CN116634827A - Perovskite solar cell added with growth regulator and preparation method thereof - Google Patents

Perovskite solar cell added with growth regulator and preparation method thereof Download PDF

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Publication number
CN116634827A
CN116634827A CN202310690502.0A CN202310690502A CN116634827A CN 116634827 A CN116634827 A CN 116634827A CN 202310690502 A CN202310690502 A CN 202310690502A CN 116634827 A CN116634827 A CN 116634827A
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growth regulator
transport layer
solar cell
precursor solution
preparing
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张懿强
王世珩
张家浩
谷振坤
宋延林
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Zhengzhou University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/30—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising bulk heterojunctions, e.g. interpenetrating networks of donor and acceptor material domains
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/50—Photovoltaic [PV] devices
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/50—Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/60—Organic compounds having low molecular weight
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/549—Organic PV cells

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Abstract

The invention discloses a perovskite solar cell added with a growth regulator and a preparation method thereof, wherein the main body of the growth regulator molecule is aromatic halide and is modified by one or more of amide groups, acyl halide groups, ester groups and carboxyl groups. The growth regulator is added into the precursor solution of the organic halide, and the nucleation and crystallization process of perovskite is improved through the strong interaction between the growth regulator and the organic halide. The added growth regulator has the effects of delaying the release rate of the organic halide and inhibiting the rapid reaction between the organic halide and the metal halide, and the growth regulator finally remained on the surface or the grain boundary of the film can effectively passivate deep energy level defects caused by uncoordinated metal ions or halogen ions, so that the performance of the perovskite solar cell is improved.

Description

Perovskite solar cell added with growth regulator and preparation method thereof
Technical Field
The invention relates to the technical field of perovskite solar cells, in particular to a perovskite solar cell added with a growth regulator and a preparation method thereof.
Background
Perovskite solar cells, which are a new generation of thin film cells that are of great interest, exhibit extremely excellent photoelectric properties on small-area devices, with a current Photoelectric Conversion Efficiency (PCE) of up to 25.7%, but the perovskite solar cells fall into large-scale repetitive production, and there are still a number of problems and challenges, such as the choice of solvent/solute components in the perovskite solution, how to ensure the uniformity and crystallization quality of the large-area perovskite thin film, and thus to improve the product yield in the production of practical perovskite devices.
The traditional perovskite film forming method is called a one-step method, mainly comprising the steps of adding metal halide and organic halide into a proper solvent together to form a precursor solution, and then spin-coating and annealing the solution to form a film, wherein the method is easy to cause random nucleation and uncontrollable crystallization of perovskite; in contrast to the natural crystallization employed in the "one-step" process, the other process, the "two-step process", is a prior process for preparing layered metal halides (in PbI 2 For example), then depositing an organic halide (exemplified by MAI) to form a perovskite film by in situ secondary reaction, with a controlled nucleation crystallization process.
One of the key factors in preparing large-area perovskite thin films using a two-step process is the regulation of PbI 2 Reaction rate with MAI. If PbI 2 The reaction with MAI is very rapid, which may lead to the formation of a dense perovskite layer at the contact interface, thereby inhibiting subsequent MAI from entering PbI 2 Structure and continue the reaction. In addition, defects of surface and deep energy levels can be caused by insufficient coordination of lead ions, segregation of iodide ions and the like in the crystallization process, so that the defect state density of the film is increased, and the photoelectric performance of the whole device is affected.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a perovskite solar cell added with a growth regulator, which comprises the following steps of:
preparing an electron transport layer on a transparent conductive substrate;
sequentially preparing a metal halide precursor solution and an organic halide precursor solution added with a growth regulator on an electron transport layer (a hole transport layer is a trans-structure) to form a perovskite light absorption layer;
preparing a hole transport layer on the perovskite light absorption layer;
vacuum evaporating a metal electrode on the hole transport layer to form a perovskite solar cell;
or alternatively, the first and second heat exchangers may be,
preparing a hole transport layer on a transparent conductive substrate;
sequentially preparing a metal halide precursor solution and an organic halide precursor solution added with a growth regulator on the hole transport layer to form a perovskite light absorption layer;
preparing an electron transport layer on the perovskite light absorption layer;
and vacuum evaporating a metal electrode on the electron transport layer to form the perovskite solar cell.
Preferably, the main body of the growth regulator molecule is aromatic halide, and is modified by one or more of amide groups, acyl halide groups, ester groups and carboxyl groups, and the addition amount is 0.06-0.2 mg/mL.
Preferably, the metal halide is PbI 2 、PbBr 2 、PbCl 2 ；SnI 2 、SnBr 2 、SnCl 2 ；CsI、CsBr、CsCl；EuI 2 、EuBr 2 、EuCl 2 ；InI 3 、InBr 3 、InCl 3 ；NdI 3 、NdBr 3 、NdCl 3 ；TbI 3 、TbBr 3 、TbCl 3 One or more of (a) and (b).
Preferably, the organic halide is methylamine iodide, methylamine bromide, methylamine chloride; formamidine iodide, formamidine bromide, formamidine chloride; ethylamine iodide, ethylamine bromide, ethylamine chloride; acetamidine iodide, acetamidine bromide, acetamidine chloride; guanidinium iodide, guanidinium bromide, guanidinium chloride; one or more of methylenediammonium iodide, methylenediammonium bromide, and methylenediammonium chloride.
Preferably, the step of preparing the metal halide precursor solution is: dissolving metal halide in a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide to obtain a metal halide precursor solution.
Preferably, the step of preparing the organic halide precursor solution is: and mixing and dissolving the organic halide and the growth regulator in an isopropanol solvent to obtain a precursor solution.
Preferably, the step of sequentially preparing a metal halide precursor solution and an organic halide precursor solution to which a growth regulator is added on the electron transport layer or the hole transport layer to form a perovskite light absorbing layer includes: after the metal halide precursor solution is coated on the substrate layer, heating and annealing are carried out under the condition of 70 ℃; and (3) coating the organic halide precursor solution added with the growth regulator on the substrate layer, and heating and annealing at 145 ℃ to obtain the perovskite light-absorbing layer added with the growth regulator.
The invention also provides a perovskite solar cell added with the growth regulator, which is prepared by adopting any one of the methods.
The invention also provides a perovskite solar cell added with the growth regulator, which is characterized in that the perovskite solar cell added with the growth regulator is prepared by adopting the method, and the structure of the perovskite solar cell added with the growth regulator comprises a transparent conductive substrate, an electron transmission layer, a perovskite light absorption layer, a hole transmission layer and a metal electrode from top to bottom in sequence; or the trans-structure is composed of a transparent conductive substrate, a hole transport layer, a perovskite light absorption layer, an electron transport layer and a metal electrode.
According to the invention, the growth regulator is introduced into the precursor solution of the organic halide, and characteristic groups (such as amino groups) in the growth regulator interact with the organic halide through hydrogen bonds (N-H … F), so that the reaction rate of the organic halide and the metal halide is retarded, the rapid reaction between the organic halide and the metal halide is inhibited, and the conversion of the metal halide to an alpha-phase perovskite phase is promoted; in addition, the multiple functional groups in the characteristic groups (such as acyl (C=O) and amino) can effectively and synergistically passivate defects in perovskite, the efficiency of the finally obtained perovskite solar cell device reaches 24.35%, and 89.6% of the initial efficiency is still maintained after continuous operation for 1400 hours under high humidity.
Drawings
FIG. 1 is a flow chart of a method of preparing a perovskite solar cell with the addition of a growth regulator;
FIG. 2 is a graph showing comparison of I-V curves and PCE statistical distributions of perovskite solar cells obtained in example 1 and comparative example;
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a method for preparing a large-area perovskite solar cell, referring to fig. 1, comprising the following steps:
s110, continuously ultrasonically washing FTO conductive glass in deionized water, acetone, ethanol and isopropanol for 15min, then drying under the condition of nitrogen, and pre-treating with ultraviolet/ozone for 20-30 min for later use; 1.0mL of 15% SnO was removed by pipette 2 Solution, adding 6.0mL deionized water, and adding SnO 2 The concentration of the solution is diluted to 2.14 percent to form an electron transport layer precursor solution, and the electron transport layer can be ZnO or TiO 2 A solution; transmitting the electronsThe precursor solution for the transfer layer is filtered and then is continuously spin-coated on the FTO conductive glass for 30 seconds at the rotating speed of 5000r/min, and an electron transfer layer is formed after annealing for 20 minutes at 180 ℃.
S120, 599.31mg of lead iodide (PbI) 2 ) Dissolved in a mixed solution of 1mLN, N-dimethylformamide and dimethyl sulfoxide (N, N-dimethylformamide: the volume ratio of dimethyl sulfoxide is 9.5:0.5 Obtaining lead iodide solution; another 60.0mg of formamide and 14.0mg of macl were dissolved in 1mL of isopropyl alcohol (IPA) solvent to obtain an organic amine salt solution, and 0.1mg of 4-Fluorobenzamide (FBAD) was added thereto as a growth regulator, and a lead iodide solution and an optimized organic amine salt solution were spin-coated in this order over the electron transport layer, with spin-coating parameters of: the rotating speed of 1500r/min is adopted for 30s when the lead iodide solution is spin-coated, and then the lead iodide solution is heated and annealed for 1min at 70 ℃; spin-coating organic amine salt solution at 1500r/min for 30s, and then heating and annealing at 145 ℃ for 15min; all the operations are required to be carried out in a glove box filled with nitrogen, and the relative humidity is ensured to be 30-40% RH.
S130, weighing 520mg of lithium bistrifluoromethane sulfonyl imide, and dissolving in 1mL of anhydrous acetonitrile to prepare a lithium bistrifluoromethane sulfonyl imide solution; 72.3mg of Spiro-OMeTAD was dissolved in 1mL of chlorobenzene, followed by the addition of 28.8. Mu.L of tributyl phosphate solution and 17.5. Mu.L of lithium bistrifluoromethane-sulfonimide solution; and sucking 75 mu L of the Spiro-OMeTAD precursor solution by using a pipetting gun, setting the rotating speed to be 3000r/min, the acceleration to be 1000r/min and the time to be 30s, and coating a hole transport material on the perovskite film to prepare a hole transport layer, wherein the thickness of the hole transport layer is about 100nm.
S140, at vacuum degree<1×10 -5 Under the condition of Torr, metal Au is evaporated on the hole transport layer at a speed of 0.1-0.3A per second, and a 100nm Au electrode is formed.
Example 2
The embodiment provides a method for preparing a large-area perovskite solar cell, referring to fig. 1, comprising the following steps:
this example differs from example 1 in that the perovskite light absorbing layer was prepared by a knife coating method in this example, so that the production and application areas could be enlarged.
S210, continuously ultrasonic washing ITO conductive glass in deionized water, acetone, ethanol and isopropanol for 15min, drying under the condition of nitrogen, and pre-treating with ultraviolet/ozone for 20-30 min for later use; weighing 5mg of PTAA and dissolving the PTAA in 1mL of chlorobenzene to prepare a hole transport layer precursor solution of 5 mg/mL; in a glove box having a room temperature and a relative humidity of less than 45%, the hole transport layer precursor solution was added to a doctor blade apparatus container, the gap between a doctor blade and ITO was adjusted to 100 to 150 μm, and then the PTAA precursor solution was coated on an ITO substrate at a speed of 15 to 20mm/s and annealed at a temperature of 70 ℃ for 10min.
S220, 599.31mg of lead iodide (PbI) 2 ) Dissolved in a mixed solution of 1mLN, N-dimethylformamide and dimethyl sulfoxide (N, N-dimethylformamide: the volume ratio of dimethyl sulfoxide is 9.5:0.5 Obtaining lead iodide solution; another 60.0mg of formamide and 14.0mg of MACl were dissolved in 1mL of isopropyl alcohol (IPA) solvent to obtain an organic amine salt solution, and 0.1mg of 4-Fluorobenzamide (FBAD) was added thereto as a growth regulator, and a lead iodide solution and an organic amine salt solution were sequentially knife-coated over the hole transport layer. A volume of the optimized lead iodide solution was measured and charged into a container (volume 5X 5 cm) of a blade coating apparatus 2 The substrate of (C) is generally 70-80. Mu.L, 10X 10cm 2 Then 140-160 mu L is generally used), a knife coater is started to drop the solution into the gap between the coating knife head and the substrate (about 0.2-0.4 mm), the knife head is controlled by a system controller to horizontally move at a speed of 15mm/s to push the solution forward, a pinhole-free wet lead iodide film is obtained, the step is repeated to scrape the organic amine salt solution again, finally the film is blown to a dry state by a nitrogen air knife, and then the film is annealed on a hot table at 100 ℃ for 10min to completely remove the solvent, and the whole process is full of N 2 Is completed in a glove box and ensures a relative humidity of 30-40% rh.
S230, weighing 20mg of PC61BM and dissolving in 1mL of anhydrous chlorobenzene to prepare 20mg/mL of PC 61 BM electron transport layer solution; 2.5mg of BCP was weighed again and dissolved in 1mL of absolute ethanol to prepare 2.5mg/mL of BCP hole blocking layer solution; the two are sequentially deposited on the substrate by spin coatingOn the perovskite light-absorbing layer, spin-coating parameters were spin-speed 2000rpm, spin-time 30s, spin-speed 5000rpm, spin-time 30s, respectively.
S240, finally, at the vacuum degree<1×10 -5 Under the condition of Torr, metal Au is evaporated on the hole transport layer at a speed of 0.1-0.3A per second, and a 100nm Au electrode is formed.
Comparative example
This comparative example provides a method of manufacturing a solar cell, in contrast to example 1, comprising the steps of:
s310, continuously ultrasonically washing FTO conductive glass in deionized water, acetone, ethanol and isopropanol for 15min, then drying under the condition of nitrogen, and pre-treating with ultraviolet/ozone for 20-30 min for later use; 1.0mL of 15% SnO was removed by pipette 2 Solution, adding 6.0mL deionized water, and adding SnO 2 The concentration of the solution is diluted to 2.14 percent to form an electron transport layer precursor solution, and the electron transport layer can be ZnO or TiO 2 A solution; and filtering the electron transport layer precursor solution, continuously spin-coating the electron transport layer precursor solution on FTO conductive glass at a rotation speed of 5000r/min for 30s, and annealing at 180 ℃ for 20min to form the electron transport layer.
S320, taking 599.31mg of lead iodide (PbI) 2 ) Dissolved in a mixed solution of 1mLN, N-dimethylformamide and dimethyl sulfoxide (N, N-dimethylformamide: the volume ratio of dimethyl sulfoxide is 9.5:0.5 Obtaining lead iodide solution; another 60.0mg of formamide and 14.0mg of macl were dissolved in 1mL of isopropyl alcohol (IPA) solvent to obtain an organic amine salt solution, and a lead iodide solution and an organic amine salt solution were spin-coated in order over the electron transport layer, with spin-coating parameters of: the rotating speed of 1500r/min is adopted for 30s when the lead iodide solution is spin-coated, and then the lead iodide solution is heated and annealed for 1min at 70 ℃; spin-coating organic amine salt solution at 1500r/min for 30s, and then heating and annealing at 145 ℃ for 15min; all the operations are required to be carried out in a glove box filled with nitrogen, and the relative humidity is ensured to be 30-40% RH.
S330, weighing 520mg of lithium bistrifluoromethane sulfonyl imide, and dissolving in 1mL of anhydrous acetonitrile to prepare a lithium bistrifluoromethane sulfonyl imide solution; 72.3mg of Spiro-OMeTAD was dissolved in 1mL of chlorobenzene, followed by the addition of 28.8. Mu.L of tributyl phosphate solution and 17.5. Mu.L of lithium bistrifluoromethane-sulfonimide solution; and sucking 75 mu L of the Spiro-OMeTAD precursor solution by using a pipetting gun, setting the rotating speed to be 3000r/min, the acceleration to be 1000r/min and the time to be 30s, and coating a hole transport material on the perovskite film to prepare a hole transport layer, wherein the thickness of the hole transport layer is about 100nm.
S340, at vacuum degree<1×10 -5 Under the condition of Torr, metal Au is evaporated on the hole transport layer at a speed of 0.1-0.3A per second, and a 100nm Au electrode is formed.
As shown in fig. 2, which is a graph comparing the I-V curve and the PCE statistical distribution of the perovskite solar cell obtained in example 2 and comparative example, it is known that the efficiency of the perovskite solar cell device obtained in the present invention and the ratio of the initial efficiency maintained after continuous operation under high humidity are well improved.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A method for preparing a perovskite solar cell with a growth regulator, comprising the steps of:
preparing an electron transport layer on a transparent conductive substrate;
sequentially preparing a metal halide precursor solution and an organic halide precursor solution added with a growth regulator on an electron transport layer (a hole transport layer is a trans-structure) to form a perovskite light absorption layer;
preparing a hole transport layer on the perovskite light absorption layer;
vacuum evaporating a metal electrode on the hole transport layer to form a perovskite solar cell;
or alternatively, the first and second heat exchangers may be,
preparing a hole transport layer on a transparent conductive substrate;
sequentially preparing a metal halide precursor solution and an organic halide precursor solution added with a growth regulator on the hole transport layer to form a perovskite light absorption layer;
preparing an electron transport layer on the perovskite light absorption layer;
and vacuum evaporating a metal electrode on the electron transport layer to form the perovskite solar cell.
2. The method for producing a perovskite solar cell with a growth regulator according to claim 1, wherein the growth regulator molecule is an aromatic halide as a main body, is modified with one or more of an amide group, an acyl halide group, an ester group and a carboxyl group, and has an addition amount of 0.06 to 0.2mg/mL.
3. The method for producing a perovskite solar cell added with a growth regulator according to claim 1, wherein the metal halide is PbI 2 、PbBr 2 、PbCl 2 ；SnI 2 、SnBr 2 、SnCl 2 ；CsI、CsBr、CsCl；EuI 2 、EuBr 2 、EuCl 2 ；InI 3 、InBr 3 、InCl 3 ；NdI 3 、NdBr 3 、NdCl 3 ；TbI 3 、TbBr 3 、TbCl 3 One or more of (a) and (b).
4. The method of preparing a growth regulator-added perovskite solar cell according to claim 1, wherein the organic halide is methylamine iodide, methylamine bromide, methylamine chloride; formamidine iodide, formamidine bromide, formamidine chloride; ethylamine iodide, ethylamine bromide, ethylamine chloride; acetamidine iodide, acetamidine bromide, acetamidine chloride; guanidinium iodide, guanidinium bromide, guanidinium chloride; one or more of methylenediammonium iodide, methylenediammonium bromide, and methylenediammonium chloride.
5. The method of preparing a growth regulator-added perovskite solar cell as claimed in claim 1, wherein the step of preparing the metal halide precursor solution comprises: dissolving metal halide in a mixed solvent of N, N-dimethylformamide and dimethyl sulfoxide to obtain a metal halide precursor solution.
6. The method for preparing a perovskite solar cell added with a growth regulator according to claim 1, wherein the step of preparing an organic halide precursor solution comprises: and mixing and dissolving the organic halide and the growth regulator in an isopropanol solvent to obtain a precursor solution.
7. The method of manufacturing a perovskite solar cell with addition of a growth regulator according to claim 1, wherein the step of sequentially preparing a metal halide precursor solution and an organic halide precursor solution with addition of a growth regulator on the electron transport layer or the hole transport layer to form a perovskite light absorbing layer comprises: after the metal halide precursor solution is coated on the substrate layer, heating and annealing are carried out under the condition of 70 ℃; and (3) coating the organic halide precursor solution added with the growth regulator on the substrate layer, and heating and annealing at 145 ℃ to obtain the perovskite light-absorbing layer added with the growth regulator.
8. A perovskite solar cell added with a growth regulator, characterized in that it is prepared by the method according to any one of claims 1 to 7.
9. The perovskite solar cell added with the growth regulator is characterized by being prepared by adopting the method of claim 8, wherein the structure of the perovskite solar cell added with the growth regulator comprises a transparent conductive substrate, an electron transport layer, a perovskite light absorption layer, a hole transport layer and a metal electrode from top to bottom in sequence; or the trans-structure is composed of a transparent conductive substrate, a hole transport layer, a perovskite light absorption layer, an electron transport layer and a metal electrode.
CN202310690502.0A 2023-06-12 2023-06-12 Perovskite solar cell added with growth regulator and preparation method thereof Pending CN116634827A (en)

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