device based on carbon quantum dot and preparation method thereof.
Background technology
In order to meet the growing demand of modern display technology, quantum dot LED is towards the research and development of more excellent character, and such as preparation technology simplifies, material is high to environmental hazard reduction, luminous intensity.At present, based on the quantum efficiency of the LED component of CdSe quantum dots close to OLED, but its environmental impact assessment is not high.Carbon quantum dot (CD) is also called fluorescent carbon quantum dot, carbon containing quantum dot, the carbon nano-particle of the spherical size of a kind at below 10nm, there is good water-soluble, chemical inertness, hypotoxicity, be easy to functionalization and the anti-light excellent properties such as Bleachability, be suitable for LED display.
The preparation of luminescent layer is technique crucial in device preparation, and quantum dot light emitting film can be obtained by vacuum vapour deposition, spin-coating method, vapour deposition process.But because raw material utilization rate is lower, the factor such as large scale preparation, experimental facilities costliness can not limit it in industrial large-scale application.
Summary of the invention
The object of the invention is for above-mentioned existing problems, a kind of electroluminescent device based on carbon quantum dot and preparation method thereof is provided, the attracting each other of the amino electrostatic with carboxyl after the method utilizes carbon quantum dot surface modification, indium tin oxide-coated glass (ITO) substrate realizes the LBL self-assembly of carbon quantum dot light-emitting film.Its preparation process is simple, film evenness is high, to obtain the rate of finished products of device high.
Technical scheme of the present invention:
A kind of electroluminescent device based on carbon quantum dot, comprise top electrode, hearth electrode and electron injecting layer, luminescent layer successively between top, hearth electrode, described electron injecting layer is lithium fluoride (LiF) film, and thickness is 1nm, described top electrode is Al, and thickness is 150nm; Hearth electrode is ITO electro-conductive glass, and thickness is 9mm, and described luminescent layer is the carbon quantum dot film of LBL self-assembly, and its thickness is 30-50nm.
A described preparation method based on the electroluminescent device of carbon quantum dot, step is as follows:
1) citric acid being added temperature is in the mixed solution of the octadecylamine of 230 DEG C and octadecylene, magnetic agitation 45min in ar gas environment, the mixed liquor obtained is added toluene, 1h is left standstill after being down to room temperature, obtain mixed liquor, the amount ratio of citric acid, octadecylamine, octadecylene and toluene is 1g:1.5g:15mL:15mL;
2) methyl alcohol being added by 1) in the mixed liquor prepared, the volume ratio of methyl alcohol and mixed liquor is 15mL:10mL, centrifugal 5min under 8000rpm, is separated lower sediment thing;
3) by above-mentioned precipitation without adding in methyl alcohol, centrifugal under 120000rpm after stirring, sediment separate out, this operation repeats 2 times, is precipitated thing;
4) by step 3) precipitate dissolves that obtains is that in the dimethyl formamide solution of 1mol/L, stirred at ambient temperature 40min, then adds sodium borohydride in concentration, heats 4h at 55 DEG C, obtains through amido modified carbon quantum dot solution (CD-NH
2), the amount ratio of sediment, dimethyl formamide solution and sodium borohydride is 50mg:50mL:0.0248g;
5) by step 3) precipitate dissolves that obtains is in the acrylic acid solution of 3mol/L in concentration, 40min is stirred at 65 DEG C, dropwise solution is added after separately sodium borohydride being dissolved in deionized water, 65 DEG C of heating 4h, obtain the carbon quantum dot solution (CD-COOH) through carboxyl modified, the amount ratio of sediment, acrylic acid solution, sodium borohydride and deionized water is 50mg:50mL:0.0248g:100mL;
6) substrate of ITO electro-conductive glass as LBL self-assembly film of 3cm × 1cm is adopted, 1cm × 1cm region, ITO electro-conductive glass center is retained, remainder concentration is the hydrochloric acid solution corrosion 10min of 10wt%, puts into drying box dry after then cleaning 5min with liquid detergent, deionized water, acetone, isopropyl alcohol and ethanolic solution respectively in supersonic cleaning machine successively;
7) ito glass after above-mentioned process is put into deionized water, ammoniacal liquor, the hydrogen peroxide mixed liquor heated sealed 1h of 160 DEG C, in this mixed liquor, the volume ratio of deionized water, ammoniacal liquor, hydrogen peroxide is 1:1:5;
8) by 7) ITO electro-conductive glass after process immerses step 4 successively) the carbon quantum dot solution (CD-NH that modifies of the amido functional group prepared
2) and step 5) 10-20min in the carbon quantum dot solution (CD-COOH) of carboxyl modified prepared, remove the surplus carbon quantum dot solution on ITO surface by washed with de-ionized water after infiltration, put into drying box 80 DEG C of dry 40min after this operation repeats 2-4 time successively, complete the preparation of luminescent layer carbon quantum dot film in device;
9) by 8) on the carbon quantum dot film prepared at 7.0x10
-4the electrode A l that electron injecting layer LiF and 150nm that under the pressure of Bar, evaporation 1nm is thick is successively thick, completes the preparation of luminescent layer carbon quantum dot film in device.
Advantage of the present invention and good effect are: being prepared as of luminescent layer of this device is obtained by LBL self-assembly method, avoid the complicated technology of vacuum evaporation and CVD method and the shortcoming of great number cost, carbon quantum dot film can be prepared by rapid large-area, prepared thin film surface planeness is high, and device prepared by this method has good rectification characteristic and stable electro optical phenomenon.
Accompanying drawing explanation
Fig. 1 is the flow chart of carbon quantum dot finishing.
Fig. 2 is the flow chart of carbon quantum dot film layer self assembly.
Fig. 3 is the schematic diagram of device architecture of the present invention.
Fig. 4 is atomic force microscope (AFM) figure of LBL self-assembly film, and this film evenness is high as seen from the figure, carbon quantum dot good dispersion.
Fig. 5 is the I-V performance diagram of device of the present invention.The I-V curve testing equipment model of device is KEITHLEY2400 semiconductor testing apparatus, and in test process, Al does negative electrode, and ITO does anode; Curve demonstrates good rectification characteristic.
Fig. 6 is the electroluminescent spectrum figure of device of the present invention.The electroluminescent spectrum testing equipment of device is the FL3 fluorescence spectrophotometer of JobinYvon.The luminescence of device is the wide range transmitting of 502nm.
Embodiment
Embodiment 1:
A kind of electroluminescent device based on carbon quantum dot, as shown in Figure 3 (accompanying drawing must be consistent with character express), comprise top electrode, hearth electrode and electron injecting layer, luminescent layer successively between top, hearth electrode, described electron injecting layer is lithium fluoride (LiF) film, thickness is 1nm, described top electrode is Al, and thickness is 150nm; Hearth electrode is ITO electro-conductive glass, and thickness is 9mm, and described luminescent layer is the carbon quantum dot film of LBL self-assembly, and its thickness is 30nm.
A described preparation method based on the electroluminescent device of carbon quantum dot, step is as follows:
1) citric acid being added temperature is in the mixed solution of the octadecylamine of 230 DEG C and octadecylene, magnetic agitation 45min in ar gas environment, the mixed liquor obtained is added toluene, 1h is left standstill after being down to room temperature, obtain mixed liquor, the amount ratio of citric acid, octadecylamine, octadecylene and toluene is 1g:1.5g:15mL:15mL;
2) methyl alcohol being added by 1) in the mixed liquor prepared, the volume ratio of methyl alcohol and mixed liquor is 15mL:10mL, centrifugal 5min under 8000rpm, is separated lower sediment thing;
3) by above-mentioned precipitation without adding in methyl alcohol, centrifugal under 120000rpm after stirring, sediment separate out, this operation repeats 2 times, is precipitated thing;
4) by step 3) precipitate dissolves that obtains is that in the dimethyl formamide solution of 1mol/L, stirred at ambient temperature 40min, then adds sodium borohydride in concentration, heats 4h at 55 DEG C, obtains through amido modified carbon quantum dot solution (CD-NH
2), the amount ratio of sediment, dimethyl formamide solution and sodium borohydride is 50mg:50mL:0.0248g;
5) by step 3) precipitate dissolves that obtains is in the acrylic acid solution of 3mol/L in concentration, 40min is stirred at 65 DEG C, dropwise solution is added after separately sodium borohydride being dissolved in deionized water, 65 DEG C of heating 4h, obtain the carbon quantum dot solution (CD-COOH) through carboxyl modified, the amount ratio of sediment, acrylic acid solution, sodium borohydride and deionized water is 50mg:50mL:0.0248g:100mL;
Fig. 1 is the flow chart of carbon quantum dot finishing, shows in figure: the carbon quantum dot after synthesis makes its surface respectively with amino or carboxyl through dimethyl formamide and acrylic acid process.
6) substrate of ITO electro-conductive glass as LBL self-assembly film of 3cm × 1cm is adopted, 1cm × 1cm region, ITO electro-conductive glass center is retained, remainder concentration is the hydrochloric acid solution corrosion 10min of 10wt%, puts into drying box dry after then cleaning 5min with liquid detergent, deionized water, acetone, isopropyl alcohol and ethanolic solution respectively in supersonic cleaning machine successively;
7) ito glass after above-mentioned process is put into deionized water, ammoniacal liquor, the hydrogen peroxide mixed liquor heated sealed 1h of 160 DEG C, in this mixed liquor, the volume ratio of deionized water, ammoniacal liquor, hydrogen peroxide is 1:1:5;
8) by 7) ITO electro-conductive glass after process immerses step 4 successively) the carbon quantum dot solution (CD-NH that modifies of the amido functional group prepared
2) and step 5) 10-20min in the carbon quantum dot solution (CD-COOH) of carboxyl modified prepared, remove the surplus carbon quantum dot solution on ITO surface by washed with de-ionized water after infiltration, drying box 80 DEG C of dry 40min are put in this operation after repeating 2 times, complete the preparation of luminescent layer carbon quantum dot film in device, wherein luminescent layer frequency of depositing is that 2-4 corresponding thickness is respectively 30nm, 40nm, 50nm.
Fig. 2 is the flow chart of carbon quantum dot film layer self assembly, and the ITO of clean surface is by after the mixture process of ammoniacal liquor, hydrogen peroxide and deionized water, and surface is with elecrtonegativity.To be immersed in the carbon quantum dot solution of modified amino with electronegative ITO electro-conductive glass, the effect lower surface in Coulomb force is adsorbed onto ITO conductive glass surface with the carbon quantum dot of Zeta positive potential, forms the film of one deck densification.ITO surface deposition being crossed amino-carbon quantum dot is immersed in carboxyl modified rear surface with in the carbon quantum dot solution of Zeta negative potential, and carbon quantum dot forms the film of one deck densification again on the surface of film.Repeat above step 2 time, ITO has been infiltrated successively in amino with the carbon quantum dot solution of carboxyl the LBL self-assembly of carbon quantum dot film.
Fig. 4 is atomic force microscope (AFM) figure of LBL self-assembly film, and this film evenness is high as seen from the figure, carbon quantum dot good dispersion.
The performance comparison experiment of device prepared by the present embodiment:
By the luminescent layer of above-mentioned preparation be three devices of 30nm, 40nm, 50nm and label is 1,2, No. 3,3 samples are carried out respectively IV test and luminous test, No. 1,2,3, device all demonstrates good rectification characteristic, cut-in voltage is 4V, wherein, the electric current of No. 1 sample is maximum, rule of thumb known, its carrier mobility of light emitting layer thickness variable effect, the electric current of this device reduces with the increase of light emitting layer thickness; In luminescence test, the luminescence of No. 2 samples is the strongest.Therefore, its luminescent layer optimum thickness is 40nm.
Fig. 5 is the I-V performance diagram of device of the present invention.The I-V curve testing equipment model of device is KEITHLEY2400 semiconductor testing apparatus, and in test process, Al does negative electrode, and ITO does anode; Curve demonstrates good rectification characteristic.
Fig. 6 is the electroluminescent spectrum figure of device of the present invention.The electroluminescent spectrum testing equipment of device is the FL3 fluorescence spectrophotometer of JobinYvon.The luminescence of device is the wide range transmitting of 502nm.
Claims (2)
1. the electroluminescent device based on carbon quantum dot, it is characterized in that: comprise top electrode, hearth electrode and electron injecting layer, luminescent layer successively between top, hearth electrode, described electron injecting layer is lithium fluoride (LiF) film, and thickness is 1nm; Described top electrode is Al, and thickness is 150nm; Hearth electrode is ITO electro-conductive glass, and thickness is 9mm, and described luminescent layer is the carbon quantum dot film of LBL self-assembly, and its thickness is 30-50nm.
2. one as claimed in claim 1 based on the preparation method of the electroluminescent device of carbon quantum dot, it is characterized in that step is as follows:
1) citric acid being added temperature is in the mixed solution of the octadecylamine of 230 DEG C and octadecylene, magnetic agitation 45min in ar gas environment, the mixed liquor obtained is added toluene, 1h is left standstill after being down to room temperature, obtain mixed liquor, the amount ratio of citric acid, octadecylamine, octadecylene and toluene is 1g:1.5g:15mL:15mL;
2) methyl alcohol being added by 1) in the mixed liquor prepared, the volume ratio of methyl alcohol and mixed liquor is 15mL:10mL, centrifugal 5min under 8000rpm, is separated lower sediment thing;
3) by above-mentioned precipitation without adding in methyl alcohol, centrifugal under 120000rpm after stirring, sediment separate out, this operation repeats 2 times, is precipitated thing;
4) by step 3) precipitate dissolves that obtains is that in the dimethyl formamide solution of 1mol/L, stirred at ambient temperature 40min, then adds sodium borohydride in concentration, heats 4h at 55 DEG C, obtains through amido modified carbon quantum dot solution (CD-NH
2), the amount ratio of sediment, dimethyl formamide solution and sodium borohydride is 50mg:50mL:0.0248g;
5) by step 3) precipitate dissolves that obtains is in the acrylic acid solution of 3mol/L in concentration, 40min is stirred at 65 DEG C, dropwise solution is added after separately sodium borohydride being dissolved in deionized water, 65 DEG C of heating 4h, obtain the carbon quantum dot solution (CD-COOH) through carboxyl modified, the amount ratio of sediment, acrylic acid solution, sodium borohydride and deionized water is 50mg:50mL:0.0248g:100mL;
6) substrate of ITO electro-conductive glass as LBL self-assembly film of 3cm × 1cm is adopted, 1cm × 1cm region, ITO electro-conductive glass center is retained, remainder concentration is the hydrochloric acid solution corrosion 10min of 10wt%, puts into drying box dry after then cleaning 5min with liquid detergent, deionized water, acetone, isopropyl alcohol and ethanolic solution respectively in supersonic cleaning machine successively;
7) ito glass after above-mentioned process is put into deionized water, ammoniacal liquor, the hydrogen peroxide mixed liquor heated sealed 1h of 160 DEG C, in this mixed liquor, the volume ratio of deionized water, ammoniacal liquor, hydrogen peroxide is 1:1:5;
8) by 7) ITO electro-conductive glass after process immerses step 4 successively) the carbon quantum dot solution (CD-NH that modifies of the amido functional group prepared
2) and step 5) 10-20min in the carbon quantum dot solution (CD-COOH) of carboxyl modified prepared, remove the surplus carbon quantum dot solution on ITO surface by washed with de-ionized water after infiltration, put into drying box 80 DEG C of dry 40min after this operation repeats 2-4 time successively, complete the preparation of luminescent layer carbon quantum dot film in device;
9) by 8) on the carbon quantum dot film prepared at 7.0x10
-4the electrode A l that electron injecting layer LiF and 150nm that under the pressure of Bar, evaporation 1nm is thick is successively thick, completes the preparation of luminescent layer carbon quantum dot film in device.
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Cited By (8)
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CN106566538A (en) * | 2016-10-08 | 2017-04-19 | 北京师范大学 | High-quantum-yield eigenstate-fluorescence-adjustable carbon dot and preparing method and application thereof |
CN107418568A (en) * | 2017-06-16 | 2017-12-01 | 南京工业大学 | The full carbon of a kind of zero dimension and two-dimentional hydridization turns white the preparation method of emitting phosphor |
CN107681042A (en) * | 2017-09-29 | 2018-02-09 | 广州正农照明科技有限公司 | A kind of quantum dot LED light source for plant growth |
CN108641705A (en) * | 2018-04-21 | 2018-10-12 | 太原理工大学 | Electroluminescent device emitting layer material based on carbon dots |
CN109294570A (en) * | 2018-10-23 | 2019-02-01 | 河南大学 | A kind of preparation method of oil phase carbon dots |
CN109671874A (en) * | 2019-01-03 | 2019-04-23 | 京东方科技集团股份有限公司 | A kind of quantum dot display panel and preparation method thereof, display device |
CN106566538B (en) * | 2016-10-08 | 2019-07-16 | 北京师范大学 | The adjustable carbon dots of eigenstate fluorescence and its preparation method of high quantum production rate and application |
CN112209635A (en) * | 2020-10-29 | 2021-01-12 | 华中科技大学 | Solid fluorescent carbon dot based on nano porous glass and preparation method thereof |
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CN103915553A (en) * | 2014-04-21 | 2014-07-09 | 吉林大学 | Current carrier injection type blue light and white light LED based on carbon dots and manufacturing method |
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CN108641705A (en) * | 2018-04-21 | 2018-10-12 | 太原理工大学 | Electroluminescent device emitting layer material based on carbon dots |
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WO2020140761A1 (en) * | 2019-01-03 | 2020-07-09 | 京东方科技集团股份有限公司 | Quantum dot display panel and method for fabrication thereof, and display device |
US11611015B2 (en) | 2019-01-03 | 2023-03-21 | Boe Technology Group Co., Ltd. | Quantum dot display panel, manufacturing method thereof, and display device |
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