CN108946808B - All-inorganic cesium-bismuth/antimony halide perovskite nanocrystal and preparation method thereof - Google Patents
All-inorganic cesium-bismuth/antimony halide perovskite nanocrystal and preparation method thereof Download PDFInfo
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Abstract
The invention provides an all-inorganic cesium-bismuth/antimony halide perovskite nanocrystalline and a preparation method thereof3M2X9Microcrystalline material, then adding Cs3M2X9Carrying out ultrasonic stripping on the microcrystalline material, and finally carrying out centrifugal purification to obtain Cs3M2X9And (4) nanocrystals. By optimizing the material components and the preparation process, the size of the nanocrystalline can be adjusted within the range of 2-100 nm. The method has simple and rapid operation and good reproducibility. Cs prepared by the method3M2X9The nano-crystalline has narrow size distribution and high stability, can be used for manufacturing photoelectric devices, and can be applied to the fields of solar cells, photoelectric detectors, photocatalysis, photoelectrocatalysis and the like.
Description
Technical Field
The invention belongs to the field of preparation of novel inorganic nano materials, and particularly relates to all-inorganic Cs3M2X9Perovskite nanocrystalline and preparation method thereof.
Background
Based on APbX3(A：Cs、CH3NH3(MA); x: lead-based perovskite nanocrystals of Cl, Br, I) have the advantages of large absorption cross section, high fluorescence quantum efficiency, tunable luminescence over the entire ultraviolet/visible light range, and the like, and have attracted much attention in recent years. However, the perovskite nanocrystals contain lead, a toxic element, which greatly limits the development of the perovskite nanocrystals, and in addition, the perovskite nanocrystals have relatively poor stability. Therefore, the synthesis of perovskite nanocrystals with low toxicity and high stability becomes a current research hotspot. Bismuth-or antimony-based perovskite phase materials have been reported in recent years to suffer from certain properties due to their lower toxicity and higher stability than lead-based perovskitesAttention is paid to. But relatively little research has been directed to bismuth or antimony-based perovskite nanocrystals. The existing method for synthesizing the perovskite nano-crystal mainly focuses on a solvent-resistant method and a thermal injection method, and has the disadvantages of complex operation, harsh reaction conditions and relatively poor reproducibility.
Disclosure of Invention
Based on the method, the invention provides a preparation method of the all-inorganic cesium-bismuth/antimony halide perovskite nanocrystal, and the method is simple, convenient and quick to operate and good in reproducibility.
The preparation method of the all-inorganic cesium-bismuth/antimony halide perovskite nanocrystal comprises the following steps:
s1: preparation of Cs3M2X9Microcrystalline material
Preparing Cs by wet method or solid phase synthesis method3M2X9A microcrystalline material.
S2: preparation of Cs3M2X9Nanocrystal
Mixing Cs3M2X9Dispersing the microcrystalline material into an organic solvent, then carrying out ultrasonic stripping, and finally obtaining Cs in the supernatant through centrifugal purification3M2X9And (4) nanocrystals.
Wherein, M is trivalent metal, and X is one or more of Cl, Br and I.
Compared with the prior art, the preparation method of the invention uses Cs3M2X9The microcrystal material is ultrasonically stripped, and Cs with narrow size distribution, low defect density, no toxic Pb element and high stability can be synthesized3M2X9The all-inorganic perovskite nanocrystalline is simple, convenient and quick to operate and good in reproducibility.
Further, M is one or two of Bi and Sb.
Further, in step S1, the wet method is to dissolve the halide metal salt, carbonate or metal oxide containing M element and the cesium-containing raw material in a solvent respectively to obtain two precursor solutions; the two precursor solutions are quickly mixed, stirred to obtain a large amount of precipitate, and the precipitate is dried to obtain Cs3M2X9A microcrystalline material.
Furthermore, the solvent in the wet synthesis is one or a mixture of several of ethanol, methanol, DMF, DMSO, acetonitrile, water, halogen acid and the like.
Further, the solid-phase synthesis method in step S1 is a method in which a halide metal salt containing M element is solid-phase stirred with CsX at room temperature or sintered at 800 ℃ or lower to obtain Cs3M2X9A microcrystalline material.
Further, a dispersant may be added to the organic solvent in step S2.
Further, the organic solvent is one or a mixture of halogenated alkane, aromatic hydrocarbon, alcohol, lipid, aldehyde and organic acid. The organic solvent can well disperse Cs3M2X9Microcrystalline material without the combination of Cs3M2X9The microcrystalline material reacts, changing its structure.
Further, the dispersing agent is one or a mixture of a plurality of solvents such as oleic acid, propionic acid and the like. The use of the dispersing agent can reduce the agglomeration of the nanocrystalline and improve the dispersing performance.
Cs prepared according to the above method3M2X9The nanocrystalline can be used for manufacturing photoelectric devices, and can be applied to the fields of solar cells, photoelectric detectors, photocatalysis, photoelectrocatalysis and the like.
Drawings
FIG. 1 shows Cs3Bi2Cl9XRD pattern of microcrystalline material;
FIG. 2 shows Cs3Bi2Cl9SEM images of microcrystalline material;
FIG. 3 shows Cs3Bi2Cl9A TEM image of the nanocrystal;
FIG. 4 shows Cs3Bi2Br9XRD pattern of microcrystalline material;
FIG. 5 shows Cs3Bi2Br9SEM images of microcrystalline material;
FIG. 6 shows Cs3Bi2Br9A TEM image of the nanocrystal;
FIG. 7 shows Cs3Bi2I9XRD pattern of microcrystalline material;
FIG. 8 shows Cs3Bi2I9SEM images of microcrystalline material;
FIG. 9 shows Cs3Bi2I9A TEM image of the nanocrystal;
FIG. 10 shows Cs3Bi2I9XRD pattern of nanocrystals;
FIG. 11 shows Cs3Sb2I9XRD pattern of microcrystalline material;
FIG. 12 shows Cs3Sb2I9SEM images of microcrystalline material;
FIG. 13 shows Cs3Sb2I9TEM images of the nanocrystals.
Detailed Description
The invention uses an ultrasonic stripping method to prepare Cs3M2X9The nanocrystalline can synthesize the Cs with narrow size distribution and high stability and can be used for manufacturing optoelectronic devices3M2X9The full inorganic perovskite nanocrystalline is simple, convenient and quick to operate and good in reproducibility. The technical solution of the present invention is described in detail below with reference to the accompanying drawings by way of specific embodiments.
Example 1
S1-1: preparation of Cs3Bi2Cl9Microcrystalline material
3mmol CsCl and 2mmol BiCl3Grinding at normal temperature after mixing to obtain Cs3Bi2Cl9A microcrystalline material.
S2-1: preparation of Cs3Bi2Cl9Nanocrystal
0.2g of Cs is taken3Bi2Cl9The microcrystalline material was dispersed in 20mL chloroform and sonicated at 300W sonication power for 20 minutes (4 seconds sonication, 4 second intervals). After low-speed centrifugation at 500rpm, the lower pellet was discarded. Then centrifuging the supernatant at 3000rpm, discarding the precipitate to obtain Cs in the supernatant3Bi2Cl9And (4) nanocrystals.
Please refer to fig. 1, which illustrates a schematic diagram of a systemCs3Bi2Cl9XRD pattern of microcrystal material, Cs prepared by said invention3Bi2Cl9Characteristic diffraction peak of (A) and ICSD #2067Cs3Bi2Cl9The perfect coincidence of the card information proves that pure Cs is obtained3Bi2Cl9. Please refer to FIG. 2, which shows Cs3Bi2Cl9SEM image of microcrystalline material. FIG. 2 shows that Cs prepared by the present invention3Bi2Cl9The crystallite material size is mainly distributed between 2 and 8 mu m.
Please refer to fig. 3, which shows Cs3Bi2Cl9TEM images of the nanocrystals. FIG. 3 shows Cs prepared by the present invention3Bi2Cl9The size of the nano crystal is mainly distributed between 20 nm and 70 nm.
Example 2
S1-2: preparation of Cs3Bi2Br9Microcrystalline material
1.5mmol of Cs2CO3，2mmol BiBr3Respectively dissolved in 10mL of hydrobromic acid, and stirred for 1 hour at 100 ℃ to be fully dissolved to obtain two precursor solutions. Quickly mixing the two precursor solutions at normal temperature, filtering to obtain a large amount of precipitate, and drying the precipitate in a drying oven to obtain Cs3Bi2Br9A microcrystalline material.
S2-2: preparation of Cs3Bi2Br9Nanocrystal
0.2g of Cs is taken3Bi2Br9The microcrystalline material was dispersed in 20mL chloroform and sonicated at 300W sonication power for 20 minutes (4 seconds sonication, 4 second intervals). Centrifuging at 500rpm, discarding the lower precipitate, and collecting Cs in the supernatant3Bi2Br9And (4) nanocrystals.
Referring to FIG. 4, Cs is shown3Bi2Br9XRD pattern of microcrystal material, Cs prepared by said invention3Bi2Br9Characteristic diffraction peak of (1) and ICSD #1142Cs3Bi2Br9The card information is matched, and the pure Cs is proved to be obtained3Bi2Br9. Please refer to FIG. 5, which shows Cs3Bi2Br9SEM image of microcrystalline material. FIG. 5 shows Cs prepared according to the present invention3Bi2Br9The crystallite material size is mainly distributed between 2 and 7 mu m.
Referring to FIG. 6, Cs is shown3Bi2Br9TEM images of the nanocrystals. FIG. 6 shows Cs prepared according to the present invention3Bi2Br9The nanocrystal size is mainly distributed between 2-5 nm.
Example 3
S1-3: preparation of Cs3Bi2I9Microcrystalline material
Adding 3mmol CsI and 2mmol BiI3Respectively dissolved in 10mL of hydroiodic acid, and stirred for 1 hour at 100 ℃ to fully dissolve the hydroiodic acid to obtain two precursor solutions. Quickly mixing the two precursor solutions at normal temperature, filtering to obtain a large amount of precipitate, and drying the precipitate in a drying oven to obtain Cs3Bi2I9A microcrystalline material.
S2-3: preparation of Cs3Bi2I9Nanocrystal
0.2g of Cs is taken3Bi2I9The microcrystalline material was dispersed in 20mL chloroform and sonicated at 300W sonication power for 20 minutes (4 seconds sonication, 4 second intervals). Then centrifuging at low speed of 500rpm, discarding the bottom precipitate, and obtaining Cs in the supernatant3Bi2I9And (4) nanocrystals.
Referring to FIG. 7, Cs is shown3Bi2I9XRD pattern of microcrystal material, Cs prepared by said invention3Bi2I9Characteristic diffraction peak and PDF #23-0847Cs3Bi2I9The card information is matched, and the pure Cs is proved to be obtained3Bi2I9. Please refer to FIG. 8, which shows Cs3Bi2I9SEM image of microcrystalline material. FIG. 8 shows Cs prepared by the present invention3Bi2I9The microcrystalline material has 2-5 μm domain and about 500nm thickness.
Please refer to FIG. 9And FIG. 10, the present invention produces Cs of relatively pure structure3Bi2I9Nanocrystalline and of size about 13 nm.
Example 4
S1-4: preparation of Cs3Sb2I9Microcrystalline material
3mmol CsI, 1mmol Sb2O3Respectively dissolved in 10mL of hydroiodic acid, and stirred for 1 hour at 100 ℃ to fully dissolve the hydroiodic acid to obtain two precursor solutions. Quickly mixing the two precursor solutions at normal temperature, filtering to obtain a large amount of precipitate, and drying the precipitate in a drying oven to obtain Cs3Sb2I9A microcrystalline material.
S2-4: preparation of Cs3Sb2I9Nanocrystal
0.2g of Cs is taken3Sb2I9The microcrystalline material was dispersed in 20mL chloroform and sonicated at 300W sonication power for 20 minutes (4 seconds sonication, 4 second intervals). Then centrifuging at low speed of 500rpm, discarding the bottom precipitate, and obtaining Cs in the supernatant3Sb2I9And (4) nanocrystals.
Please refer to fig. 11, which shows Cs3Sb2I9XRD pattern of microcrystal material, Cs prepared by said invention3Sb2I9Characteristic diffraction peak of (A) and ICSD #300002Cs3Sb2I9The card information is matched, and the pure Cs is proved to be obtained3Sb2I9. Please refer to FIG. 12, which shows Cs3Sb2I9SEM image of microcrystalline material. FIG. 12 shows Cs prepared according to the present invention3Sb2I9The microcrystalline material has a domain of 1-5 μm and a thickness of about 500 nm. Referring to FIG. 13, Cs prepared by the present invention3Sb2I9The size of the nano crystal is 12-30 nm.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (3)
1. A preparation method of all-inorganic cesium-bismuth/antimony halide perovskite nanocrystals comprises the following steps:
s1: preparation of Cs3M2X9Microcrystalline material
Preparing Cs by wet method or solid phase synthesis method3M2X9A microcrystalline material;
the wet method comprises the steps of respectively dissolving halide metal salt, carbonate or metal oxide containing M element and cesium-containing raw materials in a solvent to obtain two precursor solutions; fully mixing the two precursor solutions to obtain a large amount of precipitate, and drying the precipitate to obtain Cs3M2X9A microcrystalline material;
the solid phase synthesis method is to mix the halide metal salt containing M element with CsX solid phase at normal temperature or sinter at 800 deg.C to obtain Cs3M2X9A microcrystalline material;
s2: preparation of Cs3M2X9Nanocrystal
Mixing Cs3M2X9Dispersing the microcrystalline material into an organic solvent, then carrying out ultrasonic stripping, and finally obtaining Cs in the supernatant through centrifugal purification3M2X9A nanocrystal;
wherein, M is trivalent metal, and X is one or more of Cl, Br and I.
2. The method of claim 1, wherein: and M is one or the mixture of Bi and Sb.
3. The method of claim 1, wherein: the organic solvent is one or a mixture of halogenated alkane, aromatic hydrocarbon, alcohol, lipid, aldehyde and organic acid.
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| CN110482596B (en) * | 2019-07-23 | 2022-07-08 | 中国计量大学 | Preparation method of double lanthanide ion co-doped bismuth titanate nanosheet |
| CN112798545B (en) * | 2019-11-13 | 2022-03-29 | 中国科学院大连化学物理研究所 | Inorganic perovskite material with continuously adjustable absorption spectrum and preparation and application thereof |
| CN110937623B (en) * | 2019-12-03 | 2021-05-14 | 吉林大学 | Simple synthetic CsAgCl2Method for pure-phase inorganic non-lead perovskite |
| CN111790408B (en) * | 2020-07-20 | 2021-05-28 | 山东大学 | Bismuth/antimony-based perovskite, photocatalytic material, and preparation method and application thereof |
| CN112774719B (en) * | 2021-01-22 | 2023-08-04 | 暨南大学 | Limited domain inorganic perovskite Cs 3 Bi 2 Br 9 Photocatalytic film and preparation method and application thereof |
| CN113134376B (en) * | 2021-04-19 | 2023-01-31 | 铜陵博雅渡业新材料科技有限公司 | Cs 3 Bi 2 Cl 9 (PQDs) supported nanosheet self-assembled bismuthyl carbonate microsphere visible-light-driven photocatalyst and preparation method thereof |
| CN114437722B (en) * | 2022-01-27 | 2023-05-16 | 江西理工大学 | Rare earth based perovskite CsTmCl 3 Microcrystalline material and preparation method and application thereof |
| CN114560500B (en) * | 2022-02-18 | 2024-04-09 | 河北工业大学 | Leadless perovskite material and preparation method and application thereof |
| CN114590836B (en) * | 2022-03-08 | 2023-04-21 | 中国科学技术大学 | Lead-free halide perovskite nanocrystalline, liquid phase synthesis method thereof and application thereof in photoelectric detector |
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| CN106082329A (en) * | 2016-06-12 | 2016-11-09 | 上海科技大学 | A kind of containing bismuth and the semi-conducting material of halogen and preparation thereof and the method for analysis |
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| CN106082329A (en) * | 2016-06-12 | 2016-11-09 | 上海科技大学 | A kind of containing bismuth and the semi-conducting material of halogen and preparation thereof and the method for analysis |
Non-Patent Citations (2)
| Title |
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| Synthesis and Optical Properties of Colloidal M3Bi2I9 (M = Cs, Rb)Perovskite Nanocrystals;Jaya Pal等;《J. Phys. Chem. C.》;20180423;第10643-10649页 * |
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