CN113838980A - Polyhedral CsPbBr3@CsPbX3Core-shell perovskite heterojunction and preparation method thereof - Google Patents
Polyhedral CsPbBr3@CsPbX3Core-shell perovskite heterojunction and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 36
- 239000011258 core-shell material Substances 0.000 claims abstract description 84
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000010453 quartz Substances 0.000 claims abstract description 47
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- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 16
- 239000011261 inert gas Substances 0.000 claims abstract description 15
- 239000011812 mixed powder Substances 0.000 claims abstract description 15
- -1 cesium halide Chemical class 0.000 claims abstract description 11
- 150000004820 halides Chemical class 0.000 claims abstract description 11
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 22
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 230000035484 reaction time Effects 0.000 claims description 12
- 229910052681 coesite Inorganic materials 0.000 claims description 11
- 229910052906 cristobalite Inorganic materials 0.000 claims description 11
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- 229910052786 argon Inorganic materials 0.000 description 23
- 239000013078 crystal Substances 0.000 description 16
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 description 14
- 229910052745 lead Inorganic materials 0.000 description 12
- 229910052794 bromium Inorganic materials 0.000 description 9
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 8
- 239000002243 precursor Substances 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 7
- 230000006837 decompression Effects 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical group [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 6
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- 125000004429 atom Chemical group 0.000 description 1
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- 125000001246 bromo group Chemical group Br* 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
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Abstract
The invention discloses a polyhedral CsPbBr3@CsPbX3A core-shell heterojunction and a preparation method thereof. In the core-shell perovskite heterojunction, the polyhedron CsPbBr3As core, CsPbX3Is a shell layer, wherein X is Cl or I. The preparation method comprises the following steps: a quartz tube 2 is sleeved in a quartz tube 1 of the double-temperature-zone tube furnace, and the mixed powder of cesium halide and lead halide and the polyhedron CsPbBr are deposited on a substrate3Respectively arranged at two ends in a quartz tube 2 and respectively positioned in upstream and downstream areas of a dual-temperature-area tube furnace, setting the temperature of the upstream area to be 540-700 ℃, the temperature of the downstream area to be 270-330 ℃, and preparing in an inert gas atmosphere to obtain the polyhedron CsPbBr3@CsPbX3A core-shell heterojunction, wherein X is Cl or I. The preparation method is simple, and the obtained CsPbBr3@CsPbX3The surface of the core-shell structure is smooth, and the shell layer CsPbX is3The coating is compact and the defect density is less.
Description
Technical Field
The invention belongs to the field of perovskite photoelectric materials, and particularly relates to a polyhedral CsPbBr3@CsPbX3A core-shell perovskite heterojunction and a preparation method thereof.
Background
In recent years, halide perovskites have excellent performances such as adjustable band gap, high light absorption coefficient, high defect tolerance, high quantum yield, high carrier mobility and the like, and are ideal candidate materials for application in photoelectric devices such as photoelectric detectors, light emitting diodes, lasers, photovoltaic cells and the like. Despite the great advantages, poor stability remains a major drawback limiting the practical application and future commercialization of halogen-based perovskites. By coating a compact shell on the perovskite single crystal to form a core-shell structure, not only can the stability of halide perovskite under severe environment be improved, but also more importantly, the luminescent property can be improved, the surface defect can be reduced, the non-radiative recombination can be inhibited, and the carrier transportation can be enhanced.
The soft ionic bond nature and low lattice energy of halide perovskite nanocrystals leads to the formation of surface defects, making halide vacancy-forming energies low, creating material instability, but also favoring the formation of heterojunctions. The core-shell structure is also a special heterostructure, and a proper shell layer can be effectively used as a physical environment barrier, so that the interaction between crystals is inhibited, the existence of a surface trap state is reduced, the controllability of the band gap width is realized, the luminescent performance is improved, and the relative stability of the material in the environment is improved.
In the reported literature, the perovskite core-shell heterostructure is prepared by a liquid phase method, and the prepared core-shell heterostructure is damaged to a certain extent due to the wrapping effect of a surfactant. The crystal surface defect is large, the non-radiative recombination is serious, and the application of the perovskite core-shell structure in the field of photoelectric devices is seriously influenced. Therefore, how to find a simple method for preparing a perovskite core-shell heterostructure with complete structure and few defects is urgent.
Disclosure of Invention
The invention aims to provide a polyhedron CsPbBr3@CsPbX3A core-shell perovskite heterojunction and a preparation method thereof; the preparation method is simple, and the obtained CsPbBr3@CsPbX3The surface of the core-shell structure is smooth, and the shell layer CsPbX is3Compact and defective packageThe density is less.
In order to solve the technical problems, the invention adopts the following technical scheme:
provides a polyhedron CsPbBr3@CsPbX3Core-shell perovskite heterojunction, polyhedral CsPbBr3As core, CsPbX3Is a shell layer, wherein X is Cl or I. The polyhedron CsPbBr3@CsPbX3The nuclear shell ore heterojunction is tightly wrapped and has a smooth surface.
According to the scheme, the core polyhedron CsPbBr3The grain diameter is 3-5 mu m, and the shell CsPbX is3The thickness is 0.5 to 1 μm.
According to the scheme, the polyhedron CsPbBr3Is a regular tetrahedron CsPbBr3Or cubic CsPbBr3。
Provides the above polyhedron CsPbBr3@CsPbX3The preparation method of the core-shell perovskite heterojunction comprises the following steps:
a quartz tube 2 is sleeved in a quartz tube 1 of the double-temperature-zone tube furnace, and a polyhedron CsPbBr is deposited on a substrate3And mixed powders of cesium halide and lead halide respectively disposed at both ends in the quartz tube 2, wherein the polyhedral CsPbBr is deposited on the substrate3The method is characterized in that the method is located in the center of a downstream area of a dual-temperature-area tubular furnace, the mixed powder of cesium halide and lead halide is located in the center of an upstream-area thermocouple of the dual-temperature-area tubular furnace, the temperature of the upstream area of the dual-temperature-area tubular furnace is set to be 540-700 ℃, the temperature of the downstream area of the dual-temperature-area tubular furnace is set to be 270-330 ℃, and the polyhedron CsPbBr is prepared through reaction in an inert gas atmosphere3@CsPbX3A core-shell heterojunction, wherein X is Cl or I.
According to the scheme, the ratio of the outer diameters of the quartz tube 1 to the quartz tube 2 is 4: (1-3).
According to the above scheme, cesium halide and lead halide are mixed equimolar.
According to the scheme, the polyhedron CsPbBr3The molar ratio of the cesium halide to the cesium halide is 1: 0.5-2.
According to the scheme, the flow rate of the inert gas is controlled to be 80-150 sccm.
According to the scheme, the reaction time is 10-30 min.
According to the scheme, the substrate is SiO2a/Si substrate.
According to the scheme, the polyhedron CsPbBr3Is a regular tetrahedron CsPbBr3Or cubic CsPbBr3。
According to the scheme, the regular tetrahedron CsPbBr3The preparation method comprises the following steps:
reacting CsBr and PbBr2Fully grinding the mixture, placing the ground mixture in the central position of an upstream zone thermocouple in a quartz tube 1 in a dual-temperature zone tube furnace, placing a substrate in a quartz tube 3 and then in the central position of a downstream zone thermocouple in the quartz tube 1, setting the temperature of the upstream zone of the dual-temperature tube furnace to be 580-650 ℃, the temperature of the downstream zone to be 300-380 ℃, and reacting in an inert gas atmosphere to prepare the normal Cstetrahedron PbBr3。
Preferably, the flow rate of the inert gas is controlled to be 50-300 sccm.
Preferably, the reaction time is 10-30 min.
Preferably, CsBr and PbBr2Mixing in an equimolar way.
Preferably, the ratio of the outer diameters of the quartz tube 1 to the quartz tube 3 is 4: (1-3).
Preferably, the substrate is SiO2a/Si substrate.
Preferably, the specific steps are as follows: setting the temperature of an upstream area of the double-temperature tube furnace to be 580-650 ℃, the temperature of a downstream area to be 300-380 ℃, and accurately controlling the flow rate of the inert gas to be 50-300 sccm through a flowmeter; keeping the introduction of argon in the reaction process, closing a flow meter and an argon bottle pressure relief valve after the temperature control program is finished, and taking out a sample in time to obtain a regular tetrahedron CsPbBr with uniform size3。
According to the scheme, the cube CsPbBr3The preparation method comprises the following steps:
reacting CsBr and PbBr2Fully grinding the mixture, placing the ground mixture in the center of a thermocouple in an upstream area of a dual-temperature-area tubular furnace, placing a substrate in the center of a thermocouple in a downstream area, setting the temperature of the upstream area of the dual-temperature-area tubular furnace to be 580-670 ℃, the temperature of the downstream area to be 320-360 ℃, and reacting in an inert gas atmosphere to prepare the cube CsPbBr3。
Preferably, the flow rate of the inert gas is controlled to be 30-200 sccm.
Preferably, the reaction time is 10-30 min.
Preferably, CsBr and PbBr2Mixing in an equimolar way.
Preferably, the substrate is SiO2a/Si substrate.
Preferably, the specific steps are as follows: setting the temperature of an upstream area of the double-temperature tube furnace to be 580-670 ℃, the temperature of a downstream area to be 320-360 ℃, and controlling the flow rate of the inert gas to be 30-200 sccm through a flowmeter; keeping the introduction of argon in the reaction process, closing a flow meter and an argon bottle decompression valve after the temperature control program is finished, and taking out a sample in time to obtain the cube CsPbBr with uniform size3。
The prior art Atmospheric Pressure Chemical Vapor Deposition (APCVD) method generally directly places the precursor and the substrate respectively on the upstream and downstream of the quartz tube of the dual-temperature-zone tube furnace, but the local heating area is too large, and the precursor gas source is delivered to the surface of the substrate in a turbulent way, so that the core CsPbBr can be generated when the method is used for the invention3Decomposition is easy to occur, and it is difficult to obtain a high-quality core-shell heterojunction. According to the invention, a small quartz tube is sleeved in the quartz tube of the double-temperature-zone tube furnace, so that the heating area of a deposition part is reduced, the precursor is conveyed downstream in a laminar flow manner, and the formed CsPbBr3@CsPbX3The nuclear shell ore heterojunction is wrapped compactly, the surface is smooth, and the defect density is small.
The invention has the following beneficial effects:
1. the invention provides a polyhedron CsPbBr3@CsPbX3Core-shell perovskite heterojunction, polyhedral CsPbBr3As core, CsPbX3The heterojunction is a shell layer and is wrapped compactly, the surface of the heterojunction is smooth, the defect degree is low, the environmental stability is good (oxidation resistance and moisture resistance), and the absorption and band gap width adjustment of a blue-green band region can be realized.
2. The invention uses polyhedron CsPbBr3Taking single crystal as core, and coating a layer of CsPbX by normal pressure chemical vapor deposition method3Perovskite, successfully synthesizing polyhedral CsPbBr3@CsPbX3A core-shell perovskite heterojunction; in the process of adopting the normal-pressure chemical vapor deposition method, a small quartz tube is sleeved in the quartz tube of the double-temperature-zone tube furnace, so that the heating area of a deposition part can be reduced, the precursor is conveyed downstream in a laminar flow manner, and the prepared core-shell heterojunction is compact in package, smooth in surface and small in defect density; meanwhile, by controlling the downstream temperature, the ion diffusion degree is smaller, and the stability of the heterojunction is effectively improved.
3. The preparation method is simple, has good repeatability, does not generate gas-liquid intermediate, has high reaction efficiency, and can be used for large-scale commercial production; compared with a liquid phase method for preparing the perovskite shell-core structure, the method greatly reduces the interface defect of the perovskite heterojunction, reduces the non-radiative recombination of current carriers and holes, has better application prospect in the field of photoelectric devices, and provides a material basis for researching the optical and electrical properties of the perovskite shell-core heterostructure.
Drawings
FIG. 1 is a process flow diagram in an embodiment of the invention.
FIG. 2 shows a regular tetrahedron CsPbBr prepared in example 1 of the present invention3Single crystal (FIGS. 1 and 2) and regular tetrahedron CsPbBr3@CsPbCl3SEM images of core-shell heterojunctions (fig. 3 and (4)).
FIG. 3 shows a regular tetrahedron CsPbBr prepared in example 1 of the present invention3@CsPbCl3And (3) performing SEM of platinum high-temperature etching on the core-shell heterojunction.
FIG. 4 shows the tetragonal form CsPbBr prepared in example 1 of the present invention3Single crystal (FIGS. 1 and 2) and cubic CsPbBr3@CsPbCl3SEM image of core-shell heterojunction (3).
FIG. 5 shows a regular tetrahedron CsPbBr prepared in example 1 of the present invention3@CsPbCl3EDS picture of core-shell heterojunction.
FIG. 6 shows a cubic CsPbBr prepared in example 1 of the present invention3@CsPbCl3EDS picture of core-shell heterojunction.
FIG. 7 shows a regular tetrahedron CsPbBr prepared in example 2 of the present invention3@CsPbCl3EDS picture of core-shell heterojunction.
FIG. 8Is the cubic CsPbBr prepared in the embodiment 2 of the invention3@CsPbCl3EDS picture of core-shell heterojunction.
FIG. 9 shows a regular tetrahedron CsPbBr prepared in example 3 of the present invention3@CsPbCl3EDS picture of core-shell heterojunction.
FIG. 10 shows a cubic CsPbBr prepared in example 3 of the present invention3@CsPbCl3EDS picture of core-shell heterojunction.
FIG. 11 shows a regular tetrahedron CsPbBr prepared in example 4 of the present invention3@CsPbI3EDS picture of core-shell heterojunction.
FIG. 12 shows a cubic CsPbBr prepared in example 4 of the present invention3@CsPbI3EDS picture of core-shell heterojunction.
FIG. 13 shows a regular tetrahedron CsPbBr prepared in example 1 of the present invention3Cubic CsPbBr3Tetrahedral CsPbBr3@CsPbCl3Core-shell heterojunction, cubic CsPbBr3@CsPbCl3Steady state photoluminescence spectra of core-shell heterojunctions.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1
Polyhedron (regular tetrahedron, cube) CsPbBr3@CsPbCl3The preparation method of the core-shell heterojunction comprises the following specific steps:
(1) preparation of a precursor: 0.074g CsBr and 0.126g PbBr were weighed on an electronic balance2The powder was fully ground in a mortar, and 0.100g of ground powder was weighed and placed in a combustion boat No. 1 for use. Weighing 0.056g CsCl and 0.093g PbCl2The powder was fully ground in a mortar, 0.100g of ground powder was weighed out and put in a No. 2 burner boat for later use or 0.065g of CsI and 0.115g of PbI were weighed out2The powder was sufficiently ground in a mortar, and 0.100g by mass of the ground powder was weighed and placed in a combustion boat No. 3 for use.
(2)SiO2Preparation of the Si substrate: using a diamond pen to seal 4 inches of SiO2Substrate of/Si (commercially available)Put in a crystal of fertilizer combining department) to be cut into a substrate of 1cm multiplied by 1cm, and the cut SiO is put2Putting the/Si substrate in acetone, ethanol and ultrapure water respectively, performing ultrasonic treatment for 15min, and taking out SiO2the/Si substrate was blow-dried with ultra-pure argon (purity 99.999%) and placed on a porcelain boat for further use.
(3) Preparation of CsPbBr of regular tetrahedron with uniform size3Single crystal: placing the mixed powder of the No. 1 combustion boat obtained in the step 1 in the central position of a thermocouple in an upstream area in a quartz tube of a double-temperature-area tube furnace (the outer diameter of the quartz tube is 80mm), and placing the SiO obtained in the step 22The Si substrate is sleeved in a small quartz tube (with the outer diameter of 50mm and the length of 12cm) and placed in the center of a thermocouple in the downstream area in the quartz tube of the dual-temperature-zone tube furnace, the temperature of the upstream area of the dual-temperature-zone tube furnace is accurately set to be 610 ℃, the temperature of the downstream area of the dual-temperature-zone tube furnace is accurately set to be 350 ℃, and the flow rate of argon gas is accurately controlled to be 100sccm through a flowmeter; keeping the introduction of argon in the reaction process, closing a flow meter and an argon bottle decompression valve when the temperature control program is finished (the reaction time is 20min), and taking out a sample in time3The reaction scheme is shown in figure 1 (2).
(4) Preparation of CsPbBr in uniform size cube3Single crystal: placing the mixed powder obtained in the step 1 in the central position of a thermocouple in an upstream area in a quartz tube (the outer diameter of the quartz tube is 80mm) of the double-temperature-area tube furnace, and placing the SiO powder obtained in the step 22The method comprises the following steps that a/Si substrate is placed in the center of a thermocouple in the downstream area in a quartz tube of the double-temperature-area tube furnace, the temperature of the upstream area of the double-temperature-area tube furnace is accurately set to be 610 ℃, the temperature of the downstream area of the double-temperature-area tube furnace is set to be 350 ℃, and the flow rate of argon is accurately controlled to be 100sccm through a flowmeter; keeping the introduction of argon in the reaction process, closing a flow meter and an argon bottle decompression valve after a temperature control program is finished (the reaction time is 20min), and taking out a sample in time3The reaction scheme is shown in figure 1 (1).
(5) Preparation of polyhedral CsPbBr3@CsPbX3(X ═ Cl, I) core-shell heterojunction: a small quartz tube 2 (with the outer diameter of 50mm and the length of 60cm) is sleeved in a quartz tube 1 (with the outer diameter of 80mm) of the double-temperature-zone tube furnace, and a polyhedron CsPbBr is deposited on a substrate3(step 3 the regular tetrahedron CsPbBr3Or the cube CsPbBr obtained in the step 43) And CsCl and PbCl obtained in step 12The mixed powder (No. 2 combustion boat) is respectively arranged at two ends of a quartz tube 2, wherein the polyhedron CsPbBr3Placed in the downstream region of a two-temperature-region tube furnace, CsCl and PbCl2The mixed powder is placed in the center of a thermocouple in the upstream area of the two-temperature area tube furnace. Accurately setting the temperature of an upstream area of the double-temperature tube furnace to be 650 ℃, the temperature of a downstream area of the double-temperature tube furnace to be 290 ℃, and accurately controlling the flow rate of argon to be 100sccm through a flowmeter; keeping the introduction of argon in the reaction process, closing a flow meter and an argon bottle decompression valve after a temperature control program is finished (the reaction time is 20min), and taking out a sample in time3@CsPbCl3The reaction scheme of the core-shell heterojunction is shown in figure 1 (3).
FIG. 2 shows a regular tetrahedron CsPbBr prepared in example 1 of the present invention3Single crystal (FIGS. 1 and 2) and regular tetrahedron CsPbBr3@CsPbCl3SEM images of core-shell heterojunctions (fig. 3 and (4)); FIG. 4 shows the tetragonal form CsPbBr prepared in example 1 of the present invention3Single crystal (FIGS. 1 and 2) and cubic CsPbBr3@CsPbCl3SEM image of core-shell heterojunction (3). The results of fig. 2 and 4 show that: the core polyhedron CsPbBr3The grain diameter is 3-5 mu m, and the shell CsPbCl is3The thickness is 0.5 to 1 μm. Obtaining the regular tetrahedron and cube CsPbBr3@CsPbCl3The surface morphologies of the core-shell heterojunction are respectively shown in fig. 2(4), 4(3), it can be seen that a polyhedron (regular tetrahedron, cube) forms a clear core-shell wrapping structure, the edge has an obvious layering phenomenon, and compared with the polyhedron CsPbBr before wrapping3As shown in FIGS. 2(2), 4(2), CsPbBr3@CsPbCl3The junction of the side surface of the core-shell heterojunction is smooth, and CsPbBr is obviously wrapped3@CsPbCl3A core-shell structure.
FIG. 3 shows CsPbBr3@CsPbCl3The core-shell heterojunction is partially decomposed at high temperature, CsPbBr3With CsPbCl3Can observe obvious heterogeneous interface between the two, which shows that CsPbBr3@CsPbCl3And (3) successfully preparing the core-shell heterojunction.
As shown in the figure5. 6 Single particle polyhedron CsPbBr3@CsPbCl3The core-shell heterojunction was subjected to Energy Dispersive Spectroscopy (EDS) analysis. FIG. 5 shows a regular tetrahedron CsPbBr3@CsPbCl3The contents of Cs, Pb, Cl and Br elements of the core-shell heterojunction are respectively 18.33%, 18.87%, 56.69% and 6.11%; cubic CsPbBr shown in FIG. 63@CsPbCl3The contents of Cs, Pb, Cl and Br elements of the core-shell heterojunction are respectively 17.75%, 20.71%, 56.23% and 5.90%. Wherein the atomic content ratio of Cs, Pb and Cl is close to 1:1:3, description of regular tetrahedron, cube CsPbBr3@CsPbCl3The core-shell heterojunction is successfully prepared, the content of Br element in the regular tetrahedron and the tetragonal core-shell heterojunction is only 6.11 percent and 5.90 percent respectively, and further indicates that Br is-In CsPbBr3@CsPbCl3The ion diffusion degree of the core-shell heterojunction interface is small.
The steady-state photoluminescence spectrum obtained by excitation with 375nm laser, see FIG. 13, is comparable to that of regular tetrahedron CsPbBr3Regular tetrahedron CsPbBr3@CsPbCl3The photoluminescence peak position of the core-shell heterojunction was red-shifted from 530nm to 445 nm. Compared with the cube CsPbBr3Cubic CsPbBr3@CsPbCl3The photoluminescence peak position of the core-shell heterojunction was blue-shifted from 520nm to 460 nm. CsPbBr3@CsPbCl3The photoluminescence peak position of the core-shell heterojunction generates obvious blue shift, which indicates that the compact coated CsPbBr is formed3@CsPbCl3The core-shell heterojunction realizes adjustable absorption of a blue-green band region.
Example 2
Polyhedron (regular tetrahedron, cube) CsPbBr3@CsPbCl3The preparation method of the core-shell heterojunction comprises the following specific steps:
SiO2the/Si substrate was the same as in step 1 of example 1 above.
The precursor preparation was the same as in step 2 of example 1 above.
Preparation of CsPbBr with uniform size3The regular tetrahedron single crystal was the same as in step 3 of example 1 above.
Preparation of CsPbBr of uniform size3 Cubic single crystalStep 4 of example 1.
(5) Preparation of polyhedral CsPbBr3@CsPbCl3Core-shell heterojunctions: a small quartz tube 2 (with the outer diameter of 50mm and the length of 60cm) is sleeved in a quartz tube 1 (with the outer diameter of 80mm) of the double-temperature-zone tube furnace, and a polyhedron CsPbBr is deposited on a substrate3(step 3 the regular tetrahedron CsPbBr3Or the cube CsPbBr obtained in the step 43) And CsCl and PbCl obtained in step 12The mixed powder is respectively arranged at two ends of a quartz tube 2, wherein the polyhedron CsPbBr3Placed in the downstream region of a two-temperature-region tube furnace, CsCl and PbCl2The mixed powder (No. 2 combustion boat) was placed in the center of the thermocouple in the upstream zone of the two-zone tube furnace. Accurately setting the upstream area temperature of the double-temperature tube furnace to be 650 ℃, the downstream area temperature to be 330 ℃, and accurately controlling the argon flow rate to be 100sccm through a flowmeter; keeping the introduction of argon in the reaction process, closing a flow meter and an argon bottle decompression valve after a temperature control program is finished (the reaction time is 20min), and taking out a sample in time3@CsPbCl3A core-shell heterojunction.
For single-particle polyhedra (tetrahedron, cube) CsPbBr as shown in FIGS. 7 and 83@CsPbCl3The core-shell heterojunction was subjected to Energy Dispersive Spectroscopy (EDS) analysis. Regular tetrahedron CsPbBr3@CsPbCl3The contents of Cs, Pb, Cl and Br elements of the core-shell heterojunction are respectively 16.63%, 18.48%, 43.02% and 21.87%, and the cubic CsPbBr3@CsPbCl3The contents of Cs, Pb, Cl and Br elements of the core-shell heterojunction are respectively 19.38%, 19.91%, 35.90% and 24.81%. Wherein the atomic ratio of Cs, Pb, Cl and Br is close to 1:1:2:1, the content of Br element in the regular tetrahedron and the tetragonal core-shell heterojunction is 21.87 percent and 24.81 percent respectively, and further illustrates that Br is generated at the temperature of 330 DEG C-In CsPbBr3@CsPbCl3The ion diffusion degree of the core-shell heterojunction interface is increased due to Br at higher temperature-Obtains energy, breaks free from the constraint of ionic bonds, and diffuses to the interface, so that the upper limit temperature of the downstream is preferably not more than 330 ℃.
Example 3
A polyhedron (A)Regular tetrahedron, cube) CsPbBr3@CsPbCl3The preparation method of the core-shell heterojunction comprises the following specific steps:
SiO2the/Si substrate was the same as in step 1 of example 1 above.
The precursor preparation was the same as in step 2 of example 1 above.
Preparation of CsPbBr with uniform size3The regular tetrahedron single crystal was the same as in step 3 of example 1 above.
Preparation of CsPbBr of uniform size3Step 4 of cubic single crystal example 1.
(5) Preparation of polyhedral CsPbBr3@CsPbCl3Core-shell heterojunctions: a small quartz tube 2 (with the outer diameter of 50mm and the length of 60cm) is sleeved in a quartz tube 1 (with the outer diameter of 80mm) of the double-temperature-zone tube furnace, and a polyhedron CsPbBr is deposited on a substrate3(step 3 the regular tetrahedron CsPbBr3Or the cube CsPbBr obtained in the step 43) And CsCl and PbCl obtained in step 12The mixed powder is respectively arranged at two ends of a quartz tube 2, wherein the polyhedron CsPbBr3Placed in the downstream region of a two-temperature-region tube furnace, CsCl and PbCl2The mixed powder (No. 2 combustion boat) was placed in the center of the thermocouple in the upstream zone of the two-zone tube furnace. Accurately setting the temperature of an upstream area of the double-temperature tube furnace to be 650 ℃, the temperature of a downstream area of the double-temperature tube furnace to be 310 ℃, and accurately controlling the flow rate of argon to be 100sccm through a flowmeter; keeping the introduction of argon in the reaction process, closing a flow meter and an argon bottle decompression valve after a temperature control program is finished (the reaction time is 20min), and taking out a sample in time3@CsPbCl3A core-shell heterojunction.
For single-particle polyhedra (tetrahedron, cube) CsPbBr as shown in FIGS. 9 and 103@CsPbCl3The core-shell heterojunction was subjected to Energy Dispersive Spectroscopy (EDS) analysis. Regular tetrahedron CsPbBr3@CsPbCl3The element contents of Cs, Pb, Cl and Br of the core-shell heterojunction are respectively 18.00%, 16.95%, 57.77% and 7.28%, and the cubic CsPbBr3@CsPbCl3The element contents of Cs, Pb, Cl and Br of the core-shell heterojunction are 18.45%, 19.44%, 50.26% and 11.85% respectively. Wherein Cs,The atomic content ratio of Pb and Cl is close to 1:1:3, the Br atomic content in the regular tetrahedron and the tetragonal core-shell heterojunction is only 7.28 percent and 11.85 percent respectively, and further the Br is further explained at the temperature of 310 DEG C-In CsPbBr3@CsPbCl3The ion diffusion degree of the core-shell heterojunction interface is small.
Example 4
Polyhedron (regular tetrahedron, cube) CsPbBr3@CsPbI3The preparation method of the core-shell heterojunction comprises the following specific steps:
SiO2the/Si substrate was the same as in step 1 of example 1 above.
The precursor preparation was the same as in step 2 of example 1 above.
Preparation of CsPbBr with uniform size3The regular tetrahedron single crystal was the same as in step 3 of example 1 above.
Preparation of CsPbBr of uniform size3Step 4 of cubic single crystal example 1.
(5) Preparation of polyhedral CsPbBr3@CsPbI3Core-shell heterojunctions: a small quartz tube 2 (with the outer diameter of 50mm and the length of 60cm) is sleeved in a quartz tube 1 (with the outer diameter of 80mm) of the double-temperature-zone tube furnace, and a polyhedron CsPbBr is deposited on a substrate3(step 3 the regular tetrahedron CsPbBr3Or the cube CsPbBr obtained in the step 43) And CsI and PbI obtained in step 12The mixed powder is respectively arranged at two ends of a quartz tube 2, wherein the polyhedron CsPbBr3Placed in the downstream region of a two-temperature-region tube furnace, CsI and PbI2The mixed powder (No. 3 combustion boat) was placed in the center of the thermocouple in the upstream zone of the two-zone tube furnace. Accurately setting the temperature of an upstream area of the double-temperature tube furnace to be 610 ℃, the temperature of a downstream area to be 290 ℃, and accurately controlling the flow rate of argon to be 100sccm through a flowmeter; keeping the introduction of argon in the reaction process, and taking out a sample in time after the temperature control program is finished (the reaction time is 20min, a flow meter and an argon bottle decompression valve are closed, and the method can obtain the polyhedron CsPbBr with uniform size and compact package3@CsPbI3A core-shell heterojunction.
As shown in FIGS. 11 and 12, for single-particle polyhedron CsPbBr3@CsPbI3Core-shell heteroThe mass junctions were analyzed by Energy Dispersive Spectroscopy (EDS). Regular tetrahedron CsPbBr3@CsPbI3The element contents of Cs, Pb, I and Br of the core-shell heterojunction are respectively 17.95%, 21.78%, 51.08% and 9.18%, and the cubic CsPbBr3@CsPbI3The element contents of Cs, Pb, I and Br of the core-shell heterojunction are 16.42%, 21.8%, 48.24% and 13.53% respectively. Wherein the atom content ratio of Cs, Pb and I is close to 1:1:3, the Br atom content in the regular tetrahedron and the tetragonal core-shell heterojunction is only 9.18 percent and 13.53 percent respectively, and further illustrates that Br is generated at 290 ℃ under the temperature-In CsPbBr3@CsPbI3The ion diffusion degree of the core-shell heterojunction interface is small.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. Polyhedral CsPbBr3@CsPbX3The core-shell perovskite heterojunction is characterized in that in the core-shell perovskite heterojunction, the polyhedron CsPbBr is3As core, CsPbX3Is a shell layer, wherein X is Cl or I.
2. The core-shell perovskite heterojunction as claimed in claim 1, wherein the core polyhedron CsPbBr3The grain diameter is 3-5 mu m, and the shell CsPbX is3The thickness is 0.5 to 1 μm.
3. The core-shell perovskite heterojunction as claimed in claim 1, wherein the polyhedron CsPbBr3Is a regular tetrahedron CsPbBr3Or cubic CsPbBr3。
4. The polyhedron CsPbBr of claims 1 to 33@CsPbX3The preparation method of the core-shell perovskite heterojunction is characterized by comprising the following steps:
a quartz tube 2 is sleeved in a quartz tube 1 of the double-temperature-zone tube furnace, and a polyhedron CsPbBr is deposited on a substrate3And mixed powders of cesium halide and lead halide respectively disposed at both ends in the quartz tube 2, wherein the polyhedral CsPbBr is deposited on the substrate3The method is characterized in that the method is located in the center of a downstream area of a dual-temperature-area tubular furnace, the mixed powder of cesium halide and lead halide is located in the center of an upstream-area thermocouple of the dual-temperature-area tubular furnace, the temperature of the upstream area of the dual-temperature-area tubular furnace is set to be 540-700 ℃, the temperature of the downstream area of the dual-temperature-area tubular furnace is set to be 270-330 ℃, and the polyhedron CsPbBr is prepared through reaction in an inert gas atmosphere3@CsPbX3A core-shell heterojunction, wherein X is Cl or I.
5. The production method according to claim 4, wherein the ratio of the outer diameters of the quartz tube 1 and the quartz tube 2 is 4: (1-3).
6. The method according to claim 4, wherein cesium halide and lead halide are mixed equimolar; the polyhedron CsPbBr3The molar ratio of the cesium halide to the cesium halide is 1: 0.5-2.
7. The method according to claim 4, wherein the flow rate of the inert gas is controlled to be 80 to 150 sccm; the reaction time is 10-30 min.
8. The method according to claim 4, wherein CsPbBr is polyhedral3Is a regular tetrahedron CsPbBr3Or cubic CsPbBr3。
9. The method according to claim 8,
when the polyhedron CsPbBr3Is a regular tetrahedron CsPbBr3When, it is prepared as follows: reacting CsBr and PbBr2Mixing, grinding, placing in the central position of thermocouple at upstream region in quartz tube 1, placing substrate in quartz tube 3, placing in the central position of thermocouple at downstream region in quartz tube 1, and setting for double-temperature tube furnaceThe temperature of the upstream area is 580-650 ℃, the temperature of the downstream area is 300-380 ℃, and the regular tetrahedron CsPbBr is prepared by reaction in an inert gas atmosphere3；
When the polyhedron CsPbBr3Is cubic CsPbBr3When, it is prepared as follows: reacting CsBr and PbBr2Fully grinding the mixture, placing the ground mixture in the center of a thermocouple in an upstream area of a dual-temperature-area tubular furnace, placing a substrate in the center of a thermocouple in a downstream area, setting the temperature of the upstream area of the dual-temperature-area tubular furnace to be 580-670 ℃, the temperature of the downstream area to be 320-360 ℃, and reacting in an inert gas atmosphere to prepare the cube CsPbBr3。
10. The production method according to claim 9,
preparation of regular tetrahedron CsPbBr3The method comprises the following steps: CsBr and PbBr2Equimolar mixing, the ratio of the outside diameters of the quartz tube 1 and the quartz tube 3 was 4: (1-3); the substrate is SiO2a/Si substrate; controlling the flow rate of the inert gas to be 50-300 sccm; the reaction time is 10-30 min;
preparation of cubic CsPbBr3The method comprises the following steps: CsBr and PbBr2Equimolar mixing, the substrate is SiO2a/Si substrate; controlling the flow rate of the inert gas to be 30-200 sccm; the reaction time is 10-30 min.
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