CN110106633A - Inorganic perovskite/composite nano-polymers tunica fibrosa and its preparation method and application - Google Patents
Inorganic perovskite/composite nano-polymers tunica fibrosa and its preparation method and application Download PDFInfo
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- CN110106633A CN110106633A CN201910400715.9A CN201910400715A CN110106633A CN 110106633 A CN110106633 A CN 110106633A CN 201910400715 A CN201910400715 A CN 201910400715A CN 110106633 A CN110106633 A CN 110106633A
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- inorganic perovskite
- tunica fibrosa
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- 229920000642 polymer Polymers 0.000 title claims abstract description 93
- 239000002131 composite material Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 238000009987 spinning Methods 0.000 claims abstract description 34
- 239000002121 nanofiber Substances 0.000 claims abstract description 31
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 20
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 15
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 11
- -1 caesium halide Chemical class 0.000 claims abstract description 11
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- 150000004820 halides Chemical class 0.000 claims abstract description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 10
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N dimethyl sulfoxide Natural products CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 14
- 238000001125 extrusion Methods 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 229910052794 bromium Inorganic materials 0.000 claims description 5
- 229910052740 iodine Inorganic materials 0.000 claims description 5
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical group [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 13
- 239000000758 substrate Substances 0.000 abstract description 7
- 239000004814 polyurethane Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000031700 light absorption Effects 0.000 abstract description 4
- 229920002635 polyurethane Polymers 0.000 abstract description 3
- 239000012528 membrane Substances 0.000 description 26
- 239000000243 solution Substances 0.000 description 23
- 239000007788 liquid Substances 0.000 description 14
- 239000010408 film Substances 0.000 description 13
- 239000002243 precursor Substances 0.000 description 10
- 238000013019 agitation Methods 0.000 description 8
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 description 8
- 229910052736 halogen Inorganic materials 0.000 description 8
- 150000002367 halogens Chemical class 0.000 description 8
- 238000003756 stirring Methods 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000004528 spin coating Methods 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 229960001760 dimethyl sulfoxide Drugs 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910003472 fullerene Inorganic materials 0.000 description 2
- 230000027756 respiratory electron transport chain Effects 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229920000144 PEDOT:PSS Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 1
- MCEWYIDBDVPMES-UHFFFAOYSA-N [60]pcbm Chemical compound C123C(C4=C5C6=C7C8=C9C%10=C%11C%12=C%13C%14=C%15C%16=C%17C%18=C(C=%19C=%20C%18=C%18C%16=C%13C%13=C%11C9=C9C7=C(C=%20C9=C%13%18)C(C7=%19)=C96)C6=C%11C%17=C%15C%13=C%15C%14=C%12C%12=C%10C%10=C85)=C9C7=C6C2=C%11C%13=C2C%15=C%12C%10=C4C23C1(CCCC(=O)OC)C1=CC=CC=C1 MCEWYIDBDVPMES-UHFFFAOYSA-N 0.000 description 1
- YSGZPEILUZVKDO-UHFFFAOYSA-N [F].C1(=CC=CC=C1)N(C1=CC=CC=C1)C1=CC=CC=C1 Chemical group [F].C1(=CC=CC=C1)N(C1=CC=CC=C1)C1=CC=CC=C1 YSGZPEILUZVKDO-UHFFFAOYSA-N 0.000 description 1
- AJRXEXGVDMEBCT-UHFFFAOYSA-M [NH4+].[I-].C[N+]1=CC=CC=C1.[I-] Chemical compound [NH4+].[I-].C[N+]1=CC=CC=C1.[I-] AJRXEXGVDMEBCT-UHFFFAOYSA-M 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 230000005525 hole transport Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- RQQRAHKHDFPBMC-UHFFFAOYSA-L lead(ii) iodide Chemical compound I[Pb]I RQQRAHKHDFPBMC-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
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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
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/407—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties containing absorbing substances, e.g. activated carbon
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
- D04H1/43—Acrylonitrile series
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
- D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/30—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains
- H10K30/35—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains comprising inorganic nanostructures, e.g. CdSe nanoparticles
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E10/50—Photovoltaic [PV] energy
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Abstract
The invention belongs to perovskite technical field of composite materials, and in particular to inorganic perovskite/composite nano-polymers tunica fibrosa and its preparation method and application.Preparation method, comprising the following steps: prepared polymer solution in organic solvent, polymer include at least one of polyvinylpyrrolidone, polyacrylonitrile, polyurethane；Lead halide, caesium halide are added in polymer solution, spinning solution is obtained；Spinning solution is subjected to electrostatic spinning, inorganic perovskite/composite nano-polymers tunica fibrosa is made.The present invention is prepared for inorganic perovskite/composite nano-polymers tunica fibrosa using simple electrostatic spining technology, realize the combination of inorganic perovskite and polymer, so that perovskite material is embedded in the surface of nanofiber, is conducive to the light absorption of perovskite material, the transfer of charge and photoelectron transfer；Moreover, preparation process is simple, do not limited by substrate, energy large area preparation, this keeps it huge in the fields such as perovskite solar battery, light emitting diode application potential.
Description
Technical field
The invention belongs to perovskite technical field of composite materials, and in particular to inorganic perovskite/composite nano-polymers are fine
Tie up film and its preparation method and application.
Background technique
Lead halogen perovskite material has excellent characteristic of semiconductor, excellent absorbing properties, good luminescent properties
And low cost preparation, photovoltaic device, light emitting diode, in terms of be widely used, therefore be concerned.Lead halogen
Perovskite material mainly includes hybrid inorganic-organic lead halogen perovskite and full-inorganic lead halogen perovskite material, be related to film,
Three kinds of forms of monocrystalline and powder.Wherein, lead halogen perovskite thin film has wide in the fields such as solar battery and light emitting diode
Wealthy application prospect.
Currently, lead halogen perovskite thin film mainly passes through solution spin-coating method and the preparation of double source coevaporation method.Wherein, solution revolves
Coating includes ingredient, high speed rotation, volatilization three steps of film forming, by control time of spin coating, rotating speed acceleration, dropping liquid amount with
And the concentration of solution used, viscosity control the thickness of film forming.Centrifugal force that spin-coating method generates when being by workpiece rotation and again
Power effect, spreads the coating procedure in workpiece surface for the coating drop fallen on workpiece comprehensively.However, spin-coating method is only applicable to
One-sided coatings are prepared on planar simple workpiece, and general spin coated substrate area should not be too large, and paint waste is more.With it is molten
Liquid spin-coating method is compared, and the perovskite thin film thickness of double source coevaporation preparation is uniform, but the preparation process of double source coevaporation is complicated, energy
Consumption is high.
Electrostatic spinning is a kind of easy-to-use method for continuously preparing nanofiber and its film, the nanofiber of preparation
Surface area it is big, the advantages that fibre diameter is controllable, and electrostatic spinning apparatus is simple, low in cost, technique is controllable.This makes Static Spinning
Silk nano fibrous membrane has a wide range of applications in fields such as the energy, catalysis, environment and biologies.Perovskite is prepared using electrostatic spinning
Nano fibrous membrane can obtain more flexible its thickness of regulation of modular perovskite nano fibrous membrane, it is easier to its into
Row operation, therefore be concerned.Static Spinning perovskite nano fibrous membrane is reported individually, such as application No. is 2015102214194
Chinese invention patent disclose a kind of perovskite nanofiber film solar cell and preparation method thereof, wherein preparation method packet
It includes: hybrid inorganic-organic perovskite composite Nano fibre is made using methylpyridinium iodide ammonium and lead chloride as presoma by electrostatic spinning
Film is tieed up, as perovskite solar cell light absorbing layer.Chen etc. is prepared for polymer overmold perovskite using coaxial electrostatic spinning
Nano fibrous membrane.
Relative to hybrid inorganic-organic lead halogen perovskite material, full-inorganic lead halogen perovskite material has good
Stability.Therefore, the preparation and its application that inorganic perovskite nano fibrous membrane is perovskite material are prepared by electrostatic spinning
Important step also becomes the core content studied at present.Such as application No. is 201810359252.1 patent documents to disclose one
The preparation method of kind composite fluorescence nano fibrous membrane, preparation method include: that chlorine caesium halide is added in halogenation lead solution, to
After dissolution, polymer is added, obtains spinning solution, subsequent electrostatic spinning obtains inorganic perovskite/composite nano-polymers fiber
Film；In the composite nano fiber, perovskite is easy to be located inside nanofiber, due to blocking for polymer, its light is inhibited to capture
Efficiency, to reduce the generation efficiency of photo-generated carrier；And polymer stops having for perovskite and charge transport layer completely
Effect contact, inhibits the transfer of charge, limits it in the application in the fields such as solar battery.
Summary of the invention
Based on the above deficiencies in the existing technologies, the present invention provides inorganic perovskite/composite nano-polymers fiber
Film and its preparation method and application.
In order to achieve the above object of the invention, the invention adopts the following technical scheme:
Inorganic perovskite/composite nano-polymers tunica fibrosa preparation method, comprising the following steps:
S1, in organic solvent prepared polymer solution, the polymer include polyvinylpyrrolidone, polyacrylonitrile,
At least one of polyurethane；
S2, lead halide, caesium halide are added in the polymer solution, obtain spinning solution；
S3, the spinning solution is subjected to electrostatic spinning, inorganic perovskite/composite nano-polymers tunica fibrosa is made.
Preferably, the mass ratio of the polymer and organic solvent is 0.09~0.2:1.
Preferably, in the polymer solution gross mass and organic solvent of lead halide and caesium halide mass ratio
For 0.1~1:1, the molar ratio of lead halide and caesium halide is 0.5~5:1.
Preferably, it is 0.1~2mL/h, voltage 10 that the process conditions of the electrostatic spinning, which include: rate of extrusion,
~40kV, environment temperature are 0~50 DEG C, and humidity is 50% or less.
Preferably, the organic solvent is dimethyl sulfoxide or dimethyl formyl.
Preferably, the inorganic perovskite includes CsPbX3, X=Cl, Br or I.
The present invention also provides inorganic perovskite/composite nano-polymers tunica fibrosa, the preparation as described in any of the above-described scheme
Method is made.
Preferably, the inorganic perovskite is located at the surface of polymer nanofiber.
The present invention also provides the application of inorganic perovskite/composite nano-polymers tunica fibrosa, the inorganic perovskite/polymerization
Object composite nano-fiber membrane is applied to perovskite solar battery or light emitting diode.
Preferably, the inorganic perovskite/composite nano-polymers tunica fibrosa is as perovskite solar battery
Light absorbing layer or light emitting diode photoluminescent layers.
Compared with prior art, the present invention beneficial effect is:
The present invention is prepared for inorganic perovskite/composite nano-polymers tunica fibrosa using simple electrostatic spining technology, realizes
The combination of inorganic perovskite and polymer makes perovskite material be embedded in the surface of nanofiber, is conducive to perovskite material
Light absorption, and improve its contact with charge transport layer, promote transfer and the photoelectron transfer of charge；Meanwhile modular calcium
Titanium ore composite nano-fiber membrane is simple to operate when assembling perovskite device；And stable inorganic perovskite can improve device
Stability；In addition, the inorganic perovskite nano fibrous membrane preparation process of Static Spinning is simple, do not limited by substrate, it can large area
Preparation, this keeps it huge in the fields such as perovskite solar battery, light emitting diode application potential.
Detailed description of the invention
Fig. 1 is inorganic perovskite/composite nano-polymers tunica fibrosa digital photograph of the embodiment of the present invention 1；
Fig. 2 is that inorganic perovskite/composite nano-polymers fiber scanning electron microscope sem of the embodiment of the present invention 1,2 and 3 shines
Piece；
Fig. 3 is inorganic perovskite/composite nano-polymers tunica fibrosa X-ray diffraction XRD diagram of the embodiment of the present invention 1；
Fig. 4 be the perovskite constructed using inorganic perovskite/composite nano-polymers tunica fibrosa of the embodiment of the present invention 1 too
The structural schematic diagram of positive energy battery；
Fig. 5 is constructed using inorganic perovskite/composite nano-polymers tunica fibrosa of the embodiment of the present invention and comparative example
The photocurrent-voltage curve of perovskite solar battery；
Fig. 6 is the light-emitting diodes constructed using inorganic perovskite/composite nano-polymers tunica fibrosa of the embodiment of the present invention 1
The structural schematic diagram of pipe.
Specific embodiment
Below by specific embodiment the technical scheme of the present invention will be further described explanation.
Embodiment 1:
The specific preparation process of inorganic perovskite/composite nano-polymers tunica fibrosa of the present embodiment is as follows:
0.18 gram of polyacrylonitrile (PAN) is added in 2 grams of dimethyl sulfoxide DMSO, it is molten to obtain polymer by magnetic agitation
Liquid；
Then, 0.09 gram of PbBr is added simultaneously in a polymer solution2With 0.11 gram of CsBr, temperature be 80 DEG C at through magnetic
Power stirring stirring 6h, obtains CsPbBr3Spinning liquid as precursor；
By CsPbBr3Spinning liquid as precursor is encased in syringe, and the high voltage of 18kV is added between spinning head and reception device,
Spinning head is 10cm at a distance from receiver board, and rate of extrusion 0.1mL/h, spinning environment temperature is 2 DEG C, and humidity 10% makes
Solution is deposited directly on receiver board with disordered state forms inorganic perovskite/polymer nanofibre film, abbreviation CsPbBr3/
PAN composite nano-fiber membrane.
Inorganic perovskite to the present embodiment/polymer nanofibre film is carried out to the characterization of structure and performance below:
As shown in Figure 1, being CsPbBr3The digital photograph of/PAN composite nano-fiber membrane, nano fibrous membrane can be bent to
Circle, this illustrates CsPbBr3/ PAN composite nano-fiber membrane shows good flexibility.Fig. 2 (a) is made from this example
CsPbBr3The SEM photograph of/PAN composite nano-fiber membrane, it can be seen that nano particle is embedded in the surface of nanofiber.Fig. 3 is
CsPbBr made from this example3The X-ray diffraction spectrogram of/PAN composite nano-fiber membrane illustrates inorganic perovskite CsPbBr3Shape
At.
By the CsPbBr of the present embodiment3/ PVP composite nano-fiber membrane is applied in perovskite solar battery, by Fig. 4 institute
Show assembly device, including the successively conductive substrates 1 of lamination, charge transport layer 2, CsPbBr from bottom to top3/ PAN composite Nano is fine
Tie up film 3, charge transport layer 4 and top layer electrode 5；Wherein, charge transport layer 2 and charge transport layer 4 are respectively as electron transfer layer
Or hole transmission layer, charge transport layer can be TiO2、ZnO、SnO2、Al2O3Or one of fullerene derivate or a variety of,
Hole transmission layer can be the small molecule containing fluorine-triphenylamine structure, the small molecule containing thiophene-structure, the polymer containing aniline structure, contain
The polymer of thiophene-structure, the compound of nickel, one of the compound of the compound of copper and molybdenum or a variety of mixing；Conductive substrates
1, which can be such as conductive material of ITO, FTO, metal nanometer line or conducting polymer, deposits on glass or polymer substrates；
Top layer electrode 5, i.e. back electrode, using noble metal or carbon material.Firstly, by hole transport strata (3,4-rthylene dioxythiophene)-
Polystyrolsulfon acid (PEDOT:PSS) is coated in ITO conductive substrates, then by CsPbBr3/ PAN composite nano-fiber membrane is placed
Between hole transmission layer, subsequent spin coating fullerene derivate PCBM electron transfer layer, finally, vapor deposition gold electrode is to form calcium
Titanium ore solar battery.
The photoelectric conversion efficiency of the perovskite solar battery of the present embodiment is 0.55%, as shown in Fig. 5 (a).This implementation
The perovskite of example is located at nanofiber surface, and light capture rate and charge transport capability can be improved, and improves perovskite and charge passes
The contact of defeated layer improves the transfer ability of charge, promotes its application in solar cells.
The present embodiment is prepared for inorganic perovskite/composite nano-polymers tunica fibrosa using simple electrostatic spinning technique,
The combination for realizing inorganic perovskite and polymer makes perovskite material be embedded in the surface of nanofiber, is conducive to perovskite material
The light absorption of material, the transfer of charge and photoelectron transfer；Meanwhile modular perovskite composite nano-fiber membrane is in assembling calcium titanium
Inorganic perovskite simple to operate when mine device and stable can improve the stability of device；In addition, the inorganic calcium of Static Spinning
Titanium ore nano fibrous membrane preparation process is simple, is not limited by substrate, and energy large area preparation, this makes it in perovskite solar-electricity
The application potential in pond field is huge.
As the CsPbBr of the present embodiment3/ PAN composite nano-fiber membrane is applied to light emitting diode, as shown in fig. 6, will
CsPbBr3/ PAN composite nano-fiber membrane 7 is deposited directly in LED chip 6, CsPbBr3/ PAN composite nano-fiber membrane is used as hair
The photoluminescent layers of optical diode.
Embodiment 2:
The specific preparation process of inorganic perovskite/composite nano-polymers tunica fibrosa of the present embodiment is as follows:
0.08 gram of polyurethane PU, 0.07 gram of polyvinylpyrrolidone PVP and 0.1 gram of polyacrylonitrile (PAN) are added to 2 gram two
In methyl sulfoxide DMSO, clear solution is obtained through magnetic agitation 2h at room temperature；
0.21 gram of PbCl is then added in the solution2, 0.27 gram of PbBr2With 0.32 gram of CsBr, temperature be 80 DEG C at through magnetic
Power stirring stirring 6h obtains CsPbIBr2Spinning liquid as precursor；
Spinning liquid as precursor is encased in syringe, the high voltage of 25kV, spinning head are added between spinning head and reception device
Be 15cm at a distance from receiver board, rate of extrusion 0.3mL/h, spinning environment temperature is 10 DEG C, humidity 20%, make solution with
Disordered state, which is deposited directly on receiver board, forms inorganic perovskite/polymer nanofibre film, i.e. CsPbIBr2/ polymer is multiple
Close nano fibrous membrane.
Below by the CsPbIBr to the present embodiment2The characterization of/composite nano-polymers tunica fibrosa progress structure and performance:
It is CsPbIBr made from this example as shown in Fig. 2 (b)2The SEM photograph of/composite nano-polymers tunica fibrosa, can
To find that nano particle is embedded in the surface of nanofiber；Its digital photograph and XRD diagram are similar with the result of embodiment 1, that is, anticipate
Taste the exterior appearance of the composite nano-fiber membrane of the present embodiment, flexibility and crystal structure it is similar to Example 1.
CsPbIBr made from this example2Application of/composite nano-polymers the tunica fibrosa in perovskite solar battery,
Solar battery, photoelectric conversion efficiency 0.71%, as shown in Fig. 5 (b) are assembled with structure shown in embodiment 1.
In addition, the CsPbIBr of the present embodiment2/ composite nano-polymers tunica fibrosa can also be applied to light emitting diode, with real
Apply example 1.
Embodiment 3:
The specific preparation process of inorganic perovskite/composite nano-polymers tunica fibrosa of the present embodiment is as follows:
0.1 gram of PU, 0.1 gram of PVP and 0.1 gram of PAN are added in 2 grams of DMSO, obtained at room temperature through magnetic agitation 2h
Clear solution；
0.24 gram of PbCl is added in the solution later2, 0.32 gram of PbBr2, 0.8 gram of PbI2With 0.24 gram of CsI, it is in temperature
CsPbX is obtained through magnetic agitation stirring 6h at 80 DEG C3Spinning liquid as precursor, X=Cl, Br or I；
Spinning liquid as precursor is encased in syringe, the high voltage of 30kV, spinning head are added between spinning head and reception device
Be 25cm at a distance from receiver board, rate of extrusion 1mL/h, spinning environment temperature is 30 DEG C, and humidity 30% makes solution with nothing
Sequence state is deposited directly on receiver board, to form CsPbX3(X=Cl, Br or I) inorganic perovskite/composite nano-polymers
Tunica fibrosa.
Below by the CsPbX to the present embodiment3Inorganic perovskite/composite nano-polymers tunica fibrosa carries out structure and performance
Characterization:
It is CsPbX made from this example as shown in Fig. 2 (c)3Inorganic perovskite/composite nano-polymers tunica fibrosa is swept
Retouch electromicroscopic photograph, it is found that nano particle coats nano fibrous membrane substantially.CsPbX made from this example3Inorganic perovskite/
The X-ray diffraction spectrogram sum number code photo of composite nano-polymers tunica fibrosa is similar with embodiment 1.
CsPbX made from the present embodiment3Inorganic perovskite/composite nano-polymers tunica fibrosa is in perovskite solar battery
In application, similar to Example 1, the photoelectric conversion efficiency of solar battery of assembling has reached 1.16%, such as Fig. 5 (c)
It is shown.
In addition, the CsPbX of the present embodiment3Inorganic perovskite/composite nano-polymers tunica fibrosa can also be applied to luminous two
Pole pipe, with embodiment 1.
Embodiment 4:
The specific preparation process of inorganic perovskite/composite nano-polymers tunica fibrosa of the present embodiment is as follows:
0.1 gram of PU and 0.3 gram of PVP is added in 2.0 grams of DMSO, is obtained at room temperature through magnetic agitation 2h limpid molten
Liquid；
0.3 gram of PbBr is added in the solution later2, 1.5 grams of PbI2, 0.1 gram of CsBr and 0.1 gram of CsI, be 80 DEG C in temperature
It is lower to obtain CsPbX through magnetic agitation stirring 6h3Spinning liquid as precursor is encased in injection by spinning liquid as precursor, X=Cl, Br or I
In device, the high voltage of 40kV is added between spinning head and reception device, spinning head is 30cm at a distance from receiver board, and rate of extrusion is
2mL/h, temperature are 50 DEG C, and humidity 50% is deposited directly to solution on receiver board with disordered state, to form CsPbX3
Inorganic perovskite/composite nano-polymers tunica fibrosa.
CsPbX made from the present embodiment3Inorganic perovskite/composite nano-polymers tunica fibrosa pattern and embodiment 3
As a result similar.
CsPbX made from the present embodiment3Inorganic perovskite/composite nano-polymers tunica fibrosa is in perovskite solar battery
In application, similar to Example 1, the photoelectric conversion efficiency of solar battery of assembling has reached 1.00%, such as Fig. 5 (d)
It is shown.
In addition, the CsPbX of the present embodiment3Inorganic perovskite/composite nano-polymers tunica fibrosa can also be applied to luminous two
Pole pipe, with embodiment 1.
Comparative example 1:
The specific preparation process of inorganic perovskite/composite nano-polymers tunica fibrosa of this comparative example:
First by 0.228 gram of PbBr2And 0.101 gram of CsBr is added in 2 grams of DMSO, through magnetic agitation at being 80 DEG C in temperature
3h obtains clear solution；
0.15 gram of PVP and 0.15 gram of PAN is added in the solution later, is obtained at room temperature through magnetic agitation stirring 6h
CsPbBr3Spinning liquid as precursor；
Spinning liquid as precursor is encased in syringe, carries out electrostatic spinning (spinning technology parameter is with embodiment one), obtains
Obtain inorganic perovskite/composite nano-polymers tunica fibrosa.
The perovskite sun is formed as light-absorption layer using the inorganic perovskite/composite nano-polymers tunica fibrosa of this comparative example
Energy battery (with the structure of embodiment one), photoelectric conversion efficiency only has 0.02%, as shown in Fig. 5 (e).This is because polymerizeing
Caused by the order of addition of object, polymer adds again after lead halide and caesium halide dissolution, will lead to polymer overmold CsPbBr3
Inorganic perovskite；Due to blocking for polymer, inhibit its light capture rate, so that the generation efficiency of photo-generated carrier is reduced,
And polymer stops perovskite to contact with the effective of charge transport layer completely, inhibits the transfer of charge, so that its photoelectric conversion
Efficiency is lower.
In above-described embodiment and its alternative, the mass ratio of polymer and organic solvent can also for 0.1:1,
0.12:1,0.13:1,0.16:1,0.18:1,0.19:1 etc..
In above-described embodiment and its alternative, organic solvent can also be dimethyl formyl.
In above-described embodiment and its alternative, polymer can also include polyvinylpyrrolidone, polyacrylonitrile, gather
At least one of urethane (in addition to disclosed in above-described embodiment)；When including at least two kinds, the type of corresponding polymer
For any mass ratio.
In above-described embodiment and its alternative, in polymer solution the gross mass of lead halide and caesium halide with it is organic molten
The mass ratio of agent can also be 0.2:1,0.3:1,0.5:1,0.6:1,0.9:1 etc..
In above-described embodiment and its alternative, the molar ratio of lead halide and caesium halide can also be 0.5:1,1:1,2:
1,3:1,4:1,5:1 etc..
In above-described embodiment and its alternative, in the process conditions of electrostatic spinning:
Rate of extrusion can also be 0.5mL/h, 0.8mL/h, 1.2mL/h, 1.5mL/h, 1.8mL/h etc.；
Voltage can also be 10kV, 15kV, 20kV, 35kV etc.；
Spinning environment temperature can also be 0 DEG C, 5 DEG C, 15 DEG C, 25 DEG C, 35 DEG C, 40 DEG C, 45 DEG C etc.；
Humidity can also be 5%, 15%, 25%, 35%, 40%, 45% etc..
The above is only that the preferred embodiment of the present invention and principle are described in detail, to the common skill of this field
For art personnel, the thought provided according to the present invention will change in specific embodiment, and these changes should also regard
For protection scope of the present invention.
Claims (10)
1. inorganic perovskite/composite nano-polymers tunica fibrosa preparation method, which comprises the following steps:
S1, in organic solvent prepared polymer solution, the polymer include polyvinylpyrrolidone, polyacrylonitrile, poly- ammonia
At least one of ester；
S2, lead halide, caesium halide are added in the polymer solution, obtain spinning solution；
S3, the spinning solution is subjected to electrostatic spinning, inorganic perovskite/composite nano-polymers tunica fibrosa is made.
2. the preparation method of inorganic perovskite/composite nano-polymers tunica fibrosa according to claim 1, feature exist
In the mass ratio of the polymer and organic solvent is 0.09~0.2:1.
3. the preparation method of inorganic perovskite/composite nano-polymers tunica fibrosa according to claim 1, feature exist
In the mass ratio of the gross mass and organic solvent of lead halide and caesium halide is 0.1~1:1, lead halide in the polymer solution
Molar ratio with caesium halide is 0.5~5:1.
4. the preparation method of inorganic perovskite/composite nano-polymers tunica fibrosa according to claim 1, feature exist
In the process conditions of the electrostatic spinning include: that rate of extrusion is 0.1~2mL/h, and voltage is 10~40kV, environment temperature 0
~50 DEG C, humidity is 50% or less.
5. the preparation method of inorganic perovskite/composite nano-polymers tunica fibrosa according to claim 1, feature exist
In the organic solvent is dimethyl sulfoxide or dimethyl formyl.
6. the preparation method of inorganic perovskite/composite nano-polymers tunica fibrosa according to claim 1, feature exist
In the inorganic perovskite includes CsPbX3, X=Cl, Br or I.
7. inorganic perovskite/composite nano-polymers tunica fibrosa, which is characterized in that by as claimed in any one of claims 1 to 6
Preparation method is made.
8. inorganic perovskite/composite nano-polymers tunica fibrosa according to claim 7, which is characterized in that described inorganic
Perovskite is located at the surface of polymer nanofiber.
9. the application of inorganic perovskite/composite nano-polymers tunica fibrosa as claimed in claim 7, which is characterized in that described
Inorganic perovskite/composite nano-polymers tunica fibrosa is applied to perovskite solar battery or light emitting diode.
10. the application of inorganic perovskite/composite nano-polymers tunica fibrosa as claimed in claim 9, which is characterized in that described
Inorganic perovskite/composite nano-polymers tunica fibrosa is as the light absorbing layer of perovskite solar battery or the light of light emitting diode
Electroluminescent layer.
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