CN115537736A - 一种无甲胺组分钙钛矿薄膜的制备方法及其应用 - Google Patents
一种无甲胺组分钙钛矿薄膜的制备方法及其应用 Download PDFInfo
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- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000001704 evaporation Methods 0.000 claims abstract description 52
- 239000010409 thin film Substances 0.000 claims abstract description 48
- 150000003839 salts Chemical class 0.000 claims abstract description 46
- 230000008020 evaporation Effects 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000002243 precursor Substances 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 13
- 239000010408 film Substances 0.000 claims description 27
- 239000000843 powder Substances 0.000 claims description 20
- 238000000151 deposition Methods 0.000 claims description 19
- 238000001771 vacuum deposition Methods 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 16
- 238000000137 annealing Methods 0.000 claims description 15
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- 239000002994 raw material Substances 0.000 claims description 14
- -1 cesium compound Chemical class 0.000 claims description 11
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 11
- 229910052792 caesium Inorganic materials 0.000 claims description 10
- 230000005525 hole transport Effects 0.000 claims description 10
- PNKUSGQVOMIXLU-UHFFFAOYSA-N Formamidine Chemical class NC=N PNKUSGQVOMIXLU-UHFFFAOYSA-N 0.000 claims description 9
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- NLSCHDZTHVNDCP-UHFFFAOYSA-N caesium nitrate Chemical compound [Cs+].[O-][N+]([O-])=O NLSCHDZTHVNDCP-UHFFFAOYSA-N 0.000 claims description 6
- 150000002611 lead compounds Chemical class 0.000 claims description 6
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 4
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims description 4
- VOWZMDUIGSNERP-UHFFFAOYSA-N carbamimidoyl iodide Chemical compound NC(I)=N VOWZMDUIGSNERP-UHFFFAOYSA-N 0.000 claims description 4
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims description 4
- 230000005693 optoelectronics Effects 0.000 claims description 4
- MFEVGQHCNVXMER-UHFFFAOYSA-L 1,3,2$l^{2}-dioxaplumbetan-4-one Chemical compound [Pb+2].[O-]C([O-])=O MFEVGQHCNVXMER-UHFFFAOYSA-L 0.000 claims description 3
- 229910000003 Lead carbonate Inorganic materials 0.000 claims description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 3
- PXXJHWLDUBFPOL-UHFFFAOYSA-N benzamidine Chemical compound NC(=N)C1=CC=CC=C1 PXXJHWLDUBFPOL-UHFFFAOYSA-N 0.000 claims description 3
- ZOAIGCHJWKDIPJ-UHFFFAOYSA-M caesium acetate Chemical compound [Cs+].CC([O-])=O ZOAIGCHJWKDIPJ-UHFFFAOYSA-M 0.000 claims description 3
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 3
- YPNWGLNCDBBKNX-UHFFFAOYSA-N carbamimidoyl bromide Chemical compound NC(Br)=N YPNWGLNCDBBKNX-UHFFFAOYSA-N 0.000 claims description 3
- RYTLGWCJESCDMY-UHFFFAOYSA-N carbamimidoyl chloride Chemical compound NC(Cl)=N RYTLGWCJESCDMY-UHFFFAOYSA-N 0.000 claims description 3
- 239000007772 electrode material Substances 0.000 claims description 3
- 229940046892 lead acetate Drugs 0.000 claims description 3
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 3
- VRNINGUKUJWZTH-UHFFFAOYSA-L lead(2+);dithiocyanate Chemical compound [Pb+2].[S-]C#N.[S-]C#N VRNINGUKUJWZTH-UHFFFAOYSA-L 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- FWTZHLAHNTZZGE-UHFFFAOYSA-N NC=[NH2+].[S-]C#N Chemical compound NC=[NH2+].[S-]C#N FWTZHLAHNTZZGE-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims 6
- 238000004519 manufacturing process Methods 0.000 claims 3
- 238000010549 co-Evaporation Methods 0.000 abstract description 8
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- 230000000052 comparative effect Effects 0.000 description 8
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 8
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
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- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
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- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
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- 150000005309 metal halides Chemical class 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XDXWNHPWWKGTKO-UHFFFAOYSA-N 207739-72-8 Chemical compound C1=CC(OC)=CC=C1N(C=1C=C2C3(C4=CC(=CC=C4C2=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC(=CC=C1C1=CC=C(C=C13)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)N(C=1C=CC(OC)=CC=1)C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 XDXWNHPWWKGTKO-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- JKSIBASBWOCEBD-UHFFFAOYSA-N N,N-bis(4-methoxyphenyl)-9,9'-spirobi[fluorene]-1-amine Chemical compound COc1ccc(cc1)N(c1ccc(OC)cc1)c1cccc2-c3ccccc3C3(c4ccccc4-c4ccccc34)c12 JKSIBASBWOCEBD-UHFFFAOYSA-N 0.000 description 1
- OAAKZKGKPMPJIF-UHFFFAOYSA-N [Cl].[I] Chemical compound [Cl].[I] OAAKZKGKPMPJIF-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- QXAITBQSYVNQDR-ZIOPAAQOSA-N amitraz Chemical compound C=1C=C(C)C=C(C)C=1/N=C/N(C)\C=N\C1=CC=C(C)C=C1C QXAITBQSYVNQDR-ZIOPAAQOSA-N 0.000 description 1
- 229960002587 amitraz Drugs 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 159000000006 cesium salts Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
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- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明属于钙钛矿技术领域,具体涉及一种无甲胺组分钙钛矿薄膜的制备方法及其应用。本发明提供的一种无甲胺组分钙钛矿薄膜的制备方法,采用蒸镀多元混合熔融盐制备前驱体薄膜,有效解决了传统多源共蒸铅盐薄膜工艺难以监控蒸镀速率,实验重复性差,实验复杂度高等诸多问题,更适用于工业化生产。将该无甲胺钙钛矿薄膜用在光电器件中,可以获得更高的光电转换效率。
Description
技术领域
本发明属于钙钛矿技术领域,具体涉及一种无甲胺组分钙钛矿薄膜的制备方法及其应用。
背景技术
金属卤化物有机无机杂化钙钛矿太阳能电池作为新一代的光伏发电技术,具有成本低、制备简单等优点,受到了学术界和产业界的广泛关注,其光电转化效率较高,有望打破传统硅电池市场。与传统硅电池相比,钙钛矿电池具有载流子寿命长、扩散距离长、直接带隙且带隙可调等优点。
金属卤化物有机无机杂化钙钛矿太阳能电池按照组分划分,可以分为甲胺体系钙钛矿电池与无甲胺体系钙钛矿电池。与含有甲胺的钙钛矿薄膜相比,无甲胺体系钙钛矿具有合适的带隙和更强的稳定性,是理想的光电、光伏材料。然而由于无甲胺体系钙钛矿结晶过程和薄膜形貌难以控制等原因,其光电转换效率明显落后于含有甲胺的钙钛矿太阳能电池。
发明内容
本发明是基于发明人对以下事实和问题的发现和认识做出的:
目前钙钛矿太阳能电池制备方法分为溶液法和真空蒸镀法两种。
溶液法包含溶液一步法和溶液两步法,是一种发展较为成熟的钙钛矿制备工艺。但是制备过程中需要使用溶剂,即增加了成本,同时残余溶剂会对环境造成污染,另外溶液旋涂工艺难以应用到大面积钙钛矿模组制备中,难以实现工业化生产。
真空蒸镀法包括一步蒸镀法和两部顺序蒸镀法。一步蒸镀法的缺点是碘化铅和铵盐饱和蒸汽压相差很大,同时控制碘化铅和铵盐保持合理的沉积速率非常困难,难以避免交叉污染的问题。
传统的两步蒸镀法蒸镀铅盐步骤采用的是多源共蒸工艺,该工艺的缺点是:①难以同时对多个蒸发源的蒸镀速率进行实时监控,因而难以确定实际蒸镀速率和蒸镀厚度;②部分物料的蒸发速率不稳定,控制多个源的蒸发速率保持稳定难度较大;③实验重复性较差,批次差异明显,易造成钙钛矿电池良品率低的问题;④实验拓展性较差,实验设备复杂度会随着蒸发物料种类的增加而显著提升。
现阶段真空蒸镀工艺虽然相较于溶液法易于控制膜厚、可在各种类型基底表面进行加工,与叠层太阳能电池加工工艺兼容、易移植用于大规模工业生产等诸多优势,但是还存在实验重复性差和多蒸发源共蒸难控制的问题需要解决。
本发明旨在至少在一定程度上解决相关技术中的技术问题之一。为此,本发明的实施例提出一种无甲胺组分钙钛矿薄膜的制备方法,该方法采用蒸镀多元混合熔融盐用于两步法制备前驱体薄膜,有效解决了传统多源共蒸铅盐薄膜工艺难以监控蒸镀速率、实验重复性差、复杂度高等诸多问题,该方法具有良好的可重复性和工业生产可行性。
本发明实施例的一种无甲胺组分钙钛矿薄膜的制备方法,其特征在于,包括以下步骤:
(1)制备混合熔融盐原料粉末;
(2)采用真空蒸镀法在基底表面沉积步骤(1)制得的混合熔融盐原料粉末,得到前驱体薄膜;
(3)采用真空蒸镀法在步骤(2)所得的前驱体薄膜表面沉积甲脒盐;
(4)进行退火处理得到所述无甲胺组分钙钛矿薄膜。
本发明实施例的无甲胺组分钙钛矿薄膜的制备方法带来的优点和技术效果,1、本发明实施例中,多元混合熔融盐蒸发是一个单源蒸镀过程,可以通过膜厚仪对蒸发速率和蒸发厚度进行监控,有效解决了传统的多源共蒸中速率难以控制的难题,并降低了实验复杂度;2、本发明实施例中,熔融盐是液体且具有良好的导热性和减低的粘度,因而蒸发速率非常稳定,便于控制,显著提升了实验的可重复性。
在一些实施例中,步骤(1)中,所述熔融盐原料包括铅或铅化合物、铯或铯化合物中的至少两种。
在一些实施例中,所述铅化合物包括碘化铅、氯化铅、醋酸铅、溴化铅、硝酸铅、硫氰酸铅或碳酸铅中的至少一种,所述铯化合物包括碘化铯、氯化铯、硝酸铯、溴化铯或醋酸铯中的至少一种。
在一些实施例中,步骤(2)中,所述真空蒸镀法的真空度小于1Pa,物料蒸发速度为0.01-500nm/s,蒸镀厚度为1-6000nm;步骤(3)中,所述真空蒸镀法中真空度小于1Pa,物料蒸发速度为0.01-1000nm/s,蒸镀厚度为1-6000nm;步骤(4)中,所述退火的温度为20-170℃,退火时长为1-600min。
在一些实施例中,步骤(3)中,所述甲脒盐包含碘甲脒、溴甲脒、氯甲脒、硫氰酸甲脒和苯甲脒中的至少一种。
本发明实施例还提供了一种采用上述无甲胺组分钙钛矿薄膜的制备方法制得的无甲胺组分钙钛矿薄膜。
本发明实施例还提供了一种无甲胺组分钙钛矿薄膜在光电器件中的应用。
在一些实施例中,所述光电器件包括钙钛矿太阳能电池、有机电致发光器件、光探测器、X射线探测器中的任意一种。
本发明实施例还提供了一种钙钛矿太阳能电池,包括上述的无甲胺组分钙钛矿薄膜。
在一些实施例中,所述钙钛矿太阳能电池包括玻璃基底层、导电玻璃层、电子传输层、钙钛矿薄膜层、空穴传输层和金属电极。
本发明实施例还提供了一种钙钛矿太阳能电池的制备方法,包括以下步骤:
(1)对导电基底进行超声清洗和臭氧处理;
(2)在经过步骤(1)处理后的导电基底上沉积电子传输层;
(3)在所述电子传输层上沉积前驱体薄膜;
(4)在所述前驱体薄膜上沉积甲脒盐并进行退火处理,得到无甲胺组分钙钛矿薄膜;
(5)在所述无甲胺组分钙钛矿薄膜上制备空穴传输层;
(6)在所述空穴传输层上沉积金属电极材料。
附图说明
图1是实施例1制备的钙钛矿太阳能电池的结构示意图;
图2是实施例1、实施例2和对比例1制备的钙钛矿太阳能电池的伏安特性曲线图;
图3是实施例1和对比例1制备的电池表面扫描电子显微镜(SEM)图。
具体实施方式
下面详细描述本发明的实施例,所述实施例的示例在附图中示出。下面通过参考附图描述的实施例是示例性的,旨在用于解释本发明,而不能理解为对本发明的限制。
本发明的实施例提供了一种无甲胺组分钙钛矿薄膜的制备方法,包括以下步骤:
(1)制备混合熔融盐原料粉末;
(2)采用真空蒸镀法在基底表面沉积步骤(1)制得的混合熔融盐原料粉末,得到前驱体薄膜;
(3)采用真空蒸镀法在步骤(2)所得的前驱体薄膜表面沉积甲脒盐;
(4)进行退火处理得到所述无甲胺组分钙钛矿薄膜。
本发明实施例的无甲胺组分钙钛矿薄膜的制备方法带来的优点和技术效果,多元混合熔融盐蒸发是一个单源蒸镀过程,可以通过膜厚仪对蒸发速率和蒸发厚度进行监控,有效解决了传统的多源共蒸中速率难以控制的难题,并降低了实验复杂度;熔融盐是液体且具有良好的导热性和较低的粘度,因而蒸发速率非常稳定,便于控制,显著提升了实验的可重复性。
在一些实施例中,优选地,步骤(1)中,所述熔融盐原料包括铅或铅化合物、铯或铯化合物中的至少两种。进一步优选地,所述铅化合物包括碘化铅、氯化铅、醋酸铅、溴化铅、硝酸铅、硫氰酸铅或碳酸铅中的至少一种,所述铯化合物包括碘化铯、氯化铯、硝酸铯、溴化铯或醋酸铯中的至少一种;所述熔融盐原料粉末的质量为0.01~10g。本发明实施例中,优选了熔融盐的原料及原料粉末的质量,可以获得更适合用于制备高效率光电器件的前驱体薄膜;制备的无甲胺组分钙钛矿薄膜质量更好,含有更少的缺陷,合适的用量能够使熔融盐原料粉末在真空蒸镀时受热更加均匀。本发明实施例中,可以采用多种物料进行混合,构成二元熔融盐、三元熔融盐、四元熔融盐等多种类型的熔融盐,可以采用两种或多种不同的铅盐构成二元熔融盐、三元熔融盐、四元熔融盐,也可以采用两种或多种不同的铯盐构成二元熔融盐、三元熔融盐、四元熔融盐,还可以采用铅盐与铯盐混合构成二元熔融盐、三元熔融盐、四元熔融盐,并且对熔融盐原料中各原料的比例没有特别限制,均可以适用于本发明的方法。
在一些实施例中,优选地,步骤(2)中,所述真空蒸镀法的真空度小于1Pa,物料蒸发速度为0.01-500nm/s,蒸镀厚度为1-6000nm;步骤(3)中,所述真空蒸镀法中真空度小于1Pa,物料蒸发速度为0.01-1000nm/s,蒸镀厚度为1-6000nm;步骤(4)中,所述退火的温度为20-170℃,退火时长为1-600min。进一步优选地,所述退火在相对湿度为10~80%的空气中、氮气手套箱中或气压为10-4-105Pa的真空腔体中进行。本发明实施例中,优选了真空蒸镀的条件,能够保证蒸镀的前驱体薄膜具有更好的均一性;采用真空蒸镀法在前驱体薄膜上蒸镀铵盐能够避免有机溶剂的使用,实验重复性较好,易于在工业化生产中的推广应用;优选了退火的条件,能够消除钙钛矿薄膜的残余应力,减少变形与裂纹倾向,同时能够细化钙钛矿薄膜的晶粒,调整组织,减少缺陷的形成。
在一些实施例中,优选地,步骤(3)中,所述甲脒盐包含碘甲脒、溴甲脒、氯甲脒、硫氰酸甲脒和苯甲脒中的至少一种。
本发明实施例还提供了一种采用上述的无甲胺组分钙钛矿薄膜的制备方法制备得到的无甲胺组分钙钛矿薄膜。本发明实施例中提供的无甲胺组分钙钛矿薄膜,采用上述方法制备得到,通过蒸镀多元混合熔融盐制备得到的无甲胺组分钙钛矿薄膜,具有均一性好、缺陷少的优点。
本发明实施例还提供了一种无甲胺组分钙钛矿薄膜在光电器件中的应用。
在一些实施例中,优选地,所述光电器件包括钙钛矿太阳能电池、有机电致发光器件、光探测器、X射线探测器中的任意一种。本发明实施例中,将无甲胺组分钙钛矿薄膜应用在光电器件中,能够使得该光电器件具有更高的光电转换效率。
本发明实施例还提供了一种钙钛矿太阳能电池,包括上述的无甲胺组分钙钛矿薄膜。本发明实施例的钙钛矿太阳能电池,使用上述的无甲胺组分钙钛矿薄膜,可以提高太阳能电池的光电转换效率。
在一些实施例中,优选地,所述钙钛矿太阳能电池包括玻璃基底层、导电玻璃层、电子传输层、钙钛矿薄膜层、空穴传输层和金属电极。
本发明实施例还提供了一种钙钛矿太阳能电池的制备方法,包括以下步骤:
(1)对导电基底进行超声清洗和臭氧处理;
(2)在经过步骤(1)处理后的导电基底上沉积电子传输层;
(3)在所述电子传输层上沉积前驱体薄膜;
(4)在所述前驱体薄膜上沉积甲脒盐并进行退火处理,得到无甲胺组分钙钛矿薄膜;
(5)在所述无甲胺组分钙钛矿薄膜上制备空穴传输层;
(6)在所述空穴传输层上沉积金属电极材料。
本发明实施例的钙钛矿太阳能电池的制备方法,工艺简单,成本低廉,可重复性强,便于在工业生产中的推广应用。
下面结合具体的实施例描述本发明的技术方案。
实施例1
(1)将氧化铟锡(ITO)导电玻璃用玻璃清洗液、去离子水、乙醇和异丙醇超声清洗后,吹干,用紫外-臭氧处理15min;
(2)将氧化锡胶体颗粒旋涂到干净的ITO基底上,旋涂速度为1000rpm,时间为30s,在150℃下退火30min;
(3)称量1g碘化铅、0.5g氯化铅粉末和0.5g碘化铯粉末,使用研钵研磨充分混合均匀得到混合熔融盐粉末;
(4)将经步骤(2)处理过的基底装入真空镀膜机中,将混合混合熔融盐粉末放入钨舟中,将钨舟放到真空镀膜机底部,抽真空至真空度小于10-2Pa,使用直流电源对钨舟通入直流电,钨舟在电流热效应作用下温度上升至400℃,达到熔融盐的共熔点后开始熔化挥发。使用石英晶振探头监测蒸发速率,通过调整加热功率,使物料蒸发速率控制在1nm/s,蒸镀厚度为400nm;
(5)将样品转移至另一腔体,蒸镀400nm的碘甲脒;蒸镀条件:将碘甲脒粉末放入钨舟中,将钨舟放到真空镀膜机底部,抽真空至真空度小于10-1Pa,使用直流电源对钨舟通入直流电,钨舟在电流热效应作用下温度上升,达到200℃开始挥发;使用石英晶振探头监测蒸发速率,通过调整加热功率,使物料蒸发速率控制在0.5nm/s,蒸镀厚度为350nm;
(6)2,2',7,7'-四[N,N-二(4-甲氧基苯基)氨基]-9,9'-螺二芴(Spiro-OMeTAD)用氯苯溶解后加入18μL的双三氟甲烷磺酰亚胺锂(Li-TFSI)(520mg/mL)和30μL的过氧化苯甲酰丁脂(t-BP)溶液增加导电性;采用旋涂法涂在钙钛矿的表面,旋涂速度4000rpm,旋涂时间30s,形成空穴传输层。
(7)蒸镀100nm的Au金属背电极。
实施例1制备的钙钛矿太阳能电池的结构如图1所示。
实施例2
制备方法与实施例1相同,不同之处仅在于:称量1.5g碘化铅和0.5g碘化铯粉末,使用研钵研磨充分混合均匀得到混合熔融盐粉末。
实施例3
制备方法与实施例1相同,不同之处仅在于:称量1g碘化铅,0.5g氯化铅,0.5g溴化铯粉末,使用研钵研磨充分混合均匀得到混合熔融盐粉末。
实施例4
制备方法与实施例1相同,不同之处仅在于:称量1g碘化铅,0.5g溴化铅,0.5g碘化铯粉末,使用研钵研磨充分混合均匀得到混合熔融盐粉末。
对比例1
制备方法与实施例1相同,不同之处仅在于:蒸镀钙钛矿前驱体薄膜环节,使用碘化铅、氯化铅、碘化铯三源共蒸方案,抽真空至10-2Pa后,依次开启加热碘化铯、氯化铅、碘化铅加热源,随后开启挡板,蒸镀厚度为400nm。
对实施例1、实施例2、实施例3、实施例4和对比例1制备得到的太阳能电池进行相关性能的测试。
(1)伏安特性曲线
J-V测试设备:太阳模拟器(Newport,Oriel AAA级),源表(Keithley 2400);在AM1.5G照明下,使用红外截止滤光片(KG-3,Newport)标准硅电池校准光强。J–V测量是在环境空气中进行的,扫描范围0V→1.2V,步长0.02V,扫描速度为0.2V/s。装置的测试面积由0.1cm2的掩膜确定。
图2是实施例1、实施例2、实施例3、实施例4和对比例1制备的钙钛矿太阳能电池的伏安特性曲线图;相关的数据列于表1中。
表1钙钛矿太阳能电池的性能
由上表可以看出与对比例1相比,实施例1制备的太阳能电池的器件效率有明显的提升,光电转化效率由17.01提升到22.49%,器件效率提升的主要因素为电流和填充因子的提升。可见熔融盐蒸发方案相比于传统多源共蒸方案可以获得更合适的碘氯比和铅铯比例。
(2)扫描电子显微镜(SEM)
扫描电子显微镜测试条件:使用日本SU8220冷场发射扫描电子显微镜,电子枪加速电压为5kV。
对实施例1、对比例1制备的太阳能电池的表面进行SEM扫描,结果如图3所示。与对比例1相比,实施例1制备的钙钛矿薄膜晶粒尺寸大,结晶度高,界面处有更小的缺陷密度晶粒。该结果表明,蒸镀多元混合熔融盐用于两步法制备钙钛矿薄膜更有优势。
在本发明中,术语“一个实施例”、“一些实施例”、“示例”、“具体示例”、或“一些示例”等意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中,对上述术语的示意性表述不必须针对的是相同的实施例或示例。而且,描述的具体特征、结构、材料或者特点可以在任一个或多个实施例或示例中以合适的方式结合。此外,在不相互矛盾的情况下,本领域的技术人员可以将本说明书中描述的不同实施例或示例以及不同实施例或示例的特征进行结合和组合。
尽管已经示出和描述了上述实施例,可以理解的是,上述实施例是示例性的,不能理解为对本发明的限制,本领域普通技术人员对上述实施例进行的变化、修改、替换和变型均在本发明的保护范围内。
Claims (11)
1.一种无甲胺组分钙钛矿薄膜的制备方法,其特征在于,包括以下步骤:
(1)制备混合熔融盐原料粉末;
(2)采用真空蒸镀法在基底表面沉积步骤(1)制得的混合熔融盐原料粉末,得到前驱体薄膜;
(3)采用真空蒸镀法在步骤(2)所得的前驱体薄膜表面沉积甲脒盐;
(4)进行退火处理得到所述无甲胺组分钙钛矿薄膜。
2.根据权利要求1所述的无甲胺组分钙钛矿薄膜的制备方法,其特征在于,步骤(1)中,所述熔融盐原料包含铅或铅化合物、铯或铯化合物中的至少两种。
3.根据权利要求2所述的无甲胺组分钙钛矿薄膜的制备方法,其特征在于,所述铅化合物包括碘化铅、氯化铅、醋酸铅、溴化铅、硝酸铅、硫氰酸铅或碳酸铅中的至少一种,所述铯化合物包括碘化铯、氯化铯、硝酸铯、溴化铯或醋酸铯中的至少一种。
4.根据权利要求1所述的无甲胺组分钙钛矿薄膜的制备方法,其特征在于,步骤(2)中,所述真空蒸镀法的真空度小于1Pa,物料蒸发速度为0.01-500nm/s,蒸镀厚度为1-6000nm;步骤(3)中,所述真空蒸镀法中真空度小于1Pa,物料蒸发速度为0.01-1000nm/s,蒸镀厚度为1-6000nm;步骤(4)中,所述退火的温度为20-170℃,退火时长为1-600min。
5.根据权利要求1或4所述的无甲胺组分钙钛矿薄膜的制备方法,其特征在于,步骤(3)中,所述甲脒盐包含碘甲脒、溴甲脒、氯甲脒、硫氰酸甲脒和苯甲脒中的至少一种。
6.一种权利要求1~5中任一项所述的无甲胺组分钙钛矿薄膜的制备方法制得的无甲胺组分钙钛矿薄膜。
7.一种权利要求6所述的无甲胺组分钙钛矿薄膜在光电器件中的应用。
8.根据权利要求7所述的无甲胺组分钙钛矿薄膜在光电器件中的应用,其特征在于,所述光电器件包括钙钛矿太阳能电池、有机电致发光器件、光探测器、X射线探测器中的任意一种。
9.一种钙钛矿太阳能电池,其特征在于,包括权利要求6所述的无甲胺组分钙钛矿薄膜。
10.根据权利要求9所述的钙钛矿太阳能电池,其特征在于,所述钙钛矿太阳能电池包括玻璃基底层、导电玻璃层、电子传输层、钙钛矿薄膜层、空穴传输层和金属电极。
11.一种权利要求9或10所述的钙钛矿太阳能电池的制备方法,其特征在于,包括以下步骤:
(1)对导电基底进行超声清洗和臭氧处理;
(2)在经过步骤(1)处理后的导电基底上沉积电子传输层;
(3)在所述电子传输层上沉积前驱体薄膜;
(4)在所述前驱体薄膜上沉积甲脒盐并进行退火处理,得到无甲胺组分钙钛矿薄膜;
(5)在所述无甲胺组分钙钛矿薄膜上制备空穴传输层;
(6)在所述空穴传输层上沉积金属电极材料。
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