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WO2022035239A1 - Procédé de préparation d'un dispositif optoélectronique à base de pérovskite et dispositif optoélectronique à base de pérovskite préparé par ledit procédé - Google Patents

Procédé de préparation d'un dispositif optoélectronique à base de pérovskite et dispositif optoélectronique à base de pérovskite préparé par ledit procédé Download PDF

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WO2022035239A1
WO2022035239A1 PCT/KR2021/010692 KR2021010692W WO2022035239A1 WO 2022035239 A1 WO2022035239 A1 WO 2022035239A1 KR 2021010692 W KR2021010692 W KR 2021010692W WO 2022035239 A1 WO2022035239 A1 WO 2022035239A1
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perovskite
perovskite compound
transport layer
photoactive layer
compound
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Korean (ko)
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임상혁
허진혁
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Korea University Research and Business Foundation
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    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to a method of manufacturing a perovskite optoelectronic device and a perovskite optoelectronic device manufactured through the method, and more particularly, by using spray coating to form a photoactive layer to have a compositional gradient in the depth direction,
  • the present invention relates to a method for manufacturing a perovskite optoelectronic device capable of improving absorption wavelength range and carrier lifetime, and to a perovskite optoelectronic device manufactured through the same.
  • the solar cell refers to a cell that generates current-voltage using the photovoltaic effect of absorbing light energy from sunlight to generate electrons and holes.
  • Dye-sensitized solar cell was first successfully developed in 1991 by Professor Michael Gratzel of Lausanne Institute of Technology (EPFL) in Switzerland and introduced in Nature (Vol. 353, p. 737). became The initial structure of the dye-sensitized solar cell was a simple structure in which a light-absorbing dye was adsorbed to a porous photoanode on a transparent electrode film that conducts light and electricity, another conductive glass substrate was placed on top, and a liquid electrolyte was filled. is made of
  • liquid-type dye-sensitized solar cells The highest efficiency reported so far for liquid-type dye-sensitized solar cells has remained at 11-12% for about 20 years. Although the liquid-type dye-sensitized solar cell has relatively high efficiency, it has potential for commercialization, but there are also problems with stability over time due to volatile liquid electrolytes and cost reduction due to the use of expensive ruthenium (Ru)-based dyes.
  • ruthenium (Ru)-based dyes expensive
  • organic photovoltaic (OPV) cells which have been studied in earnest since the mid-1990s, are organic materials with electron donor (D, or sometimes called hole acceptor) characteristics and electron acceptor (A) characteristics. is composed of When a solar cell made of organic molecules absorbs light, electrons and holes are formed, which is called exciton. Excitons move to the D-A interface to separate charges, and electrons move to electron acceptors and holes move to electron donors to generate photocurrent.
  • D electron donor
  • A electron acceptor
  • the organic solar cell has a simpler manufacturing process compared to the conventional solar cell due to the easy processability, diversity, and low cost of organic materials.
  • the organic solar cell has a big problem in that the structure of the BHJ is deteriorated by moisture or oxygen in the air, so that the efficiency is rapidly reduced, that is, the stability of the solar cell.
  • stability can be increased by introducing a complete sealing technology, but there is a problem that the price increases.
  • Organic-inorganic hybrid perovskite is a next-generation light-absorbing material with excellent optical and electrical properties, low price, and easy use in the process.
  • recent organic-inorganic hybrid perovskite semiconductors have a basic chemical composition of ABX 3 , so they can be easily synthesized with various types of materials, and solar cells can be manufactured at low material costs, making them the ultimate next-generation solar cell material. It's getting a lot of attention.
  • perovskite solar cells can be solution-processed like organic solar cells, they can be used in a wide variety of large-area and flexible devices. .
  • the method of manufacturing a perovskite film includes a method of forming a uniform perovskite film by slowing the crystallization rate by controlling the solubility of the perovskite solution, and forcing the perovskite film through nonsolvent dripping.
  • There is a method of crystallization a method of forming a perovskite film by first coating PbI 2 , etc., and then dripping MAI solution or the like thereto (two step process).
  • the rough surface of the perovskite film has a problem that recombination occurs due to poor contact between the perovskite film and the charge transport layer.
  • a photoactive layer containing a perovskite compound is formed to have a composition gradient in the depth direction from the hole transport layer to the electron transport layer by a spray coating method to absorb sunlight (1-sun light soaking)
  • An object of the present invention is to provide a perovskite photoelectric device capable of improving long-term operation stability so as to have less than 10% degradation even when continuously operated for 1000 hours under the present invention, and a method for manufacturing the same.
  • the photoactive layer containing the perovskite compound is formed to have a composition gradient in the depth direction from the hole transport layer to the electron transport layer, and the absorption wavelength is expanded to 750 nm to increase the light collecting property (
  • An object of the present invention is to provide a perovskite optoelectronic device capable of improving light harvesting and a method for manufacturing the same.
  • the perovskite film can be manufactured in a large area regardless of the size of the substrate through a relatively simple process by forming a photoactive layer containing a perovskite compound by a spray coating method.
  • An object of the present invention is to provide an optoelectronic device and a method for manufacturing the same.
  • a method of manufacturing a perovskite optoelectronic device comprises: forming an electron transport layer on a first electrode; forming a photoactive layer comprising a perovskite compound on the electron transport layer by spray coating (orthogonal spray coating); forming a hole transport layer on the photoactive layer containing the perovskite compound; and forming a second electrode on the hole transport layer, wherein the photoactive layer including the perovskite compound has a composition gradient in the depth direction from the hole transport layer to the electron transport layer.
  • a band structure gradient may be continuously formed in a depth direction from the hole transport layer to the electron transport layer.
  • At least one electric field may be formed therein in the photoactive layer including the perovskite compound.
  • the perovskite compound may be represented by the following formula (1).
  • M is a divalent or trivalent metal cation
  • X is a monovalent anion
  • M is a divalent metal cation
  • a+2b c
  • M is a trivalent metal
  • a+3b c
  • a, b, and c are natural numbers.
  • the perovskite compound may be represented by the following formula (2).
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions
  • m is 0 ⁇ m ⁇ 1.
  • the perovskite compound may include at least two or more monovalent anions, and the composition ratio of the at least two or more monovalent anions may change in the depth direction.
  • Forming a photoactive layer comprising a perovskite compound by spray coating on the electron transport layer may include: coating a first perovskite compound on the electron transport layer; and coating a second perovskite compound on the coated first perovskite compound.
  • the concentration of the first perovskite compound is higher than the concentration of the second perovskite compound, and the perovskite in contact with the hole transport layer
  • the concentration of the second perovskite compound may be higher than that of the first perovskite compound.
  • the coating time of the second perovskite compound may be 0.5 seconds to 200 seconds.
  • It may include adjusting the average diameter of the perovskite compound according to the coating time of the second perovskite compound.
  • the first perovskite compound may be represented by the following Chemical Formula 3
  • the second perovskite compound may be represented by the following Chemical Formula 4.
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions.
  • Perovskite is a first electrode; an electron transport layer formed on the first electrode; a photoactive layer formed by orthogonal spray coating on the electron transport layer and including a perovskite compound; a hole transport layer formed on the photoactive layer including the perovskite compound; and a second electrode formed on the hole transport layer, wherein the photoactive layer including the perovskite compound has a composition gradient in a depth direction from the hole transport layer to the electron transport layer.
  • a band structure gradient may be continuously formed in a depth direction from the hole transport layer to the electron transport layer.
  • At least one electric field may be formed therein in the photoactive layer including the perovskite compound.
  • the perovskite compound may be represented by the following formula (1).
  • M is a divalent or trivalent metal cation
  • X is a monovalent anion
  • M is a divalent metal cation
  • a+2b c
  • M is a trivalent metal
  • a+3b c
  • a, b, and c are natural numbers.
  • the photoactive layer may be a perovskite compound represented by the following Chemical Formula 2.
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions
  • m is 0 ⁇ m ⁇ 1.
  • the perovskite compound may include at least two or more monovalent anions, and the composition ratio of the at least two or more monovalent anions may change in the depth direction.
  • the photoactive layer comprising the perovskite compound comprises a first perovskite compound and a second perovskite compound, and the photoactive layer comprising the perovskite compound in contact with the electron transport layer is a first
  • the concentration of the first perovskite compound is higher than the concentration of the second perovskite compound, and the photoactive layer including the perovskite compound in contact with the hole transport layer has a second perovskite compound concentration. It can be higher than 1 perovskite compound.
  • the photoactive layer containing the perovskite compound is formed to have a composition gradient in the depth direction from the hole transport layer to the electron transport layer by a spray coating method to absorb sunlight (1-sun light). Soaking), it is possible to improve long-term operation stability so as to have less than 10% degradation even when continuously operated for 1000 hours.
  • the photoactive layer containing the perovskite compound is formed to have a composition gradient in the depth direction from the hole transport layer to the electron transport layer to expand the absorption wavelength to 750 nm. Light harvesting can be improved.
  • the photoactive layer containing the perovskite compound is formed by a spray coating method, and the perovskite film can be manufactured in a large area regardless of the size of the substrate through a relatively simple process.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a perovskite optoelectronic device according to an embodiment of the present invention.
  • FIG. 2 is a cross-sectional view illustrating a perovskite optoelectronic device according to an embodiment of the present invention.
  • FIG. 3 is an image illustrating a band diagram of a perovskite optoelectronic device according to an embodiment of the present invention.
  • FIG. 4 is a cross-sectional scanning electron microscopy (SEM) image of a photoactive layer prepared by spray coating for 5 seconds
  • FIG. 5 is a surface scanning electron microscope image.
  • FIG. 6 is a cross-sectional scanning electron microscope image of a photoactive layer prepared by spray coating for 10 seconds
  • FIG. 7 is a surface scanning electron microscope image.
  • FIG. 8 is a cross-sectional scanning electron microscope image of a photoactive layer prepared by spray coating for 15 seconds
  • FIG. 9 is a surface scanning electron microscope image.
  • FIG. 10 is a cross-sectional scanning electron microscope image of the photoactive layer prepared by spray coating for 20 seconds
  • FIG. 11 is a surface scanning electron microscope image.
  • GIXRD 12 shows a grazing incidence X-ray diffraction (GIXRD) graph of the penetration depth of the photoactive layer according to the spray coating time.
  • GIXRD grazing incidence X-ray diffraction
  • FIG. 13 is a grazing incidence X-ray diffraction graph of the photoactive layer prepared by spray coating for 5 seconds
  • FIG. 14 is a graph showing spray coating for 10 seconds
  • FIG. 15 is spray coating for 15 seconds. It is a graph in progress
  • FIG. 16 is a graph in which spray coating was performed for 20 seconds.
  • 17 is a graph showing the depth profile of the (200) peak position of the photoactive layer according to the spray coating time.
  • 19 is a graph showing compositional depth profiles of the photoactive layer according to spray coating time.
  • CBM conduction band minimum
  • VBM valence band maximum
  • FIG. 22 is a scanning electron microscope image of a perovskite photoelectric device according to an embodiment of the present invention including a photoactive layer prepared by spray coating for 15 seconds.
  • FIG. 23 is a graph showing an absorption spectrum of a perovskite photoelectric device according to an embodiment of the present invention
  • FIG. 24 is a graph showing an external quantum efficiency spectrum (EQE spectra)
  • FIG. 25 is an open It is a graph showing the voltage (Voc)
  • Fig. 26 is a graph showing the short-circuit current (Jsc)
  • Fig. 27 is a graph showing the charging factor (FF)
  • Fig. 28 is a graph showing the energy conversion efficiency (PCE) It is a graph.
  • FIG. 29 is a graph showing current density-voltage curves (JV curves) of a perovskite photoelectric device according to an embodiment of the present invention including a photoactive layer prepared by spray coating for 5 seconds
  • FIG. 30 is It is a graph of spray coating for 10 seconds
  • FIG. 31 is a graph of spray coating for 15 seconds
  • FIG. 32 is a graph showing spray coating for 20 seconds.
  • FIG. 33 is an image showing a sub-module of a perovskite optoelectronic device according to an embodiment of the present invention
  • FIG. 34 is a graph showing a photocurrent-voltage (IV) curve of the sub-module
  • FIG. 35 is an initial stage ( It is a graph showing the stabilized power output (Stabilized power output) of the sub-module in early stage)
  • FIG. 36 is 1-sun illumination at room temperature and nitrogen (N2) atmosphere of the sub-module that is not encapsulated. It is a graph showing the results of a long-term light-soaking stability test under
  • the term 'or' means 'inclusive or' rather than 'exclusive or'. That is, unless stated otherwise or clear from context, the expression 'x employs a or b' means any of natural inclusive permutations.
  • FIG. 1 is a flowchart illustrating a method of manufacturing a perovskite optoelectronic device according to an embodiment of the present invention.
  • the method of manufacturing a perovskite optoelectronic device comprises the steps of forming an electron transport layer on the first electrode (S110), spray coating on the electron transport layer (orthogonal spray coating) on the perovskite compound. Forming a photoactive layer comprising (S120), forming a hole transport layer on the photoactive layer comprising a perovskite compound (S130), and forming a second electrode on the hole transport layer (S140) do.
  • the method of manufacturing a perovskite optoelectronic device proceeds with the step of forming an electron transport layer on the first electrode (S110).
  • an inorganic substrate or an organic substrate may be used.
  • the inorganic substrate may include at least one of glass, quartz, Al 2 O 3 , SiC, Si, GaAs, and InP.
  • the organic substrate is Kepton foil, polyimide (PI), polyethersulfone (PES), polyacrylate (PAR), polyetherimide (PEI), polyethylene naphthalate (PEN) ), polyethylene terephthalate (PET), polyphenylene sulfide (PPS), polyarylate, polycarbonate (PC), cellulose triacetate (CTA) and cellulose acetate It may include any one of propionate (cellulose acetate propionate, CAP).
  • the inorganic substrate and the organic substrate are made of a transparent material through which light is transmitted, and in general, the substrate can be used as long as it can be positioned on the front electrode.
  • the flexibility of the electrode can be increased.
  • the first electrode is located on the substrate and a conductive electrode, in particular a transparent conductive electrode, is preferred to enhance the transmission of light.
  • the first electrode may be used as long as it is an electrode material commonly used in the field of solar cells.
  • the first electrode contains, for example, fluorine doped tin oxide (FTO), indium doped tin oxide (ITO), aluminum-doped zinc oxide (AZO) and indium. At least one of indium doped zinc oxide (IZO) may be included.
  • FTO fluorine doped tin oxide
  • ITO indium doped tin oxide
  • AZO aluminum-doped zinc oxide
  • IZO indium doped zinc oxide
  • the electron transport layer may be positioned between the first electrode and the photoactive layer.
  • the electron transport layer may allow electrons generated in the photoactive layer to be easily transferred to the first electrode.
  • the electron transport layer may include at least one of fullerene (C60), a fullerene derivative, perylene, polybenzimidazole (PBI), and PTCBI (3,4,9,10-perylene-tetracarboxylic bis-benzimidazole), , the fullerene derivative may include at least one of PCBM ((6,6)-phenyl-C61-butyric acid-methylester) and PCBCR ((6,6)-phenyl-C61-butyric acid cholesteryl ester), but in this It is not limited.
  • PCBM ((6,6)-phenyl-C61-butyric acid-methylester)
  • PCBCR ((6,6)-phenyl-C61-butyric acid cholesteryl ester)
  • a TiO 2 based or Al 2 O 3 based porous material may be used as the electron transport layer in the inverted structure, but is not limited thereto.
  • the method of manufacturing a perovskite photoelectric device proceeds with the step (S120) of forming a photoactive layer containing a perovskite compound by spray coating on the electron transport layer.
  • the photoactive layer may serve as a photoelectric conversion layer that generates current by separating electrons (e) and holes (h).
  • the photoactive layer including the perovskite compound has a composition gradient in the depth direction from the hole transport layer to the electron transport layer by spray coating.
  • the photoactive layer having a composition gradient in the depth direction may be formed by performing orthogonal processable spray coating.
  • the method of manufacturing a perovskite optoelectronic device uses orthogonal spray coating that can coat the perovskite multilayer thin film in a vertical direction, a solution is used, but the spray-coated When the micro-drops fall, the solvent is evaporated instantaneously to form a multi-layer thin film in a vertical direction like vacuum deposition, and a small amount of solvent remains between the first perovskite thin film formed in the lower layer and the newly formed thin film. Inter mixing may take place to produce a perovskite film having a continuous composition change.
  • various spray coaters such as an air brush, ultrasonic spray, mega sonic spray, or electrospray may be used.
  • the method of manufacturing a perovskite optoelectronic device according to an embodiment of the present invention is not limited to a spray coater, but when ultrasonic spray coating is used, a micro drop of the sprayed perovskite solution is used. ) is small, so it is easy to precisely control in terms of process.
  • Spray coating can be performed while moving the spray nozzle at a speed of 0.001 m/min to 20 m/min. If the spray nozzle is moved at a speed of less than 0.001 m/min, the process speed is too slow, and 20 m/min. If it exceeds , the moving speed is excessively fast, so it is difficult to obtain a uniform inclined wall without pinholes.
  • the discharge amount discharged to the spray nozzle may be 0.001 ml/min to 1000 ml/min, and when the discharge amount is less than 0.001 ml/min, the amount of the solution containing the perovskite compound sprayed from the spray nozzle is small, so that the solvent is There is a disadvantage that the process time is prolonged because all of them are blown away or the amount applied is small, and when it exceeds 1000 ml/min, an excess solution is applied and it is difficult to obtain a uniform film because it is difficult to dry.
  • a photoactive layer containing a perovskite compound is formed by a spray coating method, and the perovskite film is formed through a relatively simple process regardless of the size of the substrate. It can be manufactured in a large area.
  • the method of manufacturing a perovskite photoelectric device proceeds with the step (S120) of forming a photoactive layer containing the perovskite compound by spray coating on the electron transport layer, the perovskite compound
  • the photoactive layer containing may have a composition gradient in the depth direction from the hole transport layer to the electron transport layer.
  • the perovskite compound may include a metal halide.
  • the perovskite compound of the photoactive layer having a composition gradient in the depth direction from the hole transport layer to the electron transport layer may be represented by the following formula (1).
  • M is a divalent or trivalent metal cation
  • X is a monovalent anion
  • M is a divalent metal cation
  • a+2b c
  • M is a trivalent metal
  • a+3b c
  • a, b, and c are natural numbers.
  • A is C 1-24 straight or branched chain alkyl, amine group (-NH 3 ), hydroxyl group (-OH), cyano group (-CN), halogen group, nitro group (-NO), methoxy group (-OCH 3 ) Or imidazolium group substituted C 1-24 straight or branched chain alkyl, Li + , Na + , K + , Rb + , Cs + , Fr + , Cu(I) + , Ag(I) + and Au(I) ) may include at least one of + .
  • M' is Pb 2+ , Sn 2+ , Ge 2+ , Cu 2+ , Co 2+ , Ni 2+ , Ti 2+ , Zr 2+ , Hf 2+ , Rf 2+ , In 3+ , Bi 3+ , Co 3+ , Sb 3+ , Ni 3+ , Al 3+ , Ga 3+ , Tl 3+ , Sc 3+ , Y 3+ , La 3+ , Ce 3+ , Fe 3+ , Ru 3+ , Cr 3+ , V 3+ , and Ti 3+ may be included.
  • X may include at least one of F - , Cl - , Br - , I - , SCN - , PF 6 - , and BF 4 - .
  • the perovskite compound of Chemical Formula 1 of the photoactive layer having a composition gradient in the depth direction from the hole transport layer to the electron transport layer may be represented by Chemical Formula 2 below.
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions
  • m is 0 ⁇ m ⁇ 1.
  • the step of forming a photoactive layer containing a perovskite compound by spray coating on the electron transport layer (S120) is on the electron transport layer It may include the step of coating the first perovskite compound on (S121) and coating the second perovskite compound on the coated first perovskite compound (S122).
  • the step of coating the first perovskite compound on the electron transport layer (S121) may proceed.
  • the method of manufacturing a perovskite photoelectric device is prepared by spray-coating a first perovskite compound precursor solution containing a first perovskite compound and a solvent on an electron transport layer. 1
  • a perovskite compound film can be formed.
  • the coating time of the first perovskite compound is less than 0.1 seconds, the amount of the first perovskite compound to be coated is too small, so the efficiency of the device is low, and if it exceeds 600 seconds, the first perovskite compound to be coated There are disadvantages in that the efficiency of the device is lowered or the process time is too long because the amount of the compound is too large.
  • Spray coating of the first perovskite compound can be performed while moving the spray nozzle at a speed of 0.001 m/min to 20 m/min, and the process speed is too high when the spray nozzle is moved at a speed of less than 0.001 m/min.
  • the moving speed is excessively fast, so it is difficult to obtain a uniform inclined wall without a pin hole.
  • the discharge amount discharged to the spray nozzle may be 0.001ml/min to 1000ml/min, and when the discharge amount is less than 0.001ml/min, the first perovskite compound sprayed from the spray nozzle
  • the amount of the solution contained is small, so that all the solvent is blown away before it reaches the substrate or the amount of application is small, so the process time is long.
  • the disadvantage is that it is difficult to obtain.
  • the first perovskite compound may be represented by Formula 3 below.
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions.
  • the first perovskite compound may be CsPbI 2 Br.
  • the step of coating the second perovskite compound on the coated first perovskite compound (S122) may be performed.
  • a second perovskite compound precursor solution containing a second perovskite compound and a solvent is mixed with a first perovskite compound film. It is possible to form a photoactive layer having a composition gradient in the depth direction from the hole transport layer to the electron transport layer by spray coating on it.
  • the spray coating of the second perovskite compound can be performed while moving the spray nozzle at a speed of 0.001 m/min to 20 m/min, and if the spray nozzle is moved at a speed of less than 0.001 m/min, the process speed is too high There is a disadvantage that it is slow, and when it exceeds 20 m/min, the moving speed is excessively fast, so it is difficult to obtain a uniform inclined wall without a pin hole.
  • the discharge amount discharged to the spray nozzle may be 0.001ml/min to 1000ml/min, and when the discharge amount is less than 0.001ml/min, the second perovskite compound sprayed from the spray nozzle
  • the amount of the solution contained is small, so that all the solvent is blown away before it reaches the substrate or the amount of application is small, so the process time is long.
  • the disadvantage is that it is difficult to obtain.
  • the second perovskite compound may be represented by Formula 4 below.
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions.
  • the second perovskite compound may be CsPbI 3 .
  • the second perovskite compound-derived monovalent anion eg, the second halide ion
  • the composition of at least two or more monovalent anions of the perovskite compound eg, a first halide ion and a second halide ion
  • the perovskite compound of Chemical Formula 1 of the photoactive layer having a compositional gradient in the depth direction from the hole transport layer to the electron transport layer is represented by the following Chemical Formula 2
  • the first perovskite compound is represented by Chemical Formula 3
  • the second compound When the rovskite compound is represented by Chemical Formula 4, in the method for manufacturing a perovskite photoelectric device according to an embodiment of the present invention, as the coating time of the second perovskite compound increases, X' and The composition of X" can be varied.
  • the perovskite compound contains at least two or more monovalent anions, and the composition ratio of at least two or more monovalent anions in the depth direction is changed, so that the band gap and Fermi level of the photoactive layer are continuously changed. can be formed.
  • the composition ratio of X′′/M′ may be changed in the depth direction.
  • the band gap and the Fermi level of the photoactive layer are changed continuously A band structure gradient may be formed.
  • the concentration of the first perovskite compound is higher than the concentration of the second perovskite compound, and the perovskite compound in contact with the hole transport layer
  • concentration of the second perovskite compound in the photoactive layer comprising a may be higher than that of the first perovskite compound.
  • a first perovskite compound is coated on an electron transport layer, and then a second perovskite compound is coated to form a photoactive layer
  • the perovskite compound in contact with the hole transport layer which is the upper surface portion of the photoactive layer on which the second perovskite compound is coated, has a concentration of the second perovskite compound in the first It may be higher than the concentration of the perovskite compound.
  • the photoactive layer including the perovskite compound in contact with the electron transport layer may include only the first perovskite compound, or the photoactive layer comprising the perovskite compound in contact with the hole transport layer 2 It may also contain only perovskite compounds.
  • the photoactive layer containing the perovskite compound absorbs light to generate electron-hole pairs, and the generated electrons move to the first electrode through the electron transport layer, and at the same time, the holes move to the second electrode through the hole transport layer . At this time, when the two electrodes are connected, electricity may continuously flow while electrons move to the counter electrode through an external circuit.
  • the perovskite optoelectronic device manufactured by the method for manufacturing a perovskite optoelectronic device according to an embodiment of the present invention is a photoactive layer comprising a perovskite compound in contact with the electron transport layer and the perovskite in contact with the hole transport layer Electron-hole pairs can be created in the photoactive layer containing the skyte compound, leading to the electrons and holes moving in opposite directions across the photoactive layer to the electron transport layer and hole transport layer, improving charge collection ability can be
  • the photoactive layer including the perovskite compound has a composition gradient in the depth direction, at least one electric field may be formed therein.
  • an electric field is formed at the interface where the electron transport layer and the photoactive contact and the photoactive layer and the hole transport layer contact each other.
  • Fermi level matching occurs at the interface between the first perovskite compound and the second perovskite compound, and through this, an additional electric field is generated inside the photoactive layer. Electron-hole pairs generated inside the photoactive layer are separated and moved much more effectively, so that the efficiency of the photoelectric device can be increased.
  • the coating time of the second perovskite compound may be 0.5 seconds to 200 seconds, and if the coating time of the second perovskite compound solution is less than 5 seconds, the coating amount of the second perovskite compound is too small, the composition It is difficult to manufacture the photoactive layer having an inclination, and when it exceeds 200 seconds, the surface roughness becomes too large, and it is difficult to form a uniform hole transport layer, so that device efficiency is lowered.
  • the average diameter of the perovskite compound may be adjusted according to the coating time of the second perovskite compound.
  • the average diameter of the perovskite compound particles can be continuously increased during the spray coating process, with dissolution and regrowth.
  • the second perovskite compound since the second perovskite compound has lower solubility in a solvent than the first perovskite compound, the second perovskite compound When spray-coated on the first perovskite compound, the second perovskite compound is rapidly nucleated to a higher nuclei density than the first perovskite compound, so that the average perovskite compound particles The diameter may be reduced.
  • the trap or exciton binding energy can be adjusted.
  • the method of manufacturing a perovskite optoelectronic device proceeds to the step of forming a hole transport layer on the photoactive layer containing the perovskite compound (S130).
  • the hole transport layer may be positioned between the photoactive layer and the second electrode.
  • the hole transport layer may allow holes generated in the photoactive layer to be easily transferred to the second electrode.
  • the hole transport layer is P3HT (poly[3-hexylthiophene]), MDMO-PPV (poly[2-methoxy-5-(3',7'-dimethyloctyloxyl)]-1,4-phenylene vinylene), MEH-PPV (poly[ 2-methoxy-5-(2''-ethylhexyloxy)-p-phenylene vinylene]), P3OT (poly(3-octyl thiophene)), POT( poly(octyl thiophene)), P3DT (poly(3-decyl thiophene) ), P3DDT (poly(3-dodecyl thiophene), PPV (poly(p-phenylene vinylene)), TFB (poly(9,9'-dioctylfluorene-co-N-(4-butylphenyl)diphenyl amine), Polyani
  • the method of manufacturing a perovskite optoelectronic device includes forming a second electrode on the hole transport layer ( S140 ).
  • the second electrode may be an electrode commonly used in the field of solar cells. More specifically, the second electrode is gold (Au), silver (Ag), platinum (Pt), palladium (Pd), copper (Cu), aluminum (Al), carbon (C), cobalt sulfide (CoS), sulfide At least one of copper (CuS) and nickel oxide (NiO) may be included. Since the second electrode may also be formed by the method described for the first electrode, a redundant description thereof will be omitted.
  • the photoactive layer containing the perovskite compound is a composition gradient in the depth direction from the hole transport layer to the electron transport layer by a spray coating method. Long-term operation stability can be improved so that it has less than 10% degradation even when continuously operated for 1000 hours under 1-sun light soaking.
  • the photoactive layer containing the perovskite compound is formed to have a composition gradient in the depth direction from the hole transport layer to the electron transport layer to form an absorption wavelength ( The absorption wavelength can be extended to 750 nm to improve light harvesting.
  • a perovskite optoelectronic device is a perovskite photoelectric device according to an embodiment of the present invention manufactured through a method for manufacturing a perovskite photoelectric device according to an embodiment of the present invention A photoelectric device will be described.
  • FIG. 2 is a cross-sectional view illustrating a perovskite optoelectronic device according to an embodiment of the present invention.
  • the perovskite optoelectronic device according to the embodiment of the present invention is manufactured through the manufacturing method of the perovskite optoelectronic device according to the embodiment of the present invention, and detailed descriptions of the same components will be omitted.
  • the perovskite photoelectric device is spray coated on the first electrode 110 , the electron transport layer 120 formed on the first electrode 110 , and the electron transport layer 120 . ), and formed on the photoactive layer 130 containing the perovskite compound, the hole transport layer 140 and the hole transport layer 140 formed on the photoactive layer 130 containing the perovskite compound and a second electrode 150 to be
  • a perovskite photoelectric device has a perovskite structure in which an anode electrode is disposed on a substrate or a plannar-heterojunction structure in which a cathode electrode is disposed on a substrate. It can be implemented as a photovoltaic cell.
  • the perovskite optoelectronic device includes a first electrode 110, the first electrode 110 is located on a substrate, and a conductive electrode, in particular, a transparent conductive electrode to improve light transmission. desirable.
  • the first electrode 110 is, for example, fluorine-doped tin oxide (FTO), indium-doped tin oxide (ITO), aluminum-containing zinc oxide (Al-doped Zinc Oxide, AZO) And it may include at least one of indium-doped zinc oxide (IZO).
  • FTO fluorine-doped tin oxide
  • ITO indium-doped tin oxide
  • Al-doped Zinc Oxide, AZO aluminum-containing zinc oxide
  • IZO indium-doped zinc oxide
  • the perovskite photoelectric device includes an electron transport layer 120 formed on a first electrode 110 , and the electron transport layer 120 includes the first electrode 110 and the photoactive layer 130 . ) can be located between The electron transport layer 120 may allow electrons generated in the photoactive layer to be easily transferred to the first electrode 110 .
  • the electron transport layer 120 may be formed of a TiO 2 based material, but is not limited thereto.
  • the perovskite photoelectric device is formed by spray coating (orthogonal spray coating) on the electron transport layer 120, and includes a photoactive layer 130 including a perovskite compound.
  • the highest occupied molecular orbital (HOMO) level of the hole transport layer 140 and the lowest unoccupied molecular orbital (LUMO) level of the electron transport layer 120 are perovskite, respectively. It matches well with a valence band and a conduction band of the electron, so that electrons can be transferred to the electron transport layer 120 and holes can be transferred to the hole transport layer 140 .
  • electron-hole pairs can be effectively separated into electrons and holes, and the separated electrons and holes are accumulated with an internal electric field formed by a difference in work function between the first electrode 110 and the second electrode 150 . It is collected by moving to each electrode by the difference in the concentration of charges and finally flows in the form of current through an external circuit.
  • the photoactive layer 130 including the perovskite compound may have a composition gradient in the depth direction from the hole transport layer 140 to the electron transport layer 120, and the photoactive layer having a composition gradient in the depth direction ( 130) of the perovskite compound may be represented by the following formula (2).
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions
  • m is 0 ⁇ m ⁇ 1.
  • A is C 1-24 straight or branched chain alkyl, amine group (-NH 3 ), hydroxyl group (-OH), cyano group (-CN), halogen group, nitro group (-NO), methoxy group (-OCH 3 ) Or imidazolium group substituted C 1-24 straight or branched chain alkyl, Li + , Na + , K + , Rb + , Cs + , Fr + , Cu(I) + , Ag(I) + and Au(I) ) may include at least one of + .
  • M may include at least one of Pb 2+ , Sn 2+ , Ge 2+ , Cu 2+ , Co 2+ , Ni 2+ , Ti 2+ , Zr 2+ , Hf 2+ and Rf 2+ . .
  • X' and X" may include at least one of F - , Cl - , Br - , I - , SCN - and BF 4 - .
  • the perovskite photoelectric device includes a photoactive layer 130 formed by coating a first perovskite compound and then coating a second perovskite compound, the perovskite In the compound, the composition ratio of X′′/M′ may be changed in the depth direction from the hole transport layer 140 to the electron transport layer 120 .
  • the concentration of the first perovskite compound is higher than the concentration of the second perovskite compound, and the hole transport layer 140 ) and the photoactive layer 132 including the perovskite compound in contact with the concentration of the second perovskite compound may be higher than that of the first perovskite compound.
  • the photoactive layer 131 including the perovskite compound in contact with the electron transport layer 120 may include only the first perovskite compound, or the perovskite in contact with the hole transport layer 140 .
  • the photoactive layer 132 including the skyte compound may include only the second perovskite compound,
  • electron-hole pairs can be generated in the photoactive layer including the perovskite compound in contact with the electron transport layer and the photoactive layer including the perovskite compound in contact with the hole transport layer, so that electrons and holes are separated from the photoactive layer
  • the charge collection ability can be improved by guiding electrons and holes to move in opposite directions across to the electron transport layer and the hole transport layer.
  • the photoactive layer 130 has a composition gradient in the depth direction, a band gap gradient is generated according to the composition gradient, so that the electrons and holes generated in the photoactive layer 130 reduce the loss of open-circuit voltage. Separation and migration can occur much more effectively while being visible.
  • At least one electric field may be formed therein in the photoactive layer 130 including the perovskite compound.
  • the first perovskite compound may be represented by Formula 3 below.
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions.
  • the first perovskite compound may be CsPbI 2 Br.
  • the second perovskite compound may be represented by the following formula (4).
  • A is a monovalent cation
  • M' is a divalent metal cation
  • X' and X" are monovalent anions.
  • the second perovskite compound may be CsPbI 3 .
  • the hole transport layer 140 may be PTAA (poly(triarylamine)), but is not limited thereto.
  • Gold may be used as the second electrode 150 , but is not limited thereto.
  • the perovskite photoelectric device is formed so that the photoactive layer containing the perovskite compound has a composition gradient in the depth direction from the hole transport layer to the electron transport layer by a spray coating method.
  • Long-term operation stability can be improved to have less than 10% degradation even when continuously operated for 1000 hours under 1-sun light soaking.
  • the perovskite photoelectric device is formed so that the photoactive layer including the perovskite compound has a composition gradient in the depth direction from the hole transport layer to the electron transport layer, so that the absorption wavelength is can be extended to 750 nm to improve light harvesting.
  • FIG. 3 is an image illustrating a band diagram of a perovskite optoelectronic device according to an embodiment of the present invention.
  • the perovskite photoelectric device includes a photoactive layer 130 having a composition gradient in the depth direction to the electron transport layer 120, and when illuminated by sunlight, the electron transport layer 120 is in contact with it. Electron-hole pairs may be generated in the photoactive layer 131 including the rovskite compound and the photoactive layer 132 including the perovskite compound in contact with the hole transport layer 140 .
  • electrons and holes cross the photoactive layer 130 to the electron transport layer 120 and the hole transport layer 140 to guide the electrons and holes to move in opposite directions, thereby making it easier to collect charges. there is.
  • the photoactive layer including the perovskite compound has a composition gradient in the depth direction from the hole transport layer to the electron transport layer, so that the composition ratio of at least two monovalent anions of the perovskite compound is It can be seen that the band structure gradient in which the band gap and the Fermi level of the photoactive layer are continuously changed is formed by continuously changing.
  • the organic substrates doped with patterned fluorine-doped tin oxide (FTO) were extensively cleaned using deionized water, acetone and isopropanol, followed by an airbrush (DH-125, Spamax).
  • FTO fluorine-doped tin oxide
  • DH-125, Spamax deionized water, acetone and isopropanol
  • a compact 50 nm TiO 2 (c-TiO 2 ) solution using spray-pyrolysis deposition with a 20 mM solution of titanium diisopropoxide bis(acetylacetate) (TAA) at 450°C ) layer was formed.
  • 0.5M CsPbI2Br precursor solution was sprayed at a flow rate of 0.8 mL/min for 280 seconds, and then 0.25 M CsPbI 3 precursor solution was added.
  • a graded CsPbI 3-x Br x perovskite thin film was formed on the c-TiO 2 /FTO substrate by spraying at a flow rate of 0.5 mL/min for 5 seconds.
  • the ultrasonic spray coating process conditions were a nozzle-to-substrate distance of 5 cm, a nozzle scan rate of 10 mm/s, and a CsPbI 2 Br precursor solution of 0.8 mL/min. It has a solution flow rate, a CsPbI 3 precursor solution flow rate of 0.5 mL/min (flow gas: N 2 , pressure: 7 psi), and a deposition temperature of 150°C.
  • Perovskite optoelectronic devices were fabricated in an atmospheric atmosphere under a controlled relative humidity of ⁇ 20%.
  • FIG. 4 is a cross-sectional scanning electron microscopy (SEM) image of a photoactive layer prepared by spray coating for 5 seconds (Example 1), and FIG. 5 shows a surface scanning electron microscope image.
  • SEM scanning electron microscopy
  • FIG. 6 is a cross-sectional scanning electron microscope image of the photoactive layer prepared by spray coating for 10 seconds (Example 2)
  • FIG. 7 is a surface scanning electron microscope image.
  • FIG. 8 is a cross-sectional scanning electron microscope image of a photoactive layer prepared by spray coating for 15 seconds (Example 3), and FIG. 9 is a surface scanning electron microscope image.
  • FIG. 10 is a cross-sectional scanning electron microscope image of a photoactive layer prepared by spray coating for 20 seconds (Example 4), and FIG. 11 is a surface scanning electron microscope image.
  • the thickness of the photoactive layer having a composition gradient in the depth direction increases from ⁇ 490 nm to ⁇ 500 nm.
  • GIXRD 12 shows a grazing incidence X-ray diffraction (GIXRD) graph of the penetration depth of the photoactive layer according to the spray coating time.
  • GIXRD grazing incidence X-ray diffraction
  • the photoactive layer is CsPbI 3.00 , CsPbI 2.75 Br 0.25 , CsPbI 2.50 Br 0.05 , CsPbI 2.25 Br 0.75 and CsPbI 2.00 Br 1 , and the composition of I and Br is changed in the depth direction. It can be seen that the composition has a gradient.
  • FIG. 13 is a grazing incidence X-ray diffraction graph of a photoactive layer prepared by spray coating for 5 seconds (Example 1)
  • FIG. 14 is a graph showing spray coating for 10 seconds (Example 2).
  • FIG. 15 is a graph showing spray coating for 15 seconds (Example 3)
  • FIG. 16 is a graph showing spray coating for 20 seconds (Example 4).
  • the (200) peak position of (200) CsPbI 3 is 28.69°, and the (200) peak position of CsPbI 2 Br is 29.55°, but as the grazing incidence angle increases, the (200) peak position is It can be seen that is gradually increased.
  • FIG. 17 is a graph showing the depth profile of the (200) peak position of the photoactive layer according to the spray coating time
  • FIG. 18 shows the correlation between the Br/Pb composition ratio (y) and the (200) peak position (x) It is a graph
  • FIG. 19 is a graph showing compositional depth profiles of the photoactive layer according to spray coating time.
  • Equation 1 The correlation between the Br/Pb composition ratio (y) and the (200) peak position (x) may be expressed by Equation 1 below.
  • FIG. 20 is a graph showing the depth profile of the electronic bandgap (Eg) of the photoactive layer according to the spray coating time
  • FIG. 21 is the minimum conduction band (CBM) of the photoactive layer according to the spray coating time
  • It is a graph showing the depth profile of the maximum valence band (VBM).
  • the average carrier life is increased as the spray coating time is increased from 5 seconds to 20 seconds.
  • the band gap may decrease, and the exciton binding energy may decrease, so that the emission lifetime may be increased.
  • the amount of I increases and the emission lifetime decreases due to the decrease of the exciton binding energy.
  • the electron-hole pairs generated in the perovskite photoactive layer become Separation occurs more easily, which may shorten the luminescence lifetime.
  • 22 to 32 are graphs illustrating device performance characteristics of a perovskite optoelectronic device according to an embodiment of the present invention.
  • FIG. 22 shows a scanning electron microscope image of a perovskite photoelectric device according to an embodiment of the present invention including a photoactive layer prepared by spray coating for 15 seconds (Example 3).
  • a perovskite photoelectric device FTO/bl-TiO 2 /graded CsPbI 3-x Br x /PTAA/Au
  • FTO/bl-TiO 2 /graded CsPbI 3-x Br x /PTAA/Au perovskite photoelectric device
  • FIG. 23 is a graph showing an absorption spectrum of a perovskite photoelectric device according to an embodiment of the present invention
  • FIG. 24 is a graph showing an external quantum efficiency spectrum (EQE spectra)
  • FIG. 25 is an open It is a graph showing the voltage (Voc)
  • Fig. 26 is a graph showing the short circuit current density (Jsc)
  • Fig. 27 is a graph showing the charging factor (FF)
  • Fig. 28 is a graph showing the energy conversion efficiency (PCE) It is one graph.
  • Table 1 is a table showing the electrical and optical characteristics of the perovskite optoelectronic device according to an embodiment of the present invention.
  • the absorption wavelength may gradually shift to red, which is a longer wavelength.
  • the spray coating time increases, so that the absorption wavelength gradually increases to a longer wavelength, so that the amount of light absorption increases, thereby increasing the amount of generated current density.
  • the filling factor has a maximum value when spray coating is performed for 15 seconds, and as a result, it can be seen that it has an energy conversion efficiency of 14.63 ⁇ 1.07% under 1-sun conditions.
  • FIG. 29 is a graph showing current density-voltage curves (JV curves) of a perovskite photoelectric device according to an embodiment of the present invention including a photoactive layer prepared by spray coating for 5 seconds (Example 1)
  • 30 is a graph in which spray coating is performed for 10 seconds (Example 2)
  • FIG. 31 is a graph in which spray coating is performed for 15 seconds (Example 3)
  • FIG. 32 is spray coating in progress for 20 seconds.
  • It is a graph.
  • the perovskite photoelectric device according to an embodiment of the present invention including a photoactive layer prepared by spray coating for 15 seconds (Example 3) in the case of forward scan It can be seen that 16.45%, high energy conversion efficiency of 16.81% for the reverse scan and charged particles.
  • 33 to 36 are graphs illustrating sub-modules and long-term stability characteristics of a perovskite optoelectronic device according to an embodiment of the present invention.
  • FIG. 33 is an image showing a sub-module of a perovskite optoelectronic device according to an embodiment of the present invention
  • FIG. 34 is a graph showing a photocurrent-voltage (IV) curve of the sub-module
  • FIG. 35 is an initial stage ( It is a graph showing the stabilized power output of the sub-module in the early stage; 0 to 60 sec. It is a graph showing the results of a long-term light-soaking stability test under (1-sun illumination)
  • FIG. 37 is a graph showing a photocurrent-voltage curve during a stability test for 1000 hours.
  • the western module of FIG. 33 is composed of 7 sub-cells connected in series.
  • the open circuit voltage is 7.64V
  • the current density is 281.12mA
  • the charging factor is 13.82%.
  • the sub-module of the perovskite optoelectronic device according to the embodiment of the present invention under 1-sun illumination shows a stabilized power output and has long-term stability under continuous light absorption. there is.
  • the energy conversion efficiency of the sub-module of the perovskite optoelectronic device according to the embodiment of the present invention is 12.54%, which is reduced by only ⁇ 09.3% compared to the perovskite optoelectronic device of the initial stage.

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Abstract

La présente invention concerne un dispositif optoélectronique à base de pérovskite et des particules de polymère poreuses préparées au moyen dudit procédé. La présente invention comprend les étapes consistant à : former une couche de transport d'électrons sur une première électrode; former une couche photoactive comprenant un composé de pérovskite sur la couche de transport d'électrons au moyen d'un revêtement par pulvérisation orthogonale; former une couche de transport de trous sur la couche photoactive comprenant le composé de pérovskite; et former une seconde électrode sur la couche de transport de trous, la couche photoactive comprenant le composé de pérovskite ayant un gradient de composition dans la direction de profondeur de la couche de transport de trous à la couche de transport d'électrons.
PCT/KR2021/010692 2020-08-11 2021-08-11 Procédé de préparation d'un dispositif optoélectronique à base de pérovskite et dispositif optoélectronique à base de pérovskite préparé par ledit procédé Ceased WO2022035239A1 (fr)

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CN116190491B (zh) * 2023-02-24 2024-01-16 浙江大学 一种纯无机铅卤钙钛矿异质结及其制备方法和应用

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