CN111876021A - Ink composition, preparation method thereof and quantum dot light-emitting device - Google Patents
Ink composition, preparation method thereof and quantum dot light-emitting device Download PDFInfo
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- CN111876021A CN111876021A CN201910871048.2A CN201910871048A CN111876021A CN 111876021 A CN111876021 A CN 111876021A CN 201910871048 A CN201910871048 A CN 201910871048A CN 111876021 A CN111876021 A CN 111876021A
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 145
- 239000000203 mixture Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 98
- 239000011701 zinc Substances 0.000 claims abstract description 98
- 239000002904 solvent Substances 0.000 claims abstract description 93
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 83
- 239000002243 precursor Substances 0.000 claims abstract description 73
- 239000000463 material Substances 0.000 claims abstract description 69
- 238000009835 boiling Methods 0.000 claims abstract description 27
- 239000003960 organic solvent Substances 0.000 claims abstract description 22
- 239000008139 complexing agent Substances 0.000 claims abstract description 15
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 8
- -1 carbon chain fatty alcohol Chemical class 0.000 claims description 26
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 13
- 239000000758 substrate Substances 0.000 claims description 11
- BKQICAFAUMRYLZ-UHFFFAOYSA-N 4-methylheptan-3-ol Chemical compound CCCC(C)C(O)CC BKQICAFAUMRYLZ-UHFFFAOYSA-N 0.000 claims description 10
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 7
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 claims description 6
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 claims description 6
- YIWUKEYIRIRTPP-UHFFFAOYSA-N 2-ethylhexan-1-ol Chemical compound CCCCC(CC)CO YIWUKEYIRIRTPP-UHFFFAOYSA-N 0.000 claims description 6
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 6
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- ZWRUINPWMLAQRD-UHFFFAOYSA-N nonan-1-ol Chemical compound CCCCCCCCCO ZWRUINPWMLAQRD-UHFFFAOYSA-N 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
- 229910004613 CdTe Inorganic materials 0.000 claims description 5
- 229910007709 ZnTe Inorganic materials 0.000 claims description 5
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 5
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 claims description 5
- 229910052950 sphalerite Inorganic materials 0.000 claims description 5
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 5
- XULHFMYCBKQGEE-MRXNPFEDSA-N 2-Hexyl-1-decanol Natural products CCCCCCCC[C@H](CO)CCCCCC XULHFMYCBKQGEE-MRXNPFEDSA-N 0.000 claims description 4
- XULHFMYCBKQGEE-UHFFFAOYSA-N 2-hexyl-1-Decanol Chemical compound CCCCCCCCC(CO)CCCCCC XULHFMYCBKQGEE-UHFFFAOYSA-N 0.000 claims description 4
- LEACJMVNYZDSKR-UHFFFAOYSA-N 2-octyldodecan-1-ol Chemical compound CCCCCCCCCCC(CO)CCCCCCCC LEACJMVNYZDSKR-UHFFFAOYSA-N 0.000 claims description 4
- UXMUSYTXSNVRMW-UHFFFAOYSA-N 7-phenylheptan-1-ol Chemical compound OCCCCCCCC1=CC=CC=C1 UXMUSYTXSNVRMW-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 238000000151 deposition Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- ZCYXXKJEDCHMGH-UHFFFAOYSA-N nonane Chemical compound CCCC[CH]CCCC ZCYXXKJEDCHMGH-UHFFFAOYSA-N 0.000 claims description 4
- BKIMMITUMNQMOS-UHFFFAOYSA-N normal nonane Natural products CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 claims description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- AAVRLZBLEILGHS-UHFFFAOYSA-N 1-(3-methylphenyl)pentan-1-ol Chemical compound CCCCC(O)C1=CC=CC(C)=C1 AAVRLZBLEILGHS-UHFFFAOYSA-N 0.000 claims description 3
- MNBCPXKENXMEEJ-UHFFFAOYSA-N 1-phenyloctan-1-ol Chemical compound CCCCCCCC(O)C1=CC=CC=C1 MNBCPXKENXMEEJ-UHFFFAOYSA-N 0.000 claims description 3
- WYXKGYXADPUOOM-UHFFFAOYSA-N 5-ethylnonan-2-ol Chemical compound CCCCC(CC)CCC(C)O WYXKGYXADPUOOM-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- 150000001408 amides Chemical class 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 150000004982 aromatic amines Chemical class 0.000 claims description 3
- 125000003118 aryl group Chemical group 0.000 claims description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 239000008096 xylene Substances 0.000 claims description 3
- LFEHSRSSAGQWNI-UHFFFAOYSA-N 2,6,8-trimethylnonan-4-ol Chemical compound CC(C)CC(C)CC(O)CC(C)C LFEHSRSSAGQWNI-UHFFFAOYSA-N 0.000 claims description 2
- 125000002723 alicyclic group Chemical group 0.000 claims description 2
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 claims description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 150000001735 carboxylic acids Chemical class 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 12
- 239000000243 solution Substances 0.000 description 56
- 238000003756 stirring Methods 0.000 description 24
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 14
- 238000007639 printing Methods 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 7
- 239000011787 zinc oxide Substances 0.000 description 7
- 238000007641 inkjet printing Methods 0.000 description 6
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 description 4
- 150000002191 fatty alcohols Chemical class 0.000 description 4
- 150000007942 carboxylates Chemical class 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000003495 polar organic solvent Substances 0.000 description 3
- MWRSABPHNREIIX-UHFFFAOYSA-N 9,9-dimethyldecan-1-ol Chemical compound CC(C)(C)CCCCCCCCO MWRSABPHNREIIX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- JDLYKQWJXAQNNS-UHFFFAOYSA-L zinc;dibenzoate Chemical compound [Zn+2].[O-]C(=O)C1=CC=CC=C1.[O-]C(=O)C1=CC=CC=C1 JDLYKQWJXAQNNS-UHFFFAOYSA-L 0.000 description 2
- 125000004209 (C1-C8) alkyl group Chemical group 0.000 description 1
- 150000007824 aliphatic compounds Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000007649 pad printing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004054 semiconductor nanocrystal Substances 0.000 description 1
- 238000004528 spin coating Methods 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
- 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
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
-
- 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
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention relates to an ink composition, a preparation method thereof and a quantum dot light-emitting device. The ink composition comprises the following raw material components in percentage by weight: 0.1-5% of quantum dot material, 0.1-10% of zinc precursor material, 0.1-10% of complexing agent, 25-70% of quantum dot solvent and 15-50% of zinc precursor solvent; wherein the quantum dot solvent is an organic solvent, wherein the organic solvent is an organic solvent with a dielectric constant of less than 4; the boiling point of the quantum dot solvent is less than the boiling point of the zinc precursor solvent. The ink composition can be printed at one time to form a quantum dot light-emitting layer and an electron transmission layer, and the layer thickness is uniform, so that the manufacturing steps of a QLED device are simplified, and the manufacturing efficiency is improved.
Description
Technical Field
The invention relates to the technical field of display devices, in particular to an ink composition, a preparation method thereof and a quantum dot light-emitting device.
Background
Quantum dots (quantum dots) are zero-dimensional nanomaterials, typically semiconductor nanoparticles with a particle size between 2nm and 20nm, and may therefore be referred to as semiconductor nanocrystals, strictly defined as nanocrystals with a radius less than or close to the exciton Bohr radius. The quantum dots have unique optical properties such as narrow emission spectrum, adjustable emission wavelength by controlling particle size, good light stability and the like, and have already attracted extensive interest and great attention of extensive scientific researchers. Particularly in the display field, a quantum dot electroluminescent device, quantum dot Light Emitting Diode display (QLED), has the advantages of high color gamut, self-luminescence, fast response speed, etc., has once been a research focus in recent years, and is considered as a new generation display following Organic Light-Emitting Diode (OLED) display.
The quantum dots can be dispersed in a solvent to prepare printing materials such as quantum dot ink and the like, is suitable for preparation by a solution method, and can be used for manufacturing quantum dot films by methods such as printing, pad printing, spin coating and the like. In recent years, Ink-jet printing (Ink-jet printing) technology has been widely studied and applied in the field of optoelectronic device manufacturing, and is considered to be an effective way to solve high cost and realize large area, especially in the manufacturing technology of flat panel display devices such as OLED and QLED displays.
The QLED device structure is generally a multilayer structure of ITO/HIL/HTL/QD/ETL/cathode, and the conventional method for preparing the QLED gradually forms the required device structure layer by layer, so that the time consumption is long, and the steps are complicated.
Disclosure of Invention
Based on this, there is a need for an ink composition. The ink composition can be printed at one time to form a quantum dot light-emitting layer and an electron transmission layer, and the layer thickness is uniform, so that the manufacturing steps of a QLED device are simplified, and the manufacturing efficiency is improved.
The ink composition comprises the following raw material components in percentage by weight:
0.1-5% of quantum dot material, 0.1-10% of zinc precursor material, 0.1-10% of complexing agent, 25-70% of quantum dot solvent and 15-50% of zinc precursor solvent;
wherein the quantum dot solvent is an organic solvent, wherein the organic solvent is an organic solvent with a dielectric constant of less than or equal to 4;
the boiling point of the quantum dot solvent is less than the boiling point of the zinc precursor solvent.
In one embodiment, the zinc precursor solvent is a long-carbon-chain fatty alcohol solvent, and has the following structural characteristics:
R0-OH
wherein R is0Selected from: at least one R1A substituted C5-C20 alkyl group, and at least one R1One of substituted C6-C20 aromatic groups; each R1Independently selected from H, C1-C10 alkane radical and C6-C12 aryl radical.
In one embodiment, R0Selected from: at least one R1Substituted C5-C12 alkyl; each R1Independently selected from one of alkyl groups of H, C1-C8 and phenyl groups.
In one embodiment, the boiling point of the quantum dot solvent is 80-180 ℃; and/or
The boiling point of the zinc precursor solvent is 200-350 ℃.
In one embodiment, the zinc precursor solvent is selected from at least one of heptanol, nonanol, 4-methyl-3-heptanol, 2-ethylhexanol, 2,6, 8-trimethyl-4-nonanol, 5-ethyl-2-nonanol, 2-hexyl-1-decanol, 2-octyldodecanol, 3-methylphenylpentanol, 7-phenyl-1-heptanol, and 1-phenyl-1-octanol; and/or
The quantum dot solvent is selected from at least one of octane, heptane, nonane, benzene, toluene, xylene and trimethylbenzene.
In one embodiment, the ink composition comprises the following raw material components in percentage by weight:
1-5% of quantum dot material, 1-5% of zinc precursor material, 1-5% of complexing agent, 40-50% of quantum dot solvent and 40-50% of zinc precursor solvent.
In one embodiment, the zinc precursor material is selected from at least one of zinc nitrate, zinc aliphatic carboxylate, zinc aromatic carboxylate, and zinc cycloaliphatic carboxylate; and/or
The aliphatic carboxylic acid zinc, the aromatic carboxylic acid zinc and the alicyclic carboxylic acid zinc have the carbon number of C1-C17, and respectively and independently contain 1-3 carboxyl groups and 0-2 hydroxyl groups; and/or
The quantum dot material is selected from CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdS/ZnS, CdSe/CdS/ZnS, GaAs, InP, PbS/ZnS、PbSe/ZnS、CuInS2、CuInZnS、CuInGaSe、InP、CsPbCl3、CsPbBr3、CsPbI3And CsPbBrxCl3-xAt least one of; wherein x is 1 or 2.
In one embodiment, the ink composition has a viscosity of 3 to 12cP and a surface tension of 30 to 42 dynes/cm.
The invention also provides a preparation method of the ink composition, which comprises the following steps:
dissolving a complexing agent in a zinc precursor solvent to obtain solution A;
adding a zinc precursor material into the solution A, and dissolving the zinc precursor material to obtain solution B;
dispersing the quantum dot material in a quantum dot solvent to obtain a solution C;
mixing the liquid B and the liquid C to obtain an ink composition;
wherein the quantum dot solvent is an organic solvent, wherein the organic solvent is an organic solvent with a dielectric constant of less than 4;
the boiling point of the quantum dot solvent is less than the boiling point of the zinc precursor solvent.
In one embodiment, the ink composition comprises, by weight, 0.1-5% of quantum dot material, 0.1-10% of zinc precursor material, 0.1-10% of complexing agent, 25-70% of quantum dot solvent, and 15-50% of zinc precursor solvent.
In one embodiment, the zinc precursor solvent is a long-carbon-chain fatty alcohol solvent, and has the following structural characteristics:
R0-OH
wherein R is0Selected from: at least one R1A substituted C5-C20 alkyl group, and at least one R1One of substituted C6-C20 aromatic groups; r1Each occurrence is independently one selected from the group consisting of an alkyl group of H, C1-C10 and an aryl group of C6-C12.
In one embodiment, the boiling point of the quantum dot solvent is 80-180 ℃; and/or
The boiling point of the zinc precursor solvent is 200-350 ℃.
In one embodiment, the zinc precursor material is selected from at least one of zinc nitrate, zinc aliphatic carboxylate, zinc aromatic carboxylate, and zinc cycloaliphatic carboxylate; and/or
The quantum dot material is selected from CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdS/ZnS, CdSe/CdS/ZnS, GaAs, InP, PbS/ZnS, PbSe/ZnS, CuInS2、CuInZnS、CuInGaSe、InP、CsPbCl3、CsPbBr3、CsPbI3And CsPbBrxCl3-xAt least one of; wherein x is 1 or 2; and/or
The complexing agent is at least one selected from ammonia water, aliphatic amine, alcohol amine, amide and aromatic amine.
The invention also provides a quantum dot light-emitting device which comprises a quantum dot light-emitting layer and an electron transmission layer, wherein the quantum dot light-emitting layer and the electron transmission layer are prepared from the ink composition or the ink composition prepared by the preparation method.
The invention also provides a preparation method of the quantum dot light-emitting device, which comprises the following steps:
obtaining a prefabricated member of a quantum dot light-emitting device, wherein the prefabricated member comprises a substrate and an anode layer formed on the substrate;
depositing the ink composition or the ink composition prepared by the preparation method on the surface of the prefabricated member, drying, and carrying out thermal conversion reaction to form the quantum dot light-emitting layer and the electron transmission layer.
In one embodiment, the drying is performed by: at 20-28 deg.C and vacuum degree of less than 1 × 10-5Drying under the condition of Pa in vacuum; and/or
The conditions of the thermal conversion reaction include: the temperature is 120-200 deg.C, and the time is 25-35 min.
Compared with the prior art, the invention has the following beneficial effects:
the invention innovatively discovers that a non-polar or low-polar organic solvent is used as a quantum dot solvent, a zinc precursor material capable of being converted into zinc oxide is used as an electron transport layer material in a matching manner, and the zinc precursor solvent with a boiling point larger than that of the quantum dot solvent is reasonably controlled in proportion of each component, so that an ink composition suitable for ink-jet printing can be obtained, after the ink composition is printed, the quantum dot material can be separated from the zinc precursor material in a drying process to form a quantum dot light emitting layer and a zinc precursor material layer, and the zinc precursor material layer is thermally converted to obtain the zinc oxide electron transport layer. Therefore, a two-layer structure of the quantum dot light-emitting layer and the electronic transmission layer can be formed by one-time printing, the layer thickness is uniform, the quantum dot light-emitting device is prepared by an ink-jet printing mode, the operation is simplified, and the manufacturing cost of the quantum dot light-emitting device is reduced.
Detailed Description
The ink composition, the preparation method thereof, and the quantum dot light emitting device of the present invention will be described in further detail with reference to specific examples.
The embodiment of the invention provides an ink composition, which comprises the following raw material components in percentage by weight:
0.1-5% of quantum dot material, 0.1-10% of zinc precursor material, 0.1-10% of complexing agent, 25-70% of quantum dot solvent and 15-50% of zinc precursor solvent;
wherein the quantum dot solvent is an organic solvent, wherein the organic solvent is an organic solvent with a dielectric constant of less than or equal to 4;
the boiling point of the quantum dot solvent is less than the boiling point of the zinc precursor solvent.
The inventors of the present invention have found that, since a quantum dot material is easily dispersed in a quantum dot solvent (a nonpolar or weakly polar organic solvent, specifically, an organic solvent having a dielectric constant of 4 or less), a quantum dot material solution is formed; and the zinc precursor material (namely the precursor material of the zinc oxide-based electron transport material-organic zinc complex) is heated in the air to obtain the zinc oxide, and the zinc oxide is dispersed and dissolved in a zinc precursor solvent (usually a polar organic solvent with the dielectric constant larger than 4) to form a zinc precursor material solution. After the quantum dot material solvent and the zinc-based precursor material solution are mixed into the quantum dot electronic ink, the boiling point of the quantum dot solvent is lower than that of the zinc precursor solvent, the quantum dot solvent does not contain hydrogen bonds and is more volatile than that of the zinc precursor solvent, so that after the quantum dot electronic ink is printed, the quantum dot solvent is more quickly volatilized in the drying process, and as the quantum dot solvent is reduced, the concentration of the zinc precursor solvent is increased, and the quantum dot material is firstly settled to form a quantum dot layer; and then after the residual zinc precursor solvent is volatilized, forming a zinc oxide-based precursor, and then carrying out thermal conversion to obtain the zinc oxide electron transport layer.
Preferably, the ink composition comprises the following raw material components in percentage by weight:
1-5% of quantum dot material, 1-5% of zinc precursor material, 1-5% of complexing agent, 40-50% of quantum dot solvent and 40-50% of zinc precursor solvent.
In some specific embodiments, the zinc precursor solvent is a long-carbon-chain fatty alcohol solvent, and has the following structural features:
R0-OH
wherein R is0Selected from: at least one R1A substituted C5-C20 alkyl group, and at least one R1One of substituted C6-C20 aromatic groups; r1Each occurrence is independently one selected from the group consisting of an alkyl group of H, C1-C10 and an aryl group of C6-C12.
The long carbon chain fatty alcohol is adopted as a zinc precursor solvent, one end of the long carbon chain is lipophilic, the long carbon chain fatty alcohol has a certain dispersion effect on quantum dot materials, the stability of the long carbon chain fatty alcohol cannot be influenced, and the compatibility among all components of an ink composition system is improved. In addition, the zinc precursor material is easy to dissolve in the long-carbon-chain fatty alcohol to form a solution without particles, so that the probability of blockage of an ink-jet printing nozzle can be reduced.
Preferably, R0Selected from: at least one R1Substituted C5-C12 alkyl; r1Each occurrence is independently selected from the group consisting of H, C1-C8 alkyl and phenyl.
More preferably, the zinc precursor solvent is at least one selected from the group consisting of heptanol, nonanol, 4-methyl-3-heptanol, 2-ethylhexanol, trimethylnonanol, 5-ethyl-2-nonanol, 2-hexyl-1-decanol, 2-octyldodecanol, 3-methylphenylpentanol, 7-phenyl-1-heptanol, and 1-phenyl-1-octanol.
In some specific embodiments, the quantum dot solvent may be selected from at least one of an aliphatic compound or an aromatic compound. Preferably, the quantum dot solvent is selected from at least one of octane, heptane, nonane, benzene, toluene, xylene, and trimethylbenzene. The quantum dot solvent can ensure the solubility of the quantum dot material, increase the compatibility with a zinc precursor solvent and ensure the stability of an ink composition system.
In some specific embodiments, the quantum dot solvent has a boiling point of 80-180 ℃; and/or the boiling point of the zinc precursor solvent is 200-350 ℃. The boiling point ranges of the quantum dot solvent and the zinc precursor solvent are controlled, so that the smoothness of the quantum dot light-emitting layer and the electron transport layer and the controllability of the drying process are improved.
In some specific embodiments, the zinc precursor material is selected from at least one of zinc nitrate, zinc aliphatic carboxylate, zinc aromatic carboxylate, and zinc cycloaliphatic carboxylate. More specifically, the aliphatic zinc carboxylate, the aromatic zinc carboxylate and the alicyclic zinc carboxylate have a carbon chain length of C1-C17, and each independently contains 1-3 carboxyl groups and 0-2 hydroxyl groups.
In some specific embodiments, the quantum dot material is selected from CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdS/ZnS, CdSe/CdS/ZnS, GaAs, InP, PbS/ZnS, PbSe/ZnS, CuInS2、CuInZnS、CuInGaSe、InP、CsPbCl3、CsPbBr3、CsPbI3And CsPbBrxCl3-xAt least one of; wherein x is 1 or 2.
In some specific embodiments, the complexing agent is selected from at least one of ammonia, aliphatic amines, alcohol amines, amides, and aromatic amines.
In some specific embodiments, the ink composition has a viscosity of 3-12cP and a surface tension of 30-42 dynes/cm.
The preparation method of the ink composition comprises the following steps:
dissolving a complexing agent in a zinc precursor solvent to obtain solution A;
adding a zinc precursor material into the solution A, and dissolving the zinc precursor material to obtain solution B;
dispersing the quantum dot material in a quantum dot solvent to obtain a solution C;
mixing the solution B and the solution C;
wherein the quantum dot solvent is an organic solvent, wherein the organic solvent is an organic solvent with a dielectric constant of less than 4;
the boiling point of the quantum dot solvent is less than the boiling point of the zinc precursor solvent.
In some embodiments, the solution a is heated to 50-100 ℃ before the zinc precursor material is added to the solution a, and then the zinc precursor material is added.
Embodiments of the present invention also provide a quantum dot light emitting device including a quantum dot light emitting layer and an electron transport layer made using one of the ink compositions.
In some specific embodiments, the qd-led device is a qd-led.
The preparation method of the quantum dot light-emitting device comprises the following steps:
obtaining a prefabricated part of the quantum dot light-emitting device;
and depositing one of the ink compositions on the surface of the prefabricated member, drying, and carrying out a thermal conversion reaction to form the quantum dot light-emitting layer and the electron transport layer.
It is understood that the preform refers to a basic article on which a quantum dot light emitting layer and an electron transport layer need to be formed, and includes at least a substrate and an anode layer formed on the substrate, such as a substrate (ITO) including an anode or a substrate including an anode, and a hole injection layer and a hole transport layer (ITO/HIL/HTL) sequentially stacked thereon.
In some specific embodiments, the drying is performed by: at 20-28 deg.C and vacuum degree of less than 1 × 10-5True under the condition of PaAnd (5) drying in air.
In some specific embodiments, the conditions of the thermal conversion reaction include: the temperature is 120-200 deg.C, and the time is 25-35 min.
The following are specific examples, and the raw materials used in the examples are all commercially available products unless otherwise specified.
Example 1
The electronic dot ink of the embodiment comprises the following components in parts by weight:
(1) under the condition of stirring, 3g of dodecylamine is dissolved in 45g of trimethyl nonanol under the condition of stirring to obtain solution A;
(2) heating solution A to 80 deg.C, adding 1gZn (CH)3COO)2Stirring until the solution is dissolved to obtain solution B;
(3) dispersing 1g of CdS oil-soluble quantum dots in 50g of toluene to obtain solution C;
(4) and mixing the solution C and the solution B under the stirring condition to obtain the quantum dot electronic ink.
The viscosity of the quantum dot electronic ink is 6.3cp (25 ℃), and the surface tension is 35.2dynes/cm (25 ℃).
The quantum dot light-emitting diode is manufactured by adopting the quantum dot electronic ink, and the steps are as follows:
(1) obtaining a substrate (ITO) comprising an anode;
(2) depositing the quantum dot electronic ink on the substrate in an ink-jet printing mode, then vacuumizing and drying at room temperature, and removing the solvent;
(3) and finally, heating the substrate in the air at the temperature of 150 ℃ for 30min to form a two-layer structure of the quantum dot material layer and the electron transmission material layer through one-step printing, wherein the layer thickness is uniform.
Example 2
The electronic dot ink of the embodiment comprises the following components in parts by weight:
(1) under the stirring condition, 2g of dodecylamine is dissolved in 45g of 4-methyl-3-heptanol under the stirring condition to obtain solution A;
(2) heating solution A at 80 deg.C, adding 5gZn (CH)3COO)2Stirring until the solution is dissolved to obtain solution B;
(3)3g of CdS/ZnS oil-soluble quantum dots are dispersed in 45g of dimethylbenzene to obtain a solution C;
(4) and mixing the solution C and the solution B under the stirring condition to obtain the quantum dot electronic ink.
The viscosity of the quantum dot electronic ink is 5.3cp (25 ℃), and the surface tension is 34.6dynes/cm (25 ℃).
The quantum dot light-emitting diode is manufactured by adopting the quantum dot electronic ink, and the steps are the same as those of the embodiment 1. The two-layer structure of the quantum dot material layer and the electron transmission material layer can be formed by one-time printing, and the layer thickness is uniform.
Example 3
The electronic dot ink of the embodiment comprises the following components in parts by weight:
(1) under the condition of stirring, 5g of octylamine is dissolved in 40g of 4-methyl-3-heptanol under the condition of stirring, and solution A is obtained;
(2) heating solution A at 80 deg.C, adding 3gZn (CH)3COO)2Stirring until the solution is dissolved to obtain solution B;
(3)5g of CdS/ZnS oil-soluble quantum dots are dispersed in 47g of dimethylbenzene to obtain a solution C;
(4) and mixing the solution C and the solution B under the stirring condition to obtain the quantum dot electronic ink.
The viscosity of the quantum dot electronic ink is 4.6cp (25 ℃), and the surface tension is 33.8dynes/cm (25 ℃).
The quantum dot light-emitting diode is manufactured by adopting the quantum dot electronic ink, and the steps are the same as those of the embodiment 1. The two-layer structure of the quantum dot material layer and the electron transmission material layer can be formed by one-time printing, and the layer thickness is uniform.
Example 4
The electronic dot ink of the embodiment comprises the following components in parts by weight:
(1) under the stirring condition, 3g of ammonia water is dissolved in 45g of 7-phenyl-1-heptanol under the stirring condition to obtain solution A;
(2) heating the solution A to 80 ℃, adding 1g of zinc nitrate, and stirring until the zinc nitrate is dissolved to obtain solution B;
(3) dispersing 1g of CuInGaSe oil-soluble quantum dots in 50g of nonane to obtain a solution C;
(4) and mixing the solution C and the solution B under the stirring condition to obtain the quantum dot electronic ink.
The viscosity of the quantum dot electronic ink is 5.4cp (25 ℃), and the surface tension is 31.6dynes/cm (25 ℃).
The quantum dot light-emitting diode is manufactured by adopting the quantum dot electronic ink, and the steps are the same as those of the embodiment 1. The two-layer structure of the quantum dot material layer and the electron transmission material layer can be formed by one-time printing, and the layer thickness is uniform.
Example 5
The electronic dot ink of the embodiment comprises the following components in parts by weight:
(1) under the condition of stirring, 3g of dodecylamine is dissolved in 45g of 2-octyldodecanol under the condition of stirring to obtain solution A;
(2) heating the solution A to 80 ℃, adding 1g of zinc benzoate, and stirring until the zinc benzoate is dissolved to obtain solution B;
(3)1g CsPbI3dispersing oil-soluble quantum dots in 50g of toluene to obtain solution C;
(4) and mixing the solution C and the solution B under the stirring condition to obtain the quantum dot electronic ink.
The viscosity of the quantum dot electronic ink is 5.8cp (25 ℃), and the surface tension is 32.3dynes/cm (25 ℃).
The quantum dot light-emitting diode is manufactured by adopting the quantum dot electronic ink, and the steps are the same as those of the embodiment 1. The two-layer structure of the quantum dot material layer and the electron transmission material layer can be formed by one-time printing, and the layer thickness is uniform.
Example 6
The electronic dot ink of the embodiment comprises the following components in parts by weight:
(1) under the condition of stirring, 3g of dodecylamine is dissolved in 45g of 2-hexyl-1-decanol under the condition of stirring to obtain solution A;
(2) heating the solution A to 80 ℃, adding 1g of zinc naphthanate, and stirring until the zinc naphthanate is dissolved to obtain solution B;
(3) dispersing 1g of GaAs oil-soluble quantum dots in 50g of octane to obtain a solution C;
(4) and mixing the solution C and the solution B under the stirring condition to obtain the quantum dot electronic ink.
The viscosity of the quantum dot electronic ink is 4.9cp (25 ℃), and the surface tension is 32.2dynes/cm (25 ℃).
The quantum dot light-emitting diode is manufactured by adopting the quantum dot electronic ink, and the steps are the same as those of the embodiment 1. The two-layer structure of the quantum dot material layer and the electron transmission material layer can be formed by one-time printing, and the layer thickness is uniform.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (16)
1. The ink composition is characterized by comprising the following raw material components in percentage by weight:
0.1-5% of quantum dot material, 0.1-10% of zinc precursor material, 0.1-10% of complexing agent, 25-70% of quantum dot solvent and 15-50% of zinc precursor solvent;
wherein the quantum dot solvent is an organic solvent, wherein the organic solvent is an organic solvent with a dielectric constant of less than or equal to 4;
the boiling point of the quantum dot solvent is less than the boiling point of the zinc precursor solvent.
2. The ink composition of claim 1, wherein the zinc precursor solvent is a long carbon chain fatty alcohol solvent having the following structural features:
R0-OH
wherein R is0Selected from: at least one R1A substituted C5-C20 alkyl group, and at least one R1One of substituted C6-C20 aromatic groups; each R1Independently selected from H, C1-C10 alkane radical and C6-C12 aryl radical.
3. The ink composition of claim 2, wherein R is0Selected from: at least one R1Substituted C5-C12 alkyl; each R1Independently selected from one of alkyl groups of H, C1-C8 and phenyl groups.
4. The ink composition of any of claims 1-3, wherein the quantum dot solvent has a boiling point of 80-180 ℃; and/or
The boiling point of the zinc precursor solvent is 200-350 ℃.
5. The ink composition of claim 4, wherein the zinc precursor solvent is selected from at least one of heptanol, nonanol, 4-methyl-3-heptanol, 2-ethylhexanol, 2,6, 8-trimethyl-4-nonanol, 5-ethyl-2-nonanol, 2-hexyl-1-decanol, 2-octyldodecanol, 3-methylphenylpentanol, 7-phenyl-1-heptanol, and 1-phenyl-1-octanol; and/or
The quantum dot solvent is selected from at least one of octane, heptane, nonane, benzene, toluene, xylene and trimethylbenzene.
6. The ink composition according to any one of claims 1 to 3, comprising the following raw material components in percentage by weight:
1-5% of quantum dot material, 1-5% of zinc precursor material, 1-5% of complexing agent, 40-50% of quantum dot solvent and 40-50% of zinc precursor solvent.
7. The ink composition according to any one of claims 1 to 3, wherein the zinc precursor material is selected from at least one of zinc nitrate, zinc aliphatic carboxylate, zinc aromatic carboxylate, and zinc alicyclic carboxylate; and/or
The aliphatic carboxylic acid zinc, the aromatic carboxylic acid zinc and the alicyclic carboxylic acid zinc have the carbon number of C1-C17, and respectively and independently contain 1-3 carboxyl groups and 0-2 hydroxyl groups; and/or
The quantum dot material is selected from CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdS/ZnS, CdSe/CdS/ZnS, GaAs, InP, PbS/ZnS, PbSe/ZnS, CuInS2、CuInZnS、CuInGaSe、InP、CsPbCl3、CsPbBr3、CsPbI3And CsPbBrxCl3-xAt least one of; wherein x is 1 or 2.
8. The ink composition of claim 1, wherein the ink composition has a viscosity of 3-12cP and a surface tension of 30-42 dynes/cm.
9. A method of preparing an ink composition, comprising the steps of:
dissolving a complexing agent in a zinc precursor solvent to obtain solution A;
adding a zinc precursor material into the solution A, and dissolving the zinc precursor material to obtain solution B;
dispersing the quantum dot material in a quantum dot solvent to obtain a solution C;
mixing the liquid B and the liquid C to obtain an ink composition;
wherein the quantum dot solvent is an organic solvent, wherein the organic solvent is an organic solvent with a dielectric constant of less than 4;
the boiling point of the quantum dot solvent is less than the boiling point of the zinc precursor solvent.
10. The method according to claim 9, wherein the ink composition comprises, in weight percent, 0.1 to 5% of the quantum dot material, 0.1 to 10% of the zinc precursor material, 0.1 to 10% of the complexing agent, 25 to 70% of the quantum dot solvent, and 15 to 50% of the zinc precursor solvent.
11. The method of claim 9, wherein the zinc precursor solvent is a long carbon chain fatty alcohol solvent having the following structural features:
R0-OH
wherein R is0Selected from: at least one R1A substituted C5-C20 alkyl group, and at least one R1One of substituted C6-C20 aromatic groups; r1Each occurrence is independently one selected from the group consisting of an alkyl group of H, C1-C10 and an aryl group of C6-C12.
12. The method of any one of claims 9-11, wherein the quantum dot solvent has a boiling point of 80-180 ℃; and/or
The boiling point of the zinc precursor solvent is 200-350 ℃.
13. The production method according to any one of claims 9 to 11, characterized in that the zinc precursor material is selected from at least one of zinc nitrate, zinc aliphatic carboxylate, zinc aromatic carboxylate, and zinc alicyclic carboxylate; and/or
The quantum dot material is selected from CdSe, CdS, ZnSe, ZnS, CdTe, ZnTe, CdS/ZnS, CdSe/CdS/ZnS, GaAs, InP, PbS/ZnS, PbSe/ZnS, CuInS2、CuInZnS、CuInGaSe、InP、CsPbCl3、CsPbBr3、CsPbI3And CsPbBrxCl3-xAt least one of; wherein x is 1 or 2; and/or
The complexing agent is at least one selected from ammonia water, aliphatic amine, alcohol amine, amide and aromatic amine.
14. A quantum dot light-emitting device comprising a quantum dot light-emitting layer and an electron-transporting layer, which are formed using the ink composition according to any one of claims 1 to 8 or the ink composition prepared by the preparation method according to any one of claims 9 to 13.
15. A method for preparing a quantum dot light-emitting device is characterized by comprising the following steps:
obtaining a prefabricated member of a quantum dot light-emitting device, wherein the prefabricated member comprises a substrate and an anode layer formed on the substrate;
depositing the ink composition of any one of claims 1 to 8 or the ink composition prepared by the preparation method of any one of claims 9 to 13 on the surface of the preform, drying, and performing a thermal conversion reaction to form a quantum dot light emitting layer and an electron transporting layer.
16. The method of claim 15, wherein the drying is performed by: at 20-28 deg.C and vacuum degree of less than 1 × 10-5Drying under the condition of Pa in vacuum; and/or
The conditions of the thermal conversion reaction include: the temperature is 120-200 deg.C, and the time is 25-35 min.
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