CN107442183A - A kind of graphene/nanometer crystalline substance/perovskite photocatalysis membrana and preparation method thereof - Google Patents
A kind of graphene/nanometer crystalline substance/perovskite photocatalysis membrana and preparation method thereof Download PDFInfo
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- CN107442183A CN107442183A CN201710769354.6A CN201710769354A CN107442183A CN 107442183 A CN107442183 A CN 107442183A CN 201710769354 A CN201710769354 A CN 201710769354A CN 107442183 A CN107442183 A CN 107442183A
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- perovskite
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- nanometer crystalline
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 83
- 239000000126 substance Substances 0.000 title claims abstract description 58
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 37
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 79
- 239000002243 precursor Substances 0.000 claims abstract description 37
- 239000002159 nanocrystal Substances 0.000 claims abstract description 35
- 238000004528 spin coating Methods 0.000 claims abstract description 32
- 239000011521 glass Substances 0.000 claims abstract description 25
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 20
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 15
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 239000002798 polar solvent Substances 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000011135 tin Substances 0.000 claims abstract description 11
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 11
- 239000012296 anti-solvent Substances 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 10
- 238000012545 processing Methods 0.000 claims abstract description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052802 copper Inorganic materials 0.000 claims abstract description 9
- 239000010949 copper Substances 0.000 claims abstract description 9
- 239000012046 mixed solvent Substances 0.000 claims abstract description 9
- 230000009467 reduction Effects 0.000 claims abstract description 9
- 229910052709 silver Inorganic materials 0.000 claims abstract description 9
- 239000004332 silver Substances 0.000 claims abstract description 9
- 229910052718 tin Inorganic materials 0.000 claims abstract description 9
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 8
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 150000003839 salts Chemical class 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 7
- BNOODXBBXFZASF-UHFFFAOYSA-N [Na].[S] Chemical compound [Na].[S] BNOODXBBXFZASF-UHFFFAOYSA-N 0.000 claims abstract description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 32
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical group OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 10
- 230000001476 alcoholic effect Effects 0.000 claims description 10
- 125000004177 diethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 6
- 229910002804 graphite Inorganic materials 0.000 claims description 6
- 239000010439 graphite Substances 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 claims description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910052946 acanthite Inorganic materials 0.000 claims description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Inorganic materials [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 claims description 2
- 229910052980 cadmium sulfide Inorganic materials 0.000 claims description 2
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- NMHMNPHRMNGLLB-UHFFFAOYSA-N phloretic acid Chemical compound OC(=O)CCC1=CC=C(O)C=C1 NMHMNPHRMNGLLB-UHFFFAOYSA-N 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 claims description 2
- 229940056910 silver sulfide Drugs 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims 1
- 239000010408 film Substances 0.000 description 9
- 235000011150 stannous chloride Nutrition 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 239000000443 aerosol Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- -1 octadecylene Chemical group 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 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
- 150000001661 cadmium Chemical class 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- DRHWBADNSVQEGH-UHFFFAOYSA-L diiodyloxylead Chemical compound O=I(=O)O[Pb]OI(=O)=O DRHWBADNSVQEGH-UHFFFAOYSA-L 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000007327 hydrogenolysis reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- HTRJDXQPCKIFIU-UHFFFAOYSA-N silver;ethanol;nitrate Chemical compound [Ag+].CCO.[O-][N+]([O-])=O HTRJDXQPCKIFIU-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention provides a kind of graphene/nanometer crystalline substance/perovskite photocatalysis membrana and preparation method thereof, and the film is prepared by the spin-coated method one-step method heating of graphene/nanometer crystalline substance/perovskite precursor solution, and specific preparation method is：The salt dissolving in the mixed solvent of tin, silver, copper, iron or cadmium is formed into mixed solution, the solution of Containing Sulfur sodium is slowly added dropwise, is well mixed, centrifugal filtration is washed, inorganic nano-crystal is obtained, inorganic nano-crystal is added in polar solvent again, ultrasonic disperse, obtain inorganic nano-crystal solution；Graphene oxide solution will be added in inorganic nano-crystal solution, add perovskite material, be well mixed, added hydrazine hydrate, heating reduction, obtain graphene/nanometer crystalline substance/perovskite precursor solution；It is covered in by spin-coating method on the electro-conductive glass containing coating of titanium dioxide, anti-solvent processing is carried out with chlorobenzene in spin coating process, the good electro-conductive glass of spin coating is heated, obtains graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
Description
Technical field
The invention belongs to optoelectronic materials technology, and in particular to a kind of graphene/nanometer crystalline substance/perovskite photocatalysis membrana and
Its preparation method.
Background technology
With the rapid development of dyestuff textile industry in recent years, the kind of dyes produced gradually increases, and causes dyeing waste water
A large amount of discharges, change the component and property of natural water.Therefore, dyeing waste water has become one of pollution sources.Photocatalysis skill
Art is a kind of basic nanometer technology, applied to multiple Disciplinary Frontiers such as the depollution of environment, advanced new energy and self-cleaning material, effect
Rate is high, easy to operate, nontoxic, reaction condition is gentle, has good application in degradating organic dye and improvement water pollution etc.
Prospect.
Perovskite is mineral matters most on the earth, is a kind of inorganic non-metallic material with unique physicochemical property, is changed
Learn composition and be typically expressed as ABO3, A positions are generally rare earth or alkali earth metal, and B positions are generally transition metal, A, B
Bit element can substitute other metallic element parts similar in ionic radius, and crystal structure keeps three oxygen cube points substantially
The mutually interspersed cubic structure of battle array, perovskite have oxidation reaction, nitrogen oxide decomposition, vehicle maintenance service, hydrogenation and hydrogenolysis anti-
Should, especially perovskite composite oxide strontium titanates has been widely used for the photochemical catalyst of hydrolysis.
The nanocrystalline preparation method of a kind of single size CsPbX3 perovskites disclosed in Chinese patent CN105523581B, by bromine
Change lead solid powder to be dissolved under nitrogen atmosphere in oleyl amine, oleic acid and dodecane, the octadecylene for then adding the caesium containing oleic acid is molten
In liquid, it is nanocrystalline that reaction obtains CsPbX3 perovskites, is scattered in CsPbX3 perovskites are nanocrystalline in n-hexane, lead chloride is added dropwise
Or iodate lead solution, the CsPbX3 perovskites for obtaining single size are nanocrystalline.It is a kind of disclosed in Chinese patent CN102534546A
The preparation method of perovskite type nanocrystalline thin film on glass substrate, nitrate is added to solution in ethanol, adds citric acid and treat
After being completely dissolved, regulation solution obtains perovskite precursor solution to alkalescent, by perovskite precursor solution formed droplet by
Nitrogen carries to form aerosol, and aerosol deposits on the glass substrate of heating, and being cooled to room temperature, to obtain Ca-Ti ore type nanocrystalline
Film.The nanocrystalline crystallinity of Ca-Ti ore type, thickness, surface topography to the performance impact of material, by add other materials with
The nanocrystalline combination property that will be expected to improve perovskite material of Ca-Ti ore type.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of graphene/nanometer crystalline substance/perovskite photocatalysis membrana and its preparation
Method, primary raw material is used as by perovskite, nanocrystalline and graphene, by spin-coating method, in the electro-conductive glass containing titanium dioxide
Surface in situ crystallizes the photocatalysis membrana to form one layer of even compact good crystallinity, is remarkably improved the optics and photo electric of film
Energy.
In order to solve the above technical problems, the technical scheme is that：
A kind of graphene/nanometer crystalline substance/perovskite photocatalysis membrana, the graphene/nanometer crystalline substance/perovskite photocatalysis membrana be by
The heating of graphene/nanometer crystalline substance/perovskite precursor solution spin-coated method is prepared, it is described it is nanocrystalline graphene/nanometer it is brilliant/
The concentration of perovskite precursor solution is less than 10mg/mL, and the graphene is in graphene/nanometer crystalline substance/perovskite precursor solution
Concentration be less than 5mg/mL.
As the preferred of above-mentioned technical proposal, in the graphene/nanometer crystalline substance/perovskite precursor solution it is nanocrystalline including
Energy gap is sub- in stannous sulfide of the 0.4-2.3eV particle size ranges less than 50nm, silver sulfide, copper sulfide, cuprous sulfide, vulcanization
Iron or cadmium sulfide.
The present invention provides a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana, comprises the following steps：
(1) in the mixed solvent that the salt of tin, silver, copper, iron or cadmium is dissolved in ethylene glycol and triethanolamine forms mixing
Solution, the diethyl alcoholic solution of Containing Sulfur sodium is slowly added dropwise, is well mixed, washs foreign ion with absolute ethyl alcohol and DMF, centrifuged
Filter, obtains inorganic nano-crystal, inorganic nano-crystal is added in polar solvent again, ultrasonic disperse, it is molten to obtain inorganic nano-crystal
Liquid；
(2) graphene oxide solution is added in the inorganic nano-crystal solution for preparing step (1), be well mixed, add calcium
Titanium ore material, it is well mixed, adds hydrazine hydrate, heating reduction, obtain graphene/nanometer crystalline substance/perovskite precursor solution；
(3) graphene/nanometer crystalline substance/perovskite precursor solution prepared by step (2) is covered in containing two by spin-coating method
On the electro-conductive glass of titania coating, anti-solvent processing is carried out with chlorobenzene in spin coating process, by the good electro-conductive glass of spin coating in 90-
10-90min is heated at 120 DEG C, obtains graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
As the preferred of above-mentioned technical proposal, in the step (1), tin, silver, copper, the salt of iron or cadmium are anhydrous chlorination
Stannous, silver nitrate, copper nitrate, cuprous nitrate, ferric nitrate, ferrous nitrate or cadmium nitrate.
As the preferred of above-mentioned technical proposal, in the step (1), tin, silver, copper, iron or cadmium salt and ethylene glycol and
The solid-to-liquid ratio of triethanolamine is 70-80mg:23-25mL：4.5-5g.
As the preferred of above-mentioned technical proposal, in the step (1), sodium sulphate is dense in the diethyl alcoholic solution of Containing Sulfur sodium
Spend for 8-10mg/mL, the mass ratio of the vulcanized sodium and the salt of tin, silver, copper, iron or cadmium is 15-20:70-80mg.
As the preferred of above-mentioned technical proposal, in the step (1), centrifugal rotational speed 2000-12000r/min.
As the preferred of above-mentioned technical proposal, in the step (1), polar solvent is N-N NMFs DMF, diformazan
One or several kinds in base sulfoxide DMSO, gamma-butyrolacton GBL, acetonitrile ACN and 1-METHYLPYRROLIDONE NMP.
As the preferred of above-mentioned technical proposal, in the step (2), perovskite material is that mol ratio is 1:1 CH3NH3I
And PbI2Mixture.
As the preferred of above-mentioned technical proposal, in the step (2), the graphene/nanometer crystalline substance/perovskite presoma is molten
Liquid also includes the nanocrystalline organic-inorganic perovskite including energy gap in the range of 1.3-2.3eV, the organic-inorganic calcium titanium
Ore deposit includes CH3NH3PbI3、CH3NH3Pb1-xSnxI3、CH3NH3SnI3、CH(NH3)2PbI3、CsPbI3、CsSnI3, wherein 0 ＜ x ＜
1。
Compared with prior art, the invention has the advantages that：
(1) graphene/nanometer crystalline substance/calcium titanium photocatalysis membrana prepared by the present invention is by before graphene/nanometer crystalline substance/perovskite
Drive liquid solution to obtain in the conductive glass surface containing titanium dioxide, graphene/nanometer of the invention crystalline substance/perovskite precursor solution
In containing graphene, nanocrystalline and perovskite, minimal amount of graphene oxide is coated on to nanocrystalline surface, then again with calcium
Titanium ore is mixed, then graphene oxide is reduced, and obtains precursor solution, precursor solution is by spin-coating method in electro-conductive glass
Surface form film, during heating, hydridization method directly receiving in graphene-containing that perovskite passes through in-situ crystallization
The brilliant surface of rice is crystallized, because the nanocrystalline particle diameter of graphene-containing is small, surface area ratio is larger, can be provided more extra
Forming core site so as to improve the crystallinity of perovskite material, and due to it is nanocrystalline be inorganic semiconductor material or perovskite material
Material, therefore the performance of film is not damaged, in addition by selecting the nanocrystalline and perovskite hydridization of different energy gaps, can increase
Photon absorbing intensity of the strong film material in different wavelength range, while improve its optical property.
(2) preparation technology of the invention is simple, easily controllable, and nanocrystalline concentration is adjusted by centrifugal process, simply may be used
Control, cost is low, and the film photocatalysis of preparation will not cause secondary pollution to environment, be easily recycled, and prepared by the present invention
Film electronic transmission performance it is unique, the compound of photo-generated carrier can be reduced, the photocatalysis efficiency of film is further improved, carry
High optics and photoelectric properties.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1：
(1) by 76mg anhydrous stannous chlorides be dissolved in 23mL ethylene glycol and 4.5g triethanolamines in the mixed solvent formed it is mixed
Solution is closed, the diethyl alcoholic solution of the 2mL vulcanized sodium containing 8mg/mL is slowly added dropwise, is well mixed, is washed with absolute ethyl alcohol and DMF miscellaneous
Matter ion, the centrifugal filtration under 2000r/min rotating speeds, obtains inorganic nano-crystal, and inorganic nano-crystal is added to N-N methyl first again
In acid amides DMF polar solvents, ultrasonic disperse, inorganic nano-crystal solution is obtained.
(2) 0.5mg/mL graphene oxide solution will be added in inorganic nano-crystal solution, is well mixed, adds mol ratio
For 1:1 CH3NH3I and PbI2Perovskite material, be well mixed, according to the mass ratio of graphene oxide and hydrazine hydrate be 10:1
Hydrazine hydrate is added, heating reduction 60min, obtains graphene/nanometer crystalline substance/perovskite precursor solution at 90 DEG C.
(3) graphene/nanometer crystalline substance/perovskite precursor solution is covered in containing titanium dioxide with 500r/min spin coatings 10s
On the electro-conductive glass of coating, anti-solvent processing is carried out with chlorobenzene in spin coating process, the good electro-conductive glass of spin coating is added at 100 DEG C
Hot 15min, obtain graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
Embodiment 2：
(1) by 76mg anhydrous stannous chlorides be dissolved in 23mL ethylene glycol and 4.5g triethanolamines in the mixed solvent formed it is mixed
Solution is closed, the diethyl alcoholic solution of the 2mL vulcanized sodium containing 8mg/mL is slowly added dropwise, is well mixed, is washed with absolute ethyl alcohol and DMF miscellaneous
Matter ion, the centrifugal filtration under 12000r/min rotating speeds, obtains inorganic nano-crystal, and inorganic nano-crystal is added to volume ratio 4 again:
In 1 N-N NMFs DMF and dimethyl sulfoxide (DMSO) DMSO polar solvents, ultrasonic disperse, inorganic nano-crystal solution is obtained.
(2) 2mg/mL graphene oxide solution will be added in inorganic nano-crystal solution, is well mixed, adding mol ratio is
1:1 CH3NH3I and PbI2Perovskite material, be well mixed, according to the mass ratio of graphene oxide and hydrazine hydrate be 10:3 add
Enter hydrazine hydrate, heating reduction 60min, obtains graphene/nanometer crystalline substance/perovskite precursor solution at 95 DEG C, wherein graphene/
The also CH containing 0.01mg/mL in nanocrystalline/perovskite precursor solution3NH3SnI3。
(3) graphene/nanometer crystalline substance/perovskite precursor solution is covered in containing titanium dioxide with 1000r/min spin coatings 10s
On the electro-conductive glass of coating, anti-solvent processing is carried out with chlorobenzene in spin coating process, the good electro-conductive glass of spin coating is added at 105 DEG C
Hot 20min, obtain graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
Embodiment 3：
(1) 20mg/mL silver nitrate ethanol solutions are dissolved in the in the mixed solvent shape of 25mL ethylene glycol and 5g triethanolamines
Into mixed solution, the diethyl alcoholic solution of the 3mL vulcanized sodium containing 10mg/mL is slowly added dropwise, is well mixed, with absolute ethyl alcohol and DMF
Foreign ion is washed, the centrifugal filtration under 12000r/min rotating speeds obtains inorganic nano-crystal, inorganic nano-crystal is added into volume again
Than for 4:1 enter in N-N NMFs DMF and dimethyl sulfoxide (DMSO) DMSO polar solvents, ultrasonic disperse, obtains inorganic nano
Brilliant solution.
(2) 2mg/mL graphene oxide solution will be added in inorganic nano-crystal solution, is well mixed, adding mol ratio is
1:1 CH3NH3I and PbI2Perovskite material, be well mixed, according to the mass ratio of graphene oxide and hydrazine hydrate be 10:12
Hydrazine hydrate is added, heating reduction 60min, obtains graphene/nanometer crystalline substance/perovskite precursor solution, wherein graphite at 95 DEG C
The also CH containing 0.02mg/mL in alkene/nanocrystalline/perovskite precursor solution3NH3PbI3。
(3) graphene/nanometer crystalline substance/perovskite precursor solution is covered in containing titanium dioxide with 800r/min spin coatings 10s
On the electro-conductive glass of coating, anti-solvent processing is carried out with chlorobenzene in spin coating process, the good electro-conductive glass of spin coating is added at 100 DEG C
Hot 10min, obtain graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
Embodiment 4：
(1) by 76mg anhydrous stannous chlorides be dissolved in 23mL ethylene glycol and 4.5g triethanolamines in the mixed solvent formed it is mixed
Solution is closed, the diethyl alcoholic solution of the 2mL vulcanized sodium containing 8mg/mL is slowly added dropwise, is well mixed, is washed with absolute ethyl alcohol and DMF miscellaneous
Matter ion, the centrifugal filtration under 2000-12000r/min rotating speeds, obtains inorganic nano-crystal, and inorganic nano-crystal is added into body again
Product ratio 4:In 1 N-N NMFs DMF and dimethyl sulfoxide (DMSO) DMSO polar solvents, ultrasonic disperse, inorganic nano-crystal is obtained
Solution.
(2) 1.5mg/mL graphene oxide solution will be added in inorganic nano-crystal solution, is well mixed, adds mol ratio
For 1:1 CH3NH3I and PbI2Perovskite material, be well mixed, according to the mass ratio of graphene oxide and hydrazine hydrate be 10:1
Hydrazine hydrate is added, heating reduction 60min, obtains graphene/nanometer crystalline substance/perovskite precursor solution, wherein graphite at 95 DEG C
The also CH containing 0.05mg/mL in alkene/nanocrystalline/perovskite precursor solution3NH3Pb0.9Sn0.1I3。
(3) graphene/nanometer crystalline substance/perovskite precursor solution is covered in containing titanium dioxide with 600r/min spin coatings 10s
On the electro-conductive glass of coating, anti-solvent processing is carried out with chlorobenzene in spin coating process, the good electro-conductive glass of spin coating is added at 120 DEG C
Hot 10min, obtain graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
Embodiment 5：
(1) by 76mg anhydrous stannous chlorides be dissolved in 23mL ethylene glycol and 4.5g triethanolamines in the mixed solvent formed it is mixed
Solution is closed, the diethyl alcoholic solution of the 2mL vulcanized sodium containing 8mg/mL is slowly added dropwise, is well mixed, is washed with absolute ethyl alcohol and DMF miscellaneous
Matter ion, the centrifugal filtration under 8000r/min rotating speeds, obtains inorganic nano-crystal, and inorganic nano-crystal is added to volume ratio 4 again:1
N-N NMFs DMF and dimethyl sulfoxide (DMSO) DMSO polar solvents in, ultrasonic disperse, obtain inorganic nano-crystal solution.
(2) 1.5mg/mL graphene oxide solution will be added in inorganic nano-crystal solution, is well mixed, adds mol ratio
For 1:1 CH3NH3I and PbI2Perovskite material, be well mixed, according to the mass ratio of graphene oxide and hydrazine hydrate be 10:3
Hydrazine hydrate is added, heating reduction 60min, obtains graphene/nanometer crystalline substance/perovskite precursor solution, wherein graphite at 95 DEG C
The also CH containing 0.03mg/mL in alkene/nanocrystalline/perovskite precursor solution3NH3PbI3。
(3) graphene/nanometer crystalline substance/perovskite precursor solution is covered in containing titanium dioxide with 1000r/min spin coatings 10s
On the electro-conductive glass of coating, anti-solvent processing is carried out with chlorobenzene in spin coating process, the good electro-conductive glass of spin coating is added at 105 DEG C
Hot 30min, obtain graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
Embodiment 6：
(1) the in the mixed solvent formation mixing that 80mg ferric nitrates are dissolved in 24mL ethylene glycol and 4.8g triethanolamines is molten
Liquid, the diethyl alcoholic solution of the 2.5mL vulcanized sodium containing 9mg/mL is slowly added dropwise, is well mixed, impurity is washed with absolute ethyl alcohol and DMF
Ion, the centrifugal filtration under 10000r/min rotating speeds, obtains inorganic nano-crystal, and inorganic nano-crystal is added to volume ratio again for 3:
In 1 N-N NMFs DMF and 1-METHYLPYRROLIDONE NMP polar solvents, ultrasonic disperse, it is molten to obtain inorganic nano-crystal
Liquid.
(2) 0.5mg/mL graphene oxide solution will be added in inorganic nano-crystal solution, is well mixed, adds mol ratio
For 1:1 CH3NH3I and PbI2Perovskite material, be well mixed, according to the mass ratio of graphene oxide and hydrazine hydrate be 10:2
Hydrazine hydrate is added, heating reduction 60min, obtains graphene/nanometer crystalline substance/perovskite precursor solution, wherein graphite at 90 DEG C
The also CsSnI containing 0.01mg/mL in alkene/nanocrystalline/perovskite precursor solution3。
(3) graphene/nanometer crystalline substance/perovskite precursor solution is covered in containing titanium dioxide with 850r/min spin coatings 10s
On the electro-conductive glass of coating, anti-solvent processing is carried out with chlorobenzene in spin coating process, the good electro-conductive glass of spin coating is added at 120 DEG C
Hot 60min, obtain graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
Comparative example：
It is 1 by mol ratio:1 CH3NH3I and PbI2Perovskite material solution be covered in and contain with 850r/min spin coatings 10s
On the electro-conductive glass of coating of titanium dioxide, anti-solvent processing is carried out with chlorobenzene in spin coating process, the good electro-conductive glass of spin coating is existed
60min is heated at 120 DEG C, obtains perovskite photocatalysis membrana.
After testing, embodiment 1-6 prepare graphene/nanometer crystalline substance/perovskite photocatalysis membrana and prior art it is thin
The result of film thickness, photoelectric transformation efficiency and photocatalysis performance is as follows：
As seen from the above table, the thickness of thin of graphene/nanometer crystalline substance/perovskite photocatalysis membrana prepared by the present invention, crystallinity is high,
Optical property and photocatalysis performance are good.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
- A kind of 1. graphene/nanometer crystalline substance/perovskite photocatalysis membrana, it is characterised in that：Graphene/nanometer crystalline substance/perovskite the light Catalytic membrane is prepared by the spin-coated method heating of graphene/nanometer crystalline substance/perovskite precursor solution, described nanocrystalline in graphite The concentration of alkene/nanocrystalline/perovskite precursor solution is less than 10mg/mL, and the graphene is in graphene/nanometer crystalline substance/perovskite The concentration of precursor solution is less than 5mg/mL.
- A kind of 2. graphene/nanometer crystalline substance/perovskite photocatalysis membrana according to claim 1, it is characterised in that：The graphite It is nanocrystalline in alkene/nanocrystalline/perovskite precursor solution to be less than 50nm's in 0.4-2.3eV particle size ranges including energy gap Stannous sulfide, silver sulfide, copper sulfide, cuprous sulfide, ferrous sulfide or cadmium sulfide.
- 3. a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana, it is characterised in that comprise the following steps：(1) in the mixed solvent that the salt of tin, silver, copper, iron or cadmium is dissolved in ethylene glycol and triethanolamine forms mixed solution, The diethyl alcoholic solution of Containing Sulfur sodium is slowly added dropwise, is well mixed, washs foreign ion with absolute ethyl alcohol and DMF, centrifugal filtration, obtain To inorganic nano-crystal, inorganic nano-crystal is added in polar solvent again, ultrasonic disperse, obtains inorganic nano-crystal solution；(2) graphene oxide solution is added in the inorganic nano-crystal solution for preparing step (1), be well mixed, add perovskite Material, it is well mixed, adds hydrazine hydrate, heating reduction, obtain graphene/nanometer crystalline substance/perovskite precursor solution；(3) graphene/nanometer crystalline substance/perovskite precursor solution prepared by step (2) is covered in containing titanium dioxide by spin-coating method On the electro-conductive glass of titanium coating, anti-solvent processing is carried out with chlorobenzene in spin coating process, by the good electro-conductive glass of spin coating in 90-120 10-90min is heated at DEG C, obtains graphene/nanometer crystalline substance/perovskite photocatalysis membrana.
- 4. a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana according to claim 3, its feature exist In：In the step (1), tin, silver, copper, the salt of iron or cadmium are anhydrous stannous chloride, silver nitrate, copper nitrate, cuprous nitrate, Ferric nitrate, ferrous nitrate or cadmium nitrate.
- 5. a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana according to claim 3, its feature exist In：In the step (1), tin, silver, copper, iron or the salt and ethylene glycol of cadmium and the solid-to-liquid ratio of triethanolamine are 70-80mg:23- 25mL：4.5-5g.
- 6. a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana according to claim 3, its feature exist In：In the step (1), the concentration of sodium sulphate is 8-10mg/mL in the diethyl alcoholic solution of Containing Sulfur sodium, the vulcanized sodium with Tin, silver, copper, the mass ratio of salt of iron or cadmium are 15-20:70-80mg.
- 7. a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana according to claim 3, its feature exist In：In the step (1), centrifugal rotational speed 2000-12000r/min.
- 8. a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana according to claim 3, its feature exist In：In the step (1), polar solvent is N-N NMFs DMF, dimethyl sulfoxide (DMSO) DMSO, gamma-butyrolacton GBL, acetonitrile One or several kinds in ACN and 1-METHYLPYRROLIDONE NMP.
- 9. a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana according to claim 3, its feature exist In：In the step (2), perovskite material is that mol ratio is 1:1 CH3NH3I and PbI2Mixture.
- 10. a kind of preparation method of graphene/nanometer crystalline substance/perovskite photocatalysis membrana according to claim 3, its feature exist In：In the step (2), the graphene/nanometer crystalline substance/perovskite precursor solution also exists including nanocrystalline including energy gap Organic-inorganic perovskite in the range of 1.3-2.3eV, the organic-inorganic perovskite include CH3NH3PbI3、CH3NH3Pb1- xSnxI3、CH3NH3SnI3、CH(NH3)2PbI3、CsPbI3、CsSnI3, wherein 0 ＜ x ＜ 1.
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