WO2010077226A1 - Methods for encapsulating nanocrystals and resulting compositions - Google Patents
Methods for encapsulating nanocrystals and resulting compositions Download PDFInfo
- Publication number
- WO2010077226A1 WO2010077226A1 PCT/US2008/014112 US2008014112W WO2010077226A1 WO 2010077226 A1 WO2010077226 A1 WO 2010077226A1 US 2008014112 W US2008014112 W US 2008014112W WO 2010077226 A1 WO2010077226 A1 WO 2010077226A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- disposing
- substrate
- composition
- hermetically sealed
- luminescent nanocrystals
- Prior art date
Links
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 218
- 239000000203 mixture Substances 0.000 title claims abstract description 178
- 238000000034 method Methods 0.000 title claims abstract description 109
- 238000007789 sealing Methods 0.000 claims abstract description 52
- 239000000758 substrate Substances 0.000 claims description 207
- 230000004888 barrier function Effects 0.000 claims description 63
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 47
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 36
- 239000004005 microsphere Substances 0.000 claims description 35
- 239000000565 sealant Substances 0.000 claims description 32
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims description 29
- 239000000377 silicon dioxide Substances 0.000 claims description 23
- 239000011258 core-shell material Substances 0.000 claims description 19
- 238000000231 atomic layer deposition Methods 0.000 claims description 17
- 239000011521 glass Substances 0.000 claims description 16
- 229910010272 inorganic material Inorganic materials 0.000 claims description 14
- 239000011147 inorganic material Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 229910052681 coesite Inorganic materials 0.000 claims description 13
- 229910052906 cristobalite Inorganic materials 0.000 claims description 13
- 229910052682 stishovite Inorganic materials 0.000 claims description 13
- 229910052905 tridymite Inorganic materials 0.000 claims description 13
- 238000004544 sputter deposition Methods 0.000 claims description 11
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- 238000005530 etching Methods 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 238000007650 screen-printing Methods 0.000 claims description 8
- 238000004020 luminiscence type Methods 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 75
- 239000000463 material Substances 0.000 description 35
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- 238000006243 chemical reaction Methods 0.000 description 10
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- 239000000178 monomer Substances 0.000 description 9
- 239000002114 nanocomposite Substances 0.000 description 9
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- 238000000576 coating method Methods 0.000 description 7
- 230000012010 growth Effects 0.000 description 7
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- 239000012495 reaction gas Substances 0.000 description 6
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- 230000015572 biosynthetic process Effects 0.000 description 5
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- 239000007789 gas Substances 0.000 description 5
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- 238000000926 separation method Methods 0.000 description 5
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- 229910017115 AlSb Inorganic materials 0.000 description 4
- 229910004613 CdTe Inorganic materials 0.000 description 4
- 229910002601 GaN Inorganic materials 0.000 description 4
- 229910005540 GaP Inorganic materials 0.000 description 4
- 229910005542 GaSb Inorganic materials 0.000 description 4
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 4
- 229910052581 Si3N4 Inorganic materials 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- -1 but not limited to Polymers 0.000 description 4
- 125000003700 epoxy group Chemical group 0.000 description 4
- 229910052809 inorganic oxide Inorganic materials 0.000 description 4
- 230000006911 nucleation Effects 0.000 description 4
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- 239000002904 solvent Substances 0.000 description 4
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- 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 description 3
- 229910005866 GeSe Inorganic materials 0.000 description 3
- 229910000673 Indium arsenide Inorganic materials 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
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- 229910052733 gallium Inorganic materials 0.000 description 3
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- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
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- 238000002156 mixing Methods 0.000 description 3
- 238000010422 painting Methods 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 239000004054 semiconductor nanocrystal Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
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- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910015894 BeTe Inorganic materials 0.000 description 2
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- 229910005900 GeTe Inorganic materials 0.000 description 2
- 229910004262 HgTe Inorganic materials 0.000 description 2
- GPXJNWSHGFTCBW-UHFFFAOYSA-N Indium phosphide Chemical compound [In]#P GPXJNWSHGFTCBW-UHFFFAOYSA-N 0.000 description 2
- 229910002665 PbTe Inorganic materials 0.000 description 2
- 229910005642 SnTe Inorganic materials 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 229910007709 ZnTe Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
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- 238000003486 chemical etching Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 229910052732 germanium Inorganic materials 0.000 description 2
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 150000004767 nitrides Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 230000000737 periodic effect Effects 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000009877 rendering Methods 0.000 description 2
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910052950 sphalerite Inorganic materials 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N zinc oxide Inorganic materials [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 229910052984 zinc sulfide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 206010073306 Exposure to radiation Diseases 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- 229920000106 Liquid crystal polymer Polymers 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical group [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- 229910003818 SiH2Cl2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
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- 230000003698 anagen phase Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000005315 distribution function Methods 0.000 description 1
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000008393 encapsulating agent Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004678 hydrides Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 238000007641 inkjet printing Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002074 nanoribbon Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000004792 oxidative damage Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000005240 physical vapour deposition Methods 0.000 description 1
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 1
- 229910052699 polonium Inorganic materials 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920006294 polydialkylsiloxane Polymers 0.000 description 1
- 239000013047 polymeric layer Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000003642 reactive oxygen metabolite Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical group [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 229910052716 thallium Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
- 150000003673 urethanes Chemical class 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C27/00—Joining pieces of glass to pieces of other inorganic material; Joining glass to glass other than by fusing
- C03C27/06—Joining glass to glass by processes other than fusing
- C03C27/10—Joining glass to glass by processes other than fusing with the aid of adhesive specially adapted for that purpose
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
- C09K11/025—Use of particular materials as binders, particle coatings or suspension media therefor non-luminescent particle coatings or suspension media
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
- C09K11/562—Chalcogenides
- C09K11/565—Chalcogenides with zinc cadmium
-
- 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
- C09K11/70—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing phosphorus
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/06—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising selenium or tellurium in uncombined form other than as impurities in semiconductor bodies of other materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02538—Group 13/15 materials
- H01L21/02543—Phosphides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/02557—Sulfides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02551—Group 12/16 materials
- H01L21/0256—Selenides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02587—Structure
- H01L21/0259—Microstructure
- H01L21/02601—Nanoparticles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0041—Processes relating to semiconductor body packages relating to wavelength conversion elements
Definitions
- the present invention relates to methods for hermetically sealing luminescent nanocrystals, and hermetically sealed nanocrystal compositions.
- the present invention also provides microspheres comprising luminescent nanocrystals as well as methods of making the microspheres.
- Luminescent nanocrystals when exposed to air and moisture undergo oxidative damage, often resulting in a loss of luminescence.
- the present invention provides methods and compositions for hermetically sealing luminescent nanocrystals.
- the compositions prepared according to the present invention can be applied to a variety of applications, and the methods allow for preparation of various shapes and configurations of hermetically sealed nanocrystal compositions.
- the present invention provides methods of hermetically sealing one or more compositions comprising a plurality of luminescent nanocrystals.
- a first substrate is provided, and one or more compositions comprising a plurality of luminescent nanocrystals are disposed onto the first substrate (for example, via screen printing).
- a second substrate is disposed on the first substrate so as to cover the compositions of luminescent nanocrystals. The first and second substrates are then sealed.
- the first and second substrates are glass substrates, and suitably, the substrates have one or more recesses formed therein.
- the first substrate further comprises a third substrate having one or more recesses formed therein.
- the luminescent nanocrystals for use in the practice of the present invention are core-shell luminescent nanocrystals, such as CdSe/ZnS, CdSe/CdS or InP/ZnS nanocrystals, and suitably are about 1-10 ran in size.
- the first and second substrates are sealed with a polymeric sealant, such as an epoxy sealant.
- a polymeric sealant such as an epoxy sealant.
- the luminescent nanocrystal compositions are cured prior to sealing.
- the compositions are separated from each other following the sealing of the first and second substrates.
- the methods of the present invention can further comprise disposing a barrier layer on the first and second substrates, such as an inorganic layer, for example a layer of SiO 2 , TiO 2 or AlO 2 .
- a barrier layer on the first and second substrates, such as an inorganic layer, for example a layer of SiO 2 , TiO 2 or AlO 2 .
- the barrier layers are suitably disposed by atomic layer deposition or sputtering.
- the methods of the present invention comprise forming one or more recesses in and/or on the first substrate.
- the one or more compositions comprising a plurality of luminescent nanocrystals are then disposed into the recesses, and the second substrate is disposed on the first substrate so as to cover the compositions of luminescent nanocrystals prior to sealing.
- the first substrate is etched so as to form one or more recesses.
- a third substrate having one or more recesses formed therein is disposed onto the first substrate.
- a third substrate is disposed onto the first substrate and one or more recesses are etched into the third substrate.
- third substrate is disposed onto the first substrate so as to form one or more recesses on the surface of the first substrate.
- the present invention also provides hermetically sealed compositions prepared by the various methods described throughout.
- the present invention provides microspheres.
- the microspheres comprise a central region, a first layer on an outer surface of the central region, the first layer comprising one or more luminescent nanocrystals, and a barrier layer on an outer surface of the first layer.
- the central region of the microspheres comprises silica
- the first layer comprises an inorganic material, such as silica or titania.
- the barrier layer comprises an inorganic layer, such as SiO 2 , TiO 2 or AlO 2 .
- the microspheres have a diameter of less than about 500 microns, suitably less than about 10 microns, more suitably less than about 1 micron.
- the present invention also provides method of forming microspheres.
- a particle comprising a first inorganic material is provided, and the particle is contacted with a composition comprising a precursor to a second inorganic material and one or more luminescent nanocrystals.
- a peripheral region is formed on an outer surface of the particle, the peripheral region comprising the second inorganic material and the luminescent nanocrystals.
- a barrier layer is disposed on an outer surface of the peripheral region.
- FIGs. IA- ID show a method of hermetically sealing luminescent nanocrystals in accordance with an embodiment of the present invention.
- FIG. IE shows a flowchart of a method of hermetically sealing luminescent nanocrystals in accordance with an embodiment of the present invention.
- FIGs. 2A-2G show a method of hermetically sealing luminescent nanocrystals in accordance with an embodiment of the present invention.
- FIGs. IA- ID show a method of hermetically sealing luminescent nanocrystals in accordance with an embodiment of the present invention.
- FIG. 4 shows a flowchart of a method of hermetically sealing luminescent nanocrystals in accordance with an embodiment of the present invention.
- FIG. 5 shows a microsphere in accordance with an embodiment of the present invention.
- FIG. 6 shows a flowchart of a method of preparing a microsphere in accordance with an embodiment of the present invention.
- the present invention provides various compositions comprising nanocrystals, including luminescent nanocrystals.
- the various properties of the luminescent nanocrystals can be tailored and adjusted for various applications.
- the term "nanocrystal” refers to nanostructures that are substantially monocrystalline.
- a nanocrystal has at least one region or characteristic dimension with a dimension of less than about 500 nm, and down to on the order of less than about 1 nm.
- “about” means a value of ⁇ 10% of the stated value (e.g.
- nanocrystals “about 100 nm” encompasses a range of sizes from 90 nm to 110 nm, inclusive).
- the present invention also encompasses the use of polycrystalline or amorphous nanocrystals.
- the term “nanocrystal” also encompasses " luminescent nanocrystals.”
- luminescent nanocrystals means nanocrystals that emit light when excited by an external energy source (suitably light).
- the nanocrystals are luminescent nanocrystals.
- Nanocrystals can be substantially homogenous in material properties, or in certain embodiments, can be heterogeneous.
- the optical properties of nanocrystals can be determined by their particle size, chemical or surface composition. The ability to tailor the luminescent nanocrystal size in the range between about 1 nm and about 15 run enables photoemission coverage in the entire optical spectrum to offer great versatility in color rendering. Particle encapsulation offers robustness against chemical and UV deteriorating agents.
- Nanocrystals, including luminescent nanocrystals, for use in the present invention can be produced using any method known to those skilled in the art. Suitable methods and exemplary nanocrystals are disclosed in Published U.S. Patent Application No. 2008/0237540; U.S. Patent 7,374,807; U.S. Patent Application No. 10/796,832, filed March 10, 2004; U.S. Patent No. 6,949,206; and U.S. Provisional Patent Application No. 60/578,236, filed June 8, 2004, the disclosures of each of which are incorporated by reference herein in their entireties.
- the nanocrystals for use in the present invention can be produced from any suitable material, including an inorganic material, and more suitably an.
- Suitable semiconductor materials include those disclosed in U.S. Patent Application No. 10/796,832, and include any type of semiconductor, including group II- VI, group IH-V, group IV-VI and group IV semiconductors.
- Suitable semiconductor materials include, but are not limited to, Si, Ge, Sn, Se, Te, B, C (including diamond), P, BN, BP, BAs, AlN, AlP, AlAs, AlSb, GaN, GaP, GaAs, GaSb, InN, InP, InAs, InSb, AlN, AlP, AlAs, AlSb, GaN, GaP, GaAs, GaSb, ZnO, ZnS, ZnSe, ZnTe, CdS, CdSe, CdTe, HgS, HgSe, HgTe, BeS, BeSe, BeTe, MgS, MgSe, GeS, GeSe, GeTe, SnS, Sn
- the semiconductor nanocrystals may comprise a dopant from the group consisting of: a p-type dopant or an n-type dopant.
- the nanocrystals useful in the present invention can also comprise II- VI or III-V semiconductors.
- II- VI or III-V semiconductor nanocrystals include any combination of an element from Group II, such as Zn, Cd and Hg, with any element from Group VI, such as S, Se, Te, Po, of the Periodic Table; and any combination of an element from Group III, such as B, Al, Ga, In, and Tl, with any element from Group V, such as N, P, As, Sb and Bi, of the Periodic Table.
- the nanocrystals, including luminescent nanocrystals, useful in the present invention can also further comprise ligands conjugated, cooperated, associated or attached to their surface as described throughout.
- Suitable ligands include any group known to those skilled in the art, including those disclosed in U.S. Patent 7,374,807, U.S. Patent 6,949,206 and U.S. Provisional Patent Application No. 60/578,236, the disclosures of each of which are incorporated herein by reference.
- Use of such ligands can enhance the ability of the nanocrystals to incorporate into various solvents and matrixes, including polymers.
- miscibility-enhancing ligands i.e., the ability to be mixed without separation
- nanocomposite refers to matrix materials comprising nanocrystals distributed or embedded therein.
- suitable matrix materials can be any material known to the ordinarily skilled artisan, including polymeric materials, organic and inorganic oxides.
- Nanocomposites of the present invention can be layers, encapsulants, coatings or films as described herein. It should be understood that in embodiments of the present invention where reference is made to a layer, polymeric layer, matrix, or nanocomposite, these terms are used interchangeably, and the embodiment so described is not limited to any one type of nanocomposite, but encompasses any matrix material or layer described herein or known in the art.
- Down-converting nanocomposites utilize the emission properties of luminescent nanocrystals that are tailored to absorb light of a particular wavelength and then emit at a second wavelength, thereby providing enhanced performance and efficiency of active sources (e.g., LEDs).
- active sources e.g., LEDs
- the present invention provides methods for hermetically sealing luminescent nanocrystals.
- Luminescent Nanocrystal Phosphors While any method known to the ordinarily skilled artisan can be used to create nanocrystal phosphors, suitably, a solution-phase colloidal method for controlled growth of inorganic nanomaterial phosphors is used. See Alivisatos, A.P., "Semiconductor clusters, nanocrystals, and quantum dots," Science 271:933 (1996); X. Peng, M. Schlamp, A. Kadavanich, A.P. Alivisatos, "Epitaxial growth of highly luminescent CdSe/CdS Core/Shell nanocrystals with photostability and electronic accessibility," J. Am. Chem. Soc. 30:7019-7029 (1997); and C.
- synthesis occurs as an initial nucleation event that takes place over seconds, followed by crystal growth at elevated temperature for several minutes.
- Parameters such as the temperature, types of surfactants present, precursor materials, and ratios of surfactants to monomers can be modified so as to change the nature and progress of the reaction.
- the temperature controls the structural phase of the nucleation event, rate of decomposition of precursors, and rate of growth.
- the organic surfactant molecules mediate both solubility and control of the nanocrystal shape.
- the ratio of surfactants to monomer, surfactants to each other, monomers to each other, and the individual concentrations of monomers strongly influence the kinetics of growth.
- CdSe is used as the nanocrystal material, in one example, for visible light down-conversion, due to the relative maturity of the synthesis of this material. Due to the use of a generic surface chemistry, it is also possible to substitute non-cadmium-containing nanocrystals.
- the shell material can be chosen such that the electronic levels are type I with respect to the core material (e.g., with a larger bandgap to provide a potential step localizing the electron and hole to the core). As a result, the probability of non-radiative recombination can be reduced.
- Core-shell structures are obtained by adding organometallic precursors containing the shell materials to a reaction mixture containing the core nanocrystal.
- the cores act as the nuclei, and the shells grow from their surface.
- the temperature of the reaction is kept low to favor the addition of shell material monomers to the core surface, while preventing independent nucleation of nanocrystals of the shell materials.
- Surfactants in the reaction mixture are present to direct the controlled growth of shell material and ensure solubility.
- a uniform and epitaxially grown shell is obtained when there is a low lattice mismatch between the two materials.
- the spherical shape acts to minimize interfacial strain energy from the large radius of curvature, thereby preventing the formation of dislocations that could degrade the optical properties of the nanocrystal system.
- Exemplary materials for preparing core-shell luminescent nanocrystals include, but are not limited to, Si, Ge, Sn, Se, Te, B, C (including diamond), P, Co, Au, BN, BP, BAs, AlN, AlP, AlAs, AlSb, GaN, GaP, GaAs, GaSb, InN, InP, InAs, InSb, AlN, AlP, AlAs, AlSb, GaN, GaP, GaAs, GaSb, ZnO, ZnS, ZnSe, ZnTe, CdS, CdSe, CdTe, HgS, HgSe, HgTe, BeS, BeSe, BeTe, MgS, MgSe, GeS, GeSe, GeTe, SnS, SnSe, SnTe, PbO, PbS, PbSe, PbTe, CuF, CuCl, CuBr, CuI,
- Exemplary core-shell luminescent nanocrystals for use in the practice of the present invention include, but are not limited to, (represented as Core/Shell), CdSe/ZnS, InP/ZnS, PbSe/PbS, CdSe/CdS, CdTe/CdS, CdTe/ZnS, as well as others.
- the present invention provides methods of hermetically sealing one or more compositions comprising a plurality of luminescent nanocrystals.
- the methods comprise providing a first substrate 102 in step 122.
- one or more compositions 104 comprising a plurality of luminescent nanocrystals 106 are disposed onto the first substrate 102.
- a second substrate 108 is disposed on the first substrate so as to cover the compositions 104 of luminescent nanocrystals 106 as in FIG. IB.
- the first and second substrates are then sealed.
- “hermetically sealed” are used to indicate that the compositions of luminescent nanocrystals are prepared in such a way that the quantity of gases (e.g., air) or moisture that passes through or penetrates the container or composition, and/or that contacts the luminescent nanocrystals is reduced to a level where it does not substantially effect the performance of the nanocrystals (e.g., their luminescence).
- gases e.g., air
- a “hermetically sealed composition,” for example one that comprises luminescent nanocrystals, is a composition that does not allow an amount of air (or other gas, liquid or moisture) to penetrate the composition and contact the luminescent nanocrystals such that the performance of the nanocrystals (e.g., the luminescence) is substantially effected or impacted (e.g., reduced).
- a plurality of luminescent nanocrystals means more than one nanocrystal (i.e., 2, 3, 4, 5, 10, 100, 1,000, 1,000,000, etc., nanocrystals).
- the compositions will suitably comprise luminescent nanocrystals having the same composition, though in further embodiments, the plurality of luminescent nanocrystals can be various different compositions.
- the luminescent nanocrystals can all emit at the same wavelength, or in further embodiments, the compositions can comprise luminescent nanocrystals that emit at different wavelengths.
- Suitable matrixes for use in the compositions of the present invention include polymers and organic or inorganic oxides.
- Suitable polymers for use in the matrixes of the present invention include any polymer known to the ordinarily skilled artisan that can be used for such a purpose.
- the polymer is substantially translucent, transparent, or substantially transparent.
- Such polymers include, but are not limited to, poly( vinyl butyral):poly( vinyl acetate); epoxies; urethanes; silicone and derivatives of silicone, including, but not limited to, polyphenylmethylsiloxane, polyphenylalkylsiloxane, polydiphenylsiloxane, polydialkylsiloxane, fluorinated silicones and vinyl and hydride substituted silicones; acrylic polymers and copolymers formed from monomers including but not limited to, methylmethacrylate, butylmethacrylate and laurylmethacrylate; styrene based polymers; and polymers that are crosslinked with difunctional monomers, such as divinylbenzene.
- silicone and derivatives of silicone including, but not limited to, polyphenylmethylsiloxane, polyphenylalkylsiloxane, polydiphenylsiloxane, polydialkylsiloxane, fluorinated
- the luminescent nanocrystals used the present invention can be embedded in a polymeric (or other suitable material, e.g., waxes, oils) matrix using any suitable method, for example, mixing the nanocrystals in a polymer and casting a film, mixing the nanocrystals with monomers and polymerizing them together, mixing the nanocrystals in a sol-gel to form an oxide, or any other method known to those skilled in the art.
- the term "embedded” is used to indicate that the luminescent nanocrystals are enclosed or encased within the polymer that makes up the majority component of the matrix. It should be noted that luminescent nanocrystals are suitably uniformly distributed throughout the matrix, though in further embodiments they can be distributed according to an application-specific uniformity distribution function.
- first substrate 102 and second substrate 102 are exemplary embodiments.
- first and second substrate comprise glass, though in other embodiments, one of the substrates can be glass and the other a polymeric material, or both can be polymeric materials.
- first substrate 102 is of a size such that more than one composition 104 of luminescent nanocrystals 106 can be disposed thereon.
- a single composition 104 comprising a plurality of luminescent nanocrystals 106 be disposed on a first substrate, and if desired, a plurality of first substrates can then be used to prepare multiple hermetically sealed compositions.
- the thickness of first substrate 102 is suitably on the order of about 1 ⁇ m to about 1 cm, suitably about 100 ⁇ m to about 100 mm.
- First and second substrates are suitably the same size, though in other embodiments, they can be different sizes, so long as the compositions are sealed by the substrates.
- first and second substrates are on the order of millimeters to meters in at least one lateral dimension (i.e., in the plane of the substrate).
- first substrate 102 that is transparent, translucent or semi- transparent, allows light to pass through substrate and contact the luminescent nanocrystals disposed thereon.
- the thickness and size (e.g., area of coverage) of the compositions 104 of the present invention that are disposed on the first substrate 102 can be controlled by any method known in the art, such as spin-coating, screen printing, dip-coating, painting, spraying, etc.
- the luminescent nanocrystal compositions of the present invention can be any desirable size, shape, configuration and thickness.
- the compositions can be disposed on the first substrate in the form of layers, as well as other shapes, for example, discs, drops, spheres, cubes or blocks, tubular configurations and the like.
- compositions of the present invention can be any required or desired thickness, suitably, the compositions are on the order of about 1 ⁇ m to about 500 ⁇ m in thickness (i.e., in one dimension).
- the compositions have at least one lateral dimension (i.e., in the plane of the substrate) that is in the range of about a few microns to centimeters.
- the luminescent nanocrystals can be embedded or dispersed in the various compositions/matrixes at any loading ratio that is appropriate for the desired function.
- the luminescent nanocrystals are loaded at a ratio of between about 0.001% and about 75% by volume depending upon the application, matrix and type of nanocrystals used.
- the appropriate loading ratios can readily be determined by the ordinarily skilled artisan and are described herein further with regard to specific applications.
- the amount of nanocrystals loaded in a luminescent nanocrystal compositions are on the order of about 10% by volume, to parts-per-million (ppm) levels.
- Luminescent nanocrystals for use in the present invention will suitably be less than about 100 nm in size, and down to less than about 2 nm in size.
- the luminescent nanocrystals of the present invention absorb visible light.
- visible light is electromagnetic radiation with wavelengths between about 380 and about 780 nanometers that is visible to the human eye. Visible light can be separated into the various colors of the spectrum, such as red, orange, yellow, green, blue, indigo and violet.
- the photon-filtering nanocomposites of the present invention can be constructed so as to absorb light that makes up any one or more of these colors.
- the nanocomposites of the present invention can be constructed so as to absorb blue light, red light, or green light, combinations of such colors, or any colors in between.
- blue light comprises light between about 435 nm and about 500 nm
- green light comprises light between about 520 nm and 565 nm
- red light comprises light between about 625 nm and about 740 nm in wavelength.
- the ordinarily skilled artisan will be able to construct nanocomposites that can filter any combination of these wavelengths, or wavelengths between these colors, and such nanocomposites are embodied by the present invention.
- the luminescent nanocrystals have a size and a composition such that they absorb photons that are in the ultraviolet, near- infrared, and/or infrared spectra.
- the ultraviolet spectrum comprises light between about 100 nm to about 400 nm
- the near-infrared spectrum comprises light between about 750 nm to about 100 ⁇ m in wavelength
- the infrared spectrum comprises light between about 750 nm to about 300 ⁇ m in wavelength.
- the nanocrystals are ZnS, InAs or CdSe nanocrystals, or the nanocrystals comprise various combinations to form a population of nanocrystals for use in the practice of the present invention.
- the luminescent nanocrystals are core/shell nanocrystals, such as CdSe/ZnS, CdSe/CdS or InP/ZnS.
- compositions 104 of luminescent nanocrystals 106 suitably comprise a polymeric substrate or matrix.
- the present invention comprises methods of hermetically sealing compositions comprising luminescent nanocrystals, suitably polymeric substrates comprising luminescent nanocrystals, by sealing the compositions between a first and second substrates.
- compositions 104 allow for the formation of various shapes and configurations of the compositions, simply by molding, spreading, dropping, dispensing, spraying, layering, or otherwise manipulating the compositions into the desired shape/orientation.
- a solution/suspension of luminescent nanocrystals can be prepared (e.g., luminescent nanocrystals in a polymeric matrix). This solution can then be placed into any desired mold to form a required shape, or can simply be disposed in a shape, and then cured (e.g., cooled or heated depending upon the type of polymer) to form a solid or semi-solid structure.
- the compositions can be disposed in the shapes of disks or droplets.
- compositions 104 comprising luminescent nanocrystals 106 are disposed on substrate 102 in a high-throughput format, for example, by using screen printing, ink-jet printing, or other application technique that deposit a large number of individual samples onto a substrate.
- the sealing in step 128 of flowchart 120 comprises sealing with a polymeric sealant.
- Suitable polymeric sealants that can be used in the practice of the present invention are well known in the art, and are those which when dried or cured, are transparent, or at least semitransparent, or translucent.
- Exemplary polymeric sealants which can be utilized include, but are not limited to, silicones, epoxies, various rubbers, various acrylics, etc.
- the sealant should also be impermeable, or at least substantially impermeable, to air and moisture, so as to hermetically seal the first and second substrates.
- the first 102 and second 108 substrates are sealed by introducing sealant 110 to the first and second substrates, for example, by pouring, dipping, wicking, painting, injecting, etc., sealant 110, such that the sealant forms a seal 112 between the first and second substrates.
- sealant 110 for example, by pouring, dipping, wicking, painting, injecting, etc., sealant 110, such that the sealant forms a seal 112 between the first and second substrates.
- the luminescent nanocrystal composition is cured (e.g., via heating or cooling) prior to the sealing with the sealant.
- first substrate 102 suitably comprises one or more recesses 202 formed, at least one of, in and on, the substrate.
- a "recess” refers to a hole, indentation, well, crack, imperfection, or other depression in and/or on substrate 102.
- Forming the recesses, at least one of, in and on, means that the recesses are formed in and/or on, the substrate 102.
- a recess "on" first substrate 102 refers to a recess that is above the surface of first substrate 102, for example, a recess formed in a third substrate as described herein.
- a recess that is "in" first substrate 102 refers to a recess that penetrates into the surface of first substrate 102 to any depth.
- recesses can be formed both in and on the substrate in the same composition, or can be formed only in, or only on, the substrate 102.
- recesses in substrate 102 will not pass through the entire substrate, but instead have a depth into the substrate that is less than the entire thickness of the substrate, thereby providing a reservoir for receipt of compositions 104.
- the recesses 202 are on the order of about 0.5 mm to about 10 mm in at least one lateral dimension (a dimension in the plane of first substrate 102, e.g., diameter if a circular-shaped recess is utilized), more suitably about 1 mm to about 10 mm, about 1 mm to about 9 mm, about 1 mm to about 8 mm, about 1 mm to about 7 mm, about 1 mm to about 6 mm, about 1 mm to about 5 mm, about 1 mm to about 4 mm, about 1 mm to about 3 mm, about 1 mm to about 2 mm, or about 10 mm, about 9 mm, about 8 mm, about 7 mm, about 6 mm, about 5 mm, about 4 mm, about 3 mm, about 2 mm, or about 1 mm, in at least one lateral dimension.
- Recesses will suitably be separated by sections of substrate 102 (or other materials as described herein) so that they are on the order of about 0.1 mm to about 10 mm apart (edge-to-edge separation).
- recesses 202 are separated by distances of about 1 mm to about 10 mm, 1 about 1 mm to about 9 mm, about 1 mm to about 8 mm, about 1 mm to about 7 mm, about 1 mm to about 6 mm, about 1 mm to about 5 mm, about 1 mm to about 4 mm, about 1 mm to about 3 mm, about 1 mm to about 2 mm, or about 10 mm, about 9 mm, about 8 mm, about 7 mm, about 6 mm, about 5 mm, about 4 mm, about 3 mm, about 2 mm, or about 1 mm.
- the depth of recesses 202 into the surface of substrate 102 is partially dictated by the thickness of substrate 102, though the depth suitably extends only a portion of the way into the surface of substrate 102.
- the depth of recesses 202 is on the order of about 100 ⁇ m to about 100 mm, suitably about 500 ⁇ m to about 10 mm. While in exemplary embodiments the depth of recesses 202 can be uniform across the recess, in other embodiments, the recess can have a sloping or non-inform depth.
- recesses 202 have a circular cross- section, in other embodiments, any shape can be used, e.g., rectangular, square, triangular, irregular, etc.
- first substrate 102 can further comprise a third substrate 204 that has one or more recesses 202 formed into the third substrate 204.
- the recesses in the third substrate will pass all the way through to the surface of first substrate 102 (in suitable embodiments, surface 102 may also have recesses therein), though in other embodiments, recesses 202 in third substrate 204 will not pass all the way through the third surface.
- recesses 204 can be in the form of cylinders (or other suitable shapes, e.g., rectangles, squares, irregular shapes, etc.).
- the thickness of third substrate is suitably on the order of about 100 ⁇ m to about 100 mm, suitably about 500 ⁇ m to about 10 mm, or about 500 ⁇ m to about 5 mm.
- third substrate 204 comprises a polymeric material, including a photoresistant materials.
- a photoresistant material allows for masking and etching to produce recesses 202 in the third substrate 204 (as described herein). Examples of methods of the use of photoresistant materials, as well as photoresist developers, can be found in, for example, Sze, S.M., "Semiconductor Devices, Physics and Technology," John Wiley & Sons, New York, pp. 436-442 (1985), the disclosure of which is incorporated by reference herein in its entirety.
- photoresists (such as negative photoresists) for use in the practice of the present invention comprise a polymer combined with a photosensitive compound.
- negative photoresist materials and developers include Kodak® 747, copolymer-ethyl acrylate and glycidylmethacrylate (COP), GeSe and poly(glycidyl methacrylate-co-ethyl acrylate) DCOPA.
- Disposing of negative photoresist material can be performed using any suitable method, for example, spin coating, spray coating, or otherwise layering the material.
- "positive photoresistant" materials become less chemically robust when exposed to radiation, and hence, work in the opposite manner to negative photoresistant materials.
- materials that are exposed to radiation will remain to generate the mask, while unexposed areas will be removed.
- compositions 104 comprising luminescent nanocrystals are disposed in the recesses 202.
- the recesses are filled such that there is no, or very little, gap between the top of the composition 104 and the surface of the substrate 102. This provides for a tight seal between the second substrate 108 and the first substrate 104, as shown in FIG. 2C-2E, when sealed with sealant 110, thereby providing hermetically sealed luminescent nanocrystals.
- a third substrate 204 comprising recesses 202 suitably the compositions 104 are disposed in the recesses so that there is no, or very little, gap between the top of the composition and the surface of the third substrate 102.
- the methods of the present invention can further comprise step 130, in which a barrier layer (not shown) is disposed on the surface of the first 102 and second substrates 108.
- a barrier layer is used to indicate a layer, coating, sealant or other material that is disposed on the first and second substrates.
- barrier layers provide an additional measure of hermetic sealing above and beyond the hermetic sealing provided by sealing of the first and second substrates.
- barrier layers include any material layer, coating or substance that can create an airtight seal on the substrates/compositions.
- Suitable barrier layers include inorganic layers, suitably an inorganic oxide such as an oxide of Al, Ba, Ca, Mg, Ni, Si, Ti or Zr.
- Exemplary inorganic oxide layers include SiO 2 , TiO 2 , AlO 2 and the like.
- the terms "dispose,” and "disposing" include any suitable method of application of a barrier layer. For example, disposing includes layering, coating, spraying, sputtering, plasma enhanced chemical vapor deposition, atomic layer deposition, or other suitable method of applying a barrier layer to the substrates/compositions.
- sputtering is used to dispose the barrier layer on the substrates/compositions.
- Sputtering comprises a physical vapor deposition process where high-energy ions are used to bombard elemental sources of material, which eject vapors of atoms that are then deposited in thin layers on a substrate. See for example, U.S. Patent Nos. 6,541,790; 6,107,105; and 5,667,650, the disclosures of each of which are incorporated by reference herein in their entireties.
- disposing the barrier layer can be carried out using atomic layer deposition.
- atomic layer deposition is used to dispose the barrier layer.
- Atomic layer deposition can comprise disposition of an oxide layer (e.g., TiO 2 , SiO 2 , AlO 2 , etc.) on the substrates/compositions, or in further embodiments, deposition of a non-conductive layer, such as a nitride (e.g., silicon nitride) can be used.
- ALD deposits an atomic layer (i.e., only a few molecules thick) by alternately supplying a reaction gas and a purging gas.
- a thin coating having a high aspect ratio, uniformity in a depression, and good electrical and physical properties, can be formed.
- Barrier layers deposited by the ALD method suitably have a low impurity density and a thickness of less than 1000 nm, suitably less than about 500 nm, less than about 200 nm, less than about 50 nm, less than about 20 nm, or less than about 5 nm.
- reaction gases A and B are used.
- A When only the reaction gas, A, flows into a reaction chamber, atoms of the reaction gas A are chemically adsorbed substrates/compositions. Then, any remaining reaction gas A is purged with an inert gas such as Ar or nitrogen. Then, reaction gas B flows in, wherein a chemical reaction between the reaction gases A and B occurs only on the surface of the substrates/compositions on which the reaction gas A has been adsorbed, resulting in an atomic barrier layer on the substrates/compositions.
- a non-conductive layer such as a nitride layer
- a nitride layer suitably SiH 2 Cl 2 and remote plasma enhanced NH 3 are used to dispose a silicon nitride layer. This can be performed at a low temperature and does not require the use of reactive oxygen species.
- ALD ALD-dielectric deposition
- the thickness of the barrier layer can be increased by repeating the deposition steps, thereby increasing the thickness of the layer in atomic layer units according to the number of repetitions.
- the barrier layer can be further coated with additional layers (e.g., via sputtering, CVD or ALD) to protect or further enhance the barrier.
- the ALD methods utilized in the practice of the present invention are performed at a temperature of below about 500°C, suitably below about 400°C, below about 300°C, or below about 200°C.
- Exemplary barrier materials include organic material designed to specifically reduce oxygen and moisture transmission. Examples include filled epoxies (such as alumina filled epoxies) as well as liquid crystalline polymers.
- the methods of the present invention suitably further comprise separating the one or more hermetically sealed compositions from each other following sealing of the substrate layers, as shown in FIGs. 3A-3C.
- This separation can be before or after the disposing of a barrier layer, though suitably the barrier layer, if utilized, is disposed after the separation.
- a hermetically sealed structure 302 comprising multiple, individually sealed compositions can be separated into sub-structures 304, or suitably further into individual structures 306, each comprising a single hermetically sealed composition, which in itself comprises a plurality of luminescent nanocrystals.
- preparation of a plurality of sealed compositions can lead to individual, separated compositions.
- Methods for separating the hermetically sealed compositions from each other include various methods well known in the art, such as via mechanical dicing (e.g., via knife, wedge, saw, blade, or other cutting device), via a laser, via water jet, etc.
- the present invention provides additional methods of hermetically sealing one or more compositions of luminescent nanocrystals.
- the methods comprise step 402, in which a first substrate 102 is provided.
- step 404 of flowchart 400 one or more recesses 202 are generated in and/or on the first substrate.
- step 406 of flowchart 400 one or more compositions 104 comprising a plurality of luminescent nanocrystals 106 are disposed into the recesses 204.
- step 408 a second substrate 108 is then disposed on the first substrate 102 so as to cover the compositions 104 of luminescent nanocrystals 106.
- step 410 of flowchart 400 the first and second substrates are then sealed 112.
- substrates 102 and 108 are transparent, semi-transparent or translucent substrates, such as polymer or glass substrates.
- substrates 102 and 108 are described throughout.
- Step 404 of flowchart 400 comprises generating one or more recesses
- recesses 202 are generated directly in the surface of first substrate 102. That is, material is removed from the surface of first substrate 102 so as to generate recesses 202.
- Methods for removing material from first substrate 102 include etching (e.g., chemical etching using various acids or other etchants, including those disclosed herein), gouging, cutting, whittling, drilling, etc.
- recesses 202 can be generated on first substrate 102.
- a third substrate 204 is suitably disposed on first substrate 102.
- Recesses 202 are then generated in the third substrate, for example, by etching (e.g., chemical etching using various acids), gouging, cutting, whittling, drilling, etc., into the substrate.
- a masking/etching method is used to generate recesses in the third substrate.
- recesses 202 can be generated by disposing a previously prepared third substrate in which recess have already been generated.
- recesses can be formed on the surface of first substrate 102 by disposing and arranging third substrate sections 206 on first substrate 102, wherein recesses 202 are generated or formed within the gaps/spaces between the sections, as shown in FIG. 2G.
- compositions comprising luminescent nanocrystals (e.g., polymeric compositions/matrixes) as well as suitable nanocrystals are described throughout.
- the luminescent nanocrystals are core-shell luminescent nanocrystals, such as CdSe/ZnS, CdSe/CdS and InP/ZnS.
- Exemplary sizes of nanocrystals are described herein, and suitably, the luminescent nanocrystals are between about 1-10 nm in size.
- Methods for disposing the compositions of luminescent nanocrystals in the recesses are described throughout, and include screen printing and other methods to generate a high-throughput deposition.
- second substrate is a transparent, semi-transparent or translucent substrate, such as a polymeric material or a glass.
- Hermetically sealing the compositions of luminescent nanocrystals between two glass substrates allows the nanocrystals to be utilized in various applications, such as in down-conversion in LEDs, as described herein.
- the first and second substrates are sealed with a polymeric sealant, such as a silicon-based, epoxy-based or acrylic-based sealant.
- the sealant can be introduced 110 to the first and second substrates using any suitable method, such as pouring the sealant over the substrates (and then squeezing out residual by applying pressure to the substrates), wicking the substrate into space between the substrates, injecting the sealant, dipping the substrates in a sealant, and other suitable methods.
- a sealant can simply be disposed on the outside edges of the first and second substrates, for example, by painting, spraying, spreading or otherwise applying the sealant without requiring the sealant to penetrate between the first and second substrates.
- the luminescent nanocrystals are cured in step 412 prior to sealing the first and second substrates in step 414, though in additional embodiments, the substrates can be sealed and then the compositions of luminescent nanocrystals can be cured.
- the methods of the present invention can also further comprise step
- a barrier layer on the first and second substrates to further hermetically seal the substrates.
- Methods of disposing a barrier layer e.g., atomic layer deposition, sputtering, etc. are described throughout, as are exemplary barrier layers, including inorganic layers, such as layers comprising SiO 2 , TiO 2 or AlO 2 .
- the methods suitably further comprise step
- the hermetically sealed compositions are separated from each other, as shown in FIGs. 3A-3C, for example.
- the separation can occur before of after the barrier layer is disposed.
- the methods provided allow for a high-throughput generation individual, separate samples of luminescent nanocrystals that can be used in various applications, such as in LEDs, displays, etc.
- the present invention also provides hermetically sealed compositions prepared by the various methods described herein. Exemplary compositions, sizes and characteristics of the luminescent nanocrystals, as well as the substrates, sealants and other components (e.g., barrier layers) of the sealed compositions are described throughout.
- the various steps to produce a hermetically sealed compositions of luminescent nanocrystals are performed in an inert atmosphere, i.e., either in a vacuum and/or with only N 2 or other inert gas(es) present.
- the hermetically sealed luminescent nanocrystal compositions of the present invention are used in combination with an LED or other light source.
- Applications for these sealed nanocrystal/LEDs are well known to those of ordinary skill in the art, and include the following.
- such sealed nanocrystal/LEDs can be used in microprojectors (see, e.g., U.S. Patent No.
- the hermetically sealed nanocrystals can be used in applications such as digital light processor (DLP) projectors.
- DLP digital light processor
- the hermetically sealed compositions disclosed throughout can be used to minimize the property of an optical system known as etendue (or how spread out the light is in area and angle).
- etendue an optical system known as etendue (or how spread out the light is in area and angle).
- a composition or container of the presently claimed invention By disposing, layering or otherwise covering (even partially covering) an LED or other light source with a composition or container of the presently claimed invention, and controlling the ratio of the overall area (e.g., the thickness) of the luminescent nanocrystal composition or container to the area (e.g., the thickness) of the LED, the amount or extent of etendue can be minimized, thereby increasing the amount of light captured and emitted.
- the thickness of the luminescent nanocrystal composition or container is less than about 1/5 the thickness of the LED layer.
- the luminescent nanocrystal composition or container is less than about 1/6, less than about 1/7, less than about 1/8, less than about 1/9, less than about 1/10, less than about 1/15 or less than about 1/20 of the thickness of the LED layer.
- the present invention provides microspheres 500, as shown in FIG. 5.
- the microspheres of the present invention comprise a central region 502 and a first layer 504 on an outer surface 506 of central region 502, first layer 504 comprising one or more luminescent nanocrystals 508.
- the microspheres 500 further comprise a barrier layer 512 on an outer surface 510 of first layer 504.
- Exemplary microspheres comprising a central region, a first layer, and nanoparticles, as well as methods of producing such microspheres, are disclosed in U.S. Patent No. 7,229,690, the disclosure of which is incorporated by reference herein in its entirety.
- central region 502 comprises silica
- first layer 504 comprises an inorganic material, such as silica or titania.
- Luminescent nanocrystals 508 for inclusion in the microspheres are disclosed herein, and suitably comprise core-shell luminescent nanocrystals, such as CdSe/ZnS, CdSe/CdS or InP/ZnS nanocrystals.
- the luminescent nanocrystals are between about 1-10 nm in size.
- barrier layer 512 on microspheres 500 comprises an inorganic layer SiO 2 , TiO 2 or AlO 2 , though other layers as described herein and known in the art can also be utilized.
- the microspheres 500 of the present invention have a diameter of less than about 500 microns, for example, less than about 400 microns, less than about 250 microns, less than about 100 microns, less than about 50 microns, less than about 10 microns, or less than about 1 micron, including values between these ranges.
- the present invention also provides methods of forming microspheres, as shown in flowchart 600 of FIG. 6, with reference to FIG. 5.
- a particle 502 comprising a first inorganic material is provided.
- the particle is then contacted with a composition comprising a precursor to a second inorganic material and one or more luminescent nanocrystals 508, in step 604.
- a peripheral region 504 is formed on an outer surface 506 of the particle 502, the peripheral region comprising the second inorganic material and the luminescent nanocrystals 508.
- a barrier layer 512 is disposed on an outer surface 510 of the peripheral region 504.
- a silica particle is provided, and the particle is contacted with an organic material comprising silica or titania which comprises the luminescent nanocrystals.
- the luminescent nanocrystals are suitably core-shell luminescent nanocrystals, such as CdSe/ZnS, CdSe/CdS or InP/ZnS nanocrystals with a size of about 1-10 nm. Methods for preparing silica particles and peripheral regions 504 are described throughout U.S. Patent No. 7,229,690.
- a barrier layer comprising an inorganic layer, such as SiO 2 ,
- TiO 2 or AlO 2 is disposed on the microspheres.
- the barrier layers can be disposed in various ways, including atomic layer deposition and sputtering.
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PCT/US2008/014112 WO2010077226A1 (en) | 2008-12-30 | 2008-12-30 | Methods for encapsulating nanocrystals and resulting compositions |
KR1020117015055A KR20110111391A (ko) | 2008-12-30 | 2008-12-30 | 나노결정을 캡슐화하는 방법 및 그리하여 획득되는 조성물 |
CN2008801324161A CN102257599A (zh) | 2008-12-30 | 2008-12-30 | 用于包封纳米晶体的方法及所得的复合物 |
EP08879303A EP2370993A1 (en) | 2008-12-30 | 2008-12-30 | Methods for encapsulating nanocrystals and resulting compositions |
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JP2012514071A (ja) | 2012-06-21 |
CN102257599A (zh) | 2011-11-23 |
EP2370993A1 (en) | 2011-10-05 |
KR20110111391A (ko) | 2011-10-11 |
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