CN111092160B - Method for passivating lower interface of perovskite solar cell with inverse structure - Google Patents

Method for passivating lower interface of perovskite solar cell with inverse structure Download PDF

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CN111092160B
CN111092160B CN201911184871.2A CN201911184871A CN111092160B CN 111092160 B CN111092160 B CN 111092160B CN 201911184871 A CN201911184871 A CN 201911184871A CN 111092160 B CN111092160 B CN 111092160B
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CN111092160A (en
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姜辛
邱建航
王立鹏
王高翔
邰凯平
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Institute of Metal Research of CAS
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Abstract

The invention belongs to the field of photovoltaic device preparation, and particularly relates to a method for passivating a lower interface of an inverse structural perovskite solar cell. Evaporating a thin LiF layer on the NiO surface by adopting a thermal evaporation method, and carrying out heat treatment in a rapid annealing furnace to enable Li ions to diffuse into the NiO layer; evaporation of MgF film by electron beam evaporation2Carrying out heat treatment in a rapid annealing furnace to ensure that Mg ions are diffused into the film, thereby realizing the doping of the NiO film; after the thin film is spin-coated with the lead halide perovskite transmission layer, the lower interface of the perovskite solar cell with the inverse structure can be passivated; and (3) spin-coating a PCBM electron transport layer and a BCP passivation layer on the perovskite thin film, and evaporating a silver electrode to prepare the lower interface passivated inverse structure perovskite solar cell. Due to the regulation and control of the NiO work function and the conductivity by doping Li ions and Mg ions, the transmission efficiency of current carriers at the NiO/perovskite interface is improved, and the energy conversion efficiency of the battery is improved.

Description

Method for passivating lower interface of perovskite solar cell with inverse structure
Technical Field
The invention belongs to the field of photovoltaic device preparation, and particularly relates to a method for passivating a lower interface of an inverse structural perovskite solar cell.
Background
As a new generation of photovoltaic technology, part of performance indexes of perovskite solar cells approach or exceed that of traditional thin film photovoltaic cells such as amorphous silicon, cadmium telluride, copper indium gallium selenide and the like, and the perovskite solar cells have wide civil prospect and huge market value and are paid attention by researchers and industries in various countries. The perovskite solar cell takes a lead-calcium-titanium halide light absorption material as a core and is assisted by a transparent conductive layer, an electron transport layer, a hole transport layer and a metal counter electrode. In the working process of the cell, the lead-calcium-titanium halide material absorbs sunlight, and photoproduction electrons/holes are respectively injected into the electron/hole transport layer at the interface of the lead-calcium-titanium halide material and the electron/hole transport material, so that photoproduction electron-hole separation is completed. Through the rapid development in recent years, the research center of gravity in the field of perovskite solar cells has gradually shifted from thin film preparation and performance regulation to device interface modification. Recent studies indicate that the transmission loss of photogenerated carriers at the interface of the lead-perovskite halide material and the electron/hole transport material and the deterioration and inactivation of the perovskite material caused by interface defects are main reasons of the low photoelectric conversion efficiency and the poor stability of the cell. Therefore, the development of a novel method for interface passivation of the perovskite solar cell and the optimization of the interface performance of the perovskite material and the electron transport material have important significance for improving the performance of the perovskite solar cell.
Disclosure of Invention
Aiming at the problems of low conductivity of a NiO hole transport material, energy level mismatch at the interface between the NiO hole transport material and a perovskite material and the like in the conventional perovskite solar cell with an inverse structure, the invention aims to provide a method for passivating the lower interface of the perovskite solar cell with the inverse structure. The NiO hole transport layer/perovskite thin film prepared by the method effectively improves the interface energy level mismatch of NiO/perovskite due to the regulation and control effect of doping Li ions and Mg ions on the NiO work function and the conductivity, improves the transport efficiency of current carriers at the NiO/perovskite interface, and improves the energy conversion efficiency of a battery.
The technical scheme of the invention is as follows:
a method of passivating an interface below an inverted structure perovskite solar cell, comprising the steps of:
(1) preparing a LiF ultrathin film and carrying out heat treatment: depositing a LiF film with the thickness of 0.5-5 nm on the FTO conductive film substrate coated with the NiO film by adopting a thermal evaporation method, wherein the vacuum degree of equipment is 1 multiplied by 10 during evaporation-3～1×10-4Pa, continuously annealing for 1-5 minutes in a rapid annealing furnace under the conditions of high temperature and low temperature, wherein the temperature range of a low-temperature area is 100-200 ℃, the temperature range of a high-temperature area is 500-600 ℃, the heating rate of the rapid annealing furnace is 50-200 ℃/s, the cooling rate is 50-200 ℃/min, and the annealing atmosphere is nitrogen;
(2)MgF2preparing an ultrathin film and carrying out heat treatment: depositing MgF with the thickness of 0.5-5 nm on the film obtained in the step (1) by adopting electron beam evaporation2Film, vacuum degree of equipment is 1X 10 during evaporation-2～1×10-4Pa, continuously annealing for 1-10 minutes in a rapid annealing furnace under the conditions of high temperature and low temperature, wherein the temperature range of a low-temperature region is 200-300 ℃, the temperature range of a high-temperature region is 400-600 ℃, the heating rate of the rapid annealing furnace is 100-200 ℃/s, the cooling rate is 50-200 ℃/min, and the annealing atmosphere is nitrogen;
(3) passivating the lower interface of the perovskite solar cell with the inverse structure: and (3) dropwise adding the perovskite solution on the film substrate obtained in the step (2), standing for 5-30 seconds, starting a spin coater, spin-coating at the revolution speed of 3000-6000 rpm for 20-60 seconds, taking an anti-polar solvent to wash the surface of the rotating substrate at one time after the spin coater reaches the specified revolution speed for 5-30 seconds, then placing the substrate on a hot plate furnace, baking for 2-60 minutes at the temperature of 80-150 ℃, taking down the substrate, and cooling to room temperature, namely, completing passivation of the lower interface of the NiO hole transport layer/perovskite while preparing the perovskite film.
The method for passivating the lower interface of the inverted perovskite solar cell comprises the steps of (1) preparing a LiF ultrathin film and before heat treatment, preparing a NiO colloidal solution, namely weighing 0.5-2 mmol of nickel acetate to dissolve in 5-20 mL of isopropanol, then adding 0.5-2 mmol of ethanolamine, and stirring at 60-80 ℃ for 10-15 hours.
The method for passivating the lower interface of the perovskite solar cell with the inverse structure comprises the steps of (1) preparing the LiF ultrathin film and carrying out heat treatment, spin-coating NiO colloidal solution on the FTO conductive film, wherein the rotation speed of a spin-coating machine is 1500-2000 rpm, the spin-coating time is 20-40 seconds, annealing is carried out at 200-300 ℃ for 0.5-2 hours, and the thickness of the obtained NiO film is 10-200 nm.
According to the method for passivating the lower interface of the inverse perovskite solar cell, in the step (3), when the lower interface of the inverse perovskite solar cell is passivated, the reversed-polarity solvent is diethyl ether or chlorobenzene, and the thickness of the perovskite thin film is 200-1000 nm.
According to the method for passivating the lower interface of the inverse perovskite solar cell, in the preparation of the inverse perovskite solar cell, a PCBM electron transport layer and a BCP passivation layer are spin-coated on a perovskite thin film, and a silver electrode is evaporated to prepare the inverse perovskite solar cell with the passivated lower interface.
The method for passivating the lower interface of the inverse perovskite solar cell comprises the following specific preparation steps of:
(1) spin-coating a PCBM solution on the perovskite thin film, wherein the mass concentration of the solution is 1-5 wt%, the solvent is chlorobenzene, the rotation speed of a spin-coating machine is 1000-3000 rpm, the time is 30-60 seconds, and then baking the solution on a hot plate furnace at the temperature of 80-120 ℃ for 20-40 minutes to obtain the PCBM thin film with the thickness of 50-500 nm;
(2) spin-coating a BCP solution on the PCBM film, wherein the concentration of the solution is 0.05-0.2 wt%, the rotating speed of a spin-coating machine is 4000-6000 rpm, and the time is 20-40 seconds;
(3) and (3) evaporating a silver electrode with the thickness of 50-100 nm on the BCP film by adopting a thermal method process, thus preparing the inverted-structure perovskite solar cell with passivated lower interface.
The design idea of the invention is as follows:
according to the invention, the rapid annealing method is introduced into the doping preparation of the NiO film, so that the rapid and efficient diffusion of low-valence ions such as Li and Mg in the NiO film is realized, and the conductivity and work function of the NiO film are regulated and controlled. The rapidly annealed Li/Mg-doped NiO film is taken as a hole transport layer, a perovskite film, a PCBM electron transport layer and a BCP passivation layer are spin-coated on the hole transport layer, and a silver electrode is evaporated to prepare the perovskite solar cell with the lower interface passivation and the inverse structure. In the device, due to the regulation and control effect of Li ion and Mg ion doping on the NiO work function and the conductivity, the mismatching of the NiO hole transport layer/perovskite interface energy level is effectively improved, the transport efficiency of current carriers in the NiO hole transport layer/perovskite interface and the NiO layer is improved, and the energy conversion efficiency of the battery is improved.
The invention has the following advantages and beneficial effects:
1. according to the passivation method of the lower interface of the inverted perovskite solar cell, the prepared device effectively improves the interface energy level mismatch of NiO/perovskite due to the regulation and control effect of doping of Li ions and Mg ions on the work function and the conductivity of NiO, the transmission efficiency of current carriers in the NiO/perovskite interface and the NiO layer is improved, and the energy conversion efficiency of the cell is improved.
2. The technological process of the invention is simple to operate and is beneficial to industrial popularization.
Drawings
FIG. 1: the cross-sectional scanning electron microscope (a), the ultraviolet electron energy spectrum (b), the fluorescence spectrum (c) and the photocurrent-voltage curve (d) of the device of the perovskite solar cell with the lower interface passivation inverse structure prepared in example 1.
(a) In the figure, Ag is a silver element layer, PCBM/BCP is [6,6 ]]-phenyl-C61-methyl butyrate and 2, 9-dimethyl-4, 7-diphenyl-1, 10-phenanthroline composite layer, Perovskite is Perovskite, Li/Mg, NiO is a NiO film doped with Li and Mg ions, and FTO is a fluorine-doped tin dioxide layer; (b) in the figure, the abscissa Binding Energy (eV) represents Binding Energy (electron volts), the ordinate Normalized Intensity represents Normalized Intensity (a.u.), and WfNiO is the Fermi level of the Li/Mg ion doped NiO film, WfNiO is the Fermi level of the undoped NiO film; (c) in the figure, the abscissa wavelet (nm) represents the wavelength (nanometer), the ordinate Intensity (a.u.) represents the Intensity, FTO-NiO-Perovskite represents the fluorescence Intensity of an unmodified NiO hole transport layer/Perovskite thin film, and FTO-Li/Mg NiO-Perovskite represents the fluorescence Intensity of a Li/Mg ion doped NiO hole transport layer/Perovskite thin film; (d) in the figure, the abscissa Voltage (V) represents voltage (V) and the ordinate Current Density (mA · cm)-2) Represents the current density (milliamps/square centimeter).
Detailed Description
In the specific implementation process, a NiO hole transport layer is spin-coated on the FTO conductive film and is subjected to heat treatment; evaporating a thin LiF layer on the NiO surface by adopting a thermal evaporation method, and carrying out heat treatment in a rapid annealing furnace to enable Li ions to be diffused into the NiO layer; evaporation of MgF film by electron beam evaporation2Carrying out heat treatment in a rapid annealing furnace to diffuse Mg into the film, thereby realizing the doping of the NiO surface; after the halogenated lead perovskite transport layer is prepared on the film by spin coating, the lower interface (NiO hole transport layer/perovskite interface) of the perovskite solar cell with the inverse structure can be realized) The passivation method specifically comprises the following steps:
(1) preparing a LiF ultrathin film and carrying out heat treatment: depositing a LiF film with the thickness of 0.5-5 nm on the FTO conductive film substrate coated with the NiO film by adopting a thermal evaporation method, wherein the vacuum degree of equipment is 1 multiplied by 10 during evaporation-3～1×10-4Pa, continuously annealing for 1-5 minutes in a rapid annealing furnace under the conditions of high temperature and low temperature, wherein the temperature range of a low-temperature area is 100-200 ℃, the temperature range of a high-temperature area is 500-600 ℃, the heating rate of the rapid annealing furnace is 50-200 ℃/s, the cooling rate is 50-200 ℃/min, and the annealing atmosphere is nitrogen; wherein the continuous annealing under the high and low temperature conditions has the function of enabling Li ions to diffuse into the NiO film.
(2)MgF2Preparing an ultrathin film and carrying out heat treatment: depositing MgF with the thickness of 0.5-5 nm on the film obtained in the step (1) by adopting electron beam evaporation2Film, vacuum degree of equipment is 1X 10 during evaporation-2～1×10-4Pa, continuously annealing for 1-10 minutes in a rapid annealing furnace under the conditions of high temperature and low temperature, wherein the temperature range of a low-temperature region is 200-300 ℃, the temperature range of a high-temperature region is 400-600 ℃, the heating rate of the rapid annealing furnace is 100-200 ℃/s, the cooling rate is 50-200 ℃/min, and the annealing atmosphere is nitrogen; wherein the continuous annealing under the high and low temperature conditions has the function of enabling Mg ions to diffuse into the NiO film.
(3) Passivating the lower interface of the perovskite solar cell with the inverse structure: and (3) dropwise adding the perovskite solution on the film substrate obtained in the step (2), standing for 5-30 seconds, starting a spin coater, spin-coating at the revolution speed of 3000-6000 rpm for 20-60 seconds, taking 0.5-20 mL of reverse polarity solvent after the spin coater reaches the specified revolution speed for 5-30 seconds, washing the surface of the rotary substrate at one time, then placing the substrate on a hot plate furnace, baking for 2-60 minutes at the temperature of 80-150 ℃, taking down the substrate, and cooling to room temperature, so that passivation of the lower interface of the NiO hole transport layer/perovskite can be completed while the perovskite film is prepared.
And (3) spin-coating a PCBM electron transport layer and a BCP passivation layer on the perovskite thin film, and evaporating a silver electrode to prepare the lower interface passivated inverse structure perovskite solar cell.
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
In this embodiment, the method for passivating the lower interface of the perovskite solar cell with the inverse structure is as follows:
(1) firstly preparing NiO colloidal solution, namely weighing 1mmol of Ni (Ac)2·4H2Nickel O acetate was dissolved in 10mL of isopropanol, and 1mmol of ethanolamine was added thereto, followed by stirring at 70 ℃ for 12 hours.
(2) Thereafter, MAPbI is configured3Perovskite precursor solution, namely weighing Methyl Amine Iodide (MAI) and lead iodide (PbI) with the same molar mass2) Raw materials, dissolving in dimethyl formamide (DMF) and dimethyl sulfoxide (DMSO) in a volume ratio of 1: 1, MAI and PbI2The molar concentrations of the perovskite ions were 1.6M, respectively, and the perovskite solution was stirred at room temperature for 2 hours to form a uniform, stable and transparent perovskite solution.
(3) NiO colloid solution was spin-coated on the cleaned FTO conductive film (length. times. width. times. thickness. 1.5 cm. times.1.1 mm), the spin coater rotation speed was 1800rpm, the spin coating time was 30 seconds, annealing was performed at 250 ℃ for 1 hour, and the thickness of the NiO film was about 50 nm. Depositing LiF film with thickness of 0.5nm on FTO conductive film substrate coated with NiO film by thermal evaporation method, wherein vacuum degree of the device is 1 × 10-3Pa, then continuously annealing in a rapid annealing furnace under the conditions of high temperature and low temperature, wherein the low-temperature annealing temperature is 150 ℃, the time is 2 minutes, the high-temperature annealing temperature is 550 ℃, the annealing time is 2 minutes, the temperature rise rate of the rapid annealing furnace is 100 ℃/s, the temperature reduction rate is 200 ℃/min, and the annealing atmosphere is nitrogen. Then, electron beam evaporation equipment is adopted to evaporate MgF with the thickness of 0.5nm2Ultra-thin film, vacuum degree of the equipment is 1 x 10 during evaporation-2Pa, then continuously annealing at high and low temperatures in a rapid annealing furnace, wherein the low-temperature annealing temperature is 250 ℃, the time is 2 minutes, the high-temperature annealing temperature is 550 ℃, the annealing time is 2 minutes, the heating rate of the rapid annealing furnace is 100 ℃/s, the cooling rate is 200 ℃/min, the annealing atmosphere is nitrogen, and the doping of Li and Mg ions to the NiO film is completed.
(4) Dropping the perovskite solution on the surface of the Li and Mg ion doped NiO film, standing for 5 seconds, starting a spin coater, spin-coating at the revolution of 4500rpm for 30 seconds, taking 0.5mL of ether solvent after the spin coater reaches the specified revolution for 5 seconds, washing the surface of the rotating substrate at one time, then placing the substrate on a hot plate furnace, baking at 100 ℃ for 5 minutes, taking down the substrate, and cooling to room temperature, thus completing the passivation of the NiO hole transport layer/perovskite lower interface while preparing the perovskite film, wherein the thickness of the perovskite film is about 400 nm.
(5) And then spin-coating PCBM solution on the perovskite thin film, wherein the mass concentration of the solution is 2 wt%, the solvent is chlorobenzene, the rotation speed of a spin-coating machine is 2000rpm, the time is 40 seconds, and then baking is carried out on a hot plate furnace at 100 ℃ for 30 minutes to obtain the PCBM thin film with the thickness of about 150 nm. BCP solution is spin-coated on the PCBM film, the concentration of the solution is 0.1 wt%, the rotation speed of a spin coater is 5000rpm, and the time is 30 seconds. And (3) evaporating a silver electrode with the thickness of 50-100 nm on the BCP film by adopting a thermal method process to prepare the inverted-structure perovskite solar cell with the passivated lower interface.
As shown in FIG. 1, the cross-section scanning electron microscope image, the fluorescence spectrum of the perovskite thin film and the photocurrent-voltage curve of the device of the perovskite solar cell with the lower interface passivation inverted structure prepared by the process flow are shown. As shown in FIG. 1a, the Li and Mg ion doped NiO film is positioned at the lower layer of the device, and at the NiO hole transport layer/perovskite interface, the interface energy level mismatch is improved due to the doping effect of Li and Mg ions. Ultraviolet Photoelectron Spectroscopy (UPS) analyzed the surface that the fermi level of the Li/Mg ion doped NiO film was 0.15eV lower than that of the undoped NiO film (fig. 1 b). Fluorescence analysis results show that the interface under the Li/Mg ion doped NiO hole transport layer/perovskite can efficiently separate photo-generated electron hole pairs, and the fluorescence intensity of the perovskite film is reduced and is far lower than that of the NiO hole transport layer/MAPbI with an unmodified interface3Film (fig. 1 c). The photocurrent-voltage curve of the cell under the AM 1.5G condition shows that the photoelectric conversion efficiency of the inverted-structure perovskite cell with passivated lower interface is improved by 10% to about 18% compared with the unpassivated device (fig. 1 d).
The embodiment result shows that in the perovskite solar cell with the inverted structure and the passivated lower interface, the Li ions and the Mg ions are doped to regulate and control the work function and the conductivity of NiO, so that the transmission efficiency of carriers at the NiO/perovskite interface is improved, and the energy conversion efficiency of the cell is improved.

Claims (6)

1. A method for passivating the lower interface of an inverse perovskite solar cell is characterized by comprising the following steps:
(1) preparing a LiF ultrathin film and carrying out heat treatment: depositing a LiF film with the thickness of 0.5-5 nm on the FTO conductive film substrate coated with the NiO film by adopting a thermal evaporation method, wherein the vacuum degree of equipment is 1 multiplied by 10 during evaporation-3～1×10-4Pa, continuously annealing for 1-5 minutes in a rapid annealing furnace under the conditions of high temperature and low temperature, wherein the temperature range of a low-temperature area is 100-200 ℃, the temperature range of a high-temperature area is 500-600 ℃, the heating rate of the rapid annealing furnace is 50-200 ℃/s, the cooling rate is 50-200 ℃/min, and the annealing atmosphere is nitrogen;
(2)MgF2preparing an ultrathin film and carrying out heat treatment: depositing MgF with the thickness of 0.5-5 nm on the film obtained in the step (1) by adopting electron beam evaporation2Film, vacuum degree of equipment is 1X 10 during evaporation-2～1×10-4Pa, continuously annealing for 1-10 minutes in a rapid annealing furnace under the conditions of high temperature and low temperature, wherein the temperature range of a low-temperature region is 200-300 ℃, the temperature range of a high-temperature region is 400-600 ℃, the heating rate of the rapid annealing furnace is 100-200 ℃/s, the cooling rate is 50-200 ℃/min, and the annealing atmosphere is nitrogen;
(3) passivating the lower interface of the perovskite solar cell with the inverse structure: and (3) dropwise adding the perovskite solution on the film substrate obtained in the step (2), standing for 5-30 seconds, starting a spin coater, spin-coating at the revolution speed of 3000-6000 rpm for 20-60 seconds, taking an anti-polar solvent to wash the surface of the rotating substrate at one time after the spin coater reaches the specified revolution speed for 5-30 seconds, then placing the substrate on a hot plate furnace, baking for 2-60 minutes at the temperature of 80-150 ℃, taking down the substrate, and cooling to room temperature, namely, completing passivation of the lower interface of the NiO hole transport layer/perovskite while preparing the perovskite film.
2. The method for passivating the lower interface of the inverted perovskite solar cell according to claim 1, wherein a NiO colloid solution is prepared before the preparation and the heat treatment of the LiF ultrathin film in the step (1), namely 0.5-2 mmol of nickel acetate is weighed and dissolved in 5-20 mL of isopropanol, then 0.5-2 mmol of ethanolamine is added, and the mixture is stirred for 10-15 hours at the temperature of 60-80 ℃.
3. The method for passivating the lower interface of the inverted perovskite solar cell according to claim 1, wherein during the preparation and heat treatment of the LiF ultrathin film in the step (1), NiO colloid solution is spin-coated on the FTO conductive film, the rotation speed of a spin coater is 1500-2000 rpm, the spin coating time is 20-40 seconds, and the NiO film is obtained by annealing at 200-300 ℃ for 0.5-2 hours, wherein the thickness of the NiO film is 10-200 nm.
4. The method for passivating the lower interface of the inverted perovskite solar cell according to claim 1, wherein in the step (3), during passivation of the lower interface of the inverted perovskite solar cell, the reversed-polarity solvent is diethyl ether or chlorobenzene, and the thickness of the perovskite thin film is 200-1000 nm.
5. A method for passivating the lower interface of an inverse perovskite solar cell according to claim 1, wherein in the preparation of the inverse perovskite solar cell, the PCBM electron transport layer and the BCP passivation layer are spin-coated on the perovskite thin film, and the silver electrode is evaporated to prepare the inverse perovskite solar cell with passivated lower interface.
6. A method of passivating the lower interface of an inverse perovskite solar cell according to claim 5, wherein the inverse perovskite solar cell is prepared by the following steps:
(1) spin-coating a PCBM solution on the perovskite thin film, wherein the mass concentration of the solution is 1-5 wt%, the solvent is chlorobenzene, the rotation speed of a spin-coating machine is 1000-3000 rpm, the time is 30-60 seconds, and then baking the solution on a hot plate furnace at the temperature of 80-120 ℃ for 20-40 minutes to obtain the PCBM thin film with the thickness of 50-500 nm;
(2) spin-coating a BCP solution on the PCBM film, wherein the concentration of the solution is 0.05-0.2 wt%, the rotating speed of a spin-coating machine is 4000-6000 rpm, and the time is 20-40 seconds;
(3) and (3) evaporating a silver electrode with the thickness of 50-100 nm on the BCP film by adopting a thermal method process, thus preparing the inverted-structure perovskite solar cell with passivated lower interface.
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