CN115787059A - Preparation method of perovskite single crystal film - Google Patents

Preparation method of perovskite single crystal film Download PDF

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CN115787059A
CN115787059A CN202211327942.1A CN202211327942A CN115787059A CN 115787059 A CN115787059 A CN 115787059A CN 202211327942 A CN202211327942 A CN 202211327942A CN 115787059 A CN115787059 A CN 115787059A
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single crystal
perovskite
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thin film
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刘节华
李盼盼
魏香凤
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Hefei University of Technology
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Hefei University of Technology
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Abstract

The invention discloses a preparation method of a perovskite single crystal film, which utilizes a simple interface limiting method of a double-flexible polymer film, single crystals grow between films through an in-situ imprinting method, and an organic solvent continuously diffuses to enable a precursor solution to reach supersaturation, nucleate and crystallize and grow into the single crystal film. The polymer film can isolate water vapor, and the damage of external water to the crystal is avoided, so that the crystal is ensured to have better environmental stability. The polymer film is easily peeled from the single crystal due to its non-polar characteristic, so that the single crystal is not easily damaged, thereby reducing defects of the single crystal. The imprinted structure obtained by the double-flexible interface confinement method has good crystallinity and a light capture structure, and the photoelectric detector manufactured by the method has excellent photoelectric performance.

Description

Preparation method of perovskite single crystal film
Technical Field
The invention belongs to the field of semiconductor photoelectric materials, relates to a preparation method of a perovskite single crystal film and photoelectric property research, and particularly relates to a growth method of a perovskite single crystal film with controllable size, adjustable thickness and high quality.
Background
Perovskite semiconductor single crystals have attracted much attention in photoelectric devices because of their excellent optical and optoelectronic properties, such as light absorption coefficient, controllable band gap, long carrier lifetime, few surface defects, etc. From the geometrical structure, the space occupancy rate of the polycrystalline film is low, but the grain boundary defects are more, and the recombination of carriers is increased. The thin perovskite single crystal wafer not only has the characteristic of bulk crystal, but also has a large orientation of light irradiating the crystal surface. The single wafer has the ideal geometry of an optoelectronic device. Single wafers are more stable than polycrystalline thin films or micro/nano crystals under the same conditions. Therefore, a high quality single wafer is more suitable for a compact high performance photodetector due to its inherent characteristics.
Much work has been done on the production of perovskite single crystal sheets by physical and chemical methods. With the physical method, it is difficult to obtain a single crystal wafer having a thickness of less than 50 μm by the mechanical cutting method due to the brittleness of the perovskite single crystal wafer. The flaky perovskite single crystal is synthesized by adopting chemical strategies such as a space limit method, a stripping method, a vapor deposition method and the like. The space-limiting method is a common method for obtaining a sheet-like single crystal using two hard substrates such as glass and silicon wafer. It also requires post-polishing to reduce interface defects formed by the removal of the hard substrate. In addition, polished crystal interfaces lead to loss of reflected light and interface new defects. Recently, high-quality perovskite single crystal wafers have been successfully synthesized by a liquid-liquid space confinement method without polishing to reduce surface defects of the crystal wafers.
To enhance light absorption, surface texturing is used to reduce reflection, nanoimprinting by increasing the chance of secondary reflected light absorption is a high resolution processing technique, potential applications of which include photonic and optoelectronic devices, integrated circuits, nanofluids, etc., are inspired by nanoimprinting techniques that are used to prepare perovskite nanocrystals CH 3 NH 3 PbX 3 The crystals are sensitive to humidity and, unlike chemically etched silicon crystals, it is difficult to obtain a chemical surface texture. Irradiation of CsPbBr with femtosecond laser 3 The physical micro-laser technology for direct laser imprinting treatment of single crystals also obtains microstructure patterns on the single crystal perovskite thin film, but the regional high-energy process causes more interface crystal defects, and the laser micromachining technology is not suitable for organic-inorganic hybrid perovskites, because the decomposition of organic components inevitably occurs in the high-temperature region by laser irradiation. Perovskite semiconductor single crystal thin film with texture structure due to light scattering, light reflection and high refractionThe photoelectric performance of the photoelectric device can be improved through light capture.
The invention provides a perovskite single crystal film and a growth method thereof, which utilize a double flexible interface to limit the growth of single crystals and obtain the perovskite semiconductor single crystal film with smaller thickness and adjustable area.
Disclosure of Invention
The invention provides a preparation method of a perovskite single crystal film, which has the characteristics of simple preparation, surface texture making, controllable size, high crystal quality, high environmental stability, light trap structure 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 perovskite single crystal film is characterized in that a surface texture-making structure A is prepared by an in-situ interface confinement method by utilizing the interface microstructure and the flexibility characteristic of a polymer film m BX n The perovskite semiconductor single crystal thin film material has good crystallinity and an optical trap structure, and comprises the following steps:
(1) Mixing AX and BX 2 Or BX 3 Dissolving in precursor solvent according to a certain proportion to obtain precursor solution system, heating and stirring to obtain clear and transparent A m BX n Solution of A wherein m BX n The concentration of the precursor solution is 0.1 wt percent to the concentration of a saturated solution, wherein A is methylamine ion MA + Formamidine ion FA + Butylamine ion BA + Cesium ion Cs + Silver ion Ag + B is Pb 2+ 、Sn 2+ 、Bi 3+ 、Sn 2+ 、Cu 2+ One or two of (A) and (B), X is Cl − 、Br − 、I − One or more of (a);
(2) Taking the above A m BX n The solution is dripped on a clean flexible polymer film and covered by another film, the solution is uniformly spread to form a film, and the peripheries of the two films are sealed to prevent the solution from leaking;
(3) And (4) placing the perovskite monocrystal thin film on a flat position, standing and growing for a period of time at a low temperature to obtain the perovskite monocrystal thin film.
The method for preparing a perovskite single crystal thin film as claimed in claim 1, wherein the double polymer flexible interface confinement method can obtain thinner crystals, the volume of the dropwise added precursor solution and the size of the flexible substrate can be adjusted according to the required thickness and length of the crystals, and the thickness of the obtained crystal thin film is between 100nm and 10 mm.
The method for preparing a perovskite single crystal thin film as claimed in claim 1, wherein the precursor solvent is one or more of dimethyl sulfoxide, N-dimethylformamide, N-methylpyrrolidone and gamma-butyrolactone.
The method of claim 1, wherein the polymer film is selected from the group consisting of polyethylene film, polypropylene film, polyvinyl chloride film, polyvinylidene chloride film, ethylene-tetrafluoroethylene copolymer film, polyester fiber film, and any other flexible polymer film.
The method of producing a perovskite single crystal thin film as claimed in claim 1, wherein said polymer film is permeable to a solvent and blocks the passage of ions.
The process for producing a flaky perovskite single crystal as claimed in claim 1, wherein the temperature is in the range of-10 to 120 ℃ and the growth time is 1 hour to 30 days.
The method for producing a flaky perovskite single crystal as claimed in claim 1, wherein the surface texturing structure depends on the microstructure of the polymer film.
The process for producing a perovskite single crystal thin film as claimed in claim 1, wherein A is m BX n ，0<m£5, 2£n£10。
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) Growing a single crystal by using a double-flexible interface confinement method, and inhibiting the growth of the single crystal in the thickness direction by using the interface microstructure and the confinement characteristics of a double-flexible polymer film;
(2) The perovskite single crystal thin film is synthesized by in-situ imprinting of a double-flexible polymer film microstructure, so that the single crystal perovskite thin film with a texture-making structure with light capture is obtained, and the perovskite thin film has good light capture and photoelectric characteristics.
(3) The precursor liquid can be diffused into the polymer film and volatilize, the concentration of the precursor liquid is improved, the growth of the crystal film is promoted, and the polymer film is easy to strip the single crystal film from the polymer film due to the nonpolar characteristic of the polymer film, so that the single crystal film is not easy to damage, and the defects of single crystals are reduced.
(4) The growth process is easy to operate, has good repeatability and has great application value in the growth of perovskite single crystal;
(5) The perovskite single crystal thin film with adjustable size can be obtained by the double-flexible polymer film interface confinement method, the volume and the additional pressure of the dropwise added precursor solution can be adjusted according to the required thickness and length of the crystal, and the thickness of the obtained crystal is between 100nm and 10 mm.
Drawings
FIG. 1 is a schematic diagram of the growth route of a perovskite single crystal thin film;
FIG. 2 is a 3D confocal micrograph of a perovskite single crystal thin film (left panel) and a polymer film (right panel);
FIG. 3 is an XRD spectrum of a perovskite single crystal thin film.
Detailed Description
In order to make the substantive features of the present invention and its practical application easier to understand, the following description is given with reference to the accompanying drawings and several tools
Embodiments of the present invention will be described in further detail. The following description and illustrations of the embodiments do not limit the scope of the present invention, and functional equivalents, methods, or structural equivalents thereof, which may be implemented by those skilled in the art based on the embodiments are intended to fall within the scope of the present invention:
example 1
MAPbBr 3 The experimental steps of the perovskite single crystal thin film are as follows: dissolving lead bromide and amine bromide salt in N, N-dimethylformamide, heating and stirring to dissolve, and allowing to form clear and transparent MAPbBr 3 A precursor solution, wherein the molar ratio of the lead bromide to the amine bromide salt is 1,MAPbBr 3 Precursor solutionIs 30 percent. Mixing the MAPbBr 3 Filtering the precursor solution by a filter membrane with the diameter of 0.22 mu m, and putting the filtered solution into a sample bottle for later use. Taking the filtered MAPbBr 3 Solution, the appropriate amount of solution was taken with a pipette, dropped into a clean polyethylene film and spread evenly. After the periphery of the polyethylene film is sealed, standing for a period of time at room temperature, growing perovskite seed crystals between the polyethylene films, and finally obtaining the single crystal film with adjustable area and certain thickness. The single crystal film has good crystal quality and an optical trap structure, and the prepared photoelectric detector has good photoelectric detection performance.
Example 2
MAPbCl 3 Experimental steps of the perovskite single crystal thin film: dissolving lead chloride and amine chloride salt in dimethyl sulfoxide, heating and stirring to dissolve, and forming clear and transparent MAPBCl 3 A precursor solution, wherein the molar ratio of the lead chloride to the amine chloride salt is 1,MAPbCl 3 The mass fraction of the precursor solution is 10%. Mixing the MAPbCl 3 Filtering the precursor solution by a filter membrane with the diameter of 0.22 mu m, putting the filtered solution into a sample bottle, and sealing for later use. Taking the filtered MAPbCl 3 Taking a proper amount of solution by using a pipette, dripping the solution into a clean polyvinylidene chloride film, and uniformly spreading the solution. Sealing the peripheries of the polyvinylidene chloride films, standing for a period of time at room temperature, and growing perovskite seed crystals between the polyvinylidene chloride films to finally obtain the single crystal film with adjustable area and certain thickness. The single crystal film has good crystal quality and an optical trap structure, and the prepared photoelectric detector has good photoelectric detection performance.
Example 3
MAPbI 3 Experimental steps of the perovskite single crystal thin film: 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%. Mixing the MAPbI 3 Filtering the precursor solution with a 0.22 μm filter membrane, and placing the filtered solution into a sample bottleAnd sealing for later use. Taking the filtered MAPbI 3 Taking a proper amount of solution by using a liquid transfer gun, dripping the solution into a clean polyvinyl chloride film, and uniformly spreading the solution. Sealing the periphery of the polyvinyl chloride films, standing for a period of time at room temperature, and growing perovskite seed crystals between the polyvinyl chloride films to finally obtain the single crystal film with adjustable area and certain thickness. The single crystal film has good crystal quality and an optical trap structure, and the prepared photoelectric detector has good photoelectric detection performance.
Example 4
CsPbBr 3 Experimental steps of the perovskite single crystal thin film: dissolving lead bromide and cesium bromide in dimethyl sulfoxide, heating and stirring to dissolve, and forming clear and transparent CsPbBr 3 A precursor solution, wherein the molar ratio of the lead bromide to the cesium bromide is 1,CsPbBr 3 The mass fraction of the precursor solution is 20%. Mixing the above CsPbBr 3 Filtering the precursor solution by a filter membrane with the diameter of 0.22 mu m, putting the filtered solution into a sample bottle, and sealing for later use. Taking the filtered CsPbBr 3 Taking a proper amount of solution by using a pipette, dripping the solution into a clean polypropylene film, and uniformly spreading the solution. Sealing the periphery of the polypropylene films, standing for a period of time at room temperature, and growing perovskite seed crystals between the polypropylene films to finally obtain the single crystal film with adjustable area and certain thickness. The single crystal film has good crystal quality and an optical trap structure, and the prepared photoelectric detector has good photoelectric detection performance.
Example 5
Cs 3/2 BiI 9/2 The experimental steps of the perovskite single crystal thin film are as follows: dissolving bismuth iodide and cesium iodide in N, N-dimethylformamide, heating and stirring for dissolving to form clear and transparent Cs 3/2 BiI 9/2 Precursor solution, wherein the molar ratio of bismuth iodide to cesium iodide is 3:2,Cs 3/2 BiI 9/2 The mass fraction of the precursor solution is 20%. Mixing the above Cs 3/2 BiI 9/2 Filtering the precursor solution, putting the filtered solution into a sample bottle, and sealing for later use. Taking the filtered Cs 3/2 BiI 9/2 Taking appropriate amount of solution with pipetteAnd (3) dripping the solution into a clean polyvinylidene chloride film and uniformly spreading the solution. Sealing the polyvinylidene chloride films and standing for a period of time at room temperature, and growing perovskite seed crystals between the polyvinylidene chloride films to finally obtain the single crystal film with adjustable area and certain thickness. The single crystal film has good crystal quality and an optical trap structure, and the prepared photoelectric detector has good photoelectric detection performance.
Example 6
CsCuBr 3 Experimental steps of the perovskite single crystal thin film: dissolving cupric bromide and cesium bromide in N, N-dimethylformamide, heating, stirring and dissolving to form clear and transparent CsCuBr 3 A precursor solution, wherein the molar ratio of the cupric bromide to the cesium bromide is 1, csCuBr 3 The mass fraction of the precursor solution is 15%. Mixing the above CsCuBr 3 Filtering the precursor solution, putting the filtered solution into a sample bottle, and sealing for later use. Taking the filtered CsCuBr 3 Taking a proper amount of solution by using a liquid transfer gun, dripping the solution into a clean ethylene-tetrafluoroethylene copolymer film, and uniformly spreading the solution. And sealing the periphery of the ethylene-tetrafluoroethylene copolymer films, standing for a period of time at room temperature, and growing perovskite seed crystals between the ethylene-tetrafluoroethylene copolymer films to finally obtain the single crystal film with adjustable area and certain thickness.
Example 7
AgBiI 4 Experimental steps of the perovskite single crystal thin film: dissolving silver iodide and bismuth iodide salt in N-methyl pyrrolidone, heating, stirring and dissolving to obtain clear and transparent AgBiI 4 The molar ratio of the silver iodide to the bismuth iodide is 1,AgBiI 4 The mass fraction of the precursor solution is 10%. Mixing the AgBiI 4 Filtering the precursor solution, putting the filtered solution into a sample bottle, and sealing for later use. Taking the filtered AgBiI 4 Taking a proper amount of solution by using a liquid transfer gun, dripping the solution into a clean polyester fiber film, and uniformly spreading the solution. After the periphery of the polyester fiber membrane is sealed, standing for a period of time at room temperature, growing perovskite seed crystals among the polyester fibers, and finally obtaining the perovskite seed crystals with adjustable area and certain thicknessA monocrystalline film of amorphous carbon.
Example 8
BAPbBr 3 Experimental steps of the perovskite single crystal thin film: dissolving lead bromide and butylamine bromide in N, N-dimethylformamide, heating, stirring and dissolving to obtain clear and transparent BAPbBr 3 The molar ratio of the lead bromide to the amine bromide salt is 1,BAPbBr 3 The mass fraction of the precursor solution is 30%. Mixing the above BAPbBr 3 Filtering the precursor solution, putting the filtered solution into a sample bottle, and sealing for later use. Taking the filtered BAPbBr 3 Taking a proper amount of solution by using a liquid transfer gun, dripping the solution into a clean polyvinylidene chloride film, and uniformly spreading the solution. Sealing the periphery of the polyvinylidene chloride films, standing for a period of time at room temperature, growing perovskite seed crystals between the polyvinylidene chloride films, and finally obtaining the single crystal film with adjustable area and certain thickness.
Example 9
(BA) 2/3 (MA) 2/3 PbBr 10/3 Experimental steps of the perovskite single crystal thin film: dissolving lead bromide, amine bromide and butylamine salt in N, N-dimethylformamide, heating and stirring for dissolving to obtain clear transparent (BA) 2/3 (MA) 2/3 PbBr 10/3 The molar ratio of the lead bromide to the amine bromide to the butylamine bromide in the precursor solution is 3 2/3 (MA) 2/3 PbBr 10/3 The mass fraction of the precursor solution is 20%. General the above (BA) 2/3 (MA) 2/3 PbBr 10/3 Filtering the precursor solution by a filter membrane with the diameter of 0.22 mu m, and putting the filtered solution into a sample bottle for later use. Taking the filtered (BA) 2/3 (MA) 2/3 PbBr 10/3 Taking a proper amount of solution by using a pipette, dripping the solution into a clean polyethylene film, and uniformly spreading the solution. After the periphery of the polyethylene film is sealed, standing for a period of time at room temperature, growing perovskite seed crystals between the polyethylene films, and finally obtaining the single crystal film with adjustable area and certain thickness.

Claims (8)

1. A preparation method of a perovskite single crystal film,the method is characterized in that a surface texture surface structure A is prepared by an in-situ interface confinement method by utilizing the interface microstructure and the flexible characteristic of a polymer film m BX n The perovskite semiconductor single crystal thin film material has good crystallinity and an optical trap structure, and comprises the following steps:
(1) Mixing AX and BX 2 Or BX 3 Dissolving in precursor solvent according to a certain proportion to obtain precursor solution system, heating and stirring to obtain clear and transparent A m BX n Solution of A m BX n The concentration of the precursor solution is 0.1 wt% to the concentration of a saturated solution, wherein A is methylamine ion MA + Formamidine ion FA + Butylamine ion BA + Cesium ion Cs + Silver ion Ag + B is Pb 2+ 、Sn 2+ 、Bi 3+ 、Sn 2+ 、Cu 2+ One or two of (A) and (B), X is Cl − 、Br − 、I − One or more of (a);
(2) Taking the above A m BX n The solution is dripped on a clean flexible polymer film and covered by another film, the solution is uniformly spread to form a film, and the peripheries of the two films are sealed to prevent the solution from leaking around the films;
(3) And (4) placing the perovskite monocrystal thin film on a flat position, standing and growing for a period of time at a low temperature to obtain the perovskite monocrystal thin film.
2. The method for preparing a perovskite single crystal thin film as claimed in claim 1, wherein the double polymer flexible interface confinement method can obtain thinner crystals, the volume of the dropwise added precursor solution and the size of the flexible substrate can be adjusted according to the required thickness and length of the crystals, and the thickness of the obtained crystal thin film is between 100nm and 10 mm.
3. The method for preparing a perovskite single crystal thin film as claimed in claim 1, wherein the precursor solvent is one or more of dimethyl sulfoxide, N-dimethylformamide, N-methylpyrrolidone and γ -butyrolactone.
4. The method of claim 1, wherein the polymer film is selected from the group consisting of polyethylene film, polypropylene film, polyvinyl chloride film, polyvinylidene chloride film, ethylene-tetrafluoroethylene copolymer film, polyester fiber film, and any other flexible polymer film.
5. The method of producing a perovskite single crystal thin film as claimed in claim 1, wherein said polymer film is permeable to a solvent and blocks the passage of ions.
6. The process for producing a flaky perovskite single crystal as claimed in claim 1, wherein the temperature is in the range of-10 to 120 ℃ and the growth time is 1 hour to 30 days.
7. The method for producing a flaky perovskite single crystal as claimed in claim 1, wherein the surface texture structure depends on the microstructure of the polymer film.
8. The process for producing a perovskite single crystal thin film as claimed in claim 1, wherein A is m BX n ，0<m£5, 2£n£10。
CN202211327942.1A 2022-10-27 2022-10-27 Preparation method of perovskite single crystal film Pending CN115787059A (en)

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