CN114284440A - Preparation method and application of difunctional ionic salt passivated tin-based perovskite thin film and perovskite solar cell thereof - Google Patents
Preparation method and application of difunctional ionic salt passivated tin-based perovskite thin film and perovskite solar cell thereof Download PDFInfo
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Abstract
The invention relates to a surface passivation and anti-oxidation dual-function interface treatment method for a tin-based perovskite solar cell, and belongs to the field of photoelectric materials and devices. According to the invention, a tin-based perovskite thin film is prepared by processing an upper interface of a tin-based perovskite by using a special bifunctional ionic salt ethylenediamine formate and preparing the tin-based perovskite thin film on ITO transparent conductive glass deposited with a hole transport material by using an anti-solvent method, and after the upper interface is processed and annealed, the thin film has a flat and compact surface, low defect state density and crystal orientation vertical to a substrate. The prepared tin-based perovskite solar cell has excellent photoelectric conversion efficiency and excellent device stability. N of tin-based perovskite solar cell without encapsulation after interface treatment2Under the atmosphere, the product can still be obtained after about 2000 hoursTin-based perovskite solar cell without interface treatment and without encapsulation, maintaining initial efficiency of about 95%2Only 30% of the initial efficiency was maintained after about 2000 hours under atmosphere.
Description
Technical Field
The invention relates to a surface passivation and anti-oxidation dual-function interface treatment method for a tin-based perovskite solar cell, and belongs to the field of photoelectric materials and devices. According to the invention, a tin-based perovskite thin film is prepared by processing an upper interface of a tin-based perovskite by using a special bifunctional ionic salt ethylenediamine formate and preparing the tin-based perovskite thin film on ITO transparent conductive glass deposited with a hole transport material by using an anti-solvent method, and after the upper interface is processed and annealed, the thin film has a flat and compact surface, low defect state density and crystal orientation vertical to a substrate. The prepared tin-based perovskite solar cell has excellent photoelectric conversion efficiency and excellent device stability.
Background
With the increasing demand for energy from human beings, the traditional fossil energy sources have been unable to meet the present demand of human beings. Solar energy is considered to be one of the clean energy sources which is shifted to gradually replace the traditional fossil energy source as an inexhaustible clean energy source. Solar cells have received much attention from industry personnel as the primary carrier for converting solar energy into electrical energy. At present, solar cells that have been widely commercialized are mainly focused on single crystal silicon and polycrystalline silicon cells. However, a series of problems are involved in the production and processing of crystalline silicon solar cells. Such as large energy consumption and serious environmental pollution. Therefore, under the current green development requirement of sustainable development, further development space is difficult to be provided.
Since 2009, organic-inorganic hybrid perovskite solar cells were produced, the photoelectric conversion efficiency of the organic-inorganic hybrid perovskite solar cells is improved from 3.8% to 25.5% in a short period of decades. Although the photoelectric conversion efficiency of organic-inorganic hybrid perovskite solar cells is rapidly developed, the organic-inorganic hybrid perovskite solar cells also face a plurality of problems in the process of commercial application. First, lead-based perovskite solar cells contain lead elements having high toxicity, and thus it is urgent to find an element having low toxicity capable of replacing the lead elements.
Currently, tin-based perovskite materials are considered to be one of the most promising alternatives to lead-based perovskites due to their lower environmental and biological toxicity, as well as low exciton binding energy and narrow optical band gap. However, since the divalent tin in the tin-based perovskite system is thermodynamically unstable, it is easily oxidized into tetravalent tin. In addition, the crystallization rate is high during the preparation process, so that the surface defects are more. Both of the above-mentioned two major problems are not conducive to the fabrication of high temperature efficient tin-based perovskite solar cells. Therefore, the final energy conversion efficiency and the stability of long-term operation can be effectively improved by introducing a passivation molecular layer with double high energy on the tin-based perovskite interface. After the surface of the tin-based perovskite thin film is treated by using the special bifunctional ionic salt ethylenediamine formate, the surface defects of the tin-based perovskite can be effectively reduced through strong interaction among molecules, so that the tin-based perovskite thin film with low defect state density, smooth and compact surface and highly vertically oriented crystals is obtained. In addition, the bifunctional ionic salt ethylenediamine formate can improve the thermodynamic instability of the stannous, so that the long-term stability of the stannous is improved. Finally, the performance and stability of the tin-based perovskite solar cell prepared by the anti-solvent method are remarkably improved.
Disclosure of Invention
The invention provides a bifunctional ionic salt passivated tin-based perovskite thin film and a preparation method of a perovskite solar cell thereof, which are methods for surface passivation and anti-oxidation bifunctional interface treatment of the tin-based perovskite solar cell and solve the technical problems of more defects on a tin-based perovskite interface and instability of bivalent tin. The method for preparing the tin-based perovskite thin film with flat and compact surface, low defect state density and crystal orientation vertical to the substrate and the high-efficiency and stable tin-based perovskite solar cell thereof comprises the following steps:
the divalent tin in the tin-based perovskite system is in an unstable state thermodynamically and is easily oxidized into tetravalent tin. In addition, the crystallization rate is high during the preparation process, so that the surface defects are more. Aiming at the problems, the method for introducing the bifunctional ionic salt ethylenediamine formate to the tin-based perovskite interface is provided, so that the thermodynamic instability of the divalent tin is improved, the long-term stability of the divalent tin is improved, the defects on the interface are effectively passivated, the stability of the divalent tin is improved by changing the chemical environment around the divalent tin, and the tin-based perovskite thin film with a flat and compact surface, low defect state density and crystal orientation vertical to the substrate and the high-efficiency and stable tin-based perovskite solar cell are prepared,
in order to solve the technical problem of the invention, the technical scheme is as follows: a preparation method of a tin-based perovskite thin film passivated by bifunctional ionic salt and a perovskite solar cell thereof comprises the following steps:
(1) dissolving butylamine acetate, formamidine hydroiodide, stannous iodide and stannous fluoride into a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide according to a molar ratio of 2:3:4:0.6 (the volume ratio is 4:1), adding guanidine iodide serving as an additive to prepare a low-dimensional tin-based perovskite precursor liquid I, and stirring for 1-4 hours at 30-120 ℃; dissolving phenylethylamine hydrochloride, formamidine hydroiodide, stannous iodide and stannous fluoride into a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide according to a molar ratio of 2:3:4:0.6 (the volume ratio is 4:1), adding guanidine iodide serving as an additive to prepare a low-dimensional stannyl perovskite precursor liquid II, and stirring for 1-4 hours at the temperature of 30-120 ℃; dissolving formamidine hydroiodide, stannous iodide and stannous fluoride in a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide according to a molar ratio of 1:1:0.1 (the volume ratio is 4:1), adding guanidine iodide and ammonium thiocyanate serving as additives, preparing a tin-based perovskite precursor solution III, and stirring at 30-120 ℃ for 1-4 hours; mixing a low-dimensional tin-based perovskite precursor liquid I, a low-dimensional tin-based perovskite precursor liquid II and a tin-based perovskite precursor liquid III according to a molar ratio of 1-10: 1-10: 1-10, and stirring for 1-4 hours at 30-120 ℃;
(2) spin-coating and depositing a hole transport material on the cleaned and treated ITO transparent conductive glass;
(3) preheating ITO transparent conductive glass deposited with a hole transport material and a prepared tin-based perovskite precursor liquid;
(4) depositing a tin-based perovskite thin film on preheated ITO transparent conductive glass deposited with hole transport materials by an anti-solvent method;
(5) respectively depositing cation ethylenediamine and anion formic acid on the deposited tin-based perovskite thin film, and annealing to obtain a flat and compact tin-based perovskite thin film with low defect state density and crystal orientation vertical to the substrate;
(6) vacuum thermal evaporation of an electron transport material on the tin-based perovskite thin film;
(7) the interface modifying material and the metal electrode are thermally evaporated on the electron transporting material.
Preferably, the concentrations of the low-dimensional tin-based perovskite precursor liquid I, the low-dimensional tin-based perovskite precursor liquid II and the tin-based perovskite precursor liquid III in the step (1) are all 100-600 mg/mL; the dosage of the guanidine iodide additive in the step (1) is 5 wt% of the tin-based perovskite precursor liquid; the dosage of the ammonium thiocyanate additive in the step (1) is 3 wt% of the tin-based perovskite precursor liquid; in the step (1), the mixing molar ratio of the first low-dimensional tin-based perovskite precursor liquid to the second low-dimensional tin-based perovskite precursor liquid to the third tin-based perovskite precursor liquid is 3: 7: 2.5.
preferably, the hole transport material deposited on the transparent ITO conductive glass in the step (2) is PEDOT: PSS, and the specific steps are as follows: PSS, and annealing at 120 deg.C for 30 min.
Preferably, the preheating temperature of the transparent ITO conductive glass deposited with the hole transport material in the step (3) and the prepared tin-based perovskite precursor liquid is 40-80 ℃, and the preheating time is 1-5 min.
Preferably, the antisolvent used in the antisolvent method in the step (4) is anhydrous chlorobenzene, and the dosage is 0.1-0.8 mL.
Preferably, the concentration of ethylenediamine in the chlorobenzene solution used in the step (5) is 0.025mol/L, and the concentration of formic acid in the chlorobenzene solution used is 0.05 mol/L. The method comprises the following specific steps: after spin coating, annealing was carried out at 80 ℃ for 5 min.
Preferably, the heat steaming in the step (6)The plated electron-transporting material is C60And the thickness is 50 nm.
Preferably, in the step (7), the interface modification material is LiF, the metal electrode is Al, and the specific steps are as follows:
(1) LiF is thermally evaporated on the electron transport layer, and the thickness of the electron transport layer is 1 nm;
(2) the thickness of the metal Al electrode is 100 nm.
In order to solve the technical problem of the invention, another technical scheme is provided as follows: any bifunctional ionic salt passivated tin-based perovskite thin film and perovskite solar cell prepared by the preparation method of the perovskite solar cell.
In order to solve the technical problem of the invention, another technical scheme is provided as follows: the tin-based perovskite thin film passivated by the bifunctional ionic salt and the application of the tin-based perovskite solar cell thereof in the photoelectric field.
The invention has the beneficial effects that:
(1) the method for processing the interface by using a proper amount of bifunctional ionic salt can effectively passivate defects on the interface, improve the stability of the divalent tin by changing the chemical environment around the divalent tin, and prepare the tin-based perovskite thin film with flat and compact surface, smooth and compact surface, high vertical orientation and larger crystal grains;
(2) the tin-based perovskite solar cell subjected to the interface treatment can still maintain about 95% of initial efficiency after about 2000 hours under the non-encapsulated N2 atmosphere, and the tin-based perovskite solar cell not subjected to the interface treatment can only maintain 30% of initial efficiency after about 2000 hours under the non-encapsulated N2 atmosphere.
Drawings
The invention will be further explained with reference to the drawings.
FIG. 1 is an SEM image of a tin-based perovskite thin film with low defect state density and smooth and compact surface prepared in a nitrogen atmosphere and a tin-based perovskite thin film prepared by a traditional butylamine iodonium salt;
FIG. 2 is a grazing incidence wide-angle X-ray scattering diagram of a tin-based perovskite thin film prepared in a nitrogen atmosphere according to the present invention and a tin-based perovskite thin film prepared by a conventional butylamine iodonium salt;
FIG. 3 is a block diagram of a tin-based perovskite solar cell device fabricated in a nitrogen atmosphere in accordance with the present invention;
FIG. 4 is a J-V curve of a tin-based perovskite solar cell prepared in a nitrogen atmosphere according to the present invention and a tin-based perovskite solar cell prepared by a conventional butylamine iodonium salt;
FIG. 5 is a dark current curve diagram of a tin-based perovskite solar cell prepared in a nitrogen atmosphere according to the present invention and a tin-based perovskite solar cell prepared by a conventional butylamine iodonium salt;
FIG. 6 is a time-dependent change curve of photoelectric conversion efficiency of a tin-based perovskite solar cell prepared in a nitrogen atmosphere according to the invention and a tin-based perovskite solar cell prepared from a conventional butylamine iodonium salt in nitrogen;
Detailed Description
Example 1
This embodiment is an inverted planar heterojunction solar cell prepared by the method for preparing a tin-based perovskite thin film with low defect state density, smooth and compact surface and high vertical orientation by using a bifunctional ionic salt passivated tin-based perovskite thin film and a tin-based perovskite solar cell thereof, so as to fully understand the invention, and mainly comprises the following steps:
and step 1) sequentially carrying out ultrasonic treatment on the etched ITO conductive glass in ethanol, ultrapure water, a cleaning agent, ultrapure water and ethanol for 30min respectively. And drying by nitrogen, and baking in an oven to obtain a clean ITO substrate.
Step 2) dissolving 60.96mg of ionic liquid type organic large-volume amine molecular salt butylamine acetate, 118.06mg of formamidine hydroiodide, 340.98mg of stannous iodide and 86.05mg of stannous fluoride in 0.8mL of mixed solvent of N, N-dimethylformamide and 0.2mL of dimethyl sulfoxide, adding 26mg of guanidine iodide as an additive to prepare a low-vitamin tin-based perovskite precursor solution I, and stirring at 60 ℃ for 2 hours; dissolving 66.55mg of phenethylamine hydrochloride, 108.91mg of formamidine hydroiodide, 314.54mg of stannous iodide and 79.38mg of stannous fluoride in 0.8mL of mixed solvent of N, N-dimethylformamide and 0.2mL of dimethyl maple, adding 26mg of guanidine iodide as an additive to prepare a second low-dimensional stannyl perovskite precursor liquid, and stirring at 60 ℃ for 2 hours; 164.24mg of formamidine hydroiodide, 355.76mg of stannous iodide and 14.1mg of stannous fluoride are dissolved in 0.8mL of mixed solvent of N, N-dimethylformamide and 0.2mL of dimethyl sulfoxide, 15.6mg of ammonium thiocyanate is added as an additive to prepare a third tin-based perovskite precursor solution, and the third tin-based perovskite precursor solution is stirred for 2 hours at the temperature of 60 ℃; mixing 0.30mL of the first low-dimensional tin-based perovskite precursor solution, 0.70mL of the second low-dimensional tin-based perovskite precursor solution and 0.25mL of the third tin-based perovskite precursor solution, and stirring for 2 hours at 60 ℃;
and 3) carrying out ultraviolet ozone treatment on the ITO substrate cleaned in the step 1) for 15 minutes.
Step 4), taking 50 mu L of hole transport material PEDOT: and (3) dropping the PSS onto the ITO conductive glass treated in the step 3) by using a liquid transfer gun, spin-coating at the rotating speed of 5000 revolutions for 50 seconds, and then coating PEDOT: the ITO of PSS was annealed at 120 ℃ for 30 min.
And 5) placing the ITO conductive substrate coated with the hole transport layer and annealed in the step 4) and the low-dimensional tin-based perovskite precursor solution prepared in the step 1) on a hot table at 60 ℃ and preheating for 2 min.
And 6) dripping 75 mu L of the perovskite precursor solution preheated in the step 5) onto the ITO substrate preheated in the step 5), spin-coating to form a film, and then annealing to obtain the perovskite thin film. The conditions of spin coating the perovskite precursor solution comprise that the perovskite precursor solution is spin-coated for 60 seconds at 4000 revolutions in a nitrogen atmosphere, annealed for 2min at 60 ℃ and annealed for 10min at 100 ℃.
And 7) dripping 75 mu L of 0.025mM ethylene diamine chlorobenzene solution onto the thin film deposited with the tin-based perovskite in the step 6), and spin-coating to form a film. The condition for spin coating the interface layer was 3000 spin coating for 30 seconds in a nitrogen atmosphere.
And 8) dripping 75 mu L of 0.050mM formic acid chlorobenzene solution onto the film deposited with the ethylenediamine in the step 7), spin-coating to form a film, and then annealing. The interface layer is spin-coated under the condition of 3000-turn spin-coating for 30 seconds in a nitrogen atmosphere, and annealed at 80 ℃ for 2 min.
Step 9) vacuum thermal evaporation of electron transport material on the tin-based perovskite thin film, thermal evaporationThe electron transport material of (A) is C60And the thickness is 50 nm.
And step 10) thermally evaporating an interface modification material LiF with the thickness of 1nm and a metal electrode Al on the electron transport material.
Step 11) thermal evaporation is carried out on the interface modification material LiF to form a metal electrode Al with the thickness of 100nm,
step 12) under standard test conditions (am1.5g illumination), the photoelectric conversion efficiency of the solar cell device prepared in this example was 9.40%, the open-circuit voltage was 0.60V, and the short-circuit current was 23.71mA/cm2The fill factor was 66.21%. In addition, the tin-based perovskite solar cell after interface treatment is not packaged with N2Under the atmosphere, the initial efficiency of about 95 percent can be still maintained after about 2000 hours, and the tin-based perovskite solar cell without interface treatment has no encapsulated N2Only 30% of the initial efficiency was maintained after about 2000 hours under atmosphere. N not packaged with traditional low-dimensional tin-based perovskite solar cell2Under the atmosphere, the stability data of about 90 percent of the initial efficiency can be still maintained after about 600 hours.
The invention is not limited to the specific technical solutions described in the above embodiments, and all technical solutions formed by equivalent substitutions are within the scope of the claims of the invention.
Claims (10)
1. A preparation method of a tin-based perovskite thin film passivated by bifunctional ionic salt and a perovskite solar cell thereof is characterized by comprising the following steps:
(1) dissolving butylamine acetate, formamidine hydroiodide, stannous iodide and stannous fluoride into a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide according to a molar ratio of 2:3:4:0.6 (the volume ratio is 4:1), adding guanidine iodide serving as an additive to prepare a low-dimensional tin-based perovskite precursor liquid I, and stirring for 1-4 hours at 30-120 ℃; dissolving phenylethylamine hydrochloride, formamidine hydroiodide, stannous iodide and stannous fluoride into a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide according to a molar ratio of 2:3:4:0.6 (the volume ratio is 4:1), adding guanidine iodide serving as an additive to prepare a low-dimensional stannyl perovskite precursor liquid II, and stirring for 1-4 hours at the temperature of 30-120 ℃; dissolving formamidine hydroiodide, stannous iodide and stannous fluoride in a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide according to a molar ratio of 1:1:0.1 (the volume ratio is 4:1), adding guanidine iodide and ammonium thiocyanate serving as additives, preparing a tin-based perovskite precursor solution III, and stirring at 30-120 ℃ for 1-4 hours; mixing a low-dimensional tin-based perovskite precursor liquid I, a low-dimensional tin-based perovskite precursor liquid II and a tin-based perovskite precursor liquid III according to a molar ratio of 1-10: 1-10: 1-10, and stirring for 1-4 hours at 30-120 ℃;
(2) spin-coating and depositing a hole transport material on the cleaned and treated ITO transparent conductive glass;
(3) preheating ITO transparent conductive glass deposited with a hole transport material and a prepared tin-based perovskite precursor liquid;
(4) depositing a tin-based perovskite thin film on preheated ITO transparent conductive glass deposited with hole transport materials by an anti-solvent method;
(5) respectively depositing cation ethylenediamine and anion formic acid on the deposited tin-based perovskite thin film, and annealing to obtain a flat and compact tin-based perovskite thin film with low defect state density and crystal orientation vertical to the substrate;
(6) vacuum thermal evaporation of an electron transport material on the tin-based perovskite thin film;
(7) the interface modifying material and the metal electrode are thermally evaporated on the electron transporting material.
2. The preparation method of the tin-based perovskite thin film passivated by bifunctional ionic salt and the perovskite solar cell thereof according to claim 1 is characterized in that: in the step (1), the concentrations of the first low-dimensional tin-based perovskite precursor liquid, the second low-dimensional tin-based perovskite precursor liquid and the third tin-based perovskite precursor liquid are all 100-600 mg/mL; the dosage of the guanidine iodide additive in the step (1) is 5 wt% of the tin-based perovskite precursor liquid; the dosage of the ammonium thiocyanate additive in the step (1) is 3 wt% of the tin-based perovskite precursor liquid; in the step (1), the mixing molar ratio of the first low-dimensional tin-based perovskite precursor liquid to the second low-dimensional tin-based perovskite precursor liquid to the third tin-based perovskite precursor liquid is 3: 7: 2.5.
3. the preparation method of the tin-based perovskite thin film passivated by bifunctional ionic salt and the perovskite solar cell thereof according to claim 1 is characterized in that: PSS, namely PEDOT is used as the hole transport material deposited on the transparent ITO conductive glass in the step (2), and the specific steps are as follows: PSS, and annealing at 120 deg.C for 30 min.
4. The preparation method of the tin-based perovskite thin film passivated by bifunctional ionic salt and the perovskite solar cell thereof according to claim 1 is characterized in that: the preheating temperature of the transparent ITO conductive glass deposited with the hole transport material in the step (3) and the prepared tin-based perovskite precursor liquid is 40-80 ℃, and the preheating time is 1-5 min.
5. The preparation method of the tin-based perovskite thin film passivated by bifunctional ionic salt and the perovskite solar cell thereof according to claim 1 is characterized in that: the antisolvent used in the antisolvent method in the step (4) is anhydrous chlorobenzene, and the dosage is 0.1-0.8 mL.
6. The preparation method of the tin-based perovskite thin film passivated by bifunctional ionic salt and the perovskite solar cell thereof according to claim 1 is characterized in that: the concentration of the ethylene diamine used in the step (5) is 0.025mol/L chlorobenzene solution, and the concentration of the formic acid used is 0.05mol/L chlorobenzene solution. The method comprises the following specific steps: after spin coating, annealing was carried out at 80 ℃ for 5 min.
7. The preparation method of the tin-based perovskite thin film passivated by bifunctional ionic salt and the perovskite solar cell thereof according to claim 1 is characterized in that: the electron transport material thermally evaporated in the step (6) is C60And the thickness is 50 nm.
8. The preparation method of the tin-based perovskite thin film passivated by bifunctional ionic salt and the perovskite solar cell thereof according to claim 1 is characterized in that: in the step (7), the interface modification material is LiF, the metal electrode is Al, and the specific steps are as follows:
(1) LiF is thermally evaporated on the electron transport layer, and the thickness of the electron transport layer is 1 nm;
(2) the thickness of the metal Al electrode is 100 nm.
9. The tin-based perovskite thin film passivated by bifunctional ionic salt according to any one of claims 1 to 8 and the perovskite solar cell prepared by the preparation method of the perovskite solar cell.
10. The use of the bifunctional ionic salt passivated tin-based perovskite thin film and tin-based perovskite solar cell thereof according to claim 9 in the field of optoelectronics.
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