CN112064104A - Preparation method of high-luminous-purity two-dimensional perovskite single crystal - Google Patents
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Abstract
The invention discloses a preparation method of a two-dimensional perovskite single crystal with high luminous purity, which introduces a hydrothermal technology (BA) into a solution cooling method to prepare2PbI4And (3) single crystal. Because the temperature of each part in the hydrothermal kettle is uniform, the temperature difference between the inside and the outside of the crystal can be eliminated; (BA)2PbI4As the single crystal bears gas pressure in the growth process, the BA organic cations tend to be orderly arranged, the accumulation of the cations is avoided, and two-dimension (BA) is eliminated2PbI4The double photoluminescence phenomenon of the single crystal improves the luminous purity of the single crystal. The invention adopts a hydrothermal-assisted solution cooling method to prepare (BA)2PbI4The crystal is a lamellar single crystal. [ PbI ]6]4‑The structure of the octahedron is an orthorhombic crystal structure. Compared with the prior art (solution)Cooling method) (BA)2PbI4The luminescent purity of the crystal and the sample prepared by the method is obviously improved.
Description
Technical Field
The invention belongs to the technical field of luminescent materials, and particularly relates to a preparation method of a two-dimensional perovskite single crystal with high luminescent purity.
Background
The organic-inorganic hybrid two-dimensional metal halide perovskite material has the advantages of adjustable band gap, high stability and the like, has wide application prospect in the field of luminescent devices, and is a new material in the field of luminescent materials. The material having a single emission peak and a narrower half-value width of the emission peak has higher emission purity. The improvement of the preparation method of the luminescent material and the improvement of the luminescent purity of the two-dimensional perovskite material are important ways for realizing high-performance luminescent devices, and are important measures for promoting the application of novel display technologies and the development of industries.
At present, the method for preparing the organic-inorganic hybrid two-dimensional perovskite single crystal mainly comprises a solution cooling method, an anti-solvent method, a solution slow volatilization method and the like. The anti-solvent method can realize the low-temperature preparation of the two-dimensional perovskite single crystal, but the used anti-solvent is toluene, chlorobenzene, ether, ethyl acetate and the like, and the organic solvents are toxic and are not friendly to the environment. The slow solution volatilization method is difficult to control the volatilization rate of the solution, so that the prepared two-dimensional perovskite single crystal has low quality and small size. At present, a solution cooling method is mostly adopted for preparing high-quality and large-size two-dimensional perovskite single crystals. The solubility of the perovskite material in the corresponding acid solvent decreases with decreasing temperature, and thus crystal growth can be achieved using the solution cooling method. The preparation method is simple to operate and easy to realize, and the preparation of the high-quality large-size two-dimensional perovskite single crystal is realized with the assistance of the seed crystal.
However, there is a problem that it cannot be overcome in the process of preparing an organic-inorganic hybrid two-dimensional perovskite single crystal by a solution cooling method. Namely: due to temperatureThe temperature difference between the outside and the inside of the crystal gradually decreases, particularly when the crystal size is large, and the cations in the inside crystal generate a stacking effect due to the action of the microstress. The accumulation of cations brings about a strong electro-acoustic coupling, causing the photoluminescence inside the crystal to produce a stokes shift, resulting in a new luminescence at low energy. This dual luminescence phenomenon exists in (BA) prepared by solution cooling2PbBr4、(PEA) 2PbBr4、(OA)2PbBr4、(BA) 2PbI4、(HA)2PbI4And the like (see comparison document 1, American ocean, research on growth and performance of novel organic-inorganic composite crystalline materials of the leonardite, doctor's paper, university of Shandong, 2017; 2, Qin Du, Cheng Zhu, Zixi Yin, et al, Stacking Effects on Electron-photon Coupling in Layered Hybrid Perovskates via Micromicroscopy, ACS Nano 2020, 14, 5806-. Therefore, the two-dimensional perovskite single crystal prepared by the solution cooling method has double photoluminescence, particularly luminescence with wider half-peak width from the interior of the crystal, and brings serious influence on the luminescence purity of the material.
The prior art eliminates the double luminescence phenomenon of the two-dimensional perovskite single crystal by controlling the solution cooling rate (the slowest cooling rate is 0.5 ℃/hour) (reference 1) and the annealing treatment (reference 2). The results show that the effect of the method for controlling the cooling rate is not obvious, and the internal luminescence peak of the crystal does not disappear completely although the intensity is reduced. The annealing treatment can rearrange cations to eliminate the cation accumulation effect and the double-luminescence phenomenon, but the high temperature in the annealing process can cause the migration of halogen ions to cause the decomposition of the perovskite material, so that the component purity of the material is reduced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the preparation method of the two-dimensional perovskite single crystal with high luminous purity, and the luminous purity of the prepared sample is obviously improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a two-dimensional perovskite single crystal with high luminous purity comprises the following steps:
(1) dissolving lead oxide in a mixed solution of hydriodic acid and hypophosphorous acid, heating to 100 ℃ to obtain a transparent solution A, and preserving heat in a constant-temperature water tank;
(2) slowly adding n-butylamine into a hydriodic acid solution to obtain a transparent solution B;
(3) slowly adding the solution B in the step (2) into the solution A in the step (1) under magnetic stirring to obtain a transparent orange precursor solution;
(4) quickly transferring the precursor solution in the step (3) into a liner of a hydrothermal kettle preheated at 80 ℃, closing the hydrothermal kettle in time, placing the hydrothermal kettle in an oven, heating to 100 ℃, and preserving heat for 5 minutes; and naturally cooling the hydrothermal kettle, opening the hydrothermal kettle, and taking out orange (BA)2PbI4 sheet-shaped single crystals, namely the two-dimensional perovskite single crystals.
Further, the concentration of the solution A in the step (1) is 0.8-0.9 mol/L.
Further, the volume ratio of the hydriodic acid to the hypophosphorous acid in the mixed solution of the hydriodic acid and the hypophosphorous acid in the step (1) is 10: 1.7.
Further, the concentration of the solution B in the step (2) is 1.5-2.5 mol/L.
Further, the volume ratio of the solution B to the solution A in the step (2) is 1: 1.67-3.12.
Further, the filling degree of the precursor solution in the step (4) in the hydrothermal kettle is more than or equal to 80%.
The invention has the beneficial effects that: the invention introduces hydrothermal technology into solution cooling method to prepare (BA)2PbI4And (3) single crystal. Because the temperature of each part in the hydrothermal kettle is uniform, the temperature difference between the inside and the outside of the crystal can be eliminated; in addition, (BA)2PbI4The single crystal is grown byThe organic cations of BA tend to arrange in order under the pressure of the gas, thus avoiding the accumulation of cations and thus eliminating the two-dimensional (BA)2PbI4The double photoluminescence phenomenon of the single crystal improves the luminous purity of the single crystal. Thus, the present invention is prepared by a hydrothermal assisted solution cooling method (BA)2PbI4The crystal is a lamellar single crystal. [ PbI ]6]4-The structure of the octahedron is an orthorhombic crystal structure. Compared with the (BA) prepared by the prior art (solution cooling method)2PbI4The luminescent purity of the crystal and the sample prepared by the method is obviously improved. The technology can also be popularized and applied to the preparation of other two-dimensional perovskite single crystals.
Drawings
FIG. 1 shows (BA)2PbI4Photoluminescence spectra of the crystals. 10. 20, 40, 60 and 80 are respectively 10%, 20%, 40%, 60% and 80% solution fill (BA)2PbI4Crystal No. 0 is prepared by common solution cooling method (BA)2PbI4And (4) crystals.
FIG. 2 shows (BA)2PbI4Appearance of the crystal (sample No. 80), (a) is (BA)2PbI4The overall appearance of the single crystal, and (b) is an enlarged view of the corresponding region of the rectangular frame in the drawing (a).
FIG. 3 shows (BA)2PbI4XRD test results for crystal (sample No. 80).
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
The preparation method of the high-luminous-purity two-dimensional perovskite single crystal of the present example is as follows:
(1) 2.232 g of lead oxide (PbO) were dissolved in 10 ml of hydroiodic acid (HI) and 1.7 ml of hypophosphorous acid (H)3PO2) In the mixed solution of (2), heating to 100 deg.CAnd (4) keeping the temperature of the transparent solution in a constant-temperature water tank at the temperature of DEG C.
(2) 0.924 ml of n-butylamine was slowly added to 5ml of hydroiodic acid solution to give a clear solution.
(3) Slowly adding the transparent solution obtained in the step (2) into the solution obtained in the step (1) under magnetic stirring to obtain a transparent orange precursor solution.
(4) And (4) quickly transferring the perovskite precursor solution with the volume of 2.5 ml, 5ml, 10 ml, 15 ml and 20 ml in the step (3) into a liner of the hydrothermal kettle preheated at the temperature of 80 ℃, and closing the hydrothermal kettle in time. The filling degree of the 5 parts of solution in the hydrothermal kettle is 10%, 20%, 40%, 60% and 80%. The hydrothermal kettle is a stainless steel shell and a polytetrafluoroethylene inner container, and the capacity is 25 ml.
(5) And (3) placing the hydrothermal kettle in an oven, heating to 100 ℃, preserving heat for 5 minutes, naturally cooling the hydrothermal kettle, and cooling to room temperature for about two hours. Cooling rate was about 35 ℃/hr, hydrothermal kettle was opened and orange (BA) was taken out2PbI4The plate-like single crystal was washed with ether and dried.
Material performance test results:
the filling degree of the solution in the hydrothermal kettle is a key factor influencing the vapor pressure in the kettle at the same solvent and temperature. The higher the filling degree, the higher the vapor pressure. According to the technology, 2.5 ml, 5ml, 10 ml, 15 ml and 20 ml of perovskite precursor solution are respectively filled into a hydrothermal kettle with the capacity of 25ml, the filling degree of 5 parts of solution in the hydrothermal kettle is 10%, 20%, 40%, 60% and 80%, and prepared samples are respectively named as 10%, 20%, 40%, 60% and 80%. For comparison, prepared by common solution cooling method (BA)2PbI4The crystals were designated sample No. 0.
1. Photoluminescence performance
FIG. 1 (BA)2PbI4Photoluminescence spectra of the crystals. 10. 20, 40, 60 and 80 are respectively 10%, 20%, 40%, 60% and 80% solution fill (BA)2PbI4Crystal No. 0 is prepared by common solution cooling method (BA)2PbI4And (4) crystals.
Sample holderThe product has photoluminescence spectrum, and is prepared by solution cooling method (BA)2PbI4The single crystal sample (No. 0) has two luminescence peaks with wavelengths of 504nm and 526nm, and the result is basically consistent with the luminescence peak position of the sample prepared by the solution cooling method in the prior art (related to the background art). As the filling degree of the precursor solution in the hydrothermal reactor increases, No. 2, which has a lower energy and is derived from the interior of the crystal, emits light, and the intensity thereof gradually decreases until the filling degree reaches 80%, and the light emission peak disappears. The reason is probably that the temperature of all parts in the hydrothermal kettle is uniform, so that the temperature difference between the inside and the outside of the crystal is eliminated; in addition, (BA)2PbI4During the growth of the single crystal, BA cations are orderly arranged under the driving of pressure because of bearing vapor pressure caused by volatilization of a solution, so that the accumulation effect of the cations is avoided, and the (BA) is eliminated2PbI4Double photoluminescence phenomenon of single crystal. When the filling degree of the solution in the hydrothermal kettle is low, the vapor pressure above the solution is low, namely the pressure borne by the surface of the crystal is low, so that the accumulation of BA cations cannot be completely avoided, and the phenomenon of double photoluminescence cannot be completely eliminated.
In addition, when the solution filling degree reaches 40% or more, (BA)2PbI4The crystal No. 1 luminescence peak was slightly red-shifted, about 3nm, indicating that the band gap of the sample was narrowed, probably due to vapor pressure during the growth of the crystal [ PbI ]6]4-Octahedron compression, electron cloud density increase and band gap narrowing.
2. Material appearance morphology and composition testing
We performed appearance and composition analysis on sample number 80. Grown under these conditions (BA)2PbI4The single crystal is orange yellow in color, is flaky, has a maximum size of about 5 mm, and is a layered perovskite single crystal, as shown in fig. 2 (b). The appearance of the product is similar to that of (BA) prepared by a general solution method2PbI4The crystal samples did not differ significantly.
The composition analysis was performed on the plate-like single crystal of sample No. 80. The X-ray diffraction (XRD) test results showed [ PbI6 ] for sample No. 80]4-The octahedron is an orthorhombic system. As shown in fig. 3.
Thus, the technology employs a hydrothermal-assisted solution cooling method to prepare (BA)2PbI4The crystal is a lamellar single crystal. [ PbI ]6]4-The octahedral structure belongs to the orthorhombic system. Compared with the (BA) prepared by the prior art (solution cooling method)2PbI4The luminescent purity of the crystal and the sample prepared by the method is obviously improved. The invention can also be popularized and applied to the preparation of other two-dimensional perovskite single crystals.
Example 2
A preparation method of a two-dimensional perovskite single crystal with high luminous purity comprises the following steps:
(1) dissolving lead oxide in a mixed solution of hydriodic acid and hypophosphorous acid (the volume ratio of the hydriodic acid to the hypophosphorous acid is 10: 1.7), heating to 100 ℃ to obtain a transparent solution A, and preserving heat in a constant-temperature water tank, wherein the concentration of the solution A is 0.9 mol/L;
(2) slowly adding n-butylamine into a hydriodic acid solution to obtain a transparent solution B, wherein the concentration of the solution B is 1.5 mol/L;
(3) slowly adding the solution B in the step (2) into the solution A in the step (1) under magnetic stirring to obtain a transparent orange precursor solution, wherein the volume ratio of the solution B to the solution A is 1: 1.67;
(4) quickly transferring the precursor solution in the step (3) into a liner of a hydrothermal kettle preheated at 80 ℃, closing the hydrothermal kettle in time, putting the hydrothermal kettle in an oven, heating to 100 ℃, and keeping the temperature for 5 minutes, wherein the filling degree of the precursor solution in the hydrothermal kettle is more than or equal to 80%; and naturally cooling the hydrothermal kettle, opening the hydrothermal kettle, and taking out orange (BA)2PbI4 sheet-shaped single crystals, namely the two-dimensional perovskite single crystals.
Example 3
A preparation method of a two-dimensional perovskite single crystal with high luminous purity comprises the following steps:
(1) dissolving lead oxide in a mixed solution of hydriodic acid and hypophosphorous acid (the volume ratio of the hydriodic acid to the hypophosphorous acid is 10: 1.7), heating to 100 ℃ to obtain a transparent solution A, and preserving heat in a constant-temperature water tank, wherein the concentration of the solution A is 0.8 mol/L;
(2) slowly adding n-butylamine into a hydriodic acid solution to obtain a transparent solution B, wherein the concentration of the solution B is 2.5 mol/L;
(3) slowly adding the solution B in the step (2) into the solution A in the step (1) under magnetic stirring to obtain a transparent orange precursor solution, wherein the volume ratio of the solution B to the solution A is 1: 3.12;
(4) quickly transferring the precursor solution in the step (3) into a liner of a hydrothermal kettle preheated at 80 ℃, closing the hydrothermal kettle in time, putting the hydrothermal kettle in an oven, heating to 100 ℃, and keeping the temperature for 5 minutes, wherein the filling degree of the precursor solution in the hydrothermal kettle is more than or equal to 80%; and naturally cooling the hydrothermal kettle, opening the hydrothermal kettle, and taking out orange (BA)2PbI4 sheet-shaped single crystals, namely the two-dimensional perovskite single crystals.
Example 4
A preparation method of a two-dimensional perovskite single crystal with high luminous purity comprises the following steps:
(1) dissolving lead oxide in a mixed solution of hydriodic acid and hypophosphorous acid (the volume ratio of the hydriodic acid to the hypophosphorous acid is 10: 1.7), heating to 100 ℃ to obtain a transparent solution A, and preserving heat in a constant-temperature water tank, wherein the concentration of the solution A is 0.85 mol/L;
(2) slowly adding n-butylamine into a hydriodic acid solution to obtain a transparent solution B, wherein the concentration of the solution B is 2 mol/L;
(3) slowly adding the solution B in the step (2) into the solution A in the step (1) under magnetic stirring to obtain a transparent orange precursor solution, wherein the volume ratio of the solution B to the solution A is 1: 2;
(4) quickly transferring the precursor solution in the step (3) into a liner of a hydrothermal kettle preheated at 80 ℃, closing the hydrothermal kettle in time, putting the hydrothermal kettle in an oven, heating to 100 ℃, and keeping the temperature for 5 minutes, wherein the filling degree of the precursor solution in the hydrothermal kettle is more than or equal to 80%; and naturally cooling the hydrothermal kettle, opening the hydrothermal kettle, and taking out orange (BA)2PbI4 sheet-shaped single crystals, namely the two-dimensional perovskite single crystals.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A preparation method of a two-dimensional perovskite single crystal with high luminous purity is characterized by comprising the following steps:
(1) dissolving lead oxide in a mixed solution of hydriodic acid and hypophosphorous acid, heating to 100 ℃ to obtain a transparent solution A, and preserving heat in a constant-temperature water tank;
(2) slowly adding n-butylamine into a hydriodic acid solution to obtain a transparent solution B;
(3) slowly adding the solution B in the step (2) into the solution A in the step (1) under magnetic stirring to obtain a transparent orange precursor solution;
(4) quickly transferring the precursor solution in the step (3) into a liner of a hydrothermal kettle preheated at 80 ℃, closing the hydrothermal kettle in time, placing the hydrothermal kettle in an oven, heating to 100 ℃, and preserving heat for 5-10 minutes; and naturally cooling the hydrothermal kettle, opening the hydrothermal kettle, and taking out the product to obtain the two-dimensional perovskite monocrystal.
2. The method for producing a high-luminous-purity two-dimensional perovskite single crystal according to claim 1, characterized in that: the concentration of the solution A in the step (1) is 0.8-0.9M.
3. The method for producing a high-luminous-purity two-dimensional perovskite single crystal according to claim 1, characterized in that: in the step (1), the mass concentration of the hydriodic acid is 57%, the mass concentration of the hypophosphorous acid is 50%, and the volume ratio of the hydriodic acid to the hypophosphorous acid in the mixed solution is 10: 1.7.
4. The method for producing a high-luminous-purity two-dimensional perovskite single crystal according to claim 1, characterized in that: the concentration of the solution B in the step (2) is 1.5-2.5M.
5. The method for producing a high-luminous-purity two-dimensional perovskite single crystal according to claim 1, characterized in that: the volume ratio of the solution B to the solution A in the step (3) is 1: 1.67-3.12.
6. The method for producing a high-luminous-purity two-dimensional perovskite single crystal according to claim 1, characterized in that: the filling degree of the precursor solution in the step (4) in the hydrothermal kettle is more than or equal to 80%.
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