CN110190139A - A kind of preparation method and application of inorganic perovskite film - Google Patents
A kind of preparation method and application of inorganic perovskite film Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000010408 film Substances 0.000 claims abstract description 28
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229960003237 betaine Drugs 0.000 claims abstract description 20
- 239000002243 precursor Substances 0.000 claims abstract description 19
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims abstract description 18
- 239000010409 thin film Substances 0.000 claims abstract description 18
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 5
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 5
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 5
- 239000000758 substrate Substances 0.000 claims abstract description 5
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- -1 alkyl betaine Chemical compound 0.000 claims description 4
- 238000004528 spin coating Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 230000007547 defect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 8
- 238000001000 micrograph Methods 0.000 description 5
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 description 4
- 239000000460 chlorine Substances 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000000089 atomic force micrograph Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001450 anions Chemical group 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000012296 anti-solvent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- WEUCVIBPSSMHJG-UHFFFAOYSA-N calcium titanate Chemical compound [O-2].[O-2].[O-2].[Ca+2].[Ti+4] WEUCVIBPSSMHJG-UHFFFAOYSA-N 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N methyl monoether Natural products COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
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- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
- H10F77/00—Constructional details of devices covered by this subclass
- H10F77/30—Coatings
- H10F77/306—Coatings for devices having potential barriers
- H10F77/311—Coatings for devices having potential barriers for photovoltaic cells
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
本发明公开了一种无机钙钛矿薄膜的制备方法及其应用，所述制备方法包括如下步骤：(1)按通式(CsX)nPbX2的配比，在溶剂中加入CsX和PbX2，配置得到无机钙钛矿前驱体溶液，前驱体的质量浓度为50～150 mg/ml，其中，0.8＜n＜1.5，X为Br、I、Cl中的至少一种；(2)在步骤(1)得到的前驱体溶液中加入甜菜碱，以质量计，甜菜碱的用量为钙钛矿的0.5%～5%；(3)将步骤(2)得到的溶液在衬底上进行旋涂，退火，得到无机钙钛矿薄膜。该方法得到的无机钙钛矿薄膜致密平整，载流子缺陷较少，可应用于发光二极管、太阳能电池等光电器件。
The invention discloses a preparation method and application of an inorganic perovskite thin film. The preparation method comprises the following steps: (1) adding CsX and PbX 2 into a solvent according to the ratio of the general formula (CsX) n PbX 2 , the configuration obtains the inorganic perovskite precursor solution, the mass concentration of the precursor is 50～150 mg/ml, wherein, 0.8<n<1.5, X is at least one in Br, I, Cl; (2) in step (1) Betaine is added to the obtained precursor solution, and the amount of betaine is 0.5% to 5% of perovskite in terms of mass; (3) The solution obtained in step (2) is spin-coated on the substrate , and annealed to obtain an inorganic perovskite film. The inorganic perovskite thin film obtained by the method is dense and smooth, has fewer carrier defects, and can be applied to photoelectric devices such as light-emitting diodes and solar cells.
Description
技术领域technical field
本发明属于光电材料与半导体器件领域，涉及一种用于太阳能电池的无机钛矿薄膜，具体涉及一种利用甜菜碱辅助制备无机钙钛矿薄膜的方法。The invention belongs to the field of photoelectric materials and semiconductor devices, and relates to an inorganic titanium film used for solar cells, in particular to a method for assisting the preparation of an inorganic perovskite film by using betaine.
背景技术Background technique
钙钛矿材料是一类有着与钛酸钙（CaTiO3）相同晶体结构的材料，是 Gustav Rose在1839年发现，后来由俄罗斯矿物学家L. A. Perovski命名。钙钛矿材料结构式一般为ABX3，其中A和B是两种阳离子，X是阴离子。这种奇特的晶体结构让它具备了很多独特的理化性质，比如吸光性、电催化性等等，在化学、物理领域有不小的应用。钙钛矿大家族里现已包括了数百种物质，从导体、半导体到绝缘体，范围极为广泛，其中很多是人工合成的。太阳能电池中用到的钙钛矿（CH3NH3PbI3、CH3NH3PbBr3和CH3NH3PbCl3等）属于半导体，有良好的吸光性。全无机的钙钛矿材料的分子式为CsPbX3，其中Cs是铯，Pb是铅，X是碘（I）、氯（Cl）、溴（Br）中的一种。这种无机钙钛矿具有热稳定性好、易于制备等特点，在太阳能电池、发光二极管等领域中具有很大的应用前景和研究价值。Perovskite materials are a class of materials with the same crystal structure as calcium titanate (CaTiO3), discovered by Gustav Rose in 1839, and later named by Russian mineralogist LA Perovski. The structural formula of perovskite materials is generally ABX 3 , where A and B are two cations, and X is an anion. This peculiar crystal structure gives it many unique physical and chemical properties, such as light absorption, electrocatalysis, etc., and has many applications in the fields of chemistry and physics. The perovskite family now includes hundreds of substances, ranging from conductors, semiconductors to insulators, with a wide range, many of which are artificially synthesized. Perovskites (CH 3 NH 3 PbI 3 , CH 3 NH 3 PbBr 3 and CH 3 NH 3 PbCl 3 , etc. ) used in solar cells are semiconductors and have good light absorption. The molecular formula of the all-inorganic perovskite material is CsPbX 3 , wherein Cs is cesium, Pb is lead, and X is one of iodine (I), chlorine (Cl), and bromine (Br). This inorganic perovskite has the characteristics of good thermal stability and easy preparation, and has great application prospects and research value in the fields of solar cells and light-emitting diodes.
为改善成膜性，现有技术中，对有机无机杂化钙钛矿的制备进行了较多研究。例如，中国发明专利CN106159097A公开了一种改善钙钛矿薄膜质量的新方法，钙钛矿结构式为ABX 3，式中A 为CH3NH3、NH2-CH=NH2中的一种或两种的复合物，B 为Pb，X 为I、Br、Cl 中的一种或两种的复合物，主要步骤为：在一定温度下，将钙钛矿薄膜经有机胺气体或者有机胺溶液处理一定时间，来改善钙钛矿薄膜的质量。中国发明专利申请CN108922972A公开了一种钙钛矿薄膜，所述钙钛矿薄膜包括钙钛矿型ABX3有机-无机杂化材料和聚合物，所述聚合物由丙烯酸酯单体聚合得到。聚合物含有C＝O官能团和C＝C官能团，其中C＝O官能团可与钙钛矿晶界处的B离子(如Pb2+、Sn2+、Ge2+等)通过配位键发生弱相互作用，可以有效调节钙钛矿薄膜的生长。In order to improve the film-forming properties, in the prior art, much research has been done on the preparation of organic-inorganic hybrid perovskites. For example, Chinese invention patent CN106159097A discloses a new method for improving the quality of perovskite thin films. B is Pb, X is a compound of one or two of I, Br, and Cl. The main steps are: at a certain temperature, the perovskite film is treated with organic amine gas or organic amine solution. A certain period of time to improve the quality of perovskite thin films. Chinese invention patent application CN108922972A discloses a perovskite film, which includes a perovskite type ABX 3 organic-inorganic hybrid material and a polymer, and the polymer is obtained by polymerizing acrylate monomers. The polymer contains C=O functional groups and C=C functional groups, where the C=O functional groups can form weak bonds with B ions (such as Pb 2+ , Sn 2+ , Ge 2+ , etc.) at the grain boundaries of perovskites. The interaction can effectively regulate the growth of perovskite thin films.
而对于全无机的钙钛矿材料，采用例如在溶剂中添加二甲基亚砜或者乙醚等作为反溶剂，使钙钛矿材料快速从原溶剂中析出的方法制备的钙钛矿薄膜，在薄膜晶相、颗粒形貌及覆盖率等方面仍达不到所需效果，如何提升薄膜形貌质量仍然是当前研究的关键。For all-inorganic perovskite materials, the perovskite film prepared by adding dimethyl sulfoxide or ether as an anti-solvent to the solvent to quickly precipitate the perovskite material from the original solvent, in the film Crystal phase, particle morphology and coverage still cannot achieve the desired effect, how to improve the quality of thin film morphology is still the key to current research.
发明内容Contents of the invention
本发明的发明目的是提供一种无机钙钛矿薄膜的制备方法，以获得平整致密的薄膜。本发明的另一发明目的是提供采用该方法制备的薄膜的应用。The object of the present invention is to provide a method for preparing an inorganic perovskite film to obtain a flat and dense film. Another inventive object of the present invention is to provide the application of the film prepared by this method.
为达到上述发明目的，本发明采用的技术方案是：一种无机钙钛矿薄膜的制备方法，包括如下步骤：In order to achieve the above-mentioned purpose of the invention, the technical scheme adopted in the present invention is: a kind of preparation method of inorganic perovskite film, comprises the steps:
(1) 按通式 (CsX)nPbX2的配比，在溶剂中加入CsX和PbX2，配置得到无机钙钛矿前驱体溶液，前驱体的质量浓度为50～150 mg/ml，其中，0.8＜n＜1.5，X为Br、I、Cl中的至少一种；(1) According to the ratio of general formula (CsX) n PbX 2 , add CsX and PbX 2 to the solvent to prepare an inorganic perovskite precursor solution. The mass concentration of the precursor is 50-150 mg/ml, wherein, 0.8<n<1.5, X is at least one of Br, I, Cl;
(2) 在步骤(1)得到的前驱体溶液中加入甜菜碱，以质量计，甜菜碱的用量为钙钛矿的0.5%～5%；(2) Betaine is added to the precursor solution obtained in step (1), and the amount of betaine is 0.5% to 5% of the perovskite in terms of mass;
(3) 将步骤(2)得到的溶液在衬底上进行旋涂，退火，得到无机钙钛矿薄膜。(3) The solution obtained in step (2) is spin-coated on the substrate and annealed to obtain an inorganic perovskite film.
上述技术方案中，步骤(1)中，所述溶剂为DMF、DMSO中的一种或两种。In the above technical solution, in step (1), the solvent is one or both of DMF and DMSO.
上述技术方案中，步骤(2)中，所述甜菜碱选自烷基甜菜碱、硫代甜菜碱、烷基酰胺甜菜碱、磺丙基甜菜碱和磷酸脂甜菜碱中的一种或两种以上的混合物。In the above technical scheme, in step (2), the betaine is selected from one or both of alkyl betaines, thiobetaines, alkylamide betaines, sulfopropyl betaines and phospholipid betaines a mixture of the above.
步骤(3)中，旋涂的转速为2000～10000 rpm。In step (3), the rotational speed of the spin coating is 2000-10000 rpm.
优选地，1≤n≤1.4。Preferably, 1≤n≤1.4.
优选地，前驱体的质量浓度为90～150 mg/ml。Preferably, the mass concentration of the precursor is 90-150 mg/ml.
优选地，以质量计，甜菜碱的用量为钙钛矿的1%～2%。Preferably, in terms of mass, the amount of betaine is 1%-2% of perovskite.
采用上述制备方法得到的无机钙钛矿薄膜，可以应用于制备钙钛矿发光二极管的发光层或者太阳能电池的光吸收层。The inorganic perovskite film obtained by the above preparation method can be applied to prepare the light-emitting layer of a perovskite light-emitting diode or the light-absorbing layer of a solar cell.
由于上述技术方案运用，本发明与现有技术相比具有下列优点：Due to the use of the above-mentioned technical solutions, the present invention has the following advantages compared with the prior art:
1、本发明通过在前驱体溶液中引入甜菜碱，以甜菜碱起到表面活性剂的作用，极大地减少了钙钛矿晶粒的尺寸，有利于形成平整致密的薄膜。1. The present invention introduces betaine into the precursor solution, and uses betaine as a surfactant to greatly reduce the size of perovskite crystal grains, which is conducive to the formation of a flat and dense film.
2、本发明的方法制备工艺简单。2. The preparation process of the method of the present invention is simple.
附图说明Description of drawings
图1为本发明实施例一提供的CsPbBr3薄膜的扫描电镜图。FIG. 1 is a scanning electron microscope image of a CsPbBr 3 thin film provided in Example 1 of the present invention.
图2为前驱体溶液中未加入硫代甜菜碱所制备的CsPbBr3薄膜的扫描电镜图。Figure 2 is a scanning electron microscope image of a CsPbBr 3 film prepared without adding thiobetaine to the precursor solution.
图3为本发明实施例一提供的CsPbBr3薄膜的原子力显微镜图。FIG. 3 is an atomic force microscope image of the CsPbBr 3 thin film provided in Example 1 of the present invention.
图4为本发明实施例一提供的发光二极管的外量子效率随电压变化的函数曲线。FIG. 4 is a function curve of the external quantum efficiency of the light-emitting diode provided by Embodiment 1 of the present invention as a function of voltage.
图5为本发明实施例二提供的CsPbBr3薄膜的扫描电镜图。FIG. 5 is a scanning electron micrograph of the CsPbBr 3 thin film provided in Example 2 of the present invention.
具体实施方式Detailed ways
下面结合附图及实施例对本发明作进一步描述：The present invention will be further described below in conjunction with accompanying drawing and embodiment:
实施例一：一种甜菜碱辅助制备无机钙钛矿薄膜的方法，包括以下步骤：Embodiment one: a kind of betaine assists the method for preparing inorganic perovskite film, comprises the following steps:
(1) 配置无机钙钛矿前驱体溶液。按1：1的摩尔比向DMSO溶液中加入CsBr和PbBr2，前驱体的质量浓度为100 mg/ml。(1) Prepare the inorganic perovskite precursor solution. CsBr and PbBr 2 were added to the DMSO solution at a molar ratio of 1:1, and the mass concentration of the precursor was 100 mg/ml.
(2) 在步骤(1)得到的前驱体溶液中加入硫代甜菜碱，甜菜碱与钙钛矿的质量比为1.5%。(2) Add thiobetaine to the precursor solution obtained in step (1), and the mass ratio of betaine to perovskite is 1.5%.
(3) 将步骤(2)得到的溶液在衬底上进行旋涂，退火，得到CsPbBr3无机钙钛矿薄膜。(3) The solution obtained in step (2) is spin-coated on the substrate and annealed to obtain a CsPbBr 3 inorganic perovskite film.
获得的CsPbBr3薄膜的扫描电镜图如附图1所示。The scanning electron microscope image of the obtained CsPbBr 3 film is shown in Figure 1.
不加入硫代甜菜碱，采用同样的旋涂、退火方法制备薄膜作为对比例，得到的薄膜的扫描电镜图如附图2所示。Without adding thiobetaine, a thin film was prepared by the same method of spin coating and annealing as a comparative example, and the scanning electron microscope image of the obtained thin film is shown in Figure 2.
对比图1和图2可见，本发明实施例获得的薄膜更加的致密，覆盖率更高，晶粒尺寸更小。Comparing Fig. 1 and Fig. 2, it can be seen that the film obtained in the embodiment of the present invention is denser, has higher coverage and smaller grain size.
图3为本发明实施例提供的CsPbBr3薄膜的原子力显微镜图。从图中可以看出薄膜的表面较为光滑平整。Fig. 3 is an atomic force microscope image of a CsPbBr 3 thin film provided by an embodiment of the present invention. It can be seen from the figure that the surface of the film is relatively smooth.
将本实施例获得的上述CsPbBr3无机钙钛矿薄膜应用到ITO/Pvk/ CsPbBr3/TPBi/Liq/Al的光电器件结构中，制备发光二极管。图4为发光二极管的外量子效率随电压变化的函数曲线。可见，外量子效率达到2.3%。The above-mentioned CsPbBr 3 inorganic perovskite thin film obtained in this example was applied to a photoelectric device structure of ITO/Pvk/CsPbBr 3 /TPBi/Liq/Al to prepare a light emitting diode. Fig. 4 is a function curve of external quantum efficiency of a light emitting diode as a function of voltage. It can be seen that the external quantum efficiency reaches 2.3%.
实施例二：一种甜菜碱辅助制备无机钙钛矿薄膜的方法，包括以下步骤：Embodiment two: a kind of betaine assists the method for preparing inorganic perovskite film, comprises the following steps:
(1) 配置无机钙钛矿前驱体溶液。按1.4：1的摩尔比向DMSO溶液中加入CsBr和PbBr2，前驱体的质量浓度为140 mg/ml。(1) Prepare the inorganic perovskite precursor solution. CsBr and PbBr 2 were added to the DMSO solution at a molar ratio of 1.4:1, and the mass concentration of the precursor was 140 mg/ml.
(2) 在步骤(1)得到的前驱体溶液中加入硫代甜菜碱，甜菜碱与钙钛矿的质量比为5%。(2) Add thiobetaine to the precursor solution obtained in step (1), and the mass ratio of betaine to perovskite is 5%.
(3) 将步骤(2)得到的溶液在衬底上进行旋涂，退火，得到CsPbBr3无机钙钛矿薄膜。(3) The solution obtained in step (2) is spin-coated on the substrate and annealed to obtain a CsPbBr 3 inorganic perovskite film.
获得的CsPbBr3薄膜的扫描电镜图如附图5所示。可见，本发明实施例获得的薄膜致密平整，表面光滑。The scanning electron microscope image of the obtained CsPbBr 3 film is shown in Fig. 5 . It can be seen that the films obtained in the examples of the present invention are dense and smooth, with smooth surfaces.
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| CN111403547A (en) * | 2020-03-11 | 2020-07-10 | 武汉理工大学 | A kind of perovskite solar cell and preparation method thereof |
| CN111463355A (en) * | 2020-04-13 | 2020-07-28 | 苏州大学 | Blue-light perovskite film and application thereof |
| CN111733401A (en) * | 2020-06-18 | 2020-10-02 | 浙江大学 | A kind of preparation method of high thermal conductivity inorganic lead halide perovskite composite film |
| CN111733401B (en) * | 2020-06-18 | 2021-10-22 | 浙江大学 | A kind of preparation method of high thermal conductivity inorganic lead halide perovskite composite film |
| CN112038449A (en) * | 2020-08-27 | 2020-12-04 | 上海应用技术大学 | CsPbX prepared by solution spraying method3Film, its preparation and use |
| WO2023098926A3 (en) * | 2021-12-01 | 2023-07-20 | 浙江大学 | Perovskite material having stable bipolar molecules and optoelectronic device |
| US12150375B2 (en) | 2021-12-01 | 2024-11-19 | Zhejiang University | Dipolar molecule stabilized perovskite material and optoelectronic devices |
| CN115332450A (en) * | 2022-08-22 | 2022-11-11 | 亚洲硅业(青海)股份有限公司 | Perovskite thin film, preparation method thereof and perovskite battery |
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