WO2020206873A1 - 膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池及其制备方法 - Google Patents

膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池及其制备方法 Download PDF

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WO2020206873A1
WO2020206873A1 PCT/CN2019/098048 CN2019098048W WO2020206873A1 WO 2020206873 A1 WO2020206873 A1 WO 2020206873A1 CN 2019098048 W CN2019098048 W CN 2019098048W WO 2020206873 A1 WO2020206873 A1 WO 2020206873A1
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film
hydroiodide
solar cell
hybrid perovskite
thick
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French (fr)
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吴刚
连小梅
陈杰焕
陈红征
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浙江大学
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Priority to JP2020529152A priority Critical patent/JP7102022B2/ja
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Priority to US17/149,740 priority patent/US11476432B2/en

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    • 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
    • H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
    • 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
    • H10K30/80—Constructional details
    • H10K30/81—Electrodes
    • H10K30/82—Transparent electrodes, e.g. indium tin oxide [ITO] electrodes
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/40—Thermal treatment, e.g. annealing in the presence of a solvent vapour
    • 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
    • H10K85/60—Organic compounds having low molecular weight
    • 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
    • H10K85/60—Organic compounds having low molecular weight
    • H10K85/649—Aromatic compounds comprising a hetero atom
    • H10K85/656—Aromatic compounds comprising a hetero atom comprising two or more different heteroatoms per ring
    • H10K85/6565—Oxadiazole compounds
    • 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
    • H10K30/20—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising organic-organic junctions, e.g. donor-acceptor junctions
    • 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
    • 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

Definitions

  • the invention belongs to the field of organic-inorganic hybrid perovskite materials, and specifically relates to an inverted thick film two-dimensional hybrid perovskite solar cell with insensitive film thickness and a preparation method thereof.
  • Two-dimensional perovskite materials have better moisture resistance properties than three-dimensional perovskites, but the efficiency of solar cells based on two-dimensional perovskites is lower than that of three-dimensional perovskite solar cells.
  • Improving the carrier transport capacity of the two-dimensional perovskite thin film material and improving its ability to absorb sunlight are all conducive to obtaining high-efficiency two-dimensional perovskite solar cells.
  • good research progress has been made.
  • the method of thermal spin coating, additives or mixed solvents can realize the crystal grains in the two-dimensional perovskite film. Oriented growth perpendicular to the substrate is conducive to the rapid transmission of photogenerated carriers.
  • the thickness of the two-dimensional perovskite film prepared by these methods on the PEDOT:PSS substrate is generally between 200-350 nm.
  • PEDOT PSS substrate is commonly used in inverted structure solar cells, and inverted structure is a device structure that is conducive to the large-area preparation of solar cells.
  • the purpose of the present invention is to solve the above-mentioned problems in the prior art and provide an inverted thick film two-dimensional hybrid perovskite solar cell that is insensitive to film thickness.
  • the solar cell uses a two-dimensional hybrid perovskite thick film material as the light absorption layer, and its thickness is in the range of 500-800nm, which helps to fully absorb sunlight; the thick film material can be added with guanidine hydroiodate It is obtained by deposition in the precursor solution of, composed of large crystal grains oriented along the thickness direction. In the thickness range of 500-800nm, the cell efficiency is not sensitive to the film thickness, so it can avoid the device caused by uneven film thickness during the preparation process Performance fluctuations.
  • the light absorption layer of the solar cell is a two-dimensional hybrid perovskite thick film material deposited from a precursor solution.
  • the precursor solution is a mixture of methylamine hydroiodide, spacer cation hydroiodide, guanidine hydroiodide, lead iodide and an organic solvent, and the spacer cation hydroiodide is n-butylamine and phenethylamine , Benzylamine, tert-butylamine or isobutylamine;
  • the two-dimensional hybrid perovskite thick film material is within the thickness range of 500-800nm, and the battery efficiency fluctuation range is less than 5%.
  • the present invention can further provide one or more of the following preferred implementation modes. It should be pointed out that the technical features of each preferred implementation manner of the present invention can be combined accordingly without conflicts.
  • the organic solvent is a mixture of one or more of formamide, dimethyl sulfoxide, and N,N-dimethylformamide.
  • the ratio of lead iodide to organic solvent in the precursor solution is 250-400 mg: 1 ml.
  • the specific method of the deposition is: spin-coating the precursor solution on the substrate to form a film, and annealing.
  • the temperature of the substrate is 25-150°C, and the temperature of the precursor solution is the same as that of the substrate.
  • the annealing temperature range is 70-150°C, and the annealing time range is 5-20 minutes.
  • the substrate is ITO glass covered with PEDOT:PSS.
  • the solar cell has a multilayer structure, from bottom to top, there are ITO glass, PEDOT:PSS layer, the light absorption layer, PC 61 BM layer, BCP layer (ie Bathocuproine, bath copper spirit) and silver electrode layer.
  • Another object of the present invention is to provide a method for preparing an inverted thick-film two-dimensional hybrid perovskite solar cell with insensitive film thickness. The steps are as follows:
  • methylamine hydroiodide, spacer cationic hydroiodide, guanamine hydroiodide, lead iodide and an organic solvent are mixed to prepare a precursor solution;
  • the spacer cationic hydroiodide is n-butylamine, Hydroiodide of one of phenethylamine, benzylamine, tert-butylamine or isobutylamine;
  • the organic solvent is one or more of formamide, dimethylsulfoxide, and N,N-dimethylformamide A mixture of species;
  • the ratio of lead iodide to organic solvent is 250-400 mg: 1
  • the precursor solution is spin-coated on the ITO glass substrate to form a film, and annealed to obtain a light absorption layer; during spin-coating, the temperature of the substrate is 25-150°C, and the temperature of the precursor solution used for spin-coating is the same as that of the substrate The temperature is the same; the annealing temperature range is 70-150°C, and the annealing time range is 5-20 minutes;
  • the PC 61 BM layer and the BCP layer were spin-coated on the surface of the light absorbing layer in turn, and finally a layer of silver was evaporated as the electrode layer.
  • the invention adopts high-quality two-dimensional hybrid perovskite thick film materials to prepare inverse solar cells with insensitive film thickness.
  • the solar cell light absorption layer is composed of a 500nm-800nm thick high-quality two-dimensional hybrid perovskite film with good orientation and few defects, which improves light absorption while maintaining good carrier transport characteristics, thus Improved battery efficiency.
  • the battery efficiency fluctuation range is less than 5%, which is conducive to large-area manufacturing.
  • the invention has very important significance for realizing high-efficiency optoelectronic devices that can be processed in a large area solution.
  • Figure 1 is a cross-sectional SEM image of a two-dimensional hybrid perovskite thick film material.
  • Figure 2 The relationship between the photoelectric conversion efficiency of hybrid perovskite solar cells and the thickness of two-dimensional hybrid perovskite thick film materials.
  • the preparation process of the inverted thick-film two-dimensional hybrid perovskite solar cell that is insensitive to film thickness is as follows: first, PEDOT:PSS is spin-coated on ITO glass to prepare a substrate, and then methylamine hydroiodide and spacer cation hydrogen iodide The precursor solution is prepared by mixing the acid salt, guanamine hydroiodide, lead iodide and organic solvent.
  • the spacer cationic hydroiodide is the hydroiodide of any one of n-butylamine, phenethylamine, benzylamine, tert-butylamine or isobutylamine, and the spacer cationic hydroiodide in the precursor solution: guanidine hydrogen
  • the ratio of lead iodide to organic solvent is 250-400 mg: 1 ml (different ratio will change the final film thickness); organic solvent is formamide , Dimethyl sulfoxide, N,N-dimethylformamide, one or more mixtures.
  • the precursor solution was spin-coated on the PEDOT:PSS layer on the surface of the ITO glass substrate to form a film, and then annealed.
  • the temperature of the substrate is 25-150°C
  • the temperature of the precursor solution used for spin coating is the same as the temperature of the substrate.
  • the annealing temperature range is 70-150°C
  • the annealing time range is 5-20 minutes.
  • the light absorption layer is obtained.
  • a layer of PC 61 BM and a layer of BCP were spin-coated on the surface of the light absorbing layer, and finally 100 nm silver was evaporated as the electrode layer.
  • the ITO glass substrate was ultrasonically washed with detergent, acetone, isopropanol, and ethanol for 5 minutes, then rinsed with deionized water and dried. After the dried ITO glass substrate is treated with ultraviolet-ozone, a PEDOT:PSS layer with a thickness of about 25 nm is prepared by a spin coating method, and it is baked at 140° C. for 15 minutes and then taken out.
  • the SEM image of Figure 1 shows that the two-dimensional hybrid perovskite thick film material is composed of large crystal grains oriented along the thickness direction.
  • four different sets of light absorption layer thicknesses are set, respectively 500nm, 600nm, 700nm and 800nm, and the thickness of the light absorption layer
  • the regulation is achieved by changing the ratio of lead iodide and N,N-dimethylformamide.
  • the value of M is 250, 300, 350, and 400, respectively.
  • the photoelectric conversion efficiency PCE of solar cells with different film thicknesses was measured.
  • Figure 2 shows that as the thickness of the two-dimensional hybrid perovskite thick film material increases, the photoelectric conversion efficiency of the solar cell basically remains constant: at 500nm, 600nm, At 700nm and 800nm thickness, the photoelectric conversion efficiency is 15.7%, 16.26%, 16%, 15.83%, and the fluctuation is less than 5%, indicating that the device performance is not sensitive to the thickness.
  • the ITO glass substrate was ultrasonically washed with detergent, acetone, isopropanol, and ethanol for 5 minutes, then rinsed with deionized water and dried. After the dried ITO glass substrate is treated with ultraviolet-ozone, a PEDOT:PSS layer with a thickness of about 25 nm is prepared by a spin coating method, and it is baked at 140° C. for 15 minutes and then taken out.
  • n-butylamine hydroiodide guanidine hydroiodide, methylamine hydroiodide and lead iodide in formamide
  • n-butylamine hydroiodide guanidine hydroiodide: methylamine hydroiodide
  • a film was formed by spin coating on the PEDOT:PSS layer on the surface of an ITO glass substrate at 150°C, and annealed at 150°C for 20 minutes to obtain a two-dimensional hybrid perovskite thick film material with a thickness of more than 500nm.
  • the cross-sectional morphology of the film was examined and the scan obtained
  • the electron microscope (SEM) photo is similar to Figure 1.
  • a layer of PC 61 BM and a layer of BCP were spin-coated in sequence, and a 100nm silver electrode layer was finally vapor-deposited to obtain an inverted thick-film two-dimensional hybrid perovskite solar cell.
  • different film thicknesses are also adjusted by changing the ratio of lead iodide and formamide, and the relationship between the thickness and the ratio is the same as in Example 1.
  • the change in photoelectric conversion efficiency with the increase of the thickness of the thick film material is similar to that in Figure 2, indicating that the cell efficiency is not sensitive to the thickness of the thick film material.
  • the ITO glass substrate was ultrasonically washed with detergent, acetone, isopropanol, and ethanol for 5 minutes, then rinsed with deionized water and dried. After the dried ITO glass substrate is treated with ultraviolet-ozone, a PEDOT:PSS layer with a thickness of about 25 nm is prepared by a spin coating method, and it is baked at 140° C. for 15 minutes and then taken out.
  • tert-butylamine hydroiodate Dissolve tert-butylamine hydroiodate, guanidine hydroiodide, methylamine hydroiodide, and lead iodide in dimethyl sulfoxide
  • tert-butylamine hydroiodide guanidine hydroiodide: methylamine hydroiodide
  • the PEDOT:PSS layer was spin-coated on the surface of the ITO glass substrate at °C, and annealed at 100°C for 15 minutes to obtain a two-dimensional hybrid perovskite thick film material with a thickness of more than 500nm.
  • the cross-sectional morphology of the film was investigated and the scanning electron microscope was obtained.
  • the (SEM) photo is similar to Figure 1.
  • a layer of PC 61 BM and a layer of BCP were spin-coated in sequence, and a 100nm silver electrode layer was finally vapor-deposited to obtain an inverted thick-film two-dimensional hybrid perovskite solar cell.
  • different film thicknesses are also adjusted by changing the ratio of lead iodide and dimethyl sulfoxide, and the relationship between the thickness and the ratio is the same as in Example 1.
  • the change in photoelectric conversion efficiency with the increase of the thickness of the thick film material is similar to that in Figure 2, indicating that the cell efficiency is not sensitive to the thickness of the thick film material.
  • the ITO glass substrate was ultrasonically washed with detergent, acetone, isopropanol, and ethanol for 5 minutes, then rinsed with deionized water and dried. After the dried ITO glass substrate is treated with ultraviolet-ozone, a PEDOT:PSS layer with a thickness of about 25 nm is prepared by a spin coating method, and it is baked at 140° C. for 15 minutes and then taken out.
  • the ITO glass substrate was ultrasonically washed with detergent, acetone, isopropanol, and ethanol for 5 minutes, then rinsed with deionized water and dried. After the dried ITO glass substrate is treated with ultraviolet-ozone, a PEDOT:PSS layer with a thickness of about 25 nm is prepared by a spin coating method, and it is baked at 140° C. for 15 minutes and then taken out.
  • the ITO glass substrate was ultrasonically washed with detergent, acetone, isopropanol, and ethanol for 5 minutes, then rinsed with deionized water and dried. After the dried ITO glass substrate is treated with ultraviolet-ozone, a PEDOT:PSS layer with a thickness of about 25 nm is prepared by a spin coating method, and it is baked at 140° C. for 15 minutes and then taken out.
  • the cross section of the film was investigated The morphology, the obtained scanning electron microscope (SEM) photograph is similar to Figure 1. Then, a layer of PC 61 BM and a layer of BCP were spin-coated in sequence, and a 100nm silver electrode layer was finally vapor-deposited to obtain an inverted thick-film two-dimensional hybrid perovskite solar cell.
  • different film thicknesses are also adjusted by changing the ratio of lead iodide to dimethyl sulfoxide/formamide, and the relationship between the thickness and the ratio is the same as in Example 1.
  • the change in photoelectric conversion efficiency with the increase of the thickness of the thick film material is similar to that in Figure 2, indicating that the cell efficiency is not sensitive to the thickness of the thick film material.
  • the ITO glass substrate was ultrasonically washed with detergent, acetone, isopropanol, and ethanol for 5 minutes, then rinsed with deionized water and dried. After the dried ITO glass substrate is treated with ultraviolet-ozone, a PEDOT:PSS layer with a thickness of about 25 nm is prepared by a spin coating method, and it is baked at 140° C. for 15 minutes and then taken out.
  • the ITO glass substrate was ultrasonically washed with detergent, acetone, isopropanol, and ethanol for 5 minutes, then rinsed with deionized water and dried. After the dried ITO glass substrate is treated with ultraviolet-ozone, a PEDOT:PSS layer with a thickness of about 25 nm is prepared by a spin coating method, and it is baked at 140° C. for 15 minutes and then taken out.
  • tert-butylamine hydroiodide Dissolve tert-butylamine hydroiodide, guanidine hydroiodide, methylamine hydroiodide, and lead iodide in N,N-dimethylformamide
  • tert-butylamine hydroiodide guanidine hydroiodide: formate
  • the bulk solution was spin-coated on the PEDOT:PSS layer on the surface of the ITO glass substrate at 100°C and annealed at 150°C for 15 minutes to obtain a two-dimensional hybrid perovskite thick film material with a thickness of more than 500nm.
  • the cross-sectional morphology of the film was investigated.
  • the obtained scanning electron microscope (SEM) photograph is similar to Figure 1.
  • a layer of PC 61 BM and a layer of BCP were spin-coated in sequence, and a 100nm silver electrode layer was finally vapor-deposited to obtain an inverted thick-film two-dimensional hybrid perovskite solar cell.
  • different film thicknesses are also adjusted by changing the ratio of lead iodide and N,N-dimethylformamide, and the relationship between the thickness and the ratio is the same as in Example 1.
  • the change in photoelectric conversion efficiency with the increase of the thickness of the thick film material is similar to that in Figure 2, indicating that the cell efficiency is not sensitive to the thickness of the thick film material.

Abstract

一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池及其制备方法，其属于有机-无机杂化钙钛矿材料领域。该太阳电池以二维杂化钙钛矿厚膜材料为光吸收层，其厚度范围是500-800nm，有助于对太阳光的充分吸收；该厚膜材料可以从添加了胍氢碘酸盐的前驱体溶液中沉积获得，由沿着厚度方向取向生长的大晶粒所构成，以此厚膜材料为光吸收层制备的反型结构太阳电池，在500-800nm膜厚范围内，电池效率波动范围小于5％。这对于高性能杂化钙钛矿太阳电池的大面积溶液法制备具有十分重要的价值。

Description

膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池及其制备方法 技术领域
本发明属于有机-无机杂化钙钛矿材料领域，具体涉及一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池及其制备方法。
技术背景
随着三维有机-无机杂化钙钛矿太阳电池效率的不断提高，其稳定性也受到了越来越多的关注。二维钙钛矿材料具有比三维钙钛矿更好的耐潮湿特性，但基于二维钙钛矿的太阳电池效率却低于三维钙钛矿太阳电池。
提高二维钙钛矿薄膜材料的载流子传输能力和提升其对太阳光的吸收能力都有利于获得高效率的二维钙钛矿太阳电池。在提高二维钙钛矿薄膜材料的载流子传输能力方面，目前已经获得了很好的研究进展，采用热旋涂、添加剂或者混合溶剂的方法，可以实现二维钙钛矿薄膜中晶粒垂直于基底取向生长，有利于光生载流子的快速传输。但是，这些方法在PEDOT：PSS基底上制备得到的二维钙钛矿薄膜的厚度一般在200-350nm之间。这是因为二维钙钛矿材料晶体结构的各相异性，造成其薄膜生长时，薄膜中的晶粒一般只能在较薄的厚度范围(<300nm)保持垂直取向。这就导致二维钙钛矿薄膜随厚度的增加，厚度方向晶界增多，薄膜质量下降，从而造成载流子传输能力下降，并降低太阳电池的光电转换效率。PEDOT：PSS基底为反型结构太阳电池所普遍采用，而反型结构是一种有利于太阳电池大面积制备的器件结构，因此，在PEDOT：PSS基底上实现高质量二维钙钛矿厚膜(>500nm)材料的制备，有利于太阳光的充分吸收，以提高太阳电池效率具有重要的价值。同时，杂化钙钛矿电池在大面积溶液法制备时，杂化钙钛矿薄膜的厚度往往并不完全一致，从而导致器件性能的过度波动，因此降低杂化钙钛矿电池效率对杂化钙钛矿薄膜厚度的敏感性也是非常重要的。目前，还没有关于制备膜厚不敏感的反型结构二维杂化钙钛矿太阳电池的公开报道。
发明内容
本发明的目的是解决现有技术中存在的上述问题，并提供一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池。该太阳电池以二维杂化钙钛矿厚膜材料为光吸收层，其厚度范围是500-800nm，有助于对太阳光的充分吸收；该厚膜材料可以从添加了胍氢碘酸盐的前驱体溶液中沉积获得，由沿着厚度方向取向生长的大晶粒所构成，在500-800nm厚度范围内电池效率对膜厚不敏感，因此能够避免制备过程中膜厚不均导致的器件性能波动。
本发明具体采用的技术方案如下：
一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，该太阳电池的光吸收层是从前驱体溶液中沉积获得的二维杂化钙钛矿厚膜材料，所述前驱体溶液为甲胺氢碘酸盐、间隔阳离子氢碘酸盐、胍氢碘酸盐、碘化铅与有机溶剂的混合物，所述的间隔阳离子氢碘酸盐为正丁胺、苯乙胺、苯甲胺、叔丁胺或异丁胺中一种的氢碘酸盐；所述二维杂化钙钛矿厚膜材料在500-800nm厚度范围内，电池效率波动范围小于5％。
在该方案的基础上，本发明还可以进一步提供以下一种或多种优选实现方式。需要指出的是，本发明中各个优选实现方式的技术特征在没有相互冲突的前提下，均可进行相应组合。
优选的，所述的有机溶剂为甲酰胺、二甲基亚砜、N,N-二甲基甲酰胺中一种或多种的混合物。
优选的，所述的前驱体溶液中，碘化铅与有机溶剂的配比为250-400毫克:1毫升。
优选的，所述的前驱体溶液中，以摩尔比计，间隔阳离子氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅为(2-2x):x:2:3或(2-2x):x:3:4或(2-2x):x:4:5，x＝0.01～0.3。
优选的，所述沉积的具体方法为：将所述前驱体溶液旋涂于基底上成膜，并退火。
进一步的，旋涂时，基底的温度为25-150℃，所述前驱体溶液的温度与基底相同。
进一步的，退火温度范围为70-150℃，退火时间范围为5-20分钟。
进一步的，所述的基底是覆盖有PEDOT:PSS的ITO玻璃。
进一步的，太阳电池为多层结构，从下至上依次为ITO玻璃、PEDOT:PSS层、所述光吸收层、PC 61BM层、BCP层(即Bathocuproine，浴铜灵)和银电极层。
本发明的另一目的在于提供一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池的制备方法，其步骤如下：
首先，制备表面旋涂PEDOT:PSS层的ITO玻璃基底；
然后，将甲胺氢碘酸盐、间隔阳离子氢碘酸盐、胍胺氢碘酸盐、碘化铅与有机溶剂混合制备前驱体溶液；所述的间隔阳离子氢碘酸盐为正丁胺、苯乙胺、苯甲胺、叔丁胺或者异丁胺中一种的氢碘酸盐；所述有机溶剂为甲酰胺、二甲基亚砜、N,N-二甲基甲酰胺中一种或多种的混合物；所述前驱体溶液中，以摩尔比计，间隔阳离子氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅为(2-2x):x:2:3或(2-2x):x:3:4或(2-2x):x:4:5，x＝0.01～0.3；碘化铅与有机溶剂的配比为250-400毫克:1毫升；
接着，将所述前驱体溶液旋涂于ITO玻璃基底上成膜，并退火得到光吸收层；旋涂时，基底的温度为25-150℃，用于旋涂的前驱体溶液的温度与基底温度相同；退火温度范围为70-150℃，退火时间范围为5-20分钟；
最后，在光吸收层表面依次旋涂PC 61BM层和BCP层，最后蒸镀一层银作为电极层。
本发明采用高质量二维杂化钙钛矿厚膜材料制备膜厚不敏感的反型太阳电池。一方面，太阳电池光吸收层由取向好，缺陷少的500nm-800nm厚的高质量二维杂化钙钛矿薄膜组成，在提高光吸收的同时保持了很好的载流子传输特性，从而提高了电池效率。另外，在500-800nm厚度范围内，电池效率波动范围小于5％，有利于实现大面积制造。该发明对于实现可大面积溶液加工的高效率光电器件具有十分重要的意义。
附图说明
图1是二维杂化钙钛矿厚膜材料横截面SEM图。
图2杂化钙钛矿太阳电池光电转换效率与二维杂化钙钛矿厚膜材料厚度的关系。
具体实施方式
膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池的制备过程为：首先将PEDOT:PSS旋涂在ITO玻璃上制备基底，然后将甲胺氢碘酸盐、间隔阳离子氢碘酸盐、胍胺氢碘酸盐、碘化铅与有机溶剂混合制备前驱体溶液。其中：间隔阳离子氢碘酸盐为正丁胺、苯乙胺、苯甲胺、叔丁胺或者异丁胺中的任意一种的氢碘酸盐，前驱体溶液中间隔阳离子氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅的比例(摩尔比)为(2-2x):x:2:3或(2-2x):x:3:4或(2-2x):x:4:5,x＝0.01～0.3；碘化铅与有机溶剂的配比为250-400毫克:1毫升(不同的配比会改变最终得到的膜层厚度)；有机溶剂为甲酰胺、二甲基亚砜、N,N-二甲基甲酰胺中一种或多种的混合物。然后将前驱体溶液继续旋涂于ITO玻璃基底表面的PEDOT:PSS层上成膜，并退火。旋涂时，基底的温度为25-150℃，用于旋涂的前驱体溶液的温度与基底温度相同。退火温度范围70-150℃，退火时间范围5-20分钟。退火完毕，得到光吸收层。接着在光吸收层表面依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银作为电极层。
下面基于上述制备方法，通过如下实施例对本发明作进一步的详述：
实施例1：
将ITO玻璃基底依次用洗涤剂、丙酮、异丙醇、乙醇各超声洗涤5分钟后，用去离子水漂洗并烘干。将烘干的ITO玻璃基底经紫外-臭氧处理后，用旋涂的方法制备厚度约为25nm的PEDOT:PSS层，140℃下烘烤15分钟后取出。将苯乙胺氢碘酸盐、胍氢碘酸盐、甲胺氢碘酸盐、碘化铅混合溶解于N,N-二甲基甲酰胺中，碘化铅与N,N-二甲基甲酰胺的配比为M毫克:1毫升，苯乙胺氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅(摩尔比)为(2-2x):x:2:3，x＝0.01，搅拌过夜，获得前驱体溶液；采用溶液旋涂的方法，取25℃的前驱体溶液在25℃的ITO玻璃基底表面PEDOT:PSS层上旋涂成膜，70℃退火5分钟，得到一定厚度的二维杂化钙钛矿厚膜材料，作为电池的光吸收层。接着在光吸收层上依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银电极层，得到反型厚膜二维杂化钙钛矿太阳电池。
图1的SEM图像表明二维杂化钙钛矿厚膜材料由沿着厚度方向取向生长的大晶粒所构成。本实施例中，为了体现二维杂化钙钛矿厚膜材料与膜厚的关系，设置了4组不同的光吸收层厚度，分别为500nm、600nm、700nm和800nm，而光吸收层厚度的调控是通过改变碘化铅与N,N-二甲基甲酰胺的配比实现的。500nm、600nm、700nm和800nm厚度的光吸收层中，M的取值分别为250、300、350和400。对不同膜厚的太阳电池的光电转换效率PCE进行测定，图2表明随着二维杂化钙钛矿厚膜材料的厚度的增加，太阳电池的光电转换效率基本保持恒定：在500nm、600nm、700nm和800nm厚度下，光电转换效率依次为15.7％、16.26％、16％、15.83％，波动低于5％，表明器件性能对厚度不敏感。
实施例2
将ITO玻璃基底依次用洗涤剂、丙酮、异丙醇、乙醇各超声洗涤5分钟后，用去离子水漂洗并烘干。将烘干的ITO玻璃基底经紫外-臭氧处理后，用旋涂的方法制备厚度约为25nm的PEDOT:PSS层，140℃下烘烤15分钟后取出。将正丁胺氢碘酸盐、胍氢碘酸盐、甲胺氢碘酸盐、碘化铅混合溶解于甲酰胺中，正丁胺氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅(摩尔比)为(2-2x):x:4:5，x＝0.3，搅拌过夜，获得前驱体溶液；采用溶液旋涂的方法，取150℃的前驱体溶液在150℃的ITO玻璃基底表面PEDOT:PSS层上旋涂成膜，150℃退火20分钟，得到厚度超过500nm的二维杂化钙钛矿厚膜材料，考察薄膜的横截面形貌，得到的扫描电镜(SEM)照片与图1相类似。接着依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银电极层，得到反型厚膜二维杂化钙钛矿太阳电池。本实施例中，也通过改变碘化铅与甲酰胺的配比来调整不同的膜厚，厚度与配比关系与实施例1相同。其光电转换效率随厚膜材料厚度增加的变化情况与图2相类似，表明电池效率对厚膜材料的厚度不敏感。
实施例3：
将ITO玻璃基底依次用洗涤剂、丙酮、异丙醇、乙醇各超声洗涤5分钟后，用去离子水漂洗并烘干。将烘干的ITO玻璃基底经紫外-臭氧处理后，用旋涂的方法制备厚度约为25nm的PEDOT:PSS层，140℃下烘烤15分钟后取出。将叔丁胺氢碘酸盐、胍氢碘酸盐、甲胺氢碘酸盐、碘化铅混合溶解于二甲基亚砜中，叔丁胺氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅(摩尔比)为(2-2x):x:3:4，x＝0.2，搅拌过夜，获得前驱体溶液；采用溶液旋涂的方法，取70℃的前驱体溶液在70℃的ITO玻璃基底表面PEDOT:PSS层上旋涂成膜，100℃退火15分钟，得到厚度超过500nm的二维杂化钙钛矿厚膜材料，考察薄膜的横截面形貌，得到的扫描电镜(SEM)照片与图1相类似。接着依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银电极层，得到反型厚膜二维杂化钙钛矿太阳电池。本实施例中，也通过改变碘化铅与二甲基亚砜的配比来调整不同的膜厚，厚度与配比关系与实施例1相同。其光电转换效率随厚膜材料厚度增加的变化情况与图2相类似，表明电池效率对厚膜材料的厚度不敏感。
实施例4：
将ITO玻璃基底依次用洗涤剂、丙酮、异丙醇、乙醇各超声洗涤5分钟后，用去离子水漂洗并烘干。将烘干的ITO玻璃基底经紫外-臭氧处理后，用旋涂的方法制备厚度约为25nm的PEDOT:PSS层，140℃下烘烤15分钟后取出。将异丁胺氢碘酸盐、胍氢碘酸盐、甲胺氢碘酸盐、碘化铅混合溶解于N,N-二甲基甲酰胺/二甲基亚砜中，异丁胺氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅(摩尔比)为(2-2x):x:4:5，x＝0.1，搅拌过夜，获得前驱体溶液；采用溶液旋涂的方法，取80℃的前驱体溶液在80℃的ITO玻璃基底表面PEDOT:PSS层上旋涂成膜，90℃退火10分钟，得到厚度超过500nm的二维杂化钙钛矿厚膜材料，考察薄膜的横截面形貌，得到的扫描电镜(SEM)照片与图1相类似。接着依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银电极层，得到反型厚膜二维杂化钙钛矿太阳电池。本实施例中，也通过改变碘化铅与N,N-二甲基甲酰胺/二甲基亚砜的配比来调整不同的膜厚，厚度与配比关系与实施例1相同。其光电转换效率随厚膜材料厚度增加的变化情况与图2相类似，表明电池效率对厚膜材料的厚度不 敏感。
实施例5：
将ITO玻璃基底依次用洗涤剂、丙酮、异丙醇、乙醇各超声洗涤5分钟后，用去离子水漂洗并烘干。将烘干的ITO玻璃基底经紫外-臭氧处理后，用旋涂的方法制备厚度约为25nm的PEDOT:PSS层，140℃下烘烤15分钟后取出。将异丁胺氢碘酸盐、胍氢碘酸盐、甲胺氢碘酸盐、碘化铅混合溶解于N,N-二甲基甲酰胺/甲酰胺中，异丁胺氢碘酸盐氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅(摩尔比)为(2-2x):x:3:4，x＝0.05，搅拌过夜，获得前驱体溶液；采用溶液旋涂的方法，取50℃的前驱体溶液在50℃的ITO玻璃基底表面PEDOT:PSS层上旋涂成膜，120℃退火12分钟，得到厚度超过500nm的二维杂化钙钛矿厚膜材料，考察薄膜的横截面形貌，得到的扫描电镜(SEM)照片与图1相类似。接着依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银电极层，得到反型厚膜二维杂化钙钛矿太阳电池。本实施例中，也通过改变碘化铅与N,N-二甲基甲酰胺/甲酰胺的配比来调整不同的膜厚，厚度与配比关系与实施例1相同。其光电转换效率随厚膜材料厚度增加的变化情况与图2相类似，表明电池效率对厚膜材料的厚度不敏感。
实施例6：
将ITO玻璃基底依次用洗涤剂、丙酮、异丙醇、乙醇各超声洗涤5分钟后，用去离子水漂洗并烘干。将烘干的ITO玻璃基底经紫外-臭氧处理后，用旋涂的方法制备厚度约为25nm的PEDOT:PSS层，140℃下烘烤15分钟后取出。将苯甲胺氢碘酸盐、胍氢碘酸盐、甲胺氢碘酸盐、碘化铅混合溶解于二甲基亚砜/甲酰胺中，苯甲胺氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅(摩尔比)为(2-2x):x:2:3，x＝0.25，搅拌过夜，获得前驱体溶液；采用溶液旋涂的方法，取120℃的前驱体溶液在120℃的ITO玻璃基底表面PEDOT:PSS层上旋涂成膜，130℃退火10分钟，得到厚度超过500nm的二维杂化钙钛矿厚膜材料，考察薄膜的横截面形貌，得到的扫描电镜(SEM)照片与图1相类似。接着依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银电 极层，得到反型厚膜二维杂化钙钛矿太阳电池。本实施例中，也通过改变碘化铅与二甲基亚砜/甲酰胺的配比来调整不同的膜厚，厚度与配比关系与实施例1相同。其光电转换效率随厚膜材料厚度增加的变化情况与图2相类似，表明电池效率对厚膜材料的厚度不敏感。
实施例7：
将ITO玻璃基底依次用洗涤剂、丙酮、异丙醇、乙醇各超声洗涤5分钟后，用去离子水漂洗并烘干。将烘干的ITO玻璃基底经紫外-臭氧处理后，用旋涂的方法制备厚度约为25nm的PEDOT:PSS层，140℃下烘烤15分钟后取出。将叔丁胺氢碘酸盐、胍氢碘酸盐、甲胺氢碘酸盐、碘化铅混合溶解于N,N-二甲基甲酰胺/二甲基亚砜/甲酰胺中，叔丁胺氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅(摩尔比)为(2-2x):x:4:5，x＝0.2，搅拌过夜，获得前驱体溶液；采用溶液旋涂的方法，取40℃的前驱体溶液在40℃的ITO玻璃基底表面PEDOT:PSS层上旋涂成膜，140℃退火20分钟，得到厚度超过500nm的二维杂化钙钛矿厚膜材料，考察薄膜的横截面形貌，得到的扫描电镜(SEM)照片与图1相类似。接着依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银电极层，得到反型厚膜二维杂化钙钛矿太阳电池。本实施例中，也通过改变碘化铅与N,N-二甲基甲酰胺/二甲基亚砜/甲酰胺的配比来调整不同的膜厚，厚度与配比关系与实施例1相同。其光电转换效率随厚膜材料厚度增加的变化情况与图2相类似，表明电池效率对厚膜材料的厚度不敏感。
实施例8：
将ITO玻璃基底依次用洗涤剂、丙酮、异丙醇、乙醇各超声洗涤5分钟后，用去离子水漂洗并烘干。将烘干的ITO玻璃基底经紫外-臭氧处理后，用旋涂的方法制备厚度约为25nm的PEDOT:PSS层，140℃下烘烤15分钟后取出。将叔丁胺氢碘酸盐、胍氢碘酸盐、甲胺氢碘酸盐、碘化铅混合溶解于N,N-二甲基甲酰胺中，叔丁胺氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅(摩尔比)为(2-2x):x:3:4，x＝0.15，搅拌过夜，获得前驱体溶液；采用溶液旋涂的方法，取100℃的前驱体溶液在100℃的ITO玻璃基底表面PEDOT:PSS层上旋涂成膜，150℃退火15 分钟，得到厚度超过500nm的二维杂化钙钛矿厚膜材料，考察薄膜的横截面形貌，得到的扫描电镜(SEM)照片与图1相类似。接着依次旋涂一层PC 61BM和一层BCP，最后蒸镀100nm银电极层，得到反型厚膜二维杂化钙钛矿太阳电池。本实施例中，也通过改变碘化铅与N,N-二甲基甲酰胺的配比来调整不同的膜厚，厚度与配比关系与实施例1相同。其光电转换效率随厚膜材料厚度增加的变化情况与图2相类似，表明电池效率对厚膜材料的厚度不敏感。

Claims (10)

  1. 一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于：该太阳电池的光吸收层是从前驱体溶液中沉积获得的二维杂化钙钛矿厚膜材料，所述前驱体溶液为甲胺氢碘酸盐、间隔阳离子氢碘酸盐、胍氢碘酸盐、碘化铅与有机溶剂的混合物，所述的间隔阳离子氢碘酸盐为正丁胺、苯乙胺、苯甲胺、叔丁胺或异丁胺中一种的氢碘酸盐；所述二维杂化钙钛矿厚膜材料在500-800nm厚度范围内；电池效率波动范围小于5％。
  2. 根据权利要求1所述的一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于所述的有机溶剂为甲酰胺、二甲基亚砜、N,N-二甲基甲酰胺中一种或多种的混合物。
  3. 根据权利要求1所述的一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于所述的前驱体溶液中，碘化铅与有机溶剂的配比为250-400毫克:1毫升。
  4. 根据权利要求1所述的一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于所述的前驱体溶液中，以摩尔比计，间隔阳离子氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅为(2-2x):x:2:3或(2-2x):x:3:4或(2-2x):x:4:5，x＝0.01～0.3。
  5. 根据权利要求1所述的一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于所述沉积的具体方法为：将所述前驱体溶液旋涂于基底上成膜，并退火。
  6. 根据权利要求5所述的一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于旋涂时，基底的温度为25-150℃，所述前驱体溶液的温度与基底相同。
  7. 根据权利要求5所述的一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于退火温度范围为70-150℃，退火时间范围为5-20分钟。
  8. 根据权利要求5所述的一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于所述的基底是覆盖有PEDOT:PSS的ITO玻璃。
  9. 根据权利要求1所述的一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池，其特征在于太阳电池为多层结构，从下至上依次为ITO玻璃、PEDOT:PSS层、所述光吸收层、PC 61BM 层、BCP层和银电极层。
  10. 一种膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池的制备方法，其特征在于，步骤如下：
    首先，制备表面旋涂PEDOT:PSS层的ITO玻璃基底；
    然后，将甲胺氢碘酸盐、间隔阳离子氢碘酸盐、胍胺氢碘酸盐、碘化铅与有机溶剂混合制备前驱体溶液；所述的间隔阳离子氢碘酸盐为正丁胺、苯乙胺、苯甲胺、叔丁胺或者异丁胺中一种的氢碘酸盐；所述有机溶剂为甲酰胺、二甲基亚砜、N,N-二甲基甲酰胺中一种或多种的混合物；所述前驱体溶液中，以摩尔比计，间隔阳离子氢碘酸盐:胍氢碘酸盐:甲胺氢碘酸盐:碘化铅为(2-2x):x:2:3或(2-2x):x:3:4或(2-2x):x:4:5，x＝0.01～0.3；碘化铅与有机溶剂的配比为250-400毫克:1毫升；
    接着，将所述前驱体溶液旋涂于ITO玻璃基底上成膜，并退火得到光吸收层；旋涂时，基底的温度为25-150℃，用于旋涂的前驱体溶液的温度与基底温度相同；退火温度范围为70-150℃，退火时间范围为5-20分钟；
    最后，在光吸收层表面依次旋涂PC 61BM层和BCP层，最后蒸镀一层银作为电极层。
PCT/CN2019/098048 2019-04-11 2019-07-26 膜厚不敏感的反型厚膜二维杂化钙钛矿太阳电池及其制备方法 WO2020206873A1 (zh)

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