CN113571648A - Apparatus and method for roll-to-roll fabrication of flexible perovskite and all-perovskite tandem solar cells - Google Patents

Apparatus and method for roll-to-roll fabrication of flexible perovskite and all-perovskite tandem solar cells Download PDF

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CN113571648A
CN113571648A CN202110753029.7A CN202110753029A CN113571648A CN 113571648 A CN113571648 A CN 113571648A CN 202110753029 A CN202110753029 A CN 202110753029A CN 113571648 A CN113571648 A CN 113571648A
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perovskite
chamber
roll
thermal annealing
transport layer
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CN113571648B (en
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袁宁一
钱斌辉
丁建宁
王书博
顾磊磊
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Yangzhou Carbon Neutrality Technology Innovation Research Center Of Yangzhou University
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Changzhou University
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    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
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    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
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Abstract

本发明属于太阳电池技术领域，具体涉及卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的装置及方法，装置包括依次设置的电子传输层制备模块、钙钛矿层制备模块、空穴传输层制备模块、电极制备模块以及放卷收卷模块；钙钛矿层制备模块包括钙钛矿前驱体印刷辊、溶剂萃取装置、热退火装置以及冷却氮气风刀。制备方法包括电子传输层制备、钙钛矿前驱体印刷、抽真空‑反溶剂‑抽真空萃取、热退火钙钛矿并进行冷却；空穴传输层制备；电极制备。采用该装置制备卷对卷柔性钙钛矿太阳能电池，能够实现对柔性基材的抽真空萃取，在溶剂萃取过程中柔性基材受到压力均匀，不会发生变形，产品质量高，并且兼容全钙钛矿叠层太阳能电池。The invention belongs to the technical field of solar cells, and in particular relates to a device and method for preparing flexible perovskite and full perovskite tandem solar cells by roll-to-roll. The device comprises an electron transport layer preparation module, a perovskite layer preparation module, an empty The hole transport layer preparation module, the electrode preparation module and the unwinding and winding module; the perovskite layer preparation module includes a perovskite precursor printing roller, a solvent extraction device, a thermal annealing device and a cooling nitrogen air knife. The preparation method includes electron transport layer preparation, perovskite precursor printing, vacuum-antisolvent-vacuum extraction, thermal annealing perovskite and cooling; hole transport layer preparation; electrode preparation. The device is used to prepare roll-to-roll flexible perovskite solar cells, which can realize vacuum extraction of flexible substrates. During the solvent extraction process, the flexible substrates are subjected to uniform pressure without deformation. The product has high quality and is compatible with all calcium. Titanite tandem solar cells.

Description

Device and method for preparing flexible perovskite and all-perovskite laminated solar cell in roll-to-roll mode
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to a device and a method for preparing flexible perovskite and full perovskite laminated solar cells in a roll-to-roll mode.
Background
The small area efficiency of perovskite solar cells has exceeded 25.5%, but almost all published literature uses either an anti-solvent spin coating or a two-step spin coating process. In particular, spin-on anti-solvent methods tend to have uncontrollable factors that promote perovskite thin film formation and cannot scale up to sizes of 5 x 5cm or more. For perovskite solar cell commercialization, larger areas of perovskite thin films are required.
The existing flexible solar cell has wide prospect due to the advantages of light weight, portability, low cost, excellent performance and the like, can be used on equipment such as a solar backpack, a solar open, a solar sailboat and the like, and can also be integrated on a window, a roof, an outer wall or an inner wall. Patent CN 111710783 a discloses a preparation scheme of a large-area perovskite solar cell, which aims at extracting perovskite on a rigid substrate by using a perovskite wet film reduced pressure distillation method, but the scheme placed on a flexible substrate can cause the base material to be seriously deformed, and cannot be applied to a continuous substrate. The patent CN 111341919A for extracting perovskite by means of anti-solvent soaking is very easy to cause over-extraction, and the quality of the prepared battery has uncertainty. Patent CN 1084287987 a provides a roll coating process that can be applied to flexible substrates, but is far from sufficient to form high quality thin films by simply blow-drying thermal annealing after applying the perovskite solution.
Disclosure of Invention
The invention aims to solve the technical problem that a device and a method for preparing flexible perovskite and full perovskite laminated solar cells in a roll-to-roll mode are provided based on a perovskite preparation method, and the perovskite on a flexible substrate is subjected to a process of vacuumizing, anti-solvent and vacuumizing extraction, so that ligand solvent in a perovskite precursor solution is fully extracted. The method can avoid the deformation of the flexible substrate while using the vacuum extraction, prepare the high-quality perovskite thin film and is compatible with the full perovskite tandem solar cell.
The technical scheme adopted by the invention is a device for preparing flexible perovskite and all-perovskite laminated solar cells in a roll-to-roll mode. The device comprises an electron transport layer preparation module (1), a perovskite layer preparation module (2), a hole transport layer preparation module (3), an electrode preparation module (4) and an unreeling and reeling module (5) which are sequentially arranged; the unreeling and reeling module (5) comprises a flexible base material (51), and the flexible base material (51) sequentially passes through the modules; the perovskite layer preparation module (2) comprises a perovskite precursor printing roller (21), a solvent extraction device (22), a thermal annealing device (23) and a cooling nitrogen air knife (24) which are sequentially arranged; the solvent extraction device (22) comprises an evacuating device A (221), an anti-solvent extraction chamber (222) and an evacuating device B (223) which are sequentially arranged, wherein the evacuating device A (221) comprises an upper evacuating chamber (2211) and a lower evacuating chamber (2212), the upper evacuating chamber (2211) is connected with a vacuum pump (2213) and is connected with a pressure gauge (2214) above the upper evacuating chamber (2211), the lower evacuating chamber (2212) is connected with a vacuum pump (2215) and is connected with a pressure gauge (2216) below the lower evacuating chamber (2212); introducing anti-solvent gas into the anti-solvent extraction chamber (222); the vacuumizing device B (223) comprises an upper vacuumizing chamber (2231) and a lower vacuumizing chamber (2232), wherein the upper vacuumizing chamber (2231) is connected with a vacuum pump (2233), and is connected with a pressure gauge (2234) above the upper vacuumizing chamber (2231), and the lower vacuumizing chamber (2232) is connected with a vacuum pump (2235), and is connected with a pressure gauge (2236) below the lower vacuumizing chamber (2232); the thermal annealing device (23) comprises a thermal annealing chamber (231), and a hot plate (232) is arranged inside the thermal annealing chamber (231).
The electron transport layer preparation module (1) comprises an electron transport layer printing roller (11), a thermal annealing device (12) and a cooling nitrogen air knife (13) which are sequentially arranged, wherein the thermal annealing device (12) comprises a thermal annealing chamber (121), and a hot plate (122) is placed inside the thermal annealing chamber (121).
In the vacuum extractor A (221), the flexible base material (51) is sandwiched between the upper vacuum-extracting chamber (2211) and the lower vacuum-extracting chamber (2212) to form a closed space, and the first solvent extraction is performed.
The anti-solvent gas enters an anti-solvent extraction chamber (222) for a second solvent extraction.
In the vacuum extractor B (223), the flexible substrate is clamped between the upper vacuum-extracting chamber (2231) and the lower vacuum-extracting chamber (2232) to form a closed space, and the solvent extraction is carried out for the third time.
The hole transport layer preparation module (3) comprises a hole transport layer printing roller (31) and a blow-drying nitrogen air knife (32) which are sequentially arranged.
The electrode preparation module (4) comprises an electrode printing roller (41), a thermal annealing device (42) and a cooling nitrogen air knife (43), wherein the thermal annealing device (42) comprises a thermal annealing chamber (421), and a hot plate (422) is placed inside the thermal annealing chamber (421).
The unreeling and reeling module (5) comprises a flexible base material (51), an unreeling roller (52), a plurality of supporting rollers (53) arranged along the base material transmission direction and a reeling roller (54).
The method for preparing the flexible perovskite and all-perovskite laminated solar cell in a roll-to-roll mode comprises the following steps: preparing an electron transport layer; printing a perovskite precursor, vacuumizing, anti-solvent, vacuumizing, extracting, thermally annealing and cooling; preparing a hole transport layer; and (4) preparing an electrode. The method comprises the following specific steps:
s1, printing the electron transfer layer on the flexible base material through an electron transfer layer printing roller, annealing in a thermal annealing device, adjusting the temperature of a hot plate, controlling the base material to anneal at 150 ℃ for 15min, and cooling by using a cooling nitrogen air knife to obtain a sample 1.
S2, printing a perovskite layer on the cooled sample 1 through a perovskite precursor printing roller, reducing the pressure inside the chamber to 10-1000pa through a vacuumizing device A, extracting the solvent in the chamber through an anti-solvent filled with chlorobenzene anti-solvent gas, reducing the pressure inside the chamber to 10-1000pa through a vacuumizing device B, fully extracting the ligand solvent to nucleate perovskite, annealing at 100 ℃ for 20min in a thermal annealing device, and cooling by using a cooling nitrogen air knife to obtain a sample 2.
And S3, printing the hole transport layer on the cooled sample 2 through a hole transport layer printing roller, and drying the hole transport layer by using a drying nitrogen air knife to obtain a sample 3.
S4, sample 3 was printed with an electrode by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife to obtain sample 4.
The resulting sample 3 was used as a flexible substrate (51), and the processes of S1 to S4 were performed again, whereby a full perovskite tandem flexible solar cell was prepared.
The invention has the following beneficial effects:
(1) printing a perovskite wet film, after the perovskite wet film enters an evacuation chamber, simultaneously starting a mechanical pump at two sides, synchronously reducing the pressure at two sides of a flexible substrate, partially volatilizing a ligand solvent in the wet film, avoiding the deformation of the flexible substrate, inflating a cavity, then entering an anti-solvent chamber by the perovskite film, further extracting the ligand solvent in the wet film, and finally entering the evacuation chamber again to ensure that the ligand solvent in the wet film is thoroughly volatilized.
(2) The ligand solvent is fully extracted by adopting the operations of vacuumizing, anti-solvent and vacuumizing, so that the prepared perovskite film has better compactness and better battery stability;
(3) the method can be suitable for preparing perovskite solar cells with different flexible substrates and different types.
(4) The invention can prepare the all-perovskite laminated solar cell on the basis of preparing the flexible perovskite solar cell.
Description of the drawings:
in order to more clearly illustrate the technical solution in the embodiments of the present invention, the following briefly describes the accompanying drawings.
Fig. 1 is a schematic diagram of an apparatus for roll-to-roll preparation of flexible perovskite and all-perovskite tandem solar cells.
Fig. 2 is a schematic view of the evacuation device a.
Fig. 3 is a schematic view of the evacuation device B.
The figures are labeled as follows: 1. an electronic transmission layer preparation module; 11. an electron transport layer printing roller; 12. a thermal annealing device; 121. a thermal annealing chamber; 122. a hot plate; 13 cooling the nitrogen air knife; 2. a perovskite layer preparation module; 21. a perovskite precursor printing roller; 2. a solvent extraction module; 221. a vacuumizing device A; 2211. an upper vacuum pumping chamber; 2212. a lower evacuated chamber; 2213. a vacuum pump; 2214. a pressure gauge; 2215. a vacuum pump; 2216. a pressure gauge; 222. an anti-solvent extraction chamber; 223. a vacuumizing device B; 2231. an upper vacuum pumping chamber; 2232. a lower evacuated chamber; 2233. a vacuum pump; 2234. a pressure gauge; 2235. a vacuum pump; 2236. a pressure gauge; 23. a thermal annealing device; 231. a thermal annealing chamber; 232. a hot plate; 24. cooling the nitrogen air knife; 3. a hole transport layer preparation module; 31. a hole transport layer printing roller; 32. drying the nitrogen air knife; 4. an electrode preparation module; 41. an electrode printing roller; 42. a thermal annealing device; 421. a thermal annealing chamber; 422. a hot plate; 43. cooling the nitrogen air knife; 5. an unreeling and reeling module; 51. a flexible substrate; 52. unwinding rollers; 53. a support roller; 54. and (7) winding the roller.
FIG. 4 is an X-ray diffraction pattern of perovskite thin films prepared by different perovskite layer preparation methods.
FIG. 5 is a J-V plot of solar cells made by different perovskite layer fabrication methods.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below.
Example 1
The device for preparing the flexible perovskite and all-perovskite laminated solar cell in a roll-to-roll mode comprises an electron transport layer preparation module (1), a perovskite layer preparation module (2), a hole transport layer preparation module (3), an electrode preparation module (4) and an unreeling and reeling module (5) which are sequentially arranged; the unreeling and reeling module (5) comprises a flexible base material (51), and the flexible base material (51) sequentially passes through the modules; the perovskite layer preparation module (2) comprises a perovskite precursor printing roller (21), a solvent extraction device (22), a thermal annealing device (23) and a cooling nitrogen air knife (24) which are sequentially arranged; the solvent extraction device (22) comprises an evacuating device A (221), an anti-solvent extraction chamber (222) and an evacuating device B (223) which are sequentially arranged, wherein the evacuating device A (221) comprises an upper evacuating chamber (2211) and a lower evacuating chamber (2212), the upper evacuating chamber (2211) is connected with a vacuum pump (2213) and is connected with a pressure gauge (2214) above the upper evacuating chamber (2211), the lower evacuating chamber (2212) is connected with a vacuum pump (2215) and is connected with a pressure gauge (2216) below the lower evacuating chamber (2212); introducing anti-solvent gas into the anti-solvent extraction chamber (222); the vacuumizing device B (223) comprises an upper vacuumizing chamber (2231) and a lower vacuumizing chamber (2232), wherein the upper vacuumizing chamber (2231) is connected with a vacuum pump (2233), and is connected with a pressure gauge (2234) above the upper vacuumizing chamber (2231), and the lower vacuumizing chamber (2232) is connected with a vacuum pump (2235), and is connected with a pressure gauge (2236) below the lower vacuumizing chamber (2232); the thermal annealing device (23) comprises a thermal annealing chamber (231), and a hot plate (232) is arranged inside the thermal annealing chamber (231).
In practical application, in the vacuum extractor a, the flexible substrate is sandwiched between the upper vacuum-extracting chamber and the lower vacuum-extracting chamber to form a closed space, and the first solvent extraction is performed.
In practical applications, the anti-solvent gas enters the anti-solvent extraction chamber for a second solvent extraction.
In practical application, the flexible substrate in the vacuum extractor B is clamped between the upper vacuum-pumping chamber and the lower vacuum-pumping chamber to form a closed space for the third solvent extraction.
The electron transport layer preparation module (1) comprises an electron transport layer printing roller (11), a thermal annealing device (12) and a cooling nitrogen air knife (13) which are sequentially arranged, wherein the thermal annealing device (12) comprises a thermal annealing chamber (121), and a hot plate (122) is placed inside the thermal annealing chamber (121).
The hole transport layer preparation module (3) comprises a hole transport layer printing roller (31) and a blow-drying nitrogen air knife (32) which are sequentially arranged.
The electrode preparation module (4) comprises an electrode printing roller (41), a thermal annealing device (42) and a cooling nitrogen air knife (43), wherein the thermal annealing device (42) comprises a thermal annealing chamber (421), and a hot plate (422) is placed inside the thermal annealing chamber (421).
The unreeling and reeling module (5) comprises a flexible base material (51), an unreeling roller (52), a plurality of supporting rollers (53) arranged along the base material transmission direction and a reeling roller (54).
The method for preparing the flexible perovskite and all-perovskite laminated solar cell in a roll-to-roll mode comprises the following steps: preparing an electron transport layer; printing a perovskite precursor, vacuumizing, anti-solvent, vacuumizing, extracting, thermally annealing and cooling; preparing a hole transport layer; and (4) preparing an electrode.
S1, printing the electron transport layer SnO on the flexible base material (51) PET through an electron transport layer printing roller2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 150 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 1.
S2, cooled sample 1, perovskite layer (MAPbI) printing by perovskite precursor printing roller3) Then, the pressure inside the chamber was reduced to 10pa by the vacuum extractor A, and the solvent was extracted by the anti-solvent extraction chamber filled with chlorobenzene gas (the concentration of chlorobenzene in the chamber was 1 ml/cm)3) And finally, reducing the pressure inside the chamber to 10pa by using a vacuumizing device B to fully extract the ligand solvent so as to nucleate the perovskite, finally, annealing for 20min at 100 ℃ in a thermal annealing device to obtain the thickness of the perovskite layer of 600nm, and then cooling by using a cooling nitrogen air knife to obtain a sample 2.
S3, printing the cooled sample 2 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 3.
S4, sample 3 was printed with a carbon electrode having a thickness of 1 μm by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife, to obtain sample 4.
Example 2
S1, printing the electron transport layer SnO on the flexible base material PET through an electron transport layer printing roller2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 150 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 1.
S2, cooled sample 1, perovskite layer (MAPbI) printing by perovskite precursor printing roller3) Then, the pressure inside the chamber was reduced to 10pa by the vacuum extractor A, and the solvent was extracted by the anti-solvent extraction chamber filled with chlorobenzene gas (the concentration of chlorobenzene in the chamber was 1 ml/cm)3) Finally, the pressure in the chamber is reduced to 500p by a vacuum pumping device Ba, fully extracting a ligand solvent to nucleate perovskite, finally annealing for 20min at 100 ℃ in a thermal annealing device to obtain a perovskite layer with the thickness of 600nm, and then cooling by using a cooling nitrogen air knife to obtain a sample 2.
S3, printing the cooled sample 2 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 3.
S4, sample 3 was printed with a carbon electrode having a thickness of 1 μm by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife, to obtain sample 4.
Example 3
S1, printing the electron transport layer SnO on the flexible base material PET through an electron transport layer printing roller2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 150 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 1.
S2, cooled sample 1, perovskite layer (MAPbI) printing by perovskite precursor printing roller3) Then, the pressure inside the chamber was reduced to 500pa by the vacuum extractor A, and the solvent was extracted by the anti-solvent extraction chamber filled with chlorobenzene gas (chlorobenzene concentration in the chamber was 1 ml/cm)3) And finally, reducing the pressure inside the chamber to 500pa by using a vacuumizing device B to fully extract the ligand solvent so as to nucleate the perovskite, finally, annealing for 20min at 100 ℃ in a thermal annealing device to obtain the thickness of the perovskite layer of 600nm, and then cooling by using a cooling nitrogen air knife to obtain a sample 2.
S3, printing the cooled sample 2 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 3.
S4, sample 3 was printed with a carbon electrode having a thickness of 1 μm by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife, to obtain sample 4.
Example 4
S1, printing the electron transfer layer S on the flexible base material PET through the electron transfer layer printing rollernO2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 150 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 1.
S2, cooled sample 1, perovskite layer (MAPbI) printing by perovskite precursor printing roller3) Then, the pressure inside the chamber was reduced to 500pa by the vacuum extractor A, and the solvent was extracted by the anti-solvent extraction chamber filled with chlorobenzene gas (chlorobenzene concentration in the chamber was 1 ml/cm)3) And finally, reducing the pressure inside the chamber to 1000pa by using a vacuumizing device B to fully extract the ligand solvent so as to nucleate the perovskite, finally, annealing for 20min at 100 ℃ in a thermal annealing device to obtain the thickness of the perovskite layer of 600nm, and then cooling by using a cooling nitrogen air knife to obtain a sample 2.
S3, printing the cooled sample 2 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 3.
S4, sample 3 was printed with a carbon electrode having a thickness of 1 μm by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife, to obtain sample 4.
Example 5
S1, printing the electron transport layer SnO on the flexible base material PET through an electron transport layer printing roller2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 150 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 1.
S2, cooled sample 1, perovskite layer (MAPbI) printing by perovskite precursor printing roller3) Then, the pressure inside the chamber was reduced to 1000Pa by the evacuation device A, and the solvent was extracted by the anti-solvent extraction chamber filled with chlorobenzene gas (the concentration of chlorobenzene in the chamber was 1 ml/cm)3) And finally, reducing the pressure inside the chamber to 1000pa by using a vacuumizing device B to fully extract the ligand solvent so as to nucleate the perovskite, finally, annealing for 20min at 100 ℃ in a thermal annealing device to obtain the thickness of the perovskite layer of 600nm, and then cooling by using a cooling nitrogen air knife to obtain a sample 2.
S3, printing the cooled sample 2 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 3.
S4, sample 3 was printed with a carbon electrode having a thickness of 1 μm by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife, to obtain sample 4.
Example 6
S1, printing the electron transport layer SnO on the flexible base material PET through an electron transport layer printing roller2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 150 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 1.
S2, sample 1 after cooling was printed with a perovskite precursor printing roll to form a perovskite layer (Cs)0.1FA0.9PbI2.1Br0.9) Then, the pressure inside the chamber was reduced to 500pa by the vacuum extractor A, and the solvent was extracted by the anti-solvent extraction chamber filled with chlorobenzene gas (chlorobenzene concentration in the chamber was 1 ml/cm)3) And finally, reducing the pressure inside the chamber to 500pa by using a vacuumizing device B to fully extract the ligand solvent so as to nucleate the perovskite, finally annealing the perovskite in a thermal annealing device at 100 ℃ for 30min to obtain the thickness of the perovskite layer of 600nm, and then cooling the perovskite layer by using a cooling nitrogen air knife to obtain a sample 2.
S3, printing the cooled sample 2 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 3.
S4 printing of an electron transport layer SnO on the sample 3 by an electron transport layer printing roll2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 100 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 4.
S5, sample 4 after cooling was printed with a perovskite precursor printing roll to form a perovskite layer (Cs)0.1FA0.9Pb0.5Sn0.5I3) Then by pumpingThe vacuum device A reduced the pressure inside the chamber to 500pa, and the solvent was extracted from the chamber by an anti-solvent filled with chlorobenzene gas (the concentration of chlorobenzene in the chamber was 1 ml/cm)3) And finally, reducing the pressure inside the chamber to 500pa by using a vacuumizing device B to fully extract the ligand solvent so as to nucleate the perovskite, finally, annealing for 20min at 100 ℃ in a thermal annealing device to obtain the thickness of the perovskite layer of 600nm, and then cooling by using a cooling nitrogen air knife to obtain a sample 5.
S6, printing the cooled sample 5 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 6.
S7, sample 3 was printed with a carbon electrode having a thickness of 1 μm by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife, to obtain sample 7.
Comparative example 1
S1, printing the electron transport layer SnO on the flexible base material PET through an electron transport layer printing roller2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 150 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 1.
S2, cooled sample 1, perovskite layer (MAPbI) printing by perovskite precursor printing roller3) And then reducing the pressure inside the chamber to 500pa by a vacuumizing device to nucleate the perovskite, finally annealing for 20min at 100 ℃ in a thermal annealing device to obtain the thickness of the perovskite layer to be 600nm, and then cooling by using a cooling nitrogen air knife to obtain a sample 2.
S3, printing the cooled sample 2 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 3.
S4, sample 3 was printed with a carbon electrode having a thickness of 1 μm by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife, to obtain sample 4.
Comparative example 2
S1, printing roll marks on the flexible base material PET through an electron transport layerBrush electron transport layer SnO2And the thickness was 30nm, and then annealing was performed in a thermal annealing apparatus, and the substrate was annealed at 150 ℃ for 15min by adjusting the temperature of the hot plate, followed by cooling using a cooling nitrogen air knife, to obtain sample 1.
S2, cooled sample 1, perovskite layer (MAPbI) printing by perovskite precursor printing roller3) Then, the pressure inside the chamber was reduced to 500pa by the vacuum extractor A, and the solvent was extracted by the anti-solvent extraction chamber filled with chlorobenzene gas (chlorobenzene concentration in the chamber was 1 ml/cm)3) And nucleating the perovskite, finally annealing for 20min at 100 ℃ in a thermal annealing device to obtain the perovskite layer with the thickness of 600nm, and then cooling by using a cooling nitrogen air knife to obtain a sample 2.
S3, printing the cooled sample 2 with a hole transport layer Spiro-oMeTAD through a hole transport layer printing roller, wherein the thickness is 400nm, and drying the sample by using a drying nitrogen air knife to obtain a sample 3.
S4, sample 3 was printed with a carbon electrode having a thickness of 1 μm by an electrode printing roll, solidified by a thermal annealing apparatus, and then cooled by a cooling nitrogen air knife, to obtain sample 4.
Table 1 photovoltaic performance of perovskite solar cells prepared in examples and comparative examples
Figure BDA0003145782500000121
It should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept of the present invention, and these changes and modifications belong to the protection scope of the present invention.

Claims (9)

1.卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的装置，其特征在于，所述装置包含依次设置的电子传输层制备模块(1)，钙钛矿层制备模块(2)，空穴传输层制备模块(3)，电极制备模块(4)以及放卷收卷模块(5)；所述放卷收卷模块(5)包含柔性基材(51)，柔性基材(51)依次经过各个模块；所述钙钛矿层制备模块(2)包含依次设置的钙钛矿前驱体印刷辊(21)、溶剂萃取装置(22)、热退火装置(23)、冷却氮气风刀(24)；所述溶剂萃取装置(22)包含依次设置的抽真空装置A(221)、反溶剂萃取腔室(222)、抽真空装置B(223)，所述抽真空装置A(221)包含上抽真空腔室(2211)和下抽真空腔室(2212)，上抽真空腔室(2211)与真空泵(2213)连接，并在上抽真空腔室(2211)上方与压力表(2214)连接，下抽真空腔室(2212)与真空泵(2215)连接，并在下抽真空腔室(2212)下方与压力表(2216)连接；所述反溶剂萃取腔室(222)中通入反溶剂气体；所述抽真空装置B(223)包含上抽真空腔室(2231)和下抽真空腔室(2232)，上抽真空腔室(2231)与真空泵(2233)连接，并在上抽真空腔室(2231)上方与压力表(2234)连接，下抽真空腔室(2232)与真空泵(2235)连接，并在下抽真空腔室(2232)下方与压力表(2236)连接；所述热退火装置(23)包含有一个热退火腔室(231)，在热退火腔室(231)内部放置有一个热板(232)。1. A device for preparing flexible perovskite and full perovskite tandem solar cells by roll-to-roll, characterized in that the device comprises an electron transport layer preparation module (1) arranged in sequence, a perovskite layer preparation module (2) , a hole transport layer preparation module (3), an electrode preparation module (4) and an unwinding and winding module (5); the unwinding and winding module (5) comprises a flexible substrate (51), a flexible substrate (51) ) passes through each module in sequence; the perovskite layer preparation module (2) comprises a perovskite precursor printing roller (21), a solvent extraction device (22), a thermal annealing device (23), a cooling nitrogen air knife ( 24); the solvent extraction device (22) comprises an evacuation device A (221), an anti-solvent extraction chamber (222), and a vacuum evacuation device B (223) that are arranged in sequence, and the evacuation device A (221) includes The upper vacuum chamber (2211) and the lower vacuum chamber (2212), the upper vacuum chamber (2211) is connected to the vacuum pump (2213), and is connected to the pressure gauge (2214) above the upper vacuum chamber (2211) connected, the lower vacuum chamber (2212) is connected with the vacuum pump (2215), and is connected with the pressure gauge (2216) under the lower vacuum chamber (2212); the anti-solvent extraction chamber (222) is fed with an anti-solvent gas; the vacuum device B (223) includes an upper vacuum chamber (2231) and a lower vacuum chamber (2232), the upper vacuum chamber (2231) is connected to the vacuum pump (2233), and the upper vacuum chamber (2233) is evacuated The upper part of the chamber (2231) is connected with the pressure gauge (2234), the lower vacuum chamber (2232) is connected with the vacuum pump (2235), and the lower part of the lower vacuum chamber (2232) is connected with the pressure gauge (2236); The annealing device (23) includes a thermal annealing chamber (231), and a hot plate (232) is placed inside the thermal annealing chamber (231). 2.根据权利要求1所述的卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的装置，其特征在于：电子传输层制备模块(1)包含有依次设置的电子传输层印刷辊(11)、热退火装置(12)及冷却氮气风刀(13)，其中，热退火装置(12)包含有一个热退火腔室(121)，在热退火腔室(121)内部放置有一个热板(122)。2. The device for preparing flexible perovskite and full perovskite tandem solar cells by roll-to-roll according to claim 1, characterized in that: the electron transport layer preparation module (1) comprises electron transport layer printing arranged in sequence A roll (11), a thermal annealing device (12) and a cooling nitrogen air knife (13), wherein the thermal annealing device (12) includes a thermal annealing chamber (121), and a thermal annealing chamber (121) is placed inside the thermal annealing chamber (121). A hot plate (122). 3.根据权利要求1所述的卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的装置，其特征在于：空穴传输层制备模块(3)包含有依次设置的空穴传输层印刷辊(31)、吹干氮气风刀(32)。3. The device for preparing flexible perovskite and all-perovskite tandem solar cells by roll-to-roll according to claim 1, wherein the hole transport layer preparation module (3) comprises sequentially arranged hole transport Layer printing roller (31), dry nitrogen air knife (32). 4.根据权利要求1所述的卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的装置，其特征在于：电极制备模块(4)包含有依次设置的电极印刷辊(41)、热退火装置(42)和冷却氮气风刀(43)，其中，热退火装置(42)包含有一个热退火腔室(421)，在热退火腔室(421)内部放置有一个热板(422)。4. The device for preparing flexible perovskite and full perovskite tandem solar cells by roll-to-roll according to claim 1, wherein the electrode preparation module (4) comprises electrode printing rollers (41) arranged in sequence , a thermal annealing device (42) and a cooling nitrogen air knife (43), wherein the thermal annealing device (42) includes a thermal annealing chamber (421), and a hot plate (421) is placed inside the thermal annealing chamber (421). 422). 5.根据权利要求1所述的卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的装置，其特征在于：放卷收卷模块(5)包含有柔性基材(51)、放卷辊(52)、沿基材传输方向设置的支撑辊(53)以及收卷辊(54)。5. The device for preparing flexible perovskite and full perovskite tandem solar cells by roll-to-roll according to claim 1, wherein the unwinding and winding module (5) comprises a flexible substrate (51), An unwinding roller (52), a supporting roller (53) arranged along the conveying direction of the substrate, and a winding roller (54). 6.卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的方法，其特征在于，所述方法步骤如下：6. A method for preparing flexible perovskite and full perovskite tandem solar cells by roll-to-roll, wherein the method steps are as follows: S1、将柔性基材(51)通过电子传输层印刷辊(11)印刷电子传输层，然后进入热退火装置(12)内进行退火，调整热板(122)温度，控制基材150℃退火15min，随后使用冷却氮气风刀(13)冷却，得到样品1。S1. The flexible substrate (51) is passed through the electron transport layer printing roller (11) to print the electron transport layer, then enters the thermal annealing device (12) for annealing, adjusts the temperature of the hot plate (122), and controls the substrate to anneal at 150°C for 15 minutes , followed by cooling with a cooling nitrogen air knife (13) to obtain sample 1. S2、冷却后的样品1通过钙钛矿前驱体印刷辊(21)印刷钙钛矿层，然后通过抽真空装置A(221)使腔室内部压强降为10-1000pa，再通过充满氯苯反溶剂气体的反溶剂萃取腔室(222)萃取溶剂、最后通过抽真空装置B(223)使腔室内部压强降为10-1000pa充分萃取配体溶剂，使钙钛矿成核，最后进入热退火装置(23)在100℃下退火20min，并使用冷却氮气风刀(24)冷却，得到样品2。S2. The cooled sample 1 is printed with a perovskite layer by the perovskite precursor printing roller (21), and then the pressure inside the chamber is reduced to 10-1000pa by the vacuum pumping device A (221), and then filled with chlorobenzene anti-solvent The gas anti-solvent extraction chamber (222) extracts the solvent, and finally reduces the pressure inside the chamber to 10-1000pa through the vacuum pumping device B (223) to fully extract the ligand solvent, nucleates the perovskite, and finally enters the thermal annealing device (23) Annealing at 100° C. for 20 min and cooling with a cooling nitrogen air knife (24) to obtain sample 2. S3、冷却后的样品2通过空穴传输层印刷辊(31)印刷空穴传输层，并使用吹干氮气风刀(32)进行吹干，得到样品3。S3. The cooled sample 2 prints the hole transport layer through the hole transport layer printing roller (31), and is blown dry with a nitrogen air knife (32) to obtain the sample 3. S4、对样品3通过电极印刷辊(41)印刷电极，使用热退火装置(42)进行固化后使用冷却氮气风刀(431)进行冷却，得到样品4大面积柔性钙钛矿太阳能电池。S4. Print electrodes on sample 3 through an electrode printing roller (41), use a thermal annealing device (42) to solidify, and then use a cooling nitrogen air knife (431) for cooling to obtain sample 4 large-area flexible perovskite solar cells. 7.根据权利要求6所述的卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的方法，其特征在于：柔性基材(51)为PET、PEN、柔性钙钛矿膜。7. The roll-to-roll method for preparing flexible perovskite and full perovskite tandem solar cells according to claim 6, wherein the flexible substrate (51) is PET, PEN, or flexible perovskite film. 8.根据权利要求6所述的卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的方法，其特征在于：抽真空装置A(221)中，柔性基材(51)夹于上抽真空腔室(2211)和下抽真空腔室(2212)之间形成密闭空间，进行第一次溶剂萃取；反溶剂气体进入反溶剂萃取腔室(222)中，进行进行第二次溶剂萃取；抽真空装置B(223)中，柔性基材夹于上抽真空腔室(2231)和下抽真空腔室(2232)之间形成密闭空间，进行第三次溶剂萃取。8. The roll-to-roll method for preparing flexible perovskite and full perovskite tandem solar cells according to claim 6, characterized in that: in the vacuum device A (221), the flexible substrate (51) is sandwiched between A closed space is formed between the upper vacuum chamber (2211) and the lower vacuum chamber (2212), and the first solvent extraction is performed; the anti-solvent gas enters the anti-solvent extraction chamber (222), and the second solvent extraction is performed Extraction: In the vacuum device B (223), the flexible substrate is sandwiched between the upper vacuum chamber (2231) and the lower vacuum chamber (2232) to form a closed space, and the third solvent extraction is performed. 9.根据权利要求6所述的卷对卷制备柔性钙钛矿以及全钙钛矿叠层太阳电池的方法，其特征在于：将得到的样品3作为柔性基材(51)，再次进行S1至S4的工艺，制备全钙钛矿叠层柔性太阳能电池。9. The method for preparing flexible perovskite and full perovskite tandem solar cells by roll-to-roll according to claim 6, characterized in that: using the obtained sample 3 as a flexible substrate (51), performing S1 to S4 process to prepare all perovskite tandem flexible solar cells.
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