CN113097392A - Grain boundary passivation method of perovskite solar cell - Google Patents
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Abstract
The invention discloses a grain boundary passivation method of a perovskite solar cell, which comprises the steps of firstly utilizing room-temperature solution reaction with simple operation to synthesize nano-scale C6H6NNaO6A Pb quantum dot; and then, in the process of preparing the perovskite thin film by a one-step method, the synthesized quantum dots are uniformly dispersed in an anti-solvent, so that the quantum dots are uniformly distributed in the perovskite thin film, and the perovskite grain boundary passivation is realized. The invention can effectively reduce the defect state density of the perovskite crystal boundary and improve the quality of the perovskite thin film, thereby obtaining the perovskite solar cell with high efficiency and stability. The preparation method is simple in process and low in cost, and has a good application prospect in the aspect of developing high-performance perovskite solar cells.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a grain boundary passivation method of a perovskite solar cell.
Background
Solar cells can be mainly classified into three types so far: a first generation crystalline silicon solar cell, a second generation compound thin film solar cell and a third generation novel solar cell. Among them, perovskite solar cells are superior as novel solar cells, and are widely concerned by researchers due to the advantages of high extinction coefficient, adjustable band gap, low cost, simple preparation and the like. In recent years, due to the active efforts of researchers in the directions of perovskite morphology regulation, cell structure, device physics, interface engineering, energy band engineering and the like, the perovskite solar cell is developed rapidly, and the photoelectric conversion efficiency of the device is improved to 25.5% at present from 3.8% in 2009 (https:// www.nrel.gov/pv/cell-efficienccy.
From the above development process, the perovskite solar cell is developed rapidly, the photoelectric conversion efficiency is improved year by year, and the perovskite solar cell can be compared with the silicon-based solar cell, but a certain gap exists between the perovskite solar cell and the Shockley-Queisser limit efficiency of 31% (L.Fu et al, Energy & Environmental science 2020,13, 4017-. Research shows that the crystal boundary defects of the perovskite thin film are key factors for restricting the photoelectric conversion efficiency and the device stability of the perovskite solar cell, and the existence of a large number of defects can cause serious charge recombination inside the perovskite thin film, so that the performance of the photovoltaic device is reduced (L.D. Whalley et al, Journal of Chemical physics.2017,146, 220901).
Interface engineering is an effective method for passivating the surface defects of perovskite crystals, and is expected to further improve the efficiency and stability of perovskite solar cells. The high-quality quantum dots are expected to effectively passivate perovskite crystal boundary defects and reduce defect state density in the perovskite thin film, and have important significance for developing high-performance perovskite solar cells.
Disclosure of Invention
The invention aims to provide a grain boundary passivation method of a perovskite solar cell, which is implemented through a nanometer size C6H6NNa3O6The Pb quantum dots passivate the crystal boundary defects of the perovskite thin film, so that the photoelectric conversion efficiency of the perovskite solar cell is improved, and the stability of the device is improved. Book (I)The method has the advantages of simple preparation process, low cost, easy operation, safety and the like.
The grain boundary passivation method of the perovskite solar cell comprises the following steps:
step 1: quantum dot synthesis
In the range of 0.1 to 0.2mmol C6H9NNa3O6Slowly adding 0.05-0.1 mmol Pb (CH) into the aqueous solution3COO)2Continuously stirring the solution for 1-2 h; further standing the mixed solution in air for 24-48 h, and then centrifuging, washing and drying the solution to obtain C6H6NNaO6Storing the Pb quantum dot powder material for later use;
step 2: perovskite grain boundary passivation
And depositing a wide-band-gap semiconductor material on a conductive glass substrate such as FTO or ITO to serve as an electron transport layer. The perovskite absorption layer film is prepared by adopting a one-step method. In a glove box N2In the atmosphere, firstly, uniformly spin-coating 50-150 mL of perovskite precursor solution on an electron transport layer, wherein the spin-coating rotation speed is 3500-4500 rpm; then the C synthesized in the step 16H6NNaO6The Pb quantum dots are dispersed in the anti-solvent at the concentration of 0.5-20 wt%, when the perovskite precursor solution starts to spin for 6-10 s, the anti-solvent containing the quantum dots is dripped on the substrate, after the perovskite precursor solution is spin-coated for 20-30 s, the substrate is placed on a heating table at the temperature of 100-110 ℃ for annealing for 5-15 min, and the target perovskite thin film is obtained.
And step 3: perovskite cell preparation
And (3) further spin-coating a hole transport layer and evaporating a metal electrode on the perovskite thin film obtained in the step (2) according to a conventional method to finish the preparation of the perovskite battery.
In step 2, the wide band gap semiconductor material is TiO2、SnO2ZnO, CdS, etc., preferably TiO2Or SnO2。
In step 2, the target perovskite thin film is CH3NH3PbI3(abbreviated as MAPbI)3)、HC(NH2)2PbI3(abbreviated FAPBI)3)、(Cs,MA,FA)PbI3And the like.
In step 2, the perovskite precursor solution is MAI, FAI, CsI and PbI required for preparing corresponding perovskite types by one-step method2The precursor raw material mixed solution is obtained, and the concentration range of the precursor is 0.5-1.5 g/mL; wherein the monovalent cation is iodide and PbI2According to the stoichiometric ratio, the volume ratio of DMF to DMSO is 9: 1 constitutes the solvent.
In the step 2, the anti-solvent is ethyl acetate, chlorobenzene, diethyl ether and the like.
In step 3, the hole transport layer material is spiro-OMeTAD, P3HT and the like.
In step 3, the metal electrode is Au, Ag or the like.
Compared with the prior art, the invention has the beneficial effects that:
1. the monodisperse quantum dots are generally synthesized by a traditional thermal injection method, and the thermal injection method has a complex process and high requirements on synthesis conditions. In the method, the quantum dots are only required to be prepared under the conditions of room temperature and atmospheric environment, and the method is simple and easy to operate;
2. the method can effectively passivate perovskite crystal boundaries, reduce defect state density inside the perovskite thin film, and is beneficial to developing high-performance perovskite solar cells.
Drawings
Fig. 1 is a schematic structural diagram of a perovskite solar cell using quantum dots to perform grain boundary passivation: 1 is FTO or ITO conductive glass; 2 is an electron transport layer TiO2、SnO2ZnO or CdS, etc.; 3 is a perovskite absorption layer; 4 is a quantum dot; 5 is a hole transport layer; 6 is metal electrode Au or Ag, etc.
FIG. 2 is room temperature solution synthesized C6H6NNaO6TEM images of Pb quantum dots. Therefore, the size of the quantum dots is about 3-5 nm.
FIG. 3 is a MAPbI with grain boundary passivation using quantum dots3SEM image of perovskite thin film surface. It can be seen that the perovskite crystallites are about 500 nm.
FIG. 4 is a MAPbI with and without grain boundary passivation by quantum dots3Perovskite solar cell J-V plot.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
1. cleaning of the conductive substrate: sequentially carrying out ultrasonic cleaning on the etched FTO glass for 15-20 min by using detergent, deionized water, acetone, ethanol and isopropanol, drying the glass by using a nitrogen gun after the cleaning is finished, and then carrying out UVO treatment for 25-30 min;
2、TiO2preparation of an electron transport layer: stirring 125 μ L of titanium diisopropoxybialcetylacetonate solution and 1590 μ L of n-butanol for 1h, dropping the mixed solution onto FTO glass, rotating at 500rpm for 3s, 2000rpm for 30s, annealing at 135 deg.C for 10min, and sintering at 500 deg.C for 30min to obtain TiO2Dense layer of TiO2After the mesoporous film substrate is treated by ozone for 20min, transferring to N2An ambient glove box;
3. preparation of perovskite layer: 100mL of MAPbI3Perovskite precursor solution is fully paved with TiO2Spin coating was performed on the electron transport layer at 4000 rpm. MAPbi3The perovskite precursor solution is prepared by mixing PbI2And CH3NH3I in DMF and DMSO solvent, wherein PbI is2：CH3NH3I: the mol ratio of DMSO is 1: 1: 1, DMF: the volume ratio of DMSO is 9: 1, mixing and stirring for 30 min. After 6-8 s, 100 mu L of C with a certain concentration is dripped6H6NNaO6Carrying out spin coating on an ethyl acetate anti-solvent of the Pb quantum dots for 20s, and then heating the film on a heating table at 105 ℃ for 10min to obtain a perovskite film;
4. preparation of hole transport layer: a mixture of 72.3mg of spiro-OMeTAD, 1mL of chlorobenzene, 28.8. mu.L of 4-t-butylpyridine, 17.5. mu.L of LI-TFSI, 20mg was spin-coated at 4000rpm for 30s to prepare a hole transport layer;
5. preparing a metal electrode: and (4) placing the sample prepared in the step (4) in a thermal evaporation device, and evaporating and coating a 80nm metal electrode.
TABLE 1 different mass percentages of C6H6NNaO6Pb quantum dot pair MAPbI3Perovskite solar cell performance impact
From Table 1, it can be seen that C is the antisolvent6H6NNaO6Concentration pair of Pb quantum dots to MAPbI3Perovskite solar cell efficiency has a significant impact.
Example 2:
1. cleaning of the conductive substrate: sequentially carrying out ultrasonic cleaning on the etched FTO glass for 15-20 min by using detergent, deionized water, acetone, ethanol and isopropanol, drying the glass by using a nitrogen gun after the cleaning is finished, and then carrying out UVO treatment for 25-30 min;
2. preparation of different electron transport layers: (1) TiO 22: stirring 125 μ L of titanium diisopropoxybialcetylacetonate solution and 1590 μ L of n-butanol for 1h, dropping the mixed solution onto FTO glass, rotating at 500rpm for 3s, 2000rpm for 30s, annealing at 135 deg.C for 10min, and sintering at 500 deg.C for 30min to obtain TiO2A dense layer; (2) SnO2: mixing commercial SnO2The volume ratio of the hydrosol to the deionized water is 1: 7 mix diluted and then spin coated on clean FTO at 3000rpm for 30 s. After the spin coating is finished, placing the mixture on a heating table and heating the mixture for 30min at 150 ℃; (3) ZnO: ZnO with the particle size of 20nm and absolute ethyl alcohol are selected to be diluted according to the mass ratio of 1:3, and then spin coating is carried out on cleaned FTO at the rotating speed of 2000rpm for 30 s. After the spin coating is finished, drying at 70 ℃, and then sintering at 500 ℃ for 30 min; (4) CdS: mixing 30ml of cadmium nitrate aqueous solution (15mM) with 39ml of ammonia water, stirring for 2min, adding 229ml of thiourea aqueous solution (0.1M), stirring for 2min, and vertically immersing the cleaned FTO in the mixed solutionThe stirring was continued for 4 minutes while maintaining the temperature of 65 ℃. Finally, taking out the FTO/CdS substrate, cleaning with deionized water, drying with a nitrogen gun, and heating on a heating table at 100 ℃ for 10 min;
3. preparation of perovskite layer: 100mL of MAPbI3The perovskite precursor solution is fully paved on the electron transport layer, and spin coating is carried out at the rotating speed of 4000 rpm. MAPbi3The perovskite precursor solution is prepared by mixing PbI2And CH3NH3I in DMF and DMSO solvent, wherein PbI is2：CH3NH3I: the mol ratio of DMSO is 1: 1: 1, DMF: the volume ratio of DMSO is 9: 1, mixing and stirring for 30 min. After 6-8 s, 100 mu L of C with the mass percent of 0 and 0.25wt percent is dripped6H6NNaO6Carrying out spin coating on an ethyl acetate anti-solvent of the Pb quantum dots for 20s, and then heating the film on a heating table at 105 ℃ for 10min to obtain a perovskite film;
4. preparation of hole transport layer: a mixture of 72.3mg of spiro-OMeTAD, 1mL of chlorobenzene, 28.8. mu.L of 4-t-butylpyridine, 17.5. mu.L of LI-TFSI, 20mg was spin-coated at 4000rpm for 30s to prepare a hole transport layer;
5. preparing a metal electrode: and (4) placing the sample prepared in the step (4) in a thermal evaporation device, and evaporating and coating a 80nm metal electrode.
Table 2 different electron transport layers versus quantum dot passivated MAPbI3Effect of perovskite solar cell Performance
From table 2 it can be seen that different electron transport layers are responsible for the quantum dot passivated MAPbI3Perovskite solar cell efficiency has a significant impact.
Claims (7)
1. A grain boundary passivation method of a perovskite solar cell is characterized by comprising the following steps:
firstly, the nano-scale C is synthesized by room-temperature solution reaction which is simple to operate6H6NNaO6A Pb quantum dot; then preparing the calcium and the titanium in one stepIn the process of the ore film, the synthesized quantum dots are uniformly dispersed in the anti-solvent, so that the quantum dots are uniformly distributed in the perovskite film to realize the perovskite grain boundary passivation.
2. The method according to claim 1, characterized by comprising the steps of:
step 1: quantum dot synthesis
In the range of 0.1 to 0.2mmol C6H9NNa3O6Slowly adding 0.05-0.1 mmol Pb (CH) into the aqueous solution3COO)2Continuously stirring the solution for 1-2 h; further standing the mixed solution in air for 24-48 h, and then centrifuging, washing and drying the solution to obtain C6H6NNaO6Storing the Pb quantum dot powder material for later use;
step 2: perovskite grain boundary passivation
Depositing a wide band gap semiconductor material on a conductive glass substrate as an electron transport layer; preparing a perovskite absorption layer film by adopting a one-step method; in a glove box N2In the atmosphere, firstly, uniformly spin-coating 50-150 mL of perovskite precursor solution on an electron transport layer, wherein the spin-coating rotation speed is 3500-4500 rpm; then the C synthesized in the step 16H6NNaO6The method comprises the following steps of dispersing Pb quantum dots in an anti-solvent at a concentration of 0.5-20 wt%, dropwise adding the anti-solvent containing the quantum dots on a substrate when the perovskite precursor solution starts to spin for 6-10 s, and after the substrate is spin-coated for 20-30 s, placing the substrate on a heating table at 100-110 ℃ for annealing for 5-15 min to obtain a target perovskite thin film;
and step 3: perovskite cell preparation
And (3) further spin-coating a hole transport layer and evaporating a metal electrode on the perovskite thin film obtained in the step (2) according to a conventional method to finish the preparation of the perovskite battery.
3. The method of claim 2, wherein:
in step 2, the wide band gap semiconductor material is TiO2、SnO2ZnO or CdS.
4. The method of claim 3, wherein:
the wide band gap semiconductor material is TiO2Or SnO2。
5. The method of claim 2, wherein:
in step 2, the target perovskite thin film is CH3NH3PbI3、HC(NH2)2PbI3Or (Cs, MA, FA) PbI3。
6. The method of claim 2, wherein:
in the step 2, the concentration of the perovskite precursor solution is 0.5-1.5 g/mL.
7. The method of claim 2, wherein:
in the step 2, the anti-solvent is ethyl acetate, chlorobenzene or diethyl ether.
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