WO2019074083A1 - 量子ドット及びその製造方法、量子ドットを用いた波長変換部材、照明部材、バックライト装置、並びに、表示装置 - Google Patents
量子ドット及びその製造方法、量子ドットを用いた波長変換部材、照明部材、バックライト装置、並びに、表示装置 Download PDFInfo
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- WO2019074083A1 WO2019074083A1 PCT/JP2018/038038 JP2018038038W WO2019074083A1 WO 2019074083 A1 WO2019074083 A1 WO 2019074083A1 JP 2018038038 W JP2018038038 W JP 2018038038W WO 2019074083 A1 WO2019074083 A1 WO 2019074083A1
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- Prior art keywords
- quantum dot
- solution
- fluorescence
- znse
- zinc
- Prior art date
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- 239000002096 quantum dot Substances 0.000 title claims abstract description 124
- 238000006243 chemical reaction Methods 0.000 title claims description 129
- 238000004519 manufacturing process Methods 0.000 title claims description 22
- 238000005286 illumination Methods 0.000 title claims description 7
- 238000000034 method Methods 0.000 title description 9
- 239000011669 selenium Substances 0.000 claims abstract description 51
- 239000011701 zinc Substances 0.000 claims abstract description 36
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 26
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- 229910052725 zinc Inorganic materials 0.000 claims abstract description 21
- 239000002159 nanocrystal Substances 0.000 claims abstract description 15
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 10
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000011593 sulfur Substances 0.000 claims abstract description 10
- 239000011258 core-shell material Substances 0.000 claims abstract description 4
- 239000010949 copper Substances 0.000 claims description 77
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- 239000002243 precursor Substances 0.000 claims description 24
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- 239000005749 Copper compound Substances 0.000 claims description 10
- 150000001880 copper compounds Chemical class 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
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- 229910000073 phosphorus hydride Inorganic materials 0.000 claims description 3
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 183
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 85
- 238000003756 stirring Methods 0.000 description 69
- 239000002244 precipitate Substances 0.000 description 63
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- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 34
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- 101100063942 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) dot-1 gene Proteins 0.000 description 21
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 21
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- 238000005259 measurement Methods 0.000 description 16
- 239000000203 mixture Substances 0.000 description 14
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- 239000006185 dispersion Substances 0.000 description 11
- 150000003752 zinc compounds Chemical class 0.000 description 10
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- 238000000103 photoluminescence spectrum Methods 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 7
- LPEBYPDZMWMCLZ-CVBJKYQLSA-L zinc;(z)-octadec-9-enoate Chemical compound [Zn+2].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O LPEBYPDZMWMCLZ-CVBJKYQLSA-L 0.000 description 7
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- 238000005424 photoluminescence Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 238000009835 boiling Methods 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 5
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 5
- 239000003086 colorant Substances 0.000 description 4
- 238000005401 electroluminescence Methods 0.000 description 4
- 239000011259 mixed solution Substances 0.000 description 4
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 description 4
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- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 description 4
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- 150000003573 thiols Chemical class 0.000 description 4
- 238000006478 transmetalation reaction Methods 0.000 description 4
- UAYWVJHJZHQCIE-UHFFFAOYSA-L zinc iodide Chemical compound I[Zn]I UAYWVJHJZHQCIE-UHFFFAOYSA-L 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
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- VMQMZMRVKUZKQL-UHFFFAOYSA-N Cu+ Chemical compound [Cu+] VMQMZMRVKUZKQL-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
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- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 3
- ZKXWKVVCCTZOLD-FDGPNNRMSA-N copper;(z)-4-hydroxypent-3-en-2-one Chemical compound [Cu].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O ZKXWKVVCCTZOLD-FDGPNNRMSA-N 0.000 description 3
- VTXVGVNLYGSIAR-UHFFFAOYSA-N decane-1-thiol Chemical compound CCCCCCCCCCS VTXVGVNLYGSIAR-UHFFFAOYSA-N 0.000 description 3
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- 239000011574 phosphorus Substances 0.000 description 3
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- 238000001228 spectrum Methods 0.000 description 3
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- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 1
- PHYFQTYBJUILEZ-IUPFWZBJSA-N triolein Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(OC(=O)CCCCCCC\C=C/CCCCCCCC)COC(=O)CCCCCCC\C=C/CCCCCCCC PHYFQTYBJUILEZ-IUPFWZBJSA-N 0.000 description 1
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical compound C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical compound [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
- 229960000314 zinc acetate Drugs 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 229940102001 zinc bromide Drugs 0.000 description 1
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 description 1
- RKQOSDAEEGPRER-UHFFFAOYSA-L zinc diethyldithiocarbamate Chemical compound [Zn+2].CCN(CC)C([S-])=S.CCN(CC)C([S-])=S RKQOSDAEEGPRER-UHFFFAOYSA-L 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- NRINZBKAERVHFW-UHFFFAOYSA-L zinc;dicarbamate Chemical compound [Zn+2].NC([O-])=O.NC([O-])=O NRINZBKAERVHFW-UHFFFAOYSA-L 0.000 description 1
- GPYYEEJOMCKTPR-UHFFFAOYSA-L zinc;dodecanoate Chemical compound [Zn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O GPYYEEJOMCKTPR-UHFFFAOYSA-L 0.000 description 1
- GJAPSKMAVXDBIU-UHFFFAOYSA-L zinc;hexadecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCC([O-])=O GJAPSKMAVXDBIU-UHFFFAOYSA-L 0.000 description 1
- NHXVNEDMKGDNPR-UHFFFAOYSA-N zinc;pentane-2,4-dione Chemical compound [Zn+2].CC(=O)[CH-]C(C)=O.CC(=O)[CH-]C(C)=O NHXVNEDMKGDNPR-UHFFFAOYSA-N 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
- DUBNHZYBDBBJHD-UHFFFAOYSA-L ziram Chemical compound [Zn+2].CN(C)C([S-])=S.CN(C)C([S-])=S DUBNHZYBDBBJHD-UHFFFAOYSA-L 0.000 description 1
Images
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- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/04—Binary compounds including binary selenium-tellurium compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- 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
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
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- 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
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/88—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing selenium, tellurium or unspecified chalcogen elements
- C09K11/881—Chalcogenides
- C09K11/883—Chalcogenides with zinc or cadmium
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V7/00—Reflectors for light sources
- F21V7/22—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors
- F21V7/28—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors characterised by coatings
- F21V7/30—Reflectors for light sources characterised by materials, surface treatments or coatings, e.g. dichroic reflectors characterised by coatings the coatings comprising photoluminescent substances
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F21—LIGHTING
- F21V—FUNCTIONAL FEATURES OR DETAILS OF LIGHTING DEVICES OR SYSTEMS THEREOF; STRUCTURAL COMBINATIONS OF LIGHTING DEVICES WITH OTHER ARTICLES, NOT OTHERWISE PROVIDED FOR
- F21V9/00—Elements for modifying spectral properties, polarisation or intensity of the light emitted, e.g. filters
- F21V9/30—Elements containing photoluminescent material distinct from or spaced from the light source
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- 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
- H01L33/48—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 body packages
- H01L33/50—Wavelength conversion elements
-
- 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
- H01L33/48—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 body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
- H01L33/504—Elements with two or more wavelength conversion materials
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B33/00—Electroluminescent light sources
- H05B33/12—Light sources with substantially two-dimensional radiating surfaces
- H05B33/14—Light sources with substantially two-dimensional radiating surfaces characterised by the chemical or physical composition or the arrangement of the electroluminescent material, or by the simultaneous addition of the electroluminescent material in or onto the light source
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Definitions
- the present invention relates to a cadmium-free quantum dot and a method of manufacturing the same, a wavelength conversion member using a quantum dot, an illumination member, a backlight device, and a display device.
- the quantum dot is a nanoparticle having a particle diameter of several nm to several tens of nm, which is composed of several hundreds to several thousands of atoms. Quantum dots are also called fluorescent nanoparticles, semiconductor nanoparticles, or nanocrystals. The quantum dot has a feature that the emission wavelength can be variously changed according to the particle size and the composition of the nanoparticle.
- the fluorescence quantum yield (Quantum Yield: QY) and the fluorescence half width (Full Width at Half Maximum: FWHM) can be mentioned as those representing the performance of the quantum dot.
- QY Quantum Yield
- FWHM Fluorescence Half Maximum
- Cd-free quantum dots that do not use cadmium include chalcopyrite quantum dots such as CuInS 2 and AgInS 2 and indium phosphide (InP) quantum dots are in development (for example, Patent Document 1) See).
- chalcopyrite quantum dots such as CuInS 2 and AgInS 2 and indium phosphide (InP) quantum dots
- InP indium phosphide
- ZnSe quantum dots have been developed as quantum dots, and many examples of synthesizing blue-emitting phosphors using ZnSe have been reported.
- ZnSe quantum dots having a wavelength and a half width of which would be alternatives to conventional blue LEDs.
- Non-Patent Document 1 describes in detail a direct synthesis method of ZnSe using diphenyl phosphine selenide which is considered to be relatively reactive with organic zinc compounds.
- the ZnSe obtained in this paper is not suitable for practical use because it has a fluorescence wavelength of about 430 nm and does not reach 450 nm, which is a blue fluorescence wavelength used for practical use.
- Non-Patent Document 2 a method of synthesizing ZnSe in a water system is reported. Although the reaction proceeds at a low temperature, the half width is 30 nm or more and a little broad, and the fluorescence wavelength is less than 430 nm, so it is not suitable for achieving high color gamut by using it as a substitute for conventional blue LED It is.
- quantum dots As described above, although research and development of blue quantum dots are in progress, none of the quantum dots have achieved a fluorescence wavelength of 430 nm or more and a fluorescence half width of 25 nm or less at a mass producible level.
- This invention is made in view of this point, and an object of the present invention is to provide a quantum dot which emits blue fluorescence which is Cd free and whose fluorescence half width is narrow.
- Another object of the present invention is to provide a manufacturing method capable of mass-producing the above-mentioned quantum dots safely.
- the quantum dot in the present invention is characterized by containing no cadmium (Cd) and having a fluorescence half width of 25 nm or less.
- the quantum dots are preferably nanocrystals containing zinc (Zn) and selenium (Se), or zinc (Zn), selenium (Se) and sulfur (S).
- the quantum dot has a core-shell structure in which the nanocrystal is a core and the surface of the core is coated with a shell.
- the fluorescence wavelength is preferably in the range of 410 nm to 470 nm.
- the surface of the quantum dot is preferably covered with a ligand (Ligand).
- the ligand is preferably selected from at least one or two of an aliphatic amine type, a phosphine type and an aliphatic carboxylic acid type.
- the method for producing a quantum dot according to the present invention comprises synthesizing a copper chalcogenide as a precursor from an organic copper compound or an inorganic copper compound and an organic chalcogen compound, and using the precursor, containing cadmium (Cd) It is preferable to synthesize no quantum dots.
- transmetalate copper (Cu) and zinc (Zn) of the precursor made of copper cargogenide it is preferable to transmetalate copper (Cu) and zinc (Zn) of the precursor made of copper cargogenide.
- the metal exchange reaction it is preferable to carry out the metal exchange reaction at 180 ° C. or more and 280 ° C. or less. Further, it is preferable to synthesize the copper chalcogenide at a reaction temperature of 140 ° C. or more and 250 ° C. or less.
- the quantum dots are preferably nanocrystals containing zinc and selenium, or zinc, selenium and sulfur.
- the wavelength conversion member in the present invention is characterized by including the above-described quantum dot or a quantum dot formed by the above-described method of manufacturing a quantum dot.
- the illumination member in the present invention is characterized by including the above-described quantum dot or a quantum dot formed by the above-described method of manufacturing a quantum dot.
- the backlight device in the present invention is characterized by including the above-described quantum dot or a quantum dot formed by the above-described method of manufacturing a quantum dot.
- the display device in the present invention is characterized by including the above-described quantum dot or a quantum dot formed by the above-described method of manufacturing a quantum dot.
- the present invention since it is possible to synthesize quantum dots having the same particle shape and size, it is possible to narrow the fluorescence half width and to improve the high color gamut.
- the method for producing a quantum dot of the present invention it is possible to produce a quantum dot having a narrow fluorescence half width and not containing Cd safely and in a mass producible method.
- FIG. 1A is a schematic view of a quantum dot according to an embodiment of the present invention.
- FIG. 1B is a schematic view of a quantum dot according to an embodiment of the present invention.
- 3 is a fluorescence (Photoluminescence (PL)) spectrum of ZnSe in Example 1.
- FIG. 7 is a PL spectrum of ZnSe in Example 2.
- 7 is a PL spectrum of ZnSe in Example 3.
- 7 is a PL spectrum of ZnSe in Example 4.
- 7 is a PL spectrum of ZnSe in Example 5.
- 7 is a PL spectrum of ZnSe in Example 6.
- 7 is a PL spectrum of ZnSe in Example 7.
- 7 is a PL spectrum of ZnSe in Example 8.
- FIG. 7 is a PL spectrum of ZnSe in Example 9.
- 1 is a scanning line electron microscope (SEM) photograph of ZnSe in Example 1.
- FIG. 1 is an X-ray diffraction (Xray diffraction: XRD spectrum) of ZnSe in Example 1.
- FIG. 7 is a SEM photograph of Cu 2 Se in Example 1.
- FIG. 1A and 1B are schematic views of a quantum dot in the present embodiment.
- the quantum dot 1 shown in FIG. 1A is a nanocrystal free of cadmium (hereinafter referred to as Cd).
- the quantum dots 1 are preferably nanocrystals containing zinc and selenium (hereinafter referred to as Zn and Se) or zinc and selenium and sulfur (referred to as Zn, Se and S). .
- the quantum dot 1 has fluorescence characteristics by band edge emission, and the quantum size effect is exhibited by the fact that the particle is nano-sized.
- nanoclaystal refers to nanoparticles having a particle size of about several nm to several tens of nm.
- a large number of quantum dots 1 can be generated with a substantially uniform particle size.
- Zn and Se or Zn and Se and S contained in the quantum dot 1 are main components, elements other than these elements may be contained. However, it is preferable that Cd is not contained and that phosphorus (P) is not contained.
- the organophosphorus compounds are expensive and easily oxidized in air, so the synthesis becomes unstable, and the cost increases, the fluorescence characteristics become unstable, and the production process becomes complicated.
- the quantum dot 1 of the present embodiment has a fluorescence half width of 25 nm or less.
- Fluorescent half width refers to a full width at half maximum that indicates the spread of fluorescence wavelength at half the peak value of the fluorescence intensity in the fluorescence spectrum.
- the half width of fluorescence is preferably 23 nm or less.
- the fluorescence half width is more preferably 20 nm or less.
- it is further more preferable that the fluorescence half width is 17 nm or less.
- the fluorescence half width can be narrowed, it is possible to improve the high color gamut.
- the fluorescence half width can be narrowed, and specifically, the fluorescence half width of 25 nm or less can be achieved.
- ligands 2 are coordinated to the surface of the quantum dot 1. Thereby, aggregation of quantum dot 1 comrades can be suppressed and the optical characteristic made into the objective expresses.
- the ligand which can be used for reaction is not specifically limited, For example, the following ligands are mentioned as a typical thing.
- the fluorescence quantum yield (Quantum Yield) of the quantum dot 1 in the present embodiment is 10% or more.
- the fluorescence quantum yield is more preferably 30% or more, and still more preferably 50% or more.
- the fluorescence quantum yield of the quantum dot can be increased.
- the fluorescence wavelength can be freely controlled to about 410 nm or more and 470 nm or less.
- the quantum dot 1 in the present embodiment is a solid solution based on ZnSe using a chalcogen element other than zinc.
- the fluorescence wavelength is preferably 410 nm or more, and more preferably 430 nm or more.
- the fluorescence wavelength is preferably 440 nm or more, more preferably 470 nm or less, and still more preferably 460 nm or less.
- the quantum dot 1 shown in FIG. 1B is a core-shell structure having a core 1a and a shell 1b coated on the surface of the core 1a. As shown in FIG. 1B, it is preferable that a large number of organic ligands 2 are coordinated to the surface of the quantum dot 1. Moreover, the fluorescence half width of the quantum dot 1 shown to FIG. 1B is 25 nm or less.
- the core 1a of the quantum dot 1 shown in FIG. 1B is a nanocrystal shown in FIG. 1A. Therefore, the core 1a is preferably formed of ZnSe or ZnSeS.
- the shell 1b does not contain cadmium (Cd) as the core 1a does.
- the shell 1 b is made of, for example, zinc sulfide (ZnS) or the like, although the material is not particularly limited.
- the shell 1 b may be in a solid solution state on the surface of the core 1 a. Although the boundary between the core 1a and the shell 1b is shown by a dotted line in FIG. 1B, this indicates that the boundary between the core 1a and the shell 1b may or may not be confirmed by analysis. In the present embodiment, only the ZnSe core has a feature of emitting fluorescence.
- the quantum dot 1 shown in FIG. 1B can freely control the fluorescence wavelength to about 410 nm or more and 470 nm or less. And in this embodiment, it is possible to control the fluorescence wavelength to blue.
- a copper chalcogenide (precursor) is synthesized from an organic copper compound or an inorganic copper compound and an organic chalcogen compound.
- the precursor is preferably copper selenide: Cu 2 Se or copper selenide sulfide: Cu 2 SeS.
- selenium uses an organic selenium compound (organic chalcogenide) as a raw material.
- organic selenium compound organic chalcogenide
- a solution in which selenium is dissolved at a high temperature in a high boiling point solvent which is a long chain hydrocarbon such as octadecene (Se-DDT / OLAm) or a solution in which a mixture of oleylamine and dodecanethiol is used Etc. can be used.
- a high boiling point solvent which is a long chain hydrocarbon such as octadecene (Se-DDT / OLAm) or a solution in which a mixture of oleylamine and dodecanethiol is used Etc.
- the organic copper compound or the inorganic copper compound and the organic chalcogen compound are mixed and dissolved.
- octadecene can be used as a high boiling point saturated hydrocarbon or unsaturated hydrocarbon.
- t-butylbenzene t-butylbenzene as an aromatic high-boiling solvent
- butyl butyrate C 4 H 9 COOC 4 H 9
- a benzyl butyrate C 6 as a high-boiling ester solvent
- H 5 CH 2 COOC 4 H 9 or the like but it is also possible to use an aliphatic amine type or fatty acid type compound, an aliphatic phosphorus type compound, or a mixture of these as a solvent.
- the reaction temperature is set in the range of 140 ° C. or more and 250 ° C. or less to synthesize copper chalcogenide (precursor).
- the reaction temperature is preferably 140 ° C. or more and 220 ° C. or less at a lower temperature, and more preferably 140 ° C. or more and 200 ° C. or less at a low temperature.
- reaction method is not particularly limited, it is important to synthesize Cu 2 Se and Cu 2 SeS having uniform particle sizes in order to obtain a quantum dot having a narrow half width.
- thiol for example, octadecanethiol: C 18 H 37 SH, hexanedecanethiol: C 16 H 33 SH, tetradecanethiol: C 14 H 29 SH, dodecanethiol: C 12 H 25 SH, decanethiol C 10 H 21 SH, octanethiol: C 8 H 17 SH, etc.
- organic zinc compound or an inorganic zinc compound is prepared as a raw material of ZnSe or ZnSeS.
- Organic zinc compounds and inorganic zinc compounds are raw materials that are stable in the air and easy to handle.
- the structures of the organic zinc compound and the inorganic zinc compound are not particularly limited, it is preferable to use a highly ionic zinc compound in order to efficiently carry out the transmetallation reaction.
- the following organozinc compounds and inorganic zinc compounds can be used.
- the above-described organozinc compound or inorganic zinc compound is added to the reaction solution in which the precursor of copper chalcogenide is synthesized.
- This causes a transmetallation reaction between copper (Cu) of copper chalcogenide and zinc (Zn). It is preferable to cause the metal exchange reaction to occur at 180 ° C. or more and 280 ° C. or less. Furthermore, it is more preferable to cause the transmetallation reaction to occur at a lower temperature of 180 ° C. or more and 250 ° C. or less.
- the transmetallation reaction between Cu and Zn proceed quantitatively, and the nanocrystal does not contain the precursor Cu. If the precursor Cu remains, Cu acts as a dopant, and light is emitted by another light emission mechanism to expand the half width. 100 ppm or less is preferable, as for the residual amount of this Cu, 50 ppm or less is more preferable, and 10 ppm or less is ideal.
- Compounds having the above-mentioned role include ligands that can be complexed with Cu.
- ligands that can be complexed with Cu.
- phosphorus-based ligands, amine-based ligands, and sulfur-based ligands are preferable, and among them, phosphorus-based ligands are more preferable because of their high efficiency.
- a copper chalcogenide is synthesized as a precursor from an organic copper compound or an inorganic copper compound and an organic chalcogen compound, and a quantum dot is synthesized by performing metal exchange using the precursor.
- the quantum dots are synthesized through the synthesis of the precursor and not directly synthesized.
- the precursor copper chalcogenide may be isolated and purified once and then used.
- the synthesized quantum dots exhibit fluorescence characteristics without performing various treatments such as washing, isolation and purification, coating treatment, and ligand exchange.
- the fluorescence quantum yield can be further increased by covering the core 1a made of nanocrystals such as ZnSe or ZnSeS with the shell 1b.
- the precursor copper chalcogenide is Cu 2 Se / Cu 2 S. It is possible to synthesize this by continuously adding the S raw material in one reaction vessel and subsequently performing Zn—Zn transformation to obtain ZnSe / ZnS.
- the S raw material used for the shell structure is not particularly limited, but the following raw materials can be mentioned as typical ones.
- the application of the quantum dot 1 shown in FIGS. 1A and 1B is not particularly limited, for example, the quantum dot 1 of the present embodiment emitting blue fluorescence, a wavelength conversion member, an illumination member, a backlight device, and a display It is applicable to an apparatus etc.
- the quantum dot 1 of the present embodiment is applied to a part of a wavelength conversion member, an illumination member, a backlight device, a display device, etc. and, for example, photoluminescence (PL) is adopted as a light emission principle
- UV radiation makes it possible to emit blue fluorescence.
- EL electroluminescence
- white light can be emitted by using a light emitting element (full color LED) including the quantum dots 1 of the present embodiment emitting blue fluorescence together with the quantum dots emitting green fluorescence and the quantum dots emitting red fluorescence. It will be possible.
- a light emitting element full color LED
- the wavelength conversion member is formed in a sheet form, a film form or a molded body.
- a molded body in which quantum dots are dispersed in resin is accommodated in a container having an accommodation space by press-fitting or the like.
- the refractive index of the molded body is preferably smaller than the refractive index of the container.
- part of the light entering the molded body is totally reflected by the inner wall of the container. Therefore, the beam of light leaking to the outside from the side of the container can be reduced.
- the quantum dots having a narrow fluorescent half width in the present embodiment to the wavelength conversion member, the illumination member, the backlight device, the display device, and the like, the light emission characteristics can be effectively improved.
- ⁇ Raw material> the following raw materials were used to synthesize a cadmium-free quantum dot.
- Solvent Octadecene Aldrich Co., Ltd., Idemitsu Kosan Co., Ltd.
- Oleylamine Kao Co., Ltd .: Pharmin Oleic acid: Kao Co., Ltd .: Lucac O-V
- Trioctyl phosphine manufactured by Hokuko Chemical Co., Ltd.
- Zinc chloride manufactured by Aldrich Co., Ltd. or manufactured by Kishida Chemical Co., Ltd.
- Zinc iodide manufactured by Aldrich Co.
- Zinc acetate dihydrate manufactured by Ikoma Chemical Co., Ltd.
- Example 1 In a 100 mL reaction vessel, 131 mg of acetylacetonato copper: Cu (acac) 2 , 1.5 mL of dodecanethiol: DDT, 4.75 mL of oleylamine: OLAm, and 6.25 mL of octadecene: ODE were placed. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- N 2 inert gas
- Ethanol was added to the Cu 2 Se reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- Ethanol was added to the ZnSe (S) reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 2, an optical characteristic having a fluorescence wavelength of about 446.0 nm and a fluorescence half width of about 16.6 nm was obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 30.6%.
- Example 2 In a 100 mL reaction vessel, 36.3 mg of anhydrous copper acetate: Cu (OAc) 2 , 0.3 mL of dodecanethiol: DDT, 0.4 mL of a Se-DDT / OLAm solution (0.5 M), and 10 mL of octadecene: ODE are placed. The Then, it was heated with stirring at 220 ° C. for 10 minutes under an inert gas (N 2 ) atmosphere. The resulting reaction solution (Cu 2 Se (S)) was cooled to room temperature.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 3, an optical characteristic having a fluorescence wavelength of about 445.5 nm and a fluorescence half width of about 23.0 nm was obtained.
- Example 3 In a 100 mL reaction vessel, 131 mg of acetylacetonato copper: Cu (acac) 2 , 1.5 mL of dodecanethiol: DDT, 4.75 mL of oleylamine: OLAm, and 6.25 mL of octadecene: ODE were placed. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- N 2 inert gas
- Ethanol was added to the Cu 2 SeS reaction solution to generate a precipitate, which was centrifuged to recover the precipitate, and the precipitate was dispersed by adding TOP.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 4, an optical characteristic having a fluorescence wavelength of about 454.0 nm and a fluorescence half width of about 19.7 nm was obtained.
- Example 4 In a 100 mL reaction vessel, copper oleate octadecene solution (0.2 M): Cu (OLAc) 2 -ODE 1.2 mL, Se-ODE solution 3 mL, solution dodecanethiol: DDT 0.4 mL, octadecene: ODE 3 mL Put. The solution was heated with stirring at 200 ° C. for 60 minutes. The resulting reaction solution (Cu 2 SeS) was cooled to room temperature.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 5, optical characteristics having a fluorescence wavelength of about 434.0 nm and a fluorescence half width of about 23.5 nm were obtained.
- Example 5 In a 300 mL reaction vessel, 543 mg of anhydrous copper acetate: Cu (OAc) 2 , 9 mL of dodecanethiol: DDT, 28.5 mL of oleylamine: OLAm, and 37.5 mL of octadecene: ODE were placed. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- N 2 inert gas
- Ethanol was added to the Cu 2 Se (S) reaction solution to generate a precipitate, which was centrifuged to recover the precipitate, and the precipitate was dispersed by adding ODE.
- Ethanol was added to the ZnSe (S) reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- Ethanol was added to the ZnSe (S) reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 6, an optical characteristic having a fluorescence wavelength of about 445.5 nm and a fluorescence half width of about 13.3 nm was obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 52%.
- Example 6 In a 300 mL reaction vessel, 543 mg of anhydrous copper acetate: Cu (OAc) 2 , 9 mL of dodecanethiol: DDT, 9 mL of oleylamine: OLAm, and 57 mL of octadecene: ODE were placed. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- N 2 inert gas
- Ethanol was added to the ZnSe (S) reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 7, an optical characteristic having a fluorescence wavelength of about 436.0 nm and a fluorescence half width of about 15.2 nm was obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 66%.
- Example 7 In a 300 mL reaction vessel, 546 mg of anhydrous copper acetate: Cu (OAc) 2 , 9 mL of dodecanethiol: DDT, 9 mL of oleylamine: OLAm, and 57 mL of octadecene: ODE were placed. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- N 2 inert gas
- Ethanol was added to the Cu 2 Se reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- Ethanol was added to the ZnSe (S) reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- Ethanol was added to the ZnSe (S) reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 8, an optical characteristic having a fluorescence wavelength of about 432.0 nm and a fluorescence half width of about 15.3 nm was obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 70%.
- Example 8 In a 100 mL reaction vessel, 72.6 mg of anhydrous copper acetate: Cu (OAc) 2, 0.263 mL of oleylamine OLAm, and 10 mL of octadecene: ODE were placed. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- Ethanol was added to the ZnSe reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 9, an optical characteristic having a fluorescence wavelength of about 425.5 nm and a fluorescence half width of about 22.1 nm was obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 63%.
- Example 9 In a 100 mL reaction vessel, 182 mg of anhydrous copper acetate: Cu (OAc) 2 , 3 mL of dodecanethiol: DDT, 9.5 mL of oleylamine: OLAm, and 12.5 mL of octadecene: ODE were placed. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- N 2 inert gas
- Ethanol was added to the ZnSe (S) reaction solution to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, as shown in FIG. 10, optical characteristics having a fluorescence wavelength of about 452.5 nm and a fluorescence half width of about 16.2 nm were obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 25%.
- Example 10 Into the reaction solution of Example 6, 0.6 mL of dodecylamine: DDA was added, and heated with stirring at 220 ° C. for 5 minutes under an inert gas (N 2 ) atmosphere.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 436.0 nm and a half width of fluorescence of about 14.7 nm were obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 58%.
- Example 11 In 100 mL of the reaction solution of Example 6, 1 mL of dodecylamine: DDA was added, and heated with stirring at 220 ° C. for 5 minutes under an inert gas (N 2 ) atmosphere.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 436.0 nm and a half width of fluorescence of about 15.1 nm were obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 48%.
- Example 12-1 Ethanol was added to 10 mL of the reaction solution of Example 5 to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the obtained hexane dispersion solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 445.5 nm and a fluorescence half width of about 22.5 nm were obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 3%.
- Example 12-2 Ethanol was added to 12.5 mL of the reaction solution of Example 6 to generate a precipitate, which was centrifuged to recover the precipitate, and the precipitate was dispersed by adding ODE.
- the obtained hexane dispersion solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 431.0 nm and a fluorescence half width of about 18.0 nm were obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 9%.
- Example 12-3 Ethanol was added to 10 mL of the reaction solution of Example 7 to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the obtained hexane dispersion solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 432.0 nm and a fluorescence half width of about 21.0 nm were obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 23%.
- Example 13 Ethanol was added to 10 mL of the reaction solution of Example 7 to generate a precipitate, which was centrifuged to collect the precipitate, and the precipitate was dispersed by adding ODE.
- the solution was heated with stirring at 280 ° C. for 3 minutes under an inert gas (N 2 ) atmosphere.
- the obtained hexane dispersion solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 430.0 nm and a half width of fluorescence of about 16.0 nm were obtained.
- the resulting reaction solution was measured by a quantum efficiency measurement system. As a result, the quantum yield was about 54%.
- Comparative Example 1 In a 100 mL reaction vessel, 0.833 mL of zinc oleate: Zn (OLAc) 2 -ODE solution (0.4 M) and 10 mL of Se-ODE solution (0.1 M) are placed under an inert gas (N 2 ) atmosphere, Heated with stirring at 280 ° C. for 35 minutes.
- Zn (OLAc) 2 -ODE solution 0.4 M
- Se-ODE solution 10 mL
- N 2 inert gas
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 459.0 nm and a fluorescence half width of about 45.2 nm were obtained.
- Comparative Example 2 A 100 mL reaction vessel was charged with 20 mL of a Se-ODE solution (0.1 M) and heated with stirring at 260 ° C. for 3 minutes under an inert gas (N 2 ) atmosphere.
- a Se-ODE solution 0.1 M
- N 2 inert gas
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, an optical characteristic having a fluorescence wavelength of about 461.0 nm and a fluorescence half width of about 65.8 nm was obtained.
- Example 14 In a 100 mL reaction vessel, 183 mg of anhydrous copper acetate: Cu (OAc) 2 , 0.66 mL of oleylamine: OLAm, 0.64 mL of octanoic acid, and 8.7 mL of octadecene: ODE. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- N 2 inert gas
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 406.5 nm and a fluorescence half width of about 20.8 nm were obtained.
- Example 15 A 100 mL reaction vessel was charged with 141 mg of zinc octanoate and 20 mL of octadecene: ODE. Then, the raw material was dissolved by heating while stirring under an inert gas (N 2 ) atmosphere.
- the resulting reaction solution was measured by a fluorescence spectrometer. As a result, optical characteristics having a fluorescence wavelength of about 415.0 nm and a fluorescence half width of about 22.5 nm were obtained.
- the full width at half maximum was 25 nm or less. Moreover, it turned out that it can be 20 nm or less and, further, can be controlled to 17 nm or less.
- FIG. 11 is a measurement result of a scanning electron microscope (SEM)
- FIG. 12 is a measurement result of X-ray diffraction (XRD).
- quantum dots emitting blue fluorescence can be stably obtained.
- quantum dot of the present invention By applying the quantum dot of the present invention to an LED, a backlight device, a display device, and the like, excellent light emission characteristics can be obtained in each device.
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Abstract
Description
脂肪族1級アミン系、オレイルアミン:C18H35NH2、ステアリル(オクタデシル)アミン:C18H37NH2、ドデシル(ラウリル)アミン:C12H25NH2、デシルアミン:C10H21NH2、オクチルアミン:C8H17NH2
脂肪酸、オレイン酸:C17H33COOH、ステアリン酸:C17H35COOH、パルミチン酸:C15H31COOH、ミリスチン酸:C13H27COOH、ラウリル(ドデカン)酸:C11H23COOH、デカン酸:C9H19COOH、オクタン酸:C7H15COOH
チオール系、オクタデカンチオール:C18H37SH、ヘキサンデカンチオール:C16H33SH、テトラデカンチオール:C14H29SH、ドデカンチオール:C12H25SH、デカンチオール:C10H21SH、オクタンチオール:C8H17SH
ホスフィン系、トリオクチルホスフィン:(C8H17)3P、トリフェニルホスフィン:(C6H5)3P、トリブチルホスフィン:(C4H9)3P
ホスフィンオキシド系、トリオクチルホスフィンオキシド:(C8H17)3P=O、トリフェニルホスフィンオキシド:(C6H5)3P=O、トリブチルホスフィンオキシド:(C4H9)3P=O
本発明では、カドミウムを含まない量子ドットを合成するにあたり以下の原料を用いた。
溶媒
オクタデセン:Aldrich株式会社製、出光興産株式会社製
オレイルアミン:花王株式会社製:ファーミン
オレイン酸:花王株式会社製:ルナックO-V
トリオクチルホスフィン:北興化学株式会社製
塩化亜鉛:Aldrich株式会社製、又はキシダ化学株式会社製
ヨウ化亜鉛:Aldrich株式会社製
酢酸亜鉛2水和物:生駒化学株式会社製
無水酢酸亜鉛:Aldrich株式会社製
セレン(4N:99.99%):新興化学株式会社製、又はAldrich株式会社製
硫黄:キシダ化学株式会社製
<測定機器>
蛍光分光計:日本分光株式会社製 F-2700
紫外-可視光分光光度計:日立株式会社製 V-770
量子収率測定装置:大塚電子株式会社製 QE-1100
X線回折装置(XRD):Bruker社製 D2 PHASER
走査線電子顕微鏡(SEM):日立株式会社製 SU9000
100mL反応容器に、アセチルアセトナト銅:Cu(acac)2 131mgと、ドデカンチオール:DDT 1.5mLと、オレイルアミン:OLAm 4.75mLと、オクタデセン:ODE 6.25mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、無水酢酸銅:Cu(OAc)2 36.3mgと、ドデカンチオール:DDT 0.3mLと、Se-DDT/OLAm溶液(0.5M)0.4mLと、オクタデセン:ODE 10mLを入れた。そして、不活性ガス(N2)雰囲気下、220℃で10分間、攪拌しつつ加熱した。得られた反応溶液(Cu2Se(S))を、室温まで冷却した。
100mL反応容器に、アセチルアセトナト銅:Cu(acac)2 131mgと、ドデカンチオール:DDT 1.5mLと、オレイルアミン:OLAm 4.75mLと、オクタデセン:ODE 6.25mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、オレイン酸銅のオクタデセン溶液(0.2M):Cu(OLAc)2-ODE 1.2mLと、Se-ODE溶液 3mLと、溶液ドデカンチオール:DDT 0.4mLと、オクタデセン:ODE 3mLを入れた。この溶液を200℃で60分間、攪拌しつつ加熱した。得られた反応溶液(Cu2SeS)を、室温まで冷却した。
300mL反応容器に、無水酢酸銅:Cu(OAc)2 543mgと、ドデカンチオール:DDT 9mLと、オレイルアミン:OLAm 28.5mLと、オクタデセン:ODE 37.5mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
300mL反応容器に、無水酢酸銅:Cu(OAc)2 543mgと、ドデカンチオール:DDT 9mLと、オレイルアミン:OLAm 9mLと、オクタデセン:ODE 57mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
300mL反応容器に、無水酢酸銅:Cu(OAc)2 546mgと、ドデカンチオール:DDT 9mLと、オレイルアミン:OLAm 9mLと、オクタデセン:ODE 57mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、無水酢酸銅:Cu(OAc)2 72.6mgと、オレイルアミン:OLAm 0.263mLと、オクタデセン:ODE 10mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、無水酢酸銅:Cu(OAc)2 182mgと、ドデカンチオール:DDT 3mLと、オレイルアミン:OLAm 9.5mLと、オクタデセン:ODE 12.5mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
実施例6の反応溶液に、ドデシルアミン:DDA 0.6mLを入れ、不活性ガス(N2)雰囲気下にて、220℃で5分間、攪拌しつつ加熱した。
実施例6の反応溶液100mLに、ドデシルアミン:DDA 1mLを入れ、不活性ガス(N2)雰囲気下にて、220℃で5分間、攪拌しつつ加熱した。
実施例5の反応溶液10mLに、エタノールを加え沈殿を発生させ、遠心分離を施して沈殿を回収し、その沈殿にODEを加えて分散させた。
実施例6の反応溶液12.5mLに、エタノールを加え沈殿を発生させ、遠心分離を施して沈殿を回収し、その沈殿にODEを加えて分散させた。
実施例7の反応溶液10mLに、エタノールを加え沈殿を発生させ、遠心分離を施して沈殿を回収し、その沈殿にODEを加えて分散させた。
実施例7の反応溶液10mLに、エタノールを加え沈殿を発生させ、遠心分離を施して沈殿を回収し、その沈殿にODEを加えて分散させた。
100mL反応容器に、オレイン酸亜鉛:Zn(OLAc)2-ODE溶液(0.4M)0.833mLと、Se-ODE溶液(0.1M)10mLを入れ、不活性ガス(N2)雰囲気下、280℃で35分間攪拌しつつ加熱した。
100mL反応容器に、Se-ODE溶液(0.1M)20mLを入れ、不活性ガス(N2)雰囲気下、260℃で3分間攪拌しつつ加熱した。
100mL反応容器に、無水酢酸銅:Cu(OAc)2 183mgと、オレイルアミン:OLAm 0.66mLと、オクタン酸 0.64mL、オクタデセン:ODE 8.7mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
100mL反応容器に、オクタン酸亜鉛:141mgと、オクタデセン:ODE 20mLを入れた。そして、不活性ガス(N2)雰囲気下で攪拌しながら加熱し、原料を溶解させた。
Claims (15)
- カドミウムを含まず、蛍光半値幅が、25nm以下であることを特徴とする量子ドット。
- 前記量子ドットは、亜鉛とセレン、或いは、亜鉛とセレンと硫黄とを含有するナノクリスタルであることを特徴とする請求項1に記載の量子ドット。
- 前記量子ドットは、前記ナノクリスタルをコアとし、前記コアの表面にシェルが被覆されたコアシェル構造を有することを特徴とする請求項2に記載の量子ドット。
- 蛍光波長が、410nm以上470nm以下の範囲であることを特徴とする請求項1から請求項3のいずれかに記載の量子ドット。
- 前記量子ドットの表面が配位子で覆われていることを特徴とする請求項1から請求項4のいずれかに記載の量子ドット。
- 前記配位子は、脂肪族アミン系、ホスフィン系、及び、脂肪族カルボン酸系の少なくともいずれか1種から選択されることを特徴とする請求項5に記載の量子ドット。
- 有機銅化合物、或いは、無機銅化合物と、有機カルコゲン化合物とから、前駆体としての銅カルコゲニドを合成し、銅カルコゲニド前駆体を用いて、カドミウムを含まない量子ドットを合成することを特徴とする量子ドットの製造方法。
- 前記銅カルゴゲニドからなる前駆体の銅と亜鉛とを金属交換することを特徴とする請求項7に記載の量子ドットの製造方法。
- 前記金属交換反応を、180℃以上280℃以下で行うことを特徴とする請求項8に記載の量子ドットの製造方法。
- 前記銅カルコゲニドを、140℃以上250℃以下の反応温度で合成することを特徴とする請求項7から請求項9のいずれかに記載の量子ドットの製造方法。
- 前記量子ドットは、亜鉛とセレン、或いは、亜鉛とセレンと硫黄とを含有するナノクリスタルであることを特徴とする請求項7から請求項10のいずれかに記載の量子ドットの製造方法。
- 請求項1から請求項6のいずれかに記載の量子ドット、或いは、請求項7ないし請求項11のいずれかに記載の量子ドットの製造方法で形成された量子ドットを含むことを特徴とする波長変換部材。
- 請求項1から請求項6のいずれかに記載の量子ドット、或いは、請求項7ないし請求項11のいずれかに記載の量子ドットの製造方法で形成された量子ドットを含むことを特徴とする照明部材。
- 請求項1から請求項6のいずれかに記載の量子ドット、或いは、請求項7ないし請求項11のいずれかに記載の量子ドットの製造方法で形成された量子ドットを含むことを特徴とするバックライト装置。
- 請求項1から請求項6のいずれかに記載の量子ドット、或いは、請求項7ないし請求項11のいずれかに記載の量子ドットの製造方法で形成された量子ドットを含むことを特徴とする表示装置。
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US17/405,687 Continuation US11845890B2 (en) | 2017-10-12 | 2021-08-18 | Quantum dot and method of producing the same; and wavelength converting member, lighting member, back light unit, and display device using quantum dot |
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WO2022003948A1 (ja) * | 2020-07-03 | 2022-01-06 | シャープ株式会社 | 量子ドット分散液及びそれを用いた電界発光素子の製造方法 |
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WO2022176088A1 (ja) * | 2021-02-18 | 2022-08-25 | シャープ株式会社 | 電界発光素子 |
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JP7273992B2 (ja) | 2019-12-02 | 2023-05-15 | 信越化学工業株式会社 | 量子ドット、波長変換材料、バックライトユニット、画像表示装置及び量子ドットの製造方法 |
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EP3696248A1 (en) | 2020-08-19 |
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JP7283733B2 (ja) | 2023-05-30 |
CN113583677A (zh) | 2021-11-02 |
AU2018348597A1 (en) | 2020-04-23 |
CN111201305B (zh) | 2021-07-16 |
TWI756032B (zh) | 2022-02-21 |
US20200347296A1 (en) | 2020-11-05 |
JP7473050B2 (ja) | 2024-04-23 |
JP2019081905A (ja) | 2019-05-30 |
US20210388263A1 (en) | 2021-12-16 |
KR102661236B1 (ko) | 2024-04-29 |
US11845890B2 (en) | 2023-12-19 |
CN111201305A (zh) | 2020-05-26 |
JP2023101543A (ja) | 2023-07-21 |
TW201923036A (zh) | 2019-06-16 |
US20240124774A1 (en) | 2024-04-18 |
TW202127684A (zh) | 2021-07-16 |
TWI720352B (zh) | 2021-03-01 |
KR20240058978A (ko) | 2024-05-07 |
US11124703B2 (en) | 2021-09-21 |
EP3696248A4 (en) | 2021-04-07 |
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