CN111697141A - Preparation method of silver electrode perovskite solar cell - Google Patents
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Abstract
The invention discloses a preparation method of a silver electrode perovskite solar cell, and belongs to the technical field of solar cells. The method comprises the following steps: step (1), FTO substrate treatment: carrying out ultrasonic cleaning and drying on the FTO substrate, and then attaching a high-temperature adhesive tape to the treated FTO substrate; step (2), solvent preparation: SnCl with the concentration of 0.1mol/mL is prepared by using tin dichloride solid and absolute ethyl alcohol2·2H2O solution; PbI with a concentration of 691.25mg/mol was formulated from N, N-dimethylformamide, dimethyl sulfoxide and lead iodide powder2A solution; the organic ionic solution was prepared from formamidine hydroiodide, methyl amine chloride, methyl amine bromide and isopropanol. Junction of solar cell prepared in the present inventionFormed as FTO substrate/SnO2The silver electrode perovskite solar cell comprises a thin film layer, a perovskite layer, a Spiro-OMeTAD thin film layer and Ag, wherein silver is used as a top electrode to bring good conductivity, and an organic substance Spiro-OMeTAD is used as a hole transport layer material to bring a high filling factor, so that the performance of the silver electrode perovskite solar cell is more stable.
Description
Technical Field
The invention relates to the technical field of solar cells, in particular to a preparation method of a silver electrode perovskite solar cell.
Background
Along with the development of human society, the demand of human beings for energy is increasing, and the most used fossil energy at present belongs to non-renewable energy, so that the fossil energy available on the earth is remained a few times. Meanwhile, since the large use of fossil energy has caused extremely serious environmental problems such as serious atmospheric pollution, global warming, etc., which have raised a significant challenge to the survival of all the living things on the earth.
Solar energy, as a green, clean and renewable energy source, has the advantages of abundant reserves, easy acquisition, low cost and the like, so that the solar energy becomes an excellent alternative energy source. The solar cell is a carrier for directly converting light energy into electric energy, scientists make many advances from the earliest research of silicon cells and use the advances in the space field, but due to the bottleneck of the current development of the silicon cells, the defects of energy consumption of cell preparation, serious environmental pollution of byproducts and the like cannot be solved in time to limit the development of the industry. Therefore, scientists have searched for alternative materials and new structures, and the development time of solar cells developed based on dye-sensitized cells is as short as ten years, but the development speed is very fast. The performance of each aspect is continuously optimized and the efficiency is continuously improved in a short time, the photoelectric conversion efficiency reaches 24.2%, but the performance of the solar cell is not stable enough.
Disclosure of Invention
In order to make the solar cell more stable, the embodiment of the invention provides a preparation method of a silver electrode perovskite solar cell. The method comprises the following steps:
step (1), FTO substrate treatment: carrying out ultrasonic cleaning and drying on the FTO substrate, and then attaching a high-temperature adhesive tape to the treated FTO substrate;
step (2), solvent preparation: SnCl with the concentration of 0.1mol/mL is prepared by using tin dichloride solid and absolute ethyl alcohol2·2H2O solution; PbI with a concentration of 691.25mg/mol was formulated from N, N-dimethylformamide, dimethyl sulfoxide and lead iodide powder2A solution; by means of formamidine hydroiodidePreparing organic ionic solution from methyl amine chloride, methyl amine bromide and isopropanol; preparing a Spiro-OMeTAD solution by using Spiro-OMeTAD solid and chlorobenzene;
step (3), preparing each functional layer by the prepared solvent: putting the treated FTO substrate into a preheated ultraviolet ozone processor for treatment for 20min, and spin-coating the SnCl after treatment2·2H2Preparation of SnO from O solution2A thin film layer; then the SnO is put2Treating the film layer in an ultraviolet ozone machine for 20min to remove surface groups and increase the surface wettability, and spin-coating the PbI after treatment2Preparing a perovskite layer from the solution and the organic ion solution; spin-coating the Spiro-OMeTAD solution on the perovskite layer to prepare a Spiro-OMeTAD thin film layer;
step (4), preparing the silver electrode perovskite solar cell: and after the preparation of each functional layer is finished, transferring the functional layers into a cavity of a metal vacuum evaporation plating instrument to perform Ag electrode evaporation plating by adopting a vacuum thermal evaporation deposition method, and finally obtaining the silver electrode perovskite solar cell.
Further, the PbI in the step (2)2The preparation method of the solution comprises the following steps: weighing 691.25mg of lead iodide powder in a No. 1 glass bottle by using an analytical balance, respectively taking 0.9mL of N, N-dimethylformamide and 0.1mL of dimethyl sulfoxide by using a liquid transfer gun according to the volume ratio of 9: 1, injecting the obtained mixture into the No. 1 glass bottle, putting magnetons into the glass bottle, screwing the bottle cap, sticking a label, stirring the obtained product for 1d at 70-85 ℃ on a magnetic rotary heating table, filtering the obtained product by using a 0.22 mu m organic filter tip, and heating the obtained product at 80 ℃ to obtain the PbI2And (3) solution.
Further, the preparation method of the organic ion solution in the step (2) comprises the following steps: respectively taking 90mg of formamidine hydroiodide with the concentration of 90mg/ml, 6.39mg of methyl ammonium chloride with the concentration of 6.39mg/ml and 9mg of methyl ammonium bromide with the concentration of 9mg/ml in a No. 2 glass bottle by using an analytical balance, then taking the isopropanol in the No. 2 glass bottle by using a liquid transfer gun, putting magnetons in the glass bottle, stirring the glass bottle for one day in a magnetic rotary heating table at normal temperature, and filtering the solution to obtain the organic ion solution.
Further, the preparation method of the Spiro-OMeTAD solution in the step (2) comprises the following steps: and (3) taking 72.5mg of the Spiro-OMeTAD solid by using an analytical balance, taking 1mL of chlorobenzene by using a pipette in a No. 3 glass bottle, adding magnetons, stirring for 1h on a magnetic rotary heating table at normal temperature until the chlorobenzene is clear, then adding 17.5 muL of lithium salt solution with the concentration of 520mg/mI dissolved in acetonitrile and 28.8 muL of 4-tert-butylpyridine solution in the No. 3 glass bottle, stirring for 1d at normal temperature in the dark place, and filtering to obtain the Spiro-OMeTAD solution.
Further, the specific preparation method of each functional layer comprises the following steps: taking a proper amount of SnCl2·2H2Dripping O solution at the center of the conductive surface of the FTO substrate, carrying out spin coating at 3000rpm/min for 30s, and annealing at 180 ℃ for 1h after the spin coating is finished, so that the O solution is hydrolyzed to become the SnO2A thin film layer;
taking a proper amount of PbI by using a liquid-transferring gun2The SnO is fully paved by solution2Performing two-stage spin coating process on the thin film layer, spreading the solution at a low rotation speed of 800rpm/min for 5s at the front stage, forming the film at a high speed of 3000rpm/min for 30s at the rear stage, and depositing to obtain PbI2A film; mixing the PbI2The film is placed on a hot table to be annealed at 70 ℃ for 1min, the organic ion solution is spin-coated through the two-stage spin coating process after annealing, and then the film is placed on the hot table to be annealed at 150 ℃ for 20min, and finally the perovskite layer is obtained;
and after the perovskite layer is cooled, spin-coating the Spiro-OMeTAD solution by adopting the two-stage spin-coating process, annealing for 20min at 100 ℃ after the spin-coating is finished, and evaporating the solvent to obtain the Spiro-OMeTAD film layer.
Further, the film thickness of the evaporated Ag electrode was 100 nm.
The technical scheme provided by the embodiment of the invention has the following beneficial effects: the solar cell prepared by the invention has the structure of FTO substrate/SnO2The silver electrode perovskite solar cell comprises a thin film layer, a perovskite layer, a Spiro-OMeTAD thin film layer and Ag, wherein silver is used as a top electrode to bring good conductivity, and an organic substance Spiro-OMeTAD is used as a hole transport layer material to bring a high filling factor, so that the performance of the silver electrode perovskite solar cell is more stable.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a silver electrode perovskite solar cell provided by the invention;
FIG. 2 is a schematic view of the structure of an FTO substrate provided by the present invention;
fig. 3 is a dark current test chart of the silver electrode perovskite solar cell provided by the invention and a traditional solar cell.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example one
A preparation method of a silver electrode perovskite solar cell comprises the following steps:
step (1), FTO substrate treatment: carrying out ultrasonic cleaning and drying on the FTO substrate, and then attaching a high-temperature adhesive tape to the treated FTO substrate;
step (2), solvent preparation: SnCl with the concentration of 0.1mol/mL is prepared by using tin dichloride solid and absolute ethyl alcohol2·2H2O solution; PbI with a concentration of 691.25mg/mol was formulated from N, N-dimethylformamide, dimethyl sulfoxide and lead iodide powder2A solution; preparing an organic ionic solution by formamidine hydroiodide, methyl amine chloride, methyl amine bromide and isopropanol; preparing a Spiro-OMeTAD solution by using Spiro-OMeTAD solid and chlorobenzene;
step (3), preparing each functional layer by the prepared solvent: putting the treated FTO substrate into a preheated ultraviolet ozone processor for treatment for 20min, and spin-coating SnCl after treatment2·2H2Preparation of SnO from O solution2A thin film layer; then SnO2Treating the film layer in an ultraviolet ozone machine for 20min to remove surface groups and increase the surface wettability, and spin-coating PbI after treatment2Preparing a perovskite layer by using the solution and the organic ion solution; spin-coating a Spiro-OMeTAD solution on the perovskite layer to prepare a Spiro-OMeTAD thin film layer;
step (4), preparing the silver electrode perovskite solar cell: and after the preparation of each functional layer is finished, transferring the functional layers into a cavity of a metal vacuum evaporation plating instrument to perform Ag electrode evaporation plating by adopting a vacuum thermal evaporation deposition method, and finally obtaining the silver electrode perovskite solar cell.
In the present invention, fluorine-doped tin oxide (FTO) is used as the bottom electrode substrate. The FTO substrate is purchased from Liaoning preferred energy technology Co., Ltd, the size of the FTO substrate is 20mm multiplied by 20mm, the conductive film is distributed on the substrate as shown in figure 2 after laser etching, and the blank part is the conductive film.
Example two
A preparation method of a silver electrode perovskite solar cell comprises the following steps:
step (1): FTO substrate treatment
Firstly, numbering an FTO substrate by using a metal nicking tool, placing the FTO substrate into a culture dish, pouring a proper amount of deionized water into the culture dish to immerse the FTO substrate, wiping off large particles visible to the naked eye on the surface by using a cotton swab, and placing the cleaned FTO substrate into a crystallization dish containing deionized water to immerse;
then, pouring the deionized water in the crystallization dish, pouring the deionized water, cleaning in an ultrasonic cleaning machine for 20min, pouring the deionized water, pouring acetone, cleaning in the ultrasonic cleaning machine for 20min, pouring the acetone into a recovery barrel, rinsing with the deionized water once, pouring the deionized water again, cleaning in the ultrasonic cleaning machine for 20min, pouring the deionized water, pouring isopropanol, and cleaning in the ultrasonic cleaning machine for 20 min;
and finally, pouring isopropanol into a recycling bin, putting the crystallization vessel with the FTO substrate into a drying oven, adjusting the temperature to 80 ℃ for drying, and attaching a high-temperature adhesive tape to the treated FTO substrate.
Step (2): solvent preparation
First, SnCl with the concentration of 0.1mol/mL is prepared by using tin dichloride solid and absolute ethyl alcohol2·2H2And (4) O solution.
Secondly, 691.25mg of lead iodide powder is weighed by an analytical balance and put in a No. 1 glass bottle, 0.9mLN, N-dimethylformamide and 0.1mL of dimethyl sulfoxide are respectively taken by a pipette gun with the volume ratio of 9: 1 and then poured into the No. 1 glass bottle, magnetons are put in the glass bottle, the bottle cap is screwed up, a label is pasted, the mixture is stirred for 1d at 70-85 ℃ on a magnetic rotary heating table, filtered by a 0.22 mu m organic filter tip and then heated at 80 ℃ to obtain PbI2And (3) solution.
Then, 90mg of formamidine hydroiodide with a concentration of 90mg/ml, 6.39mg of methylammonium chloride with a concentration of 6.39mg/ml and 9mg of methylammonium bromide with a concentration of 9mg/ml were taken out from a No. 2 glass bottle by an analytical balance, isopropanol was taken out from the No. 2 glass bottle by a pipette gun, magnetons were put in the glass bottle, and the glass bottle was stirred for one day in a state of a magnetic rotary heating table at normal temperature, and an organic ion solution was obtained after filtration.
Finally, 72.5mg of Spiro-OMeTAD solid is taken out by an analytical balance and put into a No. 3 glass bottle, 1mL of chlorobenzene is taken out by a pipette and put into the No. 3 glass bottle, magnetons are added, the mixture is stirred for 1h at normal temperature on a magnetic rotary heating table until the mixture is clear, 17.5 muL of lithium salt solution with the concentration of 520mg/mL dissolved in acetonitrile and 28.8 muL of 4-tert-butylpyridine solution are added into the No. 3 glass bottle, and the mixture is stirred for 1d at normal temperature in the dark to obtain Spiro-OMeTAD solution after filtering.
And (3): preparation of the functional layers by means of the prepared solvents
Firstly, taking a proper amount of SnCl2·2H2Dripping O solution at the center of the conductive surface of the FTO substrate, performing spin coating at 3000rpm/min for 30s, and annealing at 180 ℃ for 1h after the spin coating is finished to hydrolyze the O solution into SnO2A thin film layer.
Then, a proper amount of PbI is taken out by a liquid-transfering gun2SnO is fully spread in solution2Film layer ofTwo-stage spin coating process, wherein the solution is spread at a low rotation speed of 800rpm/min for 5s at the front stage, and is formed at a high speed of 3000rpm/min for 30s at the rear stage, and PbI is obtained by deposition2A film; will PbI2And (3) annealing the film on a hot table at 70 ℃ for 1min, spin-coating an organic ion solution by a two-stage spin coating process after annealing, and then annealing the film on the hot table at 150 ℃ for 20min to finally obtain the perovskite layer.
And finally, after the perovskite layer is cooled, spin-coating a Spiro-OMeTAD solution by adopting a two-stage spin-coating process, annealing for 20min at 100 ℃ after the spin-coating is finished, and evaporating the solvent to obtain the Spiro-OMeTAD film layer.
And (4): preparation of silver electrode perovskite solar cell
Firstly, after the preparation of each functional layer is finished, transferring the functional layers into a cavity of a metal vacuum evaporation instrument, opening condensed water, confirming that an air release valve is closed, and starting a main power supply of equipment and a power supply of a vacuum gauge;
then, starting the mechanical pump, opening the side angle-pumping valve in the counterclockwise direction, starting the vacuum pump, closing the side angle-pumping valve after the air pressure is lower than 10Pa, starting the front-stage valve button, closing the gate valve after 30s, starting the molecular pump after the air pressure is lower than 20Pa, and changing the air pressure to 5 × 10-4Pa; selecting a corresponding heating source switch, and turning on a film thickness meter switch; slowly adjust current to target current: 5080mA, opening an evaporation source baffle after pre-evaporation for 10s, starting evaporation, simultaneously observing the reading on a film thickness meter, and closing the baffle;
finally, after the evaporation is finished, reducing the current to 0, and turning off an evaporation power supply; closing the gate valve clockwise, and closing the power supply of the molecular pump after the speed of the molecular pump is reduced to 0; closing the front-stage valve clockwise, then closing the mechanical pump, and closing the vacuum gauge; slowly opening an inflation valve (nitrogen), then opening a vacuum gauge, and closing the inflation valve when the air pressure is 1.0 multiplied by 105 Pa; and opening the cover and taking away the sample, pumping the coating machine to 50Pa, closing the front-stage valve, the mechanical pump and the main power supply, and closing the condensed water.
Further, the film thickness of the deposited Ag electrode was 100 nm.
It should be noted that, workers have performed dark current tests on the silver electrode perovskite solar cell, the core part of the solar cell is a P-N junction, and under a dark state condition, the solar cell still generates current under the action of external voltage, and the current is called dark current (ID), and is also called reverse saturation current, layer leakage current or body leakage current. The ID is one of important means for representing the performance of the solar cell, the numerical value of the ID is closely related to the charge transport process in the cell, and the number of crystal defects, impurity ions, surface trap states and recombination centers in the solar cell is reflected. In the case of a solar cell, recombination behavior caused by these defects has a large influence on the energy conversion efficiency and performance of the solar cell, and thus, for a solar device, the smaller the ID value, the more excellent the performance of the device.
To compare a conventional solar cell with the silver electrode perovskite solar cell, experimenters measured the ID of both groups of solar cells. As shown in fig. 3 (a represents the conventional solar cell, and B represents the silver electrode perovskite solar cell), the conventional solar cell has the minimum value of the ID at-0.5V, while the curve of the silver electrode perovskite solar cell is in a right-shift trend, the voltage value corresponding to the minimum value of the ID is also right-shifted, and it can be clearly seen that the ID of the silver electrode perovskite solar cell is reduced compared with that of the conventional solar cell. Compared with the traditional solar cell, the silver electrode perovskite solar cell has the advantages that the surface defect states are reduced, and the performance of the cell is improved.
It is worth to say that the solar cell prepared by the method is structurally characterized by comprising an FTO substrate, a SnO2 thin film layer, a perovskite layer, a Spiro-OMeTAD thin film layer and Ag, silver serving as a top electrode can bring good conductivity, and organic matter Spiro-OMeTAD serving as a hole transport layer material can bring high filling factors, so that the perovskite solar cell with the silver electrode is more stable in performance.
The above-mentioned serial numbers of the embodiments of the present invention are merely for description and do not represent the merits of the embodiments.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. A preparation method of a silver electrode perovskite solar cell is characterized by comprising the following steps:
step (1), FTO substrate treatment: carrying out ultrasonic cleaning and drying on the FTO substrate, and then attaching a high-temperature adhesive tape to the treated FTO substrate;
step (2), solvent preparation: SnCl with the concentration of 0.1mol/mL is prepared by using tin dichloride solid and absolute ethyl alcohol2·2H2O solution; PbI with a concentration of 691.25mg/mol was formulated from N, N-dimethylformamide, dimethyl sulfoxide and lead iodide powder2A solution; preparing an organic ionic solution by formamidine hydroiodide, methyl amine chloride, methyl amine bromide and isopropanol; preparing a Spiro-OMeTAD solution by using Spiro-OMeTAD solid and chlorobenzene;
step (3), preparing each functional layer by the prepared solvent: putting the treated FTO substrate into a preheated ultraviolet ozone processor for treatment for 20min, and spin-coating the SnCl after treatment2·2H2Preparation of SnO from O solution2A thin film layer; then the SnO is put2Treating the film layer in an ultraviolet ozone machine for 20min to remove surface groups and increase the surface wettability, and spin-coating the PbI after treatment2Preparing a perovskite layer from the solution and the organic ion solution; spin-coating the Spiro-OMeTAD solution on the perovskite layer to prepare a Spiro-OMeTAD thin film layer;
step (4), preparing the silver electrode perovskite solar cell: and after the preparation of each functional layer is finished, transferring the functional layers into a cavity of a metal vacuum evaporation plating instrument to perform Ag electrode evaporation plating by adopting a vacuum thermal evaporation deposition method, and finally obtaining the silver electrode perovskite solar cell.
2. The method for preparing silver electrode perovskite solar cell according to claim 1, wherein the PbI in the step (2)2The preparation method of the solution comprises the following steps: 691.25mg of the lead iodide powder is weighed by an analytical balancePutting the powder into a No. 1 glass bottle, respectively taking 0.9mL of N, N-dimethylformamide and 0.1mL of dimethyl sulfoxide by using a liquid transfer gun according to the volume ratio of 9: 1, injecting the powder into the No. 1 glass bottle, putting a magneton into the glass bottle, screwing a bottle cap, sticking a label on the glass bottle, stirring the glass bottle on a magnetic rotary heating table at 70-85 ℃ for 1d, filtering the glass bottle by using a 0.22 mu m organic filter tip, and heating the glass bottle at 80 ℃ to obtain the PbI2And (3) solution.
3. The method for preparing a silver electrode perovskite solar cell according to claim 1, wherein the preparation method of the organic ion solution in the step (2) is as follows: respectively taking 90mg of formamidine hydroiodide with the concentration of 90mg/ml, 6.39mg of methyl ammonium chloride with the concentration of 6.39mg/ml and 9mg of methyl ammonium bromide with the concentration of 9mg/ml in a No. 2 glass bottle by using an analytical balance, then taking the isopropanol in the No. 2 glass bottle by using a liquid transfer gun, putting magnetons in the glass bottle, stirring the glass bottle for one day in a magnetic rotary heating table at normal temperature, and filtering the solution to obtain the organic ion solution.
4. The method for preparing silver electrode perovskite solar cell according to claim 1, wherein the preparation method of the Spiro-OMeTAD solution in the step (2) is as follows: and (3) taking 72.5mg of the Spiro-OMeTAD solid by using an analytical balance, taking 1mL of chlorobenzene by using a pipette in a No. 3 glass bottle, adding magnetons, stirring for 1h on a magnetic rotary heating table at normal temperature until the chlorobenzene is clear, then adding 17.5 muL of lithium salt solution with the concentration of 520mg/mL dissolved in acetonitrile and 28.8 muL of 4-tert-butylpyridine solution in the No. 3 glass bottle, stirring for 1d at normal temperature in the dark, and filtering to obtain the Spiro-OMeTAD solution.
5. The method for preparing silver electrode perovskite solar cell according to claim 1, wherein the method for preparing each functional layer in the step (3) is specifically as follows: taking a proper amount of SnCl2·2H2Dripping O solution at the center of the conductive surface of the FTO substrate, carrying out spin coating at 3000rpm/min for 30s, and annealing at 180 ℃ for 1h after the spin coating is finished, so that the O solution is hydrolyzed to become the SnO2A thin film layer;
taking a proper amount of PbI by using a liquid-transferring gun2The SnO is fully paved by solution2Performing two-stage spin coating process on the thin film layer, spreading the solution at a low rotation speed of 800rpm/min for 5s at the front stage, forming the film at a high speed of 3000rpm/min for 30s at the rear stage, and depositing to obtain PbI2A film; mixing the PbI2The film is placed on a hot table to be annealed at 70 ℃ for 1min, the organic ion solution is spin-coated through the two-stage spin coating process after annealing, and then the film is placed on the hot table to be annealed at 150 ℃ for 20min, and finally the perovskite layer is obtained;
and after the perovskite layer is cooled, spin-coating the Spiro-OMeTAD solution by adopting the two-stage spin-coating process, annealing for 20min at 100 ℃ after the spin-coating is finished, and evaporating the solvent to obtain the Spiro-OMeTAD film layer.
6. The method for preparing the silver electrode perovskite solar cell according to claim 1, wherein the film thickness of the evaporated Ag electrode is 100 nm.
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Application publication date: 20200922 |