CN111341919A - Continuous preparation process and device for preparing perovskite thin film in roll-to-roll mode by one-step method - Google Patents
Continuous preparation process and device for preparing perovskite thin film in roll-to-roll mode by one-step method Download PDFInfo
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- CN111341919A CN111341919A CN202010154904.5A CN202010154904A CN111341919A CN 111341919 A CN111341919 A CN 111341919A CN 202010154904 A CN202010154904 A CN 202010154904A CN 111341919 A CN111341919 A CN 111341919A
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- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000010409 thin film Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000576 coating method Methods 0.000 claims abstract description 64
- 239000011248 coating agent Substances 0.000 claims abstract description 57
- 238000000605 extraction Methods 0.000 claims abstract description 40
- 238000000137 annealing Methods 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 37
- 238000001035 drying Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000004804 winding Methods 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 13
- 239000012296 anti-solvent Substances 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims description 41
- 239000010408 film Substances 0.000 claims description 15
- 230000007704 transition Effects 0.000 claims description 15
- 238000003825 pressing Methods 0.000 claims description 12
- 238000010030 laminating Methods 0.000 claims description 11
- 238000010924 continuous production Methods 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 238000000638 solvent extraction Methods 0.000 abstract description 4
- 238000010899 nucleation Methods 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- KTSFMFGEAAANTF-UHFFFAOYSA-N [Cu].[Se].[Se].[In] Chemical compound [Cu].[Se].[Se].[In] KTSFMFGEAAANTF-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
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- H—ELECTRICITY
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- 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
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- H—ELECTRICITY
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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
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
- H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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Abstract
The invention discloses a process and a device for continuously preparing a perovskite thin film by one-step roll-to-roll preparation, wherein an unreeling device, a coating device, a drying device, an extracting device, an annealing device and a reeling device are sequentially arranged along the conveying direction of a base material, the unreeling device comprises an unreeling shaft and a plurality of supporting rolls arranged along the conveying direction of the base material, the coating device comprises a coating back roll and a slit die head, and coating liquid is supplied to one side of the slit die head, which faces the coating back roll; the drying device comprises a drying box body and a heating device arranged in the drying box body; the extraction device comprises an extraction tank and a guide roller group in the extraction tank, an anti-solvent corresponding to the coating liquid is arranged in the extraction tank, the annealing device comprises an annealing box body and a heating device arranged in the annealing box body, the winding device comprises a winding shaft, anti-solvent extraction is carried out on the perovskite layer, nucleation and growth of crystals can be greatly promoted, and therefore the perovskite thin film with good crystallization, compact arrangement and smooth surface is obtained.
Description
Technical Field
The invention relates to the technical field of photovoltaic cells, in particular to a continuous preparation process and device for preparing a perovskite thin film in a roll-to-roll manner by a one-step method.
Background
Perovskite solar cells have evolved over a short number of years and their performance has exceeded the maximum efficiency of semiconductor compounds used in solar cells, such as CdTe and CIGS (copper indium gallium selenide), over the last decade. Perovskite thin films can be prepared by a simple and inexpensive solution coating process, and have great potential in commercial solar cells. The one-step process is to prepare the perovskite into a solution, coat the solution on the surface of a substrate, and then carry out solvent extraction and high-temperature annealing to finally obtain the perovskite thin film.
In the reports of preparing large-area perovskite thin films by one-step method, a flat plate coating is utilized to heat a substrate for high-temperature coating, but the discontinuous coating has large difficulty in controlling process repeatability and much lower production efficiency than roll-to-roll coating.
Some have used roll-to-roll coating, followed by coating the perovskite and then solvent extraction using spray coating or slot coating of an anti-solvent. The method needs two continuous coating, has complex process control and needs strict control on the operation parameters of the anti-solvent, but the one-step method is only in the production mode of flat coating, but the flat coating is discontinuous coating, has great difficulty in process repeatability control, has much lower production efficiency than roll-to-roll coating, and has the improvement in the prior art.
Disclosure of Invention
In order to solve the technical problems, the invention provides a continuous preparation device for preparing a perovskite film in a roll-to-roll manner by a one-step method, and the continuous preparation device can be used for carrying out anti-solvent extraction on a perovskite layer, so that nucleation and growth of crystals can be greatly promoted, and the perovskite film with good crystallization, compact arrangement and smooth surface can be obtained.
In order to achieve the purpose, the technical scheme of the invention is as follows: the continuous preparation device for preparing the perovskite thin film in a roll-to-roll mode through the one-step method comprises an unreeling device, a coating device, a drying device, an extracting device, an annealing device and a reeling device which are sequentially arranged along the conveying direction of a base material, wherein the unreeling device comprises an unreeling shaft and a plurality of supporting rollers arranged along the conveying direction of the base material, the coating device comprises a coating back roller and a slit die head, and coating liquid is supplied to one side, facing the coating back roller, of the slit die head; the drying device comprises a drying box body and a heating device arranged in the drying box body; the extraction device comprises an extraction groove and a guide roller group in the extraction groove, an anti-solvent corresponding to the coating liquid is arranged in the extraction groove, the annealing device comprises an annealing box body and a heating device arranged in the annealing box body, and the winding device comprises a winding shaft.
The invention is further configured to: the unwinding device is single-station or double-station, the unwinding shaft is actively unwound or passively unwound, the unwinding shaft is clockwise and/or anticlockwise rotated, and the winding device are correspondingly arranged.
The invention is further configured to: the coating back roll is a rigid roll.
The invention is further configured to: guide roller set is including setting up guide roller, two settings in the extraction tank of extraction tank liquid level top turn to the roller and set up two turn to transition roller between the roller, both sides on the guide roller are provided with the spacing piece that corresponds with the substrate edge, turn to the roller symmetry and set up in substrate width direction both sides, the both sides of transition roller are provided with the spacing piece that corresponds with the substrate edge, the guide roller with the transition roller all with the surface butt that the substrate did not coat, turn to the roller and the surface butt of substrate coating.
The invention is further configured to: and the extraction tank is also connected with a circulating device for maintaining the concentration of the solute in the anti-solvent.
The invention is further configured to: the heating device is heated by infrared rays and/or hot air, and the lengths of the heating box body and the annealing box body are determined together according to the drying time and the base material transmission speed required by the process.
The invention is further configured to: the laminating device is arranged behind the annealing device and in front of the rolling device and comprises double rollers arranged in a pressing mode, one of the double rollers is a pressing back roller abutted against the uncoated surface of the base material, the pressing back roller is fixedly arranged in position, and the pressing back roller has a heating or cooling function; the other rubber roller is a rubber roller which is arranged in a pneumatic or hydraulic lifting mode, and a film is further arranged on the rubber roller.
The invention is further configured to: the coating device adopts a blade coating process or a spraying process or a slit coating process.
The invention also discloses a continuous preparation process for preparing the perovskite thin film in a roll-to-roll manner by the one-step method, which comprises the following steps: the continuous preparation device comprises the following steps
S1, the substrate coated with the bottom electrode and the electron transmission layer is discharged from the unwinding shaft in a rotating mode, the coating liquid is uniformly coated on the surface of the substrate through the slot die head by the coating device, and the thickness of the film layer on the surface of the substrate is controlled through the unwinding speed of the unwinding shaft and the liquid supply amount of the coating liquid;
s2, drying the base material in a drying device, and strictly controlling the drying degree of the base material by adjusting parameters such as the temperature in the heating device, the length of the heating box body and the like;
s3, leading the dried base material into an extraction tank through the guide roller, and controlling the soaking time of the base material in the extraction tank by adjusting the distance between the transition roller and the turning roller;
s4, annealing the base material in an annealing device, further forming and growing perovskite crystals, and finally forming a perovskite thin film with uniform and good crystallization; the annealing time can be controlled by the length of the annealing box body;
and S5, finishing winding the substrate through a winding roller.
The invention is further configured to: s6 is further arranged between the S4 and the S5, and the S6 comprises the following processes: and the substrate after annealing passes through the laminating device, the coated surface of the substrate is abutted against the rubber roll, the uncoated surface of the substrate is abutted against the pressing back roll, and the film is laminated on the surface of the substrate through the rubber roll.
In summary, the present invention has the following effects:
1. the stability of the operation of the base material in the extraction tank is ensured through the guide roller group arranged in the extraction tank, the stability of the operation of the base material in the extraction tank can be ensured through the limiting pieces arranged on the steering roller and the transition roller, meanwhile, the steering roller is only contacted with the edge of the base material, the coating surface of the base material is ensured to be fully contacted with an anti-solvent, and the influence of the contact of the base material and the steering roller on the crystallization effect is reduced;
2. the running time of the base material in the extraction tank can be adjusted by adjusting the distance between the transition roller and the turning roller, and the extraction time of the base material can be controlled;
3. the damage to the film layer before entering the next working procedure is avoided.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings used in the embodiments or the description of the prior art will be briefly described below.
FIG. 1 is a schematic view of the overall structure of a perovskite thin film continuous production apparatus;
FIG. 2 is a schematic view of the structure of an extraction apparatus;
FIG. 3 is a schematic view of the internal structure of the extraction apparatus;
FIG. 4 is a flow chart of a continuous process for roll-to-roll preparation of perovskite thin films by a one-step process.
In the figure: 1. an unwinding device; 11. unwinding rollers; 12. a support roller; 13. a substrate; 2. a coating device; 21. coating a back roll; 22. a slot die head; 3. a drying device; 4. an extraction device; 41. an extraction tank; 42. a guide roller set; 421. a guide roller; 422. a turning roll; 423. a transition roll; 43. a limiting sheet; 5. an annealing device; 6. a winding device; 7. a bonding device; 71. pressing a back roller; 72. a rubber roller; 73. a film covering unwinding roller; 74. and (5) coating a film.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
As shown in fig. 1, a continuous preparation device for preparing perovskite thin film by one-step roll-to-roll method is sequentially provided with an unreeling device, a coating device, a drying device, an extracting device, an annealing device and a reeling device along a substrate transmission direction, wherein the unreeling device comprises an unreeling shaft and a plurality of supporting rolls arranged along the substrate transmission direction, the coating device comprises a coating back roll and a slit die head, and the slit die head supplies coating liquid towards one side of the coating back roll; the drying device comprises a drying box body and a heating device arranged in the drying box body; the extraction device comprises an extraction groove and a guide roller group in the extraction groove, an anti-solvent corresponding to the coating liquid is arranged in the extraction groove, the annealing device comprises an annealing box body and a heating device arranged in the annealing box body, and the winding device comprises a winding shaft.
The laminating device is arranged behind the annealing device and in front of the rolling device and comprises double rollers arranged in a pressing mode, one of the double rollers is a pressing back roller abutted against the uncoated surface of the base material, the pressing back roller is fixedly arranged in position, and the pressing back roller has a heating or cooling function; the other rubber roller is a rubber roller which is arranged in a pneumatic or hydraulic lifting mode, and a film is further arranged on the rubber roller.
In this scheme, the guide roller group is including setting up guide roller, two settings of extraction tank liquid level top turn to the roller and set up two in the extraction tank turn to transition roller between the roller, both sides on the guide roller are provided with the spacing piece that corresponds with the substrate edge, turn to the roller symmetry and set up in substrate width direction both sides, the both sides of transition roller are provided with the spacing piece that corresponds with the substrate edge, the guide roller with the transition roller all with the surface butt that the substrate was not coated, turn to the surface butt of roller and substrate coating. And the extraction tank is also connected with a circulating device for maintaining the concentration of the solute in the anti-solvent.
Furthermore, unwinding device is single-station or duplex position, unreel the axle for initiatively unreeling or unreel passively, the turning to of unreeling the axle is clockwise setting and/or anticlockwise setting, coiling mechanism with the corresponding setting of coiling mechanism.
Further, the coating back roll is a rigid roll.
Further, the heating device is heated by infrared rays and/or hot air, and the lengths of the heating box body and the annealing box body are determined according to the drying time and the base material conveying speed required by the process.
Further, the coating device adopts a blade coating process or a spraying process or a slit coating process.
The continuous preparation process for preparing the perovskite thin film in a roll-to-roll manner by a one-step method comprises the following steps:
s1, the substrate coated with the bottom electrode and the electron transmission layer is discharged from the unwinding shaft in a rotating mode, the coating liquid is uniformly coated on the surface of the substrate through the slot die head by the coating device, and the thickness of the film layer on the surface of the substrate is controlled through the unwinding speed of the unwinding shaft and the liquid supply amount of the coating liquid;
s2, drying the base material in a drying device, and strictly controlling the drying degree of the base material by adjusting parameters such as the temperature in the heating device, the length of the heating box body and the like;
s3, leading the dried base material into an extraction tank through the guide roller, and controlling the soaking time of the base material in the extraction tank by adjusting the distance between the transition roller and the turning roller;
s4, annealing the base material in an annealing device, further forming and growing perovskite crystals, and finally forming a perovskite thin film with uniform and good crystallization; the annealing time can be controlled by the length of the annealing box body;
and S5, finishing winding the substrate through a winding roller.
Further, S6 is further disposed between S4 and S5, and S6 includes the following processes: and the substrate after annealing passes through the laminating device, the coated surface of the substrate is abutted against the rubber roll, the uncoated surface of the substrate is abutted against the pressing back roll, and the film is laminated on the surface of the substrate through the rubber roll.
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 (10)
1. The continuous preparation device for preparing the perovskite thin film in a roll-to-roll mode by the one-step method is characterized in that an unreeling device, a coating device, a drying device, an extracting device, an annealing device and a reeling device are sequentially arranged along the conveying direction of a base material, the unreeling device comprises an unreeling shaft and a plurality of supporting rolls arranged along the conveying direction of the base material, the coating device comprises a coating back roll and a slit die head, and coating liquid is supplied to one side, facing the coating back roll, of the slit die head; the drying device comprises a drying box body and a heating device arranged in the drying box body; the extraction device comprises an extraction groove and a guide roller group in the extraction groove, an anti-solvent corresponding to the coating liquid is arranged in the extraction groove, the annealing device comprises an annealing box body and a heating device arranged in the annealing box body, and the winding device comprises a winding shaft.
2. The continuous preparation device for roll-to-roll preparation of perovskite thin film according to the one-step method of claim 1, wherein the unwinding device is a single station or a double station, the unwinding shaft is active unwinding or passive unwinding, the direction of the unwinding shaft is clockwise and/or counterclockwise, and the winding device is arranged corresponding to the winding device.
3. The continuous production apparatus for producing a perovskite thin film in a roll-to-roll manner according to the one-step method of claim 1, wherein the coating back roll is a rigid roll.
4. The continuous production device for the perovskite thin film through the one-step roll-to-roll production according to claim 1, wherein the guide roller group comprises a guide roller arranged above the liquid level of the extraction tank, two turning rollers arranged in the extraction tank and a transition roller arranged between the two turning rollers, the two sides of the guide roller are provided with limiting pieces corresponding to the edges of the base material, the turning rollers are symmetrically arranged on the two sides of the base material in the width direction, the two sides of the transition roller are provided with limiting piece limiting pieces corresponding to the edges of the base material, the guide roller and the transition roller are both abutted against the uncoated surface of the base material, and the turning rollers are abutted against the coated surface of the base material.
5. The continuous production device for the perovskite thin film through the one-step method roll-to-roll production is characterized in that the extraction tank is further connected with a circulating device for maintaining the concentration of the solute in the anti-solvent.
6. The continuous production device for the perovskite thin film through the one-step method roll-to-roll production is characterized in that the heating device is infrared heating and/or hot air heating, and the lengths of the heating box body and the annealing box body are jointly determined according to the drying time and the substrate conveying speed required by the process.
7. The continuous roll-to-roll perovskite film preparation device according to the one-step method, which is characterized by further comprising a laminating device arranged behind the annealing device and in front of the rolling device, wherein the laminating device comprises double rollers arranged in a laminating manner, one of the double rollers is a laminating back roller abutted against the uncoated surface of the substrate, the laminating back roller is fixedly arranged, and the laminating back roller has a heating or cooling function; the other rubber roller is a rubber roller which is arranged in a pneumatic or hydraulic lifting mode, and a film is further arranged on the rubber roller.
8. The continuous production device for the perovskite thin film through the one-step method in a roll-to-roll mode is characterized in that the coating device adopts a blade coating process or a spraying process or a slit coating process.
9. The continuous preparation process for preparing the perovskite thin film in a roll-to-roll mode by using the one-step method, which is characterized by adopting the continuous preparation device as claimed in any one of claims 1 to 8, and comprises the following steps:
s1, the substrate coated with the bottom electrode and the electron transmission layer is discharged from the unwinding shaft in a rotating mode, the coating liquid is uniformly coated on the surface of the substrate through the slot die head by the coating device, and the thickness of the film layer on the surface of the substrate is controlled through the unwinding speed of the unwinding shaft and the liquid supply amount of the coating liquid;
s2, drying the base material in a drying device, and strictly controlling the drying degree of the base material by adjusting parameters such as the temperature in the heating device, the length of the heating box body and the like;
s3, leading the dried base material into an extraction tank through the guide roller, and controlling the soaking time of the base material in the extraction tank by adjusting the distance between the transition roller and the turning roller;
s4, annealing the base material in an annealing device, further forming and growing perovskite crystals, and finally forming a perovskite thin film with uniform and good crystallization; the annealing time can be controlled by the length of the annealing box body;
and S5, finishing winding the substrate through a winding roller.
10. The continuous preparation process of the perovskite thin film through the one-step roll-to-roll preparation method of claim 9, wherein S6 is further arranged between S4 and S5, and the S6 comprises the following steps: and the substrate after annealing passes through the laminating device, the coated surface of the substrate is abutted against the rubber roll, the uncoated surface of the substrate is abutted against the pressing back roll, and the film is laminated on the surface of the substrate through the rubber roll.
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| CN202010154904.5A CN111341919A (en) | 2020-03-06 | 2020-03-06 | Continuous preparation process and device for preparing perovskite thin film in roll-to-roll mode by one-step method |
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| CN202010154904.5A CN111341919A (en) | 2020-03-06 | 2020-03-06 | Continuous preparation process and device for preparing perovskite thin film in roll-to-roll mode by one-step method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111769238A (en) * | 2020-07-22 | 2020-10-13 | 福建巨电新能源股份有限公司 | Extraction equipment and process for solid diaphragm of lithium ion power battery |
| WO2023273879A1 (en) * | 2021-07-02 | 2023-01-05 | 常州大学 | Device and method for roll-to-roll preparation of flexible perovskite and full-perovskite laminated solar cells |
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| WO2023273879A1 (en) * | 2021-07-02 | 2023-01-05 | 常州大学 | Device and method for roll-to-roll preparation of flexible perovskite and full-perovskite laminated solar cells |
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