CN112133831B - Preparation method and application of photovoltaic device based on tin dioxide transmission layer - Google Patents
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Abstract
The invention discloses a preparation method and application of a photovoltaic device based on a tin dioxide transmission layer. The method comprises the following steps: (1) preparing a modified tin dioxide transmission layer; (2) preparing a perovskite light absorption layer film; (3) preparing a hole transport layer; (4) and preparing a top electrode. The preparation method provided by the invention has the advantages of simple process, good uniformity, good repeatability, easily available raw materials, low cost and contribution to reducing the preparation cost. The hydrogen peroxide modified tin dioxide electron transport layer prepared by the invention can effectively improve the electrical property of tin dioxide, so that the tin dioxide has a more appropriate energy band structure and less defect state density. The modified tin dioxide transmission layer film is used for preparing the solar cell, the performance of the solar cell can be effectively improved, the conversion efficiency is as high as 22.15%, the uniformity and the repeatability are better, the manufacturing capacity is improved, and the production cost is reduced. The invention has positive promotion effect on the industrial development of the solar cell and has larger application potential.
Description
Technical Field
The invention belongs to the field of photoelectron materials and devices, and particularly relates to a preparation method of a hydrogen peroxide modified electron transport layer and application of a photovoltaic device thereof.
Background
Organic-inorganic hybrid perovskite solar cells have high photoelectric conversion efficiency and low material preparation cost, so that unprecedented huge research enthusiasm is caused at home and abroad, and a plurality of research results are obtained. The perovskite light absorption material has high carrier mobility, adjustable band gap, solution preparation and high absorption coefficient, so that the perovskite battery can obtain high short circuit battery, open circuit voltage and filling factor. Planar perovskite solar cells based on tin dioxide electron transport layers have also made great progress, but there is room for improvement in performance, including photoelectric conversion efficiency, uniformity, and repeatability.
The original tin dioxide film surface has more defect states such as oxygen vacancies and other types of defects. These defects can severely compromise the performance and stability of the perovskite solar cell. Therefore, the improvement of the electrical property of the tin dioxide has important significance for obtaining photovoltaic devices which have high efficiency and good repeatability and can be used for planar perovskite solar cells. There is a need to develop a tin dioxide thin film transport layer based photovoltaic device with superior overall performance.
Disclosure of Invention
Aiming at the problems of imperfect electrical property and multiple defect states of the existing stannic oxide electron transport layer, the invention provides a preparation method and application of a photovoltaic device based on a hydrogen peroxide modified stannic oxide electron transport layer. According to the invention, the cheap and green oxidizing material hydrogen peroxide is directly added into the tin dioxide precursor solution, the electrical property of tin dioxide can be improved through spin coating and annealing processes, and the defect state density of the surface of the film is effectively reduced. Besides the modification effect on the electrical property of the tin dioxide, the hydrogen peroxide also improves the photoelectric conversion efficiency, uniformity and repeatability of the tin dioxide-based photovoltaic device, and is beneficial to further commercial production and application.
The invention proves that hydrogen peroxide is used as an additive and is used as a passivating agent in metal oxide tin dioxide for the first time, the defect state density of an electron transmission layer is effectively reduced, the oxygen atom proportion of crystal lattices is improved, the charge transmission and extraction capacity of the tin dioxide electron transmission layer is effectively improved, and the photoelectric conversion efficiency, uniformity and repeatability of the perovskite solar cell prepared by using the perovskite solar cell can be effectively improved.
The technical scheme provided by the invention is as follows:
a preparation method of a photovoltaic device based on a tin dioxide transmission layer comprises the following steps:
(1) preparing a tin dioxide transmission layer;
(1.1) mixing the tin dioxide colloidal solution, deionized water and hydrogen peroxide, and stirring to obtain a hydrogen peroxide modified tin dioxide precursor solution;
(1.2) spin-coating a hydrogen peroxide modified tin dioxide precursor solution on an ITO glass substrate, and annealing to obtain a tin dioxide transmission layer;
(2) preparing a perovskite light absorption layer film;
(2.1) adding PbI2Dissolving in an organic solvent;
(2.2) dissolving the ammonium salt in isopropanol;
(2.3) adding PbI2Solution spin-coating on tin dioxide transmission layer, annealing to room temperature, and then in PbI2The upper layer is coated with ammonium salt solution in a spinning mode, and then the perovskite light absorption layer thin film is obtained through annealing in the atmospheric environment;
(3) preparing a hole transport layer;
(3.1) dissolving lithium bistrifluoromethylenesulfonamide in acetonitrile;
(3.2) dissolving 2,2',7,7' -tetra [ N, N-di (4-methoxyphenyl) amino ] -9,9' -spirobifluorene in chlorobenzene, adding 4-tert-butylpyridine and an acetonitrile solution of lithium bistrifluoromethylsulfonimide, and heating and stirring for reaction to obtain a hole transport layer solution; preferably, the heating temperature is 40 ℃, and the stirring time is 24 h;
(3.3) spin-coating the hole transport layer solution on the perovskite light absorption layer film to obtain a hole transport layer; preferably, the spin-coating speed is 3000rpm, and the spin-coating time is 20 s;
(4) preparing a top electrode;
and evaporating a top electrode on the hole transport layer.
Further, the tin dioxide precursor solution in the step 1.1 is obtained by stirring at room temperature for 24 hours. Preferably, the volume ratio of the tin dioxide solution to the deionized water to the hydrogen peroxide is 1:3: 1.
Further, in the step 1.2, the spin coating speed is 6000rpm, and the spin coating time is 30 s; the annealing temperature is 150 ℃, and the annealing time is 30 min.
Further, in the step 2.1, the organic solvent is a mixed solvent of DMF and DMSO, and the volume ratio of the DMF to the DMSO is 19: 1; the dissolving temperature is 60 ℃, and the stirring time is 24 h.
Further, PbI in the step 2.32The annealing temperature of the solution is 70 ℃; ammonium salt bagIncluding FAI, MACl, and MABr; the humidity of the atmospheric environment is about 35 percent during annealing, the annealing temperature is 150 ℃, and the annealing time is 12 min. Preferably, the mass ratio of FAI, MACl and MABr is 60:6: 6.
Further, the ratio of the amount of 2,2',7,7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene, chlorobenzene, 4-tert-butylpyridine and lithium bistrifluoromethylenesulfonamide in acetonitrile in the step 3.2 is 72.3mg:1ml: 28.8. mu.L: 17.5. mu.L; the ratio of lithium bistrifluoromethylenesulfonate imide to acetonitrile in the lithium bistrifluoromethylenesulfonate acetonitrile solution is 520mg:1 ml.
Further, in the step 4, the top electrode to be deposited is a gold electrode.
In the preparation process, except that the hydrogen peroxide modified tin dioxide electron transport layer is carried out under the open air condition, the other layers including the perovskite, the hole transport layer and the top electrode are carried out under the inert gas protection atmosphere. In addition, after the hole transport layer is prepared, it needs to be placed in a drying cabinet for oxidation for 48h before the top electrode is prepared.
The invention also aims to provide a photovoltaic device prepared by the method, and the photovoltaic device comprises an ITO glass substrate, a tin dioxide transmission layer, a perovskite light absorption layer thin film, a hole transmission layer and a top electrode layer from bottom to top. Preferably, the thickness of the tin dioxide transmission layer is 30nm, the thickness of the perovskite light absorption layer film is 700nm, the thickness of the hole transmission layer is 80nm, and the thickness of the top electrode layer is 80 nm.
Further, the perovskite light absorption layer film is organic-inorganic hybrid perovskite (FAPBI)3)0.97(MAPbBr3)0.03。
The invention also provides application of the photovoltaic device in a solar cell.
The invention has the beneficial effects that:
1. the preparation method provided by the invention is simple, good in repeatability, improved in uniformity, low in preparation temperature, easily available in raw materials, low in cost and beneficial to reduction of preparation cost;
2. compared with the unmodified situation, the hydrogen peroxide modified tin dioxide electron transport layer prepared by the invention has less defect state density, a more matched energy band structure, and the characteristics of good substrate coverage, good stability, better repeatability and the like; moreover, the hydrogen peroxide is a green and environment-friendly oxidant, so that the environment pollution is avoided, and the environment is protected;
3. the photovoltaic device based on the hydrogen peroxide modified tin dioxide electron transport layer effectively improves the photoelectric conversion efficiency of the perovskite solar cell to 22.15%, mainly reflects the improvement of filling factors and open-circuit voltage, and has great application development potential.
Drawings
FIG. 1 is a device structure diagram of a planar perovskite thin film solar cell, wherein a 1-ITO, 2-tin dioxide transport layer, a 3-perovskite light absorption layer thin film, a 4-hole transport layer, a Spiro-OMeTAD, and a 5-top electrode;
FIG. 2 is a statistical plot of the performance of the perovskite thin film solar cell prepared in example 1;
FIG. 3 is a statistical plot of the performance of the perovskite thin film solar cell prepared in example 2;
FIG. 4 is a statistical plot of the performance of the perovskite thin film solar cell prepared in example 3;
fig. 5 is a statistical graph of the performance of the perovskite thin film solar cell prepared in comparative example 1.
Detailed Description
The invention is further described with reference to the following examples, which are intended to be illustrative of the invention and are not intended to be limiting. The invention is not limited to the specific examples and embodiments described herein. It will be apparent to those skilled in the art that further modifications and improvements may be made without departing from the spirit and scope of the invention, and these are intended to be covered by the appended claims.
In the following examples, tin dioxide colloidal solution was purchased from Alfa Aesar and hydrogen peroxide concentration was 30 wt% and purchased from national reagents.
Example 1
In this embodiment, a schematic structural diagram of a photovoltaic device based on a tin dioxide electron transport layer is shown in fig. 1, and a tin dioxide electron transport layer modified by hydrogen peroxide, a perovskite light absorption layer, a hole transport layer and a top electrode are sequentially formed from bottom to top by using conductive glass ITO as a substrate, and the specific preparation method is as follows:
1. cleaning: in the test, the ITO conductive glass substrate is cleaned and dried. And cleaning the conductive glass with proper size by using a cleaning agent, and then washing by using deionized water. Then the substrate is placed in an ultrasonic cleaner to be cleaned by acetone, ethanol and deionized water in turn, and finally the substrate with clean surface required by the experiment can be obtained by drying the substrate by nitrogen.
2. Preparing a tin dioxide transmission layer: mixing tin dioxide colloidal solution, deionized water and hydrogen peroxide in a proportion of 1: 3.5: preparing a precursor solution in a ratio of 0.5; then stirring for 24 hours at room temperature to obtain a hydrogen peroxide modified tin dioxide precursor solution; and spin-coating the hydrogen peroxide modified tin dioxide precursor solution on an ITO glass substrate at the rotating speed of 6000rpm for 30s, and then placing the ITO glass substrate on a hot bench at the temperature of 150 ℃ for annealing for 30 min. Thus obtaining the tin dioxide film modified by hydrogen peroxide, wherein the film is used as an electron transport layer. The thickness of the electron transport layer is about 30 nm.
3. Preparing a perovskite light absorption layer: will PbI2Dissolving the mixture in a composite solvent with a volume ratio of DMF to DMSO of 19:1 according to a molar concentration of 1.3M, and stirring the mixture for 24 hours at a temperature of 60 ℃, wherein DMF and DMSO respectively represent N, N-dimethylformamide and dimethyl sulfoxide; the ammonium salt was dissolved in 1ml of isopropanol at a certain mass ratio (FAI: MACl: MABr ═ 60:6:6), and stirred at room temperature for 24 hours. Uniformly spin-coating the prepared precursor lead iodide solution on the electron transport layer by using a spin coater; then annealed at 70 ℃ for 1 min. After the lead iodide is cooled to room temperature, the prepared ammonium salt solution is spin-coated on the lead iodide, and then the annealing is carried out for 12min at 150 ℃ in an atmospheric environment with the humidity of about 35%. The component can be obtained as (FAPBI)3)0.97(MAPbBr3)0.03Perovskite light absorption layer film. The thickness of the perovskite light absorbing layer is about 700 nm.
4. Preparing a hole transport layer: 2,2',7,7' -tetra [ N, N-di (4-methoxyphenyl) amino ] -9,9' -spirobifluorene (Spiro-OMeTAD) is prepared on the perovskite light absorption layer film to be used as a hole transport layer, and the preparation method comprises the following steps: 520mg of lithium bistrifluoromethylsulfonimide (Li-TFSI) are initially dissolved in 1ml of acetonitrile and stirred for 3min, then 72.3mg of 2,2',7,7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino ] -9,9' -spirobifluorene (Spiro-OMeTAD) are dissolved in 1ml of chlorobenzene, 28.8. mu.L of 4-tert-butylpyridine (TBP) and 17.5. mu.L of a solution of Li-TFSI in acetonitrile are added and stirred for 24h at 40 ℃. And spin-coating the prepared solution on the perovskite thin film, wherein the spin-coating speed is 3000rpm, and the spin-coating time is 20 s. The resulting film is a hole transport layer. The hole transport layer thickness is about 80 nm;
5. preparing a top electrode: evaporating an Au electrode on the hole transport layer to be used as a top electrode, wherein the thickness of the top electrode is about 80nm, and thus the photovoltaic device based on the stannic oxide electron transport layer can be obtained;
6. and (3) testing: in AM1.5, the active layer has an effective area of 0.05cm2The battery was tested under the conditions of (1). The obtained statistical graph of the photoelectric conversion efficiency parameters is shown in fig. 2. The statistical distribution of efficiency based on the three batches of 17 devices ranged from 20.78 ± 0.53.
Example 2
The preparation method comprises the following steps:
1. cleaning: as in example 1.
2. Preparing an electron transport layer: mixing a tin dioxide colloidal solution, deionized water and 30% hydrogen peroxide according to a volume ratio of 1:3:1, preparing a precursor solution; then stirring for 24 hours at room temperature to obtain a hydrogen peroxide modified tin dioxide precursor solution; and spin-coating the hydrogen peroxide modified tin dioxide precursor solution on an ITO glass substrate at the rotating speed of 6000rpm for 30s, and then placing the ITO glass substrate on a hot bench at the temperature of 150 ℃ for annealing for 30 min. Thus obtaining the tin dioxide film modified by hydrogen peroxide, wherein the film is used as an electron transport layer. The thickness of the electron transport layer is about 30 nm.
3. Preparing a perovskite light absorption layer: as in example 1.
4. Preparing a hole transport layer: as in example 1.
5. Preparing a top electrode: as in example 1.
6. And (3) testing: in AM1.5, activityThe effective area of the layer is 0.05cm2The battery was tested under the conditions of (1). The obtained statistical graph of the photoelectric conversion efficiency parameters is shown in fig. 3. The statistical distribution of efficiency for 34 devices based on five lots ranged 21.78 ± 0.37. With a smaller standard deviation relative to comparative example 1.
Example 3
The preparation method comprises the following steps:
1. cleaning: as in example 1.
2. Preparing an electron transport layer: mixing a tin dioxide colloidal solution, deionized water and 30% hydrogen peroxide according to a volume ratio of 1: 2: 2, preparing a precursor solution; then stirring for 24 hours at room temperature to obtain a hydrogen peroxide modified tin dioxide precursor solution; and spin-coating the hydrogen peroxide modified tin dioxide precursor solution on an ITO glass substrate at the rotating speed of 6000rpm for 30s, and then placing the substrate on a hot bench at 150 ℃ in air for annealing for 30 min. Thus obtaining the tin dioxide film modified by hydrogen peroxide, wherein the film is used as an electron transport layer. The thickness of the electron transport layer is about 30 nm.
3. Preparing a perovskite light absorption layer: as in example 1.
4. Preparing a hole transport layer: as in example 1.
5. Preparing a top electrode: as in example 1.
6. And (3) testing: in AM1.5, the active layer has an effective area of 0.05cm2The battery was tested under the conditions of (1). The obtained statistical graph of the photoelectric conversion efficiency parameters is shown in fig. 4. The statistical distribution of efficiency based on the three batches of 15 devices ranged from 21.25 ± 0.6.
Comparative example 1
The preparation method comprises the following steps:
1. cleaning: as in example 1.
2. Preparing an electron transport layer: mixing a tin dioxide colloidal solution, deionized water and 30% hydrogen peroxide according to a volume ratio of 1: 4: preparing a precursor solution according to the proportion of 0; then stirring for 24 hours at room temperature to obtain a tin dioxide precursor solution; and spin-coating the tin dioxide precursor solution on an ITO glass substrate at the rotating speed of 6000rpm for 30s, and then placing the substrate on a hot bench at 150 ℃ in air for annealing for 30 min. Thus obtaining the tin dioxide film which is used as an electron transmission layer. The thickness of the electron transport layer is about 30 nm.
3. Preparing a perovskite light absorption layer: as in example 1.
4. Preparing a hole transport layer: as in example 1.
5. Preparing a top electrode: as in example 1.
6. And (3) testing: in AM1.5, the active layer has an effective area of 0.05cm2The battery was tested under the conditions of (1). The obtained statistical graph of the photoelectric conversion efficiency parameters is shown in fig. 5. The statistical distribution of efficiency based on a total of 33 devices from five batches ranged 19.65 ± 1.5. With a larger standard deviation.
The preparation method provided by the invention has simple process, can effectively improve the photoelectric conversion efficiency (up to two percentage points), uniformity and repeatability of the device, and reduces the manufacturing time and cost. The photovoltaic device prepared by the invention has good effect when being applied to the perovskite photovoltaic cell and has larger application potential.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention.
Claims (9)
1. A preparation method of a photovoltaic device based on a tin dioxide transmission layer is characterized by comprising the following steps:
(1) preparing a tin dioxide transmission layer;
(1.1) mixing the tin dioxide colloidal solution, deionized water and hydrogen peroxide, and stirring at room temperature for 24 hours to obtain a hydrogen peroxide modified tin dioxide precursor solution;
(1.2) spin-coating a tin dioxide precursor solution modified by hydrogen peroxide on an ITO glass substrate, and annealing at 150 ℃ for 30min to obtain a tin dioxide transmission layer;
(2) preparing a perovskite light absorption layer film;
(2.1)will PbI2Dissolving in an organic solvent;
(2.2) dissolving the ammonium salt in isopropanol;
(2.3) adding PbI2Solution spin-coating on tin dioxide transmission layer, annealing to room temperature, and then in PbI2The upper layer is coated with ammonium salt solution in a spinning mode, and then the perovskite light absorption layer thin film is obtained through annealing;
(3) preparing a hole transport layer;
(3.1) dissolving lithium bistrifluoromethylenesulfonamide in acetonitrile;
(3.2) dissolving 2,2',7,7' -tetra [ N, N-di (4-methoxyphenyl) amino ] -9,9' -spirobifluorene in chlorobenzene, adding 4-tert-butylpyridine and an acetonitrile solution of lithium bistrifluoromethylsulfonimide, and heating and stirring for reaction to obtain a hole transport layer solution;
(3.3) spin-coating the hole transport layer solution on the perovskite light absorption layer film to obtain a hole transport layer;
(4) preparing a top electrode;
and evaporating a top electrode on the hole transport layer.
2. The method of claim 1, wherein: in the step 1.2, the spin coating speed is 6000rpm, and the spin coating time is 30 s.
3. The method of claim 1, wherein: in the step 2.1, the organic solvent is a mixed solvent of DMF and DMSO, and the volume ratio of the DMF to the DMSO is 19: 1; the dissolving temperature is 60 ℃, and the stirring time is 24 h.
4. The method of claim 1, wherein: PbI in the step 2.32The annealing temperature of the solution is 70 ℃; the ammonium salts include FAI, MACl and MABr; and annealing the spin-coated film in an atmospheric environment with the humidity of 35%, wherein the annealing temperature is 150 ℃, and the annealing time is 12 min.
5. The method of claim 1, wherein: the dosage ratio of the acetonitrile solution of the 2,2',7,7' -tetra [ N, N-di (4-methoxyphenyl) amino ] -9,9' -spirobifluorene, the chlorobenzene, the 4-tert-butylpyridine and the lithium bistrifluoromethylenesulfonamide in the step 3.2 is 72.3mg:1ml:28.8 muL: 17.5 muL; the ratio of lithium bistrifluoromethylenesulfonate imide to acetonitrile in the lithium bistrifluoromethylenesulfonate acetonitrile solution is 520mg:1 ml.
6. The method of claim 1, wherein: in the step 4, the evaporated top electrode is a gold electrode.
7. A photovoltaic device based on a tin dioxide transmission layer is characterized in that: prepared by the method of any one of claims 1 to 6, comprising, from bottom to top, an ITO glass substrate, a tin dioxide transport layer, a perovskite light absorbing layer thin film, a hole transport layer and a top electrode layer.
8. The photovoltaic device of claim 7, wherein: the perovskite light absorption layer film is organic-inorganic hybrid perovskite (FAPbI)3)0.97(MAPbBr3)0.03。
9. Use of the photovoltaic device of claim 7 in a solar cell.
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| CN202010967596.8A CN112133831B (en) | 2020-09-15 | 2020-09-15 | Preparation method and application of photovoltaic device based on tin dioxide transmission layer |
| PCT/CN2021/073526 WO2022057186A1 (en) | 2020-09-15 | 2021-01-25 | Preparation method for photovoltaic device based on stannic oxide transport layer, and use thereof |
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| CN103787405A (en) * | 2014-02-27 | 2014-05-14 | 东华大学 | Preparation method of rutile-phase tin dioxide sol |
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| CN111628080A (en) * | 2019-02-28 | 2020-09-04 | 北京宏泰创新科技有限公司 | Perovskite solar cell and preparation method of perovskite absorption layer |
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| CN103787405A (en) * | 2014-02-27 | 2014-05-14 | 东华大学 | Preparation method of rutile-phase tin dioxide sol |
| CN109148690A (en) * | 2018-08-27 | 2019-01-04 | 领旺（上海）光伏科技有限公司 | A kind of surface treatment method of organic inorganic hybridization perovskite thin film |
| CN111628080A (en) * | 2019-02-28 | 2020-09-04 | 北京宏泰创新科技有限公司 | Perovskite solar cell and preparation method of perovskite absorption layer |
| CN109860403A (en) * | 2019-04-10 | 2019-06-07 | 西南石油大学 | Obtain post-processing method and its application of big crystal grain high quality perovskite thin film |
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