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CN108970913B - Perovskite film coating equipment, use method and application - Google Patents

Perovskite film coating equipment, use method and application Download PDF

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Publication number
CN108970913B
CN108970913B CN201710406229.9A CN201710406229A CN108970913B CN 108970913 B CN108970913 B CN 108970913B CN 201710406229 A CN201710406229 A CN 201710406229A CN 108970913 B CN108970913 B CN 108970913B
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substrate
solvent
coating
drying device
solution
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CN108970913A (en
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请求不公布姓名
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Hangzhou Microquanta Semiconductor Co ltd
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Hangzhou Microquanta Semiconductor Co ltd
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Priority to CN201710406229.9A priority Critical patent/CN108970913B/en
Priority to PCT/CN2018/087346 priority patent/WO2018219152A1/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C9/00—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important
    • B05C9/06—Apparatus or plant for applying liquid or other fluent material to surfaces by means not covered by any preceding group, or in which the means of applying the liquid or other fluent material is not important for applying two different liquids or other fluent materials, or the same liquid or other fluent material twice, to the same side of the work
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C13/00—Means for manipulating or holding work, e.g. for separate articles
    • B05C13/02—Means for manipulating or holding work, e.g. for separate articles for particular articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C5/00—Apparatus in which liquid or other fluent material is projected, poured or allowed to flow on to the surface of the work
    • B05C5/02—Apparatus in which liquid or other fluent material is projected, poured or allowed to flow on to the surface of the work the liquid or other fluent material being discharged through an outlet orifice by pressure, e.g. from an outlet device in contact or almost in contact, with the work
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C—APPARATUS FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05C5/00—Apparatus in which liquid or other fluent material is projected, poured or allowed to flow on to the surface of the work
    • B05C5/02—Apparatus in which liquid or other fluent material is projected, poured or allowed to flow on to the surface of the work the liquid or other fluent material being discharged through an outlet orifice by pressure, e.g. from an outlet device in contact or almost in contact, with the work
    • B05C5/0254—Coating heads with slot-shaped outlet
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/04—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases
    • B05D3/0406—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to gases the gas being air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/06—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by exposure to radiation
    • 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
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • 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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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Manufacturing & Machinery (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

The invention relates to perovskite film coating equipment, which comprises a conveying device for conveying a substrate, a perovskite solution coating device, an anti-solvent spraying device and an air drying device or a heating drying device, wherein the perovskite solution coating device is provided with a perovskite coating head, and the anti-solvent spraying device is provided with an anti-solvent spraying nozzle. The substrate is driven by a conveying device to sequentially pass through a perovskite solution coating device, an anti-solvent spraying device and an air drying device or a heating drying device, and the perovskite solution and the anti-solvent on the surface of the substrate are volatilized and dried simultaneously by wind at an air outlet to form a perovskite film. The invention also relates to a use method and application of the coating device. The invention improves the existing one-step solution method and two-step solution method equipment, the using method and the application, and carries out wind blowing or infrared heating drying on the substrate sprayed or coated with the perovskite solution, thereby ensuring low production cost and improving film forming quality at the same time, and being suitable for large-area and large-scale production of perovskite films of the substrate.

Description

Perovskite film coating equipment, use method and application
Technical Field
The invention belongs to the technical field of solar cells, and particularly relates to perovskite thin film coating equipment, a using method and application thereof.
Background
In recent years, perovskite solar cells have received a great deal of attention, and there are various methods and apparatuses for producing perovskite thin films. Currently, common methods for preparing perovskite thin films include a one-step solution process, a two-step solution process, a gas-phase assisted solution process, and co-vapor deposition. The co-vapor deposition and the vapor-phase assisted solution method are unfavorable for mass production and reduce the cost due to the high cost of vacuum equipment.
The conventional one-step solution process comprises preparing perovskite solution, spin-coating a certain amount of solution, and annealing the spin-coated perovskite wet film at high temperature to form perovskite film. Although this method is convenient, fast and inexpensive, the films made by this method are not dense enough and are difficult to mass produce.
In the two-step solution method, a perovskite thin film preset layer is deposited by using a solution in the first step. The quality of the prefabricated layer film directly determines the quality of the perovskite film obtained by the subsequent process. The film obtained by the conventional perovskite film preset layer coating process is uneven, non-compact and has a plurality of defects, and the defects are specifically shown as uneven thickness of each part of the film, more pinholes on the surface of the film, large roughness, poor batch-to-batch repeatability and the like. In addition, the existing two-step solution method has the problems that the prefabricated layer cannot be dried quickly and uniformly and the prefabricated layer is easily influenced by environmental convection in the drying process, and the film manufactured by the method is difficult to produce in a large scale.
Disclosure of Invention
The invention aims to solve the technical problems of providing perovskite film coating equipment, a using method and application, improving the perovskite film coating equipment and technology, and overcoming the defects by adopting novel perovskite film coating equipment and technology. Thus, on the premise of ensuring low production cost, the film forming quality is improved, the large-scale production process is improved, and the perovskite film forming efficiency is greatly improved.
The invention is realized by the way, the perovskite film coating equipment comprises a conveying device for conveying a substrate, a perovskite solution coating device, an anti-solvent spraying device and an air drying device or a heating and drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the perovskite solution coating device is provided with a coating head, the coating head is a perovskite coating head, the anti-solvent spraying device is provided with a spraying nozzle, the spraying nozzle is an anti-solvent spraying nozzle, the air drying device is provided with an air outlet, the heating and drying device is provided with an infrared heater, the substrate is placed on the conveying belt or the conveying shaft and driven by the conveying shaft to sequentially pass through the perovskite solution coating device, the anti-solvent spraying device and the air drying device or the heating and drying device, the perovskite coating head is used for coating the anti-solvent on the surface of the substrate, the perovskite solution and the anti-solvent on the surface of the substrate are simultaneously volatilized and dried by wind of the air outlet, and the perovskite solution on the surface of the substrate are simultaneously volatilized and dried by the infrared heater and the perovskite drying device is used for respectively heating and drying the perovskite solution from the two sides of the substrate to form a film.
The invention is realized by the way, the perovskite film coating equipment comprises a conveying device for conveying a substrate, a perovskite solution spraying device, an anti-solvent spraying device and an air drying device or a heating and drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the perovskite solution spraying device is provided with a spraying nozzle, the spraying nozzle is a perovskite spraying nozzle, the anti-solvent spraying device is provided with a coating head, the coating head is an anti-solvent coating head, the air drying device is provided with an air outlet, the heating and drying device is provided with an infrared heater, the substrate is placed on the conveying belt or the conveying shaft and driven by the conveying shaft to sequentially pass through the perovskite solution spraying device, the anti-solvent spraying device and the air drying device or the heating and drying device, the perovskite spraying nozzle is used for spraying the anti-solvent on the surface of the substrate, the perovskite solution and the anti-solvent on the surface of the substrate are simultaneously volatilized and dried by wind of the air outlet, and the perovskite solution on the surface of the substrate are simultaneously evaporated and the perovskite solution on the two sides of the substrate respectively heated by the infrared heater and the perovskite drying device is used for drying the perovskite solution from the two sides of the surface of the substrate simultaneously.
The two perovskite film coating devices are all improved from the existing one-step solution method device, and the substrate sprayed or coated with the perovskite solution is subjected to wind blowing or infrared heating drying, so that the low production cost is ensured, the film forming quality is improved, and the perovskite film coating device is suitable for large-area and large-scale production of the perovskite film of the substrate.
The invention is realized by the way, the perovskite film coating equipment comprises a conveying device for conveying a substrate, a precursor solution coating device, an active layer spraying device and an air drying device or a heating drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head, the coating head is the precursor coating head, the active layer spraying device is provided with a spraying nozzle, the spraying nozzle is an active spraying nozzle, the air drying device is provided with an air outlet, the heating drying device is provided with an infrared heater, the substrate is placed on the conveying belt or the conveying shaft and driven by the infrared heater to sequentially pass through the precursor solution coating device, the active layer spraying device and the air drying device or the heating drying device, the precursor coating head coats the precursor solution on the surface of the substrate, the active spraying nozzle sprays the active solution on the surface of the substrate, wind of the air outlet volatilizes the precursor solution on the surface of the substrate and the active solution simultaneously, and the active solution is formed into a perovskite film, and the infrared heater is used for heating the precursor film and the precursor film is formed by the infrared heater and the precursor film is simultaneously heated and the active film is formed on the two sides of the active film drier.
The invention is realized by the way, the perovskite film coating equipment comprises a conveying device for conveying a substrate, a precursor solution coating device, an activation layer coating device, an anti-solvent spraying device and an air drying device or a heating and drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head, the coating head is a precursor coating head, the activation layer coating device is provided with a coating head, the coating head is an activated coating head, the anti-solvent spraying device is provided with a spraying nozzle, the spraying nozzle is an anti-solvent spraying nozzle, the air drying device is provided with an air outlet, the substrate is arranged on the conveying belt or the conveying shaft, the substrate is driven by the infrared heater to sequentially pass through the precursor solution coating device, the activation layer coating device, the anti-solvent spraying device and the air drying device or the heating and drying device, the precursor coating head coats the precursor solution on the surface of the substrate, the activated coating head sprays the precursor solution on the surface of the substrate, the anti-solvent is sprayed on the surface of the substrate, the anti-solvent is dried on the surface of the substrate, and the anti-solvent is simultaneously heated and the anti-solvent is dried on the surface of the substrate, and the surface of the precursor solution is simultaneously heated, and the anti-solvent is simultaneously dried on the surface of the substrate and the precursor solution is heated.
The invention is realized by the way, the perovskite film coating equipment comprises a conveying device for conveying a substrate, a precursor solution coating device, an activation layer spraying device, an anti-solvent coating device and an air drying device or a heating and drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head, the coating head is a precursor coating head, the anti-solvent coating device is provided with a coating head, the coating head is an anti-solvent coating head, the activation layer spraying device is provided with a spraying nozzle, the spraying nozzle is an activation spraying nozzle, the air drying device is provided with an air outlet, the substrate is placed on the conveying belt or the conveying shaft and sequentially driven by the infrared heater to pass through the precursor solution coating device, the activation layer spraying device, the anti-solvent coating device and the air drying device or the heating and drying device, the precursor coating head coats the precursor solution on the surface, the activation layer spraying nozzle sprays the activation solution on the surface of the substrate, the anti-solvent coating head and the anti-solvent coating device and the surface of the substrate are simultaneously heated and the precursor solution is simultaneously dried on the two sides of the substrate, and the surface of the precursor solution is simultaneously heated and the surface of the precursor solution is dried.
The invention is realized by the way, and provides perovskite film coating equipment, which comprises a conveying device for conveying a substrate, a precursor solution coating device, a front-stage air drying device or a front-stage heating drying device, an active layer spraying device and a rear-stage air drying device or a rear-stage heating drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head, the coating head is a precursor coating head, the front-stage air drying device is provided with a front-stage air outlet, the front-stage heating drying device is provided with an infrared heater, the active layer spraying device is provided with a spraying nozzle, the spraying nozzle is an active spraying nozzle, the rear-stage air drying device is provided with a rear-stage air outlet, the rear-stage heating drying device is provided with an infrared heater, the substrate is placed on the conveying belt or the conveying shaft and driven by the conveying shaft to sequentially pass through a precursor solution coating device, a front-stage air drying device or a front-stage heating drying device, an active layer spraying device and a rear-stage air drying device or a rear-stage heating drying device, wherein the precursor coating head coats the precursor solution on the surface of the substrate, the active spraying nozzle sprays the active solution on the surface of the substrate, the precursor solution on the surface of the substrate is volatilized and dried by the air of an air outlet of the front stage to form a precursor film, the precursor solution on the surface of the substrate is volatilized and dried by the infrared heaters of the front-stage heating drying device respectively from the upper side and the lower side of the substrate and simultaneously heated by the infrared heaters of the front-stage heating drying device to form the precursor film, the active solution on the surface of the substrate is volatilized and dried by the air of the air outlet of the rear stage to form a perovskite film, the infrared heaters of the rear-stage heating and drying device respectively heat the substrate from the upper side and the lower side simultaneously to evaporate and dry the activated solution on the surface of the substrate, and form a perovskite film.
The invention is realized by the way, and provides perovskite film coating equipment, which comprises a conveying device for conveying a substrate, a precursor solution coating device, a front-stage air drying device or a front-stage heating drying device, an activation layer coating device, an anti-solvent spraying device and a rear-stage air drying device or a rear-stage heating drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head, the coating head is a precursor coating head, the front-stage air drying device is provided with a front-stage air outlet, the front-stage heating drying device is provided with an infrared heater, the activation layer coating device is provided with a coating head, the coating head is an activation coating head, the anti-solvent spraying device is provided with a spraying nozzle, the spraying nozzle is an anti-solvent spraying nozzle, the rear-stage air drying device is provided with a rear-stage air outlet, the back-stage heating and drying device is provided with an infrared heater, the substrate is placed on the conveyor belt or the conveyor shaft and driven by the conveyor belt or the conveyor shaft to sequentially pass through a precursor solution coating device, a front-stage air drying device or a front-stage heating and drying device, an activation layer coating device, an anti-solvent spraying device and a back-stage air drying device or a back-stage heating and drying device, the precursor coating head coats the precursor solution on the surface of the substrate, the activation coating head coats the activation solution on the surface of the substrate, the anti-solvent spraying nozzle sprays the anti-solvent on the surface of the substrate, the precursor solution on the surface of the substrate is volatilized and dried by the air of the front-stage air outlet to form a precursor film, the precursor solution on the surface of the substrate is vaporized and dried by the infrared heater of the front-stage heating and drying device respectively and simultaneously heated from the upper side and the lower side of the substrate to form the precursor film, the air of the air outlet at the rear section volatilizes and dries the activation solution and the anti-solvent on the surface of the substrate simultaneously to form a perovskite film, and the infrared heater of the rear-section heating and drying device respectively heats the substrate from the upper side and the lower side simultaneously to evaporate and dry the activation solution and the anti-solvent on the surface of the substrate together to form the perovskite film.
The invention is realized by the way, and provides perovskite film coating equipment, which comprises a conveying device for conveying a substrate, a precursor solution coating device, a front-stage air drying device or a front-stage heating drying device, an activation layer spraying device, an anti-solvent coating device and a rear-stage air drying device or a rear-stage heating drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head, the coating head is a precursor coating head, the anti-solvent coating device is provided with a coating head, the coating head is an anti-solvent coating head, the front-stage air drying device is provided with a front-stage air outlet, the front-stage heating drying device is provided with an infrared heater, the activation layer spraying device is provided with a spraying nozzle, the spraying nozzle is an activation spraying nozzle, the rear-stage air drying device is provided with a rear-stage air outlet, the back-stage heating and drying device is provided with an infrared heater, the substrate is placed on the conveyor belt or the conveyor shaft and driven by the conveyor belt or the conveyor shaft to sequentially pass through a precursor solution coating device, a front-stage air drying device or a front-stage heating and drying device, an active layer spraying device, an anti-solvent coating device and a back-stage air drying device or a back-stage heating and drying device, the precursor coating head coats the precursor solution on the surface of the substrate, the active spraying nozzle sprays the active solution on the surface of the substrate, the anti-solvent coating head coats the anti-solvent on the surface of the substrate, the precursor solution on the surface of the substrate is volatilized and dried by the air of the front-stage air outlet to form a precursor film, the precursor solution on the surface of the substrate is vaporized and dried by the infrared heater of the front-stage heating and drying device from the upper side and the lower side of the substrate simultaneously to form the precursor film, the air of the air outlet at the rear section volatilizes and dries the activation solution and the anti-solvent on the surface of the substrate simultaneously to form a perovskite film, and the infrared heater of the rear-section heating and drying device respectively heats the substrate from the upper side and the lower side simultaneously to evaporate and dry the activation solution and the anti-solvent on the surface of the substrate together to form the perovskite film.
The six perovskite film coating devices are all improved to the existing two-step solution method device, and the substrate sprayed or coated with the perovskite solution is subjected to wind blowing or infrared heating drying, so that the airflow on the surface of the substrate is controlled, the drying speed of the precursor film is accelerated, the precursor film is more uniform and compact, the film forming quality is improved while the low production cost is ensured, and the perovskite film coating device is suitable for large-area large-scale production of the perovskite film of the substrate.
The invention is realized in such a way that a method for using perovskite thin film coating equipment is provided, comprising the following steps:
A1. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
A2. enabling the substrate to sequentially pass through a perovskite solution coating device, enabling a perovskite coating head to coat perovskite solution on the surface of the substrate, enabling an anti-solvent spraying nozzle to spray anti-solvent on the surface of the substrate through an anti-solvent spraying device, enabling an air outlet or an infrared heater to volatilize or evaporate the perovskite solution and the anti-solvent rapidly through an air drying device or a heating drying device, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
The invention is realized in such a way that a method for using perovskite thin film coating equipment is provided, comprising the following steps:
A3. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
A4. enabling the substrate to sequentially pass through a perovskite solution spraying device, enabling a perovskite spraying nozzle to spray perovskite solution on the surface of the substrate, enabling an anti-solvent coating head to coat anti-solvent on the surface of the substrate through an anti-solvent coating device, enabling an air outlet or an infrared heater to volatilize or evaporate the perovskite solution and the anti-solvent rapidly through an air drying device or a heating drying device, and finally obtaining and storing the substrate with the perovskite film attached to the surface.
The application method of the two perovskite film coating equipment is to improve the existing one-step solution method, wind blowing or infrared heating drying is carried out on the substrate sprayed or coated with the perovskite solution, the film forming quality is improved while the low production cost is ensured, and the perovskite film coating equipment is suitable for large-area large-scale production of the perovskite film of the substrate.
The invention is realized in such a way that a method for using perovskite thin film coating equipment is provided, comprising the following steps:
B1. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
B2. The substrate sequentially passes through a precursor solution coating device, a precursor coating head coats a precursor solution on the surface of the substrate, an activation spraying nozzle sprays an activation solution on the surface of the substrate through an activation layer spraying device, the precursor solution and the activation solution are quickly volatilized or evaporated through an air drying device or a heating drying device, and finally the substrate with the perovskite film attached on the surface is obtained and stored.
The invention is realized in such a way that a method for using perovskite thin film coating equipment is provided, comprising the following steps:
B3. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
B4. the method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling an activated coating head to coat activated solution on the surface of the substrate through an activated layer coating device, enabling an anti-solvent spraying nozzle to spray anti-solvent on the surface of the substrate through an anti-solvent spraying device, enabling an air drying device or a heating drying device to quickly volatilize or evaporate the precursor solution, the activated solution and the anti-solvent together through an air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
The invention is realized in such a way that a method for using perovskite thin film coating equipment is provided, comprising the following steps:
B6. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
B7. the method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling an activation spraying nozzle to spray activation solution on the surface of the substrate through an activation layer spraying device, enabling an anti-solvent coating head to coat anti-solvent on the surface of the substrate through an anti-solvent coating device, enabling an air drying device or a heating drying device to quickly volatilize or evaporate the precursor solution, the activation solution and the anti-solvent together through an air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and preserving the substrate.
The invention is realized in such a way that a method for using perovskite thin film coating equipment is provided, comprising the following steps:
C1. placing the substrate with the bottom electrode layer attached to the conveyor belt or conveyor shaft of the anti-solvent coating device conveyor;
C2. the method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling the precursor solution to be quickly volatilized or evaporated through a front-section air drying device or a front-section heating drying device, enabling a front-section air outlet or an infrared heater to be quickly volatilized or evaporated, enabling an activation spray nozzle to spray activation solution on the surface of the substrate through an activation layer spraying device, enabling a rear-section air drying device or a rear-section heating drying device to quickly volatilize or evaporate the activation solution through a rear-section air outlet or the infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
The invention is realized in such a way that a method for using perovskite thin film coating equipment is provided, comprising the following steps:
C3. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
C4. the method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling the precursor solution to be quickly volatilized or evaporated through a front-stage air drying device or a front-stage heating drying device, enabling an activated coating head to coat activated solution on the surface of the substrate through an activated layer coating device, enabling an anti-solvent spraying nozzle to spray anti-solvent on the surface of the substrate through an anti-solvent spraying device, enabling the activated solution and the anti-solvent to be quickly volatilized or evaporated through a rear-stage air drying device or a rear-stage heating drying device, and finally obtaining the substrate with the perovskite film attached to the surface and preserving the substrate.
The invention is realized in such a way that a method for using perovskite thin film coating equipment is provided, comprising the following steps:
C5. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
C6. The method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling the precursor solution to be quickly volatilized or evaporated through a front-stage air drying device or a front-stage heating drying device, enabling an activating solution to be sprayed on the surface of the substrate through an activating layer spraying device and an activating spraying nozzle, enabling an anti-solvent coating head to coat anti-solvent on the surface of the substrate through an anti-solvent coating device, enabling the activating solution to be quickly volatilized or evaporated through a rear-stage air drying device or a rear-stage heating drying device, enabling the activating solution and the anti-solvent to be quickly volatilized or evaporated through a rear-stage air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
The six methods for using the perovskite film coating equipment are all improved on the basis of the existing two-step solution method, and the substrate sprayed or coated with the perovskite solution is subjected to wind blowing or infrared heating drying, so that the air flow on the surface of the substrate is controlled, the drying speed of a precursor film is accelerated, the precursor film is more uniform and compact, the film forming quality is improved while the low production cost is ensured, and the perovskite film coating equipment is suitable for large-area large-scale production of the perovskite film of the substrate.
The present invention has been achieved in such a way as to provide the use of a perovskite thin film coating apparatus which may also be used to coat a solution containing at least one of the following materials:
vanadium pentoxide (V) 2 O 5 ) Tungsten oxide (WO) 3 ) Molybdenum oxide (MoOx), copper sulfide (CuS), copper sulfide (CuSCN), copper oxide (CuO), copper iodide (CuI), copper oxide (Cu) 2 O), iron disulfide (FeS) 2 ）、CDO 2 Copper-iron semiconductor, lead sulfide (PbS), cobalt oxide (CoOx), cobalt sulfide (CoS), nickel oxide doped with magnesium and lithium (nimgilio), nickel oxide (NiOx), polyethylene dioxythiophene-poly (styrenesulfonate), and highly conductive derivatives thereof (PEDOT: PSS), poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine]Poly-triaryamine, PTAA), 2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino]-9,9' -spirobifluorene (Spiro-OMeTAD), 3-hexyl-substituted polythiophene (P3 HT), titanium dioxide (TiO 2 ) Zinc oxide (ZnO), zinc sulfide (ZnS), zinc selenide (ZnSe), cadmium sulfide (CdS), cadmium selenide (CdSe), bismuth sulfide (Bi) 2 S 3 ) Indium sulfide (In) 2 S 3 ) Indium oxide (In) 2 O 3 ) Antimony sulfide (Sb) 2 S 3 ) Molybdenum disulfide (MoS) 2 ) Selenium disulfide (SnS) 2 ) Tin oxide (SnO) 2 ) PCBM, doped Aluminum Zinc Oxide (AZO), cerium oxide (CeOx), niobium oxide(NbOx), barium titanate (BaTiO) 3 ) Fullerene (C60, C70), zinc-doped cadmium sulfide (Zn) 1-x Cd x S), chromium oxide (CrOx), copper-doped chromium oxide (Cu) x Cr y O 2 ），
Wherein CDO 2 C=cu or Ag in the copper-iron semiconductor type, d= Cr, ga, al, sc, in, Y, fe.
The present invention has been achieved in such a way as to provide a use of a method for using a perovskite thin film coating apparatus which can also be used for coating a solution containing at least one of the following materials:
vanadium pentoxide (V) 2 O 5 ) Tungsten oxide (WO) 3 ) Molybdenum oxide (MoOx), copper sulfide (CuS), copper sulfide (CuSCN), copper oxide (CuO), copper iodide (CuI), copper oxide (Cu) 2 O), iron disulfide (FeS) 2 ）、CDO 2 Copper-iron semiconductor, lead sulfide (PbS), cobalt oxide (CoOx), cobalt sulfide (CoS), nickel oxide doped with magnesium and lithium (nimgilio), nickel oxide (NiOx), polyethylene dioxythiophene-poly (styrenesulfonate), and highly conductive derivatives thereof (PEDOT: PSS), poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine ]Poly-triaryamine, PTAA), 2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino]-9,9' -spirobifluorene (Spiro-OMeTAD), 3-hexyl-substituted polythiophene (P3 HT), titanium dioxide (TiO 2 ) Zinc oxide (ZnO), zinc sulfide (ZnS), zinc selenide (ZnSe), cadmium sulfide (CdS), cadmium selenide (CdSe), bismuth sulfide (Bi) 2 S 3 ) Indium sulfide (In) 2 S 3 ) Indium oxide (In) 2 O 3 ) Antimony sulfide (Sb) 2 S 3 ) Molybdenum disulfide (MoS) 2 ) Selenium disulfide (SnS) 2 ) Tin oxide (SnO) 2 ) PCBM, doped Aluminum Zinc Oxide (AZO), cerium oxide (CeOx), niobium oxide (NbOx), barium titanate (BaTiO) 3 ) Fullerene (C60, C70), zinc-doped cadmium sulfide (Zn) 1-x Cd x S), chromium oxide (CrOx), copper-doped chromium oxide (Cu) x Cr y O 2 ），
Wherein CDO 2 C=cu or Ag in the copper-iron semiconductor type, d= Cr, ga, al, sc, in, Y, fe.
Compared with the prior art, the perovskite film coating equipment, the using method and the application thereof adopt novel coating equipment and technology, make up the defect of one-step method, and improve the film forming quality and the large-scale production technology on the premise of ensuring low production cost.
Drawings
FIG. 1 is a schematic perspective view of a first preferred embodiment of a perovskite thin film coating apparatus of the invention;
FIG. 2 is a schematic perspective view of a second preferred embodiment of the perovskite thin film coating apparatus of the invention;
FIG. 3 is a schematic perspective view of a third preferred embodiment of the perovskite thin film coating apparatus of the present invention;
FIG. 4 is a schematic perspective view of a fourth preferred embodiment of the perovskite thin film coating apparatus of the present invention;
FIG. 5 is a schematic perspective view of a fifth preferred embodiment of the perovskite thin film coating apparatus of the invention;
FIG. 6 is a schematic perspective view of a sixth preferred embodiment of the perovskite thin film coating apparatus of the invention;
FIG. 7 is a schematic perspective view of a seventh preferred embodiment of the perovskite thin film coating apparatus of the invention;
FIG. 8 is a schematic perspective view of an eighth preferred embodiment of the perovskite thin film coating apparatus of the invention;
FIG. 9 is an SEM image of a perovskite thin film obtained by the method of using a perovskite thin film coating apparatus of the invention;
FIG. 10 is a J-V plot of a perovskite thin film solar cell module resulting from the method of use of a perovskite thin film coating apparatus of the invention;
fig. 11 shows preparation of PbI with a step-by-step apparatus in both the absence of an air-drying apparatus and the presence of an air-drying apparatus 2 A schematic representation of relief contrast magnification of the film surface;
FIG. 12 shows the device without the air drying device and Preparation of PbI in two states with air drying device 2 Film thickness contrast schematic;
FIG. 13 is an SEM image of a perovskite thin film obtained by using the method of using a perovskite thin film coating apparatus of the invention without opening anti-solvent coating and baking;
fig. 14 is an SEM image of a perovskite thin film obtained by starting anti-solvent coating and baking using the method of using the perovskite thin film coating apparatus of the invention.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Referring to fig. 1, a first preferred embodiment of the perovskite thin film coating apparatus of the present invention comprises a conveyor for conveying a substrate 2, a perovskite solution coating device, an anti-solvent spraying device and an air drying device. As another example, the air drying device may be replaced with a heat drying device.
The substrate 2 is prepared with a bottom electrode layer in advance, and the conveyor is provided with a conveyor belt 1 or a conveyor shaft (not shown in the figure). The perovskite solution coating device is provided with a coating head, the coating head is a perovskite coating head 3, the antisolvent spraying device is provided with a spraying nozzle, the spraying nozzle is an antisolvent spraying nozzle 4, and the air drying device is provided with an air outlet 5. The heating and drying device is provided with an infrared heater (not shown in the figure).
The substrate 2 is placed on the conveyor belt 1 or the conveyor shaft and driven by the conveyor belt to sequentially pass through a perovskite solution coating device, an antisolvent spraying device and an air drying device or a heating drying device. The perovskite coating head 3 coats the perovskite solution on the surface of the substrate 2, and the anti-solvent spraying nozzle 4 sprays the anti-solvent on the surface of the substrate 2. The perovskite solution and the anti-solvent on the surface of the substrate 2 are volatilized and dried simultaneously by the wind of the air outlet 5, and a perovskite film is formed. The infrared heaters of the heating and drying device respectively heat the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the perovskite solution and the anti-solvent on the surface of the substrate together to form a perovskite film.
The perovskite solution is BX 2 AX, a main solvent, a solvent additive and/or a mixture of organic polymer additives. Wherein B is at least one cation selected from lead (Pb), tin (Sn), tungsten, copper, zinc, gallium, germanium, arsenic, selenium, rhodium, palladium, silver, cadmium, indium, antimony, osmium, iridium, platinum, gold, mercury, thallium, bismuth and polonium. X is iodine (I), bromine (Br), chlorine (Cl), acetate (CH) 3 COO) at least one anion. A is cesium, rubidium, an amine group, an amidino group or at least one cation of the alkali group. The main solvent comprises at least one of amide solvents, sulfone/sulfoxide solvents, ester solvents, hydrocarbons, halogenated hydrocarbon solvents, alcohol solvents, ketone solvents, ether solvents and aromatic hydrocarbon solvents. The solvent additive is at least one of amide solvents, sulfone/sulfoxide solvents, ester solvents, hydrocarbons, halogenated hydrocarbon solvents, alcohol solvents, ketone solvents, ether solvents and aromatic hydrocarbons. The organic polymer additive is at least one of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, polylactic acid, polyvinyl alcohol, polyacrylic acid, polyurethane, polyethyleneimine, polythioamine, polystyrene sulfonic acid, polyvinylpyrrolidone, polyvinyl butyral resin and fluorine polymer. The antisolvent is at least one of halogenated hydrocarbon solvent, aromatic hydrocarbon solvent, amide solvent, ether solvent and ester solvent, and has a molecular weight of 200-100000.
Wherein the BX is 2 The concentration of the solution of AX and BX is 0.2-5mol/L 2 The molar ratio of (2) is 0.1-10, and the BX is 2 The molar concentration of the solvent additive and BX in the main solvent is 0.2-2 mol/L 2 The molar ratio of the organic polymer additive to BX is 0-1 2 The molar ratio of (2) is 0.05-5.
Referring to fig. 2, a second preferred embodiment of the perovskite thin film coating apparatus of the present invention comprises a conveyor for conveying a substrate 2, a perovskite solution spraying device, an anti-solvent coating device, and a heat drying device 6. As another example, the heat drying device 6 may be replaced with an air drying device.
The substrate 2 is prepared with a bottom electrode layer in advance, and the conveyor is provided with a conveyor belt 1 or a conveyor shaft (not shown in the figure). The perovskite solution spraying device is provided with a spraying nozzle, the spraying nozzle is a perovskite spraying nozzle 3 ', the anti-solvent coating device is provided with a coating head, the coating head is an anti-solvent coating head 4', and the heating and drying device is provided with an infrared heater 6. The air drying device is provided with an air outlet (not shown in the figures).
The substrate 2 is placed on the conveyor belt 1 or the conveyor shaft and driven by the conveyor belt to sequentially pass through a perovskite solution spraying device, an antisolvent coating device and an air drying device or a heating drying device. The perovskite spray nozzle 3 'sprays perovskite solution on the surface of the substrate 2, and the anti-solvent coating head 4' coats anti-solvent on the surface of the substrate 2. And the perovskite solution and the antisolvent on the surface of the substrate 2 are volatilized and dried simultaneously by wind of the air outlet, and a perovskite film is formed. The infrared heater 6 of the heating and drying device respectively heats the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the perovskite solution and the anti-solvent on the surface of the substrate together to form a perovskite film.
The other components are the same as those of the first embodiment, and will not be described again.
Referring to fig. 3, a third preferred embodiment of the perovskite thin film coating apparatus of the present invention comprises a conveyor for conveying the substrate 2, a precursor solution coating device, an active layer spraying device and an air drying device. As another example, the air drying device may be replaced with a heat drying device.
The substrate 2 is prepared with a bottom electrode layer in advance, and the conveyor is provided with a conveyor belt 1 or a conveyor shaft (not shown in the figure). The precursor solution coating device is provided with a coating head, the coating head is a precursor coating head 7, the activation layer spraying device is provided with a spraying nozzle, the spraying nozzle is an activation spraying nozzle 8, and the air drying device is provided with an air outlet 5. The heating and drying device is provided with an infrared heater (not shown in the figure).
The substrate 2 is placed on the conveyor belt 1 or the conveyor shaft and driven by the conveyor belt to sequentially pass through a precursor solution coating device, an active layer spraying device and an air drying device or a heating and drying device. The precursor coating head 7 coats the precursor solution on the surface of the substrate 2, and the activation spray nozzle 8 sprays the activation solution on the surface of the substrate 2. The wind of the air outlet 5 volatilizes and dries the precursor solution and the activation solution on the surface of the substrate 2 at the same time, and a perovskite film is formed. The infrared heaters of the heating and drying device respectively heat the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the precursor solution and the activation solution on the surface of the substrate together to form the perovskite thin film.
The precursor solution comprises BX 2 Solute, main solvent and solvent additive, the activation solution comprising a solution comprising AX solute, main solvent and organic polymer additive. Wherein B is at least one cation selected from lead (Pb), tin (Sn), tungsten, copper, zinc, gallium, germanium, arsenic, selenium, rhodium, palladium, silver, cadmium, indium, antimony, osmium, iridium, platinum, gold, mercury, thallium, bismuth and polonium. X is iodine (I), bromine (Br), chlorine (Cl), acetate (CH) 3 COO) at least one anion. A is cesium, rubidium, an amine group, an amidino group or at least one cation of the alkali group. The main solvent comprises at least one of amide solvents, sulfone/sulfoxide solvents, ester solvents, hydrocarbons, halogenated hydrocarbon solvents, alcohol solvents, ketone solvents, ether solvents and aromatic hydrocarbon solvents. The solvent additive is at least one of amide solvents, sulfone/sulfoxide solvents, ester solvents, hydrocarbons, halogenated hydrocarbon solvents, alcohol solvents, ketone solvents, ether solvents and aromatic hydrocarbons; the organic polymer additive is at least one of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, polylactic acid, polyvinyl alcohol, polyacrylic acid, polyurethane, polyethyleneimine, polythioamine, polystyrene sulfonic acid, polyvinylpyrrolidone, polyvinyl butyral resin and fluorine polymer. The antisolvent is at least one of halogenated hydrocarbon solvent, aromatic hydrocarbon solvent, amide solvent, ether solvent and ester solvent, and has a molecular weight of 200-100000.
Wherein the BX is 2 The concentration of the solution is 0.2-5mol/LThe concentration of the AX solution is 0.1 mg/ml-100 mg/ml, and the BX is 2 The molar concentration of the solvent additive and BX in the main solvent is 0.2-2 mol/L 2 The molar ratio of the organic polymer additive to the AX main solvent is 0-1, and the volume ratio of the organic polymer additive to the AX main solvent is 0-1.
Referring to fig. 4, a fourth preferred embodiment of the perovskite thin film coating apparatus of the present invention comprises a conveyor for conveying the substrate 2, a precursor solution coating device, an active layer coating device, an anti-solvent spraying device and an air drying device. As another example, the air drying device may be replaced with a heat drying device.
The substrate 2 is prepared with a bottom electrode layer in advance, and the conveyor is provided with a conveyor belt 1 or a conveyor shaft (not shown in the figure). The precursor solution coating device is provided with a coating head, the coating head is a precursor coating head 7, the activation layer coating device is provided with a coating head, the coating head is an activation coating head 8', the antisolvent spraying device is provided with a spraying nozzle, the spraying nozzle is an antisolvent spraying nozzle 4, and the air drying device is provided with an air outlet 5. The heating and drying device is provided with an infrared heater (not shown in the figure).
The substrate 2 is placed on the conveyor belt 1 or the conveyor shaft and driven by the conveyor belt to sequentially pass through a precursor solution coating device, an active layer coating device, an anti-solvent spraying device and an air drying device or a heating and drying device. The precursor coating head 7 coats the precursor solution on the surface of the substrate 2, the activated coating head 8' coats the activated solution on the surface of the substrate 2, and the anti-solvent spraying nozzle 4 sprays the anti-solvent on the surface of the substrate. The wind of the air outlet 5 volatilizes and dries the precursor solution, the activation solution and the anti-solvent on the surface of the substrate 2 at the same time, and forms a perovskite film. The infrared heaters of the heating and drying device respectively heat the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the precursor solution, the activation solution and the anti-solvent on the surface of the substrate together to form the perovskite film.
The other components are the same as those of the third embodiment, and will not be described again.
Referring to fig. 5, a fifth preferred embodiment of the perovskite thin film coating apparatus of the present invention comprises a conveyor for conveying the substrate 2, a precursor solution coating device, an active layer spraying device, an anti-solvent coating device and an air drying device. As another example, the air drying device may be replaced with a heat drying device.
The substrate 2 is prepared with a bottom electrode layer in advance, and the conveyor is provided with a conveyor belt 1 or a conveyor shaft (not shown in the figure). The precursor solution coating device is provided with a coating head, the coating head is precursor coating head 7, the antisolvent coating device is provided with a coating head, the coating head is antisolvent coating head 4', the activation layer spraying device is provided with a spraying nozzle, the spraying nozzle is an activation spraying nozzle 8, the air drying device is provided with an air outlet 5, and the heating drying device is provided with an infrared heater (not shown in the figure).
The substrate 2 is placed on the conveyor belt 1 or the conveyor shaft and driven by the conveyor belt to sequentially pass through a precursor solution coating device, an active layer spraying device, an anti-solvent coating device and an air drying device or a heating and drying device. The precursor coating head 7 coats the precursor solution on the surface of the substrate 2, the activation spray nozzle 8 sprays the activation solution on the surface of the substrate, and the anti-solvent coating head 4' coats the anti-solvent on the surface of the substrate 2. The wind of the air outlet 5 volatilizes and dries the precursor solution, the activation solution and the anti-solvent on the surface of the substrate 2 at the same time, and forms a perovskite film. The infrared heaters of the heating and drying device respectively heat the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the precursor solution, the activation solution and the anti-solvent on the surface of the substrate together to form the perovskite film.
The other components are the same as those of the third embodiment, and will not be described again.
Referring to fig. 6, a sixth preferred embodiment of the perovskite thin film coating apparatus of the present invention comprises a conveyor for conveying the substrate 2, a precursor solution coating device, a front-stage air-drying device, an active layer spraying device and a rear-stage air-drying device. As another example, the front stage air drying device may be replaced with a front stage heat drying device, and the rear stage air drying device may be replaced with a rear stage heat drying device.
The substrate 2 is prepared with a bottom electrode layer in advance, and the conveyor is provided with a conveyor belt 1 or a conveyor shaft (not shown in the figure). The precursor solution coating device is provided with a coating head, the coating head is a precursor coating head 7, the front section air drying device is provided with a front section air outlet 9, the front section heating drying device is provided with an infrared heater (not shown in the figure), the activation layer spraying device is provided with a spraying nozzle, the spraying nozzle is an activation spraying nozzle 8, the rear section air drying device is provided with a rear section air outlet 10, and the rear section heating drying device is provided with an infrared heater (not shown in the figure).
The substrate 2 is placed on the conveyor belt 1 or the conveyor shaft and driven by the conveyor belt to sequentially pass through a precursor solution coating device, a front section air drying device or a front section heating drying device, an active layer spraying device and a rear section air drying device or a rear section heating drying device. The precursor coating head 7 coats the precursor solution on the surface of the substrate 2, and the activation spray nozzle 8 sprays the activation solution on the surface of the substrate 2. The precursor solution on the surface of the substrate 2 is volatilized and dried by the wind of the front-section air outlet 9 to form a precursor film. The infrared heaters of the front-stage heating and drying device respectively heat the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the precursor solution on the surface of the substrate to form a precursor film. The wind of the rear air outlet 10 volatilizes and dries the activated solution on the surface of the substrate 2 and forms a perovskite film. The infrared heaters of the rear-stage heating and drying device respectively heat the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the activated solution on the surface of the substrate and form a perovskite film.
The other components are the same as those of the third embodiment, and will not be described again.
Referring to fig. 7, a seventh preferred embodiment of the perovskite thin film coating apparatus of the present invention comprises a conveyor for conveying the substrate 2, a precursor solution coating device, a front-stage air-drying device, an active layer coating device, an anti-solvent spraying device, and a rear-stage air-drying device. As another example, the front stage air drying device may be replaced with a front stage heat drying device, and the rear stage air drying device may be replaced with a rear stage heat drying device.
The substrate 2 is prepared with a bottom electrode layer in advance, and the conveyor is provided with a conveyor belt 1 or a conveyor shaft (not shown in the figure). The precursor solution coating device is provided with a coating head, the coating head is a precursor coating head 7, the front section air drying device is provided with a front section air outlet 9, the front section heating and drying device is provided with an infrared heater (not shown in the figure), the activation layer coating device is provided with a coating head, the coating head is an activation coating head 8', the antisolvent spraying device is provided with a spraying nozzle, and the spraying nozzle is an antisolvent spraying nozzle 4. The rear-stage air-drying device is provided with a rear-stage air outlet 10, and the rear-stage heating and drying device is provided with an infrared heater (not shown in the figure).
The substrate 2 is placed on the conveyor belt 1 or the conveyor shaft and driven by the conveyor belt to sequentially pass through a precursor solution coating device, a front-stage air drying device or a front-stage heating drying device, an activation layer coating device, an anti-solvent spraying device and a rear-stage air drying device or a rear-stage heating drying device. The precursor coating head 7 coats the precursor solution on the surface of the substrate 2, the activated coating head 8' coats the activated solution on the surface of the substrate 2, and the anti-solvent spraying nozzle 4 sprays the anti-solvent on the surface of the substrate 2. The precursor solution on the surface of the substrate 2 is volatilized and dried by the wind of the front-section air outlet 9 to form a precursor film. The infrared heaters of the front-stage heating and drying device respectively heat the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the precursor solution on the surface of the substrate to form a precursor film. The wind of the rear air outlet 10 volatilizes and dries the activating solution and the antisolvent on the surface of the substrate 2 at the same time, and forms a perovskite film. The infrared heaters of the rear-stage heating and drying device respectively heat the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the activation solution and the anti-solvent on the surface of the substrate together, and form the perovskite film.
The other components are the same as those of the third embodiment, and will not be described again.
Referring to fig. 8, an eighth preferred embodiment of the perovskite thin film coating apparatus of the present invention comprises a conveyor for conveying a substrate 2, a precursor solution coating device, a front stage heating and drying device, an active layer spraying device, an anti-solvent coating device, and a rear stage heating and drying device. As another example, the front stage heating and drying device may be replaced with the front stage air drying device, and the rear stage heating and drying device may be replaced with the rear stage air drying device.
The substrate 2 is prepared with a bottom electrode layer in advance, and the conveyor is provided with a conveyor belt 1 or a conveyor shaft (not shown in the figure). The precursor solution coating device is provided with a coating head, the coating head is a precursor coating head 7, the anti-solvent coating device is provided with a coating head, and the coating head is an anti-solvent coating head 4'. The front-stage air-drying device is provided with a front-stage air outlet (not shown in the figure), and the front-stage heating and drying device is provided with an infrared heater 11. The activation layer spraying device is provided with a spraying nozzle, and the spraying nozzle is an activation spraying nozzle 8. The rear-stage air-drying device is provided with a rear-stage air outlet (not shown in the figure), and the rear-stage heating and drying device is provided with an infrared heater 12.
The substrate 2 is placed on the conveyor belt 1 or the conveyor shaft and driven by the conveyor belt to sequentially pass through a precursor solution coating device, a front-stage air drying device or a front-stage heating drying device, an active layer spraying device, an anti-solvent coating device and a rear-stage air drying device or a rear-stage heating drying device. The precursor coating head 7 coats the precursor solution on the surface of the substrate 2, the activation spray nozzle 8 sprays the activation solution on the surface of the substrate 2, and the anti-solvent coating head 4' coats the anti-solvent on the surface of the substrate 2. And the precursor solution on the surface of the substrate 2 is volatilized and dried by wind of the front-section air outlet to form a precursor film. The infrared heater 11 of the front-stage heating and drying device respectively heats the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the precursor solution on the surface of the substrate to form a precursor film. And the wind at the air outlet at the rear section volatilizes and dries the activating solution and the antisolvent on the surface of the substrate 2 simultaneously to form a perovskite film. The infrared heater 12 of the rear-stage heating and drying device respectively heats the substrate 2 from the upper side and the lower side simultaneously to evaporate and dry the activation solution and the anti-solvent on the surface of the substrate together, and form a perovskite film.
The other components are the same as those of the third embodiment, and will not be described again.
In the foregoing embodiments, the moving speed of the conveyor belt 1 or the conveyor shaft may be uniform or variable, and the speed thereof may be controlled within a range of 0 to 5000 mm/min. The coating heads (the coating heads comprise a perovskite coating head 3, an anti-solvent coating head 4 ', a precursor coating head 7 and an activated coating head 8') are adjustable in height up and down, the vertical distance between the lowest point of the coating heads and a substrate is 1-1000 micrometers, and the fluid flow range of the coating heads is 4-10 5 Milliliters per hour. The spray nozzle (the spray nozzle comprises an antisolvent spray nozzle 4, a perovskite spray nozzle 3' and an activation spray nozzle 8) is adjustable in height, the vertical distance between the lowest point of the spray nozzle and a substrate is 1-10000 microns, the fluid flow range of the spray nozzle is 0-20 liters/min, the fluid temperature of the spray nozzle is a constant value, and the constant value is 0-300 ℃. The vertical distance between the lowest point of the air outlet and the substrate is 100 micrometers-20 cm, the air speed of the air outlet (the air outlet comprises an air outlet 5, a front section air outlet 9 and a rear section air outlet 10 of the air drying device) can be uniform or variable, the air speed is controlled within the range of 0-20 m/s, the air temperature is a fixed value, the fixed value is-10-500 ℃, and the air blowing direction of the air outlet is at least one of vertical, parallel and inclined to the surface of the substrate. The temperature of the heating and drying device is controlled to be a certain value, and the certain value is 30-500 ℃.
The coating head is provided with a slit through which fluid passes, the width of the slit is a fixed value, and the fixed value is 0.0001 cm-1 cm.
A first embodiment of a method of using a perovskite thin film coating apparatus of the present invention includes the steps of:
A1. the substrate with the bottom electrode layer attached thereto is placed on a conveyor belt or a conveyor shaft of a conveyor.
A2. Enabling the substrate to sequentially pass through a perovskite solution coating device, enabling a perovskite coating head to coat perovskite solution on the surface of the substrate, enabling an anti-solvent spraying nozzle to spray anti-solvent on the surface of the substrate through an anti-solvent spraying device, enabling an air outlet or an infrared heater to volatilize or evaporate the perovskite solution and the anti-solvent rapidly through an air drying device or a heating drying device, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
Referring to fig. 9, it can be seen that the perovskite thin film made in this way is dense and has large grains. Referring to FIG. 10, at 16.368cm 2 222.9mW can be made on the area of the perovskite thin film coating equipment, namely the conversion efficiency of 13.6 percent can be achieved, which shows that the perovskite thin film coating equipment has the capacity of large-scale mass production.
A second embodiment of a method of using a perovskite thin film coating apparatus of the present invention includes the steps of:
A3. The substrate with the bottom electrode layer attached thereto is placed on a conveyor belt or a conveyor shaft of a conveyor.
A4. Enabling the substrate to sequentially pass through a perovskite solution spraying device, enabling a perovskite spraying nozzle to spray perovskite solution on the surface of the substrate, enabling an anti-solvent coating head to coat anti-solvent on the surface of the substrate through an anti-solvent coating device, enabling an air outlet or an infrared heater to volatilize or evaporate the perovskite solution and the anti-solvent rapidly through an air drying device or a heating drying device, and finally obtaining and storing the substrate with the perovskite film attached to the surface.
A third embodiment of a method of using a perovskite thin film coating apparatus of the present invention includes the steps of:
B1. the substrate with the bottom electrode layer attached thereto is placed on a conveyor belt or a conveyor shaft of a conveyor.
B2. The substrate sequentially passes through a precursor solution coating device, a precursor coating head coats a precursor solution on the surface of the substrate, an activation spraying nozzle sprays an activation solution on the surface of the substrate through an activation layer spraying device, the precursor solution and the activation solution are quickly volatilized or evaporated through an air drying device or a heating drying device, and finally the substrate with the perovskite film attached on the surface is obtained and stored.
A fourth embodiment of a method of using a perovskite thin film coating apparatus of the present invention includes the steps of:
B3. the substrate with the bottom electrode layer attached thereto is placed on a conveyor belt or a conveyor shaft of a conveyor.
B4. The method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling an activated coating head to coat activated solution on the surface of the substrate through an activated layer coating device, enabling an anti-solvent spraying nozzle to spray anti-solvent on the surface of the substrate through an anti-solvent spraying device, enabling an air drying device or a heating drying device to quickly volatilize or evaporate the precursor solution, the activated solution and the anti-solvent together through an air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
A fifth embodiment of a method of using a perovskite thin film coating apparatus of the invention comprises the steps of:
B6. the substrate with the bottom electrode layer attached thereto is placed on a conveyor belt or a conveyor shaft of a conveyor.
B7. The method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling an activation spraying nozzle to spray activation solution on the surface of the substrate through an activation layer spraying device, enabling an anti-solvent coating head to coat anti-solvent on the surface of the substrate through an anti-solvent coating device, enabling an air drying device or a heating drying device to quickly volatilize or evaporate the precursor solution, the activation solution and the anti-solvent together through an air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and preserving the substrate.
A sixth embodiment of a method of using a perovskite thin film coating apparatus of the invention comprises the steps of:
C1. the substrate with the bottom electrode layer attached thereto is placed on a conveyor belt or a conveyor shaft of an antisolvent coating apparatus conveyor.
C2. The method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling the precursor solution to be quickly volatilized or evaporated through a front-section air drying device or a front-section heating drying device, enabling a front-section air outlet or an infrared heater to be quickly volatilized or evaporated, enabling an activation spray nozzle to spray activation solution on the surface of the substrate through an activation layer spraying device, enabling a rear-section air drying device or a rear-section heating drying device to quickly volatilize or evaporate the activation solution through a rear-section air outlet or the infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
A seventh embodiment of a method of using a perovskite thin film coating apparatus of the invention includes the steps of:
C3. the substrate with the bottom electrode layer attached thereto is placed on a conveyor belt or a conveyor shaft of a conveyor.
C4. The method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling the precursor solution to be quickly volatilized or evaporated through a front-stage air drying device or a front-stage heating drying device, enabling an activated coating head to coat activated solution on the surface of the substrate through an activated layer coating device, enabling an anti-solvent spraying nozzle to spray anti-solvent on the surface of the substrate through an anti-solvent spraying device, enabling the activated solution and the anti-solvent to be quickly volatilized or evaporated through a rear-stage air drying device or a rear-stage heating drying device, and finally obtaining the substrate with the perovskite film attached to the surface and preserving the substrate.
An eighth embodiment of a method of using a perovskite thin film coating apparatus of the invention includes the steps of:
C5. the substrate with the bottom electrode layer attached thereto is placed on a conveyor belt or a conveyor shaft of a conveyor.
C6. The method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling the precursor solution to be quickly volatilized or evaporated through a front-stage air drying device or a front-stage heating drying device, enabling an activating solution to be sprayed on the surface of the substrate through an activating layer spraying device and an activating spraying nozzle, enabling an anti-solvent coating head to coat anti-solvent on the surface of the substrate through an anti-solvent coating device, enabling the activating solution to be quickly volatilized or evaporated through a rear-stage air drying device or a rear-stage heating drying device, enabling the activating solution and the anti-solvent to be quickly volatilized or evaporated through a rear-stage air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
An embodiment of the application of the perovskite thin film coating apparatus of the present invention may also be used to coat a solution containing at least one of the following materials:
vanadium pentoxide (V) 2 O 5 ) Tungsten oxide (WO) 3 ) Molybdenum oxide (MoOx), copper sulfide (CuS), copper sulfide (CuSCN), copper oxide (CuO), copper iodide (CuI), copper oxide (Cu) 2 O), iron disulfide (FeS) 2 ）、CDO 2 Copper-iron semiconductor, lead sulfide (PbS), cobalt oxide (CoOx), cobalt sulfide (CoS), nickel oxide doped with magnesium and lithium (nimgilio), nickel oxide (NiOx), polyethylene dioxythiophene-poly (styrenesulfonate), and highly conductive derivatives thereof (PEDOT: PSS), poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine]Poly-triaryamine, PTAA), 2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino]-9,9' -spirobifluorene (Spiro-OMeTAD), 3-hexyl-substituted polythiophene (P3 HT), titanium dioxide (TiO 2 ) Zinc oxide (ZnO), zinc sulfide (ZnS), zinc selenide (ZnSe), cadmium sulfide (CdS), cadmium selenide (CdSe), bismuth sulfide (Bi) 2 S 3 ) Indium sulfide (In) 2 S 3 ) Indium oxide (In) 2 O 3 ) Antimony sulfide (Sb) 2 S 3 ) Molybdenum disulfide (MoS) 2 ) Selenium disulfide (SnS) 2 ) Tin oxide (SnO) 2 ) PCBM, doped Aluminum Zinc Oxide (AZO), cerium oxide (CeOx), niobium oxide (NbOx), barium titanate (BaTiO) 3 ) Fullerene (C60, C70), zinc-doped cadmium sulfide (Zn) 1-x Cd x S), chromium oxide (CrOx), copper-doped chromium oxide (Cu) x Cr y O 2 ），
Wherein CDO 2 C=cu or Ag in the copper-iron semiconductor type, d= Cr, ga, al, sc, in, Y, fe.
Application example of a method of using a perovskite thin film coating apparatus of the present invention, the perovskite thin film coating apparatus may also be used to coat a solution containing at least one of the following materials:
vanadium pentoxide (V) 2 O 5 ) Tungsten oxide (WO) 3 ) Molybdenum oxide (MoOx), copper sulfide (CuS), copper sulfide (CuSCN), copper oxide (CuO), copper iodide (CuI), copper oxide (Cu) 2 O), iron disulfide (FeS) 2 ）、CDO 2 Copper-iron semiconductor, lead sulfide (PbS), cobalt oxide (CoOx), cobalt sulfide (CoS), nickel oxide doped with magnesium and lithium (nimgilio), nickel oxide (NiOx), polyethylene dioxythiophene-poly (styrenesulfonate), and highly conductive derivatives thereof (PEDOT: PSS), poly [ bis (4-phenyl) (2, 4, 6-trimethylphenyl) amine]Poly-triaryamine, PTAA), 2', 7' -tetrakis [ N, N-bis (4-methoxyphenyl) amino]-9,9' -spirobifluorene (Spiro-OMeTAD), 3-hexyl-substituted polythiophene (P3 HT), titanium dioxide (TiO 2 ) Zinc oxide (ZnO), zinc sulfide (ZnS), zinc selenide (ZnSe), cadmium sulfide (CdS), cadmium selenide (CdSe), bismuth sulfide (Bi) 2 S 3 ) Indium sulfide (In) 2 S 3 ) Indium oxide (In) 2 O 3 ) Antimony sulfide (Sb) 2 S 3 ) Molybdenum disulfide (MoS) 2 ) Selenium disulfide (SnS) 2 ) Tin oxide (SnO) 2 ) PCBM, doped Aluminum Zinc Oxide (AZO), cerium oxide (CeOx), niobium oxide (NbOx), barium titanate (BaTiO) 3 ) Fullerene (C60, C70), zinc-doped cadmium sulfide (Zn) 1-x Cd x S), chromium oxide (CrOx), copper-doped chromium oxide (Cu) x Cr y O 2 ). Wherein CDO 2 C=cu or Ag in the copper-iron semiconductor type, d= Cr, ga, al, sc, in, Y, fe.
The method of using the perovskite thin film coating apparatus of the present invention will be specifically described with reference to examples.
Example 1
(1) PbBr is prepared 2 And MAI is dissolved in 1 ml of DMF according to a molar ratio of 1:1, 0.1wt% of DIO additive is added to prepare 0-2 mol/L perovskite solution, then the perovskite solution is filled into a perovskite solution coating device, the coating flow is set to 100 ml/h, and the height of a coating head is 50 microns.
(2) The antisolvent chlorobenzene was loaded into the spray apparatus, the spray flow was set at 5 liters/min, the spray fluid temperature was 60 ℃, and the nozzle height was 200 microns.
(3) The wind blowing device is started, the height of a wind gap is set to be 1cm, the wind speed is 3m/s, the wind temperature is 170 ℃, and the wind direction is perpendicular to the substrate.
(4) The substrate with the attached bottom electrode layer FTO/CuI is placed on a conveyor belt of a conveyor.
(5) Starting a conveying device, enabling the conveying belt to sequentially pass through a perovskite solution coating device to coat perovskite solution on a substrate, spraying anti-solvent through an anti-solvent spraying device, and enabling various solvents and the anti-solvent to volatilize rapidly through a blowing device to obtain the substrate with MAPbIBr attached thereto 2 A substrate of perovskite thin film.
Example 2
(1) PbI is prepared 2 And MAI was dissolved in 1 ml DMF at a molar ratio of 1:1 and 0.1wt% HI additive was added to make a 1 mole/liter perovskite solution, which was then charged to a perovskite solution spray apparatus and spray flow rate was set at 10 liters/minute, spray fluid temperature 130℃and nozzle height 300 microns.
(2) The antisolvent toluene was charged into the antisolvent coating apparatus, and the coating flow rate was set to 100 ml/hr, and the coating head height was 120. Mu.m.
(3) The heating device was turned on and the heating temperature was set at 160 ℃.
(4) The substrate with the bottom electrode layer ITO/PEDOT: PSS attached thereto was placed on a conveyor belt of a conveyor.
(5) Starting a conveying device, enabling the conveying belt to spray perovskite solution on a substrate sequentially through a perovskite solution spraying device, coating anti-solvent through an anti-solvent coating device, enabling the perovskite solution and the anti-solvent to volatilize rapidly through a heating device, and obtaining the substrate with MAPbI attached 3 A substrate of perovskite thin film.
As shown in fig. 11, the surface relief obtained without the air-drying device is significantly larger than the surface relief after the air-blowing at the air outlet of the air-drying device. The initial, middle and final film thicknesses measured at the initial, middle and final ends of the sample are shown in fig. 12, respectively, and after the air-drying apparatus is used, the film thicknesses measured at the initial, middle and final ends of the sample are relatively uniform, whereas the film thicknesses without the air-drying apparatus are not uniform, and the difference is relatively large. FIG. 13 shows an SEM image of a perovskite thin film without anti-solvent coating and treatment, with a plurality of holes visible on the surface. Fig. 14 shows SEM images of perovskite thin films obtained from anti-solvent coating and treatment, which were flat and dense in grain size.
Example 3
(1) PbI is prepared 2 Adding the powder into DMSO solvent to prepare PbI with concentration of 1.7 mol/L 2 Solution, then the prepared precursor solution PbI 2 The solution is loaded into a precursor solution applicator.
(2) CsBr was mixed with isopropanol to prepare a CsBr solution having a concentration of 10 mg/ml. Thereafter, the prepared CsBr solution was loaded into a spray apparatus.
(3) Placing the FTO substrate with the cavity transmission layer CuI deposited on a conveyor belt of a conveyor, setting the transmission speed to 800mm/min, and coating the height of the coating head to 0.5cm and PbI 2 The solution delivery flow is 3 ml/min, the CsBr solution spraying flow is 1 liter/min, the nozzle temperature is 30 ℃, the air outlet height is 2cm, the air speed is 10m/s, the air temperature is 160 ℃, and the air direction is vertically downward.
(4) Starting a transmission device, and coating PbI on the substrate sequentially through a precursor solution coating device 2 And spraying the CsBr solution through an active layer spraying device, and promoting the reaction of the precursor solution and the active solution through a blowing device. Thus, csPbI 2 A Br perovskite film is formed.
Example 4
(1) PbCl is added 2 Adding the powder into DMF solvent to prepare PbCl with concentration of 1.2 mol/L 2 Solution, then the prepared precursor solution PbCl 2 The solution is charged into the precursor solution applicator 7. MAI was mixed with isopropanol to prepare MAI solution at a concentration of 10 mg/ml. Thereafter, the formulated MAI solution is charged into the coating apparatus 8'.
(2) Placing ITO substrate with deposition bottom electrode layer PEDOT: PSS on a conveyor belt of a conveyor, setting transmission speed of 1000mm/min,the height of the coating heads was 1cm, pbCl 2 The solution delivery flow is 20 ml/min, the MAI solution delivery amount is 2 l/min, the height of an air outlet is 2cm, the air speed is 10m/s, the air temperature is 160 ℃, and the air direction is vertically downward.
(3) The antisolvent chlorobenzene was charged into the spray apparatus, the spray flow was set at 12 ml/min and the spray fluid temperature was 50 ℃.
(4) Starting a conveying device, and enabling the conveying belt to sequentially pass through the precursor solution coating device to coat PbCl 2 The solution is coated with an activating solution MAI by a coating device, chlorobenzene is sprayed by an anti-solvent spraying device, and the generation of a perovskite film and the volatilization of various solvents are promoted by an air blowing device, so that MAPbICl attached with the solution MAPbICl is obtained 2 A substrate of perovskite thin film.
Example 5
(1) SnCl is added 2 The powder was dissolved in NMP solvent to prepare a 1.3 mol/L solution. Then, snCl 2 The solution was charged to the coater 7 and the antisolvent benzene was charged to the coater 4'.
(2) The RbSCN powder was dissolved in isopropanol solvent to prepare an active layer solution RbSCN solution and the solution was loaded into a spray apparatus.
(3) Placing the FTO glass deposited with P3HT on a conveyor belt of a conveying device, setting the transmission speed to 1100mm/min, and setting the heights of coating heads to be 0.35cm and SnCl 2 The solution delivery flow rate is 6 ml/min, the antisolvent delivery flow rate is 0.3 liter/min, the nozzle height of the spraying device is 3cm, the RbSCN solution delivery flow rate is 1.2 liter/min, the nozzle temperature is 25 ℃, the air outlet height is 2cm, the air speed is 10m/s, the air temperature is 160 ℃, and the air direction is vertically downward.
(4) Starting the transmission device, and coating SnCl on the substrate sequentially through the precursor coating device 2 The solution was sprayed with the RbSCN solution by a spray device, the benzene by an antisolvent coating device, and the air blown through a fan port. Thus, rbSnCl 2 The SCN perovskite thin film is fabricated.
Example 6
(1) SnBr is prepared 2 Dissolving the powder in DMSO to obtain CsBr of 1.8 mol/L 2 The solution is prepared into a liquid preparation,then SnBr is added 2 The solution is loaded into the coating apparatus.
(2) CsBr powder was dissolved in isopropyl alcohol solvent to prepare CsBr solution and loaded into a spray apparatus.
(3) Placing ITO glass deposited with an electron transport layer TiO2 on a conveyor belt of a transport device, and setting a coating head with a height of 0.06cm and SnBr 2 The conveying capacity of the solution is 0.8 liter/min, the height of the spraying device is 3cm, the flow rate of CsBr solution is 1 liter/min, the temperature of the nozzle is 50 ℃, the heights of the front-section fan port 9 and the rear-section fan port 10 are 5cm, the wind speed is 6m/s, the wind temperature of the front-section fan is 60 ℃, the wind temperature of the rear-section fan is 160 ℃, and the directions are vertically downward.
(4) Starting a transmission device, and coating SnBr on the substrate sequentially through a precursor solution coating device 2 The solution passes through the front-stage fan, the CsBr solution spraying device and the rear-stage fan. Thus, csSnBr 3 A perovskite thin film is formed.
Example 7
(1) PbI is prepared 2 Adding the powder into DMF solvent to prepare PbI with concentration of 1.1 mol/L 2 Solution, then the prepared precursor solution PbI 2 The solution is charged into the precursor solution applicator 7. MAI was mixed with isopropanol to prepare MAI solution at a concentration of 10 mg/ml. Thereafter, the prepared MAI solution was charged into the coating apparatus 9.
(2) Loading the antisolvent toluene into a spraying device;
(3) Placing ITO substrate with deposition of bottom electrode layer PEDOT: PSS on a conveyor belt of a conveyor, setting transmission speed to 2000mm/min, and coating head I height to 1.8cm, pbI 2 The solution conveying flow rate is 3 milliliters/min, the height of the coating head II is 2cm, the MAI solution conveying flow rate is 3 liters/min, the toluene spraying flow rate is 2 liters/min, the nozzle temperature is 25 ℃, the heights of the front section air outlet and the rear section air outlet are 2cm, the wind directions are vertically downward, the wind speed of the front section fan is 7m/s and the wind temperature is 100 ℃, the wind speed of the rear section fan is 3m/s and the wind temperature is 150 ℃.
(4) Starting a transmission device, and sequentially coating a precursor solution PbI on a substrate by a coating device I 2 The solution volatilizes the solvent through a fan port, and the precursorThe solution becomes a preset film, the coating device is used for coating the MAI solution of the activation solution, the spraying device is used for spraying the anti-solvent toluene, and the later-stage air drying device is used for accelerating the formation of the perovskite film.
Example 8
(1) PbI is prepared 2 Adding the powder into NMP solvent to prepare PbI with concentration of 1.0 mol/L 2 Solution, then the prepared precursor solution PbI 2 The solution is charged into the precursor solution applicator 7. The anti-solvent toluene was charged into the coater 4'.
(2) The FAI was mixed with isopropyl alcohol to prepare a FAI solution having a concentration of 15 mg/ml. Thereafter, the formulated FAI solution is loaded into a spray apparatus.
(3) Placing ITO substrate with cavity transmission layer PTAA deposited on a conveyor belt of a conveyor, setting transmission speed to 1500mm/min, and coating head height to 1.8cm, pbI 2 The solution conveying flow is 1 ml/min, the height of the coating head II is 2cm, the toluene conveying flow is 3 l/min, the FAI solution flow is 2 l/min, the nozzle temperature is 25 ℃, the heights of the front section air outlet and the rear section air outlet are 2cm, the wind directions are vertically downward, the wind speed of the front section fan is 8m/s and the wind temperature is 50 ℃, the wind speed of the rear section fan is 3m/s and the wind temperature is 150 ℃.
(4) Starting a transmission device, and sequentially coating a precursor solution PbI on a substrate by a coating device I 2 The solution is volatilized by a heating device, the precursor solution becomes a preset film to be adhered on a substrate, the activated solution FAI solution is sprayed by a spraying device, the anti-solvent toluene is coated by a coating device, and the formation of the perovskite film is accelerated by a rear-stage heating device.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.

Claims (15)

1. The perovskite thin film coating equipment is characterized by comprising a conveying device for conveying a substrate, a precursor solution coating device, an activation layer coating device, an anti-solvent spraying device and an air drying device or a heating and drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head, the coating head is a precursor coating head, the activation layer coating device is provided with a coating head, the coating head is an activated coating head, the anti-solvent spraying device is provided with a spraying nozzle, the spraying nozzle is an anti-solvent spraying nozzle, the air drying device is provided with an air outlet, the heating and drying device is provided with an infrared heater, the substrate is placed on the conveying belt or the conveying shaft, and is driven by the infrared heater to sequentially pass through the precursor solution coating device, the activation layer coating device, the anti-solvent spraying device and the air drying device or the heating and drying device, the precursor coating head coats the precursor solution on the surface, the activation coating head coats the activated coating solution on the surface of the substrate, the anti-solvent is sprayed on the surface of the activated coating head, the anti-solvent is dried on the surface of the substrate, and the anti-solvent is simultaneously heated and the anti-solvent is dried on the surface of the substrate, and the surface of the substrate is simultaneously heated, and the anti-solvent is simultaneously dried, and the surface of the anti-solvent is simultaneously formed.
2. The perovskite thin film coating equipment is characterized by comprising a conveying device for conveying a substrate, a precursor solution coating device, an activation layer spraying device, an anti-solvent coating device and an air drying device or a heating drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head, the coating head is the precursor coating head, the anti-solvent coating device is provided with the coating head, the coating head is the anti-solvent coating head, the activation layer spraying device is provided with a spraying nozzle, the spraying nozzle is an activation spraying nozzle, the air drying device is provided with an air outlet, the substrate is placed on the conveying belt or the conveying shaft and sequentially driven by the infrared heater to pass through the precursor solution coating device, the activation layer spraying device, the anti-solvent coating device and the air drying device or the heating drying device, the precursor solution is coated on the surface of the substrate, the activation spraying nozzle sprays the precursor solution on the surface of the substrate, the anti-solvent coating head is sprayed on the surface of the substrate, the anti-solvent coating head and the anti-solvent coating device is simultaneously heated on the surface of the substrate, and the anti-solvent coating device is simultaneously heated on the two sides of the substrate, and the surface of the substrate is simultaneously heated, and the anti-solvent is simultaneously dried, and the film is formed.
3. The perovskite film coating equipment is characterized by comprising a conveying device for conveying a substrate, a precursor solution coating device, a front-stage air drying device or a front-stage heating and drying device, an activating layer coating device, an antisolvent spraying device and a rear-stage air drying device or a rear-stage heating and drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head which is a precursor coating head, the front-stage air drying device is provided with a front-stage air outlet, the front-stage heating and drying device is provided with an infrared heater, the activating layer coating device is provided with a coating head which is an activating coating head, the antisolvent spraying device is provided with a spraying nozzle which is an antisolvent spraying nozzle, the rear-stage air drying device is provided with a rear-stage air outlet, the back-stage heating and drying device is provided with an infrared heater, the substrate is placed on the conveyor belt or the conveyor shaft and driven by the conveyor belt or the conveyor shaft to sequentially pass through a precursor solution coating device, a front-stage air drying device or a front-stage heating and drying device, an activation layer coating device, an anti-solvent spraying device and a back-stage air drying device or a back-stage heating and drying device, the precursor coating head coats the precursor solution on the surface of the substrate, the activation coating head coats the activation solution on the surface of the substrate, the anti-solvent spraying nozzle sprays the anti-solvent on the surface of the substrate, the precursor solution on the surface of the substrate is volatilized and dried by the air of the front-stage air outlet to form a precursor film, the precursor solution on the surface of the substrate is vaporized and dried by the infrared heater of the front-stage heating and drying device respectively and simultaneously heated from the upper side and the lower side of the substrate to form the precursor film, the air of the air outlet at the rear section volatilizes and dries the activation solution and the anti-solvent on the surface of the substrate simultaneously to form a perovskite film, and the infrared heater of the rear-section heating and drying device respectively heats the substrate from the upper side and the lower side simultaneously to evaporate and dry the activation solution and the anti-solvent on the surface of the substrate together to form the perovskite film.
4. The perovskite film coating equipment is characterized by comprising a conveying device for conveying a substrate, a precursor solution coating device, a front-stage air drying device or a front-stage heating and drying device, an activation layer spraying device, an anti-solvent coating device and a rear-stage air drying device or a rear-stage heating and drying device, wherein the substrate is provided with a bottom electrode layer in advance, the conveying device is provided with a conveying belt or a conveying shaft, the precursor solution coating device is provided with a coating head which is a precursor coating head, the anti-solvent coating device is provided with a coating head which is an anti-solvent coating head, the front-stage air drying device is provided with a front-stage air outlet, the front-stage heating and drying device is provided with an infrared heater, the activation layer spraying device is provided with a spraying nozzle which is an activation spraying nozzle, the rear-stage air drying device is provided with a rear-stage air outlet, the back-stage heating and drying device is provided with an infrared heater, the substrate is placed on the conveyor belt or the conveyor shaft and driven by the conveyor belt or the conveyor shaft to sequentially pass through a precursor solution coating device, a front-stage air drying device or a front-stage heating and drying device, an active layer spraying device, an anti-solvent coating device and a back-stage air drying device or a back-stage heating and drying device, the precursor coating head coats the precursor solution on the surface of the substrate, the active spraying nozzle sprays the active solution on the surface of the substrate, the anti-solvent coating head coats the anti-solvent on the surface of the substrate, the precursor solution on the surface of the substrate is volatilized and dried by the air of the front-stage air outlet to form a precursor film, the precursor solution on the surface of the substrate is vaporized and dried by the infrared heater of the front-stage heating and drying device from the upper side and the lower side of the substrate simultaneously to form the precursor film, the air of the air outlet at the rear section volatilizes and dries the activation solution and the anti-solvent on the surface of the substrate simultaneously to form a perovskite film, and the infrared heater of the rear-section heating and drying device respectively heats the substrate from the upper side and the lower side simultaneously to evaporate and dry the activation solution and the anti-solvent on the surface of the substrate together to form the perovskite film.
5. The perovskite thin film coating apparatus as claimed in any one of claims 1 to 4, wherein the moving speed of the conveyor belt or the conveyor shaft may be uniform or variable, and the speed thereof is controlled to be in the range of 0 to 5000 mm/min; the vertical distance between the lowest point of the coating head and the substrate is 1-1000 micrometers, and the fluid flow range of the coating head is 4-10 5 Milliliters per hour; the vertical distance between the lowest point of the spray nozzle and the substrate is 1-10000 microns, the fluid flow range of the spray nozzle is 0-20 liters/min, the fluid temperature of the spray nozzle is a fixed value, and the fixed value is 0-300 ℃; the vertical distance between the lowest point of the air outlet and the substrate is 100 micrometers-20 cm, the air speed of the air outlet can be uniform or variable, the air speed is controlled within the range of 0-20 m/s, the air temperature is a fixed value, the fixed value is-10-500 ℃, and the air blowing direction of the air outlet is at least one of vertical, parallel and inclined to the surface of the substrate; the temperature of the heating and drying device is controlled to be a certain value, and the certain value is 30-500 ℃.
6. The perovskite thin film coating apparatus as claimed in any one of claims 1 to 4, wherein the coating head is provided with a slit through which a fluid passes, and the width of the slit is a constant value of 0.0001cm to 1cm.
7. The perovskite thin film coating apparatus as claimed in any one of claims 1 to 4, wherein the precursor solution comprises a solution containing BX 2 Solute, main solvent and solvent additive, the activation solution packageComprises an AX solute, a main solvent and an organic polymer additive; wherein B is at least one cation of lead (Pb), tin (Sn), tungsten, copper, zinc, gallium, germanium, arsenic, selenium, rhodium, palladium, silver, cadmium, indium, antimony, osmium, iridium, platinum, gold, mercury, thallium, bismuth and polonium; x is iodine (I), bromine (Br), chlorine (Cl), acetate (CH) 3 COO) at least one anion; a is cesium, rubidium, amino, amidino or at least one cation in alkali group; the main solvent comprises at least one of amide solvents, sulfone/sulfoxide solvents, ester solvents, hydrocarbons, halogenated hydrocarbon solvents, alcohol solvents, ketone solvents, ether solvents and aromatic hydrocarbon solvents; the solvent additive is at least one of amide solvents, sulfone/sulfoxide solvents, ester solvents, hydrocarbons, halogenated hydrocarbon solvents, alcohol solvents, ketone solvents, ether solvents and aromatic hydrocarbons; the organic polymer additive is at least one of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, polylactic acid, polyvinyl alcohol, polyacrylic acid, polyurethane, polyethyleneimine, polythioamine, polystyrene sulfonic acid, polyvinylpyrrolidone, polyvinyl butyral resin and fluorine polymer; the antisolvent is at least one of halogenated hydrocarbon solvent, aromatic hydrocarbon solvent, amide solvent, ether solvent and ester solvent, and has molecular weight of 200-100000.
8. The perovskite thin film coating apparatus of claim 7, wherein the BX 2 The concentration of the solution of AX is 0.2-5mol/L, the concentration of the solution of AX is 0.1 mg/ml-100 mg/ml, and the concentration of BX is 0.1mg/ml 2 The molar concentration of the solvent additive and BX in the main solvent is 0.2-2 mol/L 2 The molar ratio of the organic polymer additive to the AX is 0-1, and the volume ratio of the organic polymer additive to the AX main solvent is 0-1.
9. A method of using the perovskite thin film coating apparatus as claimed in claim 1, comprising the steps of:
B3. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
B4. the method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling an activated coating head to coat activated solution on the surface of the substrate through an activated layer coating device, enabling an anti-solvent spraying nozzle to spray anti-solvent on the surface of the substrate through an anti-solvent spraying device, enabling an air drying device or a heating drying device to quickly volatilize or evaporate the precursor solution, the activated solution and the anti-solvent together through an air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
10. A method of using the perovskite thin film coating apparatus as claimed in claim 2, comprising the steps of:
B6. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
B7. the method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling an activation spraying nozzle to spray activation solution on the surface of the substrate through an activation layer spraying device, enabling an anti-solvent coating head to coat anti-solvent on the surface of the substrate through an anti-solvent coating device, enabling an air drying device or a heating drying device to quickly volatilize or evaporate the precursor solution, the activation solution and the anti-solvent together through an air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and preserving the substrate.
11. A method of using the perovskite thin film coating apparatus as claimed in claim 3, comprising the steps of:
C3. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
C4. the method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling the precursor solution to be quickly volatilized or evaporated through a front-stage air drying device or a front-stage heating drying device, enabling an activated coating head to coat activated solution on the surface of the substrate through an activated layer coating device, enabling an anti-solvent spraying nozzle to spray anti-solvent on the surface of the substrate through an anti-solvent spraying device, enabling the activated solution and the anti-solvent to be quickly volatilized or evaporated through a rear-stage air drying device or a rear-stage heating drying device, and finally obtaining the substrate with the perovskite film attached to the surface and preserving the substrate.
12. A method of using the perovskite thin film coating apparatus as claimed in claim 4, comprising the steps of:
C5. placing the substrate with the bottom electrode layer attached on a conveyor belt or a conveyor shaft of a conveyor device;
C6. the method comprises the steps of enabling a substrate to sequentially pass through a precursor solution coating device, enabling a precursor coating head to coat precursor solution on the surface of the substrate, enabling the precursor solution to be quickly volatilized or evaporated through a front-stage air drying device or a front-stage heating drying device, enabling an activating solution to be sprayed on the surface of the substrate through an activating layer spraying device and an activating spraying nozzle, enabling an anti-solvent coating head to coat anti-solvent on the surface of the substrate through an anti-solvent coating device, enabling the activating solution to be quickly volatilized or evaporated through a rear-stage air drying device or a rear-stage heating drying device, enabling the activating solution and the anti-solvent to be quickly volatilized or evaporated through a rear-stage air outlet or an infrared heater, and finally obtaining the substrate with the perovskite film attached to the surface and storing the substrate.
13. The method of using the perovskite thin film coating apparatus as claimed in any one of claims 9 to 12, wherein the speed of movement of the conveyor belt or the conveyor shaft may be uniform or variable, and the speed is controlled within a range of 0 to 5000 mm/min; the vertical distance between the lowest point of the coating head and the substrate is 1-1000 micrometers, and the fluid flow range of the coating head is 4-10 5 Milliliters per hour; the vertical distance between the lowest point of the spray nozzle and the substrate is 1-10000 microns, the fluid flow range of the spray nozzle is 0-20 liters/min, the fluid temperature of the spray nozzle is a fixed value, and the fixed value is 0-300 ℃; the height of the air outlet can be adjusted, and the lowest point of the air outlet is perpendicular to the substrateThe distance is 100 micrometers-20 cm, the wind speed of the air outlet can be uniform or variable, the wind speed is controlled within the range of 0-20 m/s, the wind temperature is a fixed value, the fixed value is-10-500 ℃, and the wind blowing direction of the air outlet is vertical, parallel and inclined to at least one of the surfaces of the substrates; the temperature of the heating and drying device is controlled to be a certain value, and the certain value is 30-500 ℃.
14. The method of using the perovskite thin film coating apparatus as claimed in any one of claims 9 to 12, wherein the precursor solution comprises a solution containing BX 2 A solute, a primary solvent, and a solvent additive, the activation solution comprising a solution comprising AX solute, primary solvent, and an organic polymer additive; wherein B is at least one cation of lead (Pb), tin (Sn), tungsten, copper, zinc, gallium, germanium, arsenic, selenium, rhodium, palladium, silver, cadmium, indium, antimony, osmium, iridium, platinum, gold, mercury, thallium, bismuth and polonium; x is iodine (I), bromine (Br), chlorine (Cl), acetate (CH) 3 COO) at least one anion; a is cesium, rubidium, amino, amidino or at least one cation in alkali group; the main solvent comprises at least one of amide solvents, sulfone/sulfoxide solvents, ester solvents, hydrocarbons, halogenated hydrocarbon solvents, alcohol solvents, ketone solvents, ether solvents and aromatic hydrocarbon solvents; the solvent additive is at least one of amide solvents, sulfone/sulfoxide solvents, ester solvents, hydrocarbons, halogenated hydrocarbon solvents, alcohol solvents, ketone solvents, ether solvents and aromatic hydrocarbons; the organic polymer additive is at least one of polyethylene glycol, polypropylene glycol, polyvinylpyrrolidone, polylactic acid, polyvinyl alcohol, polyacrylic acid, polyurethane, polyethyleneimine, polythioamine, polystyrene sulfonic acid, polyvinylpyrrolidone, polyvinyl butyral resin and fluorine polymer; the antisolvent is at least one of halogenated hydrocarbon solvent, aromatic hydrocarbon solvent, amide solvent, ether solvent and ester solvent, and has molecular weight of 200-100000.
15. The method of using the perovskite thin film coating apparatus as claimed in claim 14, wherein theBX 2 The concentration of the solution of AX is 0.2-5mol/L, the concentration of the solution of AX is 0.1 mg/ml-100 mg/ml, and the concentration of BX is 0.1mg/ml 2 The molar concentration of the solvent additive and BX in the main solvent is 0.2-2 mol/L 2 The molar ratio of the organic polymer additive to the AX is 0-1, and the volume ratio of the organic polymer additive to the AX main solvent is 0-1.
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