LU502229A1 - Method for preparing organic-inorganic hybrid perovskite film and method for preparing semitransparent solar cell - Google Patents
Method for preparing organic-inorganic hybrid perovskite film and method for preparing semitransparent solar cell Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000002904 solvent Substances 0.000 claims abstract description 33
- 239000002243 precursor Substances 0.000 claims abstract description 30
- 239000012046 mixed solvent Substances 0.000 claims abstract description 19
- QHJPGANWSLEMTI-UHFFFAOYSA-N aminomethylideneazanium;iodide Chemical compound I.NC=N QHJPGANWSLEMTI-UHFFFAOYSA-N 0.000 claims abstract description 17
- ISWNAMNOYHCTSB-UHFFFAOYSA-N methanamine;hydrobromide Chemical compound [Br-].[NH3+]C ISWNAMNOYHCTSB-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000000137 annealing Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 13
- RAJISUUPOAJLEQ-UHFFFAOYSA-N chloromethanamine Chemical compound NCCl RAJISUUPOAJLEQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims abstract description 10
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZFPGARUNNKGOBB-UHFFFAOYSA-N 1-Ethyl-2-pyrrolidinone Chemical compound CCN1CCCC1=O ZFPGARUNNKGOBB-UHFFFAOYSA-N 0.000 claims abstract description 9
- GGYVTHJIUNGKFZ-UHFFFAOYSA-N 1-methylpiperidin-2-one Chemical compound CN1CCCCC1=O GGYVTHJIUNGKFZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 78
- 239000011521 glass Substances 0.000 claims description 35
- 230000005525 hole transport Effects 0.000 claims description 22
- 239000002184 metal Substances 0.000 claims description 12
- 229910052751 metal Inorganic materials 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 10
- CWERGRDVMFNCDR-UHFFFAOYSA-N thioglycolic acid Chemical compound OC(=O)CS CWERGRDVMFNCDR-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- FWPIDFUJEMBDLS-UHFFFAOYSA-L tin(II) chloride dihydrate Chemical compound O.O.Cl[Sn]Cl FWPIDFUJEMBDLS-UHFFFAOYSA-L 0.000 claims description 8
- 238000007738 vacuum evaporation Methods 0.000 claims description 8
- XDXWNHPWWKGTKO-UHFFFAOYSA-N 207739-72-8 Chemical compound C1=CC(OC)=CC=C1N(C=1C=C2C3(C4=CC(=CC=C4C2=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC(=CC=C1C1=CC=C(C=C13)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 XDXWNHPWWKGTKO-UHFFFAOYSA-N 0.000 claims description 7
- 150000001868 cobalt Chemical class 0.000 claims description 6
- YSHMQTRICHYLGF-UHFFFAOYSA-N 4-tert-butylpyridine Chemical compound CC(C)(C)C1=CC=NC=C1 YSHMQTRICHYLGF-UHFFFAOYSA-N 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 31
- 238000002360 preparation method Methods 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 11
- 238000004528 spin coating Methods 0.000 description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000007547 defect Effects 0.000 description 8
- 239000012296 anti-solvent Substances 0.000 description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000005520 cutting process Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000010899 nucleation Methods 0.000 description 4
- 230000006911 nucleation Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
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- 238000013461 design Methods 0.000 description 2
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- 239000011148 porous material Substances 0.000 description 2
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- 238000004458 analytical method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000010147 laser engraving Methods 0.000 description 1
- QSZMZKBZAYQGRS-UHFFFAOYSA-N lithium;bis(trifluoromethylsulfonyl)azanide Chemical compound [Li+].FC(F)(F)S(=O)(=O)[N-]S(=O)(=O)C(F)(F)F QSZMZKBZAYQGRS-UHFFFAOYSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/40—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising a p-i-n structure, e.g. having a perovskite absorber between p-type and n-type charge transport layers
-
- 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
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
-
- 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
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
- H10K85/50—Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
-
- 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
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- 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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Abstract
Disclosed are a method for preparing an organic-inorganic hybrid perovskite film and a method for preparing a semitransparent solar cell. The method for preparing an organic-inorganic hybrid perovskite film includes: dissolving and mixing methyl ammonium bromide, lead bromide, lead iodide, formamidine hydroiodide and chloromethylamine in a mixed solvent to obtain a precursor solution; and coating the precursor solution on a substrate, annealing at 65°C-75°C for 4 min-6 min, and then annealing at 145°C-155°C for 8 min-12 min to obtain the organic-inorganic hybrid perovskite film. The mixed solvent comprises DMF and a first solvent, a volume ratio of the DMF to the first solvent is 8.9-9.1: 0.9-1.1, and the first solvent comprises N-ethyl-2-pyrrolidone, N-methyl-2-piperidone and N-N-2-methylacetamide.
Description
METHOD FOR PREPARING ORGANIC-INORGANIC HYBRID PEROVSKITE FILM AND METHOD
FOR PREPARING SEMITRANSPARENT SOLAR CELL (0006668
[0001] This application claims priority to Chinese Patent Application No. 202210358946.X, filed on April 2, 2022, the entire disclosure of which is incorporated herein by reference.
[0002] The present disclosure relates to the technical field of solar cells, and in particular to a method for preparing an organic-inorganic hybrid perovskite film and a method for preparing a semitransparent solar cell.
[0003] Since the organic-inorganic hybrid perovskite solar cells were first reported in 2009, after 10 years of rapid development, the photoelectric conversion efficiency has exceeded 25% by 2021, reaching 95% of the efficiency of monocrystalline silicon solar cells, with excellent photoelectric performance. The rapid development of the organic-inorganic hybrid perovskite solar cells is attributed to the advantages of simple preparation process, low preparation cost, tunable band gap, high carrier diffusion length and high absorption coefficient. The organic-inorganic hybrid perovskite is considered as one of the candidate materials for high-efficiency solar cells (PSCs), and has potential application values in photovoltaics. However, how to construct organic-inorganic hybrid perovskite films with good morphology, high crystallinity and low defect density through suitable processes is the research focus of the commercialization of perovskite solar cells in the future for the reason that this directly affects the performance of perovskite solar cells.
[0004] Nowadays, the processes for preparing organic-inorganic hybrid perovskite films are roughly divided into continuous deposition, solution method, meteorological-assisted deposition and vacuum evaporation. In the solution method, one-step method is the most widely used. The one-step method is to prepare a perovskite precursor solution first, then spin-coat the perovskite precursor solution, and add an anti-solvent during the process of spin-coating the precursor, to promote the nucleation and crystallization of perovskite, and finally the perovskite film is obtained by annealing treatment. This method is simple to operate, but very sensitive to conditions. The solvent selection of the precursor solution, as well as the time and speed of anti-solvent addition will affect the film properties, resulting in poor control of the quality of the perovskite film. Meanwhile, annealing volatilizes the perovskite precursor solution and components, to make grain aggregate and shrink, forming gaps, holes and other defects during the spin-coating of the perovskite layer, thereby being unable to make perovskite 5229 films with uniform grain size and smooth uniformity. In addition, during the process of preparing perovskite films in large scale, in the existing one-step process, since the anti-solvent cannot be added, the prepared perovskite film has many pores, which seriously damages the performance of perovskite solar cells. Therefore, one-step spin-coating process based on anti-solvent extraction cannot be applied to the preparation of perovskite cells in large scale.
[0005] The main objective of the present disclosure is to propose a method for preparing an organic-inorganic hybrid perovskite film and a method for preparing a semitransparent solar cell, which aims to provide an organic-inorganic hybrid perovskite film with good morphology, high crystallinity, low defect density and large-scale preparation.
[0006] In order to achieve the above objective, the present disclosure provides a method for preparing an organic-inorganic hybrid perovskite film, including following steps:
[0007] dissolving and mixing methyl ammonium bromide, lead bromide, lead iodide, formamidine hydroiodide and chloromethylamine in a mixed solvent to obtain a precursor solution; and
[0008] coating the precursor solution on a substrate, annealing at 65°C-75°C for 4 min-6 min, and then annealing at 145°C-155°C for 8 min-12 min to obtain the organic-inorganic hybrid perovskite film;
[0009] the mixed solvent includes DMF and a first solvent, a volume ratio of the DMF to the first solvent is 8.9-9.1: 0.9-1.1, and the first solvent includes N-ethyl-2-pyrrolidone,
N-methyl-2-piperidone and N-N-2-methylacetamide.
[0010] In an embodiment, the volume ratio of the DMF to the first solvent is 9: 1; and/or a concentration of the precursor solution is 1.5 mol/L -1.6 mol/L.
[0011] In an embodiment, in the first solvent, a volume ratio of N-ethyl-2-pyrrolidone,
N-methyl-2-piperidone and N-N-2-methylacetamide is 2.8-3.2: 3.8-4.2: 3.
[0012] In an embodiment, in the first solvent, the volume ratio of N-ethyl-2-pyrrolidone,
N-methyl-2-piperidone and N-N-2-methylacetamide is 3: 4: 3.
[0013] In an embodiment, a mass ratio of the methyl ammonium bromide, lead bromide, lead iodide, formamidine hydroiodide and chloromethylamine is 7.5-7.8: 25-26: 647-648: 241-242: 33.
[0014] In an embodiment, the mass ratio of the methyl ammonium bromide, lead bromide,
lead iodide, formamidine hydroiodide and chloromethylamine is 7.7: 25.3: 647.4: 241.6: 33.
LU502229
[0015] The present disclosure further provides a method for preparing a semitransparent solar cell, including following steps:
[0016] providing a conductive glass;
[0017] disposing an electron transport layer on the conductive glass;
[0018] disposing an organic-inorganic hybrid perovskite film on the electron transport layer, wherein the organic-inorganic hybrid perovskite film is prepared by the method for preparing the organic-inorganic hybrid perovskite film according to any one of claims 1 to 6;
[0019] disposing a hole transport layer on the organic-inorganic hybrid perovskite film; and
[0020] disposing a metal electrode layer on the hole transport layer to obtain the semitransparent solar cell.
[0021] In an embodiment, the step of disposing the electron transport layer on the conductive glass includes:
[0022] mixing urea, hydrochloric acid, thioglycolic acid, stannous chloride dihydrate and deionized water to obtain a first solution; and
[0023] placing the conductive glass in the first solution, soaking at 80°C-100°C for 2 hours-3 hours, and annealing at 175°C-185°C for 50 minutes-70 minutes to obtain the electron transport layer disposed on the conductive glass.
[0024] In an embodiment, the step of disposing the hole transport layer on the organic-inorganic hybrid perovskite film includes:
[0025] mixing Spiro-OMeTAD, chlorobenzene, Li-TFSI solution, cobalt salt solution and 4-tert-butylpyridine to obtain a second solution; and
[0026] coating the second solution on the organic-inorganic hybrid perovskite film to obtain the hole transport layer.
[0027] In an embodiment, the step of disposing the metal electrode layer on the hole transport layer includes:
[0028] depositing Ag on the hole transport layer by vacuum evaporation to obtain the metal electrode layer.
[0029] In technical solutions of the present disclosure, the composition and ratio of the mixed solvent in the precursor solution are designed, to prepare the organic-inorganic hybrid perovskite film with good morphology, high crystallinity and low defect density, so that the perovskite solar cell prepared by the organic-inorganic hybrid perovskite film has excellent performance. Meanwhile, the addition of anti-solvent is omitted, thereby realizing the large-scale preparation of perovskite films, and the process is simple to operate, easy to control,
LU502229 and suitable for large-scale production.
[0030] In order to more clearly illustrate the embodiments of the present disclosure or the technical solutions in the prior art, the following briefly introduces the accompanying drawings that need to be used in the description of the embodiments or the prior art. Obviously, the drawings in the following description are only some embodiments of the present disclosure, and for those skilled in the art, other related drawings can also be obtained from these drawings without creative effort.
[0031] FIG. 1 is XRD images of organic-inorganic hybrid perovskite film prepared in step (4) in Example 1 and Comparative Examples 1-4 of the present disclosure.
[0032] FIG. 2 is electron microscope images of the organic-inorganic hybrid perovskite film prepared in step (4) in Example 1 and Comparative Examples 1-4 of the present disclosure.
[0033] FIG. 3 is photovoltaic characteristics of the semitransparent solar cell prepared in
Example 1 of the present disclosure.
[0034] FIG. 4 is a schematic diagram of the organic-inorganic hybrid perovskite film prepared in step (4) in Example 4 of the present disclosure.
[0035] FIG. 5 is the photovoltaic characteristics of the large-area semitransparent solar cell prepared in Example 4 of the present disclosure.
[0036] The realization of the objective, functional characteristics, and advantages of the present disclosure are further described with reference to the accompanying drawings.
[0037] To make the purposes, technical solutions and advantages of the embodiments of the present disclosure more clear, the technical solutions in the embodiments of the present disclosure will be described clearly and completely below. If the specific conditions are not indicated in the examples, it is carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used without the manufacturer's indication are conventional products that can be purchased from the market.
[0038] Besides, the meaning of “and/or” appearing in the disclosure includes three parallel scenarios. For example, “A and/or B” includes only A, or only B, or both A and B. In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the realization of those of ordinary skill in the art. When the combination of technical solutions is contradictory or cannot be achieved, it should be
LU502229 considered that such a combination of technical solutions does not exist, nor is it within the scope of the present disclosure.
[0039] Based on the embodiments in the present disclosure, all other embodiments 5 obtained by those of ordinary skill in the art without creative work fall within the scope of the present disclosure.
[0040] The present disclosure provides a method for preparing an organic-inorganic hybrid perovskite film. In an embodiment, the method includes following steps:
[0041] Step S10, dissolving and mixing methyl ammonium bromide, lead bromide, lead iodide, formamidine hydroiodide and chloromethylamine in a mixed solvent to obtain a precursor solution.
[0042] The mixed solvent includes DMF (i.e., N,N-dimethylformamide) and a first solvent, a volume ratio of the DMF to the first solvent is 8.9-9.1: 0.9-1.1, and the first solvent includes
N-ethyl-2-pyrrolidone, N-methyl-2-piperidone and N-N-2-methylacetamide. In an embodiment, the volume ratio of the DMF to the first solvent is 9: 1, and under the above ratio, the performance of the prepared perovskite film is better.
[0043] It should be noted that, for convenience of description, N-ethyl-2-pyrrolidone is abbreviated as N1, N-methyl-2-piperidone is abbreviated as N2, and N-N-2-methylacetamide is abbreviated as N3.
[0044] Further, in the first solvent, the volume ratio of N1, N2 and N3 is 2.8-3.2: 3.8-4.2: 3, that is, it can be 2.8: 4.2: 3, 2.9: 4.1: 3, 2.8: 3.8: 4, 3: 4: 3, 3: 4.2: 3, or the like. In an embodiment, the volume ratio of N1, N2 and N3 is 3: 4: 3. Under the above ratio, the mixed solvent can prepare uniform grain size and smooth perovskite film. Meanwhile, it can also promote the rapid volatilization of the mixed solvent during the annealing process, make the perovskite film reach a supersaturated state, and promote nucleation and crystallization, so that the prepared perovskite film has high crystallinity and low defect density. In addition, during the preparation process, the addition of anti-solvent is reduced, enabling large-scale preparation of perovskite films.
[0045] The concentration of the precursor solution will also affect the properties of the prepared perovskite film. In this embodiment, the concentration of the precursor solution is 1.5-1.6 mol/L, that is, it may be 1.5 mol/L, 1.51 mol/L, 1.53 mol/L, 1.54 mol/L, 1.57 mol/L, 1.6 mol/L, or the like, preferably 1.53 mol/L. mol/L is abbreviated as M.
[0046] In this embodiment, the mass ratio of the methyl ammonium bromide (MABr), lead bromide (PbBrz), lead iodide (Pblz), formamidine hydroiodide (FAI) and chloromethylamine (MACI) is 7.5-7.8: 25-26: 647-648: 241-242: 33. In an embodiment, the mass ratio of methyl ammonium bromide, lead bromide, lead iodide, formamidine hydroiodide and chloromethylamine is 7.7: 25.3: 647.4: 241.6: 33. In this way, the prepared precursor solution was (FAIPbls)o.95(MAPbBr;.2Clo.g)o.0s.
[0047] Operation S20, coating the precursor solution on a substrate, annealing at 65°C-75°C for 4 min-6 min, and then annealing at 145°C-155°C for 8 min-12 min to obtain the organic-inorganic hybrid perovskite film.
[0048] The specific method of coating is not limited in the present disclosure, and methods such as spin coating, brush coating, and spray coating may be used. In this embodiment, the spin coating is used. In an embodiment, the spin coating speed is 6000 rpm, and the spin coating time is 30 s.
[0049] The present disclosure provides a method for preparing an organic-inorganic hybrid perovskite film, the composition and ratio of the mixed solvent in the precursor solution are designed, to prepare the organic-inorganic hybrid perovskite film with good morphology, high crystallinity and low defect density, so that the perovskite solar cell prepared by the organic-inorganic hybrid perovskite film has excellent performance. Meanwhile, the addition of anti-solvent is omitted, thereby realizing the large-scale preparation of perovskite films, and the process is simple to operate, easy to control, and suitable for large-scale production.
[0050] In addition, the preparation method provided in the present disclosure optimizes parameters such as the concentration of the precursor solution, the ratio of the first solvent, and the mass ratio between the solutes, so that the prepared perovskite film has better performance.
[0051] Besides, the present disclosure further provides a method for preparing a semitransparent solar cell, including following steps:
[0052] Step A1, providing a conductive glass.
[0053] The conductive glass is FTO. The conductive glass FTO needs to be pretreated first, so that the electron transport layer can be better combined with the conductive glass. The pretreatment may include steps such as cleaning, drying, and hydrophobic modification. In this embodiment, the pretreatment step includes: ultrasonically cleaning the FTO conductive glass in deionized water, absolute ethanol, acetone and isoacetone in sequence for 15 minutes each, and finally drying with nitrogen.
[0054] Step A2, disposing an electron transport layer on the conductive glass.
[0055] The step A2 includes:
LU502229
[0056] Step A21, mixing urea, hydrochloric acid, thioglycolic acid, stannous chloride dihydrate and deionized water to obtain a first solution.
[0057] The present disclosure does not limit the addition amount of each component in the first solution. In an embodiment, the preparation method of the first solution is as follows: in 50 mL of deionized water, adding 625 mg of urea, 625 pL of hydrochloric acid, 12.5 pL of thioglycolic acid, and 137.5 mg of stannous chloride dihydrate (SnCl>e2H20), and mixing well to obtain the first solution.
[0058] Step A22, placing the conductive glass in the first solution, soaking at 80°C-100°C for 2 hours-3 hours, and annealing at 175°C-185°C for 50 minutes-70 minutes to obtain the electron transport layer disposed on the conductive glass.
[0059] In an embodiment, the conductive glass is placed in the first solution, soaked at 90°C for 2.5 hours, and then annealed at 180°C for 60 minutes to obtain the electron transport layer disposed on the conductive glass.
[0060] It should be noted that, in other embodiments of the present disclosure, step Al can also be performed after step A21, or step Al and step A21 can be performed simultaneously. It is only necessary to complete the preparation of the first solution and the conductive glass respectively before the next operation (i.e., before step A22).
[0061] Step A3, disposing an organic-inorganic hybrid perovskite film on the electron transport layer, the organic-inorganic hybrid perovskite film is prepared by the method for preparing the organic-inorganic hybrid perovskite film as described above.
[0062] That is, the precursor solution is coated on the electron transport layer, then annealed at 65-75°C for 4-6 minutes, and then annealed at 145-155°C for 8-12 minutes to obtain the organic-inorganic hybrid perovskite film.
[0063] Step A4, disposing a hole transport layer on the organic-inorganic hybrid perovskite film.
[0064] In this embodiment, the step A4 includes:
[0065] Step A41, mixing Spiro-OMeTAD, chlorobenzene, Li-TFSI solution, cobalt salt solution and 4-tert-butylpyridine to obtain a second solution.
[0066] Spiro-OMeTAD refers to 2,2',7,7'-tetrakis[N,N-bis(4-methoxyphenyl)amino]-9,9'-spirobifluorene. In the Li-TFSI (ie. lithium bistrifluoromethanesulfonimide) solution, 520 mg of Li-TFSI is added to each 1 mL of acetonitrile. In the cobalt salt solution, 300 mg of cobalt salt is added to each 1 mL of acetonitrile, the cobalt salt is FK209. In an embodiment, the preparation method of the second solution is as follows: mixing 54.75 mg of Spiro-OMeTAD with 750 pL of chlorobenzene cag), 889 13.5 ul of Li-TFSI solution, 21.75 uL of FK209 solution, and 22.5 ul of 4-tert-butylpyridine to obtain the second solution.
[0067] Step A42, coating the second solution on the organic-inorganic hybrid perovskite film to obtain the hole transport layer.
[0068] The second solution is coated on the perovskite film by spin coating. In an embodiment, the spin coating speed is 4000 rpm, and the spin coating time is 30 s.
[0069] The present disclosure does not limit the sequence of step A41 and steps A1, A2 and
A3, as long as the preparation of the second solution is completed before step A42.
[0070] Step A5, disposing a metal electrode layer on the hole transport layer to obtain the semitransparent solar cell.
[0071] In an embodiment, Ag is deposited on the hole transport layer by vacuum evaporation to obtain the metal electrode layer, thereby obtaining the organic-inorganic hybrid solar cell, that is, a semitransparent solar cell. Further, the thickness of the metal electrode layer is 80 nm-100 nm; and/or, the vacuum degree of the vacuum evaporation is 2.5x10° Pa.
[0072] The present disclosure provides a method for preparing a semitransparent solar cell.
Through the design of the composition and proportion of the precursor solution, the performance of the prepared solar cell device is better. In this way, when the thickness of the perovskite film is reduced, a high photoelectric conversion efficiency can be achieved, thereby effectively improving the transparency of the solar cell. At the same time, through the design of the composition and proportion of the precursor solution, after annealing, the prepared solar cell has higher transparency. Therefore, the present disclosure finally produces a semitransparent solar cell with good photovoltaic properties, which can be applied to the fields of photovoltaic building integration and the like.
[0073] The technical solutions of the present disclosure will be further described in detail below with reference to specific embodiments and accompanying drawings. It should be understood that the following embodiments are only used to explain the present disclosure, but are not intended to limit the present disclosure.
[0074] The formulations of the first solution and the second solution in the Examples and
Comparative Examples are given below:
[0075] Preparation of the first solution: in 50 mL of deionized water, adding 625 mg of urea, 625 pL of hydrochloric acid, 12.5 ul of thioglycolic acid, and 137.5 mg of SnCl,*2H,0, and mix well to obtain the first solution.
LU502229
[0076] Preparation of the second solution: mixing 54.75 mg of Spiro-OMeTAD with 750 ul of chlorobenzene, 13.5 ul of Li-TFSI solution, 21.75 ul of FK209 solution, and 22.5 ul of 4-tert-butylpyridine to obtain the second solution.
[0077] Example 1
[0078] (1) The FTO conductive glass was ultrasonically cleaned in deionized water, absolute ethanol, acetone and isoacetone in sequence for 15 minutes each, and finally dried with nitrogen, and then the FTO conductive glass was cut into a size of 0.8cmx1cm;
[0079] (2) The FTO conductive glass obtained by cutting was placed in the above-mentioned first solution, soaked at 90°C for 2.5 hours, and then annealed at 180°C for 60 minutes to obtain an electron transport layer disposed on the conductive glass;
[0080] (3) MABr (99.5%), PbBrz (99.99%), Pblz (99.99%), FAI (99.5%) and MACI (99.5%) were dissolved in the mixed solvent and mixed well to obtain a precursor solution with a concentration of 1.53 mol/L. The mass ratio of MABr, PbBr,, Pbl>, FAI and MACI was 7.7: 25.3: 647.4: 241.6: 33. The mixed solvent includes DMF and the first solvent. The volume ratio of the
DMF and the first solvent was 9: 1, and in the first solvent, the volume ratio of N1, N2 and N3 was 3: 4: 3;
[0081] (4) The above precursor solution was spin-coated on the electron transport layer, then annealed at 70°C for 5 min, and then annealed at 150°C for 10 min to obtain an organic-inorganic hybrid perovskite film;
[0082] (5) The second solution was spin-coated on the organic-inorganic hybrid perovskite film to obtain a hole transport layer;
[0083] (6) Ag was deposited on the hole transport layer by vacuum evaporation to obtain a metal electrode layer with a thickness of 90 nm, thereby obtaining a semitransparent solar cell.
[0084] Example 2
[0085] (1) The FTO conductive glass was ultrasonically cleaned in deionized water, absolute ethanol, acetone and isoacetone in sequence for 15 minutes each, and finally dried with nitrogen, and then the FTO conductive glass was cut into a size of 0.8cmx1cm;
[0086] (2) The FTO conductive glass obtained by cutting was placed in the above-mentioned first solution, soaked at 100°C for 2 hours, and then annealed at 185°C for 50 minutes to obtain an electron transport layer disposed on the conductive glass;
[0087] (3) MABr (99.5%), PbBrz (99.99%), Pblz (99.99%), FAI (99.5%) and MACI (99.5%) were dissolved in the mixed solvent and mixed well to obtain a precursor solution with a concentration of 1.5 mol/L. The mass ratio of MABr, PbBr», Pbla, FAI and MACI was 7.5: 26: 648: 242: 33. The mixed solvent includes DMF and the first solvent. The volume ratio of the DMF and 9 the first solvent was 8.9: 1.1, and in the first solvent, the volume ratio of N1, N2 and N3 was 2.8: 4.2: 3;
[0088] (4) The above precursor solution was spin-coated on the electron transport layer, then annealed at 75°C for 4 min, and then annealed at 155°C for 8 min to obtain an organic-inorganic hybrid perovskite film;
[0089] (5) The second solution was spin-coated on the organic-inorganic hybrid perovskite film to obtain a hole transport layer;
[0090] (6) Ag was deposited on the hole transport layer by vacuum evaporation to obtain a metal electrode layer with a thickness of 80 nm, thereby obtaining a semitransparent solar cell.
[0091] Example 3
[0092] (1) The FTO conductive glass was ultrasonically cleaned in deionized water, absolute ethanol, acetone and isoacetone in sequence for 15 minutes each, and finally dried with nitrogen, and then the FTO conductive glass was cut into a size of 0.8cmx1cm;
[0093] (2) The FTO conductive glass obtained by cutting was placed in the above-mentioned first solution, soaked at 80°C for 3 hours, and then annealed at 175°C for 70 minutes to obtain an electron transport layer disposed on the conductive glass;
[0094] (3) MABr (99.5%), PbBrz (99.99%), Pblz (99.99%), FAI (99.5%) and MACI (99.5%) were dissolved in the mixed solvent and mixed well to obtain a precursor solution with a concentration of 1.6 mol/L. The mass ratio of MABr, PbBr», Pbl,, FAI and MACI was 7.8: 25: 647: 241: 33. The mixed solvent includes DMF and the first solvent. The volume ratio of the DMF and the first solvent was 9.1: 0.9, and in the first solvent, the volume ratio of N1, N2 and N3 was 3.2: 4: 3;
[0095] (4) The above precursor solution was spin-coated on the electron transport layer, then annealed at 65°C for 6 min, and then annealed at 145°C for 12 min to obtain an organic-inorganic hybrid perovskite film;
[0096] (5) The second solution was spin-coated on the organic-inorganic hybrid perovskite film to obtain a hole transport layer;
[0097] (6) Ag was deposited on the hole transport layer by vacuum evaporation to obtain a metal electrode layer with a thickness of 100 nm, thereby obtaining a semitransparent solar cell.
[0098] Example 4
[0099] In addition to the step (1): cutting the FTO conductive glass into a size of 0.8cm x
LU502229 lcm, replace it with: use a femtosecond laser engraving template to make the FTO conductive glass into a size of 5cm x 5cm. The remaining steps were the same as in Example 1, and finally a large-area semitransparent solar cell was prepared.
[0100] Comparative Example 1
[0101] The remaining steps were the same as in Example 1, except that the volume ratio of
DMF to the first solvent was modified to 8.5: 1.5.
[0102] Comparative Example 2
[0103] The remaining steps were the same as in Example 1, except that the volume ratio of
DMF to the first solvent was modified to 9.5: 0.5.
[0104] Comparative Example 3
[0105] The remaining steps were the same as in Example 1, except that the volume ratio of
N1, N2 and N3 was modified to 3: 3: 4,
[0106] Comparative Example 4
[0107] The remaining steps were the same as in Example 1, except that the volume ratio of
N1, N2 and N3 was modified to 4: 3: 3.
[0108] (1) X-ray diffraction test
[0109] The organic-inorganic hybrid perovskite films prepared in step (4) in Example 1 and
Comparative Examples 1-4 were subjected to X-ray diffraction to obtain the XRD images shown inFIG. 1.
[0110] It can be seen from FIG. 1 that the organic-inorganic hybrid perovskite films were successfully prepared in both Example 1 and Comparative Examples 1-4.
[0111] (2) Electron microscope observation
[0112] The organic-inorganic hybrid perovskite films prepared in step (4) in Example 1 and
Comparative Examples 1-4 were observed under an electron microscope, and the results are shown in FIG. 2.
[0113] It can be seen from FIG. 2 that the nucleation of the perovskite film prepared in
Example 1 is very dense and uniform, while the perovskite films prepared in Comparative
Examples 1-4 have obvious pores. It is indicated that by optimizing the parameters in the mixed solvent, the prepared perovskite film has better morphology, higher crystallinity and lower defect density.
[0114] (3) Performance test
[0115] The photovoltaic characteristics of the solar cell prepared in Example 1 were tested,
and the results are shown in FIG. 3. The 5cmx5cm large-area perovskite solar cell prepared in
LU502229
Example 4 was tested, and its spectrum was shown in FIG. 4, and its photovoltaic characteristics were shown in FIG. 5. It can be seen from FIG. 3 that the circuit voltage (Voc) of the small-area semitransparent solar cell prepared in Example 1 is 1.015V, the short-circuit current density (Jsc) reaches 23.99 mA/cm?, the fill factor (FF) reaches 0.772%, the photoelectric conversion efficiency of the solar cell reaches 18.80%, and the hysteresis is very small.
[0116] It can be seen from FIG. 4 that the nucleation quality of the organic-inorganic hybrid perovskite film prepared in step (4) in Example 4 is good, dense and uniform. It should be noted that FIG. 4 shows four organic-inorganic hybrid perovskite films prepared in the same batch. It can be seen from FIG. 5 that the circuit voltage (Voc) of the large-area semitransparent solar cell prepared in Example 4 is 5.248V, the short-circuit current density (Jsc) reaches 3.81mA/cm?, the fill factor (FF) reaches 0.61%, the photoelectric conversion efficiency of the prepared solar cell reaches 12.2%, the difference between the forward and reverse scanning efficiency is small, and there is no obvious hysteresis.
[0117] The perovskite films and solar cells prepared in Examples 2 and 3 were subjected to the same detection and analysis as in Example 1 above. It is determined that step (4) produced an organic-inorganic hybrid perovskite film, and finally a semi-transparent solar cell was produced. The perovskite films have good morphology, high crystallinity, and low defect density, and the photovoltaic properties of semitransparent solar cells are good.
[0118] The above are some embodiments of the present disclosure, and are not intended to limit the scope of the present disclosure. For those skilled in the art, the present disclosure may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present disclosure shall be included in the scope of the present disclosure.
Claims (10)
1. A method for preparing an organic-inorganic hybrid perovskite film, comprising following steps: dissolving and mixing methyl ammonium bromide, lead bromide, lead iodide, formamidine hydroiodide and chloromethylamine in a mixed solvent to obtain a precursor solution; and coating the precursor solution on a substrate, annealing at 65°C-75°C for 4 min-6 min, and then annealing at 145°C-155°C for 8 min-12 min to obtain the organic-inorganic hybrid perovskite film; wherein the mixed solvent comprises DMF and a first solvent, a volume ratio of the DMF to the first solvent is 8.9-9.1: 0.9-1.1, and the first solvent comprises N-ethyl-2-pyrrolidone, N-methyl-2-piperidone and N-N-2-methylacetamide.
2. The method for preparing the organic-inorganic hybrid perovskite film of claim 1, wherein the volume ratio of the DMF to the first solvent is 9: 1; and/or a concentration of the precursor solution is 1.5 mol/L -1.6 mol/L.
3. The method for preparing the organic-inorganic hybrid perovskite film of claim 1, wherein in the first solvent, a volume ratio of N-ethyl-2-pyrrolidone, N-methyl-2-piperidone and N-N-2-methylacetamide is 2.8-3.2: 3.8-4.2: 3.
4. The method for preparing the organic-inorganic hybrid perovskite film of claim 3, wherein in the first solvent, the volume ratio of N-ethyl-2-pyrrolidone, N-methyl-2-piperidone and N-N-2-methylacetamide is 3: 4: 3.
5. The method for preparing the organic-inorganic hybrid perovskite film of claim 1, wherein a mass ratio of the methyl ammonium bromide, lead bromide, lead iodide, formamidine hydroiodide and chloromethylamine is 7.5-7.8: 25-26: 647-648: 241-242: 33.
6. The method for preparing the organic-inorganic hybrid perovskite film of claim 5, wherein the mass ratio of the methyl ammonium bromide, lead bromide, lead iodide, formamidine hydroiodide and chloromethylamine is 7.7: 25.3: 647.4: 241.6: 33. 13
7. A method for preparing a semitransparent solar cell, comprising following steps: LU502229 providing a conductive glass; disposing an electron transport layer on the conductive glass; disposing an organic-inorganic hybrid perovskite film on the electron transport layer, wherein the organic-inorganic hybrid perovskite film is prepared by the method for preparing the organic-inorganic hybrid perovskite film according to any one of claims 1 to 6; disposing a hole transport layer on the organic-inorganic hybrid perovskite film; and disposing a metal electrode layer on the hole transport layer to obtain the semitransparent solar cell.
8. The method for preparing the semitransparent solar cell of claim 7, wherein the step of disposing the electron transport layer on the conductive glass comprises: mixing urea, hydrochloric acid, thioglycolic acid, stannous chloride dihydrate and deionized water to obtain a first solution; and placing the conductive glass in the first solution, soaking at 80°C-100°C for 2 hours-3 hours, and annealing at 175°C-185°C for 50 minutes-70 minutes to obtain the electron transport layer disposed on the conductive glass.
9. The method for preparing the semitransparent solar cell of claim 7, wherein the step of disposing the hole transport layer on the organic-inorganic hybrid perovskite film comprises: mixing Spiro-OMeTAD, chlorobenzene, Li-TFSI solution, cobalt salt solution and 4-tert-butylpyridine to obtain a second solution; and coating the second solution on the organic-inorganic hybrid perovskite film to obtain the hole transport layer.
10. The method for preparing the semitransparent solar cell of claim 7, wherein the step of disposing the metal electrode layer on the hole transport layer comprises: depositing Ag on the hole transport layer by vacuum evaporation to obtain the metal electrode layer. 14
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