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WO2020040361A1 - Film mince, son procédé de formation et cellule solaire de pérovskite comprenant un film mince - Google Patents

Film mince, son procédé de formation et cellule solaire de pérovskite comprenant un film mince Download PDF

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Publication number
WO2020040361A1
WO2020040361A1 PCT/KR2018/016019 KR2018016019W WO2020040361A1 WO 2020040361 A1 WO2020040361 A1 WO 2020040361A1 KR 2018016019 W KR2018016019 W KR 2018016019W WO 2020040361 A1 WO2020040361 A1 WO 2020040361A1
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WIPO (PCT)
Prior art keywords
thin film
forming
solar cell
type
perovskite solar
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Ceased
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PCT/KR2018/016019
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English (en)
Korean (ko)
Inventor
염준호
양리앙
김도형
김수경
소준영
시불라케빈
이유선
최동혁
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Korea Electric Power Corp
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Korea Electric Power Corp
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/30—Coatings
    • H10F77/306—Coatings for devices having potential barriers
    • H10F77/311—Coatings for devices having potential barriers for photovoltaic cells
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F77/00—Constructional details of devices covered by this subclass
    • H10F77/10—Semiconductor bodies
    • H10F77/12—Active materials
    • 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
    • H10K85/10—Organic polymers or oligomers
    • H10K85/111—Organic polymers or oligomers comprising aromatic, heteroaromatic, or aryl chains, e.g. polyaniline, polyphenylene or polyphenylene vinylene
    • H10K85/113—Heteroaromatic compounds comprising sulfur or selene, e.g. polythiophene
    • 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
    • H10K85/20—Carbon compounds, e.g. carbon nanotubes or fullerenes
    • H10K85/211—Fullerenes, e.g. C60
    • 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 thin film, a method for forming the same, and a perovskite solar cell including the thin film (THIN FILM, METHOD OF FORMING THIN FILM, PEROVSKITE SOLARCELL INCLUDING THIN FILM), and more particularly, an electron transport layer on a predetermined substrate. Or by coating a solution for forming a hole transport layer to form a thin film through a crosslinking reaction, not only to increase the solvent resistance of the organic semiconductor, but also to maintain the electron mobility, a thin film and its formation method and a perovskite comprising the thin film It relates to a skylight solar cell.
  • the electron transporting layer is an electron transporting material
  • the electron mobility that can transport electrons must be high, and the hole transporting layer must have a high hole mobility that can transport holes.
  • Such materials include organic semiconductor materials (e.g., n-type; fullerene derivatives, etc., p-type; PEDOT: PSS, etc.) or inorganic semiconductor materials (e.g., n-type; TiO 2 , SnO 2 , ZnO P, NiOx, etc.) may be used.
  • these materials can be solution based processes, for example, spin coating, slot coating, bar coating, sol-gel coating. ), A hydrothermal method, or the like, or a vapor deposition method such as sputtering, evaporation, atomic layer deposition, or the like.
  • a vapor deposition method such as sputtering, evaporation, atomic layer deposition, or the like.
  • organic materials are deposited in solution based processes.
  • solution-treated titanium dioxide TiO 2
  • inorganic material solution-treated titanium dioxide (TiO 2 ) is typically used as an inorganic material.
  • a process of manufacturing a high crystalline based TiO 2 film requires a high temperature based process of 500 ° C., which may cause hysteresis in the device.
  • Such titanium dioxide based devices are not known to be highly reliable.
  • n-type organic material is a fullerene-based material is Phenyl-C61-Butyric acid Methyl ester (PCBM).
  • PCBM Phenyl-C61-Butyric acid Methyl ester
  • the PCBM has a high electron mobility and high solubility in an organic solvent, and thus is easily used in a solution-based process, and is used in hybrid perovskite solar cells.
  • PCBM is highly soluble in solutions used in hybrid perovskite solar cells, such as DiMethylFormamide (DMF) and DiMethyl SulfOxide (DMSO). That is, in the case of coating perovskite on the n-type fullerene-based PCBM, since the PCBM film may be dissolved, it is limited to an application field based on thin film manufacturing.
  • DMF DiMethylFormamide
  • DMSO DiMethyl SulfOxide
  • the crosslinker which is an insulator, reduces the excellent electron mobility of the crosslinked PCBM. For this reason, in this case, the amount of the crosslinking agent must be limited, and there is a limit to improving the solvent resistance. In fact, the paper shows that UV-vis spectroscopy shows that about 80% of PCBM is lost.
  • An object of the present invention by coating a solution for forming an electron transporting layer or a hole transporting layer on a predetermined substrate to form a thin film through a crosslinking reaction, not only to increase the solvent resistance of the organic semiconductor, but also to maintain the electron mobility,
  • the present invention provides a thin film, a method of forming the same, and a perovskite solar cell including the thin film.
  • Method of forming a thin film the step of coating a solution for forming an electron or hole transport layer on a predetermined substrate; And forming a thin film through a crosslinking reaction of the solution, wherein the solution is, together with an organic semiconductor material, a semiconductor consisting of an azide group functional group and a phenyl diisocyanate (PDI) functional group.
  • Type crosslinker may be included.
  • the organic semiconductor material and the semiconductor cross-linking agent may be composed of a ratio of 70% and 30%.
  • the solvent of the solution may be a polar protic organic solvent.
  • the solvent is one of DMF (N, N-dimethylformamide), DMSO (DiMethyl SulfOxide), Acetone (Acetone), Acetonitrile, Dichloromethane, THF (Tetrahydrofuran), or a mixture of two or more. It may have been.
  • the solvent may have a final concentration of 3 mg / mL.
  • the semiconductor crosslinking agent may include n-type chromophore provided with pi conjugation when the organic semiconductor material is n-type.
  • the semiconductor crosslinking agent may include a p-type chromophore having pie conjugation when the organic semiconductor material is p-type.
  • the organic semiconductor material may be an n-type fullerene derivative having an alkyl group.
  • the fullerene derivative may be PCBM (Phenyl-C61-Butyric acid Methyl ester).
  • the organic semiconductor material may be P3HT (poly (3-hexylthiophene)) having a p-type having an alkyl group.
  • the coating step may be any one of spin coating, gravure offset coating, bar coating, slot-die coating, and roll coating.
  • the forming step may induce a crosslinking reaction through heat treatment or UV treatment, and when the heat treatment is performed, it may be performed at 180 ° C. for 1 minute.
  • the thin film according to the embodiment of the present invention may be a thin film formed by the thin film forming method according to any one of claims 1 to 12.
  • the perovskite solar cell in the perovskite solar cell in which the substrate, the transparent electrode layer, the electron transport layer, the photoactive layer, the hole transport layer, the metal electrode is laminated from the lower layer, the electron transport layer
  • the hole transport layer may be coated with a solution formed by mixing an organic semiconductor material and a semiconductor crosslinking agent in a solvent, and formed into a thin film through a crosslinking reaction of the solution, wherein the semiconductor crosslinking agent includes an azide functional group and a phenyl diisocyanate. It may be composed of a functional group.
  • the electron transport layer may be an n-type organic semiconductor material having an alkyl group, n-type chromophores with pie conjugation is provided in the semiconductor cross-linking agent.
  • the hole transport layer, the organic semiconductor material may be a p-type having an alkyl group
  • the semiconductor-type cross-linking agent may include a p-type chromophore provided with pie conjugation.
  • the present invention proposes a method for producing a thin film having excellent stability using an electron transport layer incorporating a semiconductor crosslinker through the present invention, and a perovskite solar cell without an existing inorganic electron transport layer or a hole blocking layer requiring a high temperature process.
  • the p-type of the semiconductor material is changed, it can also be applied to the hole transport layer can be applied to a variety of organic semiconductor-based devices.
  • FIG. 1 is a view for explaining a thin film forming method according to an embodiment of the present invention.
  • Figure 3 shows the absorption spectrum of the PCBM in the state that the semiconductor cross-linking agent is not included
  • FIG. 4 is a view showing an absorption spectrum of a thin film formed in FIG. 1;
  • FIG. 6 is a cross-sectional view of a perovskite solar cell including the thin film of FIG. 1;
  • FIG. 1 is a view for explaining a thin film forming method according to an embodiment of the present invention.
  • a solution 20 for forming an electron transporting layer or a hole transporting layer may be coated on a predetermined substrate 10 to form a thin film 21 through a crosslinking reaction.
  • the substrate 10 may be a glass substrate, but may be any one of various substrates used in a conventional semiconductor device process, such as another substrate, such as a plastic substrate or a silicon substrate.
  • the substrate 10 may have a transparent electrode layer formed in advance.
  • the solution 20 is formed of an n-type or p-type organic semiconductor material having an alkyl group (n-type; fullerene derivative, p-type; P 3 HT [poly (3-hexylthiophene)], etc.) to form an electron transporting layer or a hole transporting layer.
  • a PDI-DA semiconductor crosslinker composed of an azide functional group and a phenyl diisocyanate (PDI) functional group is included.
  • the molecular structure of the semiconductor crosslinking agent may be represented as shown in FIG. 2.
  • 2 is a diagram showing the molecular structure of a semiconductor crosslinking agent.
  • the semiconductor crosslinking agent includes an n-type chromophore with pi conjugation when the n-type organic semiconductor material is applied, and a pie conjugation when the p-type organic semiconductor material is applied.
  • P-type chromophores with gating are included.
  • the solution 20 for forming the electron transport layer may include a fullerene derivative, and may be representatively a Phenyl-C61-Butyric acid Methyl ester (PCBM).
  • PCBM Phenyl-C61-Butyric acid Methyl ester
  • the organic semiconductor material and the semiconductor crosslinking agent are composed of 70% and 30%.
  • the solvent is a polar aprotic organic solvent having a final concentration of 3 mg / mL, for example, N, N-dimethylformamide (DMF), DiMethyl SulfOxide (DMSO), Acetone, Acetonitrile, Acetonitrile, It may be one of dichloromethane, THF (Tetrahydrofuran) or a mixture of two or more.
  • concentration of the solvent may vary depending on the desired thickness.
  • the solution 20 may use various methods, for example, spin coating, gravure offset coating, bar coating, slot-die coating, roll coating, or the like when coating on the substrate 10.
  • This solution 20 is made into a thin film 21 through a solution based process.
  • the solution 20 is coated with a predetermined thickness (about 10nm) on the substrate 10, and then formed into a thin film 21 through heat treatment or ultraviolet treatment for the crosslinking reaction.
  • the heat treatment may be performed at 100 to 200 ° C. for 10 seconds to several tens of minutes, preferably at 180 ° C. for 1 minute.
  • Crosslinking reactions occur in which the azide groups are alkyl groups of PCBM or any other type of organic material.
  • the PDI-DA structure is independent of the crosslinking reaction.
  • FIG. 3 is a view showing an absorption spectrum of the PCBM in the state that the semiconductor cross-linking agent is not included
  • Figure 4 is a view showing the absorption spectrum of the thin film formed in FIG.
  • Figure 3 is a graph showing the change in UV-vis spectroscopy (UV-vis spectroscopy) before and after immersing the PCBM thin film in the DMF solution for 2 minutes.
  • FIG. 4 is a graph showing changes in UV-vis spectroscopy before and after soaking the thin film 21 formed by crosslinking reaction between the semiconductor crosslinking agent and the PCBM in a DMF solution for 2 minutes.
  • 5 is a diagram illustrating a change in electron mobility.
  • Electron mobility may vary depending on the ratio of the PCBM or crosslinking reaction conditions.
  • the electron mobility is maintained at 10 ⁇ 5 (cm ⁇ V ⁇ 1 ⁇ s ⁇ 1 ) or more even after the crosslinking reaction occurs, and 10 ⁇ 4 (cm ⁇ V ⁇ 1 when the ratio of PCBM is increased. S -1 ) or more can be maintained.
  • FIG. 6 is a cross-sectional view of a perovskite solar cell including the thin film of FIG. 1.
  • the perovskite solar cell 100 includes a substrate 110, a transparent electrode layer 120, an electron transport layer 130, a photoactive layer 140, a hole transport layer 150, and a metal electrode 160. It includes. That is, in the perovskite solar cell 100, the substrate 110, the transparent electrode layer 120, the electron transport layer 130, the photoactive layer 140, the hole transport layer 150, and the metal electrode 160 are stacked from the lower layer. It has a structure that becomes.
  • the thin film 21 of FIG. 1 may correspond to the electron transport layer 130 or the hole transport layer 150.
  • the case in which the thin film 21 is formed in the electron transport layer 130 will be described for convenience of description.
  • the substrate 110 may be a glass substrate, a plastic substrate (PET substrate, PES substrate, etc.), a silicon substrate, or the like.
  • the transparent electrode layer 120 is formed by thinly depositing a transparent electrode material on the substrate 110.
  • the transparent electrode may be formed of indium tin oxide (ITO), transparent conducting oxide (TCO), silver nanowier, carbon nanotube (CNT), graphene, Conductive polymers may be applied.
  • the transparent electrode layer 120 is washed with a mixed solution of acetone, ultrapure water and 2-propanol (IPA) for 30 minutes before forming the electron transport layer 130, and then UV / Ozone ) For 30 minutes.
  • IPA 2-propanol
  • the electron transport layer 130 is formed on the transparent electrode layer 120 by coating a solution consisting of a mixture of a PCBM and a semiconductor crosslinking agent in a solvent, and then formed by heat treatment or ultraviolet treatment for a crosslinking reaction.
  • PCBM and a semiconductor type crosslinking agent are comprised by the ratio of 70:30, and a solvent is the density
  • the solution is spin coated to a thickness of about 10 nm on the transparent electrode layer 120.
  • the heat treatment is carried out at 180 ° C. for 1 minute.
  • the photoactive layer 140 has 35% by weight of methyl ammonium iodide (CH 3 NH 3 I) and lead iodide (PbI 2 ) in a 1: 1 ratio of N, N-dimethylformamide (N, N-dimethylformamide, DMF).
  • CH 3 NH 3 I methyl ammonium iodide
  • PbI 2 lead iodide
  • the solution dispersed in is formed as a perovskite layer on the electron transport layer 130 through spin coating.
  • the photoactive layer 140 is heat-treated at 100 °C.
  • the hole transport layer 150 is composed of organic spiroza molecule (Spiro-OMeTAD), chlorobenzene, 4-tert-butylpyridine, and lithium bis (trifluoromethylsulfonyl) amide (lithium bis). (trifluoromethylsulfonyl) imide) is mixed into a thin film on the photoactive layer 140 through spin coating.
  • Spiro-OMeTAD organic spiroza molecule
  • chlorobenzene 4-tert-butylpyridine
  • lithium bis (trifluoromethylsulfonyl) amide lithium bis.
  • (trifluoromethylsulfonyl) imide) is mixed into a thin film on the photoactive layer 140 through spin coating.
  • the organic spiroza molecule (Spiro-OMeTAD) is 2,2 ', 7,7'-tetrakis- (N, N-di-4-methoxyphenylamino) -9,9'-spirobi-fluorene.
  • Chlorobenzene may be 723 mg / mL
  • 4-tert-butylpyridine is 288 ⁇ L / mL
  • lithium bis (trifluoromethylsulfonyl) amide may be 520 mg / mL.
  • the metal electrode 160 may be formed of gold (Au) to a thickness of 80 nm.
  • the embodiment is the perovskite solar cell of FIG. 6.
  • a solution of PCBM dissolved in 3 mg / mL of chloroform was coated by spin coating to form a PCBM thin film, that is, an electron transport layer. Layers other than the electron transport layer are formed in the same manner as described in FIG.
  • the example shows a perovskite solar cell using a PCBM electron transporter containing a semiconductor crosslinking agent
  • the comparative example shows a perovskite solar cell using only an electron transporter of PCBM without a semiconductor crosslinking agent.
  • the open voltage was 0.92 V
  • the short-circuit current density was 16.7 mA / cm 2
  • the curve factor was 44.8%.
  • the energy conversion efficiency (PCE) was 6.90%.
  • the embodiment exhibits an open voltage of 0.97V, a short circuit current density of 17.7 mA / cm 2 and a curve factor of 62.0%, resulting in an energy conversion efficiency (PCE) of 10.60%.
  • the example shows device performance with improved energy conversion efficiency (PCE) characteristics than the comparative example.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Nanotechnology (AREA)
  • Photovoltaic Devices (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Manufacturing & Machinery (AREA)

Abstract

La présente invention concerne un film mince, son procédé de formation, et une cellule solaire de pérovskite comprenant le film mince. Un procédé de formation de film mince selon un mode de réalisation de la présente invention comprend les étapes consistant à : revêtir, sur un substrat prédéterminé, une solution pour former une couche de transport d'électrons ou de trous ; et former un film mince par la réaction de réticulation de la solution, la solution pouvant comprendre, conjointement avec un matériau semi-conducteur organique, un agent de réticulation de type semi-conducteur composé d'un groupe fonctionnel à base d'azide et d'un groupe fonctionnel à base de diisocyanate de phényle (PDI).
PCT/KR2018/016019 2018-08-24 2018-12-17 Film mince, son procédé de formation et cellule solaire de pérovskite comprenant un film mince Ceased WO2020040361A1 (fr)

Applications Claiming Priority (2)

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KR1020180099091A KR102065554B1 (ko) 2018-08-24 2018-08-24 박막 및 그 형성 방법과 박막을 포함하는 페로브스카이트 태양전지
KR10-2018-0099091 2018-08-24

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Cited By (2)

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CN113285035A (zh) * 2021-05-19 2021-08-20 华能新能源股份有限公司 基于共轭聚合物掺杂的复合功能薄膜及其制备方法和应用
WO2024067311A1 (fr) * 2022-09-28 2024-04-04 Tcl科技集团股份有限公司 Dispositif photoélectrique et son procédé de fabrication

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KR102855289B1 (ko) * 2023-12-29 2025-09-05 충남대학교산학협력단 높은 안정성 및 높은 효율을 가지는 페로브스카이트 광전소자의 제조방법

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113285035A (zh) * 2021-05-19 2021-08-20 华能新能源股份有限公司 基于共轭聚合物掺杂的复合功能薄膜及其制备方法和应用
WO2024067311A1 (fr) * 2022-09-28 2024-04-04 Tcl科技集团股份有限公司 Dispositif photoélectrique et son procédé de fabrication

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