CN109652059A - Quantum dot film and preparation method of alumina-coated quantum dot - Google Patents
Quantum dot film and preparation method of alumina-coated quantum dot Download PDFInfo
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- CN109652059A CN109652059A CN201910027523.8A CN201910027523A CN109652059A CN 109652059 A CN109652059 A CN 109652059A CN 201910027523 A CN201910027523 A CN 201910027523A CN 109652059 A CN109652059 A CN 109652059A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 170
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 21
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 17
- 229910052782 aluminium Inorganic materials 0.000 claims description 15
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims description 15
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 12
- 230000001681 protective effect Effects 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- YBNMDCCMCLUHBL-UHFFFAOYSA-N (2,5-dioxopyrrolidin-1-yl) 4-pyren-1-ylbutanoate Chemical compound C=1C=C(C2=C34)C=CC3=CC=CC4=CC=C2C=1CCCC(=O)ON1C(=O)CCC1=O YBNMDCCMCLUHBL-UHFFFAOYSA-N 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000012805 post-processing Methods 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims 1
- NRQNMMBQPIGPTB-UHFFFAOYSA-N methylaluminum Chemical compound [CH3].[Al] NRQNMMBQPIGPTB-UHFFFAOYSA-N 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims 1
- 239000003292 glue Substances 0.000 abstract description 21
- 239000003054 catalyst Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 230000003628 erosive effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- MGDOJPNDRJNJBK-UHFFFAOYSA-N ethylaluminum Chemical compound [Al].C[CH2] MGDOJPNDRJNJBK-UHFFFAOYSA-N 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000011247 coating layer Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 19
- 239000004411 aluminium Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- BMTAFVWTTFSTOG-UHFFFAOYSA-N Butylate Chemical group CCSC(=O)N(CC(C)C)CC(C)C BMTAFVWTTFSTOG-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 229910001234 light alloy Inorganic materials 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 238000005253 cladding Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PITRRWWILGYENJ-UHFFFAOYSA-N 2-[2-[2-[2-[2-(4-nonylphenoxy)ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CCCCCCCCCC1=CC=C(OCCOCCOCCOCCOCCO)C=C1 PITRRWWILGYENJ-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 hexamethylene, hexamethylene Chemical group 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000004530 micro-emulsion Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 229920002799 BoPET Polymers 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 241000720974 Protium Species 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 125000002370 organoaluminium group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OBROYCQXICMORW-UHFFFAOYSA-N tripropoxyalumane Chemical compound [Al+3].CCC[O-].CCC[O-].CCC[O-] OBROYCQXICMORW-UHFFFAOYSA-N 0.000 description 1
- 238000009156 water cure Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/22—Luminous paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3009—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Luminescent Compositions (AREA)
Abstract
本发明提供一种量子点薄膜及一种氧化铝包覆量子点的制备方法，所述氧化铝包覆的量子点的制备方法为：将量子点分散液与有机溶剂混合，并逐滴加入三乙基铝溶液，反应结束后得到所述氧化铝包覆的量子点。所述量子点薄膜由上述制备方法制备的氧化铝包覆的量子点为原料制备。所述材料中的氧化铝包覆层可以有效缓解胶水中的催化剂对量子点的侵蚀，使制备的量子点薄膜在使用过程中量子点的发光效率不发生衰减。
The invention provides a quantum dot film and a preparation method of alumina-coated quantum dots. The preparation method of the alumina-coated quantum dots is as follows: mixing quantum dot dispersion liquid with an organic solvent, and adding three Ethyl aluminum solution, and the alumina-coated quantum dots are obtained after the reaction is completed. The quantum dot film is prepared from the alumina-coated quantum dots prepared by the above preparation method as a raw material. The alumina coating layer in the material can effectively alleviate the erosion of the quantum dots by the catalyst in the glue, so that the luminous efficiency of the quantum dots does not decay during the use of the prepared quantum dot film.
Description
Technical field
The invention belongs to technology of quantum dots fields, are related to a kind of preparation method of alumina-coated quantum dot, more particularly to
A kind of film preparation by alumina-coated quantum dot.
Background technique
In recent years, there are many researchs about quantum dot, in the Wavelength tunable of the transmitting light of visible light wave range, half-peak breadth
Narrow, luminous efficiency is high, and display colour gamut is wide, and has powerful application latent in the application fields such as white light LEDs, QLED and display
Power.
It after the preparation of quantum dot film needs to mix QDs and glue, then is coated, or utilizes other industry films
Equipment produces quantum dot film.The homogeneity of its film will affect its luminous efficiency, meanwhile, in display field to the luminous equal of film
Evenness is very high.But quantum dot surface has the long-chain Ligands such as oleic acid, oleyl amine, after directly mixing with glue, will lead to glue
Water cure effect is poor or the decline of the viscosity of glue.In addition, the catalyst in glue also has corrosion function, meeting to quantum dot
Its QY is caused to decline, luminous efficiency reduces.The quantum dot film of conventional method preparation only directly mixes quantum dot with glue,
Not can avoid QDs reunite in glue or glue in erosion of the catalyst to QDs, the quantum dot film of this method preparation
Non-uniform light, will affect it in the application of display field.
108441207 A of CN discloses a kind of quantum dot compound and preparation method thereof, and the quantum dot compound includes
Quantum dot and the covering material for coating the quantum dot, the covering material is by three kinds of metallic element, protium, oxygen element ingredients
It forms and not soluble in water.The preparation method is that: metal alkoxide step 1): is added to the organic solvent containing quantum dot
In, form the first system；Step 2): water is introduced in Xiang Suoshu the first system；Step 3): after the step 2), described
It reacts in one system and generates quantum dot compound.The preparation method but introduces in the reaction using metal alkoxide as raw material
For water as reactant, reactivity hazard is high, should not carry out industrialized production.
Summary of the invention
For the technical problems in the prior art, the present invention provides a kind of quantum dot film and a kind of alumina-coated
The catalysis in glue can be effectively relieved in the preparation method of quantum dot, the alumina-coated layer of the quantum dot of the alumina-coated
Corrosion function of the agent to quantum dot, so that the quantum dot being prepared
The luminous efficiency of film quantum dot in use does not decay.
In order to achieve the above object, the invention adopts the following technical scheme:
It is an object of the present invention to provide a kind of preparation methods of alumina-coated quantum dot, the preparation method is that:
Quantum dot dispersion liquid is mixed with solvent, and triethyl aluminium solution is added dropwise, obtains the oxygen after reaction
Change the quantum dot of aluminium cladding.
As currently preferred technical solution, the quantum dot includes CdSe quantum dot, PbSe quantum dot, PbS quantum
In point, InP quantum dot or perovskite quantum dot any one or at least two combination, the combination is typical but non-limiting
Example has: the combination of CdSe quantum dot and PbSe quantum dot, the combination of PbSe quantum dot and PbS quantum, PbS quantum and
The combination of InP quantum dot, the combination of InP quantum dot and perovskite quantum dot, the combination of perovskite quantum dot and CdSe quantum dot
Or CdSe quantum dot, PbSe quantum dot and combination of PbS quantum etc..
As currently preferred technical solution, the quantum dot dispersion liquid concentration be 30~80mg/mL, as 30mg/mL,
35mg/mL, 40mg/mL, 45mg/mL, 50mg/mL, 55mg/mL, 60mg/mL, 65mg/mL, 70mg/mL, 75mg/mL or
80mg/mL etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally applicable.
As currently preferred technical solution, the solvent is organic solvent；
Preferably, the organic solvent includes any one in hexamethylene, n-hexane, toluene or chloroform or at least two
Combination, such as combination, the combination of n-hexane and toluene or the combination of toluene and chloroform of hexamethylene and n-hexane.
In the present invention, selecting aluminium oxide is clad compared to other unformed metal oxides of cladding or nonmetallic oxidation
The advantages of object is that have higher consistency, and the catalyst in glue is hindered directly to contact quantum dot.
Preferably, the volume ratio of the solvent and quantum dot dispersion liquid is 1000:(1~10), as 1000:1,1000:2,
1000:3,1000:4,1000:5,1000:6,1000:7,1000:8,1000:9 or 1000:10 etc., it is not limited to listed
The numerical value of act, other interior unlisted numerical value of the numberical range are equally applicable.
As currently preferred technical solution, the organo-aluminium includes triethyl aluminum, aluminium secondary butylate, aluminium isopropoxide or first
In base aluminium any one or at least two combination, such as the combination of triethyl aluminum and aluminium secondary butylate, aluminium secondary butylate and isopropanol
The combination of aluminium, the combination of aluminium isopropoxide and aluminium methyl, the combination of aluminium methyl and triethyl aluminum or triethyl aluminum, aluminium secondary butylate and different
The combination etc. of aluminium propoxide.
Preferably, the concentration for having triethyl aluminium solution be 0.5~1.2M, as 0.5M, 0.6M, 0.7M, 0.8M,
0.9M, 1.0M, 1.1M or 1.2M etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range
It is equally applicable.
Preferably, the triethyl aluminium solution and the volume ratio of quantum dot dispersion liquid are 1:(3~10), such as 1:3,1:4,1:
5,1:6,1:7,1:8,1:9 or 1:10 etc., it is not limited to cited numerical value, other interior unlisted numbers of the numberical range
It is worth equally applicable.
As currently preferred technical solution, the reaction carries out under stiring, and the rate of the stirring is 100~
500rpm, such as 100rpm, 150rpm, 200rpm, 250rpm, 300rpm, 350rpm, 400rpm, 450rpm or 500rpm, but
It is not limited in cited numerical value, other unlisted numerical value are equally applicable in the numberical range.
Preferably, the time of the reaction is 2~8h, such as 2h, 3h, 4h, 5h, 6h, 7h, 8h, it is not limited to institute
The numerical value enumerated, other interior unlisted numerical value of the numberical range are equally applicable.
Preferably, it is described be added dropwise organic aluminum solutions and it is described reaction carried out in glove box.
It preferably, is protective gas state in the glove box.
Preferably, the protective gas include in nitrogen, helium or argon gas any one or at least two combination.
As currently preferred technical solution, after being carried out after the reaction to the quantum dot of obtained alumina-coated
Reason.
Preferably, the method for the post-processing is washing and drying.
Preferably, washing 1~5 is carried out to the quantum dot of obtained alumina-coated using the solvent that reaction uses
Secondary, such as 1 time, 2 times, 3 times, 4 times or 5 inferior, it is not limited to cited numerical value, other are unlisted in the numberical range
Numerical value is equally applicable.
Preferably, the temperature of the drying is 50~80 DEG C, such as 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C or 80 DEG C
Deng it is not limited to cited numerical value, other unlisted numerical value are equally applicable in the numberical range.
As currently preferred technical solution, the quantum dot of the alumina-coated the preparation method comprises the following steps:
The quantum dot dispersion liquid that concentration is 30~80mg/mL is mixed with organic solvent, the solvent and quantum dot disperse
The volume ratio of liquid is 1000:(1~10), triethyl aluminium solution is added dropwise in protective gas state glove box, it is described organic
The volume ratio of aluminum solutions and quantum dot dispersion liquid is 1:(3~10), 2~8h, reaction knot are reacted under the stirring of 100~500rpm
Shu Hou takes out sample from glove box, using the solvent that uses of reaction to obtaining the quantum dot of the alumina-coated
Washing 1~5 time, is dried at 50~80 DEG C.
The second purpose of the present invention is to provide a kind of quantum dot of alumina-coated, the quantum dot is made by any of the above-described kind
Preparation Method is prepared.
The three of the object of the invention are to provide a kind of quantum dot film, and the quantum dot film is by above-mentioned alumina-coated
Quantum dot is prepared.
In the present invention, the quantum dot film the preparation method comprises the following steps:
The quantum dot of the above-mentioned alumina-coated being prepared is mixed with glue, is coated to the first protection after vacuum defoaming
On film, the second protective film then is covered on the quantum dot glue-line that coating obtains, the quantum dot film is obtained after solidification.
Wherein, the mass volume ratio of the quantum dot and glue of the alumina-coated is (3~8): 1, such as 3:1,4:1,5:
1,6:1,7:1 or 8:1 etc., it is not limited to cited numerical value, other interior unlisted numerical value of the numberical range are equally suitable
With.
Wherein, the glue can be A/B glue, UV glue or silica gel etc., corresponding curing mode can be curing agent solidification,
Ultra-violet curing is heating and curing.
Compared with prior art, the present invention is at least had the advantages that
(1) present invention provides a kind of preparation method of alumina-coated quantum dot, the amount that the preparation method is prepared
It is sub-, can erosion to avoid catalyst during preparing quantum dot film in glue to quantum dot, improve quantum
The stability of point, the QY of quantum dot film can keep with QY similar in pure quantum dot, or even it is higher than the QY of pure quantum dot；
(2) present invention provides a kind of quantum dot film, and the quantum dot film has good flatness.
Detailed description of the invention
Fig. 1 is the CdSe/CdS/CdZnS quantum dot before the embodiment of the present invention 1 coats；
Fig. 2 is the TEM figure of the quantum dot for the alumina-coated that the embodiment of the present invention 1 is prepared；
Fig. 3 is the high-resolution TEM figure of the quantum dot for the alumina-coated that the embodiment of the present invention 1 is prepared；
Fig. 4 is the energy spectrum diagram of the quantum dot for the alumina-coated that the embodiment of the present invention 1 is prepared；
Fig. 5 is the quantum dot and the mixed pictorial diagram of glue for the alumina-coated that the embodiment of the present invention 1 is prepared；
Fig. 6 is the quantum dot film of the quantum dot preparation for the alumina-coated being prepared using the embodiment of the present invention 1
Pictorial diagram；
Fig. 7 is alumina-coated quantum dot provided by the invention and the flow diagram for being prepared into quantum dot film.
The present invention is described in more detail below.But following examples is only simple example of the invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are subject to claims.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, of the invention is typical but non-limiting
Embodiment is as follows:
Embodiment 1
The present embodiment provides a kind of preparation methods of alumina-coated quantum dot, the preparation method is that:
By concentration be 50mg/mL feux rouges CdSe/CdS/CdZnS quantum dot dispersion liquid mixed with hexamethylene, hexamethylene and
The volume ratio of quantum dot dispersion liquid is 1000:6, is added dropwise in nitrogen state glove box triethyl aluminium solution (1M), described
Triethyl aluminium solution and the volume ratio of quantum dot dispersion liquid are 1:3, and 2h is reacted under the stirring of 300rpm, after reaction, will
Sample takes out from glove box, is washed 3 times using reaction using quantum dot of the hexamethylene to the obtained alumina-coated, then
It is dried at 60 DEG C, obtains the feux rouges CdSe/CdS/CdZnS quantum dot of pure alumina-coated.
The TEM of the feux rouges CdSe/CdS/CdZnS quantum dot for the alumina-coated that the present embodiment is prepared schemes such as Fig. 2 institute
Show, it can be seen that aluminium oxide can effective coated quantum dots, meanwhile, without obviously free quantum dot in figure, illustrate the packet of aluminium oxide
It is good to cover effect.Fig. 3 is the high-resolution of the feux rouges CdSe/CdS/CdZnS quantum dot for the alumina-coated that the present embodiment is prepared
TEM figure, shows that quantum dot is embedded in the aluminium oxide of undefined structure.Fig. 4 is the alumina-coated that the present embodiment is prepared
Feux rouges CdSe/CdS/CdZnS quantum dot energy spectrum diagram, wherein Se, Cd, Zn, S element derive from quantum dot, and O and Al element
From aluminium oxide.
Embodiment 2
The present embodiment provides a kind of preparation methods of the quantum dot of alumina-coated, the preparation method is that:
The green light alloy CdZnSeS quantum dot dispersion liquid that concentration is 30mg/mL is mixed with n-hexane, n-hexane and quantum
The volume ratio of point dispersion liquid is 1000:1, is added dropwise in nitrogen state glove box triethyl aluminium solution (0.5M), described three
The volume ratio of ethyl aluminum solutions and quantum dot dispersion liquid is 1:5,3h is reacted under the stirring of 100rpm, after reaction, by sample
Product take out from glove box, are washed 5 times using reaction using quantum dot of the n-hexane to the obtained alumina-coated, then at
It is dried at 80 DEG C, obtains the green light alloy CdZnSeS quantum dot of pure alumina-coated.
Embodiment 3
The present embodiment provides a kind of preparation methods of the quantum dot of alumina-coated, the preparation method is that:
The green light alloy CdZnSeS quantum dot dispersion liquid that concentration is 80mg/mL is mixed with chloroform, chloroform and quantum dot point
The volume ratio of dispersion liquid is 1000:10, and triethyl aluminium solution (2M), the triethyl aluminum are added dropwise in nitrogen state glove box
The volume ratio of solution and quantum dot dispersion liquid is 1:8, and 6h is reacted under the stirring of 500rpm, after reaction, by sample from hand
It is taken out in casing, is washed 1 time using reaction using quantum dot of the chloroform to the obtained alumina-coated, dried at 50 DEG C
It is dry, obtain the green light alloy CdZnSeS quantum dot of pure alumina-coated.
Embodiment 4
The present embodiment provides a kind of preparation methods of the quantum dot of alumina-coated, the preparation method is that:
The green light CdZnSe/CdZnS quantum dot dispersion liquid that concentration is 60mg/mL is mixed with toluene, toluene and quantum dot
The volume ratio of dispersion liquid is 1000:5, is added dropwise in nitrogen state glove box triethyl aluminium solution (0.8M), three second
The volume ratio of base aluminum solutions and quantum dot dispersion liquid is 1:10,4h is reacted under the stirring of 300rpm, after reaction, by sample
It takes out, is washed 5 times using reaction using quantum dot of the toluene to the obtained alumina-coated, then at 80 DEG C from glove box
Lower drying obtains the green light CdZnSe/CdZnS quantum dot quantum point of pure alumina-coated.
The quantum dot of the embodiment 1-4 alumina-coated being prepared is mixed with UV glue, the amount of the alumina-coated
The mass volume ratio of son point and glue is 5:1, is coated on first layer protective film after vacuum defoaming, the amount then obtained in coating
Second layer protective film is covered on son point glue layer, obtains interlayer type quantum dot film after UV solidification.The protective film is PE film,
It can be PET film, PC film or OPP film etc..
Comparative example 1
This comparative example provides a kind of quantum dot film, and the quantum dot that the quantum dot film uses is using silester as raw material
By reverse microemulsion process coated silica, specially 640 μ L feux rouges CdSe/CdS/CdZnS quantum dots are dispersed in 160mL ring
In hexane, 20mL Igepal Co-520 and 3mL ammonium hydroxide is added, reacts 30h, methanol demulsification is eventually adding, washs, drying.
The preparation method of quantum dot film is also same as Example 1.
Comparative example 2
This comparative example provides a kind of quantum dot film, and the quantum dot that the quantum dot film uses is using silester as raw material
By reverse microemulsion process coated silica, specially 640 μ L green light CdZnSeS quantum dots are dispersed in 160mL hexamethylene,
20mL Igepal Co-520 and 3mL ammonium hydroxide is added, 30h is reacted, methanol demulsification is eventually adding, washs, drying.Quantum dot is thin
The preparation method of film is also same as Example 1.
Comparative example 3
This comparative example provides a kind of preparation method of the quantum dot of alumina-coated, the preparation method is that:
The CdSe/CdS nanometer sheet dispersion liquid that concentration is 50mg/mL is mixed with hexamethylene, hexamethylene and quantum dot disperse
The volume ratio of liquid is 1000:3, and 200 μ L aluminium secondary butylate solution (0.6M) are added dropwise, and reacts 2h under the stirring of 300rpm,
After reaction, it is washed 3 times using reaction using quantum dot of the hexamethylene to the obtained alumina-coated, at 60 DEG C
Drying, obtains the CdSe nanometer sheet quantum dot of pure alumina-coated.
Embodiment 1-4 and comparative example the 1-3 quantum dot being prepared and embodiment 1-4 and comparative example 1-3 are provided
The performance of quantum dot film that is prepared of quantum dot tested, it is as a result as shown in Table 1 and Table 2 respectively.
Table 1
| QY/% before coating | QY/% after cladding | |
| Embodiment 1 | 64 | 53 |
| Embodiment 2 | 23 | 41 |
| Embodiment 3 | 23 | 16 |
| Embodiment 4 | 45 | 52 |
| Comparative example 1 | 64 | 38 |
| Comparative example 2 | 23 | 1 |
| Comparative example 3 | 78 | 0 |
Table 2
| QY/% | |
| Embodiment 1 | 63 |
| Embodiment 2 | 45 |
| Embodiment 3 | 20 |
| Embodiment 4 | 38 |
| Comparative example 1 | 28 |
| Comparative example 2 | 0 |
| Comparative example 3 | 0 |
From its QY after the quantum dot coated aluminum oxide that the test result of Tables 1 and 2 can be seen that embodiment 1 and embodiment 4
Declined, but only have dropped 11% and 7% respectively, the performance of quantum dot is influenced little.Embodiment 2 and embodiment 4 use
Quantum dot itself there are certain defects, the defect on quantum dot can be repaired after coated aluminum oxide, its QY is caused to have instead
Risen.Comparative example 1 and comparative example 2 are coated using silica substitution aluminium oxide, and the quantum dot of comparative example 1 coats dioxy
QY has dropped 26% after SiClx, and QY has dropped 22% after the quantum dot coated silica of comparative example 2, and the amplitude of decline wants high
In embodiment 1 and embodiment 4.The use alumina-coated CdSe/CdS nanometer sheet of comparative example 3, the thickness of nanometer sheet about 2nm, itself
Unstable, QY becomes 0 after coated aluminum oxide.
The Applicant declares that the present invention is explained by the above embodiments detailed construction feature of the invention, but the present invention is simultaneously
It is not limited to above-mentioned detailed construction feature, that is, does not mean that the present invention must rely on above-mentioned detailed construction feature and could implement.Institute
Belong to those skilled in the art it will be clearly understood that any improvement in the present invention, to the equivalence replacement of component selected by the present invention
And increase, selection of concrete mode of accessory etc., all of which fall within the scope of protection and disclosure of the present invention.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (10)
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