CN113707818A - Method for rapidly preparing all-printed perovskite solar cell - Google Patents
Method for rapidly preparing all-printed perovskite solar cell Download PDFInfo
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- CN113707818A CN113707818A CN202110995555.4A CN202110995555A CN113707818A CN 113707818 A CN113707818 A CN 113707818A CN 202110995555 A CN202110995555 A CN 202110995555A CN 113707818 A CN113707818 A CN 113707818A
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- H10K30/15—Sensitised wide-bandgap semiconductor devices, e.g. dye-sensitised TiO2
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- 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
本发明提供一种快速制备全印刷钙钛矿太阳能电池的方法，包括FTO导电基底的刻蚀和清洗、致密层的制备、介孔层的制备、间隔层和碳对电极的制备以及CH3NH3PbI3填充，最终得到电池器件。本发明间隔层印刷完后126℃保温6min，随后间隔层和碳对电极共同烧结，烧结工艺为112℃保温5min、175℃保温5min、350℃保温10min、400℃保温15min、500℃保温30min，升温速率为2~15℃/min。与常规方法相比，本发明将全印刷钙钛矿太阳能电池制备过程中的间隔层和碳对电极共同烧结，经简化烧结步骤后制备得到的电池，电池性能保持原有效率，缩短了电池制备时间，降低了电池制备过程中的能耗。The present invention provides a method for rapidly preparing full-printed perovskite solar cells, including etching and cleaning of FTO conductive substrate, preparation of dense layer, preparation of mesoporous layer, preparation of spacer layer and carbon counter electrode, and CH 3 NH 3 PbI 3 is filled, and finally the battery device is obtained. After printing the spacer layer of the present invention, the temperature is kept at 126°C for 6 minutes, and then the spacer layer and the carbon counter electrode are co-sintered. The heating rate is 2~15°C/min. Compared with the conventional method, the present invention co-sinters the spacer layer and the carbon counter electrode in the preparation process of the full-printed perovskite solar cell, and the battery prepared after the sintering step is simplified, the battery performance maintains the original efficiency, and the battery preparation is shortened. time, reducing the energy consumption in the battery preparation process.
Description
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a method for quickly preparing a full-printing perovskite solar cell.
Background
Solar cells are being developed day by day. The 2009 Miyasaka subject group first identified perovskite materials (CH)3NH3PbI3) Selected as sensitizationThe preparation is applied to a solar cell, and the photoelectric conversion efficiency of 3.8 percent is obtained. With continuous development of new materials and optimization of preparation processes by researchers, battery efficiency is continuously refreshed and stability is further improved, and by far, the maximum photoelectric conversion efficiency of the PSCs is broken through by 22%. The battery device still adopts the conventional structure (c-TiO)2/m-TiO2/CH3NH3PbI3/spiro-OMeTAD/Au), the PSCs based on the structure have high photoelectric conversion efficiency, but are not suitable for commercial application. In 2013, the Han topic group introduced carbon counter electrodes for the first time in the developed printable PSCs and achieved 6.64% photoelectric conversion efficiency. The PSCs can be printed.
In the preparation of printable PSCs, CH3NH3PbI3And finally dripping the precursor solution onto the carbon counter electrode in a dripping mode. In addition, the mesoporous layer, the spacer layer and the carbon counter electrode are main structures, and the three-layer film needs to be sintered at high temperature after being printed. Because the sintering temperature is higher, a large amount of energy is consumed in the preparation process of the battery device, and in addition, the temperature rise and temperature drop stage in the sintering process takes a quite long time, so that the preparation period of the battery device is longer, and the preparation efficiency of the battery is influenced. In order to save energy and reduce the manufacturing cycle, it is necessary to optimize the manufacturing process of the battery device. Based on the method, the spacer layer and the carbon counter electrode in the preparation process of the full-printing perovskite solar cell are sintered together, and compared with the conventional method, the battery performance obtained by simplifying the sintering step is higher, the battery performance keeps the original efficiency, the battery preparation time is shortened, and the energy consumption in the battery preparation process is reduced.
Disclosure of Invention
The invention aims to provide a method for rapidly preparing a full-printing perovskite solar cell aiming at the defects of the prior art, so that the preparation process of the full-printing perovskite solar cell is simplified and the preparation period is shortened on the basis of ensuring the cell efficiency.
The invention adopts the following technical scheme:
a method for rapidly preparing a fully printed perovskite solar cell comprises the following steps:
s1, etching and cleaning an FTO conductive substrate:
covering the part of the FTO conductive glass which does not need to be etched by using an adhesive tape, covering the exposed part by using zinc powder, dropwise adding an HCl solution on the part, flushing the zinc powder and removing the adhesive tape after a period of time, after the conductive substrate is etched, respectively ultrasonically cleaning by using soap water, glass cleaning solution, absolute ethyl alcohol and distilled water, sequentially washing by using distilled water and absolute ethyl alcohol and drying for later use;
s2, preparation of the dense layer:
adding titanium tetrachloride into distilled water to prepare a compact layer precursor solution; covering the part, which does not need to be provided with the compact layer, of the FTO conductive substrate obtained in the step S1 by using a high-temperature adhesive tape, soaking the FTO conductive substrate in the compact layer precursor solution for a period of time, taking out, washing and drying the FTO conductive substrate by using distilled water and absolute ethyl alcohol in sequence, sintering the FTO conductive substrate, and annealing for later use;
s3, preparing a mesoporous layer:
adding TiO into the mixture2Printing the slurry on the FTO conductive substrate prepared in S2, standing at room temperature, and drying; subsequent treatment of TiO2Sintering the film, and cooling to room temperature; covering the part except the mesoporous layer by using a high-temperature adhesive tape, and putting the part into an aqueous solution of titanium tetrachloride for heating and soaking until the aqueous solution of titanium tetrachloride is changed into light blue; then sequentially washing with distilled water and absolute ethyl alcohol and drying; finally, sintering for later use;
preparation of S4, spacer layer and carbon counter electrode:
S5、CH3NH3PbI3filling:
firstly, sticking an adhesive tape along the edge of a carbon counter electrode, and then preheating an FTO conductive substrate at 50 ℃; mixing trace CH3NH3PbI3And dripping the precursor solution on the surface of the carbon counter electrode, standing, and then transferring to a heating platform to heat for 1h at 70 ℃ to obtain the battery.
Further, in S1, the volume fraction of the HCl solution was 10%.
Furthermore, in S1, the etching time of the zinc powder and the HCl solution on the FTO conductive glass is 15-30S.
Further, in S2, the annealing rate of the compact layer is 2-15 ℃/min.
Further, in S2, the sintering process is: keeping the temperature at 500 ℃ for 30min, wherein the heating rate is 10 ℃/min.
Further, in S3, the sintering process is: keeping the temperature at 112 ℃ for 5min, keeping the temperature at 175 ℃ for 5min, keeping the temperature at 350 ℃ for 10min, keeping the temperature at 400 ℃ for 15min, keeping the temperature at 500 ℃ for 30min, and keeping the sintering rate at 2-15 ℃/min.
Further, in S4, the printed spacer layer was then incubated at 126 ℃ for 6 min.
Further, in S4, the sintering process comprises the steps of preserving heat at 112 ℃ for 5min, preserving heat at 175 ℃ for 5min, preserving heat at 350 ℃ for 10min, preserving heat at 400 ℃ for 15min, preserving heat at 500 ℃ for 30min, and the sintering rate is 2-15 ℃/min.
Further, in S5, CH3NH3PbI3The concentration of the solution is 0.75-1M, and the dripping amount is 1-3 mul.
The invention has the beneficial effects that:
according to the invention, the spacer layer and the carbon counter electrode in the preparation process of the full-printing perovskite solar cell are sintered together, and compared with the conventional method, the performance of the cell prepared by simplifying the sintering step keeps the original efficiency, the preparation time of the cell is shortened, and the energy consumption in the preparation process of the cell is reduced.
Description of the drawings:
FIG. 1 is a schematic diagram of the sintering process of the spacer layer and the carbon counter electrode of the example and the comparative example of the present invention;
FIG. 2 is a J-V plot of cells prepared according to examples of the present invention and comparative examples;
FIG. 3 is a bar graph of various performance parameters of cells prepared according to examples of the present invention and comparative examples;
fig. 4 is a graph comparing the performance parameters of the batteries prepared in the examples of the present invention and the comparative examples.
The specific implementation mode is as follows:
in order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The embodiment of the invention provides a method for rapidly preparing a fully-printed perovskite solar cell, which comprises the following steps:
s1, etching and cleaning FTO conductive substrate
Covering the part, which does not need to be etched, of the FTO conductive glass by using an adhesive tape, covering the exposed part by using zinc powder, dropwise adding an HCl solution (volume fraction is 10%) on the FTO conductive glass, staying for 15-30 s, washing away the zinc powder by using a large amount of clear water, removing the adhesive tape, after the etching of the conductive substrate is finished, ultrasonically cleaning the etched conductive substrate for 15min by using soap water, glass cleaning solution, absolute ethyl alcohol and distilled water respectively, then washing with the distilled water and the absolute ethyl alcohol in sequence, drying, and storing in a clean environment for later use.
S2 preparation of dense layer
Adding titanium tetrachloride into distilled water to prepare a dense layer precursor solution with the concentration of 50 mM; and (3) covering the part, which does not need to be provided with the compact layer, of the FTO conductive substrate obtained in the step (1) with a high-temperature adhesive tape, putting the FTO conductive substrate into the compact layer precursor solution, soaking for 30min at 70 ℃, taking out, sequentially washing with distilled water and absolute ethyl alcohol, drying, finally sintering the FTO conductive substrate for 30min at 500 ℃, heating at a rate of 10 ℃/min, annealing at a rate of 2-15 ℃/min, and taking out the substrate after the annealing is finished, and putting the substrate in a clean environment for later use.
S3 preparation of mesoporous layer
Adding TiO into the mixture2The slurry was printed on the FTO conductive substrate prepared in S2, left standing at room temperature for 10min,then drying at 70 ℃; subsequent treatment of TiO2Sintering the film, and cooling to room temperature; covering the part except the mesoporous layer with a high-temperature adhesive tape, putting the part into a 40mM titanium tetrachloride aqueous solution, and soaking the part for 30min at 70 ℃ until the titanium tetrachloride aqueous solution becomes light blue; then sequentially washing and drying the mixture by distilled water and absolute ethyl alcohol, and finally sintering the mixture, wherein the sintering process comprises the following steps: keeping the temperature at 112 ℃ for 5min, keeping the temperature at 175 ℃ for 5min, keeping the temperature at 350 ℃ for 10min, keeping the temperature at 400 ℃ for 15min, keeping the temperature at 500 ℃ for 30min, and taking out the substrate after the temperature rise rate is 10 ℃/min and placing the substrate in a clean environment for later use.
Preparation of S4, spacer layer and carbon counter electrode
S5、CH3NH3PbI3Filling in
Firstly, sticking an adhesive tape along the edge of a carbon counter electrode, and then preheating an FTO conductive substrate at 50 ℃; using pipette to remove small amount of CH3NH3PbI3Dripping 1-3 mul of precursor solution (with the concentration of 0.75-1M) on the surface of the carbon counter electrode, standing for 1min, and then transferring to a heating platform to heat for 1h at 70 ℃ to obtain the battery device.
The prior art (the spacing layer and the carbon counter electrode are sintered separately) is used as a comparative example, the performance of the solar cell prepared by the method is compared with that of the solar cell prepared by the embodiment 1 of the invention, and the result is shown in figures 2-4, and as can be seen from figures 2-4, compared with the conventional method, the method provided by the invention has the advantages that the spacing layer and the carbon counter electrode in the preparation process of the full-printing perovskite solar cell are sintered together, the battery prepared by simplifying the sintering step has the performance of the battery kept at the original efficiency, the preparation time of the battery is shortened, and the energy consumption in the preparation process of the battery is reduced.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention, it should be noted that, for those skilled in the art, several modifications and decorations without departing from the principle of the present invention should be regarded as the protection scope of the present invention.
Claims (9)
1. A method for rapidly preparing a fully printed perovskite solar cell is characterized by comprising the following steps:
s1, etching and cleaning an FTO conductive substrate:
covering the part of the FTO conductive glass which does not need to be etched by using an adhesive tape, covering the exposed part by using zinc powder, dropwise adding an HCl solution on the part, flushing the zinc powder and removing the adhesive tape after a period of time, after the conductive substrate is etched, respectively ultrasonically cleaning by using soap water, glass cleaning solution, absolute ethyl alcohol and distilled water, sequentially washing by using distilled water and absolute ethyl alcohol and drying for later use;
s2, preparation of the dense layer:
adding titanium tetrachloride into distilled water to prepare a compact layer precursor solution; covering the part, which does not need to be provided with the compact layer, of the FTO conductive substrate obtained in the step S1 by using a high-temperature adhesive tape, soaking the FTO conductive substrate in the compact layer precursor solution for a period of time, taking out, washing and drying the FTO conductive substrate by using distilled water and absolute ethyl alcohol in sequence, sintering the FTO conductive substrate, and annealing for later use;
s3, preparing a mesoporous layer:
adding TiO into the mixture2Printing the slurry on the FTO conductive substrate prepared in S2, standing at room temperature, and drying; subsequent treatment of TiO2Sintering the film, and cooling to room temperature; covering the part except the mesoporous layer by using a high-temperature adhesive tape, and putting the part into an aqueous solution of titanium tetrachloride for heating and soaking until the aqueous solution of titanium tetrachloride is changed into light blue; then sequentially washing with distilled water and absolute ethyl alcohol and drying; finally, sintering for later use;
preparation of S4, spacer layer and carbon counter electrode:
ZrO 2 is mixed with2Printing the slurry on the FTO conductive substrate prepared in the step S3, standing at room temperature, and then placing the FTO conductive substrate into an oven for presetting to form a spacing layer; then, printing carbon slurry on the FTO conductive substrate, standing at room temperature for a period of time, drying, and sintering for later use;
S5、CH3NH3PbI3filling:
firstly, sticking an adhesive tape along the edge of a carbon counter electrode, and then preheating an FTO conductive substrate at 50 ℃; mixing a small amount of CH3NH3PbI3And dripping the precursor solution on the surface of the carbon counter electrode, standing, and then transferring to a heating platform to heat for 1h at 70 ℃ to obtain the battery.
2. The method for rapid fabrication of fully printed perovskite solar cells according to claim 1, characterized in that: in S1, the volume fraction of HCl solution was 10%.
3. The method for rapid fabrication of fully printed perovskite solar cells according to claim 1, characterized in that: in S1, the etching time of the zinc powder and the HCl solution on the FTO conductive glass is 15-30S.
4. The method for rapid fabrication of fully printed perovskite solar cells according to claim 1, characterized in that: in S2, the annealing rate of the compact layer is 2-15 ℃/min.
5. The method for rapid fabrication of fully printed perovskite solar cells according to claim 1, characterized in that: in S2, the sintering process is as follows: keeping the temperature at 500 ℃ for 30min, wherein the heating rate is 10 ℃/min.
6. The method for rapid fabrication of fully printed perovskite solar cells according to claim 1, characterized in that: in S3, the sintering process is as follows: keeping the temperature at 112 ℃ for 5min, keeping the temperature at 175 ℃ for 5min, keeping the temperature at 350 ℃ for 10min, keeping the temperature at 400 ℃ for 15min, keeping the temperature at 500 ℃ for 30min, and keeping the sintering rate at 2-15 ℃/min.
7. The method for rapid fabrication of fully printed perovskite solar cells according to claim 1, characterized in that: in S4, after the spacer layer is printed, the temperature is kept at 126 ℃ for 6 min.
8. The method for rapid fabrication of fully printed perovskite solar cells according to claim 1, characterized in that: in S4, the sintering process comprises the steps of preserving heat at 112 ℃ for 5min, preserving heat at 175 ℃ for 5min, preserving heat at 350 ℃ for 10min, preserving heat at 400 ℃ for 15min and preserving heat at 500 ℃ for 30min, wherein the sintering rate is 2-15 ℃/min.
9. The method for rapid fabrication of fully printed perovskite solar cells according to claim 1, characterized in that: in S5, CH3NH3PbI3The concentration of the solution is 0.75-1M, and the dripping amount is 1-3 mul.
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Citations (5)
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| CN104091889A (en) * | 2014-07-24 | 2014-10-08 | 华中科技大学 | Semi-conductor perovskite solar cell and preparing method thereof |
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| CN105895804A (en) * | 2016-04-08 | 2016-08-24 | 武汉理工大学 | Low-cost perovskite solar cell and preparation method thereof |
| CN108922942A (en) * | 2018-06-12 | 2018-11-30 | 东南大学 | A kind of novel Mn:CsPbCl3From the preparation method of driving UV photodetector |
| WO2019080594A1 (en) * | 2017-10-24 | 2019-05-02 | 华中科技大学 | Ferroelectric-enhanced solar cell and preparation method therefor |
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- 2021-08-27 CN CN202110995555.4A patent/CN113707818A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104091889A (en) * | 2014-07-24 | 2014-10-08 | 华中科技大学 | Semi-conductor perovskite solar cell and preparing method thereof |
| CN105576135A (en) * | 2015-12-23 | 2016-05-11 | 华中科技大学 | Method for preparing large-area and all-solid-state perovskite mesoscopic solar cell and product |
| CN105895804A (en) * | 2016-04-08 | 2016-08-24 | 武汉理工大学 | Low-cost perovskite solar cell and preparation method thereof |
| WO2019080594A1 (en) * | 2017-10-24 | 2019-05-02 | 华中科技大学 | Ferroelectric-enhanced solar cell and preparation method therefor |
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Non-Patent Citations (1)
| Title |
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| 王亢: "无空穴传输层介观钙钛矿太阳能电池的印刷制备及优化", 中国优秀硕士学位论文全文数据库工程科技Ⅱ辑, 15 March 2018 (2018-03-15), pages 12 - 13 * |
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Application publication date: 20211126 |