CN117529203A - Perovskite precursor solution, perovskite solar cell and preparation method of perovskite solar cell - Google Patents
Perovskite precursor solution, perovskite solar cell and preparation method of perovskite solar cell Download PDFInfo
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Abstract
本发明公开了一种包括离子液体和非质子极性溶剂的钙钛矿前驱溶液，其特征在于，具体组成包括：作为溶剂的离子液体和非质子极性溶剂的混合物，所述离子液体的阳离子为二甲胺阳离子、阴离子为甲酸阴离子，所述的非质子极性溶剂为N,N‑二甲基甲酰胺和/或二甲基亚砜；以及均匀分散于所述溶剂中的溶质。本发明技术方案通过优化钙钛矿前驱体溶液配方、在前驱体中加入一定量抗氧化和促进结晶的添加剂，有效避免了钙钛矿薄膜结晶时空气中水、氧对液‑固转变过程的破坏，从而实现在空气中制备出高质量钙钛矿薄膜和低成本的钙钛矿器件，能实现钙钛矿电池大规模工业化生产及应用。
The invention discloses a perovskite precursor solution including an ionic liquid and an aprotic polar solvent. It is characterized in that the specific composition includes: a mixture of an ionic liquid as a solvent and an aprotic polar solvent, and the cation of the ionic liquid is dimethylamine cation, the anion is formic acid anion, the aprotic polar solvent is N,N-dimethylformamide and/or dimethyl sulfoxide; and the solute is evenly dispersed in the solvent. The technical solution of the present invention effectively avoids the impact of water and oxygen in the air on the liquid-solid transition process during the crystallization of the perovskite film by optimizing the perovskite precursor solution formula and adding a certain amount of antioxidant and crystallization-promoting additives to the precursor. Destruction, thereby achieving the preparation of high-quality perovskite films and low-cost perovskite devices in the air, enabling large-scale industrial production and application of perovskite batteries.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a perovskite precursor solution, a perovskite solar cell and a preparation method of the perovskite solar cell.
Background
A solar cell is a photovoltaic device capable of converting solar energy into electrical energy. Solar energy is one of the more and more important energy supply forms because of the advantages of self-cleaning, safety, wide distribution, recycling and the like. In recent years, the metal halide perovskite semiconductor material has the advantages of strong light absorption capability, low defect state density, high carrier mobility, long service life and the like, and is very suitable for being applied to the field of photovoltaic power generation, so that the metal halide perovskite semiconductor material is widely focused by people. At present, the organic-inorganic hybrid perovskite solar cell has achieved a conversion efficiency of more than 25.7%. However, perovskite materials are very sensitive to water vapor and oxygen, and particularly when perovskite films are prepared by a solution method, when a precursor in a solution state is converted into a crystalline film, the precursor is more easily damaged by water and oxygen in the air to generate side reactions, so that the material is decomposed and fails. Therefore, most perovskite material photoelectric devices are prepared in an inert gas atmosphere with very low water and oxygen content, such as a glove box, and the limitation greatly increases the cost and prevents large-scale commercialization. Meanwhile, due to the influence of water and oxygen in the air, the performance of the perovskite solar cell is continuously reduced, and the stability is still to be improved. Therefore, it is important to develop a method for preparing a corresponding device of a high-quality perovskite thin film machine in air, and to improve the stability of the device, and it is also a key technology for promoting the practical application of perovskite solar cells.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide an optimized perovskite precursor solution formulation, which effectively avoids the damage of water and oxygen to the liquid-solid transformation process in the crystallization of a perovskite film by adding a certain amount of antioxidant additives into the precursor, thereby realizing the preparation of a high-quality perovskite film and a low-cost perovskite device in the air, and realizing the large-scale industrial production and application of perovskite batteries.
To achieve the above and other related objects, the present invention provides a perovskite precursor solution comprising an ionic liquid and an aprotic polar solvent, comprising the following specific components:
the ionic liquid is a mixture of ionic liquid serving as a solvent and aprotic polar solvent, wherein cations of the ionic liquid are dimethylamine cations, anions of the ionic liquid are formic acid anions, and the aprotic polar solvent is N, N-dimethylformamide and/or dimethyl sulfoxide; and a solute uniformly dispersed in the solvent.
Further, the mass ratio of the ionic liquid to the aprotic polar solvent is 0.1% -10%.
Further, the cations in the ionic liquid can be expanded into one or any combination of dimethylamine cations, trimethylamine cations, ethylamine cations and ethylenediamine cations, and the anions can be expanded into one or any combination of formic acid anions, acetic acid anions, fluoroacetic acid anions and oxalic acid anions.
Further, the aprotic polar solvent is a mixture of one or a combination of N, N-dimethylformamide and/or dimethyl sulfoxide and/or N-methylpyrrolidone and/or butyrolactone and/or acetonitrile.
Further, the solute is specifically one or more of lead iodide, lead bromide, lead chloride, formamidine iodide, formamidine bromide, formamidine chloride, methylamine iodide, methylamine bromide, methylamine chloride, cesium iodide, cesium bromide, dimethylamine iodide, dimethylamine bromide, guanidine iodide and guanidine bromide.
Further, the molar concentration ratio of the solute to the mixture of ionic liquid and aprotic polar solvent is 0.1M-3M.
The invention also provides a method for preparing the perovskite solar cell by using the precursor solution, which comprises the following specific steps:
1) Uniformly mixing a solute with a mixture of an ionic liquid serving as a solvent and an aprotic polar solvent to obtain a perovskite precursor solution;
2) Preparing a hole transport layer on a clean conductive glass (including but not limited to FTO conductive glass, ITO conductive glass, AZO conductive glass, IZO conductive glass, etc.) substrate;
3) Preparing a hole blocking layer or an electron blocking layer on the layer obtained in the step 2);
4) Depositing a perovskite layer on the layer obtained in the step 3) by using the perovskite precursor solution prepared in the step 1);
5) Preparing an electron transport layer or a hole transport layer on the perovskite layer obtained in the step 4);
4) An electron blocking layer or a hole blocking layer on the layer obtained in step 5);
6) And preparing a back electrode layer on the layer obtained in the step 4).
Further, the hole transport layer is nickel oxide (NiO), molybdenum oxide (MoO) 3 ) Cuprous oxide (Cu) 2 O), copper iodide (CuI), copper phthalocyanine (CuPc), copper thiocyanate (CuSCN), redox graphene, poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine](PTAA), 2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino]-9,9' -spirobifluorene (Spiro-OMeTAD), poly 3, 4-ethylenedioxythiophene, polystyrene sulfonate (PEDOT: PSS), 4-butyl-N, N-diphenylaniline homopolymer (Poly-TPD), 2- (9H-carbazol-9-yl) ethyl]Phosphonic acid (PACz) and derivatives thereof, polyvinylcarbazole (PVK), and the like.
Further, the electron transport layer may be a fullerene (C 60 、C 70 ) Etc. and its derivatives, titanium oxide (TiO) 2 ) Tin oxide (SnO) 2 ) Zinc oxide (ZnO), vanadium oxide (V) 2 O 5 ) Zinc tin oxide (Zn) 2 SnO 4 ) One or more n-type semiconductor materials such as zinc selenide (SnSe).
Further, the electron blocking layer is molybdenum oxide (MoO), molybdenum sulfide (MoS), lithium fluoride (LiF), aluminum oxide (Al) 2 O 3 ) Etc.
Further, the hole blocking layer is Bath Copper (BCP), titanium tetrachloride (TiCl), titanium tetraisopropoxide (Ti (iPO) 4 ) Tin oxide (SnO), and the like.
Further, the method for depositing the perovskite layer is spin coating, knife coating, slot coating, spraying or screen printing.
Further, the step 3) specifically includes: spin-coating the perovskite precursor solution on the prepared substrate at a rotating speed of 5000 rpm for 50s, then annealing the substrate on a 60-80 ℃ hot stage for 2min, immediately transferring the substrate into a 100-150 ℃ hot stage for 30min.
The invention also provides a perovskite solar cell, which comprises a perovskite layer, wherein the perovskite layer is prepared from the perovskite precursor solution, is not limited by the structure of a photovoltaic device, and can be used as an active layer in perovskite solar cells with any structures.
The invention also provides a perovskite photoelectric device, which comprises a perovskite layer, wherein the perovskite layer is prepared from the perovskite precursor solution, is not limited by the structure of the photoelectric device, and can be used as an active layer on a photoelectric detector, a light-emitting diode and a semiconductor laser with any structures.
By adopting the technology, compared with the prior art, the invention has the remarkable advantages that:
1) According to the method, the components are destroyed by moisture and oxygen in the liquid-solid conversion process when the perovskite film is prepared by a solution method by introducing the dimethylamine formic acid plasma liquid into the precursor solution, so that the method has important significance in promoting the practicability of the perovskite battery;
2) Creatively using ionic liquid and polar aprotic solvent as precursor solvent to prepare high-quality perovskite film in air and obtain high-efficiency perovskite solar cell, wherein formic acid can inhibit organic cation in precursor solution from deprotonation, dimethylamine can inhibit halogen ion in precursor solution from being oxidized by oxygen, and the addition of polar aprotic solvent realizes the dissolution of precursor solid powder and the crystallization of subsequent steps.
Drawings
FIG. 1 is an SEM image of the interface of a perovskite solar cell according to the present invention;
FIG. 2 is a grazing incidence XRD pattern for comparative example 1 at different angles;
FIG. 3 is a grazing incidence XRD pattern for example 3 at different angles;
FIG. 4 is a photoluminescence graph of the films prepared in examples 1-3 and comparative example 1;
FIG. 5 is an electroluminescence graph of the films prepared in example 3 and comparative example 1;
FIG. 6 is a graph showing the photoluminescence stability of the perovskite thin film prepared in comparative example 1;
FIG. 7 is a graph showing the photoluminescence stability of the perovskite thin film produced in comparative example 3.
Detailed Description
For a better understanding of the present invention, the present invention will be described in further detail with reference to the following specific examples. These examples are given to illustrate the main reaction and essential features of the present invention, and are not limited to the following examples, which may be further modified according to specific requirements, but are not specified in general.
The invention will be further illustrated by the following description of examples in conjunction with the accompanying examples.
Example 1
The specific preparation process for preparing the perovskite solar cell with the p-i-n structure by using the perovskite precursor solution is as follows:
1) Preparing a lead-based perovskite precursor solution with a band gap of 1.55 eV: the specific composition comprises 0.48mmol of methylamine chloride, 1.6mmol of lead iodide, 0.03mmol of lead bromide, 0.05mmol of cesium iodide and 1.5mmol of formamidine, the mixture is dissolved in 800uL of dimethylformamide and 200uL of dimethyl sulfoxide, and after the mixture is dissolved, 5.4uL of dimethylamine formic acid (the molar content of ionic liquid is 4%) is added, and the mixture is stirred uniformly;
2) Preparing a layer of carbazole derivative Me-4PACz ([ 4- (3, 6-Dimethyl-9H-carbazol-9-yl) butyl ] phosphonic Acid) on the cleaned ITO glass substrate;
3) Depositing a layer of perovskite by a spin-on anti-solvent method in air: spin-coating the perovskite precursor solution on a prepared substrate at a rotating speed of 5000 rpm for 50s, then annealing the substrate on a heat table at 80 ℃ for 2min, immediately transferring the substrate to a heat table at 100 ℃ for annealing for 30min, and obtaining a high-quality perovskite film;
4) Preparing a layer of fullerene (C60) as an electron transport layer by thermal evaporation, wherein the thickness of the fullerene is about 25nm;
5) Use of thermal evaporation at C 60 Growing a layer of Bath Copper (BCP) with the thickness of 5nm;
6) The electrode adopts Ag evaporated by thermal evaporation, and the thickness is 120nm.
Fig. 1 shows an SEM cross-sectional view of a lead-based perovskite solar cell prepared in this example and the corresponding device structure.
Example 2
In example 2, 2.7uL of dimethylamine carboxylic acid (2% molar in ionic liquid) was added to the precursor solution and stirred well. The remaining steps were the same as in example 1.
Example 3
In example 2, 1.35uL of dimethylamine carboxylic acid (1% molar in ionic liquid) was added to the precursor solution and stirred well. The remaining steps were the same as in example 1.
Example 4
In example 4, a lead-tin mixed perovskite precursor having a band gap of 1.28eV was used, and specific compositions were 0.18mmol of methylamine chloride, 1.08mmol of lead iodide, 0.45mmol of methylamine iodide, 0.72mmol of stannous iodide, and 1.35mmol of formamidine were dissolved in a mixed solution of 800uL of dimethylformamide and 200uL of dimethylsulfoxide, and after dissolution, 6.5uL of dimethylamine formic acid (molar content of ionic liquid: 4%) was added. The remaining steps were the same as in example 1.
Example 5
In example 5, 3.2uL of dimethylamine carboxylic acid (2% molar in ionic liquid) was added to the precursor solution and stirred well. The remaining steps were the same as in example 4.
Example 6
In example 6, a wide band gap perovskite precursor having a band gap of 1.65eV was used, and a specific composition was 0.07mmol of methylamine chloride, 0.35mmol of cesium iodide, 0.21mmol of lead bromide, 1.05mmol of formamidine iodide, and 1.19mmol of lead iodide, dissolved in a mixed solution of 800uL of dimethylformamide and 200uL of dimethylsulfoxide, and after dissolution, 5.0uL of dimethylamine formic acid (molar content of ionic liquid: 4%) was added. The preparation procedure was the same as in example 1, and the perovskite preparation method can also be used for stacked photovoltaic devices based on other narrow bandgap active materials.
Example 7
In example 7, 2.5uL of dimethylamine carboxylic acid (2% molar in ionic liquid) was added to the precursor solution and stirred well. The remaining steps were the same as in example 5.
Example 8
In example 8, 1.3uL of dimethylamine carboxylic acid (1% molar in ionic liquid) was added to the precursor solution and stirred well. The remaining steps were the same as in example 5.
Example 9
In example 9, a wide band gap perovskite precursor having a band gap of 1.68eV was used, and a specific composition was 0.07mmol of methylamine chloride, 0.28mmol of cesium iodide, 0.28mmol of lead bromide, 1.12mmol of formamidine iodide, and 1.12mmol of lead iodide, dissolved in a mixed solution of 800uL of dimethylformamide and 200uL of dimethylsulfoxide, and after dissolution, 5.0uL of dimethylamine formic acid (molar content of ionic liquid: 4%) was added. The preparation procedure was the same as in example 1, and the perovskite preparation method can also be used for stacked photovoltaic devices based on other narrow bandgap active materials.
Example 10
In example 10, 2.5uL of dimethylamine carboxylic acid (2% molar in ionic liquid) was added to the precursor solution and stirred well. The remaining steps were the same as in example 9.
Example 11
In example 11, 1.3uL of dimethylamine carboxylic acid (1% molar in ionic liquid) was added to the precursor solution and stirred well. The remaining steps were the same as in example 9.
Comparative example 1
The specific preparation method was the same as in example 1 using lead-based perovskite with a band gap of 1.55eV, using dmf+dmso as solvent, without ionic liquid additives.
Comparative example 2
1) Preparing a lead-based perovskite precursor solution with a band gap of 1.55 eV: the specific composition comprises 0.12mmol of methylamine chloride, 0.4mmol of lead iodide, 0.0075mmol of lead bromide, 0.0125mmol of cesium iodide and 0.375mmol of formamidine, which are dissolved in 1mL of dimethylamine formic acid and stirred uniformly;
2) Preparing a layer of carbazole derivative Me-4PACZ ([ 4- (3, 6-Dimethyl-9H-carbazol-9-yl) butyl ] phosphonic Acid) on the cleaned ITO glass substrate;
3) Depositing a layer of perovskite by a spin-on anti-solvent method in air: spin-coating the perovskite precursor solution on a prepared substrate at a rotating speed of 4000 rpm for 50s, then annealing the substrate on a heat table at 80 ℃ for 2min, immediately transferring the substrate to a heat table at 100 ℃ for annealing for 30min, and obtaining a high-quality perovskite film;
4) Preparing a layer of fullerene (C60) as an electron transport layer by thermal evaporation, wherein the thickness of the fullerene is about 25nm;
5) Use of thermal evaporation at C 60 Growing a layer of Bath Copper (BCP) with the thickness of 5nm;
6) The electrode adopts Ag evaporated by thermal evaporation, and the thickness is 120nm.
Comparative example 3
The specific preparation method was the same as for example 4 using lead-based perovskite with a band gap of 1.28eV, using dmf+dmso as solvent, without ionic liquid additives.
Comparative example 4
The specific preparation method was the same as in example 6 using lead-based perovskite with a band gap of 1.65eV, using dmf+dmso as solvent, without ionic liquid additives.
Comparative example 5
The specific preparation method was the same as in example 9 using lead-based perovskite with a band gap of 1.68eV, using dmf+dmso as solvent, without ionic liquid additives.
The photoelectric conversion performance data of the perovskite solar cell prepared in each of the above examples and comparative examples are listed in table 1.
Example 12
Example 12 compares the grazing incidence diffraction pattern results of the perovskite thin films prepared in example 3 and comparative example 1, i.e., the thin film products obtained in step 3 in example 3 and comparative example 1. The diffraction pattern of the perovskite thin film in example 3 is shown in FIG. 2, and the diffraction pattern of the perovskite thin film in comparative example 1 is shown in FIG. 3. The spin-coated perovskite thin film in air was tested for grazing incidence XRD. Wherein the incident angles are respectively 0.6 degrees, 0.9 degrees, 1.2 degrees and 1.5 degrees, the diffraction angle 2theta is 10-50 degrees, and the X-ray wavelength is 0.154nm. The perovskite thin film of the control group without the ionic liquid showed a large amount of diffraction peaks of lead iodide near 12.6 ° in 2theta, and the incidence angle was increased, the X-ray transmission depth was increased, and the intensity of the diffraction peaks was unchanged. Indicating that the lead iodide is mainly generated at the film-air interface. The perovskite thin film of the experimental group to which the mixture of the ionic liquid and the aprotic polar solvent was added had no discernible diffraction peak of lead iodide and no other visible diffraction peak of impurities. It is explained that the ionic liquid successfully inhibits deprotonation and volatilization of the cationic component, thereby inhibiting point-vacancy defects generated thereby.
Example 13
Example 13 comparative examples 1-3 and comparative example 1 the photoluminescent results of the perovskite thin films produced in examples 1-3 and comparative example 1, i.e., the thin film products obtained in step 3 of examples 1-3 and comparative example 1. The comparison result is shown in FIG. 4. Unlike the substrates in examples 1-3, the films were prepared on cleaned electronic glass substrates. Photoluminescence efficiency measurements were performed in an integrating sphere having a radius of about 120mm, with an excitation light wavelength of 405nm and an excitation light power equivalent of about 10mW/cm 2 . As shown in FIG. 4, the photoluminescence curve peak position of the perovskite thin film prepared after the ionic liquid is added can be blue-shifted by 3-5nm (from 819nm to 815 nm), and the luminous efficiency is obviously enhanced. The photoluminescence efficiency was 2.02% in comparative example 1 containing no ionic liquid, 6.24% in comparative example 3 having a molar content of 1% of ionic liquid, 4.19% in comparative example 2 having a molar content of 2% of ionic liquid, and 2.85% in comparative example 1 having a molar content of 4% of ionic liquid. The ionic liquid additive can effectively improve the photoluminescence efficiency of the prepared perovskite film, and the optimal molar content is present and is optimal to be 1%.
Example 14
Example 14 compares the electroluminescent results of the perovskite devices prepared in example 1 and comparative example 1, namely the thin film products obtained in examples 1 to 3 and step 3 of comparative example 1. The comparison result is shown in FIG. 5. The sample in example 17 is a complete solar cell device, unlike example 16. As shown in FIG. 5, the electroluminescence efficiency of the perovskite solar cell prepared after the ionic liquid is added is obviously higher than that of the device in the control group, which indicates that the device prepared by the experimental group has higher perovskite film quality and lower open voltage loss.
Example 15
Example 15 comparative example 3 and comparative example 1 the photoluminescence stability of the perovskite thin films prepared, i.e. the relationship between the emission peak position and the intensity over time in example 13. The photoluminescence stability measurement results of the sample prepared in comparative example 1 are shown in fig. 6, and the photoluminescence stability measurement results of the sample prepared in example 3 are shown in fig. 7. The preparation method and measurement method in example 15 were the same as in example 13. When measuring the photoluminescence stability, the photoluminescence curves were scanned every 1 minute and recorded. As can be seen from comparing the results of fig. 6 and 7, the perovskite thin film as known in example 3 shows good photoluminescence stability after the ionic liquid is added. The peak position and the intensity of the emitted light are basically kept unchanged within a measurement scale of 30min, and the stability is good. Whereas the intensity of the emission curve of comparative example 1 was rapidly decreased, the peak position was shifted.
Table 1 results of performance comparisons for various examples
As can be seen from table 1, the perovskite solar cell has better photoelectric conversion efficiency and more excellent stability based on the perovskite precursor solution mixing additive strategy of the invention. As can be seen from the results of comparative example 1, the perovskite solar cell prepared by using the ionic liquid as the additive has better photoelectric conversion performance than the perovskite solar cell prepared by using the ionic liquid as the solvent. This demonstrates that a small amount of ionic liquid additive can achieve its physicochemical properties that protect the precursor solution without being fully practical as a solvent. From various comparison results, the ionic liquid additive based on the dimethylamine formic acid is suitable for various perovskite components, has the characteristic of universality from narrow-band gap perovskite to wide-band gap perovskite, is suitable for preparing perovskite films and battery devices in multiple scenes, and ensures excellent battery performance. Meanwhile, the preparation process is simple, the cost is low, and the commercialization requirements can be completely met.
In particular, the invention provides an improvement of the device performance of the dimethylamine formic acid ionic liquid additive, wherein the optimization interval of the content of the additive in the precursor solution exists, and the optimization interval is changed with perovskite components with different band gaps. In particular, for multi-cesium content wide bandgap perovskites with a bandgap greater than 1.65eV, the ionic liquid additive requires a higher addition level of 5%. For a conventional lead-based perovskite having a band gap of about 1.55eV, the ionic liquid optimized additive content is about 1%. For lead-tin mixed perovskites with a band gap of about 1.28eV, device fabrication needs to be performed in a nitrogen glove phase and the optimum additive content is about 2, since the divalent stannous component contained in the precursor is extremely sensitive to oxygen.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention are intended to be included within the scope of the present invention.
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| CN117729822A (en) * | 2024-02-07 | 2024-03-19 | 西安电子科技大学 | Large-area perovskite solar cells based on gas-phase ion doping and preparation methods thereof |
| CN118632551A (en) * | 2024-04-11 | 2024-09-10 | 武汉理工大学 | A composite hole transport layer and its application in perovskite solar cells |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117729822A (en) * | 2024-02-07 | 2024-03-19 | 西安电子科技大学 | Large-area perovskite solar cells based on gas-phase ion doping and preparation methods thereof |
| CN117729822B (en) * | 2024-02-07 | 2024-05-14 | 西安电子科技大学 | Large-area perovskite solar cell based on gas-phase ion doping and preparation method thereof |
| CN118632551A (en) * | 2024-04-11 | 2024-09-10 | 武汉理工大学 | A composite hole transport layer and its application in perovskite solar cells |
| CN118632551B (en) * | 2024-04-11 | 2024-12-10 | 武汉理工大学 | A composite hole transport layer and its application in perovskite solar cells |
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