JP5513421B2 - テルル含有結晶性材料 - Google Patents
テルル含有結晶性材料 Download PDFInfo
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- JP5513421B2 JP5513421B2 JP2011019862A JP2011019862A JP5513421B2 JP 5513421 B2 JP5513421 B2 JP 5513421B2 JP 2011019862 A JP2011019862 A JP 2011019862A JP 2011019862 A JP2011019862 A JP 2011019862A JP 5513421 B2 JP5513421 B2 JP 5513421B2
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- JP
- Japan
- Prior art keywords
- group
- cdte
- nanocrystallites
- nanocrystallite
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- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 229910052714 tellurium Inorganic materials 0.000 title abstract description 7
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 title abstract description 7
- 239000002178 crystalline material Substances 0.000 title description 2
- 239000002904 solvent Substances 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims description 37
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000004065 semiconductor Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 18
- 125000000217 alkyl group Chemical group 0.000 claims description 16
- 125000003368 amide group Chemical group 0.000 claims description 13
- 125000003342 alkenyl group Chemical group 0.000 claims description 10
- 229910052725 zinc Inorganic materials 0.000 claims description 10
- 125000003118 aryl group Chemical group 0.000 claims description 7
- 229910052793 cadmium Inorganic materials 0.000 claims description 7
- 125000000753 cycloalkyl group Chemical group 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 125000000392 cycloalkenyl group Chemical group 0.000 claims description 6
- 229910052753 mercury Inorganic materials 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims 4
- 229910052751 metal Inorganic materials 0.000 claims 4
- 229910004613 CdTe Inorganic materials 0.000 abstract description 80
- 230000012010 growth Effects 0.000 abstract description 30
- 239000002243 precursor Substances 0.000 abstract description 11
- 238000000137 annealing Methods 0.000 abstract description 6
- 238000002347 injection Methods 0.000 abstract description 6
- 239000007924 injection Substances 0.000 abstract description 6
- 229910004262 HgTe Inorganic materials 0.000 abstract description 3
- 229910017680 MgTe Inorganic materials 0.000 abstract description 3
- 229910007709 ZnTe Inorganic materials 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 36
- 238000005424 photoluminescence Methods 0.000 description 28
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 24
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 21
- 238000000034 method Methods 0.000 description 21
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 21
- 239000002245 particle Substances 0.000 description 19
- 238000006243 chemical reaction Methods 0.000 description 17
- 238000001228 spectrum Methods 0.000 description 16
- 229910052984 zinc sulfide Inorganic materials 0.000 description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 15
- 238000009826 distribution Methods 0.000 description 15
- 239000002159 nanocrystal Substances 0.000 description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 238000000862 absorption spectrum Methods 0.000 description 12
- 239000011257 shell material Substances 0.000 description 12
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 12
- 230000015572 biosynthetic process Effects 0.000 description 11
- RMZAYIKUYWXQPB-UHFFFAOYSA-N trioctylphosphane Chemical compound CCCCCCCCP(CCCCCCCC)CCCCCCCC RMZAYIKUYWXQPB-UHFFFAOYSA-N 0.000 description 11
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 10
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical group [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 description 10
- 230000006911 nucleation Effects 0.000 description 10
- 238000010899 nucleation Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 239000011701 zinc Chemical group 0.000 description 9
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 125000004432 carbon atom Chemical group C* 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 230000001681 protective effect Effects 0.000 description 7
- 230000005855 radiation Effects 0.000 description 7
- 238000004627 transmission electron microscopy Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000004062 sedimentation Methods 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 230000001965 increasing effect Effects 0.000 description 5
- 239000011669 selenium Substances 0.000 description 5
- 230000003595 spectral effect Effects 0.000 description 5
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 4
- 125000003277 amino group Chemical group 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical group [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 4
- 230000005516 deep trap Effects 0.000 description 4
- 125000004663 dialkyl amino group Chemical group 0.000 description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 4
- 239000011777 magnesium Chemical group 0.000 description 4
- KPDXRSBWIPGWLS-UHFFFAOYSA-N n-bis(dipropylamino)phosphanyl-n-propylpropan-1-amine Chemical compound CCCN(CCC)P(N(CCC)CCC)N(CCC)CCC KPDXRSBWIPGWLS-UHFFFAOYSA-N 0.000 description 4
- -1 n-propenyl group Chemical group 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 4
- 229910052717 sulfur Inorganic materials 0.000 description 4
- 238000001308 synthesis method Methods 0.000 description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 3
- 125000003545 alkoxy group Chemical group 0.000 description 3
- 125000003282 alkyl amino group Chemical group 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 125000004093 cyano group Chemical group *C#N 0.000 description 3
- 238000000295 emission spectrum Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 125000001188 haloalkyl group Chemical group 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 125000002768 hydroxyalkyl group Chemical group 0.000 description 3
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 229910052950 sphalerite Inorganic materials 0.000 description 3
- 125000001424 substituent group Chemical group 0.000 description 3
- 125000004001 thioalkyl group Chemical group 0.000 description 3
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical group [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 238000001016 Ostwald ripening Methods 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 2
- 239000012298 atmosphere Substances 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
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- HQWPLXHWEZZGKY-UHFFFAOYSA-N diethylzinc Chemical compound CC[Zn]CC HQWPLXHWEZZGKY-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical group [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 description 2
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 150000004772 tellurides Chemical class 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- FKIZDWBGWFWWOV-UHFFFAOYSA-N trimethyl(trimethylsilylselanyl)silane Chemical compound C[Si](C)(C)[Se][Si](C)(C)C FKIZDWBGWFWWOV-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000005169 Debye-Scherrer Methods 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910003481 amorphous carbon 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
- 125000002029 aromatic hydrocarbon group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 125000002837 carbocyclic group Chemical group 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000012937 correction Methods 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
- 125000003493 decenyl group Chemical group [H]C([*])=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])[H] 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
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000007773 growth pattern Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002329 infrared spectrum 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
- 125000000555 isopropenyl group Chemical group [H]\C([H])=C(\*)C([H])([H])[H] 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
- 230000007774 longterm Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 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
- 125000004370 n-butenyl group Chemical group [H]\C([H])=C(/[H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000004365 octenyl group Chemical group C(=CCCCCCC)* 0.000 description 1
- 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
- 239000003921 oil Substances 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 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
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920001343 polytetrafluoroethylene 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
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- MUSLHCJRTRQOSP-UHFFFAOYSA-N rhodamine 101 Chemical compound [O-]C(=O)C1=CC=CC=C1C(C1=CC=2CCCN3CCCC(C=23)=C1O1)=C2C1=C(CCC1)C3=[N+]1CCCC3=C2 MUSLHCJRTRQOSP-UHFFFAOYSA-N 0.000 description 1
- 230000005070 ripening Effects 0.000 description 1
- 229920002631 room-temperature vulcanizate silicone Polymers 0.000 description 1
- 229930195734 saturated hydrocarbon Natural products 0.000 description 1
- 238000010187 selection method Methods 0.000 description 1
- 150000004771 selenides Chemical class 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000000235 small-angle X-ray scattering Methods 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 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
- 125000005063 tetradecenyl group Chemical group C(=CCCCCCCCCCCCC)* 0.000 description 1
- ZMBHCYHQLYEYDV-UHFFFAOYSA-N trioctylphosphine oxide Chemical compound CCCCCCCCP(=O)(CCCCCCCC)CCCCCCCC ZMBHCYHQLYEYDV-UHFFFAOYSA-N 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/22—Amides of acids of phosphorus
- C07F9/224—Phosphorus triamides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/50—Organo-phosphines
- C07F9/53—Organo-phosphine oxides; Organo-phosphine thioxides
- C07F9/5304—Acyclic saturated phosphine oxides or thioxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/605—Products containing multiple oriented crystallites, e.g. columnar crystallites
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
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Description
特に記載がない場合には、全ての反応は、グローブボックスまたは標準的なシシュレンク(Schlenk)技術を利用して乾燥窒素雰囲気中で行った。サイズ選択沈降に用いたHPLCグレード溶媒は、窒素で5分間バブリングして溶解酸素を除去した。トリオクチルホスフィン(TOP,95%)は、フルカ(Fluka)から受け取ってそのまま用いた。テルルショット(99.999%、低酸化)は、アルファ/アエサー(Alfa/Aesar)から受け取ってそのまま用いた。ヘキサ−n−プロピル ホスホラス トリアミド(HPPT、97%、Lancaster)は、真空蒸留し、0.55Torrにおいて83−103℃で沸騰するフラクションを回収した。トリオクチルホスフィン酸化物(TOPO、90%、Strem)を真空(〜0.5Torr)で1時間乾燥した。ジメチルカドミウム(99+%、Strem)を真空移動で精製した。
ヘキサン中のCdTeナノクリスタライトのUV/可視光線吸収スペクトロスコピーは、HP8453ダイオード アレイ スペクトロメーターで1nmの解像力で行った。蛍光測定は、SPEXフルオロログ−2 スペクトロフルオロメーターであって、500nmでブレーズされた2400グルーブ/インチ回折格子を備える二つの二重モノクロメーターおよび光電子増倍管(R928)検出器を備えるものを用いて行った。CdTeサンプルは1cm石英キュベット中のヘキサンまたは〜1%TOPを有するTHFのいずれかに溶解し、第1の特徴の吸光度9.3より小さくなるまで希釈した。スペクトルは前面配置で得られ、光学素子と検出器の波長従属性を、好適な補正係数ファイル(MCOR1097.SPT)で掛けて修正した。
L=0.888(λ)/[Δ(2θ)cos(θ)]
ここで、LはX線のコヒーレンス長(シェラー長として公知である)、λはX線の波長、Δ(2θ)はラジアンのFWHMであり、θは入射角である。コヒーレンス長Lは、粒子の容積平均による実際の次元に関係する数学的な構成である。球の直径Dに対し、関係は次のように表される:
D=(4/3)L。
非被覆または「裸の」CdTeナノクリスタライトからの高量子効率についてまたはそれ自体極めて重要であるけれども、その後の保護シェル成長の試みに関する結果にも影響を与える。(CdSe)ZnSと(CdSe)CdS研究からの経験的な観察によれば、このオーバーコートプロセスが出発材料の量子効率について一般に増加効果を与えることが示され、最も輝度の高い(コア)シェルサンプルは一般に最も輝度の高いナノクリスタルコアから生じる。半導体バンドオフセットは、ポテンシャルシェル材料が電子と正孔との双方にエネルギーバリアーを提供できるかどうか決定するために比較すべきである。ナノクリスタライト用に信頼できる値が公表されていないので、バルク値は一般的なガイドとして用いることができる。図14はII−VI亜鉛、カドミウム半導体用の真空レベルに対するバンド位置を示す。ZnSとZnSeは好適なシェル材料候補であるといえる。ZnSまたはZnSeシェルのCdTeコアへの成長は、加工と操作中により強固であるコンポジット材料を提供する。(CdTe)ZnSと(CdTe)ZnSeオーバーコートナノクリスタライトは、1ステップと2ステップ合成法の双方で合成された。
CdTeナノクリスタライトは、上記のように合成された。コアが所定のサイズに達すると、温度を200℃に低下させた。各CdTeサンプル用に所定厚さのZnSシェルを成長させるために必要なZnとS前駆体の量は、次のように決定された。最初に、CdTeナノクリスタライトの平均半径はTEMまたはSAXS測定から評価された。次に、所定厚みのシェルを形成するために必要なZnSとCdTeとの比率は、コア容積の比率に対するシェル容積の比率に基づいて計算したが、球状コア、シェルと仮定し、CdTeとZnSのバルク格子パラメーターを用いた。等モル量のジエチル亜鉛(ZnEt2)とヘキサメチルジシラシアン((TMS)2S)は5−10mLのトリオクチルホスフィン(TOP)に加えた。ZnとSの前駆体溶液は、5−10分間、撹拌CdTe反応溶液に滴下した。滴下が完了した後、混合物を90℃に冷却し、数時間撹拌した。10mLのブタノールを混合物に加えて、室温に冷却した際のTOPOの固化を防止した。オーバーコート粒子を成長溶液中に貯蔵して、ナノクリスタライト表面のTOPOによる不動態化の維持を確保した。(CdTe)ZnSeは、同様にセレン源として作用するビス(トリメチルシリル)セレニド((TMS)2Se)を用いて合成した。ZnSとZnSeのオーバーコートの双方に対し、PLの量子効率は0−20%増加した。
CdTeナノクリスタライトは、上記のように合成した。ナノクリスタライトの量は、質量および/または光学吸収により決定した。20gのTOPOを真空(0.5Torr)で1時間乾燥し、その後窒素下で60℃まで冷却した。CdTeナノクリスタライトをヘキサンまたはTHFに分散し、TOPOと混合し、その後溶媒を真空で除去した。所定厚みのZnSシェルを成長させるために要するZnとSの前駆体の量は次にように決定した。最初に、CdTeナノクリスタライト平均半径をTEMまたはSAXA測定から評価した。次に、シェルの形成に必要なCdTeに対するZnSの比率は、コア容積の比率に対するシェル容積の比率に基づいて計算したが、球状コアとシェルと仮定し、CdTeとZnSのバルク格子パラメーターを用いた。等モル量のジエチル亜鉛(ZnEt2)とヘキサメチルジシラシアン((TMS)2S)は5−10mLのトリオクチルホスフィン(TOP)に加えた。ZnとSの前駆体溶液は、5−10分間、撹拌CdTe反応溶液に滴下した。滴下が完了した後、混合物を90℃に冷却し、数時間撹拌した。10mLのブタノールを混合物に加えて、室温に冷却した際のTOPOの固化を防止した。オーバーコート粒子を成長溶液中で貯蔵して、ナノクリスタライト表面のTOPOによる不動態化の維持を確保した。(CdTe)ZnSeは、同様にセレン源として作用するビス(トリメチルシリル)セレニド((TMS)2Se)を用いて合成した。ZnSとZnSeのオーバーコートの双方に対し、PLの量子効率は0−20%増加した。
第2のサイズ選択沈降法では、狭いサイズ分布が得られる。たとえば、10%RMS偏差より少ないサイズ分布が調製できる。CdTeナノクリスタルは、修正サイズ選択沈降により空気中で単離される。上記のようなCdTeナノクリスタルの合成後、フラスコを〜60℃に冷却し、10mLのトリオクチルアミンと10mLのテトラハイドロフラン(THF)と混合する。メタノールまたはアセトニトリルは、混合物が混濁するまで混合溶液に加えた。サイズ選択CdTeナノクリスタルは、遠心分離後沈降粉末として得ることができる。サイズ選択化CdTeナノクリスタルはヘキサンに適度に溶解し、THFに極めてよく溶解する。トリオクチルアミンは、サイズ選択工程中にPLの高量子効率を維持するため、さらには相分離を抑制するために加える。ナノクリスタル表面のエッチングを避けるために、サイズ選択工程前に直ちに使用すべきである。サイズ選択後、PLスペクトルの代表的なFWHMは35nmである。20nm程度のFWHMを有するスペクトルが得られる。
図15はCdTeナノクリスタライトの代表的な室温ホトルミネッセンス(PL)スペクトルを示すが、580nmから770nmにわたる光スペクトルをスパンするものである。これらのサンプルのPL量子効率は、CdTeナノクリスタライトは最も高い量子効率を有する約640nmで放射するが、40%から65%の範囲である。量子効率は、CdTeナノクリスタライトのサイズが平均サイズよりも小さくまたは大きくなると低くなる。各スペクトルの最大値の半分における全幅(FWHM)は、サイズ選択工程前は、45nmから70nmの範囲である。サイズ選択後、各放射スペクトルFWHMは35nmに低下する。図15に示されるスペクトルは、4.0nm、4.5nm、4.8nm、5.2nm、5.8nm、6.2nm、7.7nm、9.1nm、11.9nmの直径を有するCdTeナノクリスタライトを用いて得られた。
Claims (5)
- 次式で表されるTe含有化合物からなるテルル化物半導体ナノクリスタライト製造用原料:
- Z、Z’、Z’’の各々はジアルキルアミド基である請求項1に記載のテルル化物半導体ナノクリスタライト製造用原料。
- P(Z)(Z’)(Z’’)とTeとを無溶媒下で混合することにより溶液化することを含むTe含有化合物を製造する方法、ただし、Z、Z’、Z’’の一つは独立的にアミド基、アルキル基、アルケニル基、アリール基、シクロアルキル基またはシクロアルケニル基であり、Z、Z’、Z’’の少なくとも一つはアミド基である。
- Cd、Zn、Mg、およびHgからなる群から選択される少なくとも1種の金属を含む金属含有化合物と、
請求項1または2に記載のテルル化物半導体ナノクリスタライト製造用原料と、
を配位溶媒に注入し、混合物を形成することと、
該混合物を加熱することによりナノクリスタライトを成長させることと、
により得られるテルル化物半導体ナノクリスタライト。 - Cd、Zn、Mg、およびHgからなる群から選択される少なくとも1種の金属を含む金属含有化合物と、
請求項1または2に記載のテルル化物半導体ナノクリスタライト製造用原料と、
を配位溶媒に注入し、混合物を形成することと、
該混合物を加熱することによりナノクリスタライトを成長させることと、
によるテルル化物半導体ナノクリスタライトの製造方法。
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US14570899P | 1999-07-26 | 1999-07-26 | |
US60/145,708 | 1999-07-26 |
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US6607829B1 (en) | 1997-11-13 | 2003-08-19 | Massachusetts Institute Of Technology | Tellurium-containing nanocrystalline materials |
US6207392B1 (en) | 1997-11-25 | 2001-03-27 | The Regents Of The University Of California | Semiconductor nanocrystal probes for biological applications and process for making and using such probes |
US6855202B2 (en) | 2001-11-30 | 2005-02-15 | The Regents Of The University Of California | Shaped nanocrystal particles and methods for making the same |
WO2005097939A1 (ja) * | 2004-03-30 | 2005-10-20 | Idemitsu Kosan Co., Ltd. | 蛍光変換媒体及びカラー発光装置 |
EP1264375A2 (en) | 2000-03-14 | 2002-12-11 | Massachusetts Institute Of Technology | Optical amplifiers and lasers |
WO2001071354A2 (en) | 2000-03-20 | 2001-09-27 | Massachusetts Institute Of Technology | Inorganic particle conjugates |
US6576291B2 (en) * | 2000-12-08 | 2003-06-10 | Massachusetts Institute Of Technology | Preparation of nanocrystallites |
US20020110180A1 (en) | 2001-02-09 | 2002-08-15 | Barney Alfred A. | Temperature-sensing composition |
US8618595B2 (en) | 2001-07-02 | 2013-12-31 | Merck Patent Gmbh | Applications of light-emitting nanoparticles |
US6846565B2 (en) | 2001-07-02 | 2005-01-25 | Board Of Regents, The University Of Texas System | Light-emitting nanoparticles and method of making same |
AU2002320252A1 (en) * | 2001-07-02 | 2003-01-21 | Board Of Regents, University Of Texas System | Light-emitting nanoparticles and method of making same |
WO2003092043A2 (en) * | 2001-07-20 | 2003-11-06 | Quantum Dot Corporation | Luminescent nanoparticles and methods for their preparation |
AU2002326920B2 (en) | 2001-09-17 | 2007-09-13 | Massachusetts Institute Of Technology | Semiconductor nanocrystal composite |
US7150910B2 (en) | 2001-11-16 | 2006-12-19 | Massachusetts Institute Of Technology | Nanocrystal structures |
FR2838241B1 (fr) | 2002-04-09 | 2004-06-25 | Commissariat Energie Atomique | Materiaux luminescents constitues de nanocristaux a structure coeur/coquille et leur procede de preparation |
US6788453B2 (en) | 2002-05-15 | 2004-09-07 | Yissum Research Development Company Of The Hebrew Univeristy Of Jerusalem | Method for producing inorganic semiconductor nanocrystalline rods and their use |
AU2003224411B2 (en) * | 2002-05-15 | 2008-07-31 | Yissum Research Development Company Of The Hebrew University Of Jerusalem | Method for producing inorganic semiconductor nanocrystalline rods and their use |
US7319709B2 (en) | 2002-07-23 | 2008-01-15 | Massachusetts Institute Of Technology | Creating photon atoms |
US7229497B2 (en) | 2003-08-26 | 2007-06-12 | Massachusetts Institute Of Technology | Method of preparing nanocrystals |
US8137457B2 (en) | 2004-07-23 | 2012-03-20 | University Of Florida Research Foundation, Inc. | One-pot synthesis of high-quality metal chalcogenide nanocrystals without precursor injection |
US7465352B2 (en) * | 2004-07-23 | 2008-12-16 | University Of Florida Research Foundation, Inc. | One-pot synthesis of high-quality metal chalcogenide nanocrystals without precursor injection |
US7229690B2 (en) | 2004-07-26 | 2007-06-12 | Massachusetts Institute Of Technology | Microspheres including nanoparticles |
US7316967B2 (en) | 2004-09-24 | 2008-01-08 | Massachusetts Institute Of Technology | Flow method and reactor for manufacturing noncrystals |
DE102004055380B4 (de) * | 2004-11-17 | 2007-11-22 | Johannes-Gutenberg-Universität Mainz | Verfahren zur Synthese von Nanokristalliten und danach hergestellte Nanokristallite |
US8134175B2 (en) | 2005-01-11 | 2012-03-13 | Massachusetts Institute Of Technology | Nanocrystals including III-V semiconductors |
JP2007224233A (ja) * | 2006-02-27 | 2007-09-06 | Idemitsu Kosan Co Ltd | 半導体ナノ粒子の製造方法及びその製造装置 |
DE102006055218A1 (de) | 2006-11-21 | 2008-05-29 | Bayer Technology Services Gmbh | Kontinuierliches Verfahren zur Synthese von nanoskaligen metallhaltigen Nanopartikel und Nanopartikeldispersion |
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JPS58145606A (ja) * | 1982-02-22 | 1983-08-30 | Toshiba Corp | InP合成方法 |
JPS60108307A (ja) * | 1983-11-16 | 1985-06-13 | Res Dev Corp Of Japan | テルル−リン系非晶質化合物材料及びその製造法 |
JP3229620B2 (ja) * | 1991-07-22 | 2001-11-19 | 三井化学株式会社 | 半導体超微粒子の製造方法および組成物 |
JPH08328188A (ja) * | 1995-05-30 | 1996-12-13 | Konica Corp | ハロゲン化銀写真感光材料 |
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US5711803A (en) * | 1995-09-29 | 1998-01-27 | Midwest Research Institute | Preparation of a semiconductor thin film |
US6322901B1 (en) * | 1997-11-13 | 2001-11-27 | Massachusetts Institute Of Technology | Highly luminescent color-selective nano-crystalline materials |
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CA2374337C (en) | 2009-04-14 |
EP1250474A2 (en) | 2002-10-23 |
DE60023559T2 (de) | 2006-09-07 |
CA2374337A1 (en) | 2001-02-01 |
ATE307919T1 (de) | 2005-11-15 |
WO2001007689A2 (en) | 2001-02-01 |
WO2001007689A3 (en) | 2001-09-27 |
JP2011148797A (ja) | 2011-08-04 |
AU6379100A (en) | 2001-02-13 |
JP5165824B2 (ja) | 2013-03-21 |
EP1250474B1 (en) | 2005-10-26 |
JP2003505330A (ja) | 2003-02-12 |
DE60023559D1 (de) | 2005-12-01 |
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