CN113104890A - Cs (volatile organic Compounds)4CuSb2Cl12Layered halide double perovskite material and preparation method and application thereof - Google Patents
Cs (volatile organic Compounds)4CuSb2Cl12Layered halide double perovskite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a Cs4CuSb2Cl12The layered halide double perovskite material has the chemical formula as follows: cs4CuSb2Cl12. Including solution preparation and mechanical force preparation. The preparation method of the solution comprises the following steps: mixing a cesium-containing compound, an antimony-containing compound and a copper-containing compound in a proper mass ratio, and adding the mixture into a mixed solution of an organic solvent and an acidic solvent; carrying out ultrasonic treatment on the solution to obtain black precipitates, and separating the black precipitates through centrifugal treatment; washing the obtained black precipitate with acetone to obtain black Cs4CuSb2Cl12A layered halide double perovskite material. The mechanical force preparation method comprises the following steps: mixing a cesium-containing compound, an antimony-containing compound and a copper-containing compound in a proper mass ratio and putting the mixture into a mortar; grinding in a mortar to obtain a black product; scraping and collecting the powder and washing with acetoneTo obtain black Cs4CuSb2Cl12A layered halide double perovskite material. The material disclosed by the invention has good stability, is friendly to human bodies and environment, has a direct band gap of 1.77eV, is simple in preparation method, is suitable for industrial production, and has a wide application prospect in the photoelectric fields of photovoltaic cells, photodetectors, illumination, display, backlight sources and the like.
Description
Technical Field
The invention relates to the field of photoelectric materials, in particular to Cs4CuSb2Cl12Layered halide double perovskite material and a preparation method and application thereof.
Background
Halide perovskites can be a creditable star material based on the first report in 2009 by organic-inorganic lead-halogen perovskite solar cells, and the cell validation efficiency has reached 25.2% as short as a few years. Halide perovskites are highly distinctive in a plurality of photoelectron fields including photovoltaics, photoelectric detection, illumination, display, lasers, scintillators and the like because of the advantages of tunable wavelength, high light absorption coefficient, ultra-long carrier diffusion length and the like. In recent years, through the common efforts of scholars at home and abroad, perovskite materials have made great progress in controllable preparation, photoelectric property regulation and control, the photoelectron field and even the biological application. However, the conventional lead-based halogen perovskite lacks long-term stability and has toxicity to the environment and human body due to the lead ion, which is undoubtedly two problems that need to be solved most urgently in the commercial application of perovskite materials.
Recently, halide double perovskite structures have been proposed, this structure A2B'B"X6Formed by substituting a pair of non-toxic, aliovalent (i.e., monovalent and trivalent) metal cations for two toxic lead ions in the lattice, and this structure is non-lamellar. The halide double perovskite structure overcomes the defects of halide perovskite, and realizes a photoelectric material without toxicity and with good stability.
However, the existing halide double perovskite structure A2B'B"X6Due to non-laminated structure, the structure has the defects of low electronic dimension, indirect band gap, generally large band gap (larger than 3eV) and large effective carrier mass.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a non-toxic and stable layered halide double perovskite material with high electron dimension and a preparation method thereof, so as to solve the disadvantages of the traditional non-layered halide double perovskite material, such as a large indirect band gap, a large band gap (greater than 3eV), and a large effective mass of carriers.
The technical scheme adopted by the invention is as follows: a chemical formula of Cs4CuSb2Cl12The layered halide double perovskite material of (a).
Further, said one Cs4CuSb2Cl12The preparation method of the layered halide double perovskite material comprises a solution preparation method and a mechanical force preparation method, and the solution preparation method is characterized by comprising the following steps:
the method comprises the following steps: mixing a cesium-containing compound, an antimony-containing compound and a copper-containing compound in a proper mass ratio, and adding the mixture into a mixed solution of an organic solvent and an acidic solvent;
step two: carrying out ultrasonic treatment on the solution to obtain black precipitates, and separating the black precipitates through centrifugal treatment;
step three: washing the obtained black precipitate with acetone to obtain black Cs4CuSb2Cl12A layered halide double perovskite material.
The mechanical force preparation method is characterized by comprising the following steps:
the method comprises the following steps: mixing a cesium-containing compound, an antimony-containing compound and a copper-containing compound in a proper mass ratio and putting the mixture into a mortar;
step two: grinding in a mortar to obtain a black product;
step three: scraping the collected powder and washing with acetone to obtain black Cs4CuSb2Cl12A layered halide double perovskite material.
In the preparation method, the cesium-containing compound is cesium chloride and cesium carbonate, the antimony-containing compound is antimony chloride and antimony acetate, and the copper-containing compound is copper chloride dihydrate, copper chloride and copper acetate.
In the above preparation method, the organic solvent may be selected from water, formamide, trifluoroacetic acid, DMSO, acetonitrile, DMF, hexamethylphosphoramide, methanol, ethanol, acetic acid, isopropanol, pyridine, tetramethylethylenediamine, acetone, triethylamine, n-butanol, dioxane, tetrahydrofuran, methyl formate, tributylamine, methyl ethyl ketone, chloroform, ethyl acetate, trioctylamine, dimethyl carbonate, diethyl ether, isopropyl ether, n-butyl ether, trichloroethylene, diphenyl ether, dichloromethane, dichloroethane, benzene, toluene, carbon tetrachloride, carbon disulfide, cyclohexane, hexane, petroleum ether, trimethylchlorosilane, 1-octadecene, oleylamine, oleic acid, and the acidic solvent may be selected from hydrochloric acid, nitric acid, sulfuric acid.
In the above solution preparation method, the ultrasonic treatment may be replaced by stirring treatment or standing treatment.
In the mechanical force preparation method, the mortar can be made of ceramics, agate, glass, iron and alumina.
Compared with the prior art, the Cs of the invention4CuSb2Cl12The layered halide double perovskite material and the preparation method thereof have the advantages that:
1. compared with the traditional lead-based halide perovskite, the lead-free perovskite has toxicity, does not contain lead ions, has no toxicity, and is friendly to human bodies and environment;
2. compared with the characteristic that the traditional lead-based halide perovskite has poor stability under light, heat and humidity conditions, the lead-based halide perovskite has the characteristic of good light, heat and humidity stability;
3. compared with the defects of indirect band gap, generally larger band gap (larger than 3eV) and larger effective mass of a current carrier of the non-lamellar halide double perovskite, the direct band gap of the invention has the advantages of 1.77eV band gap, high conductivity and carrier mobility, and wide application prospect in the photoelectric fields of photovoltaic cells, photodetectors, illumination, display, backlight sources and the like;
4. the preparation process is simple, the production cost is low, and the industrial large-scale production is facilitated.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 shows Cs prepared according to the present invention4CuSb2Cl12SEM scanning electron microscope picture of the lamellar double perovskite;
FIG. 2 shows Cs prepared according to the present invention4CuSb2Cl12EDS energy spectra of layered double perovskites;
FIG. 3 shows Cs prepared according to the present invention4CuSb2Cl12An X-ray diffraction pattern (XRD pattern) of the layered double perovskite;
FIG. 4 shows Cs prepared according to the present invention4CuSb2Cl12Tauc plot of layered double perovskites;
Detailed Description
The following detailed description of the present disclosure is provided in conjunction with the accompanying drawings and the specific embodiments, which are set forth below and are not intended to limit the scope of the present disclosure.
Example 1 was carried out:
the method comprises the following steps: 0.6mmol CsCl and 0.5mmol SbCl3And 0.25mmol of CuCl2·2H2Mixing and adding the mixture into a mixed solution of 10ml of acetone, 0.1ml of deionized water and 2ml of hydrochloric acid;
here, the CsCl purity was 99.9%, SbCl3Has a purity of 99.9%, CuCl2·2H2The purity of O is analytically pure, the acetone is analytically pure, and the hydrochloric acid is analytically pure.
Step two: ultrasonically treating the solution for 30min to obtain black precipitate, and centrifuging at 5000rpm for 4min to separate out the black precipitate;
step three: washing the obtained black precipitate with acetone to obtain black Cs4CuSb2Cl12A layered halide double perovskite material.
FIG. 1 shows Cs produced by the production method of this example4CuSb2Cl12SEM scanning electron micrographs of the layered halide double perovskite material.
FIG. 2 shows Cs produced by the production method of this example4CuSb2Cl12EDS energy spectrum of layered halide double perovskite materialTo see that the chemical element ratio satisfies Cs4CuSb2Cl124:1:2: 12.
FIG. 3 shows Cs produced by the production method of this example4CuSb2Cl12X-ray diffraction pattern (XRD pattern) of the layered halide double perovskite material.
FIG. 4 shows Cs produced by the production method of this example4CuSb2Cl12Tauc plots diagram of layered halide double perovskite material, from which Cs can be seen4CuSb2Cl12The band gap of the double perovskite crystal is 1.77 eV.
While the present invention has been described with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, which are illustrative only and not restrictive, and various modifications which do not depart from the spirit of the present invention and which are intended to be covered by the claims of the present invention may be made by those skilled in the art.
Claims (9)
1. Cs (volatile organic Compounds)4CuSb2Cl12A layered halide double perovskite material, characterized in that the layered halide double perovskite has the chemical formula: cs4CuSb2Cl12。
2. A Cs according to claim 14CuSb2Cl12A layered halide double perovskite material, characterized in that the solution preparation method comprises the steps of:
the method comprises the following steps: mixing a cesium-containing compound, an antimony-containing compound and a copper-containing compound in a proper mass ratio, and adding the mixture into a mixed solution of an organic solvent and an acidic solvent;
step two: carrying out ultrasonic treatment on the solution to obtain black precipitates, and separating the black precipitates through centrifugal treatment;
step three: washing the obtained black precipitate with acetone to obtain black Cs4CuSb2Cl12A layered halide double perovskite material.
3. A Cs according to claim 14CuSb2Cl12The layered halide double perovskite material is characterized in that the mechanical force preparation method comprises the following steps:
the method comprises the following steps: mixing a cesium-containing compound, an antimony-containing compound and a copper-containing compound in a proper mass ratio and putting the mixture into a mortar;
step two: grinding in a mortar to obtain a black product;
step three: scraping the collected powder and washing with acetone to obtain black Cs4CuSb2Cl12A layered halide double perovskite material.
4. A Cs according to claims 2 and 34CuSb2Cl12The preparation method of the layered halide double perovskite material is characterized in that cesium-containing compounds are cesium chloride and cesium carbonate, antimony-containing compounds are antimony chloride and antimony acetate, and copper-containing compounds are copper chloride dihydrate, copper chloride and copper acetate.
5. A Cs according to claims 2 and 34CuSb2Cl12The preparation method of the layered halide double perovskite material is characterized in that the organic solvent can be selected from water, formamide, trifluoroacetic acid, DMSO, acetonitrile, DMF, hexamethylphosphoramide, methanol, ethanol, acetic acid, isopropanol, pyridine, tetramethylethylenediamine, acetone, triethylamine, n-butanol, dioxane, tetrahydrofuran, methyl formate, tributylamine, methyl ethyl ketone, chloroform, ethyl acetate, trioctylamine, dimethyl carbonate, diethyl ether, isopropyl ether, n-butyl ether, trichloroethylene, diphenyl ether, dichloromethane, dichloroethane, benzene, toluene, carbon tetrachloride, carbon disulfide, cyclohexane, hexane, petroleum ether, trimethylchlorosilane, 1-octadecene, oleylamine and oleic acid, and the acidic solvent can be selected from hydrochloric acid, nitric acid and sulfuric acid.
6. A Cs according to claim 24CuSb2Cl12The preparation method of the layered halide double perovskite material is characterized in that the ultrasonic treatment can be replaced by stirring treatment or standing treatment.
7. A Cs according to claim 34CuSb2Cl12The preparation method of the layered halide double perovskite material is characterized in that the mortar can be made of ceramics, agate, glass, iron and alumina.
8. A Cs according to claim 14CuSb2Cl12A layered halide double perovskite material, characterized in that the band gap width of the layered halide double perovskite material is between 0.9eV and 1.9 eV.
9. A Cs according to claim 14CuSb2Cl12The layered halide double perovskite material is characterized by being specifically applied to the photoelectric fields of photovoltaic cells, photodetectors, illumination, display and backlight sources.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115084471A (en) * | 2022-07-01 | 2022-09-20 | 昆明理工大学 | Layered halide double perovskite lithium ion battery cathode material and preparation method thereof |
| CN116212904A (en) * | 2023-02-23 | 2023-06-06 | 昆明理工大学 | Four perovskite photocatalytic material and application thereof |
| CN116554875A (en) * | 2023-05-15 | 2023-08-08 | 昆明理工大学 | Preparation method of rare earth ion doped layered double perovskite fluorescent material |
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2021
- 2021-03-22 CN CN202110300051.6A patent/CN113104890A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| AQEL MASHOT JAFAR等: ""Lead-free perovskite and double perovskite solar cells"", 《IOP CONFERENCE SERIES: MATERIALS SCIENCE AND ENGINEERING》 * |
| NANCY SINGHAL等: ""Low-Bandgap Cs4CuSb2Cl12 Layered Double Perovskite: Synthesis,Reversible Thermal Changes, and Magnetic Interaction"", 《CHEM. ASIAN J.》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115084471A (en) * | 2022-07-01 | 2022-09-20 | 昆明理工大学 | Layered halide double perovskite lithium ion battery cathode material and preparation method thereof |
| CN115084471B (en) * | 2022-07-01 | 2023-12-01 | 昆明理工大学 | Layered halide double perovskite lithium ion battery anode material and preparation method thereof |
| CN116212904A (en) * | 2023-02-23 | 2023-06-06 | 昆明理工大学 | Four perovskite photocatalytic material and application thereof |
| CN116212904B (en) * | 2023-02-23 | 2024-03-22 | 昆明理工大学 | Four perovskite photocatalytic material and application thereof |
| CN116554875A (en) * | 2023-05-15 | 2023-08-08 | 昆明理工大学 | Preparation method of rare earth ion doped layered double perovskite fluorescent material |
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Application publication date: 20210713 |