CN111762809B - Lead-oxygen compound dimer nanocrystalline, conductive film, preparation method and application - Google Patents
Lead-oxygen compound dimer nanocrystalline, conductive film, preparation method and application Download PDFInfo
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- CN111762809B CN111762809B CN202010562062.7A CN202010562062A CN111762809B CN 111762809 B CN111762809 B CN 111762809B CN 202010562062 A CN202010562062 A CN 202010562062A CN 111762809 B CN111762809 B CN 111762809B
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- lead
- nanocrystalline
- dimer
- trimethylsilyl
- solution
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- 239000000539 dimer Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000002159 nanocrystal Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 28
- -1 di (trimethylsilyl) oxy compound Chemical class 0.000 claims abstract description 24
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadec-1-ene Chemical compound CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 14
- 150000007524 organic acids Chemical class 0.000 claims abstract description 13
- 238000000151 deposition Methods 0.000 claims abstract description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 26
- 238000006243 chemical reaction Methods 0.000 claims description 25
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 24
- 238000007710 freezing Methods 0.000 claims description 15
- 230000008014 freezing Effects 0.000 claims description 15
- 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
- 238000004528 spin coating Methods 0.000 claims description 10
- 239000012295 chemical reaction liquid Substances 0.000 claims description 9
- 239000011521 glass Substances 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 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
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 6
- 239000012454 non-polar solvent Substances 0.000 claims description 5
- 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
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 claims description 4
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 4
- 229910000464 lead oxide Inorganic materials 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
- 229910052757 nitrogen Inorganic materials 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
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- RLECCBFNWDXKPK-UHFFFAOYSA-N bis(trimethylsilyl)sulfide Chemical compound C[Si](C)(C)S[Si](C)(C)C RLECCBFNWDXKPK-UHFFFAOYSA-N 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- FKIZDWBGWFWWOV-UHFFFAOYSA-N trimethyl(trimethylsilylselanyl)silane Chemical compound C[Si](C)(C)[Se][Si](C)(C)C FKIZDWBGWFWWOV-UHFFFAOYSA-N 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
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000021314 Palmitic acid Nutrition 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 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
- 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
- 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
- 239000010703 silicon Substances 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- XSOKHXFFCGXDJZ-UHFFFAOYSA-N telluride(2-) Chemical compound [Te-2] XSOKHXFFCGXDJZ-UHFFFAOYSA-N 0.000 claims 2
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 claims 2
- 239000003446 ligand Substances 0.000 abstract description 27
- 229910052736 halogen Inorganic materials 0.000 abstract description 2
- 150000002367 halogens Chemical class 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 2
- 239000000243 solution Substances 0.000 description 37
- 239000010408 film Substances 0.000 description 34
- 230000000052 comparative effect Effects 0.000 description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical class [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- 239000007787 solid Substances 0.000 description 9
- 230000005525 hole transport Effects 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 7
- 239000002707 nanocrystalline material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 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
- DHBXNPKRAUYBTH-UHFFFAOYSA-N 1,1-ethanedithiol Chemical compound CC(S)S DHBXNPKRAUYBTH-UHFFFAOYSA-N 0.000 description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-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
- 230000008021 deposition Effects 0.000 description 3
- 229910052740 iodine Inorganic materials 0.000 description 3
- 239000011630 iodine Substances 0.000 description 3
- 239000013110 organic ligand Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 150000004820 halides Chemical group 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011669 selenium Substances 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
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [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
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- VMDCDZDSJKQVBK-UHFFFAOYSA-N trimethyl(trimethylsilyltellanyl)silane Chemical compound C[Si](C)(C)[Te][Si](C)(C)C VMDCDZDSJKQVBK-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/002—Processes for applying liquids or other fluent materials the substrate being rotated
- B05D1/005—Spin coating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
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- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/007—Tellurides or selenides of metals
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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
- H01L31/0256—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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- H01L31/0248—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
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- H01L31/04—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
- 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 compound dimer nanocrystal, a conductive film, a preparation method and application thereof. Preparing a lead precursor by using a lead reagent, an organic acid and 1-octadecene; the di (trimethylsilyl) oxy compound, 1-octadecene and the obtained lead precursor are reacted, the obtained solution is frozen, and then the halogen doped lead oxy compound nanocrystalline is obtained through post-treatment. The lead-oxygen compound dimer nanocrystalline provided by the invention can enable the arrangement of nanocrystalline to be more disordered in the process of depositing the film, avoid the formation of grain boundaries, 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 compound dimer nanocrystal, a conductive film, a preparation method thereof and application thereof in preparation of solar cells.
Background
Group IV-VI PbX (x=sulfur, selenium, tellurium) has a very 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 the nanocrystalline material has the characteristics of large absorption coefficient, high electron mobility, adjustable energy level and the like, so that IV-VI family nanocrystalline is the most popular photovoltaic nanomaterial at the present stage, and the nanocrystalline material is expected to be a low-cost and high-efficiency solar cell of a new generation solution process.
The majority of nanocrystalline materials used in the preparation of PbX nanocrystalline solar cells are currently synthesized based on a classical thermal injection method, long-chain organic ligands (oleic acid) are needed to control the growth of nanocrystalline, but the long-chain organic ligands insulate nanocrystalline from each other, and a ligand exchange step is needed in the preparation process of photoelectric devices, and the long-chain organic ligands are exchanged into short ligands to enhance the conductivity of nanocrystalline films. 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: firstly, a nanocrystalline solution is used for preparing a film, and then the film is immersed into a solution containing short-chain ligands for exchange, so that the method has wide applicability and is the most widely applied method for early nanocrystalline solar cells. However, in the method, in order to ensure the full exchange of the ligand and the compactness of the thin film, the thickness of each thin film is controlled to be tens of nanometers, and the process is usually repeated for about 10 times to obtain the photovoltaic active layer with the required thickness, so that the preparation process is extremely complicated. Moreover, research shows that the solid state exchange has the problem of uneven exchange, and the surface of the nano crystal can be damaged by repeated polar solvent flushing, so that a defect state is introduced.
(2) Solution ligand exchange: in order to avoid the disadvantages of solid ligand exchange, recently solution ligand exchange methods have been widely studied. In the method, pbX nanocrystalline synthesized by a thermal injection method is dispersed in a nonpolar solvent (n-hexane or n-octane) and is stirred with a dimethylformamide solution of lead halide, ligand exchange is completed in a solution phase, surface oleic acid is replaced by lead halide salt, and then PbX nanocrystalline ink is formed by dispersing in a butylamine solution, so that the conductive film is directly prepared. Compared with solid state exchange, the method simplifies the preparation process of the device 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 larger toxicity, and the prepared nanocrystalline ink has poor stability, is unfavorable for mass application and has larger 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, wherein the lead-oxygen compound dimer nanocrystal is used, and the solid ligand exchange is used for realizing the one-time deposition of nanocrystal films with different thicknesses and ensuring no cracks. 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 complicated exchange of the traditional solid ligand and unstable exchange solution of the solution ligand, and is expected to provide a new way for the mass production of the nanocrystalline solar cells in the future.
In order to achieve the aim of the invention, the technical scheme adopted by the invention is to provide a preparation method of lead oxo 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, wherein the reaction solution is clear and transparent without bubbles, and a lead precursor is obtained;
2) Introducing inert gas into a reaction vessel, uniformly mixing a di (trimethylsilyl) oxy 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 centrifuging to remove sediment at the bottom;
4) And (3) precipitating the upper solution by isopropanol and acetone, centrifuging to remove the upper solution, and carrying out post-treatment of vacuum pumping to obtain the lead-oxygen compound dimer nanocrystalline.
The preparation method of the lead oxo compound dimer nanocrystalline 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, octadecylic acid and hexadecanoic 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) 2 S), bis (trimethylsilyl) selenide ((TMS) 2 Se), bis (trimethylsilyl) telluride ((TMS) 2 Te).
The conditions of the freezing treatment in the step 3) are that the freezing temperature is 0-5 ℃ and the freezing time is 10-60 minutes.
The technical scheme of the invention comprises a lead-oxygen compound dimer nanocrystal 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 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, wherein the reaction solution is clear and transparent without bubbles, and a lead precursor is obtained;
2) Introducing inert gas into a reaction vessel, uniformly mixing a di (trimethylsilyl) oxy 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 centrifuging to remove sediment at the bottom;
4) Precipitating the upper solution by isopropanol and acetone, centrifuging to remove the upper solution, and performing vacuum pumping post-treatment to obtain lead-oxygen compound dimer nanocrystalline;
5) Dissolving lead-oxygen compound dimer nanocrystalline 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 mode to form a film;
6) Dissolving iodide in alcohol solution with the concentration of 2-100 mM; and (3) dripping the solution onto the film prepared in the step (5), soaking for 50-300 seconds, spin-drying, and washing with isopropanol and acetonitrile to obtain the conductive film.
The preparation method of the conductive film based on the lead-oxygen compound dimer nanocrystalline comprises the following steps of: the nonpolar solvent comprises n-hexane, n-octane, toluene and chloroform; the substrate comprises common glass, transparent conductive glass, silicon wafer, silicon oxide, quartz and polyethylene terephthalate; the halide comprises methyl amidine halide, ammonia halide, halomethylamine, tetrabutylammonium halide and tetramethyl ammonium halide; halogen includes chlorine, bromine and iodine.
The technical scheme of the invention comprises a conductive film based on lead-oxygen compound dimer nanocrystalline obtained by the preparation method.
The technical scheme of the invention provides an application of a conductive film based on lead-oxygen compound dimer nanocrystalline in preparing 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 lead oxo compound dimer nanocrystalline;
2) The preparation method is simple and easy to implement, and the lead-oxygen compound dimer nanocrystalline can realize one-layer ligand exchange by using a simple solid-phase ligand exchange method to obtain the 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 common PbS nanocrystal and a PbS dimer nanocrystal provided by an embodiment of the present invention;
fig. 2 is a top view and a cross-section scanning electron microscope image of a film ligand prepared based on a common PbS nanocrystal and a PbS dimer nanocrystal provided by an embodiment of the present invention after exchange;
FIG. 3 is a schematic 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; fifth, hole transport layer; and sixthly, an anode layer.
Detailed Description
The invention will be further described with reference to the drawings and the specific embodiments. Materials, reagents and instruments used in the following examples are commercially available unless otherwise specifically indicated.
Example 1:
the embodiment provides a PbS dimer nanocrystalline, which is prepared by the following steps:
1) 450 mg (1 mmol) lead oxide, 1.4 g (2.5 mmol) oleic acid and 20 g 1-octadecene are added into a three-neck flask, stirred at 100 ℃ and vacuumized for 1 h to obtain a lead precursor for later use;
2) Into a three-necked flask, nitrogen was introduced, and the temperature was adjusted to 75℃to obtain 210. Mu.L (TMS) 2 S and 5 mL of 1-octadecene are mixed uniformly, and then are rapidly injected into the lead precursor by a syringe, and the reaction is continued for 10 min;
3) After the reaction is finished, cooling the water bath to room temperature, injecting 8 mL anhydrous normal hexane, transferring the reaction liquid into a centrifuge tube, transferring into a refrigerator, freezing at 4 ℃ for 60 min, centrifuging for 3 min by a centrifuge (the rotating speed is 6000 rpm), and discarding the lower layer of solid;
4) Adding isopropanol into the upper solution 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 solution, dissolving by normal hexane, centrifuging after adding acetone, discarding the upper solution, drying the residual solid in vacuum to obtain the required nanocrystalline, and storing in a glove box. The projection electron microscope image and the particle size statistics are shown in figure 1.
The procedure for the preparation of PbS nanocrystalline comparative example 1 is as follows:
1) 450 mg (1 mmol) lead oxide, 1.4 g (2.5 mmol) oleic acid and 20 g 1-octadecene are added into a three-neck flask, stirred at 100 ℃ and vacuumized for 1 h to obtain a lead precursor for later use;
2) Into a three-necked flask, nitrogen was introduced, and the temperature was adjusted to 75℃to obtain 210. Mu.L (TMS) 2 S and 5 mL of 1-octadecene are mixed uniformly, and then are rapidly injected into the lead precursor by a syringe, and the reaction is continued for 10 min;
3) After the reaction is finished, cooling to room temperature in a water bath, injecting 8 mL anhydrous n-hexane, transferring the reaction solution into a centrifuge tube, adding isopropanol until the reaction solution becomes turbid, centrifuging for 5 min by a centrifuge (the rotating speed is 8000 rpm), discarding the supernatant, dissolving by n-hexane, centrifuging after adding acetone, discarding the supernatant, and vacuumizing the residual solid to obtain the required nanocrystalline, and storing in a glove box, wherein a projection electron microscope image and 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 graph a and the graph b are respectively a projection electron microscope graph of the common PbS nanocrystalline (comparative example 1) and the PbS dimer nanocrystalline provided by the embodiment, the scale in the graph represents 20 nanometers, and the embedded high-resolution projection electron microscope scale represents 2 nanometers; figures c and d are statistical graphs of particle sizes of common PbS nanocrystals (comparative example 1) and PbS dimer nanocrystals provided in this example, respectively, and it can be seen from the graph that the conventional PbS nanocrystals were synthesized into spheres having an average diameter of 3.4 nm, and the solution was subjected to freezing treatment after the reaction, so that dimers of PbS nanocrystals having an average length of 5.5 nm could be obtained.
Example 2:
the embodiment provides a method for realizing crack-free film deposition based on PbS dimer nanocrystalline, which comprises the following specific steps:
1) The PbS dimer nanocrystalline prepared in example 1 was dissolved in n-hexane at a concentration of 50-500 mg/mL, deposited onto a substrate by spin coating at 1500 rpm.
2) An isopropyl alcohol solution of methylimidine iodide was prepared at a concentration of 25 mM. The solution was added dropwise to the film, immersed in 80 s and dried by spin. And then washing twice with isopropanol and once with acetonitrile to obtain the film based on PbS dimer nanocrystalline.
Comparative example 2 based on a common PbS nanocrystalline film was prepared as follows:
1) The common PbS nanocrystals prepared in comparative example 1 were dissolved in n-hexane at a concentration of 50-500 mg/mL and deposited onto a substrate by spin coating at 1500 rpm.
2) An isopropyl alcohol solution of methylimidine iodide was prepared at a concentration of 25 mM. The solution was added dropwise to the film, immersed in 80 s and dried by spin. And then washing twice with isopropanol and once with acetonitrile to obtain the PbS nanocrystalline film.
Referring to fig. 2, a top view and a cross-section scanning electron microscope image after the film ligand exchange prepared based on the common PbS nanocrystalline and the PbS dimer nanocrystalline provided by the embodiment of the invention are shown; wherein, the diagrams a and b are top view scanning electron microscope diagrams after the film ligand exchange prepared based on the common PbS nanocrystalline and the PbS dimer nanocrystalline provided by the embodiment of the invention, and the marked ruler in the diagrams a and b represents 4 microns; figures c and d are respectively cross-sectional scanning electron microscope images after the film ligand prepared based on the common PbS nanocrystalline and the PbS dimer nanocrystalline provided by the embodiment of the invention is exchanged, and marked rules in figures c and d represent 1 micrometer; as can be seen from the sem pictures, the film prepared using the common PbS nanocrystals had severe cracks, and the cross-sectional view showed that the cracks traversed the entire film. And the film prepared by using the PbS dimer nanocrystalline can completely avoid the generation of cracks, realize single deposition and obtain a compact film through solid-phase ligand exchange, and the thickness of the film can reach approximately 1 micron. And the dense conductive nanocrystalline film is a necessary condition for preparing high-performance devices.
Example 3:
referring to fig. 3, a schematic device structure of the nanocrystalline solar cell provided in this embodiment is shown; the solar photovoltaic device provided in this embodiment includes glass 1, and cathode layer 2 is attached to the glass, and electron transport layer 3 attached to the cathode layer, active layer 4 attached to the electron transport layer, hole transport layer 5 attached to the active layer, and anode layer 6 attached to the hole transport layer.
The present example prepared a solar cell based on PbS dimer nanocrystals, by the procedure of example 2, active layers of different thickness were deposited once, and dense, crack-free conductive films were obtained by solid-phase 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 normal 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, carrying out ligand exchange by adopting the technical scheme of the embodiment 2, spin-coating common PbS nanocrystalline (as described in the comparative example 1), carrying out ligand exchange by using ethanedithiol, and evaporating gold with the thickness of 100 nm to obtain the nano-crystalline ZnO/PbS composite material; wherein: the mass volume concentration of the active layer nanocrystalline solution is 200 mg/mL; the PbS nanocrystalline of the hole transport layer is 20 mg/mL; the rotational speed of spin coating the nanocrystalline solution was 1500 rpm for a duration of 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 nanocrystalline solution on a cleaned conductive glass substrate, carrying out ligand exchange according to the technical scheme of comparative example 2 in example 2, spin-coating common PbS nanocrystalline (as described in comparative example 1), carrying out ligand exchange by ethanedithiol, and evaporating gold with the thickness of 100 nm to obtain the nano-crystalline ZnO/common PbS composite material; wherein: the mass volume concentration of the active layer nanocrystalline solution is 200 mg/mL; the PbS nanocrystalline of the hole transport layer is 20 mg/mL; the rotational speed of spin coating the nanocrystalline solution was 1500 rpm for a duration of 20 s.
The performance parameters of the solar cells of the different devices prepared in this example are summarized in table 1.
TABLE 1 summary of the Performance parameters of solar cells for different devices
| Device and method for manufacturing the same | Short-circuit current (mA/cm) 2 ) | Open circuit voltage (V) | Fill factor (%) | Conversion efficiency (%) |
| Ordinary PbS nanocrystalline (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 performance, exhibiting excellent device performance. And the common film deposited by PbS nanocrystalline can generate serious cracks due to the action of stress in the ligand exchange process, so that the device performance is greatly reduced.
Claims (9)
1. The preparation method of the lead oxo 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, wherein the reaction solution is clear and transparent without bubbles, and a lead precursor is obtained;
2) Introducing inert gas into a reaction vessel, uniformly mixing a di (trimethylsilyl) oxy 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; the di (trimethylsilyl) oxy compound is any one of di (trimethylsilyl) sulfide, di (trimethylsilyl) selenide and di (trimethylsilyl) telluride;
3) After the reaction is finished, cooling the reaction liquid to room temperature, adding n-hexane, freezing the reaction liquid, and centrifuging to remove sediment at the bottom; the freezing treatment condition is that the freezing temperature is 0-5 ℃ and the freezing time is 10-60 minutes;
4) And (3) precipitating the upper solution by isopropanol and acetone, centrifuging to remove the upper solution, and carrying out post-treatment of vacuum pumping to obtain the lead-oxygen compound dimer nanocrystalline.
2. The method for preparing lead oxo-compound dimer nanocrystal, according to claim 1, which is characterized in that: 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, octadecylic acid and hexadecanoic acid; the solvent is any one of 1-octadecene, 1-eicosene and diphenyl ether.
3. The method for preparing lead oxo-compound dimer nanocrystal, according to claim 1, which is characterized in that: the inert gas in the step 2) is any one of nitrogen, helium and neon.
4. The method for preparing lead oxo-compound dimer nanocrystal, according to claim 1, which is characterized in that: 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. A lead-oxygen compound dimer nanocrystal obtained by the preparation method of claim 1.
6. The preparation method of the conductive film based on the lead-oxygen 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, wherein the reaction solution is clear and transparent without bubbles, and a lead precursor is obtained;
2) Introducing inert gas into a reaction vessel, uniformly mixing a di (trimethylsilyl) oxy 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; the di (trimethylsilyl) oxy compound is any one of di (trimethylsilyl) sulfide, di (trimethylsilyl) selenide and di (trimethylsilyl) telluride;
3) After the reaction is finished, cooling the reaction liquid to room temperature, adding n-hexane, freezing the reaction liquid, and centrifuging to remove sediment at the bottom; the freezing treatment condition is that the freezing temperature is 0-5 ℃ and the freezing time is 10-60 minutes;
4) Precipitating the upper solution by isopropanol and acetone, centrifuging to remove the upper solution, and performing vacuum pumping post-treatment to obtain lead-oxygen compound dimer nanocrystalline;
5) Dissolving lead-oxygen compound dimer nanocrystalline 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 mode to form a film;
6) Dissolving iodide in alcohol solution with the concentration of 2-100 mM; and (3) dripping the solution onto the film prepared in the step (5), soaking for 50-300 seconds, spin-drying, and washing with isopropanol and acetonitrile to obtain the conductive film.
7. The method for preparing a conductive film based on lead-oxygen compound dimer nanocrystalline according to claim 6, characterized in that: the nonpolar solvent is any one of n-hexane, n-octane, toluene and chloroform; the substrate is any one of common glass, transparent conductive glass, silicon wafer, silicon oxide, quartz and polyethylene terephthalate.
8. A conductive film based on lead-oxygen compound dimer nanocrystals obtained by the process of claim 6.
9. Use of a conductive film based on lead-oxygen compound dimer nanocrystals in the preparation of a solar cell as claimed in claim 8.
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