CN110707221B - Application of Amino Acid Ionic Liquids in the Preparation of Perovskite Layers in Perovskite Optoelectronic Devices - Google Patents
Application of Amino Acid Ionic Liquids in the Preparation of Perovskite Layers in Perovskite Optoelectronic Devices Download PDFInfo
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- CN110707221B CN110707221B CN201910910618.4A CN201910910618A CN110707221B CN 110707221 B CN110707221 B CN 110707221B CN 201910910618 A CN201910910618 A CN 201910910618A CN 110707221 B CN110707221 B CN 110707221B
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- ZXMGHDIOOHOAAE-UHFFFAOYSA-N 1,1,1-trifluoro-n-(trifluoromethylsulfonyl)methanesulfonamide Chemical compound FC(F)(F)S(=O)(=O)NS(=O)(=O)C(F)(F)F ZXMGHDIOOHOAAE-UHFFFAOYSA-N 0.000 description 5
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- XKZZNHPZEPVUQK-NUBCRITNSA-N [(1r)-1-carboxy-3-methylbutyl]azanium;chloride Chemical compound Cl.CC(C)C[C@@H](N)C(O)=O XKZZNHPZEPVUQK-NUBCRITNSA-N 0.000 description 2
- MEVUPUNLVKELNV-NUBCRITNSA-N [(2r)-1-methoxy-4-methylsulfanyl-1-oxobutan-2-yl]azanium;chloride Chemical compound Cl.COC(=O)[C@H](N)CCSC MEVUPUNLVKELNV-NUBCRITNSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
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- 230000007547 defect Effects 0.000 description 2
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- COQRGFWWJBEXRC-UHFFFAOYSA-N hydron;methyl 2-aminoacetate;chloride Chemical compound Cl.COC(=O)CN COQRGFWWJBEXRC-UHFFFAOYSA-N 0.000 description 2
- 150000002466 imines Chemical class 0.000 description 2
- VSDUZFOSJDMAFZ-SECBINFHSA-N methyl (2r)-2-amino-3-phenylpropanoate Chemical group COC(=O)[C@H](N)CC1=CC=CC=C1 VSDUZFOSJDMAFZ-SECBINFHSA-N 0.000 description 2
- KQSSATDQUYCRGS-UHFFFAOYSA-N methyl glycinate Chemical compound COC(=O)CN KQSSATDQUYCRGS-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
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- DVTRRYWFKKZCIE-UHFFFAOYSA-M 2-aminoacetate;1-ethyl-3-methylimidazol-3-ium Chemical compound NCC([O-])=O.CC[N+]=1C=CN(C)C=1 DVTRRYWFKKZCIE-UHFFFAOYSA-M 0.000 description 1
- XPFAJCSMHOQBQB-UHFFFAOYSA-N 2-aminoacetic acid;nitric acid Chemical compound O[N+]([O-])=O.NCC(O)=O XPFAJCSMHOQBQB-UHFFFAOYSA-N 0.000 description 1
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 1
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- 125000000296 D-methionine group Chemical group [H]N([H])[C@@]([H])(C(=O)[*])C([H])([H])C([H])([H])SC([H])([H])[H] 0.000 description 1
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- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
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- 229910019142 PO4 Inorganic materials 0.000 description 1
- DTQVDTLACAAQTR-UHFFFAOYSA-M Trifluoroacetate Chemical compound [O-]C(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-M 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 235000004279 alanine Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 1
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- 238000009792 diffusion process Methods 0.000 description 1
- JZJQCLZQSHLSFB-WCCKRBBISA-N ethyl (2s)-2-amino-3-hydroxypropanoate;hydrochloride Chemical compound Cl.CCOC(=O)[C@@H](N)CO JZJQCLZQSHLSFB-WCCKRBBISA-N 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
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- DWKPPFQULDPWHX-VKHMYHEASA-N l-alanyl ester Chemical compound COC(=O)[C@H](C)N DWKPPFQULDPWHX-VKHMYHEASA-N 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- SWVMLNPDTIFDDY-SBSPUUFOSA-N methyl (2r)-2-amino-3-phenylpropanoate;hydrochloride Chemical compound Cl.COC(=O)[C@H](N)CC1=CC=CC=C1 SWVMLNPDTIFDDY-SBSPUUFOSA-N 0.000 description 1
- ANSUDRATXSJBLY-VKHMYHEASA-N methyl (2s)-2-amino-3-hydroxypropanoate Chemical group COC(=O)[C@@H](N)CO ANSUDRATXSJBLY-VKHMYHEASA-N 0.000 description 1
- NDBQJIBNNUJNHA-DFWYDOINSA-N methyl (2s)-2-amino-3-hydroxypropanoate;hydrochloride Chemical compound Cl.COC(=O)[C@@H](N)CO NDBQJIBNNUJNHA-DFWYDOINSA-N 0.000 description 1
- LLWRXQXPJMPHLR-UHFFFAOYSA-N methylazanium;iodide Chemical compound [I-].[NH3+]C LLWRXQXPJMPHLR-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-M perchlorate Inorganic materials [O-]Cl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-M 0.000 description 1
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910001495 sodium tetrafluoroborate Inorganic materials 0.000 description 1
- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 description 1
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- ITMCEJHCFYSIIV-UHFFFAOYSA-M triflate Chemical compound [O-]S(=O)(=O)C(F)(F)F ITMCEJHCFYSIIV-UHFFFAOYSA-M 0.000 description 1
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- 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
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- H10K71/10—Deposition of organic active material
- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/15—Deposition of organic active material using liquid deposition, e.g. spin coating characterised by the solvent used
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- H—ELECTRICITY
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Abstract
本发明公开了氨基酸离子液体在制备钙钛矿光电器件中钙钛矿层的应用，所述氨基酸离子液体为氨基酸盐离子液体或氨基酸酯离子液体，所述氨基酸盐离子液体的通式为[A]n+[X‑]n，所述氨基酸酯离子液体的通式为[HA1COOR]+X‑，其中A为氨基酸，A1为A分子中羧基以外的部分，n的取值范围为1至4，X‑表示阴离子，R为1～3个碳原子的烷基。研究发现利用氨基酸离子液体能够调控钙钛矿层的表面形貌，进而提高形成的钙钛矿光电器件的性能，在钙钛矿光电器件领域具有重大的应用价值。
The invention discloses the application of an amino acid ionic liquid in the preparation of a perovskite layer in a perovskite photoelectric device. The amino acid ionic liquid is an amino acid salt ionic liquid or an amino acid ester ionic liquid. The general formula of the amino acid salt ionic liquid is [A] n+ [X ‑ ] n , the general formula of the amino acid ester ionic liquid is [HA 1 COOR] + X ‑ , wherein A is an amino acid, A 1 is a part other than the carboxyl group in the A molecule, and the value of n ranges from 1 to 4. X - represents an anion, and R is an alkyl group with 1 to 3 carbon atoms. The study found that the use of amino acid ionic liquids can regulate the surface morphology of the perovskite layer, thereby improving the performance of the formed perovskite optoelectronic devices, which has great application value in the field of perovskite optoelectronic devices.
Description
技术领域technical field
本发明涉及氨基酸离子液体，尤其是涉及氨基酸离子液体在制备钙钛矿光电器件中钙钛矿层的应用。The invention relates to an amino acid ionic liquid, in particular to the application of the amino acid ionic liquid in the preparation of a perovskite layer in a perovskite photoelectric device.
背景技术Background technique
太阳能技术是解决世界能源危机的有效手段，而高效率、低成本的太阳能电池是光伏系统的基础。作为第三代太阳能电池，自2009年问世以来，钙钛矿太阳能电池以其高吸光系数、高载流子迁移率、长载流子传输距离、成本低廉、可溶液加工等优点，受到科研人员广泛关注。短短几年发展，钙钛矿太阳能电池的光电转化效率从3.8％突破到22.7％。对于钙钛矿太阳能电池来说，如何提高其光电转化效率以及稳定性是现阶段研究的主要问题。Solar technology is an effective means to solve the world's energy crisis, and high-efficiency, low-cost solar cells are the basis of photovoltaic systems. As the third generation of solar cells, since its appearance in 2009, perovskite solar cells have been favored by researchers for their advantages of high light absorption coefficient, high carrier mobility, long carrier transmission distance, low cost, and solution processing. extensive attention. In just a few years of development, the photoelectric conversion efficiency of perovskite solar cells has broken through from 3.8% to 22.7%. For perovskite solar cells, how to improve their photoelectric conversion efficiency and stability is the main issue of current research.
钙钛矿晶体的生长是一个复杂的相变过程，反应体系中不同的溶液、温度、溶剂、添加剂等因素，都会造成最终晶体形貌、结构的不同。在平面异质结钙钛矿太阳能电池中，太阳能电池结构受界面效应及钙钛矿结晶时表面张力的影响，会造成钙钛矿薄膜结晶速度过快、成膜性差，使钙钛矿层的孔洞变多、表面粗糙度变大。后续沉积的空穴传输层或者电子传输层则会通过孔洞直接与致密层接触，使电池漏电流增大。而发生晶格畸变的钙钛矿晶体，也会对钙钛矿薄膜本身的带隙、载流子迁移率、界面载流子注入等参数带来巨大的影响。这些因素会导致平面异质结钙钛矿太阳能电池器件的性能大大降低，极大的限制了钙钛矿太阳能电池技术的发展。因此，制备高质量、低缺陷态的钙钛矿晶体薄膜，进而提高电池的光电转化效率、稳定性、重复性是该领域需要解决的关键问题之一。目前，研究人员采用多种手段调控钙钛矿层的质量，譬如2015年，黄劲松等人利用强配位溶剂DMSO添加到常用的DMF溶剂中，通过抑制碘化铅快速结晶实现晶体生长及晶体形貌的控制。2012年，Snaith等人通过在前驱体溶液中引入含氯化合物进而改变了碘化铅甲胺的结晶程度，降低了钙钛矿薄膜的缺陷，提高了载流子扩散长度。The growth of perovskite crystals is a complex phase transition process. Different solutions, temperatures, solvents, additives and other factors in the reaction system will cause differences in the final crystal morphology and structure. In the planar heterojunction perovskite solar cell, the structure of the solar cell is affected by the interface effect and the surface tension of the perovskite crystallization, which will cause the perovskite film to crystallize too fast and have poor film-forming properties, making the holes in the perovskite layer more, the surface roughness becomes larger. The subsequently deposited hole transport layer or electron transport layer will directly contact the dense layer through the holes, which will increase the leakage current of the battery. The perovskite crystal with lattice distortion will also have a huge impact on the band gap, carrier mobility, interface carrier injection and other parameters of the perovskite film itself. These factors will greatly reduce the performance of planar heterojunction perovskite solar cell devices, which greatly limits the development of perovskite solar cell technology. Therefore, preparing high-quality, low-defect perovskite crystal thin films to improve the photoelectric conversion efficiency, stability, and repeatability of cells is one of the key issues to be solved in this field. At present, researchers use various methods to control the quality of the perovskite layer. For example, in 2015, Huang Jinsong et al. added the strong coordination solvent DMSO to the commonly used DMF solvent to achieve crystal growth and crystal morphology by inhibiting the rapid crystallization of lead iodide. control. In 2012, Snaith et al. changed the crystallization degree of lead methylamine iodide by introducing chlorine-containing compounds into the precursor solution, which reduced the defects of the perovskite film and increased the carrier diffusion length.
离子液体是指全部由离子组成的液体，一般是由特定体积的相对较大的结构不对称的有机阳离子和体积较小的阴离子组成的。离子液体种类众多，理论上任意给定的有机阳离子和阴离子都可以组合成离子液体，通过改变有机阳离子和阴离子的种类即能够得到不同种类的离子液体。氨基酸离子液体属于离子液体的一种，天然氨基酸及其衍生物既可以充当离子液体的阴离子也可以充当阳离子，如甘氨酸硝酸盐(GlyNO3)、1-乙基-3甲基-咪唑甘氨酸盐(EMIGly)等。类似于常规离子液体，氨基酸离子液体具有高热稳定，此外氨基酸离子液体还具有其独特的性质如具有较强的氢键网络结构，能够溶解DNA等。目前，基于氨基酸离子液体的性能研究主要集中在其手性催化方面，至今未发现关于其对于钙钛矿层形貌调控方面的研究。Ionic liquids refer to liquids composed entirely of ions, generally composed of a relatively large organic cation with asymmetric structure and a small anion with a specific volume. There are many types of ionic liquids. In theory, any given organic cation and anion can be combined into an ionic liquid. By changing the types of organic cations and anions, different types of ionic liquids can be obtained. Amino acid ionic liquid is a kind of ionic liquid. Natural amino acid and its derivatives can act as both anion and cation of ionic liquid, such as glycine nitrate (GlyNO 3 ), 1-ethyl-3 methyl-imidazolium glycinate ( EMIGly) etc. Similar to conventional ionic liquids, amino acid ionic liquids have high thermal stability. In addition, amino acid ionic liquids also have unique properties such as a strong hydrogen bond network structure and the ability to dissolve DNA. At present, the performance research based on amino acid ionic liquids mainly focuses on its chiral catalysis, and no research on its regulation of perovskite layer morphology has been found so far.
发明内容Contents of the invention
本发明旨在至少解决现有技术中存在的技术问题之一。为此，本发明提出一种氨基酸离子液体在制备钙钛矿光电器件中钙钛矿层的应用，研究发现氨基酸类离子液体具有调控钙钛矿层形貌的作用，利于提高钙钛矿光电器件的性能。The present invention aims to solve at least one of the technical problems existing in the prior art. For this reason, the present invention proposes the application of an amino acid ionic liquid in the preparation of a perovskite layer in a perovskite optoelectronic device. It is found that the amino acid ionic liquid has the effect of regulating the morphology of the perovskite layer, which is conducive to improving the performance of the perovskite optoelectronic device .
本发明所采取的技术方案是：The technical scheme that the present invention takes is:
本发明的第一方面，提供一种氨基酸离子液体在制备钙钛矿光电器件中钙钛矿层的应用，所述氨基酸离子液体为氨基酸盐离子液体或氨基酸酯离子液体，所述氨基酸盐离子液体的通式为[A]n+[X-]n，所述氨基酸酯离子液体的通式为[HA1COOR]+X-，其中A为氨基酸，A1为A分子中羧基以外的部分，n的取值范围为1至4，X-表示阴离子，R为1～3个碳原子的烷基。The first aspect of the present invention provides an application of an amino acid ionic liquid in the preparation of a perovskite layer in a perovskite photoelectric device, the amino acid ionic liquid is an amino acid salt ionic liquid or an amino acid ester ionic liquid, the amino acid salt ionic liquid The general formula is [A] n+ [X - ] n , and the general formula of the amino acid ester ionic liquid is [HA 1 COOR] + X - , wherein A is an amino acid, A 1 is a part other than the carboxyl group in the A molecule, and n is The value ranges from 1 to 4, X- represents an anion, and R is an alkyl group with 1 to 3 carbon atoms.
根据本发明的一些实施例，所述氨基酸选自甘氨酸、D-甲硫氨酸、L-甲硫氨酸、DL-甲硫氨酸、D-丙氨酸、L-丙氨酸、DL-丙氨酸、D-缬氨酸、L-缬氨酸、DL-缬氨酸、D-亮氨酸、L-亮氨酸、DL-亮氨酸、D-异亮氨酸、L-异亮氨酸、DL-异亮氨酸、D-苯丙氨酸、L-苯丙氨酸、DL-苯丙氨酸、D-半胱氨酸、L-半胱氨酸、DL-半胱氨酸、D-胱氨酸、L-胱氨酸、DL-胱氨酸、D-苏氨酸、L-苏氨酸、DL-苏氨酸、D-谷氨酸、L-谷氨酸、DL-谷氨酸、D-谷酰胺、L-谷酰胺、DL-谷酰胺、D-天冬氨酸、L-天冬氨酸、DL-天冬氨酸、D-天冬酰胺、L-天冬酰胺、DL-天冬酰胺、D-蛋氨酸、L-蛋氨酸、DL-蛋氨酸、D-丝氨酸、L-丝氨酸、DL-丝氨酸、D-脯氨酸、L-脯氨酸、DL-脯氨酸、D-酪氨酸、L-酪氨酸、DL-酪氨酸、D-色氨酸、L-色氨酸、DL-色氨酸、D-赖氨酸、L-赖氨酸、DL-赖氨酸、D-精氨酸、L-精氨酸、DL-精氨酸、D-组氨酸、L-组氨酸、DL-组氨酸、D-鸟氨酸、L-鸟氨酸、DL-鸟氨酸、β-丙氨酸、2-氨基丁酸、3-氨基丁酸、4-氨基丁酸、2-氨基异丁酸、3-氨基异丁酸、2-氨基戊酸，2-氨基己酸、6-氨基己酸、o-氨基苯丙酸、p-氨基苯丙酸、m-氨基苯丙酸。According to some embodiments of the present invention, the amino acid is selected from glycine, D-methionine, L-methionine, DL-methionine, D-alanine, L-alanine, DL- Alanine, D-Valine, L-Valine, DL-Valine, D-Leucine, L-Leucine, DL-Leucine, D-Isoleucine, L-Iso Leucine, DL-Isoleucine, D-Phenylalanine, L-Phenylalanine, DL-Phenylalanine, D-Cysteine, L-Cysteine, DL-Cysteine amino acid, D-cystine, L-cystine, DL-cystine, D-threonine, L-threonine, DL-threonine, D-glutamic acid, L-glutamic acid , DL-glutamic acid, D-glutamine, L-glutamine, DL-glutamine, D-aspartic acid, L-aspartic acid, DL-aspartic acid, D-asparagine, L -Asparagine, DL-Asparagine, D-methionine, L-methionine, DL-methionine, D-serine, L-serine, DL-serine, D-proline, L-proline, DL-pro amino acid, D-tyrosine, L-tyrosine, DL-tyrosine, D-tryptophan, L-tryptophan, DL-tryptophan, D-lysine, L-lysine , DL-lysine, D-arginine, L-arginine, DL-arginine, D-histidine, L-histidine, DL-histidine, D-ornithine, L -Ornithine, DL-ornithine, β-alanine, 2-aminobutyric acid, 3-aminobutyric acid, 4-aminobutyric acid, 2-aminoisobutyric acid, 3-aminoisobutyric acid, 2 - Aminovaleric acid, 2-aminocaproic acid, 6-aminocaproic acid, o-aminophenylpropionic acid, p-aminophenylpropionic acid, m-aminophenylpropionic acid.
根据本发明的一些实施例，X-选自Cl-(氯离子)、Br-(溴离子)、I-(碘离子)、NO3 -(硝酸根)、ClO4 -(高氯酸酸根)、CF3CO2 -(三氟乙酸根)、CH3CO2 -(乙酸根)、NTf2 -(双三氟甲磺酰亚胺根)、PF6 -(六氟磷酸根)、BF4 -(四氟硼酸根)、CF3SO3 -(三氟甲磺酸根)中的任一种。According to some embodiments of the present invention, X - is selected from Cl - (chloride ion), Br - (bromide ion), I - (iodide ion), NO 3 - (nitrate), ClO 4 - (perchlorate) , CF 3 CO 2 - (trifluoroacetate), CH 3 CO 2 - (acetate), NTf 2 - (bistrifluoromethanesulfonimide), PF 6 - (hexafluorophosphate), BF 4 Any of - (tetrafluoroborate) and CF 3 SO 3 - (trifluoromethanesulfonate).
根据本发明的一些实施例，所述钙钛矿光电器件为钙钛矿太阳能电池。According to some embodiments of the present invention, the perovskite photovoltaic device is a perovskite solar cell.
本发明的第二方面，提供一种用于制备钙钛矿层的反溶剂，包括上述的应用中所述的氨基酸离子液体。The second aspect of the present invention provides an anti-solvent for preparing a perovskite layer, including the amino acid ionic liquid described in the above application.
根据本发明的一些实施例，还包括氯化苯。According to some embodiments of the present invention, chlorinated benzene is also included.
根据本发明的一些实施例，所述反溶剂中所述氨基酸离子液体的质量分数为0.01～2wt％。According to some embodiments of the present invention, the mass fraction of the amino acid ionic liquid in the anti-solvent is 0.01-2 wt%.
本发明的第三方面，提供一种钙钛矿太阳能电池的制备方法，包括利用反溶剂法制备钙钛矿层的步骤，其中使用的反溶剂为上述的用于制备钙钛矿层的反溶剂。The third aspect of the present invention provides a method for preparing a perovskite solar cell, including the step of preparing a perovskite layer by using an anti-solvent method, wherein the anti-solvent used is the above-mentioned anti-solvent for preparing the perovskite layer.
根据本发明的一些实施例，利用反溶剂法制备钙钛矿层的步骤具体为：取钙钛矿前驱体溶液涂覆在基体上，在涂覆的过程中滴加所述反溶剂，然后在80～100℃退火处理制得钙钛矿层。According to some embodiments of the present invention, the steps of preparing the perovskite layer by using the anti-solvent method are as follows: taking the perovskite precursor solution and coating it on the substrate, adding the anti-solvent dropwise during the coating process, and then at 80 The perovskite layer was prepared by annealing at ~100°C.
本发明的第四方面，提供一种钙钛矿太阳能电池，根据上述的钙钛矿太阳能电池的制备方法制得。The fourth aspect of the present invention provides a perovskite solar cell, which is manufactured according to the above-mentioned method for preparing a perovskite solar cell.
本发明实施例的有益效果是：The beneficial effects of the embodiments of the present invention are:
本发明实施例研究发现利用氨基酸离子液体能够有效降低钙钛矿的结晶速率，形成结晶度更大、粗糙度更低的钙钛矿层，从而降低了钙钛矿层的缺陷，改变了钙钛矿活性层的带隙，进而有效地减少钙钛矿太阳能光电器件的漏电流现象，本发明实施例利用氨基酸离子液体能够调控钙钛矿层的表面形貌，进而提高形成的钙钛矿光电器件的性能，在钙钛矿光电器件领域具有重大的应用价值。The embodiment of the present invention has found that the use of amino acid ionic liquids can effectively reduce the crystallization rate of perovskite and form a perovskite layer with greater crystallinity and lower roughness, thereby reducing the defects of the perovskite layer and changing the activity of the perovskite The band gap of the perovskite layer can effectively reduce the leakage current phenomenon of the perovskite solar photoelectric device. The embodiment of the present invention can regulate the surface morphology of the perovskite layer by using the amino acid ionic liquid, thereby improving the performance of the formed perovskite photoelectric device. It has great application value in the field of perovskite optoelectronic devices.
附图说明Description of drawings
图1为实施例1中制得的钙钛矿层和对比例1中的钙钛矿层的表面形貌图；Fig. 1 is the surface topography figure of the perovskite layer made in embodiment 1 and the perovskite layer in comparative example 1;
图2为实施例1中制得的太阳能电池和对比例1中制得的太阳能电池的性能曲线。FIG. 2 is the performance curves of the solar cell prepared in Example 1 and the solar cell prepared in Comparative Example 1. FIG.
具体实施方式Detailed ways
以下将结合实施例对本发明的构思及产生的技术效果进行清楚、完整地描述，以充分地理解本发明的目的、特征和效果。显然，所描述的实施例只是本发明的一部分实施例，而不是全部实施例，基于本发明的实施例，本领域的技术人员在不付出创造性劳动的前提下所获得的其他实施例，均属于本发明保护的范围。The conception and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments, so as to fully understand the purpose, features and effects of the present invention. Apparently, the described embodiments are only some of the embodiments of the present invention, rather than all of them. Based on the embodiments of the present invention, other embodiments obtained by those skilled in the art without creative efforts belong to The protection scope of the present invention.
实施例1Example 1
本实施例选用D-苯丙氨酸甲酯六氟磷酸盐离子液体为对象，研究其对钙钛矿层形貌以及太阳能电池性能的影响，具体实验过程如下：In this embodiment, D-phenylalanine methyl ester hexafluorophosphate ionic liquid is selected as the object, and its influence on the morphology of the perovskite layer and the performance of the solar cell is studied. The specific experimental process is as follows:
制备D-苯丙氨酸甲酯六氟磷酸盐离子液体：Preparation of D-phenylalanine methyl ester hexafluorophosphate ionic liquid:
取0.10mol D-苯丙氨酸甲酯盐酸盐和0.12mol六氟磷酸钾，在20mL乙腈中搅拌50h，过滤取滤液，滤液经旋转蒸发除去溶剂得到D-苯丙氨酸甲酯六氟磷酸盐离子液体。Take 0.10mol D-phenylalanine methyl ester hydrochloride and 0.12mol potassium hexafluorophosphate, stir in 20mL acetonitrile for 50h, filter to get the filtrate, and remove the solvent by rotary evaporation to obtain D-phenylalanine methyl hexafluoro Phosphate ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)制备反溶剂：取上述制备的D-苯丙氨酸甲酯六氟磷酸盐离子液体溶解于氯苯中，混合形成反溶剂，其中D-苯丙氨酸甲酯六氟磷酸盐离子液体的质量分数为0.1wt％。(2) Preparation of anti-solvent: Dissolve the D-phenylalanine methyl hexafluorophosphate ionic liquid prepared above in chlorobenzene, and mix to form an anti-solvent, wherein D-phenylalanine methyl hexafluorophosphate ion The mass fraction of liquid is 0.1wt%.
(3)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(3) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(4)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(4) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(5)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，将钙钛矿前驱体混合溶液滴加到空穴传输层上，在5000rpm转速下旋涂8s后滴加反溶剂，并在滴加反溶剂3s后关闭旋涂仪，在温度为80℃热台上退火10min，得到钙钛矿层。(5) Preparation of perovskite layer: transfer the ITO conductive glass with spin-coated PTAA to a constant temperature glove box protected by nitrogen gas, add the mixed solution of perovskite precursor to the hole transport layer, and spin-coat at 5000rpm After 8s, the anti-solvent was added dropwise, and the spin coater was turned off 3s after the anti-solvent was added dropwise, and annealed on a hot stage at a temperature of 80°C for 10min to obtain a perovskite layer.
(6)制备电子传输层：将20mg/mL PC61BM的氯苯溶液在2000rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 20 mg/mL PC 61 BM chlorobenzene solution at 2000 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为150nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 150 nm was evaporated by a vacuum coating machine.
对比例1：对比例1提供一种太阳能电池，与本实施例1中的太阳能电池结构和制备过程相同，不同之处在于，制备钙钛矿层的步骤(5)反溶剂中未添加D-苯丙氨酸甲酯六氟磷酸盐离子液体。Comparative Example 1: Comparative Example 1 provides a solar cell, which has the same structure and preparation process as the solar cell in Example 1, except that D-benzene is not added to the antisolvent in step (5) of preparing the perovskite layer Alanine methyl ester hexafluorophosphate ionic liquid.
对本实施例中制得的钙钛矿层和对比例1中的钙钛矿层的表面形貌进行SEM表征，结果如图1所示，图1中(a)表示添加有D-苯丙氨酸甲酯六氟磷酸盐离子液体的钙钛矿太阳能电池中钙钛矿层的SEM图，图1中(b)表示未添加该离子液体的钙钛矿太阳能电池中钙钛矿层的SEM图。从图1中可以看出，使用含有D-苯丙氨酸甲酯六氟磷酸盐离子液体的反溶剂制得的钙钛矿层的晶粒尺寸更大，边缘密度更小，结果表明D-苯丙氨酸甲酯六氟磷酸盐离子液体具有调控钙钛矿层形貌的作用。The surface morphology of the perovskite layer prepared in this example and the perovskite layer in Comparative Example 1 is characterized by SEM, the results are as shown in Figure 1, and (a) in Figure 1 represents the addition of D-phenylalanine methyl The SEM image of the perovskite layer in the perovskite solar cell of the ester hexafluorophosphate ionic liquid, (b) in Figure 1 represents the SEM image of the perovskite layer in the perovskite solar cell without the ionic liquid. It can be seen from Figure 1 that the perovskite layer prepared using the anti-solvent containing D-phenylalanine methyl hexafluorophosphate ionic liquid has larger grain size and less edge density, and the results show that D-phenylalanine Alanine methyl hexafluorophosphate ionic liquid can regulate the morphology of perovskite layer.
对本实施例中制得的太阳能电池和对比例1中制得的太阳能电池的性能进行测试，结果如图2所示，结果显示在100mW/cm2光照下经测试(有效面积0.06cm2)，本实施例中的太阳能电池的短路电流(Jsc)＝22.81mA/cm2、开路电压(Voc)＝1.07V、填充因子(FF)＝0.76、光电转化效率(PCE)＝18.5％，而对比例1中的太阳能电池的短路电流(Jsc)＝22.51mA/cm2、开路电压(Voc)＝1.02V、填充因子(FF)＝0.73、光电转化效率(PCE)＝16.7％。结果表明，使用D-苯丙氨酸甲酯六氟磷酸盐离子液体能够提高太阳能电池的性能。The performance of the solar cell made in this example and the solar cell made in Comparative Example 1 was tested, the results are shown in Figure 2, the results show that after testing under 100mW/cm 2 illumination (effective area 0.06cm 2 ), The short-circuit current (Jsc)=22.81mA/cm 2 , the open-circuit voltage (Voc)=1.07V, the fill factor (FF)=0.76, and the photoelectric conversion efficiency (PCE)=18.5% of the solar cell in this embodiment, while the comparative example The short-circuit current (Jsc) of the solar cell in 1 = 22.51 mA/cm 2 , the open-circuit voltage (Voc) = 1.02 V, the fill factor (FF) = 0.73, and the photoelectric conversion efficiency (PCE) = 16.7%. The results show that the use of D-phenylalanine methyl hexafluorophosphate ionic liquid can improve the performance of solar cells.
实施例2Example 2
本实施例提供一种太阳能电池，在制备钙钛矿层的过程中使用的反溶剂中的氨基酸离子液体选用L-丙氨酸六氟磷酸盐离子液体，具体实验过程如下：This embodiment provides a solar cell. The amino acid ionic liquid in the antisolvent used in the process of preparing the perovskite layer is L-alanine hexafluorophosphate ionic liquid. The specific experimental process is as follows:
制备L-丙氨酸六氟磷酸盐离子液体：Preparation of L-alanine hexafluorophosphate ionic liquid:
取0.10mol L-丙氨酸和0.10mol六氟磷酸溶于10mL水中，加热至60℃，后真空干燥12h，冷却得到L-丙氨酸六氟磷酸盐离子液体。Dissolve 0.10 mol L-alanine and 0.10 mol hexafluorophosphoric acid in 10 mL of water, heat to 60°C, dry in vacuum for 12 hours, and cool to obtain L-alanine hexafluorophosphate ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)制备反溶剂：取上述制备的L-丙氨酸六氟磷酸盐离子液体溶解于氯苯中，混合形成反溶剂，其中L-丙氨酸六氟磷酸盐离子液体的质量分数为0.2wt％。(2) Preparation of anti-solvent: Dissolve the L-alanine hexafluorophosphate ionic liquid prepared above in chlorobenzene, and mix to form an anti-solvent, wherein the mass fraction of L-alanine hexafluorophosphate ionic liquid is 0.2 wt%.
(3)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(3) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(4)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(4) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(5)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，将钙钛矿前驱体混合溶液滴加到空穴传输层上，在5000rpm转速下旋涂7s后滴加反溶剂，并在滴加反溶剂3s后关闭旋涂仪，在温度为85℃热台上退火10min，得到钙钛矿层。(5) Preparation of perovskite layer: transfer the ITO conductive glass with spin-coated PTAA to a constant temperature glove box protected by nitrogen gas, add the mixed solution of perovskite precursor to the hole transport layer, and spin-coat at 5000rpm After 7s, the anti-solvent was added dropwise, and after the anti-solvent was added dropwise for 3s, the spin coater was turned off, and annealed on a hot stage at a temperature of 85°C for 10min to obtain a perovskite layer.
(6)制备电子传输层：将20mg/mL PC61BM的氯苯溶液在2000rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 20 mg/mL PC 61 BM chlorobenzene solution at 2000 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为150nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 150 nm was evaporated by a vacuum coating machine.
对本实施例中制得的太阳能电池的性能进行测试，结果显示在100mW/cm2光照下经测试(有效面积0.06cm2)，本实施例中的太阳能电池的短路电流(Jsc)＝22.13mA/cm2、开路电压(Voc)＝1.08V、填充因子(FF)＝0.74、光电转化效率(PCE)＝17.7％，结果表明，使用D-苯丙氨酸甲酯六氟磷酸盐离子液体处理得到的太阳能电池具有优异的光电转化性能。 The performance of the solar cell prepared in this example was tested, and the results showed that the solar cell in this example had a short-circuit current ( Jsc ) of 22.13mA/ cm 2 , open circuit voltage (Voc) = 1.08V, fill factor (FF) = 0.74, photoelectric conversion efficiency (PCE) = 17.7%, the results show that using D-phenylalanine methyl ester hexafluorophosphate ionic liquid to obtain The solar cell has excellent photoelectric conversion performance.
实施例3Example 3
本实施例提供一种太阳能电池，在制备钙钛矿层的过程中使用的反溶剂中的氨基酸离子液体选用D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体和DL-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体，具体实验过程如下：This embodiment provides a solar cell, the amino acid ionic liquid in the anti-solvent used in the process of preparing the perovskite layer is selected from D-leucine bis(trifluoromethanesulfonyl)imide salt ionic liquid and DL-valine Acid bis(trifluoromethanesulfonyl)imide salt ionic liquid, the concrete experimental process is as follows:
制备D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体：Preparation of D-leucine bis(trifluoromethanesulfonyl)imide salt ionic liquid:
取0.10mol D-亮氨酸盐酸盐和0.12mol双(三氟甲烷磺酰)亚胺锂，溶于1mL水中，反应60h，取下层清液，后真空干燥12h，冷却得到D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体。Take 0.10mol of D-leucine hydrochloride and 0.12mol of lithium bis(trifluoromethanesulfonyl)imide, dissolve them in 1mL of water, react for 60h, remove the supernatant liquid, and then vacuum-dry for 12h, cool to obtain D-leucine Acid bis(trifluoromethanesulfonyl)imide salt ionic liquid.
制备DL-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体：Preparation of DL-valine bis(trifluoromethanesulfonyl)imide salt ionic liquid:
取0.10mol DL-缬氨酸盐酸盐和0.12mol双(三氟甲烷磺酰)亚胺锂，溶于1mL水中，反应60h，取下层清液，后真空干燥12h，冷却得到DL-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体。Take 0.10mol DL-valine hydrochloride and 0.12mol lithium bis(trifluoromethanesulfonyl)imide, dissolve them in 1mL water, react for 60h, remove the supernatant liquid, dry in vacuum for 12h, and cool to obtain DL-valine Acid bis(trifluoromethanesulfonyl)imide salt ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)制备反溶剂：取上述制备的D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体和DL-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体溶解于氯苯中，混合形成反溶剂，其中D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体的质量分数为0.1wt％，DL-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体的质量分数为0.15wt％。(2) Preparation of anti-solvent: Dissolve the D-leucine bis(trifluoromethanesulfonyl)imide salt ionic liquid and DL-valine bis(trifluoromethanesulfonyl)imide ionic liquid prepared above in In chlorobenzene, mix to form anti-solvent, wherein the mass fraction of D-leucine bis(trifluoromethanesulfonyl)imide salt ionic liquid is 0.1wt%, DL-valine bis(trifluoromethanesulfonyl)imide The mass fraction of the amine salt ionic liquid is 0.15wt%.
(3)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(3) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(4)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(4) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(5)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，将钙钛矿前驱体混合溶液滴加到空穴传输层上，在5000rpm转速下旋涂7s后滴加反溶剂，并在滴加反溶剂3s后关闭旋涂仪，在温度为90℃热台上退火8min，得到钙钛矿层。(5) Preparation of perovskite layer: transfer the ITO conductive glass with spin-coated PTAA to a constant temperature glove box protected by nitrogen gas, add the mixed solution of perovskite precursor to the hole transport layer, and spin-coat at 5000rpm The anti-solvent was added dropwise after 7s, and the spin coater was turned off 3s after the anti-solvent was added dropwise, and annealed on a hot stage at a temperature of 90°C for 8min to obtain a perovskite layer.
(6)制备电子传输层：将20mg/mL PC61BM的氯苯溶液在2000rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 20 mg/mL PC 61 BM chlorobenzene solution at 2000 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为150nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 150 nm was evaporated by a vacuum coating machine.
对本实施例中制得的太阳能电池的性能进行测试，结果显示在100mW/cm2光照下经测试(有效面积0.06cm2)，本实施例中的太阳能电池的短路电流(Jsc)＝23.17mA/cm2、开路电压(Voc)＝1.08V、填充因子(FF)＝0.75、光电转化效率(PCE)＝18.8％，结果表明，使用D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体和DL-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体处理得到的太阳能电池具有优异的光电转化性能。 The performance of the solar cell prepared in this example was tested, and the results showed that the solar cell in this example had a short-circuit current ( Jsc ) of 23.17mA/ cm 2 , open circuit voltage (Voc) = 1.08V, fill factor (FF) = 0.75, photoelectric conversion efficiency (PCE) = 18.8%, the results show that using D-leucine bis(trifluoromethanesulfonyl)imide salt The solar cell obtained by the treatment of ionic liquid and DL-valine bis(trifluoromethanesulfonyl)imide salt ionic liquid has excellent photoelectric conversion performance.
实施例4Example 4
本实施例提供一种太阳能电池，在制备钙钛矿层的过程中使用的反溶剂中的氨基酸离子液体选用L-丝氨酸甲酯六氟磷酸盐离子液体和L-丝氨酸乙酯六氟磷酸盐离子液体，具体实验过程如下：This embodiment provides a solar cell, the amino acid ionic liquid in the anti-solvent used in the process of preparing the perovskite layer is selected from L-serine methyl hexafluorophosphate ionic liquid and L-serine ethyl hexafluorophosphate ionic liquid , the specific experimental process is as follows:
制备L-丝氨酸甲酯六氟磷酸盐离子液体：Preparation of L-serine methyl hexafluorophosphate ionic liquid:
取0.10mol L-丝氨酸甲酯盐酸盐和0.12mol六氟磷酸钾，在1mL水中搅拌60h，取下层清夜，后真空干燥12h，冷却得到L-丝氨酸甲酯六氟磷酸盐离子液体。Take 0.10 mol of L-serine methyl ester hydrochloride and 0.12 mol of potassium hexafluorophosphate, stir in 1 mL of water for 60 h, remove the lower layer for clearing, dry in vacuum for 12 h, and cool to obtain L-serine methyl hexafluorophosphate ionic liquid.
制备L-丝氨酸乙酯六氟磷酸盐离子液体：Preparation of L-serine ethyl hexafluorophosphate ionic liquid:
取0.10mol L-丝氨酸乙酯盐酸盐和0.12mol六氟磷酸钾，在在1mL水中搅拌60h，取下层清夜，后真空干燥12h，冷却得到L-丝氨酸乙酯六氟磷酸盐离子液体。Take 0.10 mol of L-serine ethyl ester hydrochloride and 0.12 mol of potassium hexafluorophosphate, stir in 1 mL of water for 60 h, remove the lower layer for clearing, dry in vacuum for 12 h, and cool to obtain L-serine ethyl hexafluorophosphate ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)制备反溶剂：取上述制备的L-丝氨酸甲酯六氟磷酸盐离子液体和L-丝氨酸乙酯六氟磷酸盐离子液体溶解于氯苯中，混合形成反溶剂，其中L-丝氨酸甲酯六氟磷酸盐离子液体的质量分数为0.1wt％，L-丝氨酸乙酯六氟磷酸盐离子液体的质量分数为0.12wt％。(2) Preparation of anti-solvent: Dissolve the L-serine methyl hexafluorophosphate ionic liquid and L-serine ethyl hexafluorophosphate ionic liquid prepared above in chlorobenzene, and mix to form an anti-solvent, wherein L-serine methyl The mass fraction of the ester hexafluorophosphate ionic liquid is 0.1wt%, and the mass fraction of the L-serine ethyl hexafluorophosphate ionic liquid is 0.12wt%.
(3)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(3) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(4)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(4) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(5)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，将钙钛矿前驱体混合溶液滴加到空穴传输层上，在5000rpm转速下旋涂8s后滴加反溶剂，并在滴加反溶剂3s后关闭旋涂仪，在温度为85℃热台上退火10min，得到钙钛矿层。(5) Preparation of perovskite layer: transfer the ITO conductive glass with spin-coated PTAA to a constant temperature glove box protected by nitrogen gas, add the mixed solution of perovskite precursor to the hole transport layer, and spin-coat at 5000rpm The anti-solvent was added dropwise after 8s, and the spin coater was turned off after the anti-solvent was added dropwise for 3s, and annealed on a hot stage at a temperature of 85°C for 10min to obtain a perovskite layer.
(6)制备电子传输层：将20mg/mL PC61BM的氯苯溶液在2000rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 20 mg/mL PC 61 BM chlorobenzene solution at 2000 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为150nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 150 nm was evaporated by a vacuum coating machine.
对本实施例中制得的太阳能电池的性能进行测试，结果显示在100mW/cm2光照下经测试(有效面积0.06cm2)，本实施例中的太阳能电池的短路电流(Jsc)＝22.69mA/cm2、开路电压(Voc)＝1.06V、填充因子(FF)＝0.76、光电转化效率(PCE)＝18.3％，结果表明，使用L-丝氨酸甲酯六氟磷酸盐离子液体和L-丝氨酸乙酯六氟磷酸盐离子液体处理得到的太阳能电池具有优异的光电转化性能。 The performance of the solar cell prepared in this example was tested, and the results showed that the solar cell in this example had a short-circuit current ( Jsc ) of 22.69mA/ cm 2 , open circuit voltage (Voc) = 1.06V, fill factor (FF) = 0.76, photoelectric conversion efficiency (PCE) = 18.3%, the results show that using L-serine methyl ester hexafluorophosphate ionic liquid and L-serine ethyl The solar cells obtained by the treatment of ester hexafluorophosphate ionic liquid have excellent photoelectric conversion performance.
实施例5Example 5
本实施例提供一种太阳能电池，在制备钙钛矿层的过程中使用的反溶剂中的氨基酸离子液体选用D-甲硫氨酸甲酯六氟磷酸盐离子液体和D-甲硫氨酸甲酯四氟硼酸盐离子液体，具体实验过程如下：This embodiment provides a solar cell, the amino acid ionic liquid in the anti-solvent used in the process of preparing the perovskite layer is selected from D-methionine methyl hexafluorophosphate ionic liquid and D-methionine methyl Tetrafluoroborate ionic liquid, the specific experimental process is as follows:
制备D-甲硫氨酸甲酯六氟磷酸盐离子液体：Preparation of D-methionine methyl hexafluorophosphate ionic liquid:
取0.10mol D-甲硫氨酸甲酯盐酸盐和0.12mol六氟磷酸钾，在1mL水中搅拌60h，取下层清夜，后真空干燥12h，冷却得D-甲硫氨酸甲酯六氟磷酸盐离子液体。Take 0.10mol D-methionine methyl ester hydrochloride and 0.12mol potassium hexafluorophosphate, stir in 1mL water for 60h, remove the lower layer for clearing, then vacuum dry for 12h, and cool to obtain D-methionine methyl hexafluorophosphate salt ionic liquid.
制备D-甲硫氨酸甲酯四氟硼酸盐离子液体：Preparation of D-methionine methyl tetrafluoroborate ionic liquid:
取0.10mol D-甲硫氨酸甲酯盐酸盐和0.12mol四氟硼酸钠，1mL水中搅拌60h，取下层清夜，后真空干燥12h，冷却得D-甲硫氨酸甲酯四氟硼酸盐离子液体。Take 0.10mol D-methionine methyl ester hydrochloride and 0.12mol sodium tetrafluoroborate, stir in 1mL water for 60h, remove the lower layer for clearing, then vacuum dry for 12h, and cool to obtain D-methionine methyl tetrafluoroboric acid salt ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)制备反溶剂：取上述制备的D-甲硫氨酸甲酯六氟磷酸盐离子液体和D-甲硫氨酸甲酯四氟硼酸盐离子液体溶解于氯苯中，混合形成反溶剂，其中D-甲硫氨酸甲酯六氟磷酸盐离子液体的质量分数为0.2wt％，D-甲硫氨酸甲酯四氟硼酸盐离子液体的质量分数为0.3wt％。(2) Preparation of anti-solvent: the D-methionine methyl ester hexafluorophosphate ionic liquid and the D-methionine methyl tetrafluoroborate ionic liquid prepared above are dissolved in chlorobenzene, mixed to form an anti-solvent The solvent, wherein the mass fraction of D-methionine methyl hexafluorophosphate ionic liquid is 0.2wt%, and the mass fraction of D-methionine methyl tetrafluoroborate ionic liquid is 0.3wt%.
(3)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(3) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(4)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(4) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(5)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，将钙钛矿前驱体混合溶液滴加到空穴传输层上，在5000rpm转速下旋涂8s后滴加反溶剂，并在滴加反溶剂3s后关闭旋涂仪，在温度为100℃热台上退火8min，得到钙钛矿层。(5) Preparation of perovskite layer: transfer the ITO conductive glass with spin-coated PTAA to a constant temperature glove box protected by nitrogen gas, add the mixed solution of perovskite precursor to the hole transport layer, and spin-coat at 5000rpm After 8s, the anti-solvent was added dropwise, and after the anti-solvent was added dropwise for 3s, the spin coater was turned off, and annealed on a hot stage at a temperature of 100°C for 8min to obtain a perovskite layer.
(6)制备电子传输层：将20mg/mL PC61BM的氯苯溶液在2000rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 20 mg/mL PC61BM chlorobenzene solution at 2000 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为150nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 150 nm was evaporated by a vacuum coating machine.
对本实施例中制得的太阳能电池的性能进行测试，结果显示在100mW/cm2光照下经测试(有效面积0.06cm2)，本实施例中的太阳能电池的短路电流(Jsc)＝21.98mA/cm2、开路电压(Voc)＝1.09V、填充因子(FF)＝0.75、光电转化效率(PCE)＝18.0％，结果表明，使用D-甲硫氨酸甲酯六氟磷酸盐离子液体和D-甲硫氨酸甲酯四氟硼酸盐离子液体处理得到的太阳能电池具有优异的光电转化性能。 The performance of the solar cell prepared in this example was tested, and the results showed that the solar cell in this example had a short-circuit current ( Jsc ) of 21.98mA/ cm 2 , open circuit voltage (Voc) = 1.09V, fill factor (FF) = 0.75, photoelectric conversion efficiency (PCE) = 18.0%, the results show that using D-methionine methyl hexafluorophosphate ionic liquid and D -The solar cell obtained by the methionine methyl tetrafluoroborate ionic liquid treatment has excellent photoelectric conversion performance.
实施例6Example 6
本实施例提供一种太阳能电池，在制备钙钛矿层的过程中使用的反溶剂中的氨基酸离子液体选用甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体，具体实验过程如下：This embodiment provides a solar cell. The amino acid ionic liquid in the anti-solvent used in the process of preparing the perovskite layer is selected from glycine methyl ester bis(trifluoromethanesulfonyl)imide ionic liquid. The specific experimental process is as follows:
制备甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体：Preparation of glycine methyl ester bis(trifluoromethanesulfonyl)imide ionic liquid:
取0.10mol甘氨酸甲酯盐酸盐和0.12mol双(三氟甲烷磺酰)亚胺锂，1mL水中搅拌60h，取下层清夜，后真空干燥12h，冷却得甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体。Take 0.10mol glycine methyl ester hydrochloride and 0.12mol bis(trifluoromethanesulfonyl)imide lithium, stir in 1mL water for 60h, remove the lower layer for clearing, then vacuum dry for 12h, and cool to obtain glycine methyl ester bis(trifluoromethanesulfonyl) ) imine ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)制备反溶剂：取上述制备的甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体溶解于氯苯中，混合形成反溶剂，其中甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体的质量分数为0.1wt％。(2) Preparation of anti-solvent: Dissolve the glycine methyl ester bis(trifluoromethanesulfonyl)imide ionic liquid prepared above in chlorobenzene, and mix to form an anti-solvent, wherein glycine methyl ester bis(trifluoromethanesulfonyl)imide The mass fraction of the amine ionic liquid is 0.1wt%.
(3)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(3) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(4)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(4) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(5)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，将钙钛矿前驱体混合溶液滴加到空穴传输层上，在5000rpm转速下旋涂8s后滴加反溶剂，并在滴加反溶剂3s后关闭旋涂仪，在温度为80℃热台上退火10min，得到钙钛矿层。(5) Preparation of perovskite layer: transfer the ITO conductive glass with spin-coated PTAA to a constant temperature glove box protected by nitrogen gas, add the mixed solution of perovskite precursor to the hole transport layer, and spin-coat at 5000rpm After 8s, the anti-solvent was added dropwise, and the spin coater was turned off 3s after the anti-solvent was added dropwise, and annealed on a hot stage at a temperature of 80°C for 10min to obtain a perovskite layer.
(6)制备电子传输层：将30mg/mL PC61BM的氯苯溶液在2500rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 30 mg/mL PC61BM chlorobenzene solution at 2500 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为200nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 200 nm was evaporated by a vacuum coating machine.
对本实施例中制得的太阳能电池的性能进行测试，结果显示在100mW/cm2光照下经测试(有效面积0.06cm2)，本实施例中的太阳能电池的短路电流(Jsc)＝20.89mA/cm2、开路电压(Voc)＝1.06V、填充因子(FF)＝0.63、光电转化效率(PCE)＝14.0％，结果表明，使用甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体处理得到的太阳能电池具有优异的光电转化性能。 The performance of the solar cell prepared in this example was tested, and the results showed that the solar cell in this example had a short-circuit current ( Jsc ) of 20.89mA/ cm 2 , open circuit voltage (Voc) = 1.06V, fill factor (FF) = 0.63, photoelectric conversion efficiency (PCE) = 14.0%, the results show that using glycine methyl ester bis(trifluoromethanesulfonyl)imide ionic liquid The obtained solar cell has excellent photoelectric conversion performance.
实施例7Example 7
本实施例提供一种太阳能电池，在制备钙钛矿层的过程中使用的反溶剂中的氨基酸离子液体选用D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体和D-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体，具体实验过程如下：This embodiment provides a solar cell, the amino acid ionic liquid in the anti-solvent used in the process of preparing the perovskite layer is selected from D-leucine bis(trifluoromethanesulfonyl)imide salt ionic liquid and D-valline Acid bis(trifluoromethanesulfonyl)imide salt ionic liquid, the concrete experimental process is as follows:
制备D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体：Preparation of D-leucine bis(trifluoromethanesulfonyl)imide salt ionic liquid:
取0.10mol D-亮氨酸盐酸盐和0.12mol双(三氟甲烷磺酰)亚胺锂，1mL水中搅拌60h，取下层清夜，后真空干燥12h，冷却得D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体。Take 0.10mol of D-leucine hydrochloride and 0.12mol of lithium bis(trifluoromethanesulfonyl)imide, stir in 1mL of water for 60h, remove the lower layer for clearing, dry in vacuum for 12h, and cool to obtain D-leucine bis(trifluoromethanesulfonyl)imide Fluoromethanesulfonyl) imide salt ionic liquid.
制备D-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体：Preparation of D-valine bis(trifluoromethanesulfonyl)imide salt ionic liquid:
取0.10mol D-缬氨酸和0.12mol双(三氟甲烷磺酰)亚胺锂，1mL水中搅拌60h，取下层清夜，后真空干燥12h，冷却得到D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体。Take 0.10mol D-valine and 0.12mol lithium bis(trifluoromethanesulfonyl)imide, stir in 1mL water for 60h, remove the lower layer for clearing, dry in vacuum for 12h, and cool to obtain D-leucine bis(trifluoromethanesulfonyl) Acyl) imide salt ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)制备反溶剂：取上述制备的D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体和D-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体溶解于氯苯中，混合形成反溶剂，其中D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体的质量分数为0.1wt％，D-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体的质量分数为0.15wt％。(2) Preparation of anti-solvent: Dissolve the D-leucine bis(trifluoromethanesulfonyl)imide salt ionic liquid and D-valine bis(trifluoromethanesulfonyl)imide ionic liquid prepared above in In chlorobenzene, mix to form anti-solvent, wherein the mass fraction of D-leucine bis(trifluoromethanesulfonyl)imide salt ionic liquid is 0.1wt%, D-valine bis(trifluoromethanesulfonyl)imide The mass fraction of the amine salt ionic liquid is 0.15wt%.
(3)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(3) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(4)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(4) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(5)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，将钙钛矿前驱体混合溶液滴加到空穴传输层上，在5000rpm转速下旋涂8s后滴加反溶剂，并在滴加反溶剂3s后关闭旋涂仪，在温度为80℃热台上退火10min，得到钙钛矿层。(5) Preparation of perovskite layer: transfer the ITO conductive glass with spin-coated PTAA to a constant temperature glove box protected by nitrogen gas, add the mixed solution of perovskite precursor to the hole transport layer, and spin-coat at 5000rpm After 8s, the anti-solvent was added dropwise, and the spin coater was turned off 3s after the anti-solvent was added dropwise, and annealed on a hot stage at a temperature of 80°C for 10min to obtain a perovskite layer.
(6)制备电子传输层：将30mg/mL PC61BM的氯苯溶液在2500rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 30 mg/mL PC61BM chlorobenzene solution at 2500 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为200nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 200 nm was evaporated by a vacuum coating machine.
对本实施例中制得的太阳能电池的性能进行测试，结果显示在100mW/cm2光照下经测试(有效面积0.06cm2)，本实施例中的太阳能电池的短路电流(Jsc)＝21.04mA/cm2、开路电压(Voc)＝1.07V、填充因子(FF)＝0.58、光电转化效率(PCE)＝13.1％，结果表明，使用D-亮氨酸双(三氟甲烷磺酰)亚胺盐离子液体和D-缬氨酸双(三氟甲烷磺酰)亚胺盐离子液体处理得到的太阳能电池具有优异的光电转化性能。 The performance of the solar cell prepared in this example was tested, and the results showed that the solar cell in this example had a short-circuit current ( Jsc ) of 21.04mA/ cm 2 , open circuit voltage (Voc) = 1.07V, fill factor (FF) = 0.58, photoelectric conversion efficiency (PCE) = 13.1%, the results show that using D-leucine bis(trifluoromethanesulfonyl)imide salt The solar cell obtained by the treatment of ionic liquid and D-valine bis(trifluoromethanesulfonyl)imide salt ionic liquid has excellent photoelectric conversion performance.
实施例8Example 8
本实施例提供一种太阳能电池，在制备钙钛矿层的过程中使用的反溶剂中的氨基酸离子液体选用甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体，具体实验过程如下：This embodiment provides a solar cell. The amino acid ionic liquid in the anti-solvent used in the process of preparing the perovskite layer is selected from glycine methyl ester bis(trifluoromethanesulfonyl)imide ionic liquid. The specific experimental process is as follows:
制备甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体：Preparation of glycine methyl ester bis(trifluoromethanesulfonyl)imide ionic liquid:
取0.10mol甘氨酸甲酯盐酸盐和0.12mol双(三氟甲烷磺酰)亚胺锂，1mL水中搅拌60h，取下层清夜，后真空干燥12h，冷却得到甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体。Take 0.10mol glycine methyl ester hydrochloride and 0.12mol bis(trifluoromethanesulfonyl)imide lithium, stir in 1mL water for 60h, remove the lower layer for clearing, then vacuum dry for 12h, and cool to obtain glycine methyl ester bis(trifluoromethanesulfonyl) ) imine ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)制备反溶剂：取上述制备的甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体溶解于氯苯中，混合形成反溶剂，其中甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体的质量分数为0.5wt％。(2) Preparation of anti-solvent: Dissolve the glycine methyl ester bis(trifluoromethanesulfonyl)imide ionic liquid prepared above in chlorobenzene, and mix to form an anti-solvent, wherein glycine methyl ester bis(trifluoromethanesulfonyl)imide The mass fraction of the amine ionic liquid is 0.5wt%.
(3)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(3) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(4)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(4) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(5)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，将钙钛矿前驱体混合溶液滴加到空穴传输层上，在5000rpm转速下旋涂8s后滴加反溶剂，并在滴加反溶剂3s后关闭旋涂仪，在温度为80℃热台上退火10min，得到钙钛矿层。(5) Preparation of perovskite layer: transfer the ITO conductive glass with spin-coated PTAA to a constant temperature glove box protected by nitrogen gas, add the mixed solution of perovskite precursor to the hole transport layer, and spin-coat at 5000rpm After 8s, the anti-solvent was added dropwise, and the spin coater was turned off 3s after the anti-solvent was added dropwise, and annealed on a hot stage at a temperature of 80°C for 10min to obtain a perovskite layer.
(6)制备电子传输层：将30mg/mL PC61BM的氯苯溶液在2500rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 30 mg/mL PC61BM chlorobenzene solution at 2500 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为200nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 200 nm was evaporated by a vacuum coating machine.
对本实施例中制得的太阳能电池的性能进行测试，结果表明，使用甘氨酸甲酯双(三氟甲烷磺酰)亚胺离子液体处理得到的太阳能电池具有优异的光电转化性能。The performance of the solar cell prepared in this example was tested, and the results showed that the solar cell obtained by using glycine methyl ester bis(trifluoromethanesulfonyl)imide ionic liquid treatment had excellent photoelectric conversion performance.
实施例9Example 9
本实施例提供一种太阳能电池，在制备钙钛矿层的过程中使用的反溶剂中的氨基酸离子液体选用p-氨基苯丙酸硝酸盐离子液体和2-氨基戊酸乙酸盐离子液体，具体实验过程如下：This embodiment provides a solar cell, the amino acid ionic liquid in the anti-solvent used in the process of preparing the perovskite layer is selected from p-aminophenylpropionic acid nitrate ionic liquid and 2-aminovaleric acid acetate ionic liquid, specifically The experimental process is as follows:
制备p-氨基苯丙酸硝酸盐离子液体：Preparation of p-aminophenylpropionic acid nitrate ionic liquid:
取0.10mol p-氨基苯丙酸和0.10mol 65％硝酸溶于10mL水中，反应24h后，60℃下减压蒸馏除去水分，真空干燥24h，得到p-氨基苯丙酸硝酸盐离子液体。Dissolve 0.10 mol of p-aminophenylpropionic acid and 0.10 mol of 65% nitric acid in 10 mL of water. After reacting for 24 hours, the water was distilled off under reduced pressure at 60° C. and dried in vacuum for 24 hours to obtain p-aminophenylpropionic acid nitrate ionic liquid.
制备2-氨基戊酸乙酸盐离子液体：Preparation of 2-aminovaleric acid acetate ionic liquid:
取0.10mol 2-氨基戊酸与0.10mol三氟乙酸溶于10mL水中，反应24h后，60℃下减压蒸馏除去水分，真空干燥24h，得到2-氨基戊酸乙酸盐离子液体。Dissolve 0.10 mol of 2-aminovaleric acid and 0.10 mol of trifluoroacetic acid in 10 mL of water. After reacting for 24 hours, the water was distilled off under reduced pressure at 60° C. and dried in vacuum for 24 hours to obtain 2-aminovaleric acid acetate ionic liquid.
制备太阳能电池：Prepare solar cells:
(1)在氮气保护的恒温手套箱中称取摩尔比为1:1的碘甲胺与碘化铅，溶解于N,N-二甲基甲酰胺(DMF)溶液中，充分溶解后60℃恒温加热24h。冷却0.5h至室温，制得钙钛矿前驱体混合溶液。(1) Weigh methyl iodide and lead iodide with a molar ratio of 1:1 in a nitrogen-protected constant temperature glove box, dissolve them in N,N-dimethylformamide (DMF) solution, and dissolve them at 60°C Heating at constant temperature for 24h. Cool for 0.5h to room temperature to prepare a perovskite precursor mixed solution.
(2)将刻蚀好的ITO导电玻璃分别用光学清洗剂、蒸馏水、丙酮、异丙醇超声清洗各20min，用氮气吹干，随后用PLASMA表面清洗仪臭氧清洗15min，氮气吹净，放入无尘培养皿中，备用。(2) Clean the etched ITO conductive glass with optical cleaner, distilled water, acetone, and isopropanol ultrasonically for 20 minutes each, blow dry with nitrogen, and then clean it with ozone for 15 minutes with a PLASMA surface cleaner, blow it off with nitrogen, and put it in In a dust-free petri dish, set aside.
(3)制备空穴传输层：在已经清洗好的ITO导电玻璃上旋涂2mg/mL PTAA的甲苯溶液，控制转速为6000rpm，旋涂时间为35s，随后110℃退火20min形成空穴传输层。(3) Preparation of hole transport layer: spin-coat 2mg/mL PTAA toluene solution on the cleaned ITO conductive glass, control the rotation speed at 6000rpm, spin coating time for 35s, and then anneal at 110°C for 20min to form a hole transport layer.
(4)制备钙钛矿层：将旋涂好PTAA的ITO导电玻璃转移到氮气保护的恒温手套箱中，在5000rpm转速下将钙钛矿前驱体混合溶液旋涂空穴传输层上，在温度为80℃热台上退火10min，得到钙钛矿层。(4) Preparation of perovskite layer: transfer the ITO conductive glass that has been spin-coated with PTAA to a nitrogen-protected constant temperature glove box, and spin-coat the perovskite precursor mixed solution on the hole transport layer at a temperature of 5000 rpm. Anneal on a hot stage at 80°C for 10 minutes to obtain a perovskite layer.
(5)取p-氨基苯丙酸硝酸盐离子液体和2-氨基戊酸乙酸盐离子液体混合形成混合离子液体，将钙钛矿层浸泡在混合离子液体中1h，后取出使用氯苯冲洗、高纯氮气吹干。(5) Mix p-aminophenylpropionic acid nitrate ionic liquid and 2-aminovaleric acid acetate ionic liquid to form a mixed ionic liquid, soak the perovskite layer in the mixed ionic liquid for 1 hour, then take it out and wash it with chlorobenzene, Blow dry with high-purity nitrogen.
(6)制备电子传输层：将30mg/mL PC61BM的氯苯溶液在2500rpm转速下旋涂成膜到钙钛矿层上，旋涂时间为30s得到电子传输层。(6) Preparation of electron transport layer: Spin-coat 30 mg/mL PC61BM chlorobenzene solution at 2500 rpm to form a film on the perovskite layer for 30 s to obtain an electron transport layer.
(7)制备电子传输层修饰层：将12mg/mL ZnO的三氟乙醇溶液在4000rpm转速下旋涂成膜到电子传输层上，旋涂时间为60s形成电子传输层修饰层。(7) Preparation of electron transport layer modification layer: 12 mg/mL ZnO trifluoroethanol solution was spin-coated at 4000 rpm to form a film on the electron transport layer, and the spin coating time was 60 s to form an electron transport layer modification layer.
(8)蒸镀对电极：通过真空镀膜机蒸镀厚度为200nm的金属铝电极。(8) Vapor-deposited counter electrode: a metal aluminum electrode with a thickness of 200 nm was evaporated by a vacuum coating machine.
对本实施例中制得的太阳能电池的性能进行测试，结果表明，使用p-氨基苯丙酸硝酸盐离子液体和2-氨基戊酸乙酸盐离子液体浸泡处理后得到的太阳能电池具有优异的光电转化性能。The performance of the solar cell obtained in this example is tested, and the results show that the solar cell obtained after soaking with p-aminophenylpropionic acid nitrate ionic liquid and 2-aminovaleric acid acetate ionic liquid has excellent photoelectricity conversion performance.
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