CN113206201B - Method for optimizing lead-free perovskite solar cell thin film - Google Patents
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Abstract
The invention discloses a method for optimizing a lead-free perovskite solar cell film, which comprises the steps of firstly spin-coating a perovskite precursor solution on a hole transport layer for 50 s when an active layer is prepared, dripping an ether solution doped with chiral mandelic acid when the hole transport layer is spin-coated for 12 s, and then carrying out annealing treatment to obtain the active layer; oxygen ions in hydroxy acid molecules in the mandelic acid have lone-pair electrons, can form coordination bonds with metal ions, slow down and control the crystallization process of the perovskite, and meanwhile, as the mandelic acid is a reducing agent, oxidation of divalent tin can be inhibited, so that the crystallinity of the perovskite thin film can be improved, the quality of the thin film can be obviously improved through two-phase combination, and the power conversion efficiency of the tin-based perovskite solar cell can be improved; the absorption of the perovskite film can be enhanced by the self circularly polarized light luminescence of the chiral material mandelic acid, so that the power conversion efficiency of the device is effectively improved; and the mandelic acid is mainly extracted from plants, has wide source and is safe to use.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a method for optimizing a lead-free perovskite solar cell film.
Background
With the rapid development of science and technology, the total amount of global fossil energy is reduced day by day, and it is necessary to find green and pollution-free new energy which can replace the traditional energy. Solar energy is a hot spot of people's attention due to the advantages of easy acquisition, abundant storage, cleanness and no pollution, and a solar cell is an important way to utilize solar energy. Among them, the silicon-based solar cell is the most rapidly developed and widely used cell material at present, but the problems of high cost and high energy consumption caused by the necessity of using expensive high-purity silicon in the preparation process severely restrict the wide application of the silicon-based solar cell.
The optical and electrical properties of Pb-based perovskites are almost perfect for solar cells. However, lead-based perovskite solar cells also have two major problems: poor stability and high toxicity. Therefore, it is important to find a non-lead perovskite battery which is non-toxic and has high stability.
Among the non-lead perovskite solar cells, the tin-based perovskite solar cell is the most promising material among various lead-free perovskites due to excellent optical and electrical properties such as high absorption coefficient, small exciton binding energy and high charge carrier mobility. However, in the tin-based perovskite solar cell, since Sn vacancy forming energy is low, Sn 2+ Is very easily oxidized into Sn 4+ And stannous iodide (SnI) which is one of perovskite precursors 2 ) The reaction rate with organic amine salts is too fast, which makes the crystallization rate of perovskite so fast that it is difficult to obtain a uniform and dense crystal thin film, which seriously hinders the improvement of efficiency and stability of solar cells.
Chinese patent CN 111952455A discloses a low-dimensional tin-based perovskite thin film prepared from ionic liquid type organic large-volume amine molecular salt, a solar cell and application thereof, wherein a precursor liquid of the low-dimensional tin-based perovskite is prepared by using special ionic liquid type organic large-volume amine molecular salt butylamine acetate, and the low-dimensional tin-based perovskite thin film is prepared on ITO transparent conductive glass deposited with a hole transport material by using an anti-solvent method 2+ The oxidation is carried out, the preparation of the precursor solution is complicated, the source of the ionic liquid type organic bulky amine molecule salt butylamine acetate is narrow, the use safety needs to be improved, the overall preparation efficiency is influenced, and the large-scale production and application are not facilitated.
Disclosure of Invention
The invention aims to provide a method for optimizing a lead-free perovskite solar cell film, which particularly takes mandelic acid as an additive, ether as an anti-solvent and PEDOT (Poly ethylene glycol ether) PSS (PolyEthyl Ether) as a vacancyHole transport layer, C 60 A tin-based perovskite solar cell is designed for an electron transport layer, the morphology of the film is improved, the crystallinity of the perovskite film is improved, and good power conversion efficiency and stability are obtained.
The technical scheme of the invention is as follows: a method for optimizing a lead-free perovskite solar cell film comprises the steps of firstly, spin-coating a perovskite precursor solution on a hole transport layer for 50 s when an active layer is prepared, dripping an ether solution doped with chiral mandelic acid when the hole transport layer is subjected to spin-coating for 12 s, and then annealing to obtain the active layer; the precursor solution is tin iodide (SnI) 2 ) Formamide (FAI), Methylamine (MAI) and tin fluoride (SnF) 2 ) Formed after dissolving in a mixed solvent of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO).
Further, the concentration of the chiral mandelic acid in the ether solution is 0.01-0.05 mg/mL.
Further, the molar ratio of tin iodide, formamide, methylamine and tin fluoride is 1: 0.75:0.25:0.1.
Further, the spin coating process is performed after being filled with N 2 The spin coating speed in the glove box of (1) was 3500 and 5000 rpm.
Further, the annealing temperature is 65-70 ℃, and the annealing time is 10-15 min.
Further, the volume ratio of N, N-Dimethylformamide (DMF) to dimethyl sulfoxide (DMSO) was 4: 1.
Compared with the prior art, the invention has the following advantages:
1. according to the preparation method, a chiral material mandelic acid is used as an additive when an active layer is prepared, oxygen ions in hydroxy acid molecules in the mandelic acid have lone-pair electrons, and can form coordinate bonds with metal ions, so that the crystallization process in the perovskite formation process is slowed down and controlled, and in addition, the mandelic acid is a reducing agent, so that the oxidation of divalent tin can be inhibited, the crystallinity of the perovskite film can be further improved, the perovskite film with low defect state density and smooth and compact surface can be obtained, the film quality is improved, and the power conversion efficiency of the tin-based perovskite solar cell is improved;
2. the additive mandelic acid used in the preparation of the active layer is a chiral material, and the absorption of the perovskite thin film can be enhanced by circularly polarized light luminescence of the chiral material, so that the power conversion efficiency of the device is effectively improved;
3. the additive mandelic acid used in the preparation of the active layer is alpha-hydroxy acid from almond, is mainly extracted from plants, has wide source, low cost and safe use, and cannot cause secondary pollution in the use process.
Drawings
FIG. 1 is a structural diagram of perovskite solar cell devices prepared in comparative example 1 and examples 1 and 2,
wherein, 1-transparent anode, 2-hole transmission layer, 3-perovskite active layer, 4-electron transmission layer, 5-hole barrier layer, 6-metal cathode;
FIG. 2 is a J-V plot of perovskite solar cell devices prepared in comparative example 1 and examples 1, 2;
FIG. 3 shows an active layer FA prepared in comparative example 1 and examples 1 and 2 0.75 MA 0.25 SnI 3 XRD pattern of the film;
in FIG. 4, three small graphs from left to right are active layers FA prepared in comparative example 1 and examples 1 and 2, respectively 0.75 MA 0.25 SnI 3 SEM image of thin film.
Detailed Description
The technical solution of the present invention is further described below with reference to the accompanying drawings, but not limited thereto, and any modification or equivalent replacement of the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention shall be covered by the protection scope of the present invention.
The structures of the battery devices prepared in comparative example 1 and examples 1 and 2 are shown in fig. 1, and the battery devices respectively comprise a transparent anode, a hole transport layer, a perovskite active layer, an electron transport layer, an electron blocking layer and a metal cathode from bottom to top.
Comparative example 1
1. Preparing a precursor solution: adding tin iodide SnI 2 Formamide FAI and methylamine MAI according to the ratio of 1:0.75:0.25Dissolving in mixed solvent of N, N-dimethylformamide DMF and dimethyl sulfoxide DMSO solution at a molar ratio (DMF and DMSO volume ratio is 4: 1), and adding 10% SnF at a molar ratio 2 Stirring the mixed solution at room temperature for 48 hours to prepare a perovskite precursor solution with the concentration of 1mol/L for later use;
2. and (3) anode treatment: washing the ITO conductive glass sheet with a washing solution, deionized water, acetone and ethanol in sequence twice, putting the ITO substrate into a constant-temperature oven at 80 ℃ for drying for more than half an hour, and performing Plasma treatment for 2 min after drying;
3. preparation of hole transport layer: spin-coating PEDOT (PSS) on the ITO conductive glass processed by the Plasma at the rotation speed of 4000rpm by using a spin coater, wherein the spin-coating time is 60 s, and then annealing the ITO conductive glass in the air at the temperature of 130 ℃ for 20 min to form a hole transport layer;
4. preparation of the perovskite active layer: putting the annealed wafer into a glove box, spin-coating the perovskite precursor solution on a PEDOT (PolyEthyl Ether) PSS layer at the rotation speed of 4000rpm for 50 s, quickly drop-coating ethyl ether when spin-coating for 12 s, and annealing at 70 ℃ for 10 min to form a perovskite active layer;
5. preparation of an electron transport layer: evaporating C on perovskite active layer by using vacuum evaporation equipment 60 ，C 60 The thickness is 20 nm, the evaporation rate is 0.1A/s, and the vapor pressure environment of the evaporation is less than 4 multiplied by 10 -4 Pa；
6. Preparation of a hole blocking layer: using vacuum evaporation equipment at C 60 Evaporating organic micromolecular material BCP to form a hole blocking layer, wherein the thickness of the hole blocking layer is 5.5 nm, the evaporation rate is 0.4A/s, and the air pressure environment of evaporation is less than 4 multiplied by 10 -4 Pa；
7. Preparation of metal cathode: evaporating metal Ag on the hole blocking layer to form a metal cathode layer, wherein the thickness of the metal cathode layer is 100 nm, the evaporation rate is 0.8A/s, and the air pressure environment of evaporation is less than 4 multiplied by 10 -4 Pa；
8. The prepared device is coated with epoxy resin material, irradiated by ultraviolet light for 10 min and packaged.
The J-V curve of the device under room temperature conditions,as shown in FIG. 2, it can be seen that the open circuit voltage of the device is 0.323V and the short circuit current is 13.19 mA cm -2 The fill factor was 0.562 and the efficiency was 2.39%.
Example 1
1. Preparing a precursor solution: dissolving tin iodide, formamide and methylamine in a molar ratio of 1:0.75:0.25 in a mixed solvent of N, N-dimethylformamide DMF and dimethyl sulfoxide DMSO solution (the volume ratio of DMF to DMSO is 4: 1), and adding 10% of SnF in a molar ratio 2 Stirring the mixed solution at room temperature for 48 hours to prepare a perovskite precursor solution with the concentration of 1mol/L for later use;
2. and (3) anode treatment: washing the ITO conductive glass sheet with a washing solution, deionized water, acetone and ethanol in sequence twice, putting the ITO substrate into a constant-temperature oven at 80 ℃ for drying for more than half an hour, and performing Plasma treatment for 2 min after drying;
3. preparation of hole transport layer: PSS (PEDOT: PSS) is spin-coated on the ITO conductive glass processed by the Plasma at the rotating speed of 4000rpm, the spin-coating time is 60 s, and then annealing is carried out for 20 min at the temperature of 130 ℃ in the air to form a hole transport layer;
4. preparation of the perovskite active layer: putting the annealed sheet into a glove box, spin-coating the perovskite precursor solution on a PEDOT (PSS) layer at the rotating speed of 4000rpm for 50 s, quickly dripping ether solution doped with 0.03 mg/mL dextromandelic acid (R- (-) -MA) when spin-coating for 12 s, and annealing at 70 ℃ for 10 min to form a perovskite active layer;
5. preparation of an electron transport layer: evaporating C on the perovskite active layer by using vacuum evaporation equipment 60 ，C 60 The thickness is 20 nm, the evaporation rate is 0.1A/s, and the vapor pressure environment of the evaporation is less than 4 multiplied by 10 -4 Pa；
6. Preparation of a hole blocking layer: using vacuum evaporation equipment at C 60 Evaporating organic micromolecular material BCP to form a hole blocking layer, wherein the thickness of the hole blocking layer is 5.5 nm, the evaporation rate is 0.4A/s, and the air pressure environment of evaporation is less than 4 multiplied by 10 -4 Pa；
7. Preparation of metal cathode: in the cavityMetal Ag is evaporated on the barrier layer to form a metal cathode layer, the thickness of the metal cathode layer is 100 nm, the evaporation rate is 0.8A/s, and the air pressure environment of evaporation is less than 4 multiplied by 10 -4 Pa。
8. The prepared device is coated with epoxy resin material, irradiated by ultraviolet light for 10 min and packaged.
Under room temperature, the J-V curve of the device under test is shown in FIG. 2, from which it can be seen that the open circuit voltage of the device is 0.327V and the short circuit current is 17.9 mA cm -2 The fill factor was 0.626 and the efficiency was 3.67%.
Example 2
1. Preparing a precursor solution: dissolving tin iodide, formamide and methylamine in a molar ratio of 1:0.75:0.25 in a mixed solvent of N, N-dimethylformamide DMF and dimethyl sulfoxide DMSO solution (the volume ratio of DMF to DMSO is 4: 1), and adding 10% of SnF in a molar ratio 2 Stirring the mixed solution at room temperature for 48 hours to prepare a perovskite precursor solution with the concentration of 1mol/L for later use;
2. and (3) anode treatment: washing the ITO conductive glass sheet with a washing solution, deionized water, acetone and ethanol in sequence twice, putting the ITO substrate into a constant-temperature oven at 80 ℃ for drying for more than half an hour, and performing Plasma treatment for 2 min after drying;
3. preparation of hole transport layer: spin-coating PEDOT (PSS) on the ITO conductive glass processed by the Plasma at the rotation speed of 4000rpm by using a spin coater, wherein the spin-coating time is 60 s, and then annealing treatment is carried out for 20 min at the temperature of 130 ℃ in the air to form a hole transport layer;
4. preparing a perovskite active layer: putting the annealed sheet into a glove box, spin-coating the perovskite precursor solution on a PEDOT (PSS) layer at the rotating speed of 4000rpm for 50S, quickly dripping an ether solution doped with 0.03 mg/mL levomandelic acid (S- (+) -MA) when spin-coating is carried out for 12S, and then annealing at 70 ℃ for 10 min to form a perovskite light absorption layer;
5. preparation of an electron transport layer: evaporating C on perovskite light absorption layer by using vacuum evaporation equipment 60 ，C 60 The thickness is 20 nm, the evaporation rate is 0.1A/s, and the air pressure environment for evaporation is smallAt 4X 10 -4 Pa；
6. Preparation of a hole blocking layer: using vacuum evaporation equipment at C 60 Evaporating organic micromolecular material BCP to form a hole blocking layer, wherein the thickness of the hole blocking layer is 5.5 nm, the evaporation rate is 0.4A/s, and the air pressure environment of evaporation is less than 4 multiplied by 10 -4 Pa；
7. Preparation of metal cathode: evaporating metal on the hole blocking layer to form a metal cathode layer, wherein the thickness of the metal cathode layer is 100 nm, the evaporation rate is 0.8A/s, and the vapor pressure environment of evaporation is less than 4 multiplied by 10 -4 Pa；
8. The prepared device is coated with epoxy resin material, irradiated by ultraviolet light for 10 min and packaged.
Under room temperature, the J-V curve of the device under test is shown in FIG. 2, from which it can be seen that the open circuit voltage of the device is 0.316V and the short circuit current is 17.58 mA cm -2 The fill factor was 0.634 and the efficiency was 3.52%.
The SEM images of the perovskite layers prepared in comparative example 1 and examples 1 and 2 are shown in fig. 4, and it can be seen from the SEM images that after adding a chiral material mandelic acid as an additive to an ether antisolvent, grain boundary defects can be significantly reduced, so that the prepared perovskite light absorption layer has high crystallinity and low defect density, a high-quality light absorption layer is obtained, which is beneficial to extraction of electrons, balances transmission of carriers, further improves photoelectric properties of the device, and finally improves conversion efficiency of the perovskite solar cell.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present specification and drawings, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. The method for optimizing the lead-free perovskite solar cell film is characterized in that when an active layer is prepared, a perovskite precursor solution is firstly spin-coated on a hole transport layer for 50 s, an ether solution doped with chiral mandelic acid is dropwise coated when the hole transport layer is spin-coated for 12 s, and then annealing treatment is carried out to obtain the active layer;
the precursor solution is formed by dissolving tin iodide, formamide, methylamine and tin fluoride in a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide;
the concentration of the chiral mandelic acid in the ether solution is 0.01-0.05 mg/mL.
2. The method of optimizing a lead-free perovskite solar cell thin film as claimed in claim 1, wherein the molar ratio of tin iodide, formamide, methylamine and tin fluoride is 1: 0.75:0.25:0.1.
3. The method of optimizing lead-free perovskite solar cell thin film as claimed in claim 1, wherein the spin coating process is performed after being filled with N 2 The spin coating speed in the glove box of (1) was 3500 and 5000 rpm.
4. The method for optimizing a lead-free perovskite solar cell thin film as claimed in claim 1, wherein the annealing temperature is 65-70 ℃ and the annealing time is 10-15 min.
5. The method of optimizing a lead-free perovskite solar cell thin film as claimed in claim 1, wherein the volume ratio of N, N-dimethylformamide to dimethylsulfoxide is 4: 1.
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| CN113707810B (en) * | 2021-09-24 | 2024-05-17 | 嘉兴学院 | PEDOT doped with AuNCs: tin-containing perovskite solar cell with PSS as hole transport layer and preparation method thereof |
| CN115286939B (en) * | 2022-08-01 | 2024-02-23 | 昆山协鑫光电材料有限公司 | Lead-free tin-based halide perovskite film, preparation composition, preparation method and application |
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