CN108447992B - Method for improving stability and efficiency of organic metal halide perovskite solar cell - Google Patents

Method for improving stability and efficiency of organic metal halide perovskite solar cell Download PDF

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CN108447992B
CN108447992B CN201810285981.7A CN201810285981A CN108447992B CN 108447992 B CN108447992 B CN 108447992B CN 201810285981 A CN201810285981 A CN 201810285981A CN 108447992 B CN108447992 B CN 108447992B
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张帅
陆永婷
王妍
陈涌创
袁宁一
丁建宁
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Changzhou University
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    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
    • H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
    • H10K30/151—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2 the wide bandgap semiconductor comprising titanium oxide, e.g. TiO2
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Abstract

The invention provides a method for improving the stability and efficiency of an organic metal halide perovskite solar cell, and belongs to the field of solar cells. The invention uses physical vapor deposition method to deposit on FTO/TiO2Sequentially depositing PbCl on the surface2And PbI2Then lead halide is converted into corresponding organic metal halide perovskite layer to obtain double-layer perovskite, and CH in the double-layer perovskite structure3NH3PbI3‑XClXThe layer has the functions of interface modification and passivation, and can make TiO2The bonding between the titanium ore and the titanium ore is firmer, so that the TiO is2The electric charge at the perovskite/perovskite interface is not easy to accumulate, and the grain size of the perovskite is increased, so that the stability of the battery is improved. In addition, CH3NH3PbI3‑XClXThe layer may also inhibit TiO2The generation of defects at the perovskite interface can reduce the recombination at the interface and improve the efficiency of the battery.

Description

Method for improving stability and efficiency of organic metal halide perovskite solar cell
Technical Field
The invention relates to the field of solar cells, in particular to an interface modification method for improving the stability and efficiency of an organic metal halide perovskite solar cell.
Background
Among various types of solar cells, an organic metal halide perovskite solar cell (hereinafter simply referred to as a perovskite cell) combines low-cost solution processing and excellent photoelectric conversion performance. Through the development of 6-7 years, the energy conversion efficiency of the device in the laboratory breaks through 22%, which is the statistical efficiency increase of the National Renewable Energy Laboratory (NREL) in the United statesThe fastest class of solar cells is therefore considered to be a very promising photovoltaic technology. However, perovskite solar cell efficiencies are far from the Schockley-queesser limit, which may be related to recombination caused by defects at the perovskite solar cell interface. In addition, the most commonly used electron transport layer material for perovskite solar cells, TiO2Not firmly bonded to the perovskite, TiO2The charge at the/perovskite interface tends to build up, which also causes degradation of the stability of the perovskite thin film. Therefore, research on the regulation of the interface of the perovskite solar cell is a hot spot in the research field of perovskite cells.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems of low photoelectric conversion efficiency and poor stability of devices caused by defects at the interface of the perovskite solar cell, a double-layer perovskite heterojunction structure (CH) is developed3NH3PbI3-XClX/CH3NH3PbI3) Thereby utilizing CH3NH3PbI3-XClXLayer modified TiO2And CH3NH3PbI3The photoelectric conversion efficiency and stability of the device are improved.
The technical scheme of the invention is as follows: in order to improve the photoelectric conversion efficiency and stability of the perovskite solar cell, a method for modifying a device interface is provided. The method utilizes CH3NH3PbI3-XClXAs an interface modification layer material, the preparation method comprises the following steps:
(1) cleaning FTO glass: sequentially putting the FTO glass into deionized water, acetone and ethanol, respectively ultrasonically cleaning for half an hour, drying by using nitrogen, and treating for 10min by using oxygen plasma;
(2) preparation of TiO2A dense layer: the cleaned FTO glass was immersed in 200mM TiCl4Heating in water solution at 70 deg.C for 1 hr, repeatedly washing with water and ethanol, blowing with nitrogen gas, and drying at 100 deg.C for 1 hr to obtain FTO/TiO2；
(3) Preparing a hole transport material solution in a glove box: firstly, dissolving Li-TFSI in acetonitrile to prepare a Li-TFSI solution with the concentration of 520mg/ml, then dissolving 72.3mg of spiro-MeOTAD, 28.8ul of 4-tert-butylpyridine and 17.5ul of the Li-TFSI solution in 1ml of chlorobenzene, and stirring for 12 hours to obtain a hole transport material solution;
(4) preparation of FTO/TiO in a glovebox2/PbCl2/PbI2: physical vapor deposition on FTO/TiO2Sequentially evaporating PbCl2And PbI2Layer of PbCl2The thickness of the layer is 2-30nm, PbI2The thickness of the layer is 100-300nm, and the evaporation rate is controlled to be 0.1-1 nm/min;
(5) in a glove box, FTO/TiO2/PbCl2/PbI2Placing into a quartz crucible with cover, wherein the bottom of the crucible is coated with a layer of uniform CH3NH3Powder I, FTO/TiO2/PbCl2/PbI2Then adhered to the back of the crucible cover to lead PbI to be adhered to the crucible cover2Layer facing CH3NH3I, powder;
(6) placing the crucible in the step (5) on a heating table at 170 ℃ in a glove box for heating for 5-20 min;
(7) the sample on the back of the crucible cover was removed in a glove box and the surface was rinsed with isopropyl alcohol and annealed at 70 ℃ for 10min to obtain FTO/TiO2/CH3NH3PbI3-XClX/CH3NH3bI3Perovskite layer of which CH3NH3PbI3-XClXThickness of 3-50nm, CH3NH3bI3The thickness is 150-450 nm;
(8) and spin-coating a hole transport material solution on the perovskite layer in a glove box, rotating for 30s under the condition of 5000r/min, and finally evaporating a gold electrode on the hole transport layer by using a physical vapor deposition method.
Preferably, PbCl is used in the step (4)2And PbI2The thickness of the film is 5-15nm and 150-250nm respectively, and the evaporation rate is 0.2-0.8 nm/min.
Preferably, the heating time in the step (6) is 7-15 min.
The steps (3) to (8) are all finished in a glove box, and preferably, the water oxygen concentration of the glove box is controlled to be below 10 ppm.
Preferably, the thickness of the gold-evaporated electrode in the step (8) is 50-150 nm.
The invention has the technical effects that: the invention adopts the physical vapor deposition method to deposit on FTO/TiO2Sequentially depositing PbCl on the surface2And PbI2Then converting the lead halide into the corresponding organo-metal halide perovskite layer (CH)3NH3PbI3-XClXAnd CH3NH3PbI3). The research shows that: relative to FTO/TiO2/CH3NH3PbI3Double layer perovskite (FTO/TiO)2/CH3NH3PbI3- XClX/CH3NH3PbI3) The stability of the heterojunction structure under the atmospheric environment and illumination is greatly improved, and the corresponding battery efficiency is higher. The stability and efficiency improvement resulting from the double-layer perovskite structure is mainly due to CH3NH3PbI3-XClXThe layer serves for interface modification and passivation. CH (CH)3NH3PbI3-XClXThe layer may be TiO2The bonding between the titanium and the titanium ore is firmer, and the TiO2The electric charge at the perovskite/perovskite interface is not easy to accumulate, and the grain size of the perovskite is increased, so that the stability of the battery is improved. In addition, CH3NH3PbI3-XClXThe layer may also inhibit TiO2The formation of defects at the perovskite interface, and therefore recombination at the interface can be reduced, thereby improving the efficiency of the cell.
Drawings
FIG. 1 shows a structure containing CH3NH3PbI3-XClXAn interface modification layer (a) and not containing CH3NH3PbI3-XClXThe structural schematic diagram of the perovskite solar cell of the interface modification layer (b).
FIG. 2 shows FTO/TiO in comparative example 12/CH3NH3PbI3Surface morphology of perovskite thin film.
FIG. 3 shows FTO/TiO in example 12/CH3NH3PbI3-XClX/CH3NH3PbI3Surface morphology of perovskite thin film.
FIG. 4 shows FTO/TiO in example 22/CH3NH3PbI3-XClX/CH3NH3PbI3Surface morphology of perovskite thin film.
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
Step 1: FTO glass (1.5 x 2cm, commercially available) was sequentially placed in deionized water, acetone, and ethanol, respectively ultrasonically cleaned for half an hour, blown dry with nitrogen, and treated with oxygen plasma for 10 min.
Step 2: dipping the FTO glass cleaned in the step 1 into 200mM TiCl4Heating (AR, commercially available) water solution at 70 deg.C for 1 hr, repeatedly washing with water and ethanol, blowing with nitrogen gas, and drying at 100 deg.C for 1 hr to obtain FTO/TiO2。
And step 3: first, Li-TFSI (AR, commercially available) was dissolved in acetonitrile (AR, commercially available) to control the concentration to 520 mg/ml; then, 72.3mg of spiro-MeOTAD (AR, commercially available), 28.8ul of 4-t-butylpyridine (AR, commercially available) and 17.5ul of Li-TFSI solution were dissolved in 1ml of chlorobenzene (AR, commercially available) and stirred for 12 hours to obtain a hole transporting material solution. The above operations are all completed in the glove box.
And 4, step 4: FTO/TiO prepared in step 2 by physical vapor deposition2Surface evaporation of 200nm thick PbI2Layer (PbI)2AR, commercially available) and the evaporation rate was controlled at 0.2-0.5 nm/min. The above operations are all completed in the glove box.
And 5: mixing FTO/TiO2/PbI2Placing into a quartz crucible with cover, wherein the bottom of the crucible is coated with a layer of uniform CH3NH3Powder I (AR, commercially available), FTO/TiO2/PbI2Then adhered to the back surface of the crucible cover (PbI)2Layer facing CH3NH3I powder). The above operations are all completed in the glove box.
Step 6: the quartz crucible in step 5 was placed on a hot stage at 170 ℃ and heated for 10 min. The above operations are all completed in the glove box.
And 7: after the crucible was cooled to room temperature in step 6, the sample on the back of the crucible cover was taken off and the surface was rinsed with isopropyl alcohol (AR, commercially available), and annealed at 70 ℃ for 10min to obtain FTO/TiO2/CH3NH3PbI3. The above operations are all completed in the glove box.
And 8: in CH3NH3PbI3And (3) coating the hole transport material solution prepared in the step (3) on the layer, rotating for 30s under the condition of 5000r/min, and finally evaporating a gold electrode (80nm) on the hole transport layer by using a physical vapor deposition method to obtain the battery. The above operations are all completed in the glove box.
FTO/TiO obtained in step 7 of comparative example 12/CH3NH3PbI3SEM characterization was performed, and the surface SEM image is shown in FIG. 2. The obtained cell was subjected to an I-V curve test (under simulated sunlight of am1.5g) and had an efficiency of 12.1%. The cell was stored in an atmospheric environment at 50% humidity, and after 1 week the efficiency dropped to about 50% (5.95%) of the original efficiency.
Comparative example 2
In comparative example 1, step 4, evaporated PbI2The thickness of the layer was adjusted to 100 nm. The heating time was changed to 7min in step 6.
The cell obtained in comparative example 2 was subjected to an I-V curve test (under simulated sunlight of am1.5g) and had an efficiency of 9.81%. The cell was stored in an atmospheric environment at 50% humidity, and after 1 week the efficiency dropped to about 30% (3.02%) of the original efficiency.
Example 1
Comparative example 1 step 4, in turn at FTO/TiO2Surface evaporation of 5nm thick PbCl2And 200nm thick PbI2。
FTO/TiO obtained in step 7 of example 12/CH3NH3PbI3-XClX/CH3NH3PbI3SEM characterization was performed, and the surface SEM image is shown in FIG. 3. To the obtained electricityThe cell was tested for I-V curve (in AM1.5G simulated sunlight) and its efficiency was 14.52%. The cell was stored in an atmosphere at 50% humidity and after 1 week the efficiency dropped to more than about 70% (10.2%) of the original efficiency.
Example 2
Comparative example 1 step 4, in turn at FTO/TiO2Surface evaporation of 15nm thick PbCl2And 200nm thick PbI2。
FTO/TiO obtained in step 7 of example 22/CH3NH3PbI3-XClX/CH3NH3PbI3SEM characterization was performed, and the surface SEM image is shown in FIG. 4. The obtained cell was tested for its I-V curve (under simulated sunlight at am1.5g) and its efficiency was 15.8%. The cell was stored in an atmosphere at 50% humidity and after 1 week the efficiency dropped to more than about 80% (12.86%) of the original efficiency.
Example 3
Comparative example 1 step 4, in turn at FTO/TiO2Surface evaporation of 15nm thick PbCl2And 100nm thick PbI2。
The cell obtained in example 3 was tested for its I-V curve (under simulated sunlight at am1.5g) efficiency at 12.36%. The cell was stored in an atmosphere at 50% humidity and after 1 week the efficiency dropped to about 80% (9.85%) of the original efficiency.

Claims (5)

1. A method for improving the stability and efficiency of an organic metal halide perovskite solar cell is characterized by comprising the following specific operation steps:
(1) cleaning FTO glass: sequentially putting the FTO glass into deionized water, acetone and ethanol, ultrasonically cleaning for half an hour, drying by using nitrogen, and treating for 10min by using oxygen plasma;
(2) preparation of TiO2A dense layer: the cleaned FTO glass was immersed in 200mM TiCl4Heating in water solution at 70 deg.C for 1 hr, washing with water and ethanol, blowing with nitrogen gas, and drying at 100 deg.C for 1 hr to obtain FTO/TiO2；
(3) Preparing a hole transport material solution in a glove box: firstly, dissolving Li-TFSI in acetonitrile to prepare a Li-TFSI solution with the concentration of 520mg/ml, then dissolving 72.3mg of spiro-MeOTAD, 28.8ul of 4-tert-butylpyridine and 17.5ul of the Li-TFSI solution in 1ml of chlorobenzene, and stirring for 12 hours to obtain a hole transport material solution;
(4) preparation of FTO/TiO in a glovebox2/PbCl2/PbI2: physical vapor deposition on FTO/TiO2Sequentially evaporating PbCl2And PbI2Layer of PbCl2The thickness of the layer was 2 ‒ 30nm, PbI2The thickness of the layer is 100 ‒ 300nm, and the evaporation rate is controlled at 0.1 ‒ 1 nm/min;
(5) in a glove box, FTO/TiO2/PbCl2/PbI2Placing into a quartz crucible with cover, wherein the bottom of the crucible is coated with a layer of uniform CH3NH3Powder I, FTO/TiO2/PbCl2/PbI2Then adhered to the back of the crucible cover to lead PbI to be adhered to the crucible cover2Layer facing CH3NH3I, powder;
(6) placing the crucible in step (5) on a heating table at 170 ℃ in a glove box for heating for 5 ‒ 20 min;
(7) the sample on the back of the crucible cover was removed in a glove box and the surface was rinsed with isopropyl alcohol and annealed at 70 ℃ for 10min to obtain FTO/TiO2/CH3NH3PbI3-XClX/CH3NH3PbI3Perovskite layer of which CH3NH3PbI3-XClXThickness of 3 ‒ 50nm, CH3NH3bI3The thickness is 150 ‒ 450 nm; wherein CH is utilized3NH3PbI3-XClXLayer modified TiO2And CH3NH3PbI3The interface of the device improves the photoelectric conversion efficiency and stability of the device;
(8) and spin-coating a hole transport material solution on the perovskite layer in a glove box, rotating for 30s under the condition of 5000r/min, and finally evaporating a gold electrode on the hole transport layer by using a physical vapor deposition method.
2. The method of improving the stability and efficiency of an organo-metal halide perovskite solar cell as claimed in claim 1, step (4) of PbCl2And PbI2The thickness of (A) is 5 ‒ 15nm and 150 ‒ 250nm respectively, and the evaporation rate is 0.2 ‒ 0.8 nm/min.
3. The method for improving stability and efficiency of an organo-metal halide perovskite solar cell as claimed in claim 1, wherein the heating time of step (6) is 7 ‒ 15 min.
4. The method for improving the stability and efficiency of an organo-metal halide perovskite solar cell as claimed in claim 1, wherein the water oxygen concentration of the glove box is controlled to be less than 10 ppm.
5. The method for improving stability and efficiency of an organo-metal halide perovskite solar cell as claimed in claim 1, wherein the thickness of the evaporated gold electrode of step (8) is 50 ‒ 150 nm.
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