CN109244201A - Metal-doped nanocrystalline and preparation method thereof, QLED device - Google Patents
Metal-doped nanocrystalline and preparation method thereof, QLED device Download PDFInfo
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- CN109244201A CN109244201A CN201710560567.8A CN201710560567A CN109244201A CN 109244201 A CN109244201 A CN 109244201A CN 201710560567 A CN201710560567 A CN 201710560567A CN 109244201 A CN109244201 A CN 109244201A
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- metal
- nanocrystalline
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- doping metals
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- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 229910052751 metal Inorganic materials 0.000 claims abstract description 71
- 239000002184 metal Substances 0.000 claims abstract description 69
- 239000007788 liquid Substances 0.000 claims abstract description 61
- 239000012682 cationic precursor Substances 0.000 claims abstract description 46
- 239000002243 precursor Substances 0.000 claims abstract description 38
- 150000001450 anions Chemical class 0.000 claims abstract description 27
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 22
- 150000002367 halogens Chemical class 0.000 claims abstract description 22
- 230000001603 reducing effect Effects 0.000 claims abstract description 18
- 229910017053 inorganic salt Inorganic materials 0.000 claims abstract description 17
- 238000009938 salting Methods 0.000 claims abstract description 17
- -1 metals Acetate Chemical class 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 229920002521 macromolecule Polymers 0.000 claims abstract description 9
- 150000002739 metals Chemical class 0.000 claims description 36
- 150000001768 cations Chemical class 0.000 claims description 31
- 150000003839 salts Chemical class 0.000 claims description 26
- 239000013078 crystal Substances 0.000 claims description 12
- 230000012010 growth Effects 0.000 claims description 12
- 239000012266 salt solution Substances 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 9
- 239000002096 quantum dot Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical group [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 6
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 5
- 229960001763 zinc sulfate Drugs 0.000 claims description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 4
- 229910000337 indium(III) sulfate Inorganic materials 0.000 claims description 4
- 150000004040 pyrrolidinones Chemical class 0.000 claims description 4
- QBTYOZHMFJONLX-UHFFFAOYSA-N [In].S(O)(O)=O Chemical compound [In].S(O)(O)=O QBTYOZHMFJONLX-UHFFFAOYSA-N 0.000 claims description 3
- CHUYYOSIZBKMJD-UHFFFAOYSA-N acetic acid;gold Chemical compound [Au].CC(O)=O CHUYYOSIZBKMJD-UHFFFAOYSA-N 0.000 claims description 3
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 3
- 229940009827 aluminum acetate Drugs 0.000 claims description 3
- QCUOBSQYDGUHHT-UHFFFAOYSA-L cadmium sulfate Chemical compound [Cd+2].[O-]S([O-])(=O)=O QCUOBSQYDGUHHT-UHFFFAOYSA-L 0.000 claims description 3
- JGIATAMCQXIDNZ-UHFFFAOYSA-N calcium sulfide Chemical compound [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 claims description 3
- QDVBBRPDXBHZFM-UHFFFAOYSA-N calcium;selenium(2-) Chemical compound [Ca+2].[Se-2] QDVBBRPDXBHZFM-UHFFFAOYSA-N 0.000 claims description 3
- VZZSRKCQPCSMRS-UHFFFAOYSA-N dipotassium;selenium(2-) Chemical compound [K+].[K+].[Se-2] VZZSRKCQPCSMRS-UHFFFAOYSA-N 0.000 claims description 3
- XGCKLPDYTQRDTR-UHFFFAOYSA-H indium(iii) sulfate Chemical compound [In+3].[In+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O XGCKLPDYTQRDTR-UHFFFAOYSA-H 0.000 claims description 3
- 229920001083 polybutene Polymers 0.000 claims description 3
- 230000027756 respiratory electron transport chain Effects 0.000 claims description 3
- VPQBLCVGUWPDHV-UHFFFAOYSA-N sodium selenide Chemical compound [Na+].[Na+].[Se-2] VPQBLCVGUWPDHV-UHFFFAOYSA-N 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 229910000331 cadmium sulfate Inorganic materials 0.000 claims description 2
- BYJADUSHMADYRW-UHFFFAOYSA-L cadmium(2+);sulfite Chemical compound [Cd+2].[O-]S([O-])=O BYJADUSHMADYRW-UHFFFAOYSA-L 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- PIJPYDMVFNTHIP-UHFFFAOYSA-L lead sulfate Chemical compound [PbH4+2].[O-]S([O-])(=O)=O PIJPYDMVFNTHIP-UHFFFAOYSA-L 0.000 claims description 2
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 2
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 2
- 229940071536 silver acetate Drugs 0.000 claims description 2
- WYCFMBAHFPUBDS-UHFFFAOYSA-L silver sulfite Chemical compound [Ag+].[Ag+].[O-]S([O-])=O WYCFMBAHFPUBDS-UHFFFAOYSA-L 0.000 claims description 2
- 239000011775 sodium fluoride Substances 0.000 claims description 2
- 235000013024 sodium fluoride Nutrition 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims 1
- 238000002161 passivation Methods 0.000 abstract description 4
- 238000004140 cleaning Methods 0.000 abstract description 3
- 230000001376 precipitating effect Effects 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 18
- 239000000126 substance Substances 0.000 description 13
- 229910021645 metal ion Inorganic materials 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 239000010949 copper Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 239000012298 atmosphere Substances 0.000 description 6
- 238000002156 mixing Methods 0.000 description 5
- UMRSVAKGZBVPKD-UHFFFAOYSA-N acetic acid;copper Chemical compound [Cu].CC(O)=O UMRSVAKGZBVPKD-UHFFFAOYSA-N 0.000 description 4
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- 239000002159 nanocrystal Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000004528 spin coating Methods 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 125000002091 cationic group Chemical group 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- GEQBRULPNIVQPP-UHFFFAOYSA-N 2-[3,5-bis(1-phenylbenzimidazol-2-yl)phenyl]-1-phenylbenzimidazole Chemical compound C1=CC=CC=C1N1C2=CC=CC=C2N=C1C1=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=CC(C=2N(C3=CC=CC=C3N=2)C=2C=CC=CC=2)=C1 GEQBRULPNIVQPP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 230000003698 anagen phase Effects 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 244000144992 flock Species 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000002707 nanocrystalline material Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
- 241001274216 Naso Species 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 229910001508 alkali metal halide Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910052924 anglesite Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 1
- 229910000369 cadmium(II) sulfate Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011258 core-shell material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003682 fluorination reaction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- ICIWUVCWSCSTAQ-UHFFFAOYSA-M iodate Chemical compound [O-]I(=O)=O ICIWUVCWSCSTAQ-UHFFFAOYSA-M 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- XCAUINMIESBTBL-UHFFFAOYSA-N lead(ii) sulfide Chemical compound [Pb]=S XCAUINMIESBTBL-UHFFFAOYSA-N 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000011686 zinc sulphate Substances 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
-
- 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
- H01L33/0083—Processes for devices with an active region comprising only II-VI compounds
-
- 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
- H01L33/16—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 particular crystal structure or orientation, e.g. polycrystalline, amorphous or porous
- H01L33/18—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 particular crystal structure or orientation, e.g. polycrystalline, amorphous or porous within the light emitting region
-
- 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
- H01L33/26—Materials of the light emitting region
- H01L33/28—Materials of the light emitting region containing only elements of Group II and Group VI of the Periodic Table
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Computer Hardware Design (AREA)
- Manufacturing & Machinery (AREA)
- Nanotechnology (AREA)
- Chemical & Material Sciences (AREA)
- Optics & Photonics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Biophysics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Luminescent Compositions (AREA)
- Electroluminescent Light Sources (AREA)
Abstract
The present invention discloses metal-doped nanocrystalline and preparation method thereof, QLED device.Include: to mix cationic precursor salting liquid with doping metals Acetate Solution, continues addition reducing inorganic salt then to inorganic halogen is added in mixed liquor and then add non-ionic macromolecule compound into mixed liquor again, body liquid before obtaining；Before anion precursor salting liquid is added in body liquid, then by centrifuge separation, cleaning precipitating, obtain metal-doped nanocrystalline.For the present invention by the above method, the metal that halogen passivation can be prepared mixes nanocrystalline, the to be prepared nanocrystalline fluorescence intensity and photoelectric properties having had.
Description
Technical field
The present invention relates to nanocrystalline material preparation technical fields and light emitting diode with quantum dots technical field more particularly to one
A kind of kind metal-doped nanocrystalline and preparation method thereof, QLED device.
Background technique
In recent years, nano crystal semiconductor luminescent material was known as " nano-phosphor ", and it is great to cause researcher
Interest, this is because they have novel and uncommon structure and corresponding electrical and optical properties.The nanocrystalline master of sulfur family
There are ZnS, CdS, CdSe/ZnS etc..It is distinguished from structure, they have single structure, core-shell structure and alloy structure etc..
These are nanocrystalline, which to present interesting phenomenon, is: size can change the radiation wavelength of visible light and the length of radiation lifetime etc.
Performance；Electroluminescent diode apparatus can be prepared using these materials and there is lower bright voltage.
Improve nanocrystalline radiation lifetime and fluorescence efficiency by way of doping metals by in-depth study.It is existing
The method of technology, due in nanocrystalline growth course due to the doping of element can make lattice occur dislocation and be difficult to realize adulterate
The co-precipitation of metal will lead to generation nonradiative transition, and the half-peak breadth that may lead glow peak broadens, to influence color
It is pure.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of metal-doped nanocrystalline and its systems
Preparation Method, QLED device.
Technical scheme is as follows:
A kind of preparation method of metal doping nano crystalline substance, wherein include:
A kind of cationic precursor liquid containing doping metals is provided, the cationic precursor liquid containing doping metals includes by cation
Precursor salt solution, metal acetate salting liquid, reducing inorganic salt, inorganic halogen are mixed with to obtain；
A kind of anion precursor salt solution is provided；
The anion precursor salt solution is added in the cationic precursor liquid containing doping metals and carries out crystal growth,
It is prepared described metal-doped nanocrystalline.
The preparation method of the metal doping nano crystalline substance, wherein in the cationic precursor liquid containing doping metals also
Including non-ionic macromolecule compound, the non-ionic macromolecule compound includes polyvinylpyrrolidone, polypropylene pyrrole
One of pyrrolidone, polybutene pyrrolidones are a variety of.
The preparation method of the metal doping nano crystalline substance, wherein the cation precursor salt is zinc sulfate, sulfuric acid
One of cadmium, lead sulfate, indium sulfate are a variety of.
The preparation method of the metal doping nano crystalline substance, wherein the doping metals acetate is acetic acid gold, acetic acid
One of silver, copper acetate, ferric acetate, aluminum acetate are a variety of.
The preparation method of the metal doping nano crystalline substance, wherein the reducing inorganic salt is sodium sulfite, sulfurous acid
One of cadmium, lead sulfite, sulfurous acid indium, silver sulfite are a variety of.
The preparation method of the metal doping nano crystalline substance, wherein the inorganic halogen is sodium chloride, sodium bromide, iodate
One of sodium, sodium fluoride are a variety of.
The preparation method of the metal doping nano crystalline substance, wherein the anion precursor salt is vulcanized sodium, vulcanization
One of potassium, calcium sulfide, sodium selenide, potassium selenide, calcium selenide are a variety of.
The preparation method of the metal doping nano crystalline substance, wherein in the cationic precursor liquid containing doping metals, sun
The concentration of ion is 0.005-0.05mmol/ml.
The preparation method of the metal doping nano crystalline substance, wherein rub by the cation with doping metals acetate
You are than being prepared the cationic precursor liquid containing doping metals for 5-20.
The preparation method of the metal doping nano crystalline substance, wherein by the reducing inorganic salt and cationic presoma
The molar ratio of cation element is that the cationic precursor liquid containing doping metals is prepared in 0.1-0.5 in salt.
The preparation method of the metal doping nano crystalline substance, wherein by the inorganic halogen and cationic precursor salt
The molar ratio of cation element is that the cationic precursor liquid containing doping metals is prepared in 0.02-0.2.
The metal-doped nanocrystalline preparation method, wherein the anion precursor salting liquid it is mole dense
Degree range is 0.05-1mmol/ml, by cation member in anion element in anion precursor salt and cationic precursor salt
The molar ratio of element is that 10-20 carries out the anion precursor salting liquid addition cationic precursor liquid containing doping metals
Crystal growth.
The metal-doped nanocrystalline preparation method, wherein by the non-ionic macromolecule compound and sun
The molar ratio of cation element is that the cationic forerunner containing doping metals is prepared in 0.05-0.1 in ion precursor salt
Liquid.
It is a kind of metal-doped nanocrystalline, wherein using as above any metal-doped nanocrystalline preparation side
Method is prepared.
A kind of QLED device, including cathode, anode, electron transfer layer, hole transmission layer and quantum dot light emitting layer, wherein
The material of the quantum dot light emitting layer include method as described above be prepared it is metal-doped nanocrystalline.
The utility model has the advantages that the present invention is in crystal growing process, it can be to avoid doping metals by oxygen using reducing inorganic salt
Change, so that doping metals be enable to be co-precipitated with nanocrystalline material, obtains preferably doping effect, avoid doping metals that from receiving
Meter Jing's makes lattice misplace, and obtaining nanocrystalline band gap is improved, the good quantum dot of fluorescent effect.In nanocrystalline growth
Stage adds inorganic halogen to adjust concentration of the different valence state metal ion in mixed liquor, can obtain both having metal ion
Doping with the nanocrystalline of halogen passivation, substantially improves the band gap and photoelectric properties of luminescent material again.The method of the present invention behaviour
Make simply, the requirement of apparatus and process condition is low, is easy to repeat, and has good prospects for commercial application.
Specific embodiment
The present invention provides a kind of metal doping nano crystalline substance and preparation method thereof, QLED device, to make the purpose of the present invention, skill
Art scheme and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that tool described herein
Body embodiment is only used to explain the present invention, is not intended to limit the present invention.
The metal-doped nanocrystalline preparation method preferred embodiment of one kind of the invention, wherein include:
A kind of cationic precursor liquid containing doping metals is provided, the cationic precursor liquid containing doping metals includes by cation
Precursor salt solution, metal acetate salting liquid, reducing inorganic salt, the preparation of inorganic halogen are mixed to get；
A kind of anion precursor salt solution is provided；
The anion precursor salt solution is added in the cationic precursor liquid containing doping metals and carries out crystal growth,
It is prepared described metal-doped nanocrystalline.
The cationic precursor liquid containing doping metals is that doping metals acetic acid is added by mixing precursor salting liquid
Salting liquid, reducing inorganic salt, inorganic halogen.The doping metals Acetate Solution, reducing inorganic salt, inorganic is added in mixing
The atmosphere of halogen is air atmosphere, vacuum atmosphere or inert atmosphere.
For example, the cationic precursor liquid containing doping metals is by such as lower section in a kind of specific embodiment
What method was prepared: at room temperature, cationic precursor salting liquid being mixed with doping metals Acetate Solution, and lazy
5-15min is mixed under property atmosphere；Reducing inorganic salt and inorganic halogen are continuously added, and stirs 5-15min under an inert atmosphere,
The cationic precursor liquid containing doping metals is prepared.
Further, non-ionic macromolecule compound is added into mixed liquor, and 1-3h is stirred at room temperature, and obtains preceding body
Liquid.
It is understood that the cation precursor salt solution, metal acetate salting liquid, anion precursor salt solution
The solvent of middle selection is can provide the solvent of reaction environment for crystal growth.
In order to increase the viscosity of mixed liquor in crystal growing process, reaction rate is reduced, keeps the nanocrystalline size generated equal
One property is good, non-ionic macromolecule compound can further be added, the cationic precursor liquid containing doping metals is prepared.Institute
Stating non-ionic macromolecule compound can be polyvinylpyrrolidone (PVP), polyvinyl pyrilodone, polybutene pyrrolidones
One of or it is a variety of.
Preferably, it rubs by the non-ionic macromolecule compound and cation element in the cationic precursor salt
You are than being prepared the cationic precursor liquid containing doping metals for 0.05-0.1, this is because ratio is excessively high, viscosity is excessive,
Cause reaction rate too low；Conversely, the purpose of control reaction rate is then equally not achieved.
Cation precursor salt of the present invention can provide stable cation for the nanocrystalline of subsequent preparation doping, and
Cation is not easy to be reduced.Preferably, the cationic precursor salt can be zinc sulfate (ZnSO4), cadmium sulfate (CdSO4), sulphur
Lead plumbate (PbSO4), indium sulfate (In2(SO4)3) one of or it is a variety of.
Preferably, the cation member in the cationic precursor liquid containing doping metals, in the cation precursor salt
The concentration of element is 0.005-0.05mmol/ml, this is because concentration is excessive, corresponding cation is excessive, and reaction rate is too fast；Such as
Fruit concentration is too small, and reaction rate is lower.
It preferably, is 5-20 by the molar ratio of cation element and doping metals acetate in the cationic precursor salt
The cationic precursor liquid containing doping metals is prepared, this is because the ratio between mole dosage is excessively high, the metallic element of doping
Dosage is less, doping it is ineffective；Otherwise the ratio between mole dosage is too low, and the metallic element dosage of doping is excessively high, influences to adulterate
Effect can be easy to cause alloying.Preferably, the doping metals acetate can be acetic acid gold, silver acetate, copper acetate, vinegar
One of sour iron, aluminum acetate etc. are a variety of.Because acetate preferably can dissolve to form metal ion solution and have
Doping effect.
Preferably, the reducing inorganic salt can be sodium sulfite, cadmium sulfite, lead sulfite, sulfurous acid indium, sulfurous
One of sour silver etc. are a variety of.Since the low price doped metal ion in doping metals acetate has stronger reproducibility,
It is easily oxidized, to influence to adulterate effect.The present invention can be avoided the low price doping gold using the reducing inorganic salt
Belong to ion to be oxidized, in crystal growing process, miscellaneous metal ion is co-precipitated with nanocrystalline, improves doping effect.
Molar ratio by the cation element in the reducing inorganic salt and the cationic precursor salt is 0.1-0.5
The cationic precursor liquid containing doping metals is prepared.If the reducing inorganic salt dosage is excessively high, it be easy to cause mixed
The pH value meta-alkalescence having in liquid is closed, the growth of subsequent Doped nanocrystal is unfavorable for；If the reducing inorganic salt dosage mistake
It is low, it easily causes low valence metal ion to be oxidized to high volence metal ion, influences to adulterate effect.
Preferably, the inorganic halogen is alkali metal halide salt, such as can be sodium chloride, sodium bromide, sodium iodide, fluorination
One of sodium etc. is a variety of.The inorganic halogen can ionize out halide ion and the metal in situ of nanocrystal surface is (described
Cationic metal element) it combines, nanocrystalline realization is passivated, so as to improve nanocrystalline luminous efficiency.
Preferably, it is prepared by the molar ratio of inorganic halogen and cation element in cationic precursor salt for 0.02-0.2
To the cationic precursor liquid containing doping metals.This is because mole dosage ratio is too low or excessively high, passivation effect can be all influenced
Fruit.
Preferably, the anion precursor salt can ionize the anion provided compared with strong reducing property, anti-for participating in
It answers.Such as: the anion precursor salt can be in vulcanized sodium, potassium sulfide, calcium sulfide, sodium selenide, potassium selenide, calcium selenide etc.
It is one or more.
The molar concentration range of the anion precursor salting liquid is 0.05-1mmol/ml, this is because concentration is too low,
Reaction rate is excessively slow；Otherwise excessive concentration, then reaction rate is too fast.By anion element in anion precursor salt and cation
The molar ratio of cation element is 10-20 anion precursor salting liquid addition is described containing doping metals in precursor salt
Cationic precursor liquid carry out crystal growth.Further, the anion precursor salting liquid can be using being gradually added
Mode is added in the cationic precursor liquid containing doping metals or described containing mixing using being added to of being once all added
Crystal growth is carried out in the cationic precursor liquid of miscellaneous metal.Preferably, crystal growth is carried out by the way of being gradually added.
The present invention adds inorganic halogen in nanocrystalline preparation process, in nanocrystalline growth phase to adjust different price
Concentration of the state metal ion in mixed liquor, and then can be effectively obtained not only with metal ion mixing, but also have halogen blunt
That changes is nanocrystalline, substantially improves the band gap and photoelectric properties of luminescent material.Corresponding mechanism of action is mainly: by halogen
The chemical bond that the dipole effect in the metal cation vacancy of ion and nanocrystal surface is formed, it is blunt come the surface of completing nanocrystalline
Change, and then improves nanocrystalline fluorescence intensity and corresponding photoelectric properties.The method of the present invention is easy to operate, is easy to repeat, solution
Determined it is existing nanocrystalline band gap is changed by doping after, the problem of causing the half-peak breadth of glow peak to broaden, influence colour purity.
A kind of QLED device of the invention, the QLED device include cathode, anode, hole transmission layer, electron transfer layer
And quantum dot light emitting layer, wherein the material of the quantum dot light emitting layer of the QLED is as described above metal-doped nanocrystalline.
Below by several embodiments, the present invention is described in detail.
Embodiment 1
1, the preparation method of the Cu doping ZnS nanocrystalline of the present embodiment, includes the following steps:
1), the preparation of precursor liquid:
The acetic acid copper solution of the zinc sulfate solution and 0.01mmol that take 10ml to contain 0.1mmol mixes, and under nitrogen atmosphere
10min is stirred, the NaSO for adding 0.08mmol is continued3, for passing through SO2Gas generation reduce Cu+To Cu2+Conversion；To
The sodium chloride (NaCl) of 0.02mmol is added in mixed liquor and stirs 10min；The polyethylene of 0.01mmol is added into mixed liquor
Pyrrolidones (PVP), and it is vigorously stirred 5min, obtain precursor liquid.
2), Cu adulterates the synthesis of ZnS nanocrystalline:
Take the Na of the 0.1mmol of 10ml2S solution, using being added drop-wise in above-mentioned precursor liquid, until occurring white flock in mixed liquor
Stop that Na is added dropwise after precipitating2S solution.Then by centrifuge separation, cleaning precipitating, corresponding Cu doping ZnS nanocrystalline is obtained.
2, the preparation method of the QLED device of the present embodiment, includes the following steps:
After PEDPOT:PSS(AI4083) solution is filtered using 0.45 micron of filter, when using revolving speed as 4000rpm
Between for 60s in the ito glass on piece spin coating cleaned up, then use 150 DEG C of annealing 15min, using same revolving speed and when
Between spin coating hole transmission layer and electronic barrier layer (containing PVK chlorobenzene solution, concentration 6mg/ml), then the Cu prepared is mixed
Miscellaneous ZnS nanoparticles solution uses the condition spin-on deposition that revolving speed is 60s for the 2000rpm time in glove box, finally in height
Vacuum 2 × 104The aluminium of TPBI and the 150nm thickness of 40 nm thickness is deposited under Pa pressure by way of a mask plate is steamed using heat
Electrode, the QLED device area of preparation are 4cm2。
Embodiment 2
1, the preparation method of the Cu doping ZnS nanocrystalline of the present embodiment, includes the following steps:
1), containing the preparation of precursor liquid:
The acetic acid copper solution of the zinc sulfate solution and 0.01mmol that take 10ml to contain 0.1mmol mixes, and under nitrogen atmosphere
10min is stirred, the CdSO for adding 0.08mmol is continued3, for passing through SO2Gas generation reduce Cu+To Cu2+Conversion；To
The sodium fluoride (NaF) of 0.02mmol is added in mixed liquor and stirs 10min；The polyethylene pyrrole of 0.01mmol is added into mixed liquor
Pyrrolidone (PVP), and it is vigorously stirred 5min, obtain precursor liquid.
2) synthesis of Copper-cladding Aluminum Bar ZnS nanocrystalline:
Take the Na of the 0.1mmol of 10ml2S solution is slowly added drop-wise in above-mentioned precursor liquid, until mixed liquor using certain rate
In occur stopping after white flock precipitate that Na is added dropwise2S solution.Then it by centrifuge separation, cleaning precipitating, obtains corresponding Cu and mixes
Miscellaneous ZnS nanocrystalline.
2, the preparation method of the QLED device of the present embodiment, includes the following steps:
After PEDPOT:PSS(AI4083) solution is filtered using 0.45 micron of filter, when using revolving speed as 4000rpm
Between for 60s in the ito glass on piece spin coating cleaned up, then use 150 DEG C of annealing 15min, using same revolving speed and when
Between spin coating hole transmission layer and electronic barrier layer (containing PVK chlorobenzene solution, concentration 6mg/ml), then the Cu prepared is mixed
Miscellaneous ZnS nanocrystalline solution uses revolving speed for the condition spin-on deposition that the 2000rpm time is 60 s in glove box, finally in Gao Zhen
Sky 2 × 104 The aluminium electricity of TPBI and the 150nm thickness of 40nm thickness is deposited under Pa pressure by way of a mask plate is steamed using heat
Pole, the QLED device area of preparation are 4cm2。
In conclusion nanocrystalline and preparation method thereof, QLED device that one kind provided by the invention is metal-doped.The present invention
In nanocrystalline preparation process, inorganic halogen is added in different growth phases and is being mixed to adjust different valence state metal ion
Concentration in liquid, and then can be effectively obtained not only with metal ion mixing, but also with the nanocrystalline of halogen passivation.The present invention
Method is easy to operate, is easy to repeat.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of metal-doped nanocrystalline preparation method characterized by comprising
A kind of cationic precursor liquid containing doping metals is provided, the cationic precursor liquid containing doping metals includes by cation
Precursor salt solution, metal acetate salting liquid, reducing inorganic salt, inorganic halogen are mixed with to obtain；
A kind of anion precursor salt solution is provided；
The anion precursor salt solution is added in the cationic precursor liquid containing doping metals and carries out crystal growth,
It is prepared described metal-doped nanocrystalline.
2. metal-doped nanocrystalline preparation method according to claim 1, which is characterized in that described to contain doping metals
Cationic precursor liquid in further include non-ionic macromolecule compound.
3. metal-doped nanocrystalline preparation method according to claim 2, which is characterized in that the non-ionic height
Molecular compound is one of polyvinylpyrrolidone, polyvinyl pyrilodone, polybutene pyrrolidones or a variety of.
4. according to claim 1 to nanocrystalline preparation method metal-doped described in 3 any one, which is characterized in that institute
Stating cationic precursor salt is one of zinc sulfate, cadmium sulfate, lead sulfate, indium sulfate or a variety of；
And/or the doping metals acetate is one of acetic acid gold, silver acetate, copper acetate, ferric acetate, aluminum acetate or more
Kind；
And/or the reducing inorganic salt is sodium sulfite, cadmium sulfite, lead sulfite, sulfurous acid indium, one in silver sulfite
Kind is a variety of；
And/or the inorganic halogen is one of sodium chloride, sodium bromide, sodium iodide, sodium fluoride or a variety of；
And/or the anion precursor salt is vulcanized sodium, potassium sulfide, calcium sulfide, sodium selenide, potassium selenide, one in calcium selenide
Kind is a variety of.
5. metal-doped nanocrystalline preparation method according to claim 1, which is characterized in that body before the cation
The concentration of cation element is 0.005-0.05mmol/ml in body salting liquid.
6. according to claim 1 to nanocrystalline preparation method metal-doped described in 3 any one, which is characterized in that press
The molar ratio of cation element and doping metals acetate is to contain to mix described in 5-20 is prepared in the cation precursor salt
The cationic precursor liquid of miscellaneous metal；
It and/or by the molar ratio of cation element in the reducing inorganic salt and cationic precursor salt is prepared by 0.1-0.5
Obtain the cationic precursor liquid containing doping metals；
And/or it is prepared by the molar ratio of the inorganic halogen and cation element in cationic precursor salt for 0.02-0.2
The cationic precursor liquid containing doping metals.
7. metal-doped nanocrystalline preparation method according to claim 1, which is characterized in that body before the anion
The concentration of anion element in body salting liquid is 0.05-1mmol/ml, by the anion member in the anion precursor salt
The molar ratio of element and cation element in cationic precursor salt is 10-20, and the anion precursor salting liquid is added
Enter in the cationic precursor liquid containing doping metals and carries out crystal growth.
8. metal-doped nanocrystalline preparation method according to claim 1, which is characterized in that the non-ionic height
The molar ratio of cation element is 0.05-0.1 in molecular compound and cationic precursor salt.
9. a kind of metal-doped nanocrystalline, which is characterized in that is received using a method as claimed in any one of claims 1-8 metal-doped
The preparation method of meter Jing is prepared.
10. a kind of QLED device, which is characterized in that sent out including cathode, anode, electron transfer layer, hole transmission layer and quantum dot
Photosphere, the material of the quantum dot light emitting layer of the QLED include as claimed in claim 9 metal-doped nanocrystalline.
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