CN105655447B - Large-area preparation method of perovskite films suitable for various substrate shapes - Google Patents
Large-area preparation method of perovskite films suitable for various substrate shapes Download PDFInfo
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- 239000000758 substrate Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 28
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 4
- 239000010408 film Substances 0.000 claims description 61
- 239000010409 thin film Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000005987 sulfurization reaction Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 230000031700 light absorption Effects 0.000 abstract description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 2
- 230000003321 amplification Effects 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 238000007654 immersion Methods 0.000 abstract 2
- 229940056932 lead sulfide Drugs 0.000 abstract 2
- 229910052981 lead sulfide Inorganic materials 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- 239000008139 complexing agent Substances 0.000 abstract 1
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 229910052717 sulfur Inorganic materials 0.000 abstract 1
- 239000011593 sulfur Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 14
- 238000004528 spin coating Methods 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 2
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical group [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 208000003556 Dry Eye Syndromes Diseases 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- NPNMHHNXCILFEF-UHFFFAOYSA-N [F].[Sn]=O Chemical compound [F].[Sn]=O NPNMHHNXCILFEF-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- JYMITAMFTJDTAE-UHFFFAOYSA-N aluminum zinc oxygen(2-) Chemical compound [O-2].[Al+3].[Zn+2] JYMITAMFTJDTAE-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 229940071870 hydroiodic acid Drugs 0.000 description 1
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- RQQRAHKHDFPBMC-UHFFFAOYSA-L lead(ii) iodide Chemical compound I[Pb]I RQQRAHKHDFPBMC-UHFFFAOYSA-L 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention discloses a large-area preparation method of perovskite films suitable for various substrate shapes. The method is characterized by comprising steps as follows: lead nitrate is used as a lead source, thiourea is used as a sulfur source, ammonia water is used as a complexing agent, the reaction speed and temperature are controlled, and lead sulfide films are produced on substrates in any shapes through chemical baths; then the lead sulfide films are converted into perovskite light absorption layer film materials with a solution immersion method or a chemical vapor deposition method. Perovskite light absorption layers are prepared through the chemical baths in combination with the solution immersion method or the chemical vapor deposition method, the method has the advantages of low cost, simplicity in operation, capability of realizing large-area amplification and the like, meanwhile, the prepared films are not affected by the substrate shapes and materials, and the high-quality perovskite films can be prepared on rigid or flexible substrates in various complex shapes such as curved surfaces, spherical surfaces and the like.
Description
Technical field
The present invention relates to a kind of perovskite thin film large area preparation method being suitable to various substrate shape, belong to the film sun
The preparation technology field of energy cell photovoltaic device.
Background technology
With the high speed development of human society, people also increase sharply to the demand of the energy, thus lead to energy crisis and
The gradually aggravation of environmental pollution, has caused the active demand to sustainable energy for the people.In wind-powered electricity generation, water power, geothermal energy, living beings
Can and the various regenerative resources such as solar energy in, solar energy is safe and pollution-free, do not limited by geographical conditions, range of application
Extensively, most rising one kind.2009, hybrid inorganic-organic perovskite was applied to for the first time by Miyasaka et al.
Photovoltaic art, using CH3NH3PbI23As light absorbing zone, achieve 3.8% photoelectric transformation efficiency.Hereafter, a few years
Interior, perovskite solar cell achieves major progress in photoelectric transformation efficiency.According to U.S.'s regenerative resource laboratory
The new battery efficiency data announced, the peak efficiency up to 20.1% of the current certification of perovskite solar cell is so as to surmount
Traditional DSSC and organic solar batteries, become the third generation film sun of most practical application foreground
Can battery.Perovskite solar cell also therefore by《Science》It is chosen as one of ten big sciences breakthroughs in 2013.
Perovskite solar cell is generally by being sequentially depositing electron transfer layer, perovskite light absorbs on electro-conductive glass
Layer film, hole transmission layer and top electrode and formed；The preparation method of wherein high-quality perovskite light absorbing zone film is calcium titanium
One of key technology of ore deposit solar cell industrialization.Traditional perovskite solar cell light absorption layer method for manufacturing thin film is general
It is divided into double source coevaporation method, solwution method, gas phase auxiliary law.Snaith et al. has developed double source coevaporation method, and to prepare perovskite thin
Film, will perovskite presoma PbI2And CH3NH3I is deposited with substrate in the case of high vacuum, and then annealing obtains calcium
Titanium ore film (Nature, 501,395-398,2013), the uniformity of film that this method obtains, crystallinity are all very high, but
It is that vacuum equipment needed for the method is expensive, preparation process is complicated, and parameter request controls accurately, required governing factor is more.
Yin Hangtian of Xi'an Communications University et al. prepares perovskite thin film by solwution method, and in spin coating final stage, by dropping
Organic solvent is processed to film, obtains uniform and smooth perovskite thin film (CN 104900810 A).HeFei University of Technology
Sieve send peak et al. pass through spin coating PbI2Film, then gas phase auxiliary law prepare densification, uniform perovskite thin film (CN
104393109 A).Above-mentioned solwution method and gas phase auxiliary law are required to spin coating precursor solution, and using of solution spin-coating method limits
Make the extensive preparation of perovskite thin film, the film that spin coating goes out has rough porous, poor repeatability, film coverage etc. and lacks
Point.What is more important, spin-coating method cannot prepare large-area film it is difficult to industrial applications are amplified.Meanwhile, spin coating proceeding
Backing material be necessarily the rigid substrate of planar structure, the rigid substrate for complicated shapes such as curved surface, spheres is it is difficult to molten
Prepared by liquid spin-coating method；And flexible substrate is more difficult to carry out spin coating operation, limit the exploitation of flexible perovskite photovoltaic device
Application.For this reason, research and development inexpensive, simple to operate, can large area amplify and be suitable to various substrate shape structures and material growth
Perovskite thin film material preparation technology is just particularly important.
Content of the invention
For the defect of above prior art, the present invention provides a kind of big face of perovskite thin film being suitable to various substrate shape
Long-pending preparation method, the method is with low cost, simple to operate, can large area amplify, simultaneously no special to substrate shape and material will
Ask.
The present invention solves technical problem, adopts the following technical scheme that：
The present invention is suitable to the perovskite thin film large area preparation method of various substrate shape, and its feature is including walking as follows
Suddenly：
1) rigidity of arbitrary shape or flexible substrate are cleaned, dried up, standby；
2) plumbi nitras, thiocarbamide, ammoniacal liquor and deionized water are added in beaker, stirring and dissolving, obtain vulcanized lead reaction solution；
3) by step 1) process after substrate put into step 2) in the vulcanized lead reaction solution prepared, be then placed in water-bath
Middle reaction, generates PbS film in substrate surface；React taking-up after terminating, deionized water flushing surface, dry up, standby；
4) first PbS film and Iod R are converted into PbI2Film；Then by PbI2Film is immersed in CH3NH3In I solution,
Perovskite light absorbing zone CH is obtained by solution infusion method3NH3PbI3Film；
Or：By PbS film and CH3NH3I powder, as reactant, obtains perovskite light by chemical vapour deposition technique and inhales
Receive layer CH3NH3PbI3Film.
Above-mentioned preparation method is specifically carried out as follows：
1) rigidity of arbitrary shape or flexible substrate are cleaned with suds, acetone, EtOH Sonicate successively, then use nitrogen wind
Dry up, standby.
2) Pb (NO for 0.015M by 20mL concentration3)2Solution, 10mL concentration are the thiourea solution of 1.5M, 26mL mass is dense
Spend the ammoniacal liquor for 25～28% and 144mL deionized water adds in the beaker of 250mL, then at room temperature with 500～1500rpm
Speed stir 5 minutes, that is, obtain vulcanized lead reaction solution.
3) by step 1) process after substrate put into step 2) in the vulcanized lead reaction solution prepared, being then placed in temperature is
React in 60～90 DEG C of water-bath 5～40 minutes, generate PbS film in substrate surface；Reaction terminate after take out, spend from
Sub- water rinses surface, dries up, standby；
Step 4) PbS film and 1～10g iodine are positioned on warm table, and covered with black lid, it is heated to 60～
150 DEG C, react 10～120 minutes, obtain PbI2Film；By PbI2Film temperature be 20～70 DEG C, concentration be 10mg/mL
CH3NH3Soak 1～20 minute in I aqueous isopropanol, then take out, dry up, that is, obtain perovskite light absorbing zone CH3NH3PbI3Thin
Film；
Or：CH by PbS film and 2g3NH3I powder, as reactant, is positioned over full of on the warm table of atmosphere protection,
It is heated to 100～250 DEG C, react 5～120 minutes, that is, obtain perovskite light absorbing zone CH3NH3PbI3Film.Wherein, described gas
Atmosphere is protected as inert gas (as nitrogen, argon gas) protection or vacuum environment.
Above-mentioned CH3NH3The preparation method of I powder referring to patent CN 104393109A, step is：The methylamine methyl alcohol of 24mL is molten
The aqueous solution (45wt%) the reaction 2h of the hydroiodic acid of liquid (33wt%) and 10mL or HCl, the precipitation obtaining is dissolved in 80mL ethanol,
Add 300mL ether, the precipitation obtaining is dried 24h, that is, obtains white CH3NH3I.
In above-mentioned preparation method, substrate has transparent electrode material (as fluorine tin-oxide (FTO), the oxidation of indium tin for growth
Thing (ITO), aluminium zinc oxide (AZO) etc.) nonbreakable glass or flexiplast, its shape can be plane, curved surface or sphere etc.
Variously-shaped.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1st, the preparation method of perovskite thin film of the present invention, is not affected by substrate shape and material, can be in curved surface, sphere etc.
High-quality perovskite thin film is prepared on variously-shaped rigidity or flexible substrate, range of application is widely；
2nd, the preparation method of the present invention is simple, can be prevented effectively from the loaded down with trivial details glove box of current perovskite solar cell preparation
Operation and expensive vacuum evaporation apparatus put into, and in normal circumstances, realize the low-cost and high-quality of perovskite light absorbing zone film
Preparation；
3rd, the preparation method of the present invention is with low cost, large area can prepare perovskite light absorbing zone film, and this chemical bath
Method can industrialize amplification easily, and the commercial applications promoting perovskite solar cell are had great importance；
Brief description
Fig. 1 be the embodiment of the present invention 1 prepared by large area, curved surface CH3NH3PbI3The photo of film；
Fig. 2 (a) is the CH prepared by the embodiment of the present invention 13NH3PbI3The XRD (Fig. 2 (a)) of film and light absorbs figure
(Fig. 2 (b))；
Fig. 3 is the CH prepared by the embodiment of the present invention 13NH3PbI3The SEM figure of film；
Specific embodiment
Embodiment 1
The present embodiment, with curved surface nonbreakable glass as substrate, is prepared perovskite light absorbing zone film, is comprised the following steps that：
A, clean bend glass substrate 20 minutes with suds, acetone, EtOH Sonicate respectively, then use nitrogen wind to do, standby
With；
B, in the beaker of 250mL add 20mL concentration be 0.015M Pb (NO3)2Solution, 10mL concentration are the sulphur of 1.5M
Urea solution, 26mL mass concentration are 26% ammoniacal liquor and the addition of 144mL deionized water, then at room temperature with the speed of 1000rpm
Degree stirring 5 minutes, that is, obtain vulcanized lead reaction solution.
C, the substrate of wash clean is put in vulcanized lead reaction solution, then beaker is put in 70 DEG C of water-bath, instead
Answer 30 minutes；Terminate through chemical bath reaction, substrate taken out and deionized water is rinsed sample surfaces, used nitrogen wind dry-eye disease,
Obtain high-quality PbS precursor thin-film；
D, by the CH of PbS film and 2g3NH3I powder, as reactant, is placed on the warm table full of nitrogen atmosphere protection,
It is heated to 150 DEG C, react 120 minutes, obtain final product CH3NH3PbI3Film.
Fig. 1 is large area, curved surface perovskite CH prepared by the present embodiment3NH3PbI3The photo of film and size comparison's figure,
As can be seen from the figure the present embodiment is prepared in curved substrate perovskite thin film unusual light, uniformly；
Fig. 2 (a) is the CH prepared by the present embodiment3NH3PbI3The XRD of film, as can be seen from the figure the present embodiment is made
Standby CH3NH3PbI3The peak of film is 14.04 °, 28.38 °, 31.79 ° and 43.08 °, and PbS has been completely converted into CH3NH3PbI3；
Fig. 2 (b) is the CH prepared by the present embodiment3NH3PbI3The light absorbs figure of film, as can be seen from the figure this enforcement
CH prepared by example3NH3PbI3The ABSORPTION EDGE of film is 790nm, and optical band gap is 1.57eV；
Fig. 3 is CH3NH3PbI3The SEM figure of film, the as can be seen from the figure CH prepared by the present embodiment3NH3PbI3Film
Quality is high, substrate spreadability is good.
Embodiment 2
The present embodiment prepares perovskite light absorbing zone CH by embodiment 1 identical mode3NH3PbI3Film, difference only exists
In：In step d, the temperature of warm table is 180 DEG C, and the reaction time is 30 minutes.
Through characterizing, the CH prepared by the present embodiment3NH3PbI3Film to be that embodiment 1 is similar, surface is uniform and smooth, film
Quality is high.
Embodiment 3
The present embodiment prepares perovskite light absorbing zone CH by embodiment 1 identical mode3NH3PbI3Film, differs only in
Step d is to carry out as follows：
Using PbS film as reactant, it is positioned on warm table, aside puts 2g iodine, then use black lid lid
Live, be heated to 100 DEG C, react 60 minutes, obtain PbI2Film；
By PbI2Film is immersed in the CH that concentration is 10mg/mL3NH3In I aqueous isopropanol, soak time is 2 minutes, leaching
Bubble temperature is 25 DEG C, and reaction completes to take out and dries up, and obtains final product CH3NH3PbI3Film.
Through characterizing, the CH prepared by the present embodiment3NH3PbI3Film to be that embodiment 1 is similar, surface is uniform and smooth, film
Quality is high.
Embodiment 4
The present embodiment prepares CH by embodiment 3 identical mode3NH3PbI3Film, differs only in：Step d prepares PbI2
During film, the temperature of warm table is 80 DEG C, and the reaction time is 50 minutes.
Through characterizing, the CH prepared by the present embodiment3NH3PbI3Film to be that embodiment 1 is similar, surface is uniform and smooth, film
Quality is high.
Embodiment 5
The present embodiment prepares perovskite light absorbing zone CH by embodiment 1 identical mode3NH3PbI3Film, difference only exists
In：Substitute glass rigid substrate using flexible polyimides (PI) substrate.
Through characterizing, the CH prepared by the present embodiment3NH3PbI3Film to be that embodiment 1 is similar, surface is uniform and smooth, film
Quality is high.
Claims (6)
1. a kind of perovskite thin film large area preparation method being suitable to various substrate shape is it is characterised in that comprise the steps：
1) rigidity of arbitrary shape or flexible substrate are cleaned, dried up, standby；
2) plumbi nitras, thiocarbamide, ammoniacal liquor and deionized water are added in beaker, stirring and dissolving, obtain vulcanized lead reaction solution；
3) by step 1) process after substrate put into step 2) in the vulcanized lead reaction solution prepared, be then placed in water-bath anti-
Should, generate PbS film in substrate surface；React taking-up after terminating, deionized water flushing surface, dry up, standby；
4) by PbS film and CH3NH3I powder, as reactant, obtains perovskite light absorbing zone by chemical vapour deposition technique
CH3NH3PbI3Film.
2. preparation method according to claim 1 it is characterised in that：Step 1) method be：Rigidity by arbitrary shape
Or flexible substrate cleaned with suds, acetone, EtOH Sonicate successively, nitrogen wind is then used to do, standby.
3. preparation method according to claim 1 it is characterised in that：Step 2) method be：20mL concentration is
Pb (the NO of 0.015M3)2Solution, 10mL concentration are the thiourea solution of 1.5M, 26mL mass concentration be 25～28% ammoniacal liquor and
144mL deionized water adds in beaker, is then stirred 5 minutes with the speed of 500～1500rpm at room temperature, that is, obtains sulfuration
Lead reaction solution.
4. preparation method according to claim 1 it is characterised in that：Step 3) in water-bath temperature be 60～90 DEG C,
Reaction time is 5～40 minutes.
5. preparation method according to claim 1 it is characterised in that：Step 4) method be：
By PbS film and CH3NH3I powder as reactant, be positioned over full of on the warm table of atmosphere protection, being heated to 100～
250 DEG C, react 5～120 minutes, that is, obtain perovskite light absorbing zone CH3NH3PbI3Film.
6. preparation method according to claim 5 it is characterised in that：Described atmosphere protection is inert gas shielding or vacuum
Environment.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103440988A (en) * | 2013-07-22 | 2013-12-11 | 华侨大学 | Preparation method of hybridization solar battery for perovskite-like sensitized photoanode |
| CN104103759A (en) * | 2014-07-17 | 2014-10-15 | 北京化工大学 | Fibrous solar battery based on perovskite type organic lead and iodine compound and preparation method thereof |
| CN104393109A (en) * | 2014-10-28 | 2015-03-04 | 合肥工业大学 | Chemical vapor deposition preparation method for perovskite solar cell |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103440988A (en) * | 2013-07-22 | 2013-12-11 | 华侨大学 | Preparation method of hybridization solar battery for perovskite-like sensitized photoanode |
| CN104103759A (en) * | 2014-07-17 | 2014-10-15 | 北京化工大学 | Fibrous solar battery based on perovskite type organic lead and iodine compound and preparation method thereof |
| CN104393109A (en) * | 2014-10-28 | 2015-03-04 | 合肥工业大学 | Chemical vapor deposition preparation method for perovskite solar cell |
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| CN105655447A (en) | 2016-06-08 |
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