CN113106535B - Preparation method of two-dimensional perovskite single crystal - Google Patents
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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- C30B7/06—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using non-aqueous solvents
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Abstract
The invention discloses a preparation method of a two-dimensional perovskite single crystal, which utilizes a liquid level limiting method to grow the single crystal, the growth of the single crystal in the thickness direction can be inhibited by the thickness of a precursor solvent layer, the growth of the crystal in other directions is not influenced while the liquid level in the thickness direction is limited, and the large-size perovskite single crystal with controllable thickness can be obtained. Secondly, limiting the thickness of the perovskite single crystal by the liquid surface rather than the substrate reduces the contact of the perovskite single crystal with the substrate, thereby reducing defects of the single crystal. In addition, the precursor liquid can diffuse into the limiting phase solvent and volatilize, the concentration of the precursor liquid is improved, the growth is promoted, compared with an inverse temperature growth method, the temperature is low, the growth is slow, the crystallization quality is guaranteed, the surface trap density of the prepared optical detector is lower, and the photoelectric performance is excellent. The ultrathin perovskite single crystal has good application prospect in the field of photoelectricity.
Description
Technical Field
The invention belongs to the field of semiconductor photoelectric materials, relates to a preparation method of a two-dimensional perovskite single crystal and photoelectric property research, and particularly relates to a growth method of a planar perovskite single crystal with a large surface area to volume ratio, a large area and high quality.
Background
Perovskite materials have been widely studied for their excellent photophysical properties, such as adjustable optical properties, large absorption coefficient, low defect density, long carrier diffusion length, etc. These properties make them of great potential in solar cells, light emitting diodes, lasers and photodetectors. The research on the influence of the size, the structure and the composition of the nano structure on the performance of the nano material and the design of the nano structure with new or enhanced performance and application prospect are one of the hot spots of the current domestic and foreign research. On the basis of reducing the dimension of three-dimensional hybrid metal halide perovskites to improve the photoelectric properties of the three-dimensional hybrid metal halide perovskites, a great deal of literature researches the application of low-dimensional perovskite in a photoelectric detector, and the two-dimensional perovskites are concerned due to the special properties of large exciton binding energy, high photoluminescence quantum yield (PLQY), high crystallinity, good stability and the like. Defects in two-dimensional perovskites depend primarily on their composition, diameter or thickness, growth and processing methods, which have a large effect on the properties of the two-dimensional material. However, perovskite with thickness not meeting the definition of the original two-dimensional material (thickness less than 100 nm) has a thickness smaller than the carrier diffusion length due to the disappearance of the grain boundary, and most importantly, the performance of the perovskite changes with the change of the thickness, so that single crystals with large surface area to volume ratio are also in the spotlight.
At present, the growing method of the ultrathin perovskite single crystal mainly comprises a spin coating method, a chemical vapor deposition method, a Top-down method, a space limitation method and the like. However, these methods have respective drawbacks, such as that although the thickness of single crystals prepared by spin coating and chemical vapor deposition methods can reach several tens of nanometers, the transverse dimension is difficult to reach millimeter level; the Top-down method is difficult to cut the thickness of the crystal to be below 100 mu m due to the brittleness of the crystal; according to the space limitation method, two substrates are used for limiting the crystal growth space, the quality of single crystals is easily affected by defects on the substrates, and the crystals below 100 mu m are difficult to prepare.
The single crystals prepared by the existing methods are often small in area or large in thickness. The invention provides a two-dimensional perovskite single crystal and a growth method thereof, which utilize a liquid-liquid interface to limit the growth of the single crystal in the thickness direction to obtain ABX with small thickness and large area 3 A single crystal.
Disclosure of Invention
The invention provides a preparation method of a two-dimensional perovskite single crystal, which has the characteristics of simple preparation, low cost, small thickness, large area, no need of an anti-solvent, high crystal quality and the like, and makes up for the defects in the prior art.
The experimental protocol of the present invention is shown as follows:
the preparation method of the two-dimensional perovskite single crystal is characterized in that a liquid-liquid phase confinement method is utilized to prepare two-dimensional ABX 3 The upper surface of the obtained two-dimensional crystal of the perovskite semiconductor material is not contacted with the substrate, thereby reducing defects and obtaining the high-quality two-dimensional plane perovskite single crystal. The method comprises the following steps:
(1) mixing AX and BX 2 Dissolving in a precursor solvent according to a certain proportion to obtain a precursor solution system, heating and stirring to obtain clear and transparent ABX 3 And (3) solution. Wherein ABX 3 The concentration of the precursor solution is 0.1 wt% to the concentration of a saturated solution, wherein A is MA + 、FA + 、Cs + B is Pb 2+ 、Sn 2+ Or two, X is Cl − 、Br − 、I − One or more of (a) and (b).
(2) Taking the above ABX 3 Dripping the solution on a clean plane substrate and spreading the solution to form a film;
(3) dropping limiting phase solvent to ABX 3 The solution film is covered completely to form a liquid-liquid interface, limiting the thickness of the solution and isolating moisture from air. Wherein the limiting layer solution is mixed with ABX 3 The solution is immiscible or has little solubility and should have a density less than ABX 3 The density of the solution;
(4) standing and growing for a period of time at low temperature to obtain the two-dimensional perovskite monocrystal.
A preparation method of a two-dimensional perovskite single crystal is characterized in that the volume of a precursor solution to be dripped and the size of a substrate can be adjusted according to the required crystal thickness, and the obtained crystal thickness is between 100 nm and 5 mm.
The preparation method of the two-dimensional perovskite single crystal is characterized in that the precursor solvent is one or a mixture of dimethyl sulfoxide, dimethylformamide, N-methylpyrrolidone and gamma-butyrolactone.
The preparation method of the two-dimensional perovskite single crystal is characterized in that the planar substrate can be glass, silicon wafer, polyethylene terephthalate, polytetrafluoroethylene or other foreseeable planar substrates.
The preparation method of the two-dimensional perovskite single crystal is characterized in that the limiting solution is silicone oil or a polycarboalkane nonpolar solvent meeting the density condition.
The preparation method of the two-dimensional perovskite single crystal is characterized in that the low-temperature range is 0-80 ℃, and the growth time is 0.1 hour-10 days.
Compared with common perovskite single crystals with large surface area to volume ratio, the perovskite single crystal provided by the invention has the following advantages:
(1) the single crystal is grown by using a liquid-liquid phase confinement method, the growth of the single crystal in the thickness direction can be inhibited by the thickness of a precursor solvent layer, the growth of the crystal in other directions is not influenced while the liquid level in the thickness direction is limited, and the obtained single crystal is small in thickness and large in area;
(2) the contact between the perovskite single crystal and the substrate is reduced through liquid-liquid interface limitation, so that the defects of the single crystal are reduced;
(3) the precursor liquid can diffuse into the limiting solution and slowly volatilize, the concentration of the precursor liquid is improved, the growth is promoted, and compared with an inverse temperature growth method, the method is low in required temperature and slow in growth, and the crystallization quality is guaranteed;
(4) the growth process is simple, the operation is easy, the growth period is short, and the method has great application value in the growth of the perovskite single crystal;
(5) the maximum size of the prepared single crystal reaches 8 mm, the thickness of the prepared single crystal is only 50 mu m, and compared with the existing report, the prepared single crystal has the advantages of large size and small thickness.
Drawings
FIG. 1 is a schematic of a perovskite single crystal growth route;
FIG. 2 is MAPbCl 3 3D confocal micrographs of the perovskite single crystals on a substrate and cross-section thickness maps of the perovskite single crystals;
FIG. 3 is MAPbCl 3 XRD pattern of perovskite single crystal.
Detailed Description
In order to make the essential features of the present invention and its practical application easier to understand, the following detailed description of the technical solution of the present invention is made with reference to the accompanying drawings and several embodiments. However, the following description and illustrations of the embodiments do not limit the scope of the present invention, and functional, methodological, or structural equivalents or substitutions that may be made by those skilled in the art according to the embodiments are within the scope of the present invention:
example 1
MAPbBr 3 Experimental procedure for perovskite single crystal:
(1) dissolving lead bromide and amine bromide in dimethylformamide, heating and stirring to dissolve, and forming clear and transparent MAPbBr 3 The molar ratio of the lead bromide to the amine bromide is 1:1, and MAPbBr is added to the precursor solution 3 The mass fraction of the precursor solution is 30 percent;
(2) mixing the MAPbBr 3 Precursor solutionStanding at constant temperature for 6-12 h, filtering the precursor solution with 0.22 μm nylon filter head, placing the filtered solution into a sample bottle, and sealing for use;
(3) respectively ultrasonically cleaning a glass substrate by using detergent, deionized water, acetone and isopropanol and drying for later use;
(4) taking the filtered MAPbBr 3 Solution, a proper amount of solution is measured by a pipette, the solution is dripped on a glass plate and naturally spread to form a film, and the schematic diagram is shown in figure 1;
(5) 1 ml of silicone oil was added dropwise to MAPbBr with a dropper 3 And completely covering the solution film, limiting the thickness of the solution film, isolating moisture and air, standing in an incubator for several hours, growing ultrathin planar perovskite single crystal seeds on a glass plate, and obtaining larger crystals after about 1-2 days.
Example 2
Flexible MAPbBr 3 Experimental procedure for perovskite single crystals:
(1) dissolving lead bromide and amine bromide in dimethylformamide, heating, stirring, and dissolving to obtain clear and transparent MAPbBr 3 The molar ratio of the lead bromide to the amine bromide is 1:1, and MAPbBr is adopted as the precursor solution 3 The mass fraction of the precursor solution is 30%;
(2) mixing the MAPbBr 3 Standing the precursor solution at constant temperature for 6-12 h, filtering the solution with a nylon filter head of 0.22 μm, placing the filtered solution into a sample bottle, and sealing for later use;
(3) cleaning and drying the peeled mica sheet substrate for later use;
(4) taking the filtered MAPbBr 3 Solution, a proper amount of solution is measured by a pipette, and the solution is dripped on the mica and naturally spread to form a film;
(5) 1 ml of silicone oil was added dropwise to MAPbBr with a dropper 3 Covering the solution film completely to limit the thickness of the solution and isolate water and air, standing in a heat insulating box for several hours to grow ultrathin planar perovskite monocrystal seed on mica, and obtaining large and flexible crystal after about 1-2 days。
Example 3
MAPbCl 3 Experimental procedure for perovskite single crystals:
(1) dissolving lead chloride and amine chloride salt in dimethyl sulfoxide, heating and stirring to dissolve, and forming clear and transparent MAPbCl 3 The molar ratio of the lead chloride to the amine chloride salt is 1:1, and MAPbCl is adopted as a precursor solution 3 The mass fraction of the precursor solution is 30 percent;
(2) mixing the MAPbCl 3 Standing the precursor solution at constant temperature for 6-12 h, filtering the solution with a nylon filter head of 0.22 μm, placing the filtered solution into a sample bottle, and sealing for later use;
(3) ultrasonically cleaning a glass substrate with detergent, deionized water, acetone and isopropanol respectively and drying for later use;
(4) taking the filtered MAPbCl 3 Precursor solution, taking a proper amount of solution by using a liquid transfer gun, dripping the solution on a glass plate and naturally spreading the solution to form a film;
(5) 1 mL of silicone oil is added to MAPbCl dropwise by a dropper 3 And (3) completely covering the solution film, limiting the thickness of the solution film, isolating moisture and air, standing in an insulation box for about 1 day, growing ultrathin planar perovskite single crystal seeds on a glass plate, and obtaining larger crystals after about 3-4 days, wherein the size of the crystals can reach 2 mm and the thickness of the crystals is only 40 mu m as shown in figure 2. Fig. 3 is an XRD image of the perovskite single crystal, which shows diffraction peaks of 15.57 °, 31.43 °, 47.95 °, and 65.62 °, respectively, corresponding to (100), (200), (300), and (400) crystal planes of the cubic crystal structure. The full width at half maximum (FWHM) is respectively 0.049 degrees, 0.058 degrees, 0.067 degrees and 0.085 degrees, and is at the leading position in literature reports, which indicates that the crystal has higher quality.
Example 4
MAPbI 3 Experimental procedure for perovskite single crystal:
(1) dissolving lead iodide and amine iodide in gamma-butyrolactone, heating and stirring to dissolve, and forming clear and transparent MAPbI 3 The precursor solution, wherein the molar ratio of the lead iodide to the amine iodide salt is 1:1, MAPbI 3 The mass fraction of the precursor solution is 30 percent;
(2) mixing the MAPbI 3 Standing the precursor solution at constant temperature for 6-12 h, filtering the solution with a nylon filter head of 0.22 μm, placing the filtered solution into a sample bottle, and sealing for later use;
(3) ultrasonically cleaning a glass substrate with detergent, deionized water, acetone and isopropanol respectively and drying for later use;
(4) taking the filtered MAPbI 3 Solution, a proper amount of solution is measured by a liquid transfer gun, and the solution is dripped on a glass plate and naturally spread to form a film;
(5) 1 mL of silicone oil was added dropwise to the MAPbI solution with a dropper 3 And completely covering the solution film, limiting the thickness of the solution film, isolating moisture and air, standing in an incubator for about 1 day, growing ultrathin planar perovskite single crystal seeds on a glass plate, and obtaining larger crystals after about 3-4 days.
Example 5
CsPbBr 3 Experimental procedure for perovskite single crystals:
(1) dissolving lead bromide and cesium bromide in dimethyl sulfoxide, heating and stirring for dissolving to form clear and transparent CsPbBr 3 The molar ratio of the lead bromide to the cesium bromide is 1:1, and CsPbBr is added to the precursor solution 3 The mass fraction of the precursor solution is 30 percent;
(2) mixing the above CsPbBr 3 Standing the solution at constant temperature for a period of time, filtering the solution with a 0.22 μm nylon filter head, placing the filtered solution into a sample bottle, and sealing for later use;
(3) respectively ultrasonically cleaning a glass substrate by using detergent, deionized water, acetone and isopropanol and drying for later use;
(4) taking the filtered CsPbBr 3 Solution, a proper amount of solution is measured by a liquid transfer gun, and the solution is dripped on a glass plate and naturally spread to form a film;
(5) dropping silicone oil to CsPbBr by dropper 3 Covering the solution film completely to limit the thickness of the solution and isolate water and air, and standing in an incubatorAfter a day, ultra-thin planar perovskite single crystal seeds are grown on the glass plate, and after about 5 days, larger crystals are obtained.
Example 6
CsPbCl 3 Experimental procedure for perovskite single crystals:
(1) dissolving lead chloride and cesium chloride in dimethyl sulfoxide, heating and stirring for dissolving to form clear and transparent CsPbCl 3 The molar ratio of the lead bromide to the cesium bromide is 1:1, and CsPbCl is added to the precursor solution 3 The mass fraction of the precursor solution is 30 percent;
(2) mixing the above CsPbCl 3 Standing the solution at constant temperature for a period of time, filtering the solution with a 0.22 μm nylon filter head, placing the filtered solution into a sample bottle, and sealing for later use;
(3) respectively ultrasonically cleaning a glass substrate by using detergent, deionized water, acetone and isopropanol and drying for later use;
(4) taking the filtered CsPbCl 3 Measuring a proper amount of solution by using a liquid transfer gun, dripping the solution on a glass plate, and naturally spreading the solution to form a film;
(5) dropping silicone oil to CsPbCl by dropper 3 And (3) completely covering the solution film, limiting the thickness of the solution and isolating moisture and air, standing in an incubator for several days, growing ultrathin planar perovskite single crystal seeds on a glass plate, and obtaining larger crystals after about 5 days.
Claims (5)
1. A preparation method of a two-dimensional perovskite single crystal is characterized in that the two-dimensional perovskite single crystal is prepared by a liquid-liquid phase confinement method, the upper surface of the obtained two-dimensional perovskite single crystal is not contacted with a substrate, so that defects are reduced, and the high-quality two-dimensional perovskite single crystal is obtained, and the preparation method comprises the following steps:
(1) mixing AX and BX 2 Dissolving in precursor solvent according to a certain proportion to obtain precursor solution system, heating and stirring to obtain clear and transparent ABX 3 Precursor solution of ABX 3 The concentration of the precursor solution is 0.1 wt% to the concentration of a saturated solution, wherein A is MA + 、FA + 、Cs + B is Pb 2+ 、Sn 2+ One or two of them, X is Cl − 、Br − 、I − One or more of;
(2) taking the above ABX 3 Dripping the precursor solution on a clean plane substrate and spreading the precursor solution to form a film;
(3) dropping limiting phase solvent to ABX 3 Covering the precursor solution film completely to form a liquid-liquid interface, and isolating water and air by limiting the thickness of the phase solvent, wherein the phase solvent and ABX are limited 3 The precursor solution is immiscible and has a density less than ABX 3 Density of the precursor solution;
(4) standing at low temperature for a period of time to obtain a two-dimensional perovskite single crystal;
the limiting phase solvent is silicone oil.
2. The method for producing a two-dimensional perovskite single crystal as claimed in claim 1, wherein ABX is added dropwise in an adjustable manner according to a desired thickness of the two-dimensional perovskite single crystal 3 The volume of the precursor solution and the size of the substrate, and the thickness of the obtained two-dimensional perovskite single crystal is between 100 nm and 5 mm.
3. The method for preparing a two-dimensional perovskite single crystal as claimed in claim 1, wherein the precursor solvent is one of dimethyl sulfoxide, dimethylformamide, N-methylpyrrolidone, gamma-butyrolactone or a mixture thereof.
4. The method for preparing a two-dimensional perovskite single crystal as claimed in claim 1, wherein the planar substrate is a glass or silicon wafer or polyethylene terephthalate or polytetrafluoroethylene.
5. The process for producing a two-dimensional perovskite single crystal as claimed in claim 1, wherein said low temperature is in the range of 0 to 80 ℃ and the growth time is in the range of 0.1 hour to 10 days.
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