CN110993803B - Interface modification method of solar cell based on all-inorganic metal halide perovskite material - Google Patents
Interface modification method of solar cell based on all-inorganic metal halide perovskite material Download PDFInfo
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Abstract
The invention belongs to the field of solar cells, and discloses an interface modification method of a solar cell based on an all-inorganic metal halide perovskite material. CsPbI using strong UV light or humid atmosphere 2 Br or CsPbI 3 Partial decomposition occurs at the surface and grain boundaries and lead halide is generated; dripping the ultra-dry methanol solution of CsBr or CsCl on the perovskite layer and standing to generate CsPbBr on the surface and grain boundary of the perovskite 3 Or CsPbCl 3 A finishing layer; washing with methanol solvent to remove unreacted CsBr or CsCl; and finally, annealing. The method can form a passivation layer on the perovskite crystal boundary and the interface of the perovskite/hole transport layer, inhibit interface recombination and accelerate the extraction of holes, thereby improving the efficiency of the device. In addition, the stability of the material of the modified layer is superior to CsPbI 2 Br or CsPbI 3 The stability of the device is improved, and the method has important significance for the industrialization of the perovskite solar cell.
Description
Technical Field
The invention belongs to the field of solar cells, and particularly relates to an interface modification method of a solar cell based on an all-inorganic metal halide perovskite material.
Background
In recent years, perovskite materials have attracted extensive attention in academia and industry due to their excellent optical properties, high conversion efficiency, and low processing cost. In particular, organic-inorganic hybrid perovskite solar cells have rapidly developed, and conversion efficiency has been improved from the initial 3.8% to over 25%. However, the poor stability of organic cations in hybrid perovskites to heat and ultraviolet light has hindered the commercial application of such materials.
Compared with organic-inorganic hybrid perovskite, the all-inorganic metal halide perovskite material has similar photoelectric conversion performance and more excellent thermal and ultraviolet stability, and is expected to replace the organic-inorganic hybrid perovskite material. At present, the all-inorganic metal halide perovskite material with leading photoelectric conversion efficiency is mainly CsPbI 3 And CsPbI 2 Br, however, the two materials are extremely easy to be affected with damp and decomposed in the atmospheric environment, and the development of the solar cell based on the all-inorganic perovskite material is severely restricted. Anchoring some small organic molecules to the surface of these perovskite materials is a common approach to improve moisture resistance. However, these small organic molecules tend to adversely affect the photovoltaic performance of the cell due to poor carrier mobility. In addition, the ultraviolet stability of the small organic molecules is poor, and the protective effect of the small organic molecules on the perovskite material gradually declines in the actual use process. Therefore, research on a related interface modification method to improve the stability and photoelectric conversion efficiency of a solar cell based on an all-inorganic perovskite material plays an important role in realizing the industrialization of perovskite solar cells.
Disclosure of Invention
The purpose of the invention is as follows: based on all-inorganic perovskite materials (CsPbI) under atmospheric environment 3 Or CsPbI 2 Br) solar cell, developing a method for modifying perovskite thin film grain boundary and interface between the perovskite thin film grain boundary and a Hole Transport Layer (HTL), and generating ultrathin CsPbBr at the position 3 Or CsPbCl 3 And the passivation layer further improves the stability and the photoelectric conversion efficiency of the device in a humid environment.
The technical scheme of the invention is as follows: in order to improve the moisture resistance stability and the photoelectric conversion efficiency of the all-inorganic perovskite thin film based solar cell, an interface modification method is provided. The method comprises the steps of firstly utilizing strong ultraviolet light or moist atmosphere to enable the perovskite thin film to be partially decomposed at grain boundaries and surfaces to form lead halide, then utilizing CsBr or CsCl solution to react with the lead halide generated by decomposition, and finally forming CsPbBr 3 Or CsPbCl 3 A passivation layer (as shown in fig. 1). Preparation thereofThe method comprises the following steps:
(1) Cleaning FTO conductive glass: soaking the FTO conductive glass in a cleaning agent for 10min, wiping stains on the surface with dust-free cloth, sequentially placing the FTO conductive glass into deionized water, acetone and absolute ethyl alcohol, respectively ultrasonically cleaning for 20min, and placing the FTO conductive glass into an oven to dry (75 ℃).
(2) Water bath method for preparing TiO 2 Electron transport layer: 4.5mL of TiCl 4 Slowly dropwise adding the glass powder to an ice surface frozen by 200mL of deionized water, and soaking the FTO conductive glass cleaned in the step (1) into TiCl after the ice is melted 4 Reacting in water solution at 70 deg.C for 80min, washing with deionized water for three times, drying in oven at 100 deg.C for 1 hr to obtain FTO/TiO 2 ；
(3) Preparing an all-inorganic perovskite precursor solution:
a. preparation of CsPbI 2 Br precursor solution: weighing 0.2075g of PbI 2 0.1652g of PbBr 2 0.2338g of CsI was dissolved in 1mL of a mixed solvent (N, N-Dimethylformamide (DMF): dimethyl sulfoxide (DMSO) =4:1 (v/v)), stirred for 8h and filtered for standby;
or b. formulating CsPbI 3 Precursor solution: will PbI 2 And CsI is dissolved in 1mL of mixed solvent (N, N-Dimethylformamide (DMF): dimethyl sulfoxide (DMSO) =4:1 (v/v)) according to the stoichiometric ratio of 1:1, and is stirred for 8h and filtered for standby;
(4) Preparing a passivation layer precursor solution: weighing 0.001g-0.1g CsBr or CsCl, dissolving in 10mL of ultra-dry methanol solution, stirring for 8h, and filtering for later use;
(5) HTL solution: li-TFSI (Lithium-bis (trifluoromethylphenyl) imide) was first dissolved in acetonitrile to prepare a 520mg/ml Li-TFSI solution, and 5754 zft 5754 mg spiro-MeOTAD (3252 zft 3252 ', 3532 zft 3532 ' -Tetrakis [ N, N-di (4-methoxyphenyl) amino ] -3425 zft 3425 ' -spiro-bifluorene), 40.32uL4-t-butylpyridine and 24.5uL of Li-TFSI solution were dissolved in 1ml chlorobenzene, stirred for 12h and then filtered.
(6) TiO of the substrate prepared in step (2) 2 And (4) spin-coating the perovskite precursor solution prepared in the step (3) on the surface, and sequentially spin-coating according to the following steps:
(1) the rotating speed is 1000rpm/min, the acceleration a =800rpm/s, and the spin coating maintaining time t =10s
(2) The rotating speed is 4000rpm/min, the acceleration a =3500rpm/s, and the spin coating maintenance time t =35s
(3) Rotating speed 6000rpm/min, acceleration a =4500rpm/s, spin-coating time t =30s, and when t =15s, dropwise adding an anti-solvent chlorobenzene;
(7) And (3) placing the perovskite thin film prepared in the step (6) on a hot table for annealing: moving to a 160 ℃ hot bench for annealing for 2min after color change is observed on the 40 ℃ hot bench;
(8) Carrying out strong ultraviolet irradiation on the perovskite thin film prepared in the step (7) or placing the perovskite thin film in a humid atmosphere for a plurality of times;
subjecting the perovskite thin film to intense ultraviolet light or placing the perovskite thin film in a humid atmosphere can cause the parts with poor stability (namely, the parts with more defects, such as crystal boundaries and surfaces) in the thin film to be preferentially subjected to partial decomposition to generate lead halide (such as PbI) 2 ) And converted to CsPbBr in the subsequent step 3 Or CsPbCl 3 . Ultraviolet light intensity, atmospheric humidity and treatment time have important influence on the decomposition degree of the perovskite thin film. These three experimental conditions need to be controlled to properly decompose the perovskite thin film. If the decomposition is insufficient, the subsequent generated CsPbBr 3 Or CsPbCl 3 The decoration effect is insufficient; if the decomposition is excessive, the photoelectric properties of the entire perovskite thin film are degraded.
(9) Dripping 0.2mL of CsBr or CsCl solution prepared in the step (4) on the surface of the perovskite thin film treated in the step (8), standing for a period of time, washing with ultra-dry methanol while rotating (rotating speed 2000rpm/min, acceleration a =1000rpm/s, spin coating maintenance time t =30 s), then placing on a hot bench, and annealing at 60 ℃ for 5min;
(10) And (3) spin-coating the HTL solution prepared in the step (5) (the rotation speed is 4000rpm/min, the acceleration is a =2000rpm/s, and the spin-coating maintenance time is t =30 s) on the perovskite layer prepared in the step (9), and finally, evaporating a gold electrode on the hole transport layer by using a physical vapor deposition method.
Step (4) weighing 0.01g-0.05g CsBr or CsCl.
The quantity of the anti-solvent dropped in the step (6) is 80-150 mu L.
Purple in step (7)The intensity of the external light is 30-200mW/cm 2 The illumination time is 20s-10min.
In the step (7), the atmospheric humidity is 30-80%, and the standing time is 1-120s.
Steps (3) to (10) are carried out in a glove box, unless otherwise specified, and preferably, the water oxygen concentration in the glove box is controlled to 10ppm or less.
The invention has the technical effects that: csPbBr 3 Or CsPbCl 3 CsPbI ratio in atmospheric environment 3 Or CsPbI 2 Br is more stable, but the former has a large forbidden band width and is not an ideal photoelectric conversion material. By CsBr or CsCl with CsPbI 2 Br or CsPbI 3 Lead halide reaction at the surface and internal grain boundary of perovskite layer due to decomposition to generate CsPbBr 3 Or CsPbCl 3 The modification layer can effectively prevent water vapor from invading the perovskite film, passivate the perovskite/hole transport layer interface and the crystal boundary defects inside the perovskite, and reduce the carrier recombination at the interface, thereby improving the stability of the device and improving the photoelectric conversion efficiency.
Drawings
FIG. 1 is a schematic representation of interfacial modification.
FIG. 2 is a J-V curve diagram of an unmodified perovskite solar cell and photoelectric performance parameters thereof.
Fig. 3-5 are J-V curves and their photoelectric performance parameters of the perovskite solar cells subjected to interface modification under different conditions in examples 1, 2 and 4, respectively.
Detailed Description
The present invention is further illustrated by the following examples, but the scope of the present invention is not limited to the following examples.
Comparative example 1
(1) Cleaning FTO conductive glass: soaking FTO conductive glass in a cleaning agent for 10min, wiping stains on the surface with dust-free cloth, sequentially placing the FTO conductive glass into deionized water, acetone and absolute ethyl alcohol to respectively perform ultrasonic cleaning for 20min, and finally placing the FTO conductive glass into an oven to be dried (75 ℃);
(2) Water bath method for preparing TiO 2 Electron transport layer: 4.5ml of TiCl 4 (AR, commercially available) slowly droppingAdding to 200mL of ice frozen with deionized water, and soaking the cleaned FTO conductive glass (1.5 x 2.5cm, commercially available) of step 1) in TiCl after the ice melts to form an ice-water mixture 4 Reacting in water solution at 70 deg.C for 80min, washing with deionized water for three times, and drying in oven at 100 deg.C for 1 hr to obtain FTO/TiO 2 ；
(3) Preparing an all-inorganic perovskite precursor solution:
a. preparation of CsPbI 2 Br precursor solution: weighing 0.2075g of PbI 2 0.1652g of PbBr 2 0.2338g of CsI was dissolved in 1mL of a mixed solvent (N, N-Dimethylformamide (DMF): dimethyl sulfoxide (DMSO) =4:1 (v/v)), stirred for 8h and filtered for standby;
b. preparation of CsPbI 3 Precursor solution: will PbI 2 And CsI is dissolved in 1mL of mixed solvent (N, N-Dimethylformamide (DMF): dimethyl sulfoxide (DMSO) =4:1 (v/v)) according to the stoichiometric ratio of 1:1, and is stirred for 8h and filtered for standby;
(4) HTL solution: li-TFSI (Lithium-bis (trifluoromethylphenyl) imide) (AR, commercially available) was first dissolved in acetonitrile (AR, commercially available) to prepare a 520mg/ml Li-TFSI solution, 5754 zft 5754 mg spiro-MeOTAD (3252 zft 3252 ', 3532 zft 3532 ' -Tetrakis [ N, N-di (4-methoxyphenyl) amino ] -3425 zft 3425 ' -spiro-bifluorene) (AR, commercially available), 40.32uL 4-tert-butylpyridine (AR, commercially available) and 24.5uL of Li-TFSI solution were dissolved in 1ml chlorobenzene (AR, commercially available) and filtered after stirring for 12 h.
(5) TiO of the substrate prepared in step (2) 2 Surface spin coating of the perovskite precursor (CsPbI) prepared in step (3) 2 Br or CsPbI 3 ) The solution, spin coating process is as follows:
(1) the rotating speed is 1000rpm/min, the acceleration a =800rpm/s, and the spin coating maintaining time t =10s
(2) The rotating speed is 4000rpm/min, the acceleration a =3500rpm/s, and the spin coating maintenance time t =35s
(3) Rotating speed of 6000rpm/min, acceleration a =4500rpm/s, spin coating time t =30s, and 100 μ L of anti-solvent chlorobenzene is dripped when t =15 s;
(6) Placing the perovskite thin film prepared in the step (5) on a hot table for annealing (the perovskite thin film is moved to the hot table at 160 ℃ for annealing for 2min after discoloration is observed at 40 ℃);
(7) And (3) spin-coating the hole transport layer solution prepared in the step (5) on the perovskite layer prepared in the step (6) (the rotating speed is 4000rpm/min, the acceleration is a =2000rpm/s, and the spin-coating maintaining time is t =30 s), and finally, evaporating a gold electrode on the hole transport layer by using a physical vapor deposition method.
The cell prepared in step 7 of comparative example 1 was tested for I-V curve (under simulated sunlight of AM 1.5G) and had an efficiency of 10.44% (as shown in fig. 2). The cell was stored in an atmosphere at 30-50% humidity in an unpackaged condition, and the efficiency dropped to about 25% (2.60%) of the initial efficiency after 72 h.
Comparative example 2
(1) 0.25mg of 2,9,16, 23-tetra-tert-butyl-29H, 31H-phthalocyanine (AR, commercially available) is weighed into 1ml of chlorobenzene and stirred for 8h until it is completely dissolved;
(2) Replacing the anti-solvent chlorobenzene in the spin coating process (3) in the step (5) in the comparative example 1 with the phthalocyanine solution prepared in the step (1) in the comparative example 2;
(3) The subsequent steps were the same as in comparative example 1.
The prepared cell was tested for its I-V curve (under AM 1.5G of simulated sunlight) and its efficiency was 10.80%. The cell was stored in an atmosphere at 30-50% humidity in an unpackaged condition, and the efficiency dropped to about 40% (4.30%) of the initial efficiency after 72 h.
Example 1
(1) Weighing 0.05g CsBr, adding into 10ml of ultra-dry methanol solution, and stirring for 8 hours until the CsBr is completely dissolved;
(2) CsPbI prepared in step (6) of comparative example 1 2 The Br perovskite film is placed in a humid atmosphere with the humidity of 50% and treated for 20s;
(3) The CsPbI treated in step (2) of example 1 was added 2 Putting the Br perovskite film into a glove box, dropwise adding 0.2mL of CsBr solution prepared in the step (1) of the embodiment 1 on the surface of the Br perovskite film, and standing for 10s;
(4) CsPbI is washed by ultra-dry methanol while rotating 2 Br film (rotation speed 2000rpm/min, acceleration a =1000rpm/s, spin coating maintenance time t =30 s), after which it was placed on a hot stage on a hot plateAnnealing at 60 deg.C for 5min;
(5) The subsequent steps were the same as in step (7) of comparative example 1.
The prepared cell was tested for I-V curve (under AM 1.5G of simulated sunlight) and its efficiency was 13.20% (as shown in fig. 3). The cell was stored in an atmosphere at 30-50% humidity in an unpackaged condition, and the efficiency dropped to about 70% (9.26%) of the initial efficiency after 72 h.
Example 2
(1) Weighing 0.05g CsCl, adding into 10ml of ultra-dry methanol solution, and stirring for 8 hours until the CsCl is completely dissolved;
(2) CsPbI prepared in step (6) of comparative example 1 3 The perovskite thin film is placed in a humid atmosphere with the humidity of 30% and treated for 20s;
(3) CsPbI treated in step (2) of example 2 3 Putting the perovskite thin film into a glove box, dropwise adding 0.2mL of CsCl solution prepared in the step (1) of the example 2 on the surface of the perovskite thin film, and standing for 10s;
(4) The subsequent steps were the same as in steps (4) to (5) of example 1.
The prepared cell was tested for I-V curve (under AM 1.5G of simulated sunlight) and had an efficiency of 13.48% (as shown in fig. 4). The cell was stored in an atmosphere of 30-50% humidity in an unpackaged condition, and the efficiency dropped to about 65% (8.78%) of the initial efficiency after 72 h.
Example 3
(1) Weighing 0.023g CsBr, adding into 10ml of ultra-dry methanol solution, and stirring for 8h until the CsBr is completely dissolved;
(2) CsPbI prepared in step (6) of comparative example 1 2 The Br perovskite film is placed in a humid atmosphere with the humidity of 70% and treated for 5s;
(3) CsPbI treated in step (2) of example 3 2 Putting the Br perovskite film into a glove box, dropwise adding 0.2mL of CsBr solution prepared in the step (1) of the embodiment 3 on the surface of the Br perovskite film, and standing for 10s;
(4) The subsequent steps were the same as in steps (4) to (5) of example 1.
The prepared cell was tested for I-V curve (under AM 1.5G of simulated sunlight) and had an efficiency of 13.79%. The cell was stored in an atmosphere at 30-50% humidity in an unpackaged condition, and the efficiency dropped to about 70% (9.65%) of the initial efficiency after 72 h.
Example 4
(1) Weighing 0.023g CsCl and adding the CsCl into 10ml of ultra-dry methanol solution, and stirring for 8 hours until the CsCl is completely dissolved;
(2) CsPbI prepared in step (6) of comparative example 1 3 Placing the perovskite thin film under a strong ultraviolet lamp for illumination treatment for 2min (the illumination intensity is 80 mW/cm) 2 )；
(3) CsPbI treated in step (2) of example 4 3 Putting the perovskite thin film into a glove box, dropwise adding 0.2mL of CsCl solution prepared in the step (1) of the example 4 on the surface of the perovskite thin film, and standing for 10s;
(4) The subsequent steps were the same as in steps (4) to (5) of example 1.
The prepared cell was tested for I-V curve (under AM 1.5G of simulated sunlight) and had an efficiency of 12.23% (as shown in fig. 5). The cell was stored in an atmosphere of 30-50% humidity in an unpackaged condition, and the efficiency dropped to 80% (9.78%) of the initial efficiency after 72 h.
Example 5
(1) Weighing 0.023g CsBr, adding the CsBr into 10ml of ultra-dry methanol solution, and stirring for 8 hours until the CsBr is completely dissolved;
(2) CsPbI prepared in step (6) of comparative example 1 2 Placing Br perovskite thin film under strong ultraviolet lamp for illumination treatment for 0.5min (illumination intensity is 180 mW/cm) 2 )；
(3) CsPbI treated in step (2) of example 5 2 Putting the Br perovskite film into a glove box, dropwise adding 0.2mL of CsBr solution prepared in the step (1) of the example 5 on the surface of the Br perovskite film, and standing for 10s;
(4) The subsequent steps were the same as in steps (4) to (5) of example 1.
The prepared cell was tested for its I-V curve (under AM 1.5G of simulated sunlight) and its efficiency was 12.86%. The cell was stored in an atmosphere at 30-50% humidity in an unpackaged condition, and the efficiency dropped to about 85% (10.94%) of the initial efficiency after 72 h.
Comparative example 3
In example 4, the UV irradiation time was extended to 30min. The prepared cell was tested for its I-V curve (under AM 1.5G of simulated sunlight) and its efficiency was 8.33%. The cell was stored in an atmosphere of 30-50% humidity in an unpackaged condition, and the efficiency dropped to about 40% (3.33%) of the initial efficiency after 72 h.
Comparative example 4
The humid air treatment time was extended to 10min in example 1. The prepared cell was tested for its I-V curve (under AM 1.5G of simulated sunlight) and its efficiency was 3.56%. The cell was stored in an atmosphere at 30-50% humidity in an unpackaged condition, and the efficiency dropped to about 20% (0.72%) of the initial efficiency after 72 h.
Claims (6)
1. An interface modification method of a solar cell based on an all-inorganic metal halide perovskite material is characterized by comprising the following steps:
(1) Cleaning FTO conductive glass: soaking the FTO conductive glass in a cleaning agent for 10min, wiping stains on the surface with dust-free cloth, sequentially placing the FTO conductive glass into deionized water, acetone and absolute ethyl alcohol, respectively ultrasonically cleaning for 20min, and placing the FTO conductive glass into an oven to dry at 75 ℃;
(2) Water bath method for preparing TiO 2 Electron transport layer: mixing TiCl 4 Slowly dropwise adding the FTO conductive glass into ice surface frozen by deionized water, and soaking the FTO conductive glass cleaned in the step (1) into TiCl after the ice is melted 4 Reacting in water solution at 70 deg.C for 80min, washing with deionized water for three times, drying in oven at 100 deg.C for 1 hr to obtain FTO/TiO 2 ；
(3) Preparing an all-inorganic perovskite precursor solution:
a. preparation of CsPbI 2 Br precursor solution: weighing 0.2075g of PbI 2 0.1652g of PbBr 2 0.2338g of CsI is dissolved in 1mL of mixed solvent, stirred for 8h and filtered for standby;
or b. formulating CsPbI 3 Precursor solution: will PbI 2 And CsI is dissolved in 1mL of mixed solvent according to the stoichiometric ratio of 1:1, and the mixture is stirred for 8 hours and filtered for standby;
wherein the volume ratio of N, N-Dimethylformamide (DMF) to dimethyl sulfoxide (DMSO) in the mixed solvent is 4:1;
(4) Preparing a passivation layer precursor solution: weighing 0.001g-0.1g CsBr or CsCl, dissolving in 10mL of ultra-dry methanol solution, stirring for 8h, and filtering for later use;
(5) HTL solution: li-TFSI (Lithium-bis (tri fl uoromethonesulphonyl) imide) is firstly dissolved in acetonitrile to prepare a Li-TFSI solution with the concentration of 520mg/ml, 101.22mg of spiro-MeOTAD (2,2 ',7,7' -Tetrakis [ N, N-di (4-methoxyphenyl) amino ] -9,9' -spiro-bifluorene), 40.32uL 4-tert-butylpyridine and Li-TFSI solution of 24.5uL are dissolved in 1ml chlorobenzene, and filtered after stirring for 12 h;
(6) TiO of the substrate prepared in step (2) 2 Spin-coating the surface of the perovskite precursor solution prepared in the step (3);
the spin coating process comprises the following steps:
(7) And (3) placing the perovskite thin film prepared in the step (6) on a hot table for annealing: moving to a 160 ℃ hot bench for annealing for 2min after color change is observed on the 40 ℃ hot bench;
(8) Performing strong ultraviolet illumination on the perovskite thin film prepared in the step (7) or placing the perovskite thin film in humid atmosphere;
the intensity of the ultraviolet light is 30-200mW/cm 2 The illumination time is 20s-10 min;
the atmospheric humidity is 30-80%, and the standing time is 1-120 s;
(9) Dropwise adding the CsBr or CsCl solution prepared in the step (4) on the surface of the perovskite thin film treated in the step (8), standing, washing with ultra-dry methanol while rotating, then placing on a hot bench, and annealing at 60 ℃ for 5min;
(10) And (4) spin-coating the HTL solution prepared in the step (5) on the perovskite layer prepared in the step (9), and finally evaporating a gold electrode on the hole transport layer by using a physical vapor deposition method.
2. The method for interface modification of a solar cell according to claim 1, wherein in the step (4), 0.01g to 0.05g of CsBr or CsCl is dissolved in 10mL of an ultra-dry methanol solution.
3. The method for modifying the interface of a solar cell according to claim 1, wherein the spin speed during the ultra-dry methanol rinsing in step (9) is 2000rpm/min, the acceleration a =1000rpm/s, and the spin-coating maintenance time t =30s.
4. The method for modifying the interface of the solar cell according to claim 1, wherein the rotation speed of the HTL solution in the spin coating of step (10) is 4000rpm/min, the acceleration a =2000rpm/s, and the spin coating maintenance time t =30s.
5. The method for modifying an interface of a solar cell according to claim 1, wherein the steps (3) to (10) are performed in a glove box unless otherwise specified.
6. The method for modifying an interface of a solar cell according to claim 5, wherein a water oxygen concentration of the glove box is controlled to 10ppm or less.
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