CN107799654B - High-efficiency planar perovskite solar cell and preparation method thereof - Google Patents
High-efficiency planar perovskite solar cell and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-efficiency planar perovskite solar cell, which comprises a transparent conductive substrate, an electron conduction layer, a perovskite layer, a hole conduction layer and a metal electrode, wherein the transparent conductive substrate is provided with a plurality of holes; the electron conduction layer is a gallium-doped titanium dioxide dense layer prepared by a low-temperature process solution method. The invention also relates to a preparation method of the high-efficiency planar perovskite solar cell, which comprises the steps of adding gallium nitrate in the process of preparing the titanium dioxide dense layer by hydrolyzing titanium tetrachloride and carrying out low-temperature heat treatment to obtain the gallium-doped titanium dioxide dense layer, and assembling the perovskite solar cell by using the gallium-doped titanium dioxide dense layer. The planar perovskite solar cell provided by the invention adopts the gallium-doped titanium dioxide dense layer prepared by a low-temperature process solution method as the electron conduction layer, and the collection and conduction of the titanium dioxide electron conduction layer to photoelectrons are promoted by gallium doping, so that the planar perovskite solar cell has the advantages of high photoelectric conversion efficiency, high cell efficiency and easiness in preparation.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a high-efficiency planar perovskite solar cell and a preparation method thereof.
Background
In recent years, perovskite solar cells have attracted much attention because of their high photoelectric conversion efficiency. The photoelectric characteristics of the electron conducting layer in the perovskite solar cell determine the light absorption of the cell and the conduction and collection of photon-generated carriers, and the microstructure influences the microstructure and the photoelectric characteristics of the perovskite layer, and determines the photoelectric conversion efficiency of the cell to a certain extent, so that the perovskite solar cell is particularly important.
Although the highest conversion efficiency of perovskite cells certified by NREL in the united states has exceeded 22%, the low temperature CH currently reported is3NH3PbI3-xClxThe photoelectric conversion efficiency of the basal plane perovskite solar cell is only about 13% generally, and the space capable of being improved is large. It is one of the feasible ideas to improve the photoelectric conversion efficiency of the cell by promoting the conduction and collection of photo-generated electrons from the viewpoint of regulating the photoelectric characteristics of the electron conduction layer. At present, the planar CH with a gallium-doped titanium dioxide dense layer as the electron-conducting layer has not yet appeared3NH3PbI3-xClxBased on perovskite solar cells, the assembly of high-efficiency plane CH by preparing gallium-doped titanium dioxide dense layer at low temperature is not shown3NH3PbI3-xClxRelevant reports of perovskite-based solar cells.
Disclosure of Invention
Based on the above, the present invention provides a high efficiency planar perovskite solar cell, which uses a gallium-doped titanium dioxide dense layer as an electron conduction layer, wherein the gallium-doped titanium dioxide dense layer has the advantages of being prepared by a low temperature process, and the assembled cell has high photoelectric conversion efficiency.
The technical scheme adopted by the invention is as follows:
a high efficiency planar perovskite solar cell comprises a transparent conductive substrate, an electron conducting layer, a perovskite layer, a hole conducting layer and a metal electrode; the electron conduction layer is a gallium-doped titanium dioxide compact layer, and the gallium-doped titanium dioxide compact layer is prepared by adding gallium nitrate in the process of depositing the titanium dioxide compact layer by a low-temperature hydrolysis method.
Compared with the prior art, the planar perovskite solar cell adopts a gallium-doped titanium dioxide dense layer (Ga) TiO for short2Dense layer) as an electron conduction layer, and the mobility of the electron layer is improved by gallium doping to promote the conduction and collection of photo-generated electrons, so that the photoelectric conversion efficiency of the cell is improved. The planar perovskite solar cell provided by the invention has obviously higher cell efficiency than the planar perovskite solar cell using the undoped titanium dioxide dense layer as an electron conduction layer.
Further, the molar ratio of gallium atoms to titanium atoms in the gallium-doped titanium dioxide dense layer is 3-9: 100. By adjusting the doping amount of gallium within a proper range, the planar perovskite solar cell is ensured to have high cell efficiency.
Further, the transparent conductive substrate is fluorine-doped tin dioxide conductive glass (FTO conductive glass), and the perovskite layer is CH3NH3PbI3-xClxA layer of a basic perovskite of the formula,the hole conduction layer is a Spiro-OMeTAD layer, and the metal electrode is a silver electrode.
The invention also provides a preparation method of any one of the high-efficiency planar perovskite solar cells, which comprises the following steps:
(1) preparation of the electron conducting layer: firstly, adding gallium nitrate into an ice water mixture, then adding a titanium tetrachloride aqueous solution, preparing a gallium-doped titanium dioxide colloidal solution, then putting a clean transparent conductive substrate into the gallium-doped titanium dioxide colloidal solution at the temperature of 60-80 ℃ for soaking for 40-60 minutes, taking out the transparent conductive substrate, sequentially washing the transparent conductive substrate with deionized water and ethanol, and then carrying out heat treatment at the temperature of 180-220 ℃ for 30-60 minutes to obtain a gallium-doped titanium dioxide dense layer which is prepared on the transparent conductive substrate and is used as an electronic conductive layer;
(2) preparation of perovskite layer: mixing CH with a molar ratio of 3:13NH3I and PbCl2Dissolving the perovskite precursor solution in dimethylformamide to obtain a perovskite precursor solution, carrying out ultraviolet light treatment on the gallium-doped titanium dioxide compact layer obtained in the step (1) for 8-15 minutes, then dropwise adding the perovskite precursor solution on the gallium-doped titanium dioxide compact layer, carrying out spin coating, and carrying out heat treatment at 80-120 ℃ for 50-70 minutes to obtain CH (carbon-oxygen) serving as a perovskite layer on the gallium-doped titanium dioxide compact layer3NH3PbI3-xClxA perovskite-based layer;
(3) preparation of hole conducting layer: CH obtained in step (2)3NH3PbI3-xClxSpin coating on the perovskite-based layer containing 0.08M 2,2',7,7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino]A chlorobenzene mixed solution of-9, 9' -spirobifluorene (Spiro-OMeTAD), 0.064M lithium bistrifluoromethanesulfonylimide (LiTFSI) and 0.064M Tetrabutylpyridine (TBP), and then the mixed solution is placed in dark and dry air for 6-8 hours to obtain the compound prepared in CH3NH3PbI3-xClxA Spiro-OMeTAD layer as a hole-conducting layer on the perovskite-based layer;
(4) preparing a metal electrode: and (4) evaporating and plating a metal electrode with the thickness of 80-150 nm on the Spiro-OMeTAD layer obtained in the step (3) by adopting a thermal evaporation method to obtain the high-efficiency planar perovskite solar cell.
Further, in the step (1), the volume ratio of titanium tetrachloride to water in the titanium tetrachloride aqueous solution is 1.5-4: 100, and the molar ratio of gallium atoms to titanium atoms in the obtained gallium-doped titanium dioxide dense layer is 3-9: 100. By adjusting the dosage of the gallium nitrate, the doping amount of the gallium is in an appropriate range, and the planar perovskite solar cell is ensured to have high cell efficiency.
Further, in the step (1), the transparent conductive substrate is fluorine-doped tin dioxide conductive glass (FTO conductive glass), and the fluorine-doped tin dioxide conductive glass is subjected to ultraviolet light treatment for 10-20 minutes and then is soaked in a gallium-doped titanium dioxide colloidal solution.
Further, in the step (1), the transparent conductive substrate is placed into a gallium-doped titanium dioxide colloidal solution at 70 ℃ to be soaked for 50 minutes, and then the transparent conductive substrate is taken out and washed by deionized water and ethanol in sequence, and then is subjected to heat treatment at 200 ℃.
Further, in the step (2), CH is contained in the perovskite precursor liquid3NH3I and PbCl2The total mass percentage of (a) is 40%.
Further, in the step (2), the time of the ultraviolet light treatment is 10 minutes; the spin coating speed is 3000 r/min, and the time is 30 seconds; the temperature of the heat treatment is 100 ℃, and the time is 60 minutes; both the spin coating and the heat treatment were carried out in a glove box.
Further, in the step (4), the metal electrode is a silver electrode, and the thermal evaporation is performed in a thermal evaporator at (6 × 10)-6)～(1×10-8) Vapor deposition is performed at a rate of 1 to 10nm/min under millitorr.
The preparation method of the invention prepares TiO by hydrolyzing titanium tetrachloride2Adding a proper amount of gallium nitrate in the process of the compact layer, and then carrying out low-temperature heat treatment to obtain (Ga) TiO2A dense layer and use of the (Ga) TiO2The compact layer is used as an electron conduction layer, and the prepared structure is as follows: FTO/(Ga) TiO2/CH3NH3PbI3-xClxa/Spiro-OMeTAD/Ag high efficiency planar perovskite cell. The preparation method of the inventionEasy realization, easy control of parameter conditions of each step and low preparation cost.
The invention is not limited to adopting FTO conductive glass as a transparent conductive substrate and CH3NH3PbI3The perovskite-based layer is used as the perovskite layer, the Spiro-OMeTAD layer is used as a hole conducting layer, the silver electrode is used as a metal electrode, and all the gallium-doped TiO prepared by the low-temperature process of the invention2The electronic layer is assembled into the perovskite solar cell with any structure, and the perovskite solar cell is within the protection scope of the invention.
For a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
Fig. 1 is a schematic structural view of a high efficiency planar perovskite solar cell of the present invention.
Detailed Description
As shown in fig. 1, the high-efficiency planar perovskite solar cell provided by the present invention includes a transparent conductive substrate 1, an electron conducting layer 2, a perovskite layer 3, a hole conducting layer 4, and a metal electrode 5, which are sequentially stacked.
Specifically, the transparent conductive substrate 1 is fluorine-doped tin dioxide conductive glass. The electron conduction layer 2 is a gallium-doped titanium dioxide dense layer, wherein the molar ratio of gallium atoms to titanium atoms is 3-9: 100. The perovskite layer 3 is CH3NH3PbI3-xClxA perovskite-based layer. The hole-conducting layer 4 is a Spiro-OMeTAD layer. The metal electrode 5 is a silver electrode with the thickness of 80-150 nm.
The preparation method of the high-efficiency planar perovskite solar cell provided by the invention comprises the following steps:
(1) preparation of the electron conducting layer: firstly, adding gallium nitrate into an ice water mixture, and then adding a titanium tetrachloride aqueous solution to prepare a gallium-doped titanium dioxide colloidal solution. And then, putting the clean transparent conductive substrate into a gallium-doped titanium dioxide colloidal solution at the temperature of 60-80 ℃ for soaking for 40-60 minutes, taking out, sequentially washing with deionized water and ethanol, and then carrying out heat treatment at the temperature of 180-220 ℃ for 30-60 minutes to obtain the gallium-doped titanium dioxide dense layer serving as an electronic conduction layer and prepared on the transparent conductive substrate.
(2) Preparation of perovskite layer: mixing CH with a molar ratio of 3:13NH3I and PbCl2Dissolving the perovskite precursor solution in dimethylformamide to obtain a perovskite precursor solution, carrying out ultraviolet light treatment on the gallium-doped titanium dioxide compact layer obtained in the step (1) for 8-15 minutes, then dropwise adding the perovskite precursor solution on the gallium-doped titanium dioxide compact layer, carrying out spin coating, and carrying out heat treatment at 80-120 ℃ for 50-70 minutes to obtain CH (carbon-oxygen) serving as a perovskite layer on the gallium-doped titanium dioxide compact layer3NH3PbI3-xClxA perovskite-based layer.
(3) Preparation of hole conducting layer: CH obtained in step (2)3NH3PbI3-xClxSpin-coating a chlorobenzene mixed solution containing 0.08M Spiro-OMeTAD, 0.064M LiTFSI and 0.064M Spiro-OMeTAD on the perovskite-based layer, and then placing the chlorobenzene mixed solution in dark and dry air for 6-8 hours to obtain the perovskite-based paint prepared on CH3NH3PbI3-xClxA Spiro-OMeTAD layer as a hole conducting layer on the perovskite-based layer.
(4) Preparing a metal electrode: and (4) evaporating and plating a metal electrode with the thickness of 80-150 nm on the Spiro-OMeTAD layer obtained in the step (3) by adopting a thermal evaporation method to obtain the high-efficiency planar perovskite solar cell.
Example 1
The preparation of the high-efficiency planar perovskite solar cell in the embodiment is specifically carried out according to the following steps:
(1) preparing a gallium-doped titanium dioxide dense layer: firstly, adding gallium nitrate into an ice water mixture, then adding a titanium tetrachloride water solution with the volume ratio of titanium tetrachloride to water being 1.5-4: 100, and preparing a gallium-doped titanium dioxide colloidal solution. And then, after the clean fluorine-doped tin dioxide conductive glass is irradiated by an ultraviolet lamp for 10-20 minutes, putting the clean fluorine-doped tin dioxide conductive glass into a gallium-doped titanium dioxide colloidal solution at 70 ℃ for soaking for 50 minutes, taking the clean fluorine-doped tin dioxide conductive glass out, washing the clean fluorine-doped tin dioxide conductive glass by deionized water and ethanol in sequence, and then carrying out heat treatment at 200 ℃ for 30-60 minutes to obtain a gallium-doped titanium dioxide dense layer prepared on the fluorine-doped tin dioxide conductive glass, wherein the molar ratio of gallium atoms to titanium atoms in the gallium-doped titanium dioxide dense layer is 5: 100.
(2)CH3NH3PbI3-xClxPreparation of the perovskite-based layer: mixing CH with a molar ratio of 3:13NH3I and PbCl2Dissolving in dimethylformamide to obtain CH3NH3I and PbCl2The perovskite precursor solution with the total mass percentage of 40 percent. Carrying out ultraviolet light treatment on the gallium-doped titanium dioxide compact layer obtained in the step (1) for 10 minutes, then dropwise adding a perovskite precursor solution on the gallium-doped titanium dioxide compact layer, carrying out spin coating at the speed of 3000 r/min for 30 seconds, and then carrying out heat treatment at the temperature of 100 ℃ for 60 minutes to obtain CH prepared on the gallium-doped titanium dioxide compact layer3NH3PbI3-xClxA perovskite-based layer. Both the spin coating and the heat treatment were carried out in a glove box.
(3) Preparation of a Spiro-OMeTAD layer: CH obtained in step (2)3NH3PbI3-xClxSpin-coating a chlorobenzene mixed solution containing 0.08M Spiro-OMeTAD, 0.064M LiTFSI and 0.064M Spiro-OMeTAD on the perovskite-based layer, and then placing the chlorobenzene mixed solution in dark and dry air for 6-8 hours to fully oxidize the chlorobenzene mixed solution to obtain the perovskite-based catalyst prepared on CH3NH3PbI3-xClxA Spiro-OMeTAD layer on the perovskite-based layer.
(4) Preparation of silver electrode in thermal evaporator at (6 × 10)-6)～(1×10-8) And (4) evaporating and plating a silver electrode with the thickness of 80-150 nm on the Spiro-OMeTAD layer obtained in the step (3) at the speed of 1-10 nm/min under the air pressure of millitorr, and taking out the battery with the evaporated silver electrode to obtain the prepared high-efficiency planar perovskite solar battery.
Example 2
The procedure for preparing a high efficiency planar perovskite solar cell of this example is substantially the same as example 1, except that: in the step (1), the molar ratio of gallium atoms to titanium atoms in the prepared gallium-doped titanium dioxide dense layer is 7: 100.
Example 3
The procedure for preparing a high efficiency planar perovskite solar cell of this example is substantially the same as example 1, except that: in the step (1), the molar ratio of gallium atoms to titanium atoms in the prepared gallium-doped titanium dioxide dense layer is 9: 100.
Comparative example
This comparative example the procedure for the preparation of a high efficiency planar perovskite solar cell was substantially the same as example 1, except that: step (1) is the preparation process of the titanium dioxide dense layer, gallium nitrate is not added into the ice-water mixture, and the undoped titanium dioxide dense layer is prepared.
Under room temperature environment, using a Newport 91159 sunlight simulator, with light intensity of 100mW/cm2The performance tests were performed on the planar perovskite solar cells prepared in examples 1 to 3 and comparative example, respectively, under the conditions.
The test results are: the photovoltaic efficiency of a planar perovskite solar cell assembled with a gallium-doped dense layer of titanium dioxide (gallium to titanium molar ratio of 5:100) of example 1 was 16.06%. The photovoltaic efficiency of a planar perovskite solar cell assembled with a gallium-doped dense layer of titanium dioxide (gallium to titanium molar ratio of 7:100) of example 2 was 17.09%. The photovoltaic efficiency of a planar perovskite solar cell assembled with a gallium-doped dense layer of titanium dioxide (gallium to titanium molar ratio 9:100) of example 3 was 14.19%. The photovoltaic efficiency of the planar perovskite solar cell assembled with the dense layer of titanium dioxide of the comparative example was 14.22%.
The test results show that the cell efficiency of the planar perovskite solar cell using the gallium-doped titanium dioxide dense layer as the electron conduction layer is obviously higher than that of the planar perovskite solar cell using the undoped titanium dioxide dense layer as the electron conduction layer.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
All perovskite solar cells assembled by adopting the electronic layers prepared by the low-temperature process belong to the protection scope of the invention.
Claims (8)
1. A high efficiency planar perovskite solar cell comprises a transparent conductive substrate, an electron conducting layer, a perovskite layer, a hole conducting layer and a metal electrode; the method is characterized in that: the electron conduction layer is a gallium-doped titanium dioxide compact layer, and the gallium-doped titanium dioxide compact layer is prepared by adding gallium nitrate in the process of depositing the titanium dioxide compact layer by a low-temperature hydrolysis method of titanium tetrachloride; the molar ratio of gallium atoms to titanium atoms in the gallium-doped titanium dioxide dense layer is 5-7: 100; the perovskite layer is CH3NH3PbI3-xClxA perovskite-based layer;
the preparation method of the planar perovskite solar cell comprises the following steps:
(1) preparation of the electron conducting layer: firstly, adding gallium nitrate into an ice water mixture, then adding a titanium tetrachloride aqueous solution, preparing a gallium-doped titanium dioxide colloidal solution, then putting a clean transparent conductive substrate into the gallium-doped titanium dioxide colloidal solution at the temperature of 60-80 ℃ for soaking for 40-60 minutes, taking out the transparent conductive substrate, sequentially washing the transparent conductive substrate with deionized water and ethanol, and then carrying out heat treatment at the temperature of 180-220 ℃ for 30-60 minutes to obtain a gallium-doped titanium dioxide dense layer which is prepared on the transparent conductive substrate and is used as an electronic conductive layer;
(2) preparation of perovskite layer: mixing CH with a molar ratio of 3:13NH3I and PbCl2Dissolving in dimethylformamide to obtain perovskite precursor solution, wherein CH3NH3I and PbCl2The total mass percent of the titanium dioxide layer is 40%, the gallium-doped titanium dioxide dense layer obtained in the step (1) is subjected to ultraviolet light treatment for 8-15 minutes, then perovskite precursor liquid is dripped on the gallium-doped titanium dioxide dense layer, and heat treatment is carried out for 50-70 minutes at 80-120 ℃ after spin coating, so that CH which is prepared on the gallium-doped titanium dioxide dense layer and serves as a perovskite layer is obtained3NH3PbI3-xClxA perovskite-based layer;
(3) preparing a hole conduction layer;
(4) and (4) preparing a metal electrode.
2. The high efficiency planar perovskite solar cell of claim 1, wherein: the transparent conductive substrate is fluorine-doped tin dioxide conductive glass, the hole conduction layer is a Spiro-OMeTAD layer, and the metal electrode is a silver electrode.
3. The method of manufacturing a high efficiency planar perovskite solar cell as claimed in claim 1 or 2, characterized in that: the method comprises the following steps:
(1) preparation of the electron conducting layer: firstly, adding gallium nitrate into an ice water mixture, then adding a titanium tetrachloride aqueous solution, preparing a gallium-doped titanium dioxide colloidal solution, then putting a clean transparent conductive substrate into the gallium-doped titanium dioxide colloidal solution at the temperature of 60-80 ℃ for soaking for 40-60 minutes, taking out the transparent conductive substrate, sequentially washing the transparent conductive substrate with deionized water and ethanol, and then carrying out heat treatment at the temperature of 180-220 ℃ for 30-60 minutes to obtain a gallium-doped titanium dioxide dense layer which is prepared on the transparent conductive substrate and is used as an electronic conductive layer; the molar ratio of gallium atoms to titanium atoms in the obtained gallium-doped titanium dioxide compact layer is 5-7: 100;
(2) preparation of perovskite layer: mixing CH with a molar ratio of 3:13NH3I and PbCl2Dissolving in dimethylformamide to obtain perovskite precursor solution, wherein CH3NH3I and PbCl2The total mass percent of the titanium dioxide layer is 40%, the gallium-doped titanium dioxide dense layer obtained in the step (1) is subjected to ultraviolet light treatment for 8-15 minutes, then perovskite precursor liquid is dripped on the gallium-doped titanium dioxide dense layer, and heat treatment is carried out for 50-70 minutes at 80-120 ℃ after spin coating, so that CH which is prepared on the gallium-doped titanium dioxide dense layer and serves as a perovskite layer is obtained3NH3PbI3-xClxA perovskite-based layer;
(3) preparation of hole conducting layer: CH obtained in step (2)3NH3PbI3-xClxThe perovskite-based layer was spin-coated with a mixed solution of chlorobenzene containing 0.08MSpiro-OMeTAD, 0.064M LiTFSI and 0.064M Spiro-OMeTAD, and then subjected to spin-coatingPlacing the mixture in dark dry air for 6-8 hours to obtain the compound of CH3NH3PbI3-xClxA Spiro-OMeTAD layer as a hole-conducting layer on the perovskite-based layer;
(4) preparing a metal electrode: and (4) evaporating and plating a metal electrode with the thickness of 80-150 nm on the Spiro-OMeTAD layer obtained in the step (3) by adopting a thermal evaporation method to obtain the high-efficiency planar perovskite solar cell.
4. The method of manufacturing a high efficiency planar perovskite solar cell according to claim 3, characterized in that: in the step (1), the volume ratio of titanium tetrachloride to water in the titanium tetrachloride water solution is 1.5-4: 100.
5. The method of manufacturing a high efficiency planar perovskite solar cell according to claim 4, wherein: in the step (1), the transparent conductive substrate is fluorine-doped tin dioxide conductive glass, and the fluorine-doped tin dioxide conductive glass is subjected to ultraviolet light treatment for 10-20 minutes and then is soaked in a gallium-doped titanium dioxide colloidal solution.
6. The method of manufacturing a high efficiency planar perovskite solar cell according to claim 5, wherein: in the step (1), the transparent conductive substrate is placed into a gallium-doped titanium dioxide colloidal solution at 70 ℃ to be soaked for 50 minutes, and then the transparent conductive substrate is taken out and washed by deionized water and ethanol in sequence, and then is subjected to heat treatment at 200 ℃.
7. The method of manufacturing a high efficiency planar perovskite solar cell according to claim 6, wherein: in the step (2), the ultraviolet light treatment time is 10 minutes; the spin coating speed is 3000 r/min, and the time is 30 seconds; the temperature of the heat treatment is 100 ℃, and the time is 60 minutes; both the spin coating and the heat treatment were carried out in a glove box.
8. A method of making a high efficiency planar perovskite solar cell as claimed in claim 3 which isCharacterized in that in the step (4), the metal electrode is a silver electrode, the thermal evaporation is carried out in a thermal evaporator, and the temperature is controlled at (6 × 10)-6)～(1×10-8) Vapor deposition is performed at a rate of 1 to 10nm/min under millitorr.
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