CN111762809A - Lead-oxygen family compound dimer nanocrystalline, conductive film, preparation method and application - Google Patents
Lead-oxygen family compound dimer nanocrystalline, conductive film, preparation method and application Download PDFInfo
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- CN111762809A CN111762809A CN202010562062.7A CN202010562062A CN111762809A CN 111762809 A CN111762809 A CN 111762809A CN 202010562062 A CN202010562062 A CN 202010562062A CN 111762809 A CN111762809 A CN 111762809A
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- lead
- nanocrystal
- oxygen
- dimer
- nanocrystalline
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- 239000000539 dimer Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 150000001875 compounds Chemical class 0.000 title claims abstract description 25
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 24
- 239000001301 oxygen Substances 0.000 title claims abstract description 24
- 239000002159 nanocrystal Substances 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 32
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadec-1-ene Chemical compound CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims abstract description 24
- -1 bis (trimethylsilyl) oxide compound Chemical class 0.000 claims abstract description 18
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 238000007710 freezing Methods 0.000 claims abstract description 13
- 230000008014 freezing Effects 0.000 claims abstract description 13
- 150000007524 organic acids Chemical class 0.000 claims abstract description 13
- 238000000151 deposition Methods 0.000 claims abstract description 7
- 229910000464 lead oxide Inorganic materials 0.000 claims abstract description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 24
- 239000012295 chemical reaction liquid Substances 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 239000002904 solvent Substances 0.000 claims description 11
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 10
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 10
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 10
- 239000005642 Oleic acid Substances 0.000 claims description 10
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 10
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 10
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 10
- 239000011521 glass Substances 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 238000004528 spin coating Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 5
- 239000012454 non-polar solvent Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 4
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 4
- 229910052740 iodine Inorganic materials 0.000 claims description 4
- 239000011630 iodine Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- VAMFXQBUQXONLZ-UHFFFAOYSA-N n-alpha-eicosene Natural products CCCCCCCCCCCCCCCCCCC=C VAMFXQBUQXONLZ-UHFFFAOYSA-N 0.000 claims description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229940106006 1-eicosene Drugs 0.000 claims description 2
- FIKTURVKRGQNQD-UHFFFAOYSA-N 1-eicosene Natural products CCCCCCCCCCCCCCCCCC=CC(O)=O FIKTURVKRGQNQD-UHFFFAOYSA-N 0.000 claims description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- RLECCBFNWDXKPK-UHFFFAOYSA-N bis(trimethylsilyl)sulfide Chemical compound C[Si](C)(C)S[Si](C)(C)C RLECCBFNWDXKPK-UHFFFAOYSA-N 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims description 2
- 229910052736 halogen Inorganic materials 0.000 claims description 2
- 150000002367 halogens Chemical class 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 229940046892 lead acetate Drugs 0.000 claims description 2
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N mono-methylamine Natural products NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 2
- 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 claims description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 125000004079 stearyl 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])[H] 0.000 claims description 2
- FKIZDWBGWFWWOV-UHFFFAOYSA-N trimethyl(trimethylsilylselanyl)silane Chemical compound C[Si](C)(C)[Se][Si](C)(C)C FKIZDWBGWFWWOV-UHFFFAOYSA-N 0.000 claims description 2
- VMDCDZDSJKQVBK-UHFFFAOYSA-N trimethyl(trimethylsilyltellanyl)silane Chemical compound C[Si](C)(C)[Te][Si](C)(C)C VMDCDZDSJKQVBK-UHFFFAOYSA-N 0.000 claims description 2
- 239000003446 ligand Substances 0.000 abstract description 26
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 32
- 239000010408 film Substances 0.000 description 29
- 230000000052 comparative effect Effects 0.000 description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical class [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- 238000001000 micrograph Methods 0.000 description 8
- 230000005525 hole transport Effects 0.000 description 7
- 239000002245 particle Substances 0.000 description 5
- 239000010409 thin film Substances 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000002707 nanocrystalline material Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- DHBXNPKRAUYBTH-UHFFFAOYSA-N 1,1-ethanedithiol Chemical compound CC(S)S DHBXNPKRAUYBTH-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000013110 organic ligand Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- QHJPGANWSLEMTI-UHFFFAOYSA-N aminomethylideneazanium;iodide Chemical compound I.NC=N QHJPGANWSLEMTI-UHFFFAOYSA-N 0.000 description 2
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000011669 selenium Chemical group 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- VYMPLPIFKRHAAC-UHFFFAOYSA-N 1,2-ethanedithiol Chemical compound SCCS VYMPLPIFKRHAAC-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical group [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 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
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/21—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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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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- 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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- 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
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- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
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- 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
- H01L31/0256—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 the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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- H01L31/06—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 adapted as photovoltaic [PV] conversion devices characterised by potential barriers
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Abstract
The invention discloses a lead-oxygen family compound dimer nanocrystal, a conductive film, a preparation method and application. Preparing a lead precursor by using a lead reagent, organic acid and 1-octadecene; reacting a bis (trimethylsilyl) oxide compound and 1-octadecene with the obtained lead precursor, freezing the obtained solution, and performing post-treatment to obtain the halogen-doped lead oxide compound nanocrystal. The lead-oxygen family compound dimer nanocrystalline provided by the invention can enable the arrangement of the nanocrystalline to be more disordered in the process of depositing the film, avoid the formation of crystal boundary, and further avoid the formation of cracks in the subsequent ligand exchange process. By utilizing the preparation method provided by the invention, the preparation process of the nanocrystalline solar cell device can be greatly simplified.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a lead-oxygen family compound dimer nanocrystal, a conductive film, a preparation method thereof and application thereof in preparing a solar cell.
Background
PbX of groups IV-VI (X = sulfur, selenium, tellurium) has a large bohr radius, making its quantum confinement effect particularly pronounced. The band gap of the nanocrystalline material can be greatly adjusted through size adjustment, the absorption spectrum of the nanocrystalline material can be well matched with the solar spectrum reaching the earth surface, and meanwhile, the nanocrystalline material has the characteristics of large absorption coefficient, high electron mobility, adjustable energy level and the like, so that the IV-VI group nanocrystalline becomes the most popular photovoltaic nanomaterial at the present stage, and is expected to become a low-cost and high-efficiency solar cell of a new generation of solution process.
At present, most of nanocrystalline materials used in the preparation of PbX nanocrystalline solar cells are synthesized based on a classical thermal injection method, the method needs to use a long-chain organic ligand (oleic acid) to control the growth of nanocrystals, but the long-chain organic ligand enables the nanocrystals to be mutually insulated, and the long-chain organic ligand is exchanged into a short ligand to enhance the conductivity of a nanocrystalline film in the process of preparing a photoelectric device through a ligand exchange step. The ligand exchange step is an extremely important link in the preparation process of the PbS nanocrystalline solar cell, and can be divided into the following two types according to different ligand exchange modes:
(1) solid-state ligand exchange: the method is wide in applicability and is the most widely applied method for early nanocrystalline solar cells. However, in order to ensure sufficient ligand exchange and film compactness in the method, the thickness of each film layer can be controlled to be dozens of nanometers, the process usually needs to be repeated for about 10 times to obtain a photovoltaic active layer with the required thickness, and the preparation process is extremely complicated. And researches show that the solid-state exchange has the problem of uneven exchange, and the surface of the nanocrystal can be damaged by repeated polar solvent washing, so that a defect state is introduced.
(2) Solution phase ligand exchange: to avoid the disadvantages of solid-state ligand exchange, solution phase ligand exchange processes have recently been extensively studied. In the method, PbX nano-crystals synthesized by a thermal injection method are dispersed in a non-polar solvent (n-hexane or n-octane) and stirred with a dimethylformamide solution of lead halide, ligand exchange is completed in a solution phase, surface oleic acid is replaced by lead halide, and then the PbX nano-crystals are dispersed in a butylamine solution to form PbX nano-crystal ink which is directly prepared into a conductive film. Compared with solid-state exchange, the method simplifies the device preparation process and avoids the damage of multiple exchanges to the surface of the nanocrystal. However, the method needs to consume a large amount of expensive lead halide salt and a solvent with high toxicity, and the prepared nanocrystalline ink has poor stability, is not beneficial to large-scale application and still has great limitation.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a lead-oxygen compound dimer nanocrystal, a conductive film, a preparation method and application thereof. The device performance of the nanocrystalline prepared by the method in the solar cell is further used for preparing the corresponding solar cell. The method can effectively solve the problems of complex solid ligand exchange and unstable solution phase ligand exchange solution in the prior art, and is expected to provide a new way for the mass production of nanocrystalline solar cells in the future.
In order to achieve the above object, the present invention adopts a technical scheme that a preparation method of a lead-oxygen family compound dimer nanocrystal is provided, which comprises the following steps:
1) adding a lead reagent, an organic acid and a solvent into a reaction container, wherein the molar ratio of the lead reagent to the organic acid is 1: 2.5-5; stirring and vacuumizing for 1-2 hours until the lead reagent is completely dissolved, and obtaining a lead precursor, wherein the reaction liquid is bubble-free and is clear and transparent;
2) introducing inert gas into a reaction container, uniformly mixing a bis (trimethylsilyl) oxygen compound and 1-octadecene serving as a solvent at the temperature of 60-180 ℃, quickly transferring the mixture into the lead precursor obtained in the step 1), and continuously reacting for 0.5-30 minutes;
3) after the reaction is finished, cooling the reaction liquid to room temperature, adding n-hexane, freezing the reaction liquid, and removing bottom sediment through centrifugation;
4) and precipitating the upper solution by isopropanol and acetone, centrifuging, removing the upper solution, and performing vacuum pumping to obtain the lead-oxygen compound dimer nanocrystal.
The preferable scheme of the preparation method of the lead-oxygen family compound dimer nanocrystal is as follows:
the lead reagent in the step 1) is any one of lead oxide, lead acetate, lead chloride, lead bromide and lead iodide; the organic acid is any one of oleic acid, octadecyl acid and hexadecyl acid; the solvent is any one of 1-octadecene, 1-eicosene and diphenyl ether; in the step 1), the organic acid is oleic acid, and the molar ratio of the lead reagent to the oleic acid is 1: 2.5.
The inert gas in the step 2) is any one of nitrogen, helium and neon; the bis (trimethylsilyl) oxy compound is bis (trimethylsilyl) sulfide ((TMS)2S), bis (trimethylsilyl) selenide ((TMS)2Se), bis (trimethylsilyl) telluride ((TMS)2Te) is used.
The condition of the freezing treatment in the step 3) is that the freezing temperature is 0-5 ℃ and the freezing time is 10-60 minutes.
The technical scheme of the invention comprises the lead-oxygen family compound dimer nanocrystalline obtained by the preparation method.
The technical scheme of the invention also provides a preparation method of the conductive film based on the lead-oxygen family compound dimer nanocrystalline, which comprises the following steps:
1) adding a lead reagent, an organic acid and a solvent into a reaction container, wherein the molar ratio of the lead reagent to the organic acid is 1: 2.5-5; stirring and vacuumizing for 1-2 hours until the lead reagent is completely dissolved, and obtaining a lead precursor, wherein the reaction liquid is bubble-free and is clear and transparent;
2) introducing inert gas into a reaction container, uniformly mixing a bis (trimethylsilyl) oxygen compound and 1-octadecene serving as a solvent at the temperature of 60-180 ℃, quickly transferring the mixture into the lead precursor obtained in the step 1), and continuously reacting for 0.5-30 minutes;
3) after the reaction is finished, cooling the reaction liquid to room temperature, adding n-hexane, freezing the reaction liquid, and removing bottom sediment through centrifugation;
4) precipitating the upper layer solution by isopropanol and acetone, centrifuging, removing the upper layer solution, and performing vacuum pumping to obtain lead-oxygen compound dimer nanocrystal;
5) dissolving lead-oxygen family compound dimer nano-crystal in a nonpolar solvent, wherein the concentration of the solution is 10-1000 mg/mL, and depositing the solution on a substrate in a spin coating manner to form a film;
6) dissolving iodide in an alcohol solution, wherein the concentration of the solution is 2-100 mM; and (3) dropwise adding the solution onto the film prepared in the step 5), soaking for 50-300 seconds, then spin-drying, and then washing with isopropanol and acetonitrile to obtain the conductive film.
The preparation method of the conductive film based on the lead-oxygen compound dimer nanocrystal preferably adopts the following scheme: the nonpolar solvent comprises normal hexane, normal octane, toluene and chloroform; the substrate comprises common glass, transparent conductive glass, a silicon wafer, silicon oxide, quartz and polyethylene terephthalate; the halide comprises formamidine halide, ammonia halide, methylamine halide, tetrabutylammonium halide and tetramethylammonium halide; halogens include chlorine, bromine and iodine.
The technical scheme of the invention comprises the conductive film based on the lead-oxygen family compound dimer nanocrystalline obtained by the preparation method.
The technical scheme of the invention provides an application of a conductive film based on a lead-oxygen family compound dimer nanocrystal in preparation of a solar cell.
Compared with the prior art, the invention adopting the technical scheme has the following advantages:
1) the preparation method of the invention provides a simple method for preparing the lead-oxygen family compound dimer nanocrystal;
2) the preparation method is simple and easy to implement, and the lead-oxygen family compound dimer nanocrystalline is used for realizing one-layer ligand exchange through a simple solid-phase ligand exchange method to obtain a conductive nanocrystalline film without cracks so as to prepare the solar cell, and the whole preparation process is greatly simplified compared with the traditional method.
Drawings
Fig. 1 is a projection electron microscope image and a particle size statistical image of a general PbS nanocrystal and a PbS dimer nanocrystal provided by an embodiment of the present invention;
fig. 2 is a top view and a cross-sectional scanning electron microscope image after ligand exchange of a thin film prepared based on a common PbS nanocrystal and a PbS dimer nanocrystal provided by an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a nanocrystalline solar cell device;
FIG. 4 is a graph of current versus voltage for different device structures;
in the figure, 1. a glass substrate; 2. a cathode layer; 3. an electron transport layer; 4. an active layer; a hole transport layer; and 6, anode layer.
Detailed Description
The invention is further described with reference to the following figures and specific embodiments. Unless otherwise specifically indicated, materials, reagents and instruments used in the following examples are commercially available.
Example 1:
this example provides a PbS dimer nanocrystal, which is prepared by the following steps:
1) adding 450 mg (1 mmol) of lead oxide, 1.4 g (2.5 mmol) of oleic acid and 20 g of 1-octadecene into a three-neck flask, stirring at 100 ℃, and vacuumizing for 1 h to obtain a lead precursor for later use;
2) introducing nitrogen into a three-neck flaskAir, and adjust the temperature to 75 ℃, 210 μ L (TMS)2S and 5 mL of 1-octadecene are uniformly mixed, quickly injected into the lead precursor by an injector and continuously reacted for 10 min;
3) after the reaction is finished, cooling the water bath to room temperature, injecting 8 mL of anhydrous n-hexane, transferring the reaction liquid into a centrifuge tube, transferring the reaction liquid into a refrigerator, freezing the reaction liquid at 4 ℃ for 60 min, centrifuging the reaction liquid for 3 min by a centrifuge (the rotating speed is 6000 rpm), and removing the lower-layer solid;
4) adding isopropanol into the upper layer solution obtained in the step 3) until the reaction solution becomes turbid, centrifuging for 5 min by a centrifuge (the rotating speed is 8000 rpm), discarding the upper layer solution, dissolving by using n-hexane, adding acetone, centrifuging, discarding the upper layer solution, drying the residual solid in vacuum to obtain the required nanocrystal, and storing in a glove box. The transmission electron microscope image and the particle size statistics are shown in FIG. 1.
The procedure for preparing PbS nanocrystalline comparative example 1 was as follows:
1) adding 450 mg (1 mmol) of lead oxide, 1.4 g (2.5 mmol) of oleic acid and 20 g of 1-octadecene into a three-neck flask, stirring at 100 ℃, and vacuumizing for 1 h to obtain a lead precursor for later use;
2) into a three-necked flask, nitrogen gas was introduced while adjusting the temperature to 75 ℃ and 210. mu.L of (TMS)2S and 5 mL of 1-octadecene are uniformly mixed, quickly injected into the lead precursor by an injector and continuously reacted for 10 min;
3) after the reaction is finished, cooling the water bath to room temperature, injecting 8 mL of anhydrous n-hexane, transferring the reaction liquid into a centrifuge tube, adding isopropanol until the reaction liquid becomes turbid, centrifuging for 5 min by a centrifuge (the rotation speed is 8000 rpm), discarding the supernatant, dissolving by the n-hexane, adding acetone, centrifuging, discarding the supernatant, drying the residual solid under vacuum to obtain the required nanocrystal, placing the nanocrystal in a glove box for storage, wherein the projection electron microscope diagram and the particle size statistics are shown in figure 1.
Referring to fig. 1, it is a projection electron microscope image and a particle size statistical image of a common PbS nanocrystal (comparative example 1) and a PbS dimer nanocrystal provided in this example; wherein, the images a and b are respectively projection electron microscope images of a common PbS nanocrystal (comparative example 1) and a PbS dimer nanocrystal provided by the embodiment, the scale in the images represents 20 nm, and the scale in the embedded high-resolution projection electron microscope represents 2 nm; and c and d are particle size statistical graphs of a common PbS nanocrystal (comparative example 1) and the PbS dimer nanocrystal provided in this example, respectively, and it can be seen from the graphs that the synthesis of the conventional PbS nanocrystal is spherical with an average diameter of 3.4 nm, and the invention can obtain the PbS dimer with an average length of 5.5 nm by freezing the solution after the reaction.
Example 2:
the embodiment provides a method for realizing crack-free film deposition based on PbS dimer nanocrystals, which comprises the following steps:
1) the PbS dimer nanocrystal prepared in example 1 is dissolved in n-hexane, the concentration is 50-500 mg/mL, and the PbS dimer nanocrystal is deposited on a substrate in a spin coating mode, wherein the rotation speed is 1500 rpm.
2) A solution of formamidine iodide in isopropanol was prepared at a concentration of 25 mM. The solution was added dropwise to the above film, soaked for 80 s and then spin-dried. And washing twice with isopropanol and once with acetonitrile to obtain the film based on the PbS dimer nanocrystal.
A comparative example 2 based on a common PbS nanocrystalline film was prepared as follows:
1) and dissolving the common PbS nano-crystal prepared in the comparative example 1 in n-hexane, wherein the concentration of the nano-crystal is 50-500 mg/mL, and depositing the nano-crystal on a substrate in a spin coating mode at the rotating speed of 1500 rpm.
2) A solution of formamidine iodide in isopropanol was prepared at a concentration of 25 mM. The solution was added dropwise to the above film, soaked for 80 s and then spin-dried. And washing twice with isopropanol and once with acetonitrile to obtain the PbS nanocrystalline film.
Referring to fig. 2, a top view and a cross-sectional scanning electron microscope image after ligand exchange of a thin film prepared based on a common PbS nanocrystal and a PbS dimer nanocrystal provided by an embodiment of the present invention are shown; wherein, the images a and b are respectively top scanning electron microscope images after ligand exchange of films prepared based on the common PbS nanocrystals and the PbS dimer nanocrystals provided by the embodiment of the invention, and the scale in the images a and b represents 4 microns; c, d are respectively cross-sectional scanning electron microscope images after ligand exchange of films prepared on the basis of the common PbS nanocrystals and the PbS dimer nanocrystals provided by the embodiment of the invention, and the scale in the c, d represents 1 micron; as can be seen from the scanning electron microscope pictures, the film prepared using the conventional PbS nanocrystals had severe cracks, and the cross-sectional view showed that the cracks would traverse the entire film. The film prepared by the PbS dimer nanocrystalline can completely avoid the generation of cracks, and a compact film is obtained by single deposition through solid phase ligand exchange, and the thickness of the film can reach nearly 1 micron. And obtaining a dense conductive nanocrystalline thin film is a necessary condition for preparing high-performance devices.
Example 3:
referring to fig. 3, it is a schematic diagram of a device structure of the nanocrystalline solar cell provided in this embodiment; the solar photovoltaic device provided by the embodiment comprises glass 1, wherein a cathode layer 2 is attached to the glass, an electron transport layer 3 attached to the cathode layer, an active layer 4 attached to the electron transport layer, a hole transport layer 5 attached to the active layer, and an anode layer 6 attached to the hole transport layer.
In this example, a solar cell based on PbS dimer nanocrystals was fabricated by depositing active layers of different thicknesses at a time through the steps in example 2, and obtaining a dense crack-free conductive thin film through solid-phase ligand exchange. In this embodiment, the active layer 4 is an iodine-coated PbS dimer nanocrystal, the hole transport layer 5 is an ethylene dithiol-coated ordinary PbS nanocrystal, and the anode layer 6 is gold.
The preparation method comprises the following steps: sequentially spin-coating ZnO and PbS dimer nanocrystalline solution on a cleaned conductive glass substrate, adopting the technical scheme of the embodiment 2 to perform ligand exchange, then spin-coating common PbS nanocrystalline (as described in a comparative example 1), performing ethanedithiol ligand exchange, and then evaporating gold with the thickness of 100 nm to obtain the nano-gold-doped zinc oxide/zinc oxide composite material; wherein: the mass volume concentration of the active layer nanocrystal solution is 200 mg/mL; the PbS nanocrystal of the hole transport layer is 20 mg/mL; the rotation speed when the nanocrystalline solution was spin coated was 1500 rpm for 20 s.
The preparation method of the common PbS nanocrystalline solar cell comparative example 3 is as follows:
the device structure of the nanocrystalline solar cell is shown in fig. 3, in which: the active layer 4 is iodine-coated PbS common nanocrystalline, the hole transport layer 5 is ethanedithiol-coated common PbS nanocrystalline, the cathode layer 2 is ITO, the electron transport layer 3 is zinc oxide, and the anode layer 6 is gold.
The preparation method comprises the following steps: sequentially spin-coating ZnO and common PbS nanocrystal solution on a cleaned conductive glass substrate, performing ligand exchange according to the technical scheme of comparative example 2 in example 2, then spin-coating common PbS nanocrystals (as described in comparative example 1), performing ethanedithiol ligand exchange, and then evaporating gold with the thickness of 100 nm to obtain the final product; wherein: the mass volume concentration of the active layer nanocrystal solution is 200 mg/mL; the PbS nanocrystal of the hole transport layer is 20 mg/mL; the rotation speed when the nanocrystalline solution was spin coated was 1500 rpm for 20 s.
A summary of the performance parameters of the solar cells of the different devices prepared in this example is given in table 1.
TABLE 1 summary of solar cell Performance parameters for different devices
| Device with a metal layer | Short circuit current (mA/cm)2) | Open circuit voltage (V) | Filling factor (%) | Conversion efficiency (%) |
| Ordinary PbS nanocrystal (comparative example 3) | 25.31 | 0.62 | 68.0 | 10.67 |
| PbS dimer nanocrystal (example) | 22.06 | 0.41 | 53.5 | 4.84 |
As can be seen from table 1, the active layer thin film prepared by PbS dimer nanocrystals can achieve complete crack-free, exhibiting excellent device properties. However, the film deposited by the common PbS nanocrystal can generate serious cracks due to the stress action in the ligand exchange process, and the performance of the device is greatly reduced.
Claims (10)
1. A preparation method of lead-oxygen family compound dimer nanocrystalline is characterized by comprising the following steps:
1) adding a lead reagent, an organic acid and a solvent into a reaction container, wherein the molar ratio of the lead reagent to the organic acid is 1: 2.5-5; stirring and vacuumizing for 1-2 hours until the lead reagent is completely dissolved, and obtaining a lead precursor, wherein the reaction liquid is bubble-free and is clear and transparent;
2) introducing inert gas into a reaction container, uniformly mixing a bis (trimethylsilyl) oxygen compound and 1-octadecene serving as a solvent at the temperature of 60-180 ℃, quickly transferring the mixture into the lead precursor obtained in the step 1), and continuously reacting for 0.5-30 minutes;
3) after the reaction is finished, cooling the reaction liquid to room temperature, adding n-hexane, freezing the reaction liquid, and removing bottom sediment through centrifugation;
4) and precipitating the upper solution by isopropanol and acetone, centrifuging, removing the upper solution, and performing vacuum pumping to obtain the lead-oxygen compound dimer nanocrystal.
2. The method for preparing a lead-oxygen family compound dimer nanocrystal according to claim 1, wherein the method comprises the following steps: the lead reagent in the step 1) is any one of lead oxide, lead acetate, lead chloride, lead bromide and lead iodide; the organic acid is any one of oleic acid, octadecyl acid and hexadecyl acid; the solvent is any one of 1-octadecene, 1-eicosene and diphenyl ether.
3. The method for preparing a lead-oxygen family compound dimer nanocrystal according to claim 1, wherein the method comprises the following steps: the inert gas in the step 2) is any one of nitrogen, helium and neon; the bis (trimethylsilyl) oxygen family compound is any one of bis (trimethylsilyl) sulfide, bis (trimethylsilyl) selenide and bis (trimethylsilyl) telluride.
4. The method for preparing a lead-oxygen family compound dimer nanocrystal according to claim 1, wherein the method comprises the following steps: in the step 1), the organic acid is oleic acid, and the molar ratio of the lead reagent to the oleic acid is 1: 2.5.
5. The method for preparing a lead-oxygen family compound dimer nanocrystal according to claim 1, wherein the method comprises the following steps: the condition of the freezing treatment in the step 3) is that the freezing temperature is 0-5 ℃ and the freezing time is 10-60 minutes.
6. A lead-oxygen family compound dimer nanocrystal obtained by the preparation method of claim 1.
7. A preparation method of a conductive film based on lead-oxygen family compound dimer nanocrystalline is characterized by comprising the following steps:
1) adding a lead reagent, an organic acid and a solvent into a reaction container, wherein the molar ratio of the lead reagent to the organic acid is 1: 2.5-5; stirring and vacuumizing for 1-2 hours until the lead reagent is completely dissolved, and obtaining a lead precursor, wherein the reaction liquid is bubble-free and is clear and transparent;
2) introducing inert gas into a reaction container, uniformly mixing a bis (trimethylsilyl) oxygen compound and 1-octadecene serving as a solvent at the temperature of 60-180 ℃, quickly transferring the mixture into the lead precursor obtained in the step 1), and continuously reacting for 0.5-30 minutes;
3) after the reaction is finished, cooling the reaction liquid to room temperature, adding n-hexane, freezing the reaction liquid, and removing bottom sediment through centrifugation;
4) precipitating the upper layer solution by isopropanol and acetone, centrifuging, removing the upper layer solution, and performing vacuum pumping to obtain lead-oxygen compound dimer nanocrystal;
5) dissolving lead-oxygen family compound dimer nano-crystal in a nonpolar solvent, wherein the concentration of the solution is 10-1000 mg/mL, and depositing the solution on a substrate in a spin coating manner to form a film;
6) dissolving iodide in an alcohol solution, wherein the concentration of the solution is 2-100 mM; and (3) dropwise adding the solution onto the film prepared in the step 5), soaking for 50-300 seconds, then spin-drying, and then washing with isopropanol and acetonitrile to obtain the conductive film.
8. The method for preparing a conductive film based on lead-oxygen family compound dimer nanocrystalline according to claim 7, characterized in that: the nonpolar solvent comprises normal hexane, normal octane, toluene and chloroform; the substrate comprises common glass, transparent conductive glass, a silicon wafer, silicon oxide, quartz and polyethylene terephthalate; the halide comprises formamidine halide, ammonia halide, methylamine halide, tetrabutylammonium halide and tetramethylammonium halide; halogens include chlorine, bromine and iodine.
9. A conductive film based on a lead-oxygen family compound dimer nanocrystal obtained by the preparation method of claim 7.
10. Use of a conductive film based on nanocrystals of lead-oxy group compounds dimers as defined in claim 9 for the preparation of solar cells.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050120946A1 (en) * | 2003-12-04 | 2005-06-09 | Hines Margaret A. | Synthesis of colloidal PbS nanocrystals with size tunable NIR emission |
| CN1952038A (en) * | 2005-10-21 | 2007-04-25 | 中国科学院上海应用物理研究所 | Cadmium sulfide bare quantum spot and preparation process |
| CN101208605A (en) * | 2005-05-04 | 2008-06-25 | 新加坡科技研究局 | New type water-solubility nanocrystalline containing low molecular weight coating agent and preparation method thereof |
| US20120132891A1 (en) * | 2010-07-14 | 2012-05-31 | University Of Utah Research Foundation | Precision quantum dot clusters |
| CN102969560A (en) * | 2012-10-26 | 2013-03-13 | 中国科学院福建物质结构研究所 | Cu2S-ZnS dimer heterojunction nano antenna with adjustable resonance wavelength and synthetic method thereof |
| CN103413892A (en) * | 2013-07-17 | 2013-11-27 | 苏州大学 | Alloy quantum dot PbSxSe1-x, preparation method thereof and application of alloy quantum dot PbSxSe1-x in solar cell |
| CN105161562A (en) * | 2015-09-15 | 2015-12-16 | 华南理工大学 | PbS quantum dot heterojunction solar cell employing solvent regulation and control and preparation method of PbS quantum-dot heterojunction solar cell |
| CN105679858A (en) * | 2016-01-20 | 2016-06-15 | 苏州大学 | Nanocrystalline composite center-based stacked solar cell and preparation method thereof |
| CN105742384A (en) * | 2016-03-18 | 2016-07-06 | 苏州大学 | Halogen-doped lead chalcogenide nanometer crystal and preparation method and application thereof |
| CN109273601A (en) * | 2018-09-06 | 2019-01-25 | 华中科技大学 | A kind of perovskite solar battery and preparation method thereof |
-
2020
- 2020-06-18 CN CN202010562062.7A patent/CN111762809B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050120946A1 (en) * | 2003-12-04 | 2005-06-09 | Hines Margaret A. | Synthesis of colloidal PbS nanocrystals with size tunable NIR emission |
| CN101208605A (en) * | 2005-05-04 | 2008-06-25 | 新加坡科技研究局 | New type water-solubility nanocrystalline containing low molecular weight coating agent and preparation method thereof |
| CN1952038A (en) * | 2005-10-21 | 2007-04-25 | 中国科学院上海应用物理研究所 | Cadmium sulfide bare quantum spot and preparation process |
| US20120132891A1 (en) * | 2010-07-14 | 2012-05-31 | University Of Utah Research Foundation | Precision quantum dot clusters |
| CN102969560A (en) * | 2012-10-26 | 2013-03-13 | 中国科学院福建物质结构研究所 | Cu2S-ZnS dimer heterojunction nano antenna with adjustable resonance wavelength and synthetic method thereof |
| CN103413892A (en) * | 2013-07-17 | 2013-11-27 | 苏州大学 | Alloy quantum dot PbSxSe1-x, preparation method thereof and application of alloy quantum dot PbSxSe1-x in solar cell |
| CN105161562A (en) * | 2015-09-15 | 2015-12-16 | 华南理工大学 | PbS quantum dot heterojunction solar cell employing solvent regulation and control and preparation method of PbS quantum-dot heterojunction solar cell |
| CN105679858A (en) * | 2016-01-20 | 2016-06-15 | 苏州大学 | Nanocrystalline composite center-based stacked solar cell and preparation method thereof |
| CN105742384A (en) * | 2016-03-18 | 2016-07-06 | 苏州大学 | Halogen-doped lead chalcogenide nanometer crystal and preparation method and application thereof |
| CN109273601A (en) * | 2018-09-06 | 2019-01-25 | 华中科技大学 | A kind of perovskite solar battery and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| BARBARA K. HUGHES ET AL.: "Synthesis and Spectroscopy of PbSe Fused Quantum-Dot Dimers", vol. 136, pages 4670 - 4679, XP055675487, DOI: 10.1021/ja413026h * |
| 刘娟;李云白;侯延冰;王越;吕龙峰;: "基于PVK/PbS纳米晶有机无机复合薄膜电双稳器件性能研究", no. 07, pages 12 - 17 * |
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