JP5689575B2 - 青色発光半導体ナノクリスタル物質 - Google Patents
青色発光半導体ナノクリスタル物質 Download PDFInfo
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- JP5689575B2 JP5689575B2 JP2007502908A JP2007502908A JP5689575B2 JP 5689575 B2 JP5689575 B2 JP 5689575B2 JP 2007502908 A JP2007502908 A JP 2007502908A JP 2007502908 A JP2007502908 A JP 2007502908A JP 5689575 B2 JP5689575 B2 JP 5689575B2
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- nanocrystal
- nanocrystals
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- blue light
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- 239000004054 semiconductor nanocrystal Substances 0.000 title claims description 39
- 239000000463 material Substances 0.000 title claims description 33
- 239000002159 nanocrystal Substances 0.000 claims description 149
- 150000001875 compounds Chemical class 0.000 claims description 30
- 150000001412 amines Chemical class 0.000 claims description 27
- 239000004065 semiconductor Substances 0.000 claims description 25
- 230000005516 deep trap Effects 0.000 claims description 21
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 11
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000011162 core material Substances 0.000 description 61
- 229910052984 zinc sulfide Inorganic materials 0.000 description 41
- 229910052950 sphalerite Inorganic materials 0.000 description 40
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 33
- 239000011257 shell material Substances 0.000 description 25
- 239000000243 solution Substances 0.000 description 23
- 230000012010 growth Effects 0.000 description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 21
- 239000011258 core-shell material Substances 0.000 description 19
- 238000009826 distribution Methods 0.000 description 19
- 239000002904 solvent Substances 0.000 description 17
- 239000002245 particle Substances 0.000 description 16
- 238000000862 absorption spectrum Methods 0.000 description 15
- 150000003839 salts Chemical class 0.000 description 14
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 13
- -1 alkenyl amine Chemical class 0.000 description 13
- 239000002243 precursor Substances 0.000 description 13
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 12
- 238000005424 photoluminescence Methods 0.000 description 11
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 10
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 10
- 238000000103 photoluminescence spectrum Methods 0.000 description 10
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 10
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 9
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical compound [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000002356 single layer Substances 0.000 description 9
- 239000003446 ligand Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000002184 metal Substances 0.000 description 8
- 229910052717 sulfur Inorganic materials 0.000 description 8
- 239000011593 sulfur Substances 0.000 description 8
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 8
- 150000000180 1,2-diols Chemical class 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 7
- 150000001299 aldehydes Chemical class 0.000 description 7
- 125000000217 alkyl group Chemical group 0.000 description 7
- 230000003287 optical effect Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 6
- 239000007983 Tris buffer Substances 0.000 description 5
- 229910007709 ZnTe Inorganic materials 0.000 description 5
- RLECCBFNWDXKPK-UHFFFAOYSA-N bis(trimethylsilyl)sulfide Chemical compound C[Si](C)(C)S[Si](C)(C)C RLECCBFNWDXKPK-UHFFFAOYSA-N 0.000 description 5
- 238000000295 emission spectrum Methods 0.000 description 5
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 5
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 5
- 238000004627 transmission electron microscopy Methods 0.000 description 5
- 239000011701 zinc Chemical group 0.000 description 5
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052793 cadmium Inorganic materials 0.000 description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical group [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 4
- 238000005401 electroluminescence Methods 0.000 description 4
- 238000006862 quantum yield reaction Methods 0.000 description 4
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 description 4
- 229910052725 zinc Inorganic materials 0.000 description 4
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical group [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 3
- 229910000673 Indium arsenide Inorganic materials 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 150000003973 alkyl amines Chemical class 0.000 description 3
- 238000007872 degassing Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 229910052733 gallium Inorganic materials 0.000 description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 3
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000004020 luminiscence type Methods 0.000 description 3
- 239000011777 magnesium Chemical group 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical group [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000006911 nucleation Effects 0.000 description 3
- 238000010899 nucleation Methods 0.000 description 3
- 150000003003 phosphines Chemical class 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 229910052716 thallium Chemical group 0.000 description 3
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical group [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 description 3
- 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 2
- 229910017115 AlSb Inorganic materials 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- 229910005540 GaP Inorganic materials 0.000 description 2
- 229910005542 GaSb Inorganic materials 0.000 description 2
- 229910005543 GaSe Inorganic materials 0.000 description 2
- 229910001218 Gallium arsenide 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
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 229910002665 PbTe Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000000137 annealing Methods 0.000 description 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- KPWJBEFBFLRCLH-UHFFFAOYSA-L cadmium bromide Chemical compound Br[Cd]Br KPWJBEFBFLRCLH-UHFFFAOYSA-L 0.000 description 2
- OKIIEJOIXGHUKX-UHFFFAOYSA-L cadmium iodide Chemical compound [Cd+2].[I-].[I-] OKIIEJOIXGHUKX-UHFFFAOYSA-L 0.000 description 2
- VQNPSCRXHSIJTH-UHFFFAOYSA-N cadmium(2+);carbanide Chemical compound [CH3-].[CH3-].[Cd+2] VQNPSCRXHSIJTH-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000007942 carboxylates Chemical class 0.000 description 2
- 150000004770 chalcogenides Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- PPQREHKVAOVYBT-UHFFFAOYSA-H dialuminum;tricarbonate Chemical compound [Al+3].[Al+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O PPQREHKVAOVYBT-UHFFFAOYSA-H 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- HFJRKMMYBMWEAD-UHFFFAOYSA-N dodecanal Chemical group CCCCCCCCCCCC=O HFJRKMMYBMWEAD-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002513 implantation Methods 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 description 2
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical group [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 150000002902 organometallic compounds Chemical class 0.000 description 2
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- OCGWQDWYSQAFTO-UHFFFAOYSA-N tellanylidenelead Chemical compound [Pb]=[Te] OCGWQDWYSQAFTO-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- VNDYJBBGRKZCSX-UHFFFAOYSA-L zinc bromide Chemical compound Br[Zn]Br VNDYJBBGRKZCSX-UHFFFAOYSA-L 0.000 description 2
- UAYWVJHJZHQCIE-UHFFFAOYSA-L zinc iodide Chemical compound I[Zn]I UAYWVJHJZHQCIE-UHFFFAOYSA-L 0.000 description 2
- ZVYYAYJIGYODSD-LNTINUHCSA-K (z)-4-bis[[(z)-4-oxopent-2-en-2-yl]oxy]gallanyloxypent-3-en-2-one Chemical compound [Ga+3].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O ZVYYAYJIGYODSD-LNTINUHCSA-K 0.000 description 1
- BTOOAFQCTJZDRC-UHFFFAOYSA-N 1,2-hexadecanediol Chemical compound CCCCCCCCCCCCCCC(O)CO BTOOAFQCTJZDRC-UHFFFAOYSA-N 0.000 description 1
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical group [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical group [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- CUJRVFIICFDLGR-UHFFFAOYSA-N acetylacetonate Chemical compound CC(=O)[CH-]C(C)=O CUJRVFIICFDLGR-UHFFFAOYSA-N 0.000 description 1
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 description 1
- WRYNUJYAXVDTCB-UHFFFAOYSA-M acetyloxymercury Chemical compound CC(=O)O[Hg] WRYNUJYAXVDTCB-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- CECABOMBVQNBEC-UHFFFAOYSA-K aluminium iodide Chemical compound I[Al](I)I CECABOMBVQNBEC-UHFFFAOYSA-K 0.000 description 1
- 229940009827 aluminum acetate Drugs 0.000 description 1
- 229940118662 aluminum carbonate Drugs 0.000 description 1
- 229940024545 aluminum hydroxide Drugs 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000003698 anagen phase Effects 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- 125000001204 arachidyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical group [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- QUXFOKCUIZCKGS-UHFFFAOYSA-N bis(2,4,4-trimethylpentyl)phosphinic acid Chemical compound CC(C)(C)CC(C)CP(O)(=O)CC(C)CC(C)(C)C QUXFOKCUIZCKGS-UHFFFAOYSA-N 0.000 description 1
- LHQLJMJLROMYRN-UHFFFAOYSA-L cadmium acetate Chemical compound [Cd+2].CC([O-])=O.CC([O-])=O LHQLJMJLROMYRN-UHFFFAOYSA-L 0.000 description 1
- 229910000011 cadmium carbonate Inorganic materials 0.000 description 1
- PLLZRTNVEXYBNA-UHFFFAOYSA-L cadmium hydroxide Chemical compound [OH-].[OH-].[Cd+2] PLLZRTNVEXYBNA-UHFFFAOYSA-L 0.000 description 1
- 229940075417 cadmium iodide Drugs 0.000 description 1
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 1
- GKDXQAKPHKQZSC-UHFFFAOYSA-L cadmium(2+);carbonate Chemical compound [Cd+2].[O-]C([O-])=O GKDXQAKPHKQZSC-UHFFFAOYSA-L 0.000 description 1
- KJNYWDYNPPTGLP-UHFFFAOYSA-L cadmium(2+);diacetate;hydrate Chemical compound O.[Cd+2].CC([O-])=O.CC([O-])=O KJNYWDYNPPTGLP-UHFFFAOYSA-L 0.000 description 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000007771 core particle Substances 0.000 description 1
- XHXMPURWMSJENN-UHFFFAOYSA-N coumarin 480 Chemical compound C12=C3CCCN2CCCC1=CC1=C3OC(=O)C=C1C XHXMPURWMSJENN-UHFFFAOYSA-N 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- FYWVTSQYJIPZLW-UHFFFAOYSA-K diacetyloxygallanyl acetate Chemical compound [Ga+3].CC([O-])=O.CC([O-])=O.CC([O-])=O FYWVTSQYJIPZLW-UHFFFAOYSA-K 0.000 description 1
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000005442 diisocyanate group Chemical group 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001194 electroluminescence spectrum Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 238000001215 fluorescent labelling Methods 0.000 description 1
- 229910021513 gallium hydroxide Inorganic materials 0.000 description 1
- SRVXDMYFQIODQI-UHFFFAOYSA-K gallium(iii) bromide Chemical compound Br[Ga](Br)Br SRVXDMYFQIODQI-UHFFFAOYSA-K 0.000 description 1
- DNUARHPNFXVKEI-UHFFFAOYSA-K gallium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[Ga+3] DNUARHPNFXVKEI-UHFFFAOYSA-K 0.000 description 1
- DWRNSCDYNYYYHT-UHFFFAOYSA-K gallium(iii) iodide Chemical compound I[Ga](I)I DWRNSCDYNYYYHT-UHFFFAOYSA-K 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002430 hydrocarbons Chemical group 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- SKWCWFYBFZIXHE-UHFFFAOYSA-K indium acetylacetonate Chemical compound CC(=O)C=C(C)O[In](OC(C)=CC(C)=O)OC(C)=CC(C)=O SKWCWFYBFZIXHE-UHFFFAOYSA-K 0.000 description 1
- AMNSWIGOPDBSIE-UHFFFAOYSA-H indium(3+);tricarbonate Chemical compound [In+3].[In+3].[O-]C([O-])=O.[O-]C([O-])=O.[O-]C([O-])=O AMNSWIGOPDBSIE-UHFFFAOYSA-H 0.000 description 1
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 125000002463 lignoceryl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000001748 luminescence spectrum Methods 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 description 1
- 229910001623 magnesium bromide Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- BLQJIBCZHWBKSL-UHFFFAOYSA-L magnesium iodide Chemical compound [Mg+2].[I-].[I-] BLQJIBCZHWBKSL-UHFFFAOYSA-L 0.000 description 1
- 229910001641 magnesium iodide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AKTIAGQCYPCKFX-FDGPNNRMSA-L magnesium;(z)-4-oxopent-2-en-2-olate Chemical compound [Mg+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O AKTIAGQCYPCKFX-FDGPNNRMSA-L 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- NGYIMTKLQULBOO-UHFFFAOYSA-L mercury dibromide Chemical compound Br[Hg]Br NGYIMTKLQULBOO-UHFFFAOYSA-L 0.000 description 1
- QKEOZZYXWAIQFO-UHFFFAOYSA-M mercury(1+);iodide Chemical compound [Hg]I QKEOZZYXWAIQFO-UHFFFAOYSA-M 0.000 description 1
- LVLLOPZOJPLJQT-FDGPNNRMSA-L mercury(2+);(z)-4-oxopent-2-en-2-olate Chemical compound [Hg+2].C\C([O-])=C\C(C)=O.C\C([O-])=C\C(C)=O LVLLOPZOJPLJQT-FDGPNNRMSA-L 0.000 description 1
- HIJSSUKZLPXDPU-UHFFFAOYSA-L mercury(2+);carbonate Chemical compound [Hg+2].[O-]C([O-])=O HIJSSUKZLPXDPU-UHFFFAOYSA-L 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 125000001421 myristyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003606 oligomerizing effect Effects 0.000 description 1
- 239000011022 opal Substances 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- MPQXHAGKBWFSNV-UHFFFAOYSA-N oxidophosphanium Chemical class [PH3]=O MPQXHAGKBWFSNV-UHFFFAOYSA-N 0.000 description 1
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- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Chemical group 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
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- 239000006228 supernatant Substances 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical group [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- PUGUQINMNYINPK-UHFFFAOYSA-N tert-butyl 4-(2-chloroacetyl)piperazine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCN(C(=O)CCl)CC1 PUGUQINMNYINPK-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 229910021515 thallium hydroxide Inorganic materials 0.000 description 1
- HQOJMTATBXYHNR-UHFFFAOYSA-M thallium(I) acetate Chemical compound [Tl+].CC([O-])=O HQOJMTATBXYHNR-UHFFFAOYSA-M 0.000 description 1
- PGAPATLGJSQQBU-UHFFFAOYSA-M thallium(i) bromide Chemical compound [Tl]Br PGAPATLGJSQQBU-UHFFFAOYSA-M 0.000 description 1
- DASUJKKKKGHFBF-UHFFFAOYSA-L thallium(i) carbonate Chemical compound [Tl+].[Tl+].[O-]C([O-])=O DASUJKKKKGHFBF-UHFFFAOYSA-L 0.000 description 1
- QGYXCSSUHCHXHB-UHFFFAOYSA-M thallium(i) hydroxide Chemical compound [OH-].[Tl+] QGYXCSSUHCHXHB-UHFFFAOYSA-M 0.000 description 1
- CMJCEVKJYRZMIA-UHFFFAOYSA-M thallium(i) iodide Chemical compound [Tl]I CMJCEVKJYRZMIA-UHFFFAOYSA-M 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- TVIVIEFSHFOWTE-UHFFFAOYSA-K tri(quinolin-8-yloxy)alumane Chemical compound [Al+3].C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1.C1=CN=C2C([O-])=CC=CC2=C1 TVIVIEFSHFOWTE-UHFFFAOYSA-K 0.000 description 1
- JKNHZOAONLKYQL-UHFFFAOYSA-K tribromoindigane Chemical compound Br[In](Br)Br JKNHZOAONLKYQL-UHFFFAOYSA-K 0.000 description 1
- IYMHCKVVJXJPDB-UHFFFAOYSA-N tributyl(selanylidene)-$l^{5}-phosphane Chemical compound CCCCP(=[Se])(CCCC)CCCC IYMHCKVVJXJPDB-UHFFFAOYSA-N 0.000 description 1
- RMUKCGUDVKEQPL-UHFFFAOYSA-K triiodoindigane Chemical compound I[In](I)I RMUKCGUDVKEQPL-UHFFFAOYSA-K 0.000 description 1
- FKIZDWBGWFWWOV-UHFFFAOYSA-N trimethyl(trimethylsilylselanyl)silane Chemical compound C[Si](C)(C)[Se][Si](C)(C)C FKIZDWBGWFWWOV-UHFFFAOYSA-N 0.000 description 1
- ZAKSIRCIOXDVPT-UHFFFAOYSA-N trioctyl(selanylidene)-$l^{5}-phosphane Chemical compound CCCCCCCCP(=[Se])(CCCCCCCC)CCCCCCCC ZAKSIRCIOXDVPT-UHFFFAOYSA-N 0.000 description 1
- PIOZWDBMINZWGJ-UHFFFAOYSA-N trioctyl(sulfanylidene)-$l^{5}-phosphane Chemical compound CCCCCCCCP(=S)(CCCCCCCC)CCCCCCCC PIOZWDBMINZWGJ-UHFFFAOYSA-N 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 229940102001 zinc bromide Drugs 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 1
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 1
- 229940007718 zinc hydroxide Drugs 0.000 description 1
- 239000011787 zinc oxide Substances 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
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- B82—NANOTECHNOLOGY
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- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/56—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing sulfur
- C09K11/562—Chalcogenides
- C09K11/565—Chalcogenides with zinc cadmium
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- 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
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Description
本明細書は、35 U.S.C. § 119(e)の下で、2004年3月8日に出願された米国特許出願番号第60/550,314号に対して優先権を主張し、かつ“青色発光半導体ナノクリスタル物質”と題された、2005年3月4日にUSPTOにおいて出願された代理人整理番号14952.0329の出願に対して優先権を主張する。これらのそれぞれは、全体として引用により組み込まれている。
(連邦政府によって後援を受けた研究、又は成果)
米国政府は、NSFによる契約書第DMR0213282号、及び米国陸軍研究室による契約書第DAAD−19−02−0002号に準拠したこの発明において一定の権利を有し得る。
(技術分野)
本発明は、青色発光半導体ナノクリスタルに関するものである。
小さい直径を有する半導体ナノクリスタルは、分子と、物質のバルク形態との間の中間的な特性を有し得る。例えば、小さい直径を有する半導体物質を基礎とするナノクリスタルは、3次元すべてにおいて、電子及び正孔、双方の量子閉じ込めを示すことができ、ナノクリスタルサイズの減少とともに、該物質の有効バンドギャップを増加させる。その結果、ナノクリスタルの光吸収、及び発光の双方は、該ナノクリスタルサイズの減少に伴い、青(すなわち、高エネルギー)側にシフトする。半導体ナノクリスタルは、狭い蛍光バンドを有することができ、その発光波長は、該ナノクリスタルのサイズ、及び物質で整調される。
安定した、青色発光物質は、カラー表示用途において高度に望ましい。発光性の半導体ナノクリスタルは、有機発光化合物よりもより安定であり得る。また、半導体ナノクリスタルは、有機化合物と比較して狭い発光バンド幅を有し得る。
別の態様において、半導体ナノクリスタルの集団、該集団のそれぞれのナノクリスタルは、第一半導体物質含有コア、及び該コア上の第二半導体物質含有オーバーコーティングを含む。それぞれのナノクリスタルは、深いトラップ発光部位が実質的にない。該集団は、励起した場合、青色光を発する。
別の態様において、発光デバイスは、マトリックス含有層、該層に隣接する第一電極、該第一電極と向かい合う第二電極、及び該第一電極と該第二電極との間に配置された複数の半導体ナノクリスタルを含む。該半導体ナノクリスタルは、深いトラップ発光部位が実質的にない。該ナノクリスタルは、励起された場合に青色光を発する。
さらに別の態様において、ナノクリスタルの製造方法は、半導体ナノクリスタルの単分散集団とM含有化合物、Xドナー、及びアミンとを、該ナノクリスタルを個々にオーバーコートするのに十分な温度で接触させることを含む。該オーバーコートされたナノクリスタルは、深いトラップ発光部位が実質的になく、かつ該オーバーコートされたナノクリスタルは、励起された場合に青色光を発する。
他の特徴、目的、及び利点は、該記述、及び図面から、並びに、特許請求の範囲から明らかとなるであろう。
狭いサイズ分布、及び高い発光効率を有する半導体ナノクリスタルは、光電子デバイス、及び生物学的蛍光ラベリングのような用途において、有機分子に代わるものとして魅力的である。例えば、V. L. Colvinらの論文、Nature 1994, 370, 354;B. O. Dabbousiらの論文、Appl. Phys. Lett. 1995, 66, 1316;M. Bruchez Jr.らの論文、Science 1998, 281, 2013;W. C. W. Chan、及びS. Nieの論文、Science 1998, 281, 2016;及びH. Mattoussiらの論文、J. Am. Chem. Soc. 2000, 122, 12142を参照されたい。それらの各々は、全体として引用により組み込まれている。半導体ナノクリスタルは、光酸化より安定であり、有機分子と比較してより飽和された蛍光(すなわち、より狭い発光バンド幅)を有し得る。これらのサイズ調整可能な光学特性は、これらの安定性、及び飽和色発光と、これらの化学特性とから独立し、広面積(cm2)ハイブリッド有機/無機半導体ナノクリスタル発光デバイス(LED)における活性物質として、特に興味深いものとされている。例えば、S. Coeらの論文、Nature 2002, 420, 800;N. Tesslerらの論文、Science 2002, 295, 1506;及びJ. S. Steckelらの論文、Adv. Mater. 2003, 15, 1862を参照されたい。これらの各々は、全体として引用により組み込まれている。効率的な赤、及び緑色発光の半導体ナノクリスタルLEDは、(CdSe)ZnSコア−シェルナノクリスタルで実現された。フラットパネルディスプレー用途におけるLEDの理想的な青色発光スペクトルは、国際ドエクライレージ委員会(CIE)色度図(Commission International d'Eclairage (CIE) Chromaticity Diagram)におけるその対等色が、現在の全国テレビジョン方式委員会(National Television System Committee)(NTSC)標準色三角の外側にあるような、狭いバンド幅、及び波長を有する。30nmの半値全幅(FWHM)、及び最大限の認識されるパワーを有するガウス発光スペクトルにとって、表示用途のための青色発光の理想的な波長は、〜470nmである。470nmより短い波長(より青側)は、ヒトの目に認識されるのが難しくなるが、470nmよりも長い波長(より赤側)は、標準NTSC色三角内に位置する座標を有する。
該配位溶媒中のアミンは、該M含有塩、及びXドナーから得られるナノクリスタルの品質に寄与する。好ましくは、該配位溶媒は、例えば、該アミンとアルキルホスフィンオキシドとのモル比が10:90、30:70、又は50:50の混合物である。該混合溶媒は、サイズ分散を減少させることができ、かつ該ナノクリスタルの光ルミネッセンス量子収量を改善することができる。好ましいアミンは、C2−C20アルキルアミン、C2−C20アルケニルアミン、好ましくはC8−C18アルキルアミン、又はC8−C18アルケニルアミンのような、第一級アルキルアミン、又は第一級アルケニルアミンである。例えばトリ−オクチルホスフィンオキシド(TOPO)との混合に適切なアミンは、1−ヘキサデシルアミン、又はオレイルアミンを含む。該1,2−ジオール、又はアルデヒド、及び該アミンを、該M含有塩と混合して使用し、ナノクリスタルの集団を形成する場合、該光ルミネッセンス量子効率、及びナノクリスタルサイズの分布は、該1,2−ジオール、又はアルデヒド、又は該アミンなしで加工されたナノクリスタルと比較して、改善される。
(CdS)ZnSコア−シェルナノクリスタルを調製するために、二段階合成経路を使用した。第一段階において、該CdSコアは、脱気(100℃、1時間の真空下)オレイルアミン(7ml、98% Pfaltz & Bauer社)、及びトリオクチルホスフィン(TOP)(8ml、97% Strem)を含む丸底フラスコに該前駆体溶液を素早く注入し、250−280℃で素早く撹拌し、次に250℃で15〜30分間成長させることにより調製した。例えば、B. K. H. Yenらの論文, Adv. Mater. 2003, 15, 1858を参照されたい。これは、全体として引用により組み込まれている。該前駆体溶液は、酢酸カドミウム水和物(1−2mmol)、TOP(6ml)、及び1−2mmolのビス(2,4,4−トリメチルペンチル)ホスフィン酸[BTMPPA、シアネックス+272抽出剤(Cyanex+ 272 Extractant)(Cytec Canada社)として販売されている。全体として引用により組み込まれている、刊行された米国特許出願第2002/0144644号を参照されたい。]の脱気(100℃、1時間の真空下)混合物を、オレイルアミン(3ml)中の単体硫黄(1−2mmol)の脱気(室温、1時間の真空下)溶液と混合することにより作った。該サイズは、硫黄対カドミウム対BTMPPAの割合を1:1:1に維持しながら、注入温度、成長時間、及び前駆体の濃度を変えることによって整調した。
図1は、狭いサイズ分布を示すCdSナノクリスタルの一連のサイズに対する、光学吸収スペクトルを示す。該CdSナノクリスタルは、直径3.7±0.4nm〜5.2±0.4nmのサイズ範囲であった。スペクトルの最も長波長側の吸収特徴は、(a)λ=422nm、(b)427nm、(c)432nm、(d)435nm、(e)439nm、(f)444nm、及び(g)448nmである。448nmで第一吸収特徴を有する最も大きな粒子(コア直径5.2±0.4nm)は、第二、及び第三吸収特徴も示す。
加工後のこれらのCdSナノクリスタルに対する光ルミネッセンス量子効率は、3−6%であった。該CdSコアナノクリスタルの光ルミネッセンスは、顕著な量の深いトラップ発光を含み、UVランプを用いて励起された場合、該コア物質に紫色の様相を与える。図3中の点線は、裸CdSナノクリスタルの規格化光ルミネッセンススペクトルである。図3において、深いトラップ発光は、該ピーク発光よりもより長い波長を有する広い特徴として示される。
図5aは、4.9±0.4nmの裸CdSナノクリスタルに対するX線粉末パターンを示し、これは、002方向に沿って閃亜鉛鉱積層欠陥を有するウルツ鉱構造であるように見える。〜2単層(図5b)、及び〜3単層(図5c)のZnS被覆を有するコア−シェルナノクリスタルのX線粉末パターンは、全体の回折パターン上で、ウルツ鉱ZnSシェルの顕著な影響を示した。小さなZnS粒子の証拠は、TEM、又は光学分光学でほとんど見られなかったが、それでもZnS粒子が、XRD、及びWDS測定で存在しないことを確実にするために、試料調製時に注意を払った。
より短時間で単体硫黄、及びオレイルアミンの混合物を脱気することにより、CdSコアの単分散を増進し得る。CdSコアの調製は、単体硫黄、及びオレイルアミンの混合物を10−15分間脱気することを除き、上記のように実行した。結果として、以下の反応は、完全には進まない。従って、より少ないH2S(これは気体として残る)、及びより少ない(RHN)2Sn−1(これはCdSコア形成の速度を変化させる)が生成する。
2RNH2+Sn→(RNH)2Sn−1+H2S
他の実施態様は、下記の特許請求の範囲の範囲内である。
(図面の説明)
Claims (20)
- 第一半導体物質含有コア;及び
該コア上の第二半導体物質含有オーバーコーティングを含む、半導体ナノクリスタルであって、
該第一半導体物質は、CdSであり、かつ該第二半導体物質は、ZnSであり、
該半導体ナノクリスタルは、該コアの単分散集団を、M含有化合物、Xドナー、並びにオレイルアミン及びオレイルアミンとヘキサデシルアミンとの混合物から選択されるアミンと、該コアを個々にオーバーコートするのに十分な温度で接触させることにより製造されたものであり、該ナノクリスタルは、深いトラップ発光が実質的になく、かつ励起された場合に青色光を発し、該第二半導体物質は、M含有化合物とXドナーとの反応により形成される式MXを有する化合物であり、MはZnであり、かつXはSである、前記ナノクリスタル。 - 前記アミンが、オレイルアミンである、請求項1記載のナノクリスタル。
- 前記アミンが、オレイルアミンとヘキサデシルアミンとの混合物である、請求項1記載のナノクリスタル。
- 前記コアの単分散集団が、CdSナノクリスタルの単分散集団である、請求項1記載のナノクリスタル。
- 励起された場合に、少なくとも10%の量子効率で青色光を発する、請求項1記載のナノクリスタル。
- 励起された場合に、少なくとも30%の量子効率で青色光を発する、請求項1記載のナノクリスタル。
- 励起された場合に、少なくとも50%の量子効率で青色光を発する、請求項1記載のナノクリスタル。
- 前記青色光が、40nm以下の半値全幅を有する、請求項1〜7のいずれか1項記載のナノクリスタル。
- 前記青色光が、30nm以下の半値全幅を有する、請求項1〜7のいずれか1項記載のナノクリスタル。
- 前記青色光が、20nm以下の半値全幅を有する、請求項1〜7のいずれか1項記載のナノクリスタル。
- 前記青色光が、470nmよりも短いピーク波長を有する、請求項1記載のナノクリスタル。
- 前記青色光が、深いトラップ発光の強度よりも少なくとも5倍大きい強度を有する、請求項1記載のナノクリスタル。
- 前記青色光が、深いトラップ発光の強度よりも少なくとも10倍大きい強度を有する、請求項1記載のナノクリスタル。
- 前記青色光が、深いトラップ発光の強度よりも少なくとも20倍大きい強度を有する、請求項1記載のナノクリスタル。
- 半導体ナノクリスタル集団であって、該集団の各ナノクリスタルが、請求項1〜14のいずれか1項記載のナノクリスタルである、前記集団。
- 第一電極;該第一電極と向かい合う第二電極;及び該第一電極と該第二電極との間に配置された複数の半導体ナノクリスタルを含む、発光デバイスであって、各半導体ナノクリスタルは、請求項1〜14のいずれか1項記載のナノクリスタルである、前記発光デバイス。
- コアの単分散集団を、M含有化合物、Xドナー、並びにオレイルアミン及びオレイルアミンとヘキサデシルアミンとの混合物から選択されるアミンと、該コアを個々にオーバーコートするのに十分な温度で接触させることを含む、請求項1〜14のいずれか1項記載のナノクリスタルの製造方法であって、該オーバーコートされたナノクリスタルは、深いトラップ発光が実質的になく、かつ励起された場合に青色光を発する、前記製造方法。
- 前記アミンが、オレイルアミンである、請求項17記載の方法。
- 前記アミンが、オレイルアミンとヘキサデシルアミンとの混合物である、請求項17記載の方法。
- 前記コアの単分散集団が、CdSナノクリスタルの単分散集団である、請求項17記載の方法。
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