CN111313238B - Tapered perovskite micro-nano crystal laser and preparation method thereof - Google Patents

Tapered perovskite micro-nano crystal laser and preparation method thereof Download PDF

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CN111313238B
CN111313238B CN202010133021.6A CN202010133021A CN111313238B CN 111313238 B CN111313238 B CN 111313238B CN 202010133021 A CN202010133021 A CN 202010133021A CN 111313238 B CN111313238 B CN 111313238B
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nano crystal
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CN111313238A (en
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杨中民
徐涛
虞华康
刘旺旺
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South China University of Technology SCUT
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/30—Structure or shape of the active region; Materials used for the active region
    • H01S5/36—Structure or shape of the active region; Materials used for the active region comprising organic materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S5/00—Semiconductor lasers
    • H01S5/04—Processes or apparatus for excitation, e.g. pumping, e.g. by electron beams
    • H01S5/041—Optical pumping
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S2304/00—Special growth methods for semiconductor lasers
    • H01S2304/06—LPE

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Abstract

The invention discloses a conical perovskite micro-nano crystal laser and a preparation method thereof. The method is realized by a solution method and comprises the following steps: firstly, preparing a perovskite precursor solution with a certain concentration, quantitatively dripping the solution on a substrate containing the perovskite material seed crystal at room temperature, placing the substrate in a closed environment of an anti-solvent, and volatilizing the solvent after a period of time to obtain the tapered perovskite micro-nano crystal. The preparation method has the advantages of simple equipment, high speed, convenience, simple operation, low cost, high repeatability, good appearance and excellent laser behavior, the high-purity micro-nano crystal improves various performances of the semiconductor laser, reduces the threshold value of the semiconductor laser, improves the stability of the laser, the conical crystal inhibits axial resonance, good whispering gallery mode single-mode laser can be generated at an angular direction, and the preparation method has high application value.

Description

Tapered perovskite micro-nano crystal laser and preparation method thereof
Technical Field
The invention belongs to the field of micron and nanometer semiconductor photoelectric materials, and particularly relates to a conical perovskite micro-nano crystal laser and a preparation method thereof.
Background
The micron/nanometer semiconductor photoelectric material is a novel photoelectric functional material and is a hot subject of current scientific research. Because the size of the micro-nano structure unit is in the micron-nano level, the physical and chemical properties of the micro-nano material and the micro-nano structure are different from those of microscopic atoms, molecules and macroscopic objects, and therefore the cognitive field of people is extended to the intermediate field between the macroscopic objects and the microscopic objects. In the field of microelectronics, smaller size means more complex chips, faster reaction, lower price, lower energy consumption, better performance. However, the micro-nano material device still has a certain distance from wide industrial application, and further theoretical research and technical challenges are needed.
The lead trihalide perovskite has longer carrier service life, longer carrier diffusion length and higher carrier mobility, and is a photoelectric material with great development prospect. The excellent performances enable the halogenated lead perovskite material to be widely applied to the aspects of solar cells, light emitting diodes, photoelectric detectors, lasers and the like. At present, although the CH has various regular shapes3NH3PbX3Perovskite micro-nano lasers (X is halogen) have been studied preliminarily, for example, in the literature (Zhu, H.; Fu, Y.; Meng, F.; Wu, X.; Gong, Z.; Ding, Q.; Gustafsson, M. V.; Trinh, M. T.; Jin, S.; Zhu, X. Y., Lead halide perovskite nanolaser with low laser threshold and high quality factors).Nature Materials 2015,14636.), report perovskite nanometer line laser, but the FP chamber that the nanometer line constitutes is mostly with multimode laser outgoing, only the short chamber that the shorter nanometer line (length is less than 10 μm) constitutes can realize single mode laser outgoing, and the short chamber again can lead to gain inadequately, and the outgoing laser intensity is low.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a tapered perovskite micro-nano crystal laser and a preparation method thereof.
The invention aims to provide a method for preparing a tapered perovskite micro-nano crystal laser.
The purpose of the invention is realized by at least one of the following technical solutions.
The method for preparing the tapered perovskite micro-nano crystal laser is a solution method, and comprises the following steps:
preparing perovskite precursor solution with a certain concentration, wherein the fluorescent material used by the invention is organic-inorganic hybrid perovskite CH3NH3PbX3The solvent is chromatographic grade DMF and GBL, and is mixed according to a certain proportion. At room temperature, dropwise adding a certain amount of prepared perovskite precursor solution into the solution containing CH3NH3PbX3A seed crystal on a substrate and placing it in a chamber containing CH3NH3PbX3Saturated evaporation of insoluble solventsStanding for a period of time in a sealed environment of steam, and volatilizing the solvent to obtain the tapered perovskite micro-nano crystal. And transferring the crystal onto a glass sheet, and pumping by 400nm femtosecond laser to obtain laser emitted by the tapered perovskite micro-nano crystal after reaching a threshold value.
The invention provides a method for preparing a tapered perovskite micro-nano crystal laser, which comprises the following steps:
(1) adding a certain amount of lead halide and methyl ammonium halide into a solvent, and uniformly mixing to obtain a perovskite precursor solution;
(2) dropwise adding the perovskite precursor solution obtained in the step (1) on a substrate containing perovskite material seed crystals to obtain a dropwise added substrate;
(3) and (3) placing the substrate dropwise added in the step (2) in an anti-solvent gas environment, diffusing the anti-solvent into the dropwise added precursor solution to cause crystallization, and volatilizing the solvent to obtain the tapered perovskite micro-nano crystal on the substrate, namely the tapered perovskite micro-nano crystal laser, which has better laser behavior.
Further, the perovskite material in the step (1) is organic-inorganic hybrid perovskite CH3NH3PbX3And X is halogen.
Further, the solvent in the step (1) is a mixed solution of DMF and GBL; the volume ratio of DMF to GBL is 1: 20-1: 8. the DMF (dimethylformamide) and GBL (gamma-butyrolactone) are both in chromatographic grade.
Further, the concentration of the precursor solution in the step (1) is 10-30 mmol/L.
Further, the substrate containing the perovskite material seed crystal in the step (2) is a glass substrate containing the perovskite material seed crystal; the perovskite material seed crystal in the step (2) is the perovskite material seed crystal in the step (1); the perovskite material seed crystal is obtained by reacting a lead halide film on a glass substrate with a methyl ammonium halide solution.
Further, the lead halide film is obtained by dripping 0.2-1.5 mol/L lead halide solution on a substrate and drying; the concentration of the methyl ammonium halide solution is 4-20 mg/mL. The solvent of the lead halide solution is chromatographic grade DMF. The solvent of the methyl ammonium halide solution is chromatographic grade isopropanol.
Preferably, the drying is: oven drying at 90 deg.C for 30 min.
Further, the pressure of the anti-solvent gas environment in the step (3) is the saturated vapor pressure at room temperature. The environment is a relatively temperature stable environment.
Further, the antisolvent in the step (3) is chloroform; the volatilization time is longer than 12h so as to completely volatilize the liquid.
The invention provides a conical perovskite micro-nano crystal laser prepared by the preparation method, and the laser emitted by the conical perovskite micro-nano crystal can be obtained by pumping through 400nm femtosecond laser.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the preparation method provided by the invention, organic and inorganic hybrid perovskite is used as a raw material, and crystallization is controlled by an anti-solvent diffusion method to prepare a micro-nano crystal;
(2) according to the tapered perovskite micro-nano crystal laser provided by the invention, as the crystal is tapered in the axial direction (such as a micron line in fig. 1, fig. 2 and fig. 3), the end face loss is very large, the start oscillation of an axial FP mode is inhibited, the radial dimension of the crystal can support the start oscillation of a Whispering Gallery Mode (WGM), the radial dimension is small, the laser obtained by resonance is generally single-mode laser (such as fig. 4), and under the condition of uniform pumping, the laser can be emitted in the radial direction of the whole crystal (such as an optical microscope photo in fig. 4), so that the single-mode laser with higher power can be obtained. In addition, the laser can also be applied to scenes such as a laser array and the like;
(3) according to the preparation method provided by the invention, the used instruments and equipment are simple to operate, the preparation method is short in time consumption and small in raw material amount, multiple targets of economy, environmental protection, energy conservation and the like are realized, single-mode laser with high energy can be obtained, and the application of a micro-nano laser is facilitated.
Drawings
FIG. 1 is a scanning electron micrograph of a tapered perovskite micro-nano crystal laser obtained in example 1;
FIG. 2 is a scanning electron micrograph of the tapered perovskite micro-nano crystal laser obtained in example 2;
FIG. 3 is a scanning electron micrograph of the tapered perovskite micro-nano crystal laser obtained in example 3;
FIG. 4 shows the laser photograph, laser spectrum and scanning electron micrograph of the sample obtained by pumping the obtained product with 400nm femtosecond laser.
Detailed Description
The following examples are presented to further illustrate the practice of the invention, but the practice and protection of the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
In the following examples, organic-inorganic hybrid perovskite material MAPbBr is used3For illustration purposes.
Example 1
0.1145g of lead bromide and 0.035g of methylammonium bromide were weighed and dissolved in a mixed solvent of 1mL of DMF and 8mL of GBL to obtain a precursor solution. Preparing 0.2mol/L lead bromide solution, wherein the solvent is DMF. 4mg/mL of methyl ammonium bromide solution is prepared, and the solvent is isopropanol. 10 mu L of lead bromide solution is dripped on a cleaned glass sheet (with the size of 20 x 20 mm), and the glass sheet is placed in an oven at 90 ℃ to be dried to obtain a lead bromide film. Placing the obtained lead bromide film in 2mL of 4mg/mL methyl ammonium bromide solution for reaction for 5min to obtain MAPbBr3And (4) taking out the seed crystal, dripping 30 mu L of precursor solution on the seed crystal, placing the seed crystal in a closed container containing chloroform saturated steam, and standing for 24 hours. After the solvent is volatilized, the cone-shaped micro-nano crystal (as shown in figure 1) can be obtained. The micro-nano crystal is a conical micro-nano crystal laser.
Example 2
0.1145g of lead bromide and 0.035g of methylammonium bromide were weighed and dissolved in a mixed solvent of 1mL of DMF and 9mL of GBL to obtain a precursor solution. Preparing 0.5mol/L lead bromide solution, wherein the solvent is DMF.8mg/mL of methyl ammonium bromide solution is prepared, and the solvent is isopropanol. 10 mu L of lead bromide solution is dripped on a cleaned glass sheet (with the size of 20 x 20 mm), and the glass sheet is placed in an oven at 90 ℃ to be dried to obtain a lead bromide film. Placing the obtained lead bromide film in 2mL of 8mg/mL methyl ammonium bromide solution for reaction for 5min to obtain MAPbBr3And (4) taking out the seed crystal, dripping 30 mu L of precursor solution on the seed crystal, placing the seed crystal in a closed container containing chloroform saturated steam, and standing for 24 hours. After the solvent is volatilized, the cone-shaped micro-nano crystal (as shown in figure 2) can be obtained. The micro-nano crystal is a conical micro-nano crystal laser.
Example 3
0.1145g of lead bromide and 0.035g of methylammonium bromide were weighed and dissolved in a mixed solvent of 1mL of DMF and 20mL of GBL to obtain a precursor solution. 1.5mol/L lead bromide solution is prepared, and the solvent is DMF. Preparing 20mg/mL methyl ammonium bromide solution, wherein the solvent is isopropanol. 10 mu L of lead bromide solution is dripped on a cleaned glass sheet (with the size of 20 x 20 mm), and the glass sheet is placed in an oven at 90 ℃ to be dried to obtain a lead bromide film. Placing the obtained lead bromide film in 2mL of 20mg/mL methyl ammonium bromide solution for reaction for 5min to obtain MAPbBr3And (4) taking out the seed crystal, dripping 30 mu L of precursor solution on the seed crystal, placing the seed crystal in a closed container containing chloroform saturated steam, and standing for 24 hours. After the solvent is volatilized, the cone-shaped micro-nano-crystal (as shown in figure 3) can be obtained. The micro-nano crystal is a conical micro-nano crystal laser.
The axial length of the micro-nano crystals is mainly distributed in the range of 5-30 μm, and the radial dimension is in the range of 1-3 μm. The laser emitted by the conical micro-nano crystal can be obtained by pumping with 400nm femtosecond laser.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.

Claims (8)

1. The preparation method of the conical perovskite micro-nano crystal laser is characterized by comprising the following steps:
(1) adding lead halide and methyl ammonium halide into a solvent, and uniformly mixing to obtain a perovskite precursor solution;
(2) dropwise adding the perovskite precursor solution obtained in the step (1) on a substrate containing perovskite material seed crystals to obtain a dropwise added substrate; the substrate containing the perovskite material seed crystal is a glass substrate containing the perovskite material seed crystal; the perovskite material seed crystal is the perovskite material seed crystal in the step (1); the perovskite material seed crystal is obtained by reacting a lead halide film on a glass substrate with a methyl ammonium halide solution;
(3) and (3) placing the substrate dropwise added in the step (2) in an anti-solvent gas environment, diffusing the anti-solvent into the dropwise added precursor solution to cause crystallization, and volatilizing the solvent to obtain the tapered perovskite micro-nano crystal on the substrate, namely the tapered perovskite micro-nano crystal laser.
2. The preparation method of the tapered perovskite micro-nano crystal laser according to claim 1, wherein the perovskite precursor material in the step (1) is organic-inorganic hybrid perovskite CH3NH3PbX3And X is halogen.
3. The preparation method of the tapered perovskite micro-nano crystal laser according to claim 1, wherein the solvent in the step (1) is a mixed solution of DMF and GBL; the volume ratio of DMF to GBL is 1: 20-1: 8.
4. the preparation method of the tapered perovskite micro-nano crystal laser according to claim 1, wherein the concentration of the perovskite precursor solution in the step (1) is 10-30 mmol/L.
5. The preparation method of the conical perovskite micro-nano crystal laser according to claim 1, wherein the lead halide thin film is obtained by dripping 0.2-1.5 mol/L lead halide solution on a substrate and drying; the concentration of the methyl ammonium halide solution is 4-20 mg/mL.
6. The method for preparing a tapered perovskite micro-nano crystal laser according to claim 1, wherein the anti-solvent gas environment in the step (3) is saturated steam at room temperature.
7. The preparation method of the tapered perovskite micro-nano crystal laser according to claim 1, wherein the anti-solvent in the step (3) is chloroform; the anti-solvent is an insoluble solvent of perovskite; the volatilization time is longer than 12h, so that the liquid is completely volatilized.
8. The conical perovskite micro-nano crystal laser prepared by the preparation method of any one of claims 1 to 7 is characterized in that laser emitted by conical perovskite micro-nano crystals can be obtained by pumping with 400nm femtosecond laser.
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CN112349846A (en) * 2019-08-09 2021-02-09 杭州纤纳光电科技有限公司 Seed crystal and method for preparing perovskite solar cell by using same
CN114292195A (en) * 2021-12-29 2022-04-08 青岛科技大学 Method for designing white-light perovskite through strain regulation

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CN110387223A (en) * 2019-07-11 2019-10-29 浙江大学 A kind of hydroxyl halogen lead ore/lead halogen perovskite composite micro-nano rice material and preparation method thereof
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CN105140419A (en) * 2015-07-03 2015-12-09 北京大学 Quick film forming method based on low-concentration organic-inorganic hybrid perovskite solution
CN105405979A (en) * 2015-12-03 2016-03-16 中国科学院半导体研究所 Preparation method of organic and inorganic hybrid perovskite single crystal
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