CN113697855B - Cu-doped double perovskite material and preparation method thereof - Google Patents
Cu-doped double perovskite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a Cu-doped double perovskite material and a preparation method thereof, wherein the chemical formula of the Cu-doped double perovskite material is Cs2(Ag1‑xBi1‑xCu2x)Br6，0＜x＜0.25。
Description
Technical Field
The invention relates to a Cu-doped double perovskite material and a preparation method thereof, in particular to a method for improving the light absorption performance of a metal halide double perovskite material by doping Cu, and belongs to the field of perovskite material preparation.
Background
The organic-inorganic hybrid perovskite material has unique photoelectric properties of high molar extinction coefficient, adjustable band gap, strong electron/hole transmission capability and the like, and has the advantages of low raw material cost, easy device processing and wide application prospect. Two major challenges facing the current further development of organic-inorganic hybrid perovskite photovoltaic materials are the intrinsic stability of the materials and the environmental friendliness of lead elements. The adoption of non-toxic/low-toxic elements to replace lead elements to construct environment-friendly stable lead-free perovskite is an important direction for future development in the field. A new method for obtaining lead-free perovskites using trivalent bismuth and monovalent silver instead of divalent lead was reported in 2016. Ag and Bi alternately occupy adjacent octahedral lattices to form Cs2AgBiBr6A double perovskite structure. The structure shows good stability to environmental factors such as light, heat, humidity and the like, has longer carrier life and excellent structural stability, and has potential application value. However, Cs2AgBiBr6The relatively weak light absorption capacity limits the further application of the optical fiber in photoelectric devices。
Therefore, the increase of the photon utilization rate through the regulation and control of the precise structure and the improvement of the light absorption performance of the material become the core problem of future photoelectric application.
Disclosure of Invention
Therefore, the invention aims to provide a Cu-doped double perovskite material and a preparation method thereof.
In one aspect, the invention provides a Cu-doped double perovskite material, wherein the chemical formula of the Cu-doped double perovskite material is Cs2(Ag1-xBi1-xCu2x)Br6X is more than 0 and less than 0.25. Preferably, 0.01. ltoreq. x.ltoreq.0.20, more preferably 0.02. ltoreq. x.ltoreq.0.15, and most preferably 0.05.
In the present disclosure, the Ag/Bi site is doped with a small amount of elements, and the electronic structure is controlled by the interaction between the Cu-3d orbital and the Bi-6s/Ag-4d, Bi-6p orbitals. Meanwhile, the high-efficiency light absorption is realized by combining the local defects generated after Cu atoms enter crystal lattices.
Preferably, the Cs2(Ag1-xBi1-xCu2x)Br6The grain size of the crystal grains is 45 to 200 μm.
Preferably, the Cs2(Ag1-xBi1-xCu2x)Br6The light absorption intensity in the wavelength range of 300-1000 nm is Cs2AgBiBr6Is significantly improved, i.e. the light absorption intensityCs2(Ag1-xBi1-xCu2x)Br6Light absorption intensityCs2AgBiBr6。
On the other hand, the invention also provides a preparation method of the Cu-doped double perovskite material, which comprises the following steps:
(1) CsBr, AgBr, BiBr3、CuBr2According to a molar ratio of 2: 1-x: 1-x: 2, adding the mixture into hydrobromic acid after mixing, and heating and stirring to obtain a precursor solution;
(2) and placing the obtained precursor solution into a reaction kettle, reacting at 100-200 ℃, cooling to room temperature, filtering, washing and drying to obtain the Cu-doped double perovskite material. Wherein, the x range is between 0 and 0.25, and pure phase Cs can be obtained2(Ag1-xBi1-xCu2x)Br6. x is too large, phase separation occurs in the product, and pure phase Cs cannot be obtained2(Ag1-xBi1-xCu2x)Br6Causing a decrease in light absorption performance.
Preferably, according to CsBr: AgBr: BiBr3：CuBr2The molar ratio is 2: 1-x: 1-x: 2x, Cs in the precursor solution2(Ag1-xBi1-xCu2x)Br6The concentration of (B) is 0.04-0.12M.
Preferably, in the step (1), the heating and stirring temperature is 80-120 ℃.
Preferably, in the step (2), the reaction time is 24 to 48 hours.
Has the advantages that:
in the invention, the use of copper atom pair Cs is innovatively proposed2AgBiBr6The method for regulating and controlling the electronic structure, the orbital hybridization and the defect state density so as to improve the light absorption property of the material has potential practical value for the application of photoelectric devices made of the material. In the present invention, Cs is obtained2(Ag1-xBi1-xCu2x)Br6Perovskite compared to Cs2AgBiBr6The light absorption intensity in the wavelength range of 300-1000 nm is obviously improved.
Drawings
FIG. 1 shows Cs2(Ag1-xBi1-xCu2x)Br6Comparative example 1Cs2AgBiBr6A picture of a perovskite crystal entity;
FIG. 2 shows Cs2(Ag1-xBi1-xCu2x)Br6Comparative example 1Cs2AgBiBr6Scanning electron micrographs of perovskite crystals;
FIG. 3 shows Cs2(Ag1-xBi1-xCu2x)Br6Comparative example 1Cs2AgBiBr6An X-ray diffraction pattern of the perovskite crystal;
FIG. 4 shows Cs2(Ag1-xBi1-xCu2x)Br6Comparative example 1Cs2AgBiBr6Calcium titaniumAbsorption spectrum of mineral crystal.
Detailed Description
The present invention is further illustrated by the following examples, which are to be understood as merely illustrative and not restrictive.
In the present disclosure, Cs is first doped with copper atoms (Cu)2AgBiBr6Double perovskite material to improve its light absorption properties. The chemical formula of the double perovskite material is Cs2(Ag1-xBi1-xCu2x)Br6Wherein 0 < x < 0.25, preferably 0 < x < 0.2. And, in Cs2AgBiBr6In the structure, Ag and Bi are respectively in +1 valence state and +3 valence state, the two valence states alternately occupy octahedral crystal lattices, the doping element of the invention is bivalent copper, and the doping type is Ag/Bi position co-doping.
In one embodiment of the present invention, the Cs is prepared by a hydrothermal method2(Ag1-xBi1-xCu2x)Br6The preparation method of the double perovskite material is simple, no specific organic solvent is required to be added, the specific cooling rate is not required to be controlled, and the obtained Cs2(Ag1-xBi1- xCu2x)Br6The grain size distribution of the crystal is uniform. Cs is exemplified below2(Ag1-xBi1-xCu2x)Br6A preparation method of a double perovskite material.
CsBr, AgBr, BiBr3、CuBr2The four precursors are as follows: 1-x: 1-x: adding 2x mol ratio (x is more than 0 and less than 0.25) into hydrobromic acid, heating and stirring to dissolve the hydrobromic acid to obtain a precursor solution. Wherein, Cs2(Ag1-xBi1-xCu2x)Br6The concentration of the precursor solution in hydrobromic acid can be 0.04-0.12M, and actually, all raw materials in the precursor solution are only dissolved in the hydrobromic acid and do not have Cs2(Ag1- xBi1-xCu2x)Br6And (4) generating. The temperature of heating and stirring (dissolving) is controlled to be 80-120 ℃, and the time can be controlled to be 2-4 hours. In the heating and stirring process, the precursor can be ensured to be completely dissolved so as to form transparent precursor solution.
And (3) quickly transferring the precursor solution to a polytetrafluoroethylene reaction kettle, heating and preserving heat for a plurality of times, and carrying out hydrothermal reaction: (2CsBr + (1-x) AgBr + (1-x) BiBr3+2xCuBr2→Cs2(Ag1-xBi1-xCu2x)Br6). Wherein the temperature of the hydrothermal reaction can be 100-200 ℃. The heat preservation time of the hydrothermal reaction can be 24-48 hours. The invention adopts an aqueous solution system (hydrobromic acid aqueous solution) and can prepare the Cs by a one-step hydrothermal mode2(Ag1-xBi1-xCu2x)Br6Crystal, and the crystal structure is uniform.
And taking out the reaction kettle, and naturally cooling to room temperature. Finally, taking out the reaction solution, filtering, washing and drying to obtain Cs2(Ag1-xBi1-xCu2x)Br6And (4) crystals. The filtered portion can be washed with water and an organic solvent, respectively. The drying mode can be vacuum drying.
In the present invention, Cs is obtained2(Ag1-xBi1-xCu2x)Br6The crystal grain size of the crystal is 45 to 200 μm. Comparative example Cs2AgBiBr6，Cs2(Ag1-xBi1-xCu2x)Br6The light absorption performance of the crystal is obviously improved within the wavelength range of 300-1000 nm.
The present invention will be described in detail by way of examples. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that certain insubstantial modifications and adaptations of the invention by those skilled in the art may be made in light of the above teachings. The specific process parameters and the like of the following examples are also merely one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
Example 1
(1) CsBr, AgBr, BiBr3、CuBr2According to the weight ratio of 2.00: 0.95: 0.95: 0.10 mol ratio is mixed and addedHeating and stirring the mixture for about 2 hours at the temperature of 110 ℃ in 15mL of hydrobromic acid to obtain a precursor solution with the concentration of 0.07M;
(2) quickly transferring the precursor solution into a polytetrafluoroethylene reaction kettle, and heating and preserving heat at 150 ℃ for 24 hours;
(3) and taking the reaction kettle out, and naturally cooling at room temperature. The reaction solution was taken out and filtered. Washing the filtered part with water and organic solvent, and vacuum drying to obtain Cs2(Ag0.95Bi0.95Cu0.10)Br6And (4) crystals.
Cs obtained in example 12(Ag0.95Bi0.95Cu0.10)Br6The picture of the crystal is shown in FIG. 1, and the comparative example is Cs2AgBiBr6Is an orange-red crystal, and Cs2(Ag0.95Bi0.95Cu0.10)Br6It is dark brown crystal.
Cs obtained in example 12(Ag0.95Bi0.95Cu0.10)Br6The crystal is subjected to a scanning electron microscope test (see figure 2), and the grain size distribution of the crystal is 45-150 mu m.
Cs obtained in example 12(Ag0.95Bi0.95Cu0.10)Br6The crystals were subjected to X-ray diffraction test (see FIG. 3), and the obtained Cs2(Ag0.95Bi0.95Cu0.10)Br6The material structure of the crystal still maintains Cs2AgBiBr6The cubic phase structure of the perovskite phase has a slightly reduced unit cell volume. Taking into account Cu2+The ionic radius is less than Ag+And Bi3+It was confirmed that Cu ions entered the crystal lattice.
The Cs obtained in this example 1 was analyzed by UV-visible and near-IR spectrophotometers2(Ag0.95Bi0.95Cu0.10)Br6The crystals were subjected to absorption spectrum test (see FIG. 4) with light absorption intensity in the wavelength range of 300 to 1000nm as compared with that of comparative example 1Cs2AgBiBr6Compared with the crystal, the crystal is improved by 1 time.
Example 2
(1) CsBr, AgBr, BiBr3、CuBr2According to the weight ratio of 2.00: 0.95: 0.95: mixing the materials according to a molar ratio of 0.10, adding the mixture into 20mL of hydrobromic acid, heating and stirring the mixture for about 2 hours at a temperature of 110 ℃, and obtaining a precursor solution with a concentration of 0.05M;
(2) quickly transferring the precursor solution into a polytetrafluoroethylene reaction kettle, and heating and preserving heat for 24 hours at 170 ℃;
(3) and taking the reaction kettle out, and naturally cooling at room temperature. The reaction solution was taken out and filtered. Washing the filtered part with water and organic solvent, and vacuum drying to obtain Cs2(Ag0.95Bi0.95Cu0.10)Br6And (4) crystals.
Cs obtained in example 22(Ag0.95Bi0.95Cu0.10)Br6The crystal size and properties were similar to those of example 1.
Example 3
(1) CsBr, AgBr, BiBr3、CuBr2According to the following ratio of 2.00: 0.90: 0.90: mixing at a molar ratio of 0.20, adding into 20mL of hydrobromic acid, heating and stirring at 115 ℃ for about 3 hours to obtain a precursor solution with a concentration of 0.07M;
(2) quickly transferring the precursor solution into a polytetrafluoroethylene reaction kettle, and heating and preserving heat for 36h at 150 ℃;
(3) and taking the reaction kettle out, and naturally cooling at room temperature. The reaction solution was taken out and filtered. Washing the filtered part with water and organic solvent, and vacuum drying to obtain Cs2(Ag0.90Bi0.90Cu0.20)Br6And (4) crystals.
Cs obtained in example 32(Ag0.90Bi0.90Cu0.20)Br6The crystal grain size distribution of the crystal is 50-200 μm (see figure 2), and the crystal structure maintains Cs2AgBiBr6Cubic phase structure of perovskite phase (see fig. 3). Light absorption intensity of comparative example 1Cs2AgBiBr6The crystal phase ratio was nearly 1-fold improved (see fig. 4).
Example 4
(1) CsBr, AgBr, BiBr3、CuBr2According to the following ratio of 2.00: 0.90: 0.90: mixing at 0.20 mol ratio, adding into 20mL hydrobromic acid, heating at 115 deg.CStirring for about 4 hours to obtain a precursor solution with the concentration of 0.10M;
(2) quickly transferring the precursor solution into a polytetrafluoroethylene reaction kettle, and heating and preserving heat for 36 hours at 180 ℃;
(3) and taking the reaction kettle out, and naturally cooling at room temperature. The reaction solution was taken out and filtered. Washing the filtered part with water and organic solvent, and vacuum drying to obtain Cs2(Ag0.90Bi0.90Cu0.20)Br6And (4) crystals.
Cs obtained in example 42(Ag0.90Bi0.90Cu0.20)Br6The crystal size and properties were similar to those of example 3.
Example 5
(1) CsBr, AgBr, BiBr3、CuBr2According to the following ratio of 2.00: 0.85: 0.85: mixing the materials according to a molar ratio of 0.30, adding the mixture into 20mL of hydrobromic acid, heating and stirring the mixture for about 3 hours at a temperature of 115 ℃ to obtain a precursor solution with a concentration of 0.05M;
(2) quickly transferring the precursor solution into a polytetrafluoroethylene reaction kettle, and heating and preserving heat for 36h at 150 ℃;
(3) and taking the reaction kettle out, and naturally cooling at room temperature. The reaction solution was taken out and filtered. Washing the filtered part with water and organic solvent, and vacuum drying to obtain Cs2(Ag0.85Bi0.85Cu0.30)Br6And (4) crystals.
Cs obtained in example 52(Ag0.85Bi0.85Cu0.30)Br6The crystal grain size distribution of the crystal is 50-200 μm (see FIG. 2), and the crystal structure maintains Cs2AgBiBr6Cubic phase structure of perovskite phase (see fig. 3). Light absorption intensity of comparative example 1Cs2AgBiBr6The crystal phase ratio is improved but is lower than Cs2(Ag0.95Bi0.95Cu0.10)Br6And Cs2(Ag0.90Bi0.90Cu0.20)Br6(see fig. 4).
Example 6
(1) CsBr, AgBr, BiBr3、CuBr2According to the weight ratio of 2.00:0.85: 0.85: mixing the materials according to a molar ratio of 0.30, adding the mixture into 20mL of hydrobromic acid, heating, stirring and dissolving the mixture for about 4 hours at 115 ℃ to obtain a precursor solution with a concentration of 0.08M;
(2) quickly transferring the precursor solution into a polytetrafluoroethylene reaction kettle, and heating and preserving heat for 36 hours at 180 ℃;
(3) and taking the reaction kettle out, and naturally cooling at room temperature. The reaction solution was taken out and filtered. Washing the filtered part with water and organic solvent, respectively, and vacuum drying to obtain Cs2(Ag0.85Bi0.85Cu0.30)Br6And (4) crystals.
Cs obtained in example 62(Ag0.85Bi0.85Cu0.30)Br6The crystal size and properties were similar to those of example 5.
Example 7
The preparation process of Cu-doped double perovskite material in this example 7 is as follows: x is 0.02. The light absorption intensity of the sample is equal to that of comparative example 1Cs2AgBiBr6The crystal phase ratio is improved to be lower than Cs2(Ag0.95Bi0.95Cu0.10)Br6(see fig. 4).
Comparative example 1
(1) CsBr, AgBr, BiBr3According to the following steps: 1: 1 mol ratio, adding the mixture into 15mL of hydrobromic acid, heating and stirring the mixture for about 2 hours at 110 ℃ to obtain a precursor solution with the concentration of 0.07M;
(2) quickly transferring the precursor solution into a polytetrafluoroethylene reaction kettle, and heating and preserving heat at 150 ℃ for 24 hours;
(3) and taking the reaction kettle out, and naturally cooling at room temperature. The reaction solution was taken out and filtered. Washing the filtered part with water and organic solvent, respectively, and vacuum drying to obtain Cs2AgBiBr6And (4) crystals.
Claims (8)
1. The Cu-doped double perovskite material is characterized in that the chemical formula of the Cu-doped double perovskite material is Cs2(Ag1-xBi1-xCu2x)Br6，0＜x＜0.25。
2. The Cu-doped double perovskite material of claim 1, wherein 0.01. ltoreq. x.ltoreq.0.20.
3. The Cu-doped double perovskite material of claim 1, wherein 0.02 ≦ x ≦ 0.15.
4. The Cu-doped double perovskite material of claim 1, wherein x = 0.05.
5. The Cu-doped double perovskite material of claim 1, wherein the Cs2(Ag1-xBi1-xCu2x)Br6The grain size of the crystal is 45 to 200 μm.
6. The Cu-doped double perovskite material of claim 1, wherein the Cs2(Ag1-xBi1-xCu2x)Br6The light absorption intensity is more than Cs within the wavelength range of 300-1000 nm2AgBiBr6。
7. A method for preparing a Cu-doped double perovskite material as defined in claim 1, comprising:
(1) CsBr, AgBr, BiBr3、CuBr2According to a molar ratio of 2: 1-x: 1-x: 2, adding the mixture into hydrobromic acid after mixing, and heating and stirring to obtain a precursor solution; the heating and stirring temperature is 80-120 ℃;
(2) and placing the obtained precursor solution into a reaction kettle, reacting at 100-200 ℃ for 24-48 hours, cooling to room temperature, filtering, washing and drying to obtain the Cu-doped double perovskite material.
8. The method according to claim 7, wherein Cs is present in the precursor solution2(Ag1-xBi1-xCu2x)Br6The concentration of (B) is 0.04-0.12M.
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| Phase Diagrams and Stability of Lead-Free Halide Double Perovskites Cs2BB " X-6: B = Sb and Bi, B " = Cu, Ag, and Au, and X = Cl, Br, and I;Filip, Marina R et al.;《JOURNAL OF PHYSICAL CHEMISTRY C》;20171128;158-170 * |
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