WO2019000642A1 - A method for preparing a flexible perovskite solar cell by blade coating - Google Patents

A method for preparing a flexible perovskite solar cell by blade coating Download PDF

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Publication number
WO2019000642A1
WO2019000642A1 PCT/CN2017/100919 CN2017100919W WO2019000642A1 WO 2019000642 A1 WO2019000642 A1 WO 2019000642A1 CN 2017100919 W CN2017100919 W CN 2017100919W WO 2019000642 A1 WO2019000642 A1 WO 2019000642A1
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transport layer
blade coating
perovskite
layer
hole transport
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PCT/CN2017/100919
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French (fr)
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Baomin Xu
Jishu GAO
Hang HU
Jiabang CHEN
Chang Liu
Jianchang Wu
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South University Of Science And Technology Of China
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/10—Deposition of organic active material
    • H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/40—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising a p-i-n structure, e.g. having a perovskite absorber between p-type and n-type charge transport layers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K77/00—Constructional details of devices covered by this subclass and not covered by groups H10K10/80, H10K30/80, H10K50/80 or H10K59/80
    • H10K77/10—Substrates, e.g. flexible substrates
    • H10K77/111—Flexible substrates
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K85/00—Organic materials used in the body or electrodes of devices covered by this subclass
    • H10K85/50—Organic perovskites; Hybrid organic-inorganic perovskites [HOIP], e.g. CH3NH3PbI3
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
    • H10K30/50—Photovoltaic [PV] devices
    • 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

Definitions

  • the present disclosure belongs to the field related to the energy material technology, and relates to a method for preparing a flexible perovskite solar cell, especially to a method for preparing a flexible perovskite solar cell by blade coating.
  • Perovskite solar cell is a novel solar cell evolved from the dye-sensitized solar cell.
  • the perovskite layer first absorbs photons to produce electron-hole pairs when accepting irradiation from sunlight. Due to the difference in the exciton binding energy of the perovskite material, these carriers either become free carriers or form excitons. Then, these uncomposited electrons and holes are collected separately by the electron transport layer and the hole transport layer, i.e., the electrons are transported from the perovskite layer to the electron transport layer and finally collected by the conductive substrate; and the holes are transported from the perovskite layer to the hole transport layer and finally collected by the metal electrode.
  • Perovskite solar cell comprises from bottom to top a glass conductive substrate (FTO) , an electron transport layer (ETM) , a perovskite light absorption layer (including a porous support) , a hole transport layer (HTM) and a back electrode, respectively.
  • FTO glass conductive substrate
  • ETM electron transport layer
  • HTM hole transport layer
  • the spin coating method is still the major method, and a uniform perovskite film can be obtained more conveniently by this method.
  • this technique has the disadvantages of great loss of raw materials, high cost, low rate, and is unsuitable for large-scale industrial production.
  • the perovskite layer and other major related functional layers are mainly prepared in a glove box depending on the protection from inert gas. This is a huge restriction to the future mass production of the perovskite.
  • Conductive glass substrate is commonly used in the current technologies, however the glass substrate has strong brittleness, and cannot be bent, which will bring limitations to the subsequent preparation of the functional layers, meanwhile seriously restricting the large-scale use of the perovskite solar cells.
  • the present disclosure aims at providing a simple and efficient method for preparing a flexible perovskite solar cell by use of blade coating, which mainly shows benefits of more simple and efficient printing preparation method, low requirement for the equipment and cost saving, moreover a high-quality flexible perovskite solar cell can be prepared efficiently in the air using the method according to the present disclosure.
  • the present disclosure provides a method for preparing a flexible perovskite solar cell by blade coating, which comprises the following step:
  • a hole transport layer, a perovskite layer and an electron transport layer can be prepared successively on the flexible conductive substrate by a blade coating method, then a back electrode is prepared on the electron transport layer.
  • an electron transport layer, a perovskite layer and a hole transport layer can be prepared successively on a flexible conductive substrate by a blade coating method, then a back electrode is prepared on the hole transport layer.
  • the back electrode is any one or a combination of both of a metal electrode and a carbon electrode.
  • the method comprises the following steps:
  • the flexible conductive substrate is heated at 60°C-70°C, the blade coating speed is 20 mm/s-25 mm/s, and the height of the blade is 50 ⁇ m-60 ⁇ m;
  • the temperature of the hole transport layer is 130°C-135°C
  • the temperature of the mixed solution is 80°C-90°C
  • the blade coating speed is 15 mm/s-20 mm/s
  • the height of the blade is 50 ⁇ m-80 ⁇ m
  • the temperature of the perovskite layer is 25°C-30°C
  • the blade coating speed is 18 mm/s-25 mm/s
  • the height of the blade is 65 ⁇ m-80 ⁇ m
  • the method for allowing the temperature of the hole transport layer to be 130°C in step (2) can be in such a manner that the composite layer composed of the flexible conductive substrate and the hole transport layer is placed on a hot stage which is heated to 130°C.
  • the composite layer is immediately removed away from the hot stage after the completion of blade coating in step (2) .
  • the method comprises the following steps:
  • the temperature of the flexible conductive substrate is 25°C-30°C
  • the blade coating speed is 18 mm/s-25 mm/s
  • the height of the blade is 65 ⁇ m-80 ⁇ m
  • the temperature of the electron transport layer is 130°C-135°C
  • the temperature of the mixed solution is 80°C-90°C
  • the blade coating speed is 15 mm/s-20 mm/s
  • the height of the blade is 50 ⁇ m-80 ⁇ m
  • the perovskite layer is heated at a temperature of 60°C-70°C, the blade coating speed is 20 mm/s-25 mm/s, and the height of the blade is 50 ⁇ m-60 ⁇ m;
  • the method for allowing the temperature of the electron transport layer to be 130°C in step (2) can be in such a manner that the composite layer composed of the flexible conductive substrate and the electron transport layer is placed on a hot stage which is heated to 130°C.
  • the size of the flexible conductive substrate is (2 cm-4 cm) ⁇ (2 cm-4 cm) , for example 2 cm ⁇ 2 cm, 3 cm ⁇ 3 cm or 4 cm ⁇ 4 cm, and the like.
  • the size of the flexible conductive substrate according to the present disclosure is preferably (2 cm-4 cm) ⁇ (2 cm-4 cm) , such that more uniform film-forming area can be obtained on a larger area by use of the blade coating process, and the performance of the resulting flexible perovskite solar cell can be improved by selecting a uniform film-forming area for the subsequent steps.
  • the flexible conductive substrate is a transparent polymer film with indium tin oxide (ITO) , preferably any one of polyethylene naphthalate (PEN) /ITO, polyethylene terephthalate (PET) /ITO or polyimide (PI) /ITO.
  • ITO indium tin oxide
  • PEN polyethylene naphthalate
  • PET polyethylene terephthalate
  • PI polyimide
  • the solution of the hole transport layer is a mixed solution of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS) , polystyrene sulfonic acid (PSSA) and isopropanol.
  • PEDOT polyethylenedioxythiophene
  • PSSA polystyrene sulfonic acid
  • the mass ratio of (PEDOT: PSS) , PSSA and isopropanol is 1: (0.25-0.5) : (3-5) .
  • the solution of the hole transport layer is filtered prior to use in order to improve the uniformity and increase the film-forming effect.
  • the ratio of the volume of the solution of the hole transport layer to the area of the flexible conductive substrate is 35 ⁇ L/ (1.5 cm ⁇ 1.5 cm) , and under the condition of such ratio, a suitable film-forming thickness and good uniformity can be obtained.
  • the precursor solution of the perovskite is prepared by the method of mixing lead acetate and methylamine iodide in a molar ratio of 1: 1, then dissolving the resulting mixture in N,N-dimethylformamide (DMF) .
  • DMF N,N-dimethylformamide
  • the concentration of the precursor solution of the perovskite is 500 mg/ml-600 mg/ml, for example 500 mg/ml, 540 mg/ml, 550 mg/ml, 560 mg/ml, 580 mg/ml or 600 mg/ml, and the like, and preferably 580 mg/ml.
  • the ratio of the volume of the precursor solution of the perovskite to the area of the flexible conductive substrate is 70 ⁇ L/ (1.5 cm ⁇ 1.5 cm) . Under the condition of such ratio, a suitable film-forming thickness and good uniformity can be obtained, and the contact with the electron transport layer or the hole transport layer is better as well.
  • the precursor solution of the electron transport layer is a solution of methyl [6.6] -phenyl-C61-butyrate (PCBM) and/or methyl [6.6] -phenyl-C71-butyrate (PCBM) in chlorobenzene.
  • PCBM methyl [6.6] -phenyl-C61-butyrate
  • PCBM methyl [6.6] -phenyl-C71-butyrate
  • the concentration of the precursor solution of the electron transport layer is 15 mg/ml-20 mg/ml, and preferably 20 mg/ml.
  • the solution of the electron transport layer is filtered prior to use in order to improve the uniformity and increase the film-forming effect.
  • the ratio of the volume of the precursor solution of the electron transport layer to the area of the flexible conductive substrate is (35 ⁇ L-40 ⁇ L) / (1.5 cm ⁇ 1.5 cm) , and under the condition of such ratio, a suitable film-forming thickness and good uniformity can be obtained, and the contact with the perovskite layer is better as well.
  • the standing time is 25 min-35 min, and preferably 30 min.
  • the method for preparing a back electrode on the perovskite layer is any one of evaporation, screen printing or printing.
  • the method further comprises a step of cutting or cropping the flexible solar cell for test or for preparing the device.
  • the present disclosure has the following beneficial effects:
  • the present disclosure adopts a transparent polymer film flexible substrate with ITO instead of the traditional glass substrate, and all the functional layers (the hole transport layer, the perovskite layer and the electron transport layer) are coated with a blade coating method instead of a spin coating method, furthermore, the lead source is limited to lead acetate and the parameters such as the temperature of the blade coating solution during blade coating, the temperature of the flexible conductive substrate or the composite substrate (i.e.
  • a composite substrate consisted of a flexible conductive substrate and a hole transport layer and/or an electron transport layer
  • the blade coating speed and the height of blade, etc. are adjusted, such that a high-quality flexible perovskite solar cell can be prepared efficiently in the air (air humidity is 30 or lower) , thereby replacing the preparation in a glove box, making the operation easier and reducing the cost, meanwhile reducing the effect of introduction of unfavorable factors on the preparation method and properties of the products.
  • Figure 1 is a schematic diagram of the structure of a flexible perovskite solar cell according to Example 1.
  • Figure 2 is a schematic diagram of the structure of a flexible perovskite solar cell according to Example 2.
  • Figure 3 is a schematic diagram of the structure of a flexible perovskite solar cell according to Example 3.
  • Figure 4 is a schematic diagram of the structure of a flexible perovskite solar cell according to Example 4.
  • the present example provides a method for preparing a flexible perovskite solar cell by blade coating, specifically the method comprises the steps of first coating a hole transport layer on a flexible substrate, followed by coating a perovskite layer as a photosensitive layer on the basis of the hole transport layer, then coating an electron transport layer on the perovskite layer, and finally evaporating a metal electrode.
  • the flexible conductive substrate was heated at 60°C, the blade coating speed was 20 mm/s, and the height of the blade was 50 ⁇ m;
  • the temperature of the hole transport layer was 130°C
  • the temperature of the mixed solution was 85°C
  • the blade coating speed was 20 mm/s
  • the height of the blade was 50 ⁇ m
  • the temperature of the perovskite layer was 25°C
  • the blade coating speed was 20 mm/s
  • the height of the blade was 75 ⁇ m
  • the present example provides a method for preparing a flexible perovskite solar cell by blade coating, specifically the method comprises the steps of first coating an electron transport layer on a flexible substrate, followed by coating a perovskite layer as a photosensitive layer on the basis of the electron transport layer, then coating a hole transport layer on the perovskite layer, and finally evaporating a metal electrode.
  • the temperature of the flexible conductive substrate was 25°C-30°C, the blade coating speed was 18 mm/s, and the height of the blade was 75 ⁇ m;
  • the temperature of the electron transport layer was 132°C
  • the temperature of the mixed solution was 90°C
  • the blade coating speed was 15 mm/s
  • the height of the blade was 80 ⁇ m
  • the temperature of the perovskite layer was 68°C, the blade coating speed was 25mm/s, and the height of the blade was 63 ⁇ m;
  • the present example provides a method for preparing a flexible perovskite solar cell by blade coating, specifically the method comprises the steps of first coating a hole transport layer on a flexible substrate, followed by coating a perovskite layer as a photosensitive layer on the basis of the hole transport layer, then coating an electron transport layer on the perovskite layer, and finally printing a carbon electrode.
  • the flexible conductive substrate was heated at 65°C, the blade coating speed was 25 mm/s, and the height of the blade was 60 ⁇ m;
  • the temperature of the hole transport layer was 135°C
  • the temperature of the mixed solution was 88°C
  • the blade coating speed was 22 mm/s
  • the height of the blade was 65 ⁇ m
  • the present example provides a method for preparing a flexible perovskite solar cell by blade coating, specifically the method comprises the steps of first coating an electron transport layer on a flexible substrate, followed by coating a perovskite layer as a photosensitive layer on the basis of the electron transport layer, then coating a hole transport layer on the perovskite layer, and finally printing a carbon electrode.
  • blade coating 45 ⁇ L of a solution of an electron transport layer (a solution of PCBM in chlorobenzene with a concentration of 30 mg/ml) on a flexible conductive substrate (1.5 cm ⁇ 1.5 cm), which was then allowed to stand for 40 min and dried to obtain an electron transport layer on the flexible conductive substrate;
  • the temperature of the electron transport layer was 130°C
  • the temperature of the mixed solution was 90°C
  • the blade coating speed was 20 mm/s
  • the height of the blade was 65 ⁇ m
  • the temperature of the perovskite layer was 70°C
  • the blade coating speed was 20 mm/s
  • the height of the blade was 60 ⁇ m

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Abstract

A method for preparing a flexible perovskite solar cell by blade coating, which comprises the following steps: preparing a hole transport layer, a perovskite layer and an electron transport layer on a flexible conductive substrate by a blade coating method. The method is simple in preparation process and has low requirements for the equipment, the advantages from using the blade coating method lie in that the costs can be saved to the greatest extent and the green production can be realized.

Description

A METHOD FOR PREPARING A FLEXIBLE PEROVSKITE SOLAR CELL BY BLADE COATING FIELD
The present disclosure belongs to the field related to the energy material technology, and relates to a method for preparing a flexible perovskite solar cell, especially to a method for preparing a flexible perovskite solar cell by blade coating.
BACKGROUND
Perovskite solar cell is a novel solar cell evolved from the dye-sensitized solar cell. The perovskite layer first absorbs photons to produce electron-hole pairs when accepting irradiation from sunlight. Due to the difference in the exciton binding energy of the perovskite material, these carriers either become free carriers or form excitons. Then, these uncomposited electrons and holes are collected separately by the electron transport layer and the hole transport layer, i.e., the electrons are transported from the perovskite layer to the electron transport layer and finally collected by the conductive substrate； and the holes are transported from the perovskite layer to the hole transport layer and finally collected by the metal electrode. Perovskite solar cell comprises from bottom to top a glass conductive substrate (FTO) , an electron transport layer (ETM) , a perovskite light absorption layer (including a porous support) , a hole transport layer (HTM) and a back electrode, respectively.
In the existing methods, the spin coating method is still the major method, and a uniform perovskite film can be obtained more conveniently by this method. However, this technique has the disadvantages of great loss of raw materials, high cost, low rate, and is unsuitable for large-scale industrial production. In the current technologies, the perovskite layer and other major related functional layers are mainly prepared in a glove box depending on the protection from inert gas. This is a huge restriction to the future mass production of the perovskite. Conductive glass substrate is commonly used in the current technologies, however the glass substrate has strong brittleness, and cannot be bent, which will bring limitations to the subsequent preparation of the functional layers, meanwhile seriously restricting the large-scale use of the perovskite solar cells.
SUMMARY
In view of the above-mentioned problems existing in the related technics, the present disclosure aims at providing a simple and efficient method for preparing a flexible perovskite solar cell by use of blade coating, which mainly shows benefits of more simple and efficient printing preparation method, low requirement for the equipment and cost saving, moreover a high-quality flexible perovskite solar cell can be prepared efficiently in the air using the method according to the present disclosure.
To achieve the above objects, the present disclosure adopts the following technical solution:
The present disclosure provides a method for preparing a flexible perovskite solar cell by blade coating, which comprises the following step:
preparing a hole transport layer, a perovskite layer and an electron transport layer on a flexible conductive substrate by a blade coating method.
In the present disclosure, a hole transport layer, a perovskite layer and an electron transport layer can be prepared successively on the flexible conductive substrate by a blade coating method, then a back electrode is prepared on the electron transport layer. Alternatively, an electron transport layer, a perovskite layer and a hole transport layer can be prepared successively on a flexible conductive substrate by a blade coating method, then a back electrode is prepared on the hole transport layer.
Preferably, the back electrode is any one or a combination of both of a metal electrode and a carbon electrode.
As a preferred technical solution of the method according to the present disclosure, the method comprises the following steps:
(1) blade coating a precursor solution of a hole transport layer on a flexible conductive substrate, then annealing at 110℃-120℃ for 15 min-20 min to obtain a hole transport layer on the flexible conductive substrate；
wherein during blade coating, the flexible conductive substrate is heated at 60℃-70℃, the blade coating speed is 20 mm/s-25 mm/s， and the height of the blade is 50 μm-60 μm；
(2) blade coating a precursor solution of perovskite on the hole transport layer, then annealing at 90℃-95℃ for 10 min-30 min to obtain a perovskite layer on the hole transport layer；
wherein during blade coating, the temperature of the hole transport layer is 130℃-135℃, the temperature of the mixed solution is 80℃-90℃, the blade coating speed is 15 mm/s-20 mm/s, and the height of the blade is 50 μm-80 μm；
(3) blade coating a solution of an electron transport layer on the perovskite layer, which is then allowed to stand and dried to obtain an electron transport layer on the perovskite layer；
wherein during blade coating, the temperature of the perovskite layer is 25℃-30℃, the blade coating speed is 18 mm/s-25 mm/s， and the height of the blade is 65 μm-80 μm；
(4) preparing a back electrode on the electron transport layer to obtain a flexible perovskite solar cell.
In this preferred technical solution, the method for allowing the temperature of the hole transport layer to be 130℃ in step (2) can be in such a manner that the composite layer composed of the flexible conductive substrate and the hole transport layer is placed on a hot stage which is  heated to 130℃.
In this preferred technical solution, the composite layer is immediately removed away from the hot stage after the completion of blade coating in step (2) .
As a further preferred technical solution of the method according to the present disclosure, the method comprises the following steps:
(1) blade coating a solution of an electron transport layer on a flexible conductive substrate, which is then allowed to stand and dried to obtain an electron transport layer on the flexible conductive substrate；
wherein during blade coating, the temperature of the flexible conductive substrate is 25℃-30℃, the blade coating speed is 18 mm/s-25 mm/s， and the height of the blade is 65 μm-80 μm；
(2) blade coating a precursor solution of perovskite on the electron transport layer, then annealing at 90℃-95℃ for 10 min-30 min to obtain a perovskite layer on the electron transport layer；
wherein during blade coating, the temperature of the electron transport layer is 130℃-135℃, the temperature of the mixed solution is 80℃-90℃, the blade coating speed is 15 mm/s-20 mm/s, and the height of the blade is 50 μm-80 μm；
(3) blade coating a solution of a hole transport layer on the perovskite layer, then annealing at 110℃-120℃ for 15 min-20 min to obtain a hole transport layer on the perovskite layer；
wherein during blade coating, the perovskite layer is heated at a temperature of 60℃-70℃, the blade coating speed is 20 mm/s-25 mm/s， and the height of the blade is 50 μm-60 μm；
(4) preparing a back electrode on the hole transport layer to obtain a flexible perovskite solar cell.
In this preferred technical solution, the method for allowing the temperature of the electron transport layer to be 130℃ in step (2) can be in such a manner that the composite layer composed of the flexible conductive substrate and the electron transport layer is placed on a hot stage which is heated to 130℃.
Preferably, the size of the flexible conductive substrate is (2 cm-4 cm) × (2 cm-4 cm) , for example 2 cm × 2 cm, 3 cm × 3 cm or 4 cm × 4 cm, and the like.
The size of the flexible conductive substrate according to the present disclosure is preferably (2 cm-4 cm) × (2 cm-4 cm) , such that more uniform film-forming area can be obtained on a larger area by use of the blade coating process, and the performance of the resulting flexible perovskite solar cell can be improved by selecting a uniform film-forming area for the subsequent steps.
Preferably, the flexible conductive substrate is a transparent polymer film with indium tin  oxide (ITO) , preferably any one of polyethylene naphthalate (PEN) /ITO, polyethylene terephthalate (PET) /ITO or polyimide (PI) /ITO.
Preferably, the solution of the hole transport layer is a mixed solution of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS) , polystyrene sulfonic acid (PSSA) and isopropanol.
Preferably, in the solution of the hole transport layer, the mass ratio of (PEDOT: PSS) , PSSA and isopropanol is 1: (0.25-0.5) : (3-5) .
Preferably, the solution of the hole transport layer is filtered prior to use in order to improve the uniformity and increase the film-forming effect.
Preferably, the ratio of the volume of the solution of the hole transport layer to the area of the flexible conductive substrate is 35 μL/ (1.5 cm × 1.5 cm) ， and under the condition of such ratio， a suitable film-forming thickness and good uniformity can be obtained.
Preferably, the precursor solution of the perovskite is prepared by the method of mixing lead acetate and methylamine iodide in a molar ratio of 1: 1, then dissolving the resulting mixture in N,N-dimethylformamide (DMF) .
Preferably, the concentration of the precursor solution of the perovskite is 500 mg/ml-600 mg/ml, for example 500 mg/ml, 540 mg/ml, 550 mg/ml, 560 mg/ml, 580 mg/ml or 600 mg/ml, and the like, and preferably 580 mg/ml.
Preferably, the ratio of the volume of the precursor solution of the perovskite to the area of the flexible conductive substrate is 70 μL/ (1.5 cm × 1.5 cm) . Under the condition of such ratio， a suitable film-forming thickness and good uniformity can be obtained, and the contact with the electron transport layer or the hole transport layer is better as well.
The precursor solution of the electron transport layer is a solution of methyl [6.6] -phenyl-C61-butyrate (PCBM) and/or methyl [6.6] -phenyl-C71-butyrate (PCBM) in chlorobenzene.
Preferably, the concentration of the precursor solution of the electron transport layer is 15 mg/ml-20 mg/ml, and preferably 20 mg/ml.
Preferably, the solution of the electron transport layer is filtered prior to use in order to improve the uniformity and increase the film-forming effect.
Preferably, the ratio of the volume of the precursor solution of the electron transport layer to the area of the flexible conductive substrate is (35 μL-40 μL) / (1.5 cm × 1.5 cm) ， and under the condition of such ratio, a suitable film-forming thickness and good uniformity can be obtained, and the contact with the perovskite layer is better as well.
Preferably, the standing time is 25 min-35 min, and preferably 30 min.
Preferably, the method for preparing a back electrode on the perovskite layer is any one of evaporation, screen printing or printing.
Preferably, the method further comprises a step of cutting or cropping the flexible solar cell for test or for preparing the device.
Compared with the related technics, the present disclosure has the following beneficial effects:
(1) the present disclosure adopts a transparent polymer film flexible substrate with ITO instead of the traditional glass substrate, and all the functional layers (the hole transport layer, the perovskite layer and the electron transport layer) are coated with a blade coating method instead of a spin coating method, furthermore, the lead source is limited to lead acetate and the parameters such as the temperature of the blade coating solution during blade coating, the temperature of the flexible conductive substrate or the composite substrate (i.e. a composite substrate consisted of a flexible conductive substrate and a hole transport layer and/or an electron transport layer) , the blade coating speed and the height of blade, etc., are adjusted, such that a high-quality flexible perovskite solar cell can be prepared efficiently in the air (air humidity is 30 or lower) , thereby replacing the preparation in a glove box, making the operation easier and reducing the cost, meanwhile reducing the effect of introduction of unfavorable factors on the preparation method and properties of the products.
(2) The process for preparing the flexible perovskite solar cell according to the present disclosure is simple and has low requirements for the equipment, the advantages from using the blade coating method lie in that the costs can be saved to the greatest extent and the green production can be realized； use of flexible substrate to replace the traditional glass substrate can achieve the flexibility of the perovskite solar cell, broaden the application scope of the perovskite solar cell, and open a door for marketization of the perovskite solar cell.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 is a schematic diagram of the structure of a flexible perovskite solar cell according to Example 1.
Figure 2 is a schematic diagram of the structure of a flexible perovskite solar cell according to Example 2.
Figure 3 is a schematic diagram of the structure of a flexible perovskite solar cell according to Example 3.
Figure 4 is a schematic diagram of the structure of a flexible perovskite solar cell according to Example 4.
DETAILED DESCRIPTION
The technical solution of the present disclosure will be further described below by way of  specific embodiments in combination with accompanying drawings.
Example 1
The present example provides a method for preparing a flexible perovskite solar cell by blade coating, specifically the method comprises the steps of first coating a hole transport layer on a flexible substrate, followed by coating a perovskite layer as a photosensitive layer on the basis of the hole transport layer, then coating an electron transport layer on the perovskite layer, and finally evaporating a metal electrode.
The schematic diagram of the structure of a flexible perovskite solar cell according to the present example is shown in Figure 1.
Preparation:
(1) blade coating 35 μL of a precursor solution of a hole transport layer (a mixed solution obtained by mixing (PEDOT: PSS) , PSSA and isopropanol in a mass ratio of 1: 0.25: 3) on a flexible conductive substrate (1.5 cm × 1.5 cm) , then annealing at 110℃ for 15 min to obtain a hole transport layer on the flexible conductive substrate；
wherein during blade coating, the flexible conductive substrate was heated at 60℃, the blade coating speed was 20 mm/s， and the height of the blade was 50 μm；
(2) blade coating 70 μL of a precursor solution of perovskite (with a concentration of 580 mg/ml) on the hole transport layer, then annealing at 90℃ for 10 min to obtain a perovskite layer on the hole transport layer；
wherein during blade coating, the temperature of the hole transport layer was 130℃, the temperature of the mixed solution was 85℃, the blade coating speed was 20 mm/s, and the height of the blade was 50 μm；
(3) blade coating 40 μL of a precursor solution of an electron transport layer (asolution of PCBM in chlorobenzene with a concentration of 20 mg/ml) on the perovskite layer, which was then allowed to stand for 30 min and dried to obtain an electron transport layer on the perovskite layer；
wherein during blade coating, the temperature of the perovskite layer was 25℃, the blade coating speed was 20 mm/s， and the height of the blade was 75 μm；
(4) evaporating Ag electrode on the electron transport layer to obtain a flexible perovskite solar cell.
Example 2
The present example provides a method for preparing a flexible perovskite solar cell by blade coating, specifically the method comprises the steps of first coating an electron transport layer on a flexible substrate, followed by coating a perovskite layer as a photosensitive layer on the basis of the electron transport layer, then coating a hole transport layer on the perovskite layer, and finally  evaporating a metal electrode.
The schematic diagram of the structure of a flexible perovskite solar cell according to the present example is shown in Figure 2.
(1) blade coating 50 μL of a solution of an electron transport layer (asolution of PCBM in chlorobenzene with a concentration of 5 mg/ml) on a flexible conductive substrate (2 cm × 2 cm) , which was then allowed to stand for 50 min and dried to obtain an electron transport layer on the flexible conductive substrate, a uniform film-forming area was selected for the subsequent steps；
wherein during blade coating, the temperature of the flexible conductive substrate was 25℃-30℃, the blade coating speed was 18 mm/s， and the height of the blade was 75 μm；
(2) blade coating 50 μl of a precursor solution of perovskite on the electron transport layer， then annealing at 95℃ for 30 min to obtain a perovskite layer on the electron transport layer；
wherein during blade coating, the temperature of the electron transport layer was 132℃, the temperature of the mixed solution was 90℃, the blade coating speed was 15 mm/s, and the height of the blade was 80 μm；
(3) blade coating a solution of a hole transport layer on the perovskite layer, then annealing at 116℃ for 15 min to obtain a hole transport layer on the perovskite layer；
wherein during blade coating, the temperature of the perovskite layer was 68℃, the blade coating speed was 25mm/s, and the height of the blade was 63 μm；
(4) evaporating Ag electrode on the hole transport layer to obtain a flexible perovskite solar cell.
Example 3
The present example provides a method for preparing a flexible perovskite solar cell by blade coating, specifically the method comprises the steps of first coating a hole transport layer on a flexible substrate, followed by coating a perovskite layer as a photosensitive layer on the basis of the hole transport layer, then coating an electron transport layer on the perovskite layer, and finally printing a carbon electrode.
The schematic diagram of the structure of a flexible perovskite solar cell according to the present example is shown in Figure 3.
(1) blade coating 30 μL of a precursor solution of a hole transport layer (a mixed solution obtained by mixing (PEDOT: PSS) , PSSA and isopropanol in a mass ratio of 1: 0.5: 4) on a flexible conductive substrate (3 cm × 3 cm) , then annealing at 120℃ for 18 min to obtain a hole transport layer on the flexible conductive substrate, a uniform film-forming area was selected for the subsequent steps；
wherein during blade coating, the flexible conductive substrate was heated at 65℃, the blade  coating speed was 25 mm/s， and the height of the blade was 60 μm；
(2) blade coating 80 μL of a precursor solution of perovskite on the hole transport layer， then annealing at 95℃ for 20 min to obtain a perovskite layer on the hole transport layer；
wherein during blade coating, the temperature of the hole transport layer was 135℃, the temperature of the mixed solution was 88℃, the blade coating speed was 22 mm/s, and the height of the blade was 65 μm；
(3) blade coating 55 μL of a precursor solution of an electron transport layer (a solution of PCBM in chlorobenzene with a concentration of 15 mg/ml) on the perovskite layer, which was then allowed to stand for 45 min and dried to obtain an electron transport layer on the perovskite layer； wherein during blade coating, the temperature of the perovskite layer was 30℃, the blade coating speed was 20 mm/s， and the height of the blade was 80 μm；
(4) printing carbon electrode on the electron transport layer to obtain a flexible perovskite solar cell.
Example 4
The present example provides a method for preparing a flexible perovskite solar cell by blade coating, specifically the method comprises the steps of first coating an electron transport layer on a flexible substrate, followed by coating a perovskite layer as a photosensitive layer on the basis of the electron transport layer, then coating a hole transport layer on the perovskite layer, and finally printing a carbon electrode.
The schematic diagram of the structure of a flexible perovskite solar cell according to the present example is shown in Figure 4.
(1) blade coating 45 μL of a solution of an electron transport layer (a solution of PCBM in chlorobenzene with a concentration of 30 mg/ml) on a flexible conductive substrate (1.5 cm × 1.5 cm), which was then allowed to stand for 40 min and dried to obtain an electron transport layer on the flexible conductive substrate；
(2) blade coating 90 μl of a precursor solution of perovskite on the electron transport layer, then annealing at 90℃ for 12 min to obtain a perovskite layer on the electron transport layer；
wherein during blade coating, the temperature of the electron transport layer was 130℃, the temperature of the mixed solution was 90℃, the blade coating speed was 20 mm/s, and the height of the blade was 65 μm；
(3) blade coating a solution of a hole transport layer on the perovskite layer, then annealing at 115℃ for 20 min to obtain a hole transport layer on the perovskite layer；
wherein during blade coating, the temperature of the perovskite layer was 70℃, the blade coating speed was 20 mm/s， and the height of the blade was 60 μm；
(4) printing a carbon back electrode on the hole transport layer to obtain a flexible perovskite solar cell.
Applicant has stated that although the detailed methods of the present disclosure have been described by the above examples in the present disclosure, the present disclosure is not limited thereto, that is to say, it is not meant that the present disclosure has to be implemented depending on the above detailed methods. It will be apparent to those skilled in the art that any improvements made to the present disclosure, equivalent replacements to the raw materials of the products of the present disclosure and addition of adjuvant ingredients, and selections of the specific implementations, etc., all fall within the protection scope and the disclosure scope of the present disclosure.

Claims (10)

  1. A method for preparing a flexible perovskite solar cell by blade coating, wherein the method comprises the following step:
    preparing a hole transport layer, a perovskite layer and an electron transport layer on a flexible conductive substrate by a blade coating method.
  2. The method according to claim 1, wherein a hole transport layer, a perovskite layer and an electron transport layer are prepared successively on a flexible conductive substrate by a blade coating method；
    preferably, an electron transport layer, a perovskite layer and a hole transport layer are prepared successively on a flexible conductive substrate by a blade coating method.
  3. The method according to claim 1 or 2, wherein the method further comprises the step of preparing a back electrode on the hole transport layer or the electron transport layer；
    preferably, the back electrode is any one or a combination of both of a metal electrode and a carbon electrode.
  4. The method according to any one of claims 1-3, wherein the method comprises the following steps:
    (1) blade coating a precursor solution of a hole transport layer on a flexible conductive substrate, then annealing at 110℃-120℃ for 15 min-20 min to obtain a hole transport layer on the flexible conductive substrate；
    wherein during blade coating, the flexible conductive substrate is heated at 60℃-70℃, the blade coating speed is 20 mm/s-25 mm/s， and the height of the blade is 50 μm-60 μm；
    (2) blade coating a precursor solution of perovskite on the hole transport layer, then annealing at 90℃-95℃ for 10 min-30 min to obtain a perovskite layer on the hole transport layer；
    wherein during blade coating, the temperature of the hole transport layer is 130℃-135℃, the temperature of the mixed solution is 80℃-90℃, the blade coating speed is 15 mm/s-20 mm/s, and the height of the blade is 50 μm-80 μm；
    (3) blade coating a solution of an electron transport layer on the perovskite layer, which is then allowed to stand and dried to obtain an electron transport layer on the perovskite layer；
    wherein during blade coating, the temperature of the perovskite layer is 25℃-30℃, the blade coating speed is 18 mm/s-25 mm/s， and the height of the blade is 65 μm-80 μm；
    (4) preparing a back electrode on the electron transport layer to obtain a flexible perovskite solar cell.
  5. The method according to any one of claims 1-3, wherein the method comprises the following steps:
    (1) blade coating a solution of an electron transport layer on a flexible conductive substrate, which is then allowed to stand and dried to obtain an electron transport layer on the flexible  conductive substrate；
    wherein during blade coating, the temperature of the flexible conductive substrate is 25℃-30℃, the blade coating speed is 18 mm/s-25 mm/s, and the height of the blade is 65 μm-80 μm；
    (2) blade coating a precursor solution of a perovskite on the electron transport layer, then annealing at 90℃-95℃ for 10 min-30 min to obtain a perovskite layer on the electron transport layer；
    wherein during blade coating, the temperature of the electron transport layer is 130℃-135℃, the temperature of the mixed solution is 80℃-90℃, the blade coating speed is 15 mm/s-20 mm/s, and the height of the blade is 50 μm-80 μm；
    (3) blade coating a solution of a hole transport layer on the perovskite layer, then annealing at 110℃-120℃ for 15 min-20 min to obtain a hole transport layer on the perovskite layer；
    wherein during blade coating, the perovskite layer is heated at a temperature of 60℃-70℃, the blade coating speed is 20 mm/s-25 mm/s， and the height of the blade is 50 μm-60 μm；
    (4) preparing a back electrode on the hole transport layer to obtain a flexible perovskite solar cell.
  6. The method according to claim 4 or 5, wherein the size of the flexible conductive substrate is (2 cm -4 cm) × (2 cm -4 cm) ；
    preferably, the flexible conductive substrate is a transparent polymer film with indium tin oxide (ITO) , preferably any one of polyethylene naphthalate (PEN) /ITO, polyethylene terephthalate (PET) /ITO or polyimide (PI) /ITO；
    preferably, the solution of the hole transport layer is a mixed solution of poly (3, 4-ethylenedioxythiophene) -polystyrene sulfonic acid (PEDOT: PSS) , polystyrene sulfonic acid (PSSA) and isopropanol；
    preferably, the mass ratio of PEDOT: PSS, PSSA and isopropanol in the precursor solution of the hole transport layer is 1: (0.25-0.5) : (3-5) ；
    preferably, the solution of the hole transport layer is filtered prior to use；
    preferably, the ratio of the volume of the solution of the hole transport layer to the area of the flexible conductive substrate is 35 μL/ (1.5 cm × 1.5 cm) .
  7. The method according to claim 4 or 5, wherein the precursor solution of the perovskite is prepared by a method of mixing lead acetate and methylamine iodide in a molar ratio of 1: 1, then dissolving the resulting mixture in N, N-dimethylformamide (DMF) ；
    preferably, the concentration of the precursor solution of the perovskite is 500 mg/ml-600 mg/ml, and preferably 580 mg/ml；
    preferably, the ratio of the precursor solution of the perovskite to the area of the flexible conductive substrate is 70 μL/ (1.5 cm × 1.5 cm) .
  8. The method according to claim 4 or 5, wherein the precursor solution of the electron transport layer is a solution of methyl [6.6] -phenyl-C61-butyrate (PCBM) and/or methyl [6.6] -phenyl-C71-butyrate (PCBM) in chlorobenzene；
    preferably, the concentration of the precursor solution of the electron transport layer is 15 mg/ml-20 mg/ml, and preferably 20 mg/ml；
    preferably, the solution of the electron transport layer is filtered prior to use；
    preferably, the ratio of the volume of the precursor solution of the electron transport layer to the area of the flexible conductive substrate is (35 μL-40 μL) / (1.5 cm × 1.5 cm) .
  9. The method according to claim 4 or 5, wherein the standing time is 25 min-50 min, preferably 30 min；
    preferably, the method for preparing a back electrode on the perovskite layer is any one of evaporation, screen printing or printing.
  10. The method according to any one of claims 1-9, wherein the method further comprises a step of cutting or cropping the flexible perovskite solar cell.
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