EP2819952A1 - Formation de nanoparticules d'antimoniures a partir du trihydrure d'antimoine comme source d'antimoine - Google Patents
Formation de nanoparticules d'antimoniures a partir du trihydrure d'antimoine comme source d'antimoineInfo
- Publication number
- EP2819952A1 EP2819952A1 EP13716418.2A EP13716418A EP2819952A1 EP 2819952 A1 EP2819952 A1 EP 2819952A1 EP 13716418 A EP13716418 A EP 13716418A EP 2819952 A1 EP2819952 A1 EP 2819952A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- nanoparticles
- antimony
- antimonide
- nanocrystals
- indium
- 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.)
- Withdrawn
Links
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 67
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 65
- OUULRIDHGPHMNQ-UHFFFAOYSA-N stibane Chemical compound [SbH3] OUULRIDHGPHMNQ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 24
- 230000015572 biosynthetic process Effects 0.000 title claims description 30
- 229910052751 metal Inorganic materials 0.000 claims abstract description 38
- 239000002184 metal Substances 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims description 66
- 239000002159 nanocrystal Substances 0.000 claims description 56
- WPYVAWXEWQSOGY-UHFFFAOYSA-N indium antimonide Chemical compound [Sb]#[In] WPYVAWXEWQSOGY-UHFFFAOYSA-N 0.000 claims description 38
- 239000000243 solution Substances 0.000 claims description 38
- 239000012429 reaction media Substances 0.000 claims description 33
- 239000002243 precursor Substances 0.000 claims description 31
- 230000008569 process Effects 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 19
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadec-1-ene Chemical group CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 18
- 239000006185 dispersion Substances 0.000 claims description 13
- 229910052738 indium Inorganic materials 0.000 claims description 13
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 9
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 9
- 239000000194 fatty acid Substances 0.000 claims description 9
- 229930195729 fatty acid Natural products 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 9
- 229910052700 potassium Inorganic materials 0.000 claims description 9
- 239000011591 potassium Substances 0.000 claims description 9
- TWJNQYPJQDRXPH-UHFFFAOYSA-N 2-cyanobenzohydrazide Chemical compound NNC(=O)C1=CC=CC=C1C#N TWJNQYPJQDRXPH-UHFFFAOYSA-N 0.000 claims description 8
- 235000021360 Myristic acid Nutrition 0.000 claims description 8
- TUNFSRHWOTWDNC-UHFFFAOYSA-N Myristic acid Natural products CCCCCCCCCCCCCC(O)=O TUNFSRHWOTWDNC-UHFFFAOYSA-N 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 8
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 150000004665 fatty acids Chemical class 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- AVTYONGGKAJVTE-OLXYHTOASA-L potassium L-tartrate Chemical compound [K+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O AVTYONGGKAJVTE-OLXYHTOASA-L 0.000 claims description 7
- 239000001472 potassium tartrate Substances 0.000 claims description 7
- 229940111695 potassium tartrate Drugs 0.000 claims description 7
- 235000011005 potassium tartrates Nutrition 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 239000011651 chromium Substances 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- ZDVNRCXYPSVYNN-UHFFFAOYSA-K di(tetradecanoyloxy)indiganyl tetradecanoate Chemical group [In+3].CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCC([O-])=O ZDVNRCXYPSVYNN-UHFFFAOYSA-K 0.000 claims description 6
- VBXWCGWXDOBUQZ-UHFFFAOYSA-K diacetyloxyindiganyl acetate Chemical compound [In+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VBXWCGWXDOBUQZ-UHFFFAOYSA-K 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 239000011572 manganese Substances 0.000 claims description 6
- 239000010955 niobium Substances 0.000 claims description 6
- 239000010948 rhodium Substances 0.000 claims description 6
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 239000003446 ligand Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 4
- 230000002378 acidificating effect Effects 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical group [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910052793 cadmium Inorganic materials 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 claims description 4
- 239000010941 cobalt Substances 0.000 claims description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- -1 docecylamine Chemical compound 0.000 claims description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052733 gallium Inorganic materials 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 229910052716 thallium Inorganic materials 0.000 claims description 4
- BKVIYDNLLOSFOA-UHFFFAOYSA-N thallium Chemical compound [Tl] BKVIYDNLLOSFOA-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 150000001412 amines Chemical class 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 3
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 3
- 229910052804 chromium Inorganic materials 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052758 niobium Inorganic materials 0.000 claims description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052763 palladium Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229910052703 rhodium Inorganic materials 0.000 claims description 3
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052701 rubidium Inorganic materials 0.000 claims description 3
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 3
- 229910052707 ruthenium Inorganic materials 0.000 claims description 3
- 229910052706 scandium Inorganic materials 0.000 claims description 3
- SIXSYDAISGFNSX-UHFFFAOYSA-N scandium atom Chemical compound [Sc] SIXSYDAISGFNSX-UHFFFAOYSA-N 0.000 claims description 3
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052709 silver Inorganic materials 0.000 claims description 3
- 239000004332 silver Substances 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 3
- JBQYATWDVHIOAR-UHFFFAOYSA-N tellanylidenegermanium Chemical compound [Te]=[Ge] JBQYATWDVHIOAR-UHFFFAOYSA-N 0.000 claims description 3
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052727 yttrium Inorganic materials 0.000 claims description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- MHZGKXUYDGKKIU-UHFFFAOYSA-N Decylamine Chemical compound CCCCCCCCCCN MHZGKXUYDGKKIU-UHFFFAOYSA-N 0.000 claims description 2
- 239000005639 Lauric acid Substances 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 235000021314 Palmitic acid Nutrition 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- PLZVEHJLHYMBBY-UHFFFAOYSA-N Tetradecylamine Chemical compound CCCCCCCCCCCCCCN PLZVEHJLHYMBBY-UHFFFAOYSA-N 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
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- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
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- 229910052959 stibnite Inorganic materials 0.000 description 1
- IHBMMJGTJFPEQY-UHFFFAOYSA-N sulfanylidene(sulfanylidenestibanylsulfanyl)stibane Chemical compound S=[Sb]S[Sb]=S IHBMMJGTJFPEQY-UHFFFAOYSA-N 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical group [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 229940095064 tartrate Drugs 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G30/00—Compounds of antimony
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0352—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions
- H01L31/035209—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures
- H01L31/035218—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by their shape or by the shapes, relative sizes or disposition of the semiconductor regions comprising a quantum structures the quantum structure being quantum dots
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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
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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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
- 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
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/76—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by a space-group or by other symmetry indications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/70—Nanostructure
- Y10S977/773—Nanoparticle, i.e. structure having three dimensions of 100 nm or less
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/84—Manufacture, treatment, or detection of nanostructure
- Y10S977/895—Manufacture, treatment, or detection of nanostructure having step or means utilizing chemical property
- Y10S977/896—Chemical synthesis, e.g. chemical bonding or breaking
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/902—Specified use of nanostructure
- Y10S977/932—Specified use of nanostructure for electronic or optoelectronic application
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/902—Specified use of nanostructure
- Y10S977/932—Specified use of nanostructure for electronic or optoelectronic application
- Y10S977/936—Specified use of nanostructure for electronic or optoelectronic application in a transistor or 3-terminal device
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S977/00—Nanotechnology
- Y10S977/902—Specified use of nanostructure
- Y10S977/932—Specified use of nanostructure for electronic or optoelectronic application
- Y10S977/953—Detector using nanostructure
Definitions
- the present invention relates to the field of the manufacture of antimonide nanoparticle-based materials. More particularly, it relates to a novel process for preparing nanocrystals of semiconductor antimonides, in particular indium antimonide (InSb).
- semiconductor antimonides in particular indium antimonide (InSb).
- Antimonide nanocrystals can be used in many fields, for example in the development of photovoltaic cells, light-emitting diodes, photodetectors, gas sensors, thermoelectric devices or fluorescent markers in biology.
- nanocrystals In general, semiconductor nanocrystals, crystalline particles whose dimensions are typically between a few nanometers and a few tens of nanometers, have been the subject of numerous studies. Such nanocrystals have proved particularly interesting in view of the appearance of a phenomenon of "quantum confinement" in these particles when their size is smaller than the excitonic Bohr radius. This phenomenon is reflected in particular by a significant increase in the forbidden band energy, so ranges of wavelengths that can be absorbed or emitted by the nanocrystal, compared to the solid semiconductor. By acting only on the particle size of a given semiconductor material, it is thus possible to adjust its optical properties to meet the requirements of the intended application.
- colloidal chemical synthesis advantageously enables the production, at low cost and in large quantities, of particles having a small size dispersion.
- This technique gives very satisfactory results in the case of cadmium chalcogenides (CdS, CdSe and CdTe).
- CdS, CdSe and CdTe cadmium chalcogenides
- the European RoHS directive aims to outlaw the use of such substances for the construction of electronic devices marketed in Europe after July 2006. It therefore seems essential to turn to alternative materials that do not harm the health of living organisms.
- indium antimonium is an advantageous option, given, on the one hand, its innocuousness and, on the other hand, its particularly interesting intrinsic physical properties.
- the electron mobility values obtained for indium antimonide can reach 78,000 cm 2 / Vs (against 1 450 cm 2 / Vs in solid silicon).
- Indium antimonide therefore represents a prime candidate for the development of optical devices, provided that it makes good use of the strong quantum confinement phenomenon that can be exerted in this material if the particle sizes are sufficiently small.
- the lithography technique is generally used in the shaping processes of many devices based on semiconductor materials.
- the liquid deposition methods spin- or spray-coating for example
- printing or inkjet may sometimes advantageously replace lithography.
- the different modes of synthesis used to obtain inorganic nanocrystals are based on the use of liquid or gaseous phases.
- the particles obtained are polydisperse and strongly attached to the substrate. It is therefore difficult to detach them for use in an ink.
- this method is very expensive because it uses the use of specific substrates as well as constraining experimental conditions (working under high vacuum).
- Li et al. [7] implement a reaction of this type to obtain nanocrystals of InSb and GaSb.
- the main disadvantage of this approach lies in the fact that the nanocrystals thus obtained are relatively large and highly poly-dispersed (their diameter varies between 20 and 60 nm).
- the present invention relates to a method for preparing nanoparticles of antimonide element (s) metal (s), characterized in that it implements antimony trihydride as a of antimony source.
- the antimonide nanoparticles are more particularly obtained in the form of a colloidal solution.
- antimonide is meant the combination of antimony with one or more metallic element (s).
- Said metal element may be chosen especially from aluminum (Al), gallium (Ga), indium (In), thallium (Tl), zinc (Zn), cadmium (Cd), iron (Fe) ), cobalt (Co), nickel (Ni), bismuth (Bi), scandium (Se), titanium (Ti), vanadium (V), chromium (Cr), manganese (Mn), copper (Cu), rubidium (Rb), strontium (Sr), yttrium (Y), zirconium (Zr), niobium (Nb), ruthenium (Ru), rhodium (Rh), palladium (Pd), silver (Ag), cesium (Cs), barium (Ba), hafnium (Hf), iridium (Ir), platinum (Pt), gold (Au), tin (Sn), lead (Pb), and mixtures thereof.
- antimony
- source of antimony is meant the precursor capable of providing the supply of Sb atoms necessary for the growth of nanoparticles antimonide.
- Antimony trihydride (SbH 3 ) is in the form of a gas at temperatures above -17 ° C. This compound is also more commonly referred to as “stibnite”. By “antimony trihydride” is meant for the purposes of the invention the compound in gaseous form.
- nanoparticle in particular, a particle of the nanocrystal type.
- the antimony trihydride may be more particularly formed and injected as it is formed, in a liquid medium, hereinafter referred to as a reaction medium, comprising at least one precursor of an element metal of which it is desired to form the antimonide.
- the antimonide nanoparticles obtained by the process of the invention have the desired characteristics, in particular in terms of composition, crystallinity, size dispersion and photoluminescence, for their integration into optoelectronic devices.
- the nanoparticles obtained according to the invention can be isolated, in other words they are not trapped in a matrix or attached to a substrate, which advantageously allows their implementation by a liquid route or else in an ink for inkjet in the development of optoelectronic devices.
- Such nanoparticles can thus be used in solar cells, in photodetectors, light converters, light-emitting diodes, transistors, as fluorescent markers or in chemical or optical sensors.
- the method of the invention makes it possible to produce discrete and globally spherical antimonide nanoparticles whose average diameter is preferably less than or equal to 30 nm.
- discrete particles is intended to denote particles that are not aggregated with each other, that is to say non-agglomerated and that can be isolated individually.
- the present invention relates to metal antimonide nanoparticles (s) that can be obtained according to the method of the invention.
- the nanoparticles may more particularly be used in the form of a colloidal solution in a solvent, in particular in an apolar solvent, such as, for example, hexane, toluene or chloroform.
- apolar solvent such as, for example, hexane, toluene or chloroform.
- the colloidal solutions formed from the nanoparticles of the invention have good stability properties.
- the present invention relates to a colloidal solution of indium antimonide nanoparticles, comprising nanocrystals crystallized according to the Ino i5 Sbo cubic phase, and nanocrystals crystallized according to the Ino phase i4 Sbo, 6, with said nanoparticles having a dispersion in size less than 30%.
- the present invention relates to a colloidal solution of nanoparticles obtained by suspending the nanoparticles as defined above in a solvent. According to yet another of its aspects, the present invention aims at the use of these nanoparticles or a colloidal solution as defined above in solar cells, photodetectors, light converters, light emitting diodes, transistors , as fluorescent markers or in chemical or optical sensors.
- the method of the invention is more particularly aimed at the formation of antimonide nanoparticles whose metallic element is chosen from aluminum (Al), gallium (Ga), indium (In), thallium (Tl), zinc (Zn), cadmium (Cd), iron (Fe), cobalt (Co), nickel (Ni), bismuth (Bi), scandium (Se), titanium (Ti), vanadium (V), chromium (Cr), manganese (Mn), copper (Cu), rubidium (Rb), strontium (Sr), yttrium (Y), zirconium (Zr), niobium ( Nb), ruthenium (Ru), rhodium (Rh), palladium (Pd), silver (Ag), cesium (Cs), barium (Ba), hafhium (Hf), iridium ( Ir), platinum (Pt), gold (Au), tin (Sn), lead (Pb), and mixtures thereof.
- metallic element is chosen from aluminum
- the method of the invention allows the formation of antimonide nanoparticles whose metal element (s) is (are) chosen from aluminum, gallium , indium, thallium and mixtures thereof.
- the method of the invention makes it possible to form nanoparticles of indium antimonide (InSb).
- InSb indium antimonide
- the method of the invention more particularly comprises at least one step of placing antimony trihydride in contact with at least one precursor of a metal element under conditions conducive to the formation of said nanoparticles.
- the method of the invention comprises at least the steps of:
- reaction medium comprising at least one precursor of a metallic element whose antimonide and at least one solvent are to be formed
- Step (ii) more particularly comprises the injection of antimony trihydride into said reaction medium.
- Said precursor of the metal element may be the complex of said metal element with a fatty acid, in particular having a linear or branched carbon chain, saturated or unsaturated, having between 4 and 36 carbon atoms, preferably an alkyl chain linear comprising between 12 and 18 carbon atoms.
- Said fatty acid may be more particularly chosen from lauric acid, myristic acid, palmitic acid, stearic acid and oleic acid.
- an indium precursor may be indium myristate.
- said precursor of the metal element can be formed beforehand by reaction in a solvent, in particular under a primary vacuum, of an organic or inorganic salt of said metal element with a fatty acid with a chain linear or branched carbonaceous, saturated or unsaturated, having between 4 and 36 carbon atoms, preferably a linear alkyl chain having between 12 and 18 carbon atoms.
- organic or inorganic salt of said metal element is chosen in accordance with the general knowledge of those skilled in the art, and typically, for example, from acetates, acetylacetonates or metal halides.
- the solvent is an organic compound having a boiling point greater than 150 ° C., in particular chosen from saturated or unsaturated hydrocarbons, such as 1-octadecene.
- the precursor of the metal element may be present in a proportion of 1 to 100 millimoles per liter in the reaction medium.
- the formation reaction of said precursor of the metal element from the mixture of the salt of said metal element and the fatty acid may be more particularly carried out at a temperature ranging from 25 to 200 ° C., under vacuum or at ambient pressure.
- indium myristate can be obtained by reaction of indium acetate (In (Ac) 3 ) and myristic acid, in particular at a temperature of 220 ° C. under argon for fifteen minutes. minutes.
- the fatty acid or acids may be present in a proportion of 1 to 6 molar equivalents, relative to the organic or inorganic salt of the metal element.
- Said metal precursor may be generated, within the reaction medium, prior to the step (ii) of introduction of antimony trihydride.
- the reaction medium may further comprise one or more co-ligands.
- the presence of one or more co-ligands makes it possible to influence the size of the nanoparticles or to reduce their size dispersion.
- the said co-ligand (s) may be more particularly chosen from amines, in particular octylamine, decylamine, dodecylamine, tetradecylamine, hexadecylamine or oleylamine. Preferably, it is dodecylamine.
- the said co-ligand (s) may be present in the reaction medium in a proportion of 1 to 6 molar equivalents relative to the precursor of the metal element.
- the antimony trihydride can be produced from an aqueous solution of acidic pH (less than 7) of potassium tartrate and antimony, and potassium borohydride.
- the antimony trihydride can be generated by adding an acidic pH solution, for example sulfuric acid, with a mixture of tartrate of potassium and antimony and potassium borohydride, maintained at basic pH for example in a solution of potassium hydroxide.
- an acidic pH solution for example sulfuric acid
- a mixture of tartrate of potassium and antimony and potassium borohydride maintained at basic pH for example in a solution of potassium hydroxide.
- antimony trihydride is carried out under an inert atmosphere, for example under an argon or nitrogen atmosphere.
- antimony trihydride It is of course up to those skilled in the art to adjust the experimental conditions to form antimony trihydride.
- An example of a method for producing antimony trihydride is presented in the following examples.
- the antimony trihydride is formed simultaneously with its use in step (ii).
- the process of the invention may comprise the injection of antimony trihydride into the reaction medium as described above.
- the antimony trihydride is formed, for example according to the method described above, simultaneously with its introduction into said reaction medium.
- the method of the invention may thus comprise the following steps:
- step (b) contacting the antimony trihydride formed in step (a) with said reaction medium comprising at least one precursor of said metallic element, under conditions conducive to the formation of the antimonide nanoparticles,
- the antimony trihydride is introduced, as it is formed, into the reaction medium.
- a suitable installation as described in the following text and illustrated by the experimental setup of Figure 1.
- the reaction medium is maintained at a temperature T 2 ranging from 140 to 250 ° C., preferably from 150 ° C. to 220 ° C., throughout the duration of formation of the antimonide nanoparticles.
- the reaction medium is maintained under an inert atmosphere, for example under an argon atmosphere, for the entire duration of formation of the antimonide nanoparticles.
- the antimonide nanoparticles are more particularly obtained in the form of a colloidal solution of nanoparticles.
- the method may include one or more subsequent steps of washing and / or purifying the nanoparticles.
- the method of the invention may comprise a subsequent thermal annealing step of the nanoparticles. This annealing step makes it possible to increase the crystallinity of the nanoparticles formed.
- This annealing can be carried out at a temperature T 3 ranging from 200 to 300 ° C., in particular around 220 ° C., in particular under an inert atmosphere. It can be operated for a period ranging from 30 minutes to 4 hours, in particular for about 1 hour.
- the annealing is carried out in situ, so as to avoid bringing the solution into contact with the ambient air.
- the average diameter of the antimonide nanoparticles obtained may be between 2 and 150 nm, in particular between 5 and 85 nm.
- the average diameter can be evaluated by scanning electron scanning (STEM).
- the antimonide nanoparticles obtained according to the process of the invention have an average diameter less than or equal to 30 nm, preferably less than or equal to 20 nm.
- the nanoparticles obtained have a good dispersion in size, especially less than or equal to 30%, preferably less than or equal to 20%.
- the nanoparticles may have a dispersion in size ranging from 20 to 30%.
- the size dispersion can be evaluated by nanocrystal analysis by STEM.
- the antimonide nanoparticles obtained can be suspended in a solvent, in particular in an apolar solvent, such as, for example, hexane, toluene or chloroform, to form a stable colloidal solution.
- a solvent such as, for example, hexane, toluene or chloroform
- the method of the invention can be implemented using a suitable antimonide nanoparticle production facility, comprising at least:
- reaction medium comprising at least one precursor of the metal element whose antimonide is to be formed
- said first and second containers being connected by a fluid communication channel, adapted to ensure the passage of the antimony trihydride from the first vessel into the reaction medium of the second vessel.
- Figure 1 shows an experimental laboratory setup.
- This assembly is composed more particularly of a first flask (1) in which is formed the reaction medium including in particular said metal precursor, a second flask (2) in which is formed antimony trihydride, and a pipe (3) connecting the two balloons, and allowing the injection of the antimony trihydride generated from the balloon (2) to the balloon (1).
- the assembly assembly is maintained, during the implementation of the process of the invention, under an inert atmosphere, in particular under argon or nitrogen atmosphere.
- Figure 1 Diagram of an assembly used for the formation of antimonide nanoparticles.
- Figure 3 STEM image of InSb nanoparticles obtained according to the protocol described in Example 2.1. after purification and HRTEM cliché (box) of an isolated indium antimonide nanoparticle.
- FIG. 4 STEM image of the nanoparticles of InSb obtained according to the protocol described in example 2.2. after purification;
- Figure 5 Diagram of the assembly used for the formation of indium antimonide nanoparticles as an example 2.3. ;
- FIG. 6 STEM plate (FIG. 6.a) and histogram of the size dispersion (FIG. 6.b) of the InSb nanoparticles obtained according to the protocol described in example 2.3; HRTEM ( Figure 6.c) and Fourier transform (Figure 6.d) of an isolated nanoparticle.
- reaction medium 1st part of the assembly: reaction medium
- a first assembly is formed of the tricol (1) in which the reaction medium is previously prepared at the temperature Ti (80 ° C) under an inert atmosphere.
- the flask is connected to a water cooler, itself connected to a vacuum ramp arranged under a extractor hood. These operations are carried out in such a way that the reaction medium remains under an inert atmosphere during the entire process (Schlenk technique). Unused neck passes are sealed with septa.
- the upper end of the refrigerant is connected to a trap (4) containing an aqueous solution of silver nitrate (AgNO 3 ) (concentration 3 ⁇ 10 -2 mol / L) to neutralize the molecules of SbH 3 which does not have not reacted during the growth of nanocrystals.
- AgNO 3 silver nitrate
- inert gas argon
- T 2 140-250 ° C.
- the central neck of a second tricolor (2) in which the antimony trihydride will be produced, is connected to a desiccant column (6) containing a few grams of phosphorus pentoxide powder (P 2 0 5 ).
- Another neck of the balloon (2) is then connected to the vacuum ramp to establish a circulation of inert gas (argon) in the assembly, while the last mouth of the tricol has been closed by a septum.
- the top of the desiccant column is connected to the tricolor (1) via a pipe (3) terminated by a metal needle which we will take care to plunge into the reaction medium through one of the two free septa of the tricolor (1).
- the antimony trihydride thus produced, dried and then conveyed to the flask (1) will be dissociated in the reaction medium, resulting in the germination and then the growth of the antimonide nanocrystals of the element M.
- the excess of gas will be neutralized by reaction with silver nitrate in the trapping device (4) at the outlet of the refrigerant.
- the mixture is first agitated and inert, then heated to about 80 ° C under primary vacuum for about one hour to allow it to degass. After reestablishing the argon circulation, the solution is heated at 220 ° C for about fifteen minutes to form the indium precursor (indium myristate). The solution contained in the flask (1) is then brought to a temperature of 155 ° C.
- the tricolor (2) is in turn placed under an inert atmosphere and about 3 mL of sulfuric acid solution 1 mol / L previously degassed are introduced therein. 1.5 ml of solution (also degassed) of potassium hydroxide (KOH) at 0.8 mol / l are then added to the glass vial (a) already containing 0.15 mmol of potassium tartrate and antimony (APT) . After complete dissolution (an ultrasonic bath can advantageously accelerate the process), the mixture is transferred to the vial (b) in which 0.23 mmol of potassium borohydride (KBH 4 ) has been deposited. Everything is then injected as quickly as possible into the flask (2) in order to begin the production of SbH 3 .
- the pH of the mixture prepared in the bottle (b), initially basic, is in contact with the acid contained in the flask (2) brought to a value of less than 7. This has the effect of initiating the reaction between the powders APT and KBH 4 and start, with stirring, the production of antimony trihydride.
- the translucent solution contained in the flask (2) then rapidly turns black. During the first minutes of synthesis, the initially colorless reaction medium contained in the flask (1) quickly becomes pale yellow. The color then turns in a few minutes to dark yellow then to black-brown, a sign of the growth of nanocrystals. After a quarter of an hour after the start of production of antimony trihydride, the gas injection needle is removed from the tricolor (1) and immersed in a trap containing a silver nitrate solution .
- the nanocrystals thus obtained are annealed at 220 ° C. for forty-five minutes.
- the mixture is then rapidly cooled to 70-80 ° C and then injected into a vessel containing about 5 mL of toluene to prevent solidification of the dodecylamine (mp 27-29 ° C).
- EDX Energy dispersive analysis
- the diffractogram X (FIG. 2, curve a) is produced on a deposit of these purified nanocrystals and deposited on a disoriented silicon substrate. This diffractogram was recorded by a Philips X'Pert device with a cobalt source operating at 50 kV and 35 mA.
- the diffractogram X obtained has peaks corresponding to a structure "zinc zinc" identical to that of solid indium antimonide (JCPDS card No. 04-001-0014). Other peaks, less intense, would appear to come from a slightly richer cubic crystalline phase of antimony type Ino i4 Sbo, 6 (JCPDS map No. 01-074-5940), marked with asterisks (*) on Figure 2.
- the high-resolution transmission electron microscopy (HRTEM) (JEOL 4000EX, used at 400 kV) of an isolated nanocrystal (box, FIG. 3) confirms that the nanocrystals obtained are well crystallized.
- the atomic planes can indeed be distinguished there.
- the mixture is first stirred and inert, and then heated under vacuum at 80 ° C for about two hours to allow it to degass.
- the indium precursor indium myristate
- the solution contained in the flask (1) is then raised to a temperature of 215 ° C.
- the tricolor (2) is in turn put under an inert atmosphere and about 2 mL of sulfuric acid solution 1 mol / L degassed before are introduced therein. 1 ml of solution (also degassed) of potassium hydroxide (KOH) at 0.8 mol / l are then added to the glass vial (a) already containing 0.1 mmol of potassium tartrate and antimony (APT). After complete dissolution (an ultrasonic bath can advantageously accelerate the process), the mixture is transferred to the vial (b) in which 0.15 mmol of potassium borohydride (KBH 4 ) was deposited. Everything is then injected as quickly as possible into the flask (2) in order to begin the production of SbH 3 .
- KOH potassium hydroxide
- the coloration of the initially translucent reaction medium turns black in a few seconds.
- the gas injection needle is removed from the tricolor (1) and immersed in a trap containing a solution of silver nitrate. The mixture is then rapidly cooled to 70-80 ° C, and then injected into a vessel containing about 10 mL of toluene to prevent solidification of the dodecylamine (mp 27-29 ° C).
- the diffractogram X (FIG. 2, curve b) produced on a deposit of these same nanocrystals comprises peaks corresponding to a "zinc blende" structure identical to that of solid indium antimonide (JCPDS card No. 04 -001 to 0014). Other peaks, less intense, would seem to come from a cubic crystalline phase slightly richer in antimony type Ino i4 Sbo, 6 (JCPDS card No. 01-074-5940).
- the STEM shows that the particles have an average diameter of 85 nm, with a size dispersion of about 20%.
- the protocol implemented from the assembly described in FIG. 5, is as follows.
- the mixture is first agitated and inert, then heated to about 80 ° C under primary vacuum for about one hour to allow it to degass. After reestablishing the circulation of argon, the solution is heated to 220 ° C for about fifteen minutes to form the indium precursor (indium myristate). The solution contained in the flask (1) is then brought to a temperature of 165 ° C.
- the tricolor (2) is in turn placed under an inert atmosphere and about 6 mL of sulfuric acid solution 1 mol / L previously degassed are introduced therein. 3 ml of solution (also degassed) of potassium hydroxide (KOH) at 0.8 mol / l are then added to the glass vial (a) already containing 0.28 mmol of potassium tartrate and antimony (APT). After complete dissolution (an ultrasonic bath can advantageously accelerate the process), the mixture is transferred to the vial (b) in which 0.42 mmol of potassium borohydride (KBH 4 ) has been deposited. After closing valves RI and R2, the whole is then injected into the balloon (2) to begin the production of SbH 3 .
- KOH potassium hydroxide
- the pH of the mixture prepared in the bottle (b), initially basic, is in contact with the acid contained in the flask (2) brought to a value of less than 7. This has the effect of initiating the reaction between the powders APT and KBH 4 and start, with stirring, the production of antimony trihydride.
- the translucent solution contained in the flask (2) then rapidly turns black. After about a minute, the valves R1 and R2 are simultaneously open to allow the free flow of gas to the balloon (1).
- the initially colorless reaction medium contained in the flask (1) quickly becomes pale yellow. The color then turns in a few minutes to dark yellow then to black-brown, a sign of the growth of nanocrystals.
- the valves R1 and R2 are simultaneously closed. The gas injection needle is removed from the tricolor (1) and immersed in a trap containing a silver nitrate solution.
- the nanocrystals thus obtained are annealed at 220 ° C. for forty-five minutes.
- the mixture is then rapidly cooled to 70-80 ° C, and then injected into a vessel containing about 5 mL of toluene to prevent solidification of the dodecylamine.
- the scanning electron microscopy (STEM) image (Cari Zeiss Ultra 55+) (FIG. 6. a) shows that the particles have an average diameter of 9 nm, with a dispersion in size of less than 15% (FIG. .b).
Abstract
Description
Claims
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Application Number | Priority Date | Filing Date | Title |
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FR1251843A FR2987356B1 (fr) | 2012-02-29 | 2012-02-29 | Formation de nanoparticules d'antimoniures a partir du trihydrure d'antimoine comme source d'antimoine. |
PCT/IB2013/051452 WO2013128352A1 (fr) | 2012-02-29 | 2013-02-22 | Formation de nanoparticules d'antimoniures a partir du trihydrure d'antimoine comme source d'antimoine |
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EP2819952A1 true EP2819952A1 (fr) | 2015-01-07 |
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EP13716418.2A Withdrawn EP2819952A1 (fr) | 2012-02-29 | 2013-02-22 | Formation de nanoparticules d'antimoniures a partir du trihydrure d'antimoine comme source d'antimoine |
Country Status (4)
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US (1) | US20150053897A1 (fr) |
EP (1) | EP2819952A1 (fr) |
FR (1) | FR2987356B1 (fr) |
WO (1) | WO2013128352A1 (fr) |
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EP2959989B1 (fr) * | 2014-06-23 | 2017-08-02 | Belenos Clean Power Holding AG | Nanocristaux Sb ou nanocristaux d'alliage de Sb pour anodes de batterie Li-on et Na-ion à charge/décharge rapide |
DE102018202240A1 (de) * | 2018-02-14 | 2019-08-14 | Osram Gmbh | Verfahren zur objekterkennung |
CN108534055B (zh) * | 2018-03-05 | 2020-02-11 | 清华大学 | 一种荧光集光太阳能照明系统 |
CN113353979B (zh) * | 2021-06-04 | 2022-12-30 | 中国科学技术大学 | 一种Ga-GaSb纳米材料及其制备方法 |
WO2023171404A1 (fr) * | 2022-03-07 | 2023-09-14 | 富士フイルム株式会社 | Film semi-conducteur, élément de photodétection, capteur d'image et procédé de production de point quantique semi-conducteur |
WO2023171405A1 (fr) * | 2022-03-07 | 2023-09-14 | 富士フイルム株式会社 | Film semi-conducteur, élément de photodétection, capteur d'image, liquide de dispersion, et procédé de fabrication de film semi-conducteur |
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US5505928A (en) * | 1991-11-22 | 1996-04-09 | The Regents Of University Of California | Preparation of III-V semiconductor nanocrystals |
US5371257A (en) * | 1993-11-30 | 1994-12-06 | Gedridge, Jr.; Robert | Preparation of diisopropyl stibines and use thereof |
JP2006124262A (ja) * | 2004-11-01 | 2006-05-18 | Dainippon Printing Co Ltd | InSbナノ粒子 |
JPWO2008016154A1 (ja) * | 2006-07-31 | 2009-12-24 | Hoya株式会社 | 微粒子の製造方法および有機カルボン酸インジウムの製造方法 |
US20100116326A1 (en) * | 2006-10-19 | 2010-05-13 | The Regents Of The University Of California | Hybrid Solar Cells with 3-Dimensional Hyperbranched Nanocrystals |
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2012
- 2012-02-29 FR FR1251843A patent/FR2987356B1/fr not_active Expired - Fee Related
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2013
- 2013-02-22 EP EP13716418.2A patent/EP2819952A1/fr not_active Withdrawn
- 2013-02-22 WO PCT/IB2013/051452 patent/WO2013128352A1/fr active Application Filing
- 2013-02-22 US US14/382,103 patent/US20150053897A1/en not_active Abandoned
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FR2987356A1 (fr) | 2013-08-30 |
US20150053897A1 (en) | 2015-02-26 |
WO2013128352A1 (fr) | 2013-09-06 |
FR2987356B1 (fr) | 2015-03-06 |
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