CN108258127A - A kind of method that spraying prepares perovskite nano-crystal film - Google Patents
A kind of method that spraying prepares perovskite nano-crystal film Download PDFInfo
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- CN108258127A CN108258127A CN201810023684.5A CN201810023684A CN108258127A CN 108258127 A CN108258127 A CN 108258127A CN 201810023684 A CN201810023684 A CN 201810023684A CN 108258127 A CN108258127 A CN 108258127A
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- crystal film
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- perovskite
- spray gun
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- 239000002159 nanocrystal Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000005507 spraying Methods 0.000 title claims abstract description 27
- 239000007921 spray Substances 0.000 claims abstract description 100
- 239000000758 substrate Substances 0.000 claims abstract description 75
- 239000007788 liquid Substances 0.000 claims abstract description 56
- 239000006185 dispersion Substances 0.000 claims abstract description 31
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 238000000137 annealing Methods 0.000 claims abstract description 4
- 239000002096 quantum dot Substances 0.000 claims description 62
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 22
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000010408 film Substances 0.000 description 59
- 238000006073 displacement reaction Methods 0.000 description 14
- 239000010409 thin film Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- 238000004528 spin coating Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 241000549556 Nanos Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
Abstract
A kind of method that spraying prepares perovskite nano-crystal film is distributed to perovskite is nanocrystalline in organic solvent, obtains the nanocrystalline dispersion liquid of perovskite；The nanocrystalline dispersion liquid of perovskite is fitted into spray bottle, is installed on spray gun, adjusts spray gun and the distance of substrate, the liquid outlet quantity of spray gun and air pressure；Then it is sprayed after substrate is heated, after annealing, obtains perovskite nano-crystal film.Perovskite nano-crystal film compactness that the present invention obtains is high, surfacing, it can be applied to prepare the photoelectric devices such as solar cell, photodetector and light emitting diode, while this method has the advantages that stock utilization is high, film forming speed is fast, can large area preparation.
Description
Technical field
The invention belongs to nano-crystalline thin field of membrane preparation, and in particular to a kind of spraying prepares the side of perovskite nano-crystal film
Method.
Background technology
The solwution method controllable preparation of metal and semiconductor nano material achieves the development advanced by leaps and bounds in recent years, in order to
By Application of micron in nano-crystal film photoelectric device, including quantum dot film solar cell, light emitting diode and photoelectricity
Detector is developed a variety of thin film preparation processes to obtain the adjustable nano-crystal film of fine and close smooth and thickness.It is a variety of
Include spin-coating method, czochralski method, spray coating method and solution self-assembly method etc. suitable for the nano-crystal film preparation process of solution-processible,
But their applicable situation is but not quite similar.Extra solvent and solute are thrown away substrate by spin-coating method using centrifugal force, can
The smooth nano-crystal film of tens to hundreds of nano thickness is prepared, shortcoming is to be suitable only for the preparation of small area film, material profit
It is low with rate, it is very high to solution dispersion, concentration and viscosity requirement.Czochralski method is to be attached to when substrate leaves liquid level by nanocrystalline
In substrate, nano-crystalline thin film thickness can be regulated and controled by lifting number, shortcoming is film compactness and lack of homogeneity.Solution is from group
Dress method is suitable for the preparation of the ordered nanos crystalline substance film such as nanocrystalline superlattices, and shortcoming is that deposition efficiency is low, and it is small to prepare film size.
Spray coating method is to be atomized nanocrystal solution using high-speed flow, forms nano-crystal film in substrate after the solvent is volatilized, tool
Have the advantages that stock utilization is high, film forming speed is fast, can large area prepare, these advantages just compensate for spin-coating method, czochralski method
With the disadvantage of solution self-assembly method.
Existing spray coating method exists during preparing nano-crystal film without the drop using substrate heating, continuous spray formation
Substrate surface cannot be evaporated rapidly, form non-uniform film.A plurality of types of perovskites are nanocrystalline to be synthesized by solwution method
Out, but it is nanocrystalline to prepare perovskite compared to the nanocrystalline difference of traditional type there is presently no spray coating method for its stability of solution
The report of film, therefore very it is necessary to optimize spraying process, it is hereby achieved that the controllable perovskite of even compact, thickness is received
The brilliant film of rice.
Invention content
The purpose of the present invention is to provide a kind of method that spraying prepares perovskite nano-crystal film, this method can be prepared
The adjustable perovskite nano-crystal film of smooth, fine and close and thickness.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of method that spraying prepares perovskite nano-crystal film, includes the following steps：
1) it is distributed to perovskite is nanocrystalline in organic solvent, obtains the nanocrystalline dispersion liquid of perovskite；
2) the nanocrystalline dispersion liquid of perovskite is fitted into spray bottle, be installed on spray gun, adjust distance, the spray of spray gun and substrate
The liquid outlet quantity of rifle and air pressure；Then it is sprayed after substrate is heated, after annealing, obtains perovskite nano-crystal film.
Further improve of the invention is that organic solvent is in n-hexane, chloroform, toluene, normal octane in step 1)
It is one or more of.
The present invention, which further improves, to be, a concentration of 0.01~5mg/ of the nanocrystalline dispersion liquid of perovskite in step 1)
mL。
Further improve of the invention is that it is CsPbBr that perovskite is nanocrystalline in step 1)3Quantum dot, CsPbBr3Nanometer
Piece, CsPbI3Quantum dot, CsPbI3Nanometer sheet, CsPbCl3Quantum dot, CsPbCl3Nanometer sheet, CH3NH3PbI3Quantum dot,
CH3NH3PbI3Nanometer sheet, CH3NH3PbBr3Quantum dot, CH3NH3PbBr3Nanometer sheet, CH3NH3PbCl3Quantum dot, CH3NH3PbCl3
Nanometer sheet, FAPbI3Quantum dot, FAPbI3Nanometer sheet, FAPbBr3Quantum dot, FAPbBr3Nanometer sheet, FAPbCl3Quantum dot or
FAPbCl3Nanometer sheet.
Further improve of the invention is that the substrate in step 2) is rigid basement or flexible substrates.
Further improve of the invention is that rigid basement is glass or silicon chip；Flexible substrates are PET or PI.
Further improve of the invention is that the distance of spray gun and substrate is 2~10cm in step 2), and substrate is horizontal positioned
Or vertical placement.
Of the invention further improve be, the liquid outlet quantity of spray gun is 0.02mL/s in step 2), air pressure for 50~
400kPa。
Further improve of the invention is that the temperature heated in step 3) is 25~150 DEG C；Spray time in step 3)
For 10~360s.
Further improve of the invention is that the temperature annealed in step 4) is 90~250 DEG C, and the time is 5~60min.
Compared with prior art, the device have the advantages that：The nanocrystalline dispersion liquid of perovskite is passed through spray by the present invention
Rifle is sprayed in substrate, after annealing, obtains perovskite nano-crystal film.By adjusting the distance of spray gun and substrate, spray gun goes out
Liquid measure and air pressure can obtain fine and close smooth nano-crystal film, and 40% stock utilization is obtained by process modification, into
Film speed is fast (spray time is 30~360s), can large area prepare (4~100cm of spray area2), the perovskite nanometer of preparation
Brilliant film can be applied to solar cell, light emitting diode and photodetector.
Description of the drawings
Fig. 1 is the schematic diagram of paint finishing that the present invention uses.
Fig. 2 is the schematic diagram that the present invention prepares large area perovskite nano-crystal film.
Fig. 3 is CsPbBr prepared by the embodiment of the present invention 13The surface SEM figures of perovskite nano-crystal film.
Fig. 4 is CsPbBr prepared by the embodiment of the present invention 23The surface SEM figures of perovskite nano-crystal film.
Fig. 5 is CsPbBr prepared by the embodiment of the present invention 33The surface SEM figures of perovskite nano-crystal film.
Fig. 6 is CsPbBr prepared by the embodiment of the present invention 43The surface SEM figures of perovskite nano-crystal film.
Fig. 7 is CsPbBr prepared by the embodiment of the present invention 53The surface SEM figures of perovskite nano-crystal film.
Fig. 8 is CsPbBr prepared by 1-5 of the embodiment of the present invention3The transmittance curve figure of perovskite nano-crystal film.
In figure, 1 is spray gun, and 2 be spray bottle, and 3 be stream pressure controller, and 4 be substrate warm table, and 5 be horizontal position moving stage, 6
For substrate.
Specific embodiment
The present invention is described in further detail with reference to the accompanying drawings and embodiments.
Embodiment 1
1) by CsPbBr3Quantum dot is distributed in n-hexane, obtains the CsPbBr of a concentration of 0.5mg/mL3Quantum dot disperses
Liquid；
2) by CsPbBr3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 2 × 2cm2, adjust
Spray gun and the distance of horizontal positioned substrate of glass are 4cm, pass through the Ultimus of EFD companiesTMI dispensings platform can be controlled accurately
Air pressure processed is 100Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) substrate at the uniform velocity on mobile and horizontal displacement platform, 30s is sprayed at 25 DEG C；
4) by CsPbBr3Quantum dot film is annealed 15min in 90 DEG C of thermal station, obtains perovskite nano-crystal film.
Embodiment 2
1) by CsPbBr3Quantum dot is distributed in n-hexane, obtains the CsPbBr of a concentration of 0.5mg/mL3Quantum dot disperses
Liquid；
2) by CsPbBr3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 2 × 2cm2, adjust
Spray gun and the distance of horizontal positioned silicon chip substrate are 4cm, pass through the Ultimus of EFD companiesTMI dispensings platform can be controlled accurately
Air pressure processed is 100Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 60 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 30s；
4) by CsPbBr3Quantum dot film is annealed 15min in 90 DEG C of thermal station.
Embodiment 3
1) by CsPbBr3Quantum dot is distributed in n-hexane, obtains the CsPbBr of a concentration of 0.5mg/mL3Quantum dot disperses
Liquid；
2) by CsPbBr3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 2 × 2cm2, adjust
Spray gun and the distance of horizontal positioned PET base are 4cm, pass through the Ultimus of EFD companiesTMI dispensings platform can be controlled accurately
Air pressure is 100Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 90 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 30s；
4) by CsPbBr3Quantum dot film is annealed 15min in 90 DEG C of thermal station.
Embodiment 4
1) by CsPbBr3Quantum dot is distributed in n-hexane, obtains the CsPbBr of a concentration of 0.5mg/mL3Quantum dot disperses
Liquid；
2) by CsPbBr3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 2 × 2cm2, adjust
Spray gun and the distance of horizontal positioned PI substrates are 4cm, pass through the Ultimus of EFD companiesTMI dispensings platform can be controlled accurately
Air pressure is 100Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 120 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 30s；
4) by CsPbBr3Quantum dot film is annealed 15min in 90 DEG C of thermal station.
Embodiment 5
1) by CsPbBr3Quantum dot is distributed in n-hexane, obtains the CsPbBr of a concentration of 0.5mg/mL3Quantum dot disperses
Liquid；
2) by CsPbBr3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 2 × 2cm2, adjust
Spray gun and the distance of horizontal positioned PI substrates are 4cm, pass through the Ultimus of EFD companiesTMI dispensings platform can be controlled accurately
Air pressure is 100Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 150 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 30s；
4) by CsPbBr3Quantum dot film is annealed 15min in 90 DEG C of thermal station.
Embodiment 6
1) by CsPbBr3Nanometer sheet is distributed in chloroform, obtains the CsPbBr of a concentration of 0.01mg/mL3Nanometer sheet is disperseed
Liquid；
2) by CsPbBr3Nanometer sheet dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 2 × 10cm2, adjust
Spray gun and the distance of horizontal positioned PET base are 4cm, pass through the Ultimus of EFD companiesTMI dispensings platform can be controlled accurately
Air pressure is 100Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 90 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 30s；
4) by CsPbBr3Nanometer sheet film is annealed 15min in 90 DEG C of thermal station.
Embodiment 7
1) by CsPbCl3Quantum dot is distributed in toluene, obtains the quantum dot dispersion liquid of a concentration of 5mg/mL；
2) by CsPbCl3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 5 × 5cm2, adjust
Spray gun and the distance of horizontal positioned silicon chip substrate are 2cm, pass through the Ultimus of EFD companiesTMI dispensings platform can be controlled accurately
Air pressure processed is 50Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 90 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 30s；
4) by CsPbCl3Perovskite nano-crystal film is annealed 10min in 250 DEG C of thermal station.
Embodiment 8
1) by CsPbI3Quantum dot is distributed to volume ratio n-hexane：Normal octane=3:In 1, obtain a concentration of 1mg/mL's
CsPbI3Quantum dot dispersion liquid；
2) by CsPbI3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 5 × 10cm2, adjust
Spray gun and the distance of horizontal positioned substrate of glass are 10cm, pass through the Ultimus of EFD companiesTMI dispensings platform can be controlled accurately
Air pressure processed is 400Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 90 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 30s；
4) by CsPbI3Quantum dot film is annealed 30min in 200 DEG C of thermal station.
Embodiment 9
1) by CH3NH3PbI3Quantum dot is distributed in n-hexane, obtains the CH of a concentration of 0.05mg/mL3NH3PbI3Quantum
Point dispersion liquid；
2) by CH3NH3PbI3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 10 × 10cm2,
It is 5cm to adjust spray gun and the distance of horizontal positioned substrate of glass, passes through the Ultimus of EFD companiesTMI dispensings platform can essence
True control pressure is 200Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 90 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 30s；
4) by CH3NH3PbI3Quantum dot film is annealed 60min in 90 DEG C of thermal station.
As shown in fig.1, the paint finishing that the present invention uses mainly is made of 4 parts, it is spray gun 1, spray bottle 2, gas respectively
Flowing pressure controller 3 and substrate warm table 4.
As shown in fig.2, horizontal position moving stage 5 is arranged on by the present invention by the way that substrate 6 is installed in horizontal position moving stage 5
On substrate warm table 4, and substrate 6 can be moved by horizontal position moving stage 5 in two dimensional surface, different so as to fulfill substrate 6
The uniform film covering in region.Spray gun 1 is located above substrate, and spray bottle 2 is installed to spray gun 1 by spray bottle 2 for holding dispersion liquid
On, in the case of fixed 1 position of spray gun, by adjusting different location of the substrate 6 in horizontal position moving stage 5, prepare uniform
Perovskite nano-crystal film.It can be in the flexible substrates such as the rigid basements such as glass, silicon chip and PET, PI by horizontal position moving stage 5
On, the maximum coated area of realization is 10 × 10cm2。
Analysis chart 3- Fig. 7 has found that in other technological parameters base reservoir temperature is to spraying nano crystal film under the same conditions
Flatness has conclusive influence, and the nano-crystal film coverage rate of room temperature spraying is poor, and there are many holes；Substrate is heated to 60
DEG C, 90 DEG C, the nano-crystal film that sprays after 120 DEG C and 150 DEG C do not find hole, show that film coverage is very high, but base
The nano-crystal film that bottom heating obtains is there are irregular protrusion, and to correspond to nano-crystal film different degrees of for different base reservoir temperatures
Flatness.Determine to add in perovskite it is nanocrystalline it is identical in quality under the premise of, spray identical time 30s, room temperature spraying obtains
The most thin about 130nm of the nano-crystal film obtained, respective material utilization rate is 10%；Substrate be heated to 60 DEG C, 90 DEG C, 120 DEG C and
The close about 500nm of nano-crystalline thin film thickness of acquisition is sprayed after 150 DEG C, respective material utilization rate is 40%, it was demonstrated that substrate
Heating greatly improves stock utilization.
It can be seen that under identical spray time by Fig. 8 nano-crystal film transmittance curves, room temperature spraying obtains
Nano-crystal film is most thin, and the nano-crystalline thin film thickness that different base heating temperature obtains is very similar, with scanning electron microscope observation
As a result it is consistent.
Base reservoir temperature can not only influence the flatness that shows of film, also have a great impact to film thickness, substrate adds
Heat greatly improves the stock utilization that spray coating method prepares perovskite nano-crystal film.
Embodiment 10
1) by CH3NH3PbBr3Nanometer sheet is distributed in the mixed liquor of n-hexane, chloroform and toluene, obtains a concentration of 2mg/
The CH of mL3NH3PbBr3Nanometer sheet dispersion liquid；
2) by CH3NH3PbBr3Nanometer sheet dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 5 × 5cm2,
It is 7cm to adjust spray gun and the distance of substrate of glass placed vertically, passes through the Ultimus of EFD companiesTMI dispensings platform can essence
True control pressure is 100Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 40 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 10s, then at 150 DEG C
Anneal 5min in thermal station.
Embodiment 11
1) by CH3NH3PbCl3Quantum dot is distributed in the mixed liquor of toluene and normal octane, obtains a concentration of 3mg/mL's
CH3NH3PbCl3Quantum dot dispersion liquid；
2) by CH3NH3PbCl3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 5 × 5cm2,
It is 8cm to adjust spray gun and the distance of silicon chip substrate placed vertically, passes through the Ultimus of EFD companiesTMI dispensings platform can essence
True control pressure is 300Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 110 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 360s, then at 180 DEG C
Thermal station on anneal 40min.
Embodiment 12
1) by CH3NH3PbCl3Nanometer sheet is distributed in the mixed liquor of chloroform and toluene, obtains a concentration of 4mg/mL's
CH3NH3PbCl3Nanometer sheet dispersion liquid；
2) by CH3NH3PbCl3Nanometer sheet dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 5 × 5cm2,
It is 6cm to adjust spray gun and the distance of PET base placed vertically, passes through the Ultimus of EFD companiesTMI dispensings platform can be accurate
Control pressure is 350Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 130 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 200s, then at 220 DEG C
Thermal station on anneal 50min.
Embodiment 13
1) by CH3NH3PbBr3Quantum dot is distributed in the mixed liquor of n-hexane and chloroform, obtains a concentration of 2mg/mL's
CH3NH3PbBr3Quantum dot dispersion liquid；
2) by CH3NH3PbBr3Quantum dot dispersion liquid is fitted into spray bottle, is installed on spray gun, and area of base is 5 × 5cm2,
It is 7cm to adjust spray gun and the distance of PI substrates placed vertically, passes through the Ultimus of EFD companiesTMI dispensings platform can be accurate
Control pressure is 100Kpa, and the liquid outlet quantity of spray gun is 0.02mL/s；
3) after substrate being heated to 40 DEG C, the substrate at the uniform velocity on mobile and horizontal displacement platform sprays 100s, then at 150 DEG C
Thermal station on anneal 5min.
The present invention realizes spray coating method and prepares perovskite nano-crystal film, and it is CsPbBr that wherein perovskite is nanocrystalline3Quantum
Point, CsPbBr3Nanometer sheet, CsPbI3Quantum dot, CsPbI3Nanometer sheet, CsPbCl3Quantum dot, CsPbCl3Nanometer sheet,
CH3NH3PbI3Quantum dot, CH3NH3PbI3Nanometer sheet, CH3NH3PbBr3Quantum dot, CH3NH3PbBr3Nanometer sheet, CH3NH3PbCl3
Quantum dot, CH3NH3PbCl3Nanometer sheet, FAPbI3Quantum dot, FAPbI3Nanometer sheet, FAPbBr3Quantum dot, FAPbBr3Nanometer sheet,
FAPbCl3Quantum dot or FAPbCl3Nanometer sheet.The present invention, which is directed to, prepares perovskite nano-crystal film, paint finishing reasonable design,
By setting horizontal position moving stage on substrate warm table, it can realize substrate two in terms of level by mobile and horizontal displacement platform
The movement of dimension, it is ensured that the preparation of large area uniform film.
Claims (10)
1. a kind of method that spraying prepares perovskite nano-crystal film, which is characterized in that include the following steps：
1) it is distributed to perovskite is nanocrystalline in organic solvent, obtains the nanocrystalline dispersion liquid of perovskite；
2) the nanocrystalline dispersion liquid of perovskite is fitted into spray bottle, be installed on spray gun, adjust the distance of spray gun and substrate, spray gun
Liquid outlet quantity and air pressure；Then it is sprayed after substrate is heated, after annealing, obtains perovskite nano-crystal film.
2. the method that a kind of spraying according to claim 1 prepares perovskite nano-crystal film, which is characterized in that step 1)
Middle organic solvent is one or more of n-hexane, chloroform, toluene, normal octane.
3. the method that a kind of spraying according to claim 1 prepares perovskite nano-crystal film, which is characterized in that step 1)
A concentration of 0.01~5mg/mL of the middle nanocrystalline dispersion liquid of perovskite.
4. the method that a kind of spraying according to claim 1 prepares perovskite nano-crystal film, which is characterized in that step 1)
Nanocrystalline middle perovskite is CsPbBr3Quantum dot, CsPbBr3Nanometer sheet, CsPbI3Quantum dot, CsPbI3Nanometer sheet, CsPbCl3Amount
Sub- point, CsPbCl3Nanometer sheet, CH3NH3PbI3Quantum dot, CH3NH3PbI3Nanometer sheet, CH3NH3PbBr3Quantum dot,
CH3NH3PbBr3Nanometer sheet, CH3NH3PbCl3Quantum dot, CH3NH3PbCl3Nanometer sheet, FAPbI3Quantum dot, FAPbI3Nanometer sheet,
FAPbBr3Quantum dot, FAPbBr3Nanometer sheet, FAPbCl3Quantum dot or FAPbCl3Nanometer sheet.
5. the method that a kind of spraying according to claim 1 prepares perovskite nano-crystal film, which is characterized in that step 2)
In substrate be rigid basement or flexible substrates.
6. the method that a kind of spraying according to claim 5 prepares perovskite nano-crystal film, which is characterized in that rigid base
Bottom is glass or silicon chip；Flexible substrates are PET or PI.
7. the method that a kind of spraying according to claim 1 prepares perovskite nano-crystal film, which is characterized in that step 2)
The distance of middle spray gun and substrate is 2~10cm, and substrate is horizontal positioned or vertical placement.
8. the method that a kind of spraying according to claim 1 prepares perovskite nano-crystal film, which is characterized in that step 2)
The liquid outlet quantity of middle spray gun is 0.02mL/s, and air pressure is 50~400kPa.
9. the method that a kind of spraying according to claim 1 prepares perovskite nano-crystal film, which is characterized in that step 3)
The temperature of middle heating is 25~150 DEG C；Spray time is 10~360s in step 3).
10. the method that a kind of spraying according to claim 1 prepares perovskite nano-crystal film, which is characterized in that step
4) temperature annealed in is 90~250 DEG C, and the time is 5~60min.
Priority Applications (1)
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| CN110886017A (en) * | 2019-11-29 | 2020-03-17 | 上海应用技术大学 | Preparation method of all-inorganic cesium-lead halogen perovskite nanocrystalline film |
| CN110896129A (en) * | 2018-09-13 | 2020-03-20 | 中国科学院大连化学物理研究所 | Multi-exciton dissociation heterojunction based on perovskite nanocrystalline and acene molecular material |
| CN112038449A (en) * | 2020-08-27 | 2020-12-04 | 上海应用技术大学 | CsPbX prepared by solution spraying method3Film, its preparation and use |
| CN112239409A (en) * | 2019-07-17 | 2021-01-19 | 深圳市惠能材料科技研发中心(有限合伙) | Equipment and method for preparing perovskite material based on atomized gas-liquid solid thermal deposition method |
| CN113782684A (en) * | 2021-09-10 | 2021-12-10 | 华能新能源股份有限公司 | Perovskite thin film and preparation method thereof |
| CN113903859A (en) * | 2021-12-02 | 2022-01-07 | 中国华能集团清洁能源技术研究院有限公司 | Method for preparing perovskite layer by dry method and perovskite type solar device |
| CN115957947A (en) * | 2022-11-29 | 2023-04-14 | 北京大学长三角光电科学研究院 | Coating printing method and apparatus |
| CN115999862A (en) * | 2022-12-29 | 2023-04-25 | 南方科技大学 | Semiconductor porous film and preparation method and application thereof |
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| CN110896129A (en) * | 2018-09-13 | 2020-03-20 | 中国科学院大连化学物理研究所 | Multi-exciton dissociation heterojunction based on perovskite nanocrystalline and acene molecular material |
| CN112239409A (en) * | 2019-07-17 | 2021-01-19 | 深圳市惠能材料科技研发中心(有限合伙) | Equipment and method for preparing perovskite material based on atomized gas-liquid solid thermal deposition method |
| CN112239409B (en) * | 2019-07-17 | 2023-06-27 | 深圳市惠能材料科技研发中心(有限合伙) | Device and method for preparing perovskite material based on atomization gas-liquid-solid thermal deposition method |
| CN110886017A (en) * | 2019-11-29 | 2020-03-17 | 上海应用技术大学 | Preparation method of all-inorganic cesium-lead halogen perovskite nanocrystalline film |
| CN112038449A (en) * | 2020-08-27 | 2020-12-04 | 上海应用技术大学 | CsPbX prepared by solution spraying method3Film, its preparation and use |
| CN113782684A (en) * | 2021-09-10 | 2021-12-10 | 华能新能源股份有限公司 | Perovskite thin film and preparation method thereof |
| CN113782684B (en) * | 2021-09-10 | 2022-10-21 | 华能新能源股份有限公司 | Perovskite thin film and preparation method thereof |
| CN113903859A (en) * | 2021-12-02 | 2022-01-07 | 中国华能集团清洁能源技术研究院有限公司 | Method for preparing perovskite layer by dry method and perovskite type solar device |
| CN115957947A (en) * | 2022-11-29 | 2023-04-14 | 北京大学长三角光电科学研究院 | Coating printing method and apparatus |
| CN115957947B (en) * | 2022-11-29 | 2023-08-29 | 北京大学长三角光电科学研究院 | Coating printing method and apparatus |
| CN115999862A (en) * | 2022-12-29 | 2023-04-25 | 南方科技大学 | Semiconductor porous film and preparation method and application thereof |
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