CN111326951A - Perovskite micro-ring resonator array, preparation method and application thereof - Google Patents
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- H01S5/00—Semiconductor lasers
- H01S5/10—Construction or shape of the optical resonator, e.g. extended or external cavity, coupled cavities, bent-guide, varying width, thickness or composition of the active region
- H01S5/1082—Construction or shape of the optical resonator, e.g. extended or external cavity, coupled cavities, bent-guide, varying width, thickness or composition of the active region with a special facet structure, e.g. structured, non planar, oblique
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- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
- 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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- G—PHYSICS
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- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/12007—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind forming wavelength selective elements, e.g. multiplexer, demultiplexer
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
- G02B6/13—Integrated optical circuits characterised by the manufacturing method
Abstract
The invention discloses a perovskite micro-ring resonator array, a preparation method and application thereof, belonging to the technical field of perovskite crystal patterning3Limiting the precursor solution in the middle of a template with a microstructure, heating to ensure that perovskite crystals nucleate and crystallize along the edge of the microstructure of the protruding part on the template, removing the template after crystallization is finished, and finally preparing MAPbBr3Micro-ring resonator arrayAnd (4) columns. The main principle is that the edge of the micro-column structure protruding from the template is utilized to induce crystallization, the crystallization process is controlled at the edge of the micro-column, and finally the micro-ring resonator array with the shape consistent with the shape and the size of the structure of the template micro-column array is obtained.
Description
Technical Field
The invention belongs to the technical field of perovskite crystal patterning, and particularly relates to a perovskite micro-ring resonator array, a preparation method and application thereof.
Background
In recent years, the development of optoelectronic information technology requires higher integration level of optoelectronic devices, and thus, due to the advantages of compact structure, high integration level, rich functions and the like, microring resonators are widely used as one of basic construction elements in photonic integrated systems. Although the preparation process of the micro-ring is mature and simple in other material systems, the micro-ring resonator is difficult to realize in the perovskite material system due to the inherent crystallization tendency. At present, the main preparation method of the perovskite micro-ring resonator is to control the crystal shape through polystyrene spheres. However, this method faces difficulties in achieving controllability of the size, designability of the shape, and accuracy of the position of the micro-ring resonator of the perovskite.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problems to be solved by the invention are as follows: a perovskite micro-ring resonator array, a preparation method and application thereof are provided. The invention relates to organic and inorganic hybrid perovskite MAPbBr3Limiting the precursor solution in the middle of a template with a microstructure, heating to ensure that perovskite crystals nucleate and crystallize along the edge of the microstructure of the protruding part on the template, removing the template after crystallization is finished, and finally preparing MAPbBr3An array of microring resonators. The main principle is that the edge of the micro-column structure protruding from the template is utilized to induce crystallization, the crystallization process is controlled at the edge of the micro-column, and finally the micro-ring resonator array with the shape consistent with the shape and the size of the structure of the template micro-column array is obtained.
The invention is realized by the following technical scheme:
a preparation method of a perovskite micro-ring resonator array comprises the following specific steps:
(1) preparing a template;
the method comprises the following specific steps: preparing a master template by utilizing a photoetching process: firstly, sequentially carrying out ultrasonic treatment on a silicon wafer for 2min by using acetone, ethanol and deionized water, then wiping the silicon wafer clean by using ethanol absorbent cotton, washing the silicon wafer by using deionized water and then drying the silicon wafer; then spin-coating SU8-2025 photoresist on the clean silicon wafer and pre-baking; then, exposing the spin-coated photoresist SU8-2025 through a mask plate with an opaque dot array by using ultraviolet light; finally, post-baking and developing the exposed sample to obtain a silicon master template with a micron-scale concave structure array;
uniformly mixing a polydimethylsiloxane prepolymer and a curing agent, centrifuging to remove bubbles, spin-coating on a silicon main template, curing at 95 ℃, and obtaining the polydimethylsiloxane template with the convex micro-column structure array after curing;
(2) organic-inorganic hybrid perovskite MAPbBr3Preparing a precursor solution;
the method comprises the following specific steps: mixing powdered MABr and PbBr2Respectively dissolving the raw materials in N, N-dimethylformamide according to the molar ratio of 1: 1; then the two solutions are uniformly mixed and heated and stirred uniformly to obtain the organic-inorganic hybrid perovskite MAPbBr3Precursor solution;
(3) preparing an organic-inorganic hybrid perovskite micro-ring resonator array;
the method comprises the following specific steps: firstly, cleaning a glass sheet serving as a substrate according to the cleaning method in the step (1), then covering a polydimethylsiloxane template with a micro-column array structure prepared in the step (1) on the glass substrate, and then dropwise adding the organic-inorganic hybrid perovskite MAPBBr prepared in the step (2) into the polydimethylsiloxane template3Heating the precursor solution on a heating table until the solvent is completely volatilized and crystallized, and finally removing the polydimethylsiloxane template to obtain MAPbBr3An array of microring resonators.
Further, the size of the silicon wafer in the step (1) is 25 × 25mm, the thickness is 1-2mm, the amount of SU8-2025 photoresist used for spin coating is 1-5ml, the spin coating rotation speed and time are 1500-4000rmp and 20-30s, the pre-baking temperature and time are 60-85 ℃ and 15-30min respectively, the post-baking temperature and time are 15-30min respectively, the weight ratio of the prepolymer of polydimethylsiloxane to the curing agent is 1:1, the centrifugation time is 5-15min, the spin coating rotation speed and time of polydimethylsiloxane are 150-450rmp and 10-40s respectively, the curing temperature and time of polydimethylsiloxane are 80-100 ℃ and 30-90min respectively, and the diameter of the prepared microcolumn on the polydimethylsiloxane template is 5-150 micrometers and the height is 1-10 micrometers.
Further, the synthesized organic-inorganic hybrid perovskite MAPbBr in the step (2)3The concentration of the precursor solution is 10-30 wt%, the heating and stirring temperature is 60 ℃, and the time is 8 hours.
Further, the size of the glass substrate in the step (3) is 25 × 25mm, the thickness is 100-1000 μm, the volume of the MAPbBr3 precursor solution is 10-30 μ L, the heating temperature of the heating stage is 60-80 ℃, and the heating time is 2-10 min.
The invention also provides the application of the perovskite micro-ring resonator array as a laser resonant cavity, namely the preparation method of the perovskite micro-ring resonator array has designable shape and controllable size and is suitable for being used as a laser resonant cavity.
Compared with the prior art, the invention has the following advantages:
(1) the preparation method of the perovskite micro-ring resonator array can realize MAPbBr with adjustable size, designable shape and controllable position3The micro-ring resonator array has huge application potential in integrated optoelectronic systems and related fields;
(2) organic-inorganic hybrid perovskite micro-ring resonator array MAPbBr prepared by using preparation method of perovskite micro-ring resonator array3The method has the advantages of short time consumption in the preparation process, no need of complex microstructure technology for preparing the template and easy batch preparation, and is suitable for industrial production;
(3) organic-inorganic hybrid perovskite micro-ring resonator array MAPbBr prepared by using preparation method of perovskite micro-ring resonator array3Has uniform and complete appearance and is suitable for preparing high-quality laser resonators.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a perovskite micro-ring resonator array according to the present invention;
FIG. 2 is a scanning electron microscope image of a PDMS template of a perovskite micro-ring resonator array of the present invention, wherein: a is a front view, b is a 30-degree inclined view;
FIG. 3 is a fluorescent microscope image of a perovskite microring resonator array of the present invention;
FIG. 4 is a scanning electron microscope image of a perovskite micro-ring resonator array of the present invention;
FIG. 5 is a partially enlarged scanning electron microscope image of a perovskite micro-ring resonator array according to the present invention;
FIG. 6 is an atomic force microscope image of a single micro-ring in a perovskite micro-ring resonator array of the present invention;
FIG. 7 is a scanning electron microscope image of resonant cavities of different shapes of a perovskite micro-ring resonator array of the present invention, wherein a is a triangle, b is a square, c is a regular pentagon, d is a regular hexagon, and e is a pentagon-shaped ring resonator;
FIG. 8 is a schematic diagram of a perovskite microring resonator array of the present invention as a laser resonator;
FIG. 9 shows a laser emission spectrum of a perovskite micro-ring resonator array under 400nm laser pumping according to the present invention;
FIG. 10 is a graph of the relationship between the fluorescence intensity and the pumping intensity of a perovskite micro-ring resonator array of the present invention;
FIG. 11 shows laser emission patterns of different size resonators of a perovskite microring resonator array of the present invention.
Detailed Description
Example 1
A perovskite micro-ring resonator array is prepared by subjecting perovskite MAPbBr to chemical mechanical polishing3The precursor solution is limited between the template and the substrate, solvent evaporation is promoted by heating, the solution shrinks to the junction of the template micro-column structure and the substrate to form a circle of high-concentration precursor solution surrounding the micro-column, crystallization is started to surround the micro-column after the concentration reaches a value to form annular crystals, and the micro-ring resonator array corresponding to the template structure is obtained after the template is uncovered.
A perovskite micro-ring resonator array comprises the following specific steps:
(1) preparing a template;
the method comprises the specific steps of preparing a master template by utilizing a photoetching process, namely ultrasonically treating a silicon wafer with the size of 25 × 25mm and the thickness of 1mm for 2min by using acetone, ethanol and deionized water in sequence, cleaning the silicon wafer by using ethanol absorbent cotton, washing the cleaned silicon wafer by using the deionized water, drying the cleaned silicon wafer for 15min at the temperature of 90 ℃, spin-coating 3ml of photoresist SU8-2025 on the cleaned silicon wafer at the rotating speed of 3000rmp for 30s to form a uniform thin film with the thickness of 1-10 mu m, baking the thin film in an oven at the temperature of 80 ℃ for 15min to finish pre-baking, exposing the spin-coated photoresist SU8-2025 for 1min by using ultraviolet light through a mask with a non-light-transmission point circular array with other shapes, and finally post-baking the exposed sample at the temperature of 90 ℃ for 15min and developing the sample for 30s to obtain the silicon master template with a micron-scale concave structure array.
Uniformly mixing a polydimethylsiloxane prepolymer and a curing agent in a weight ratio of 10:1, centrifuging for 5min to remove bubbles, spin-coating the mixture on a silicon main template at a rotating speed of 300rmp for 30s, and curing at 95 ℃ for 45 min. And after the curing is finished, the polydimethylsiloxane template with the convex micro-column structure array with the height of 4 microns can be obtained.
(2) Organic-inorganic hybrid perovskite MAPbBr3Preparing a precursor solution;
the method comprises the following specific steps: powdered MABr and PbBr were added in amounts of 0.1 g and 3.28 g, respectively2Respectively dissolving the components in N, N-dimethylformamide with the weight of 0.3 g and 0.98 g; then the two solutions are uniformly mixed and heated and stirred for 8 hours at the temperature of 60 ℃ to obtain 25 wt% organic-inorganic hybrid perovskite MAPbBr3And (3) precursor solution.
(3) Preparing an organic-inorganic hybrid perovskite micro-ring resonator array;
the method comprises the specific steps of firstly ultrasonically treating a silicon wafer with the size of 25 × 25mm and the thickness of 0.1mm for 2min by using acetone, ethanol and deionized water in sequence, then cleaning the silicon wafer by using ethanol absorbent cotton, washing the silicon wafer by using deionized water, drying the silicon wafer at the temperature of 90 ℃ for 15min, and then drying the silicon wafer with the microcolumns prepared in the step (1)Covering a polydimethylsiloxane template with an array structure on a cleaned glass substrate, and dripping 1 mu L of 25 wt% organic-inorganic hybrid perovskite MAPBBr on the polydimethylsiloxane template3Precursor solution, heating the system on a 60 deg.C heating table for 5min until the solvent is completely volatilized and crystallized, and finally removing the polydimethylsiloxane template to obtain MAPbBr3An array of microring resonators.
As can be seen from fig. 1, the formation of the micro-ring structure only requires dropping a small amount of precursor solution on the substrate, heating for several minutes, and removing the template after crystallization is completed, so as to obtain the micro-ring resonator of the array.
As can be seen from fig. 2, the size and shape of the template are uniform and programmable.
As can be seen from fig. 3, the obtained micro-rings have bright fluorescence under excitation of the 405 nm laser, and the luminescence of all the micro-rings is very uniform, suggesting that the obtained micro-rings have high crystalline quality. The dark areas represent the substrate without crystals, which indicates that the crystallization position is precisely controlled.
As can be seen from fig. 4 and 5, all the microrings have uniform morphology and size, which is attributed to the control of the template, each microring having superior morphology. Although the microring is a curved, string-like crystal, there are no obvious cracks and flaws.
As can be seen from fig. 6, the prepared ring resonator has not only a perfectly circular shape but also a uniform height.
As can be seen from fig. 7, triangular, square, regular pentagonal, regular hexagonal, and pentastar-shaped ring resonators can be easily manufactured using PDMS having a cylindrical structure of triangular, square, regular pentagonal, regular hexagonal, and pentastar-shaped as a template.
Example 2
Based on MAPbBr3The micro-ring resonator is applied to a laser resonant cavity.
The perovskite micro-ring resonator array has the characteristics of designable size and shape, simple preparation process and short time consumptionThe laser device has the advantage of complete appearance, and can be used as a resonator in laser equipment. Due to the MAPbBr obtained3The micro-ring is a crystal and has very good light emitting performance, so that the micro-ring can be used as a resonator and a gain medium. Under the action of certain pump light, the micro-ring resonator limits light with different specific wavelengths in the ring and amplifies and outputs the light, so that laser emission is realized.
A perovskite micro-ring resonator array is used as micro-ring resonant cavity laser, and the method comprises the following specific steps:
the procedures (1), (2) and (3) are the same as those in example 1.
(4) And preparing micro-ring resonant cavity laser: MAPbBr is obtained through the steps (1), (2) and (3)3The micro-ring resonator array can be directly used as a device under test.
(5) Laser emission test based on MAPbBr3 micro-ring resonator: the test environment is atmospheric environment, the relative humidity is 20-40%, and the temperature is 20-35 ℃. Laser light with the wavelength of 400 nanometers, which is obtained by passing laser emitted by a Ti sapphire femtosecond amplifier with the wavelength of 800 nanometers through a frequency doubling crystal, is used as a pumping source, the pulse frequency is 1kHz, and the laser light is focused on a micro-ring through an objective with the amplification factor of 40 and the numerical aperture of 0.65, as shown in figure 8. The fluorescence generated on the microring is collected by the same objective lens and coupled into a spectrometer (idus CCD, Andor) through a lens. And storing fluorescence emission data of the micro-ring under different pumping intensities, deriving the obtained spectral data, processing and mapping, and calculating the quality factor Q value of the micro-ring resonator according to a formula Q ═ lambda/delta lambda, wherein lambda is the peak wavelength and delta lambda is the peak width at half maximum. According to the formula Δ λ m ═ λ2/L[n-λ(dn/dλ)]And verifying the linear relation between the laser mode spacing and the size of the micro-rings with different sizes.
As can be seen from fig. 9, at low pump light intensity, the fluorescence of the microring exhibits a broad spontaneous emission. When the pump intensity exceeds a threshold, a series of sharp, discrete narrow peaks are observed, which demonstrates the cavity effect of the microring, with a quality factor Q greater than 800.
As can be seen from FIG. 10, the threshold of the prepared MAPbBr3 micro-ring resonator laser is 70.8 μ J/cm2。
As can be seen from fig. 11, laser emission with different mode numbers was obtained in the microrings with different sizes. The method can realize the regulation and control of the laser mode by regulating and controlling the size of the laser resonator, and has great significance for the practical application of the perovskite micro-ring resonator.
Claims (6)
1. A preparation method of a perovskite micro-ring resonator array is characterized by comprising the following specific steps:
(1) preparing a template;
the method comprises the following specific steps: preparing a master template by utilizing a photoetching process: firstly, sequentially carrying out ultrasonic treatment on a silicon wafer for 2min by using acetone, ethanol and deionized water, then wiping the silicon wafer clean by using ethanol absorbent cotton, washing the silicon wafer by using deionized water and then drying the silicon wafer; then spin-coating SU8-2025 photoresist on the clean silicon wafer and pre-baking; then, exposing the spin-coated photoresist SU8-2025 through a mask plate with an opaque dot array by using ultraviolet light; finally, post-baking and developing the exposed sample to obtain a silicon master template with a micron-scale concave structure array;
uniformly mixing a polydimethylsiloxane prepolymer and a curing agent, centrifuging to remove bubbles, spin-coating on a silicon main template, curing at 95 ℃, and obtaining the polydimethylsiloxane template with the convex micro-column structure array after curing;
(2) organic-inorganic hybrid perovskite MAPbBr3Preparing a precursor solution;
the method comprises the following specific steps: mixing powdered MABr and PbBr2Respectively dissolving the raw materials in N, N-dimethylformamide according to the molar ratio of 1: 1; then the two solutions are uniformly mixed and heated and stirred uniformly to obtain the organic-inorganic hybrid perovskite MAPbBr3Precursor solution;
(3) preparing a perovskite micro-ring resonator array;
the method comprises the following specific steps: firstly, cleaning a glass sheet serving as a substrate according to the cleaning method in the step (1), then covering the polydimethylsiloxane template with the micro-column array structure prepared in the step (1) on the glass substrate, and connectingThen, dripping the organic-inorganic hybrid perovskite MAPbBr prepared in the step (2) into a polydimethylsiloxane template3Heating the precursor solution on a heating table until the solvent is completely volatilized and crystallized, and finally removing the polydimethylsiloxane template to obtain MAPbBr3An array of microring resonators.
2. The method for preparing the perovskite micro-ring resonator array as claimed in claim 1, wherein the size of the silicon wafer in the step (1) is 25 × 25mm, the thickness is 1-2mm, the amount of SU8-2025 photoresist used for spin coating is 1-5ml, the spin coating rotation speed and time are 1500-4000rmp and 20-30s, the pre-baking temperature and time are 60-85 ℃ and 15-30min respectively, the post-baking temperature and time are 15-30min respectively, the weight ratio of the prepolymer of the polydimethylsiloxane to the curing agent is 1:1, the centrifugation time is 5-15min, the rotation speed and time of the spin coating polydimethylsiloxane is 150-450rmp and 10-40s respectively, the curing temperature and time of the polydimethylsiloxane are 80-100 ℃ and 30-90min respectively, the diameter of the prepared micro-pillar on the polydimethylsiloxane template is 5-150 μm, and the height is 1-10 μm.
3. The method for preparing the perovskite micro-ring resonator array as claimed in claim 1, wherein the synthesized organic-inorganic hybrid perovskite MAPbBr in the step (2)3The concentration of the precursor solution is 10-30 wt%, the heating and stirring temperature is 60 ℃, and the time is 8 hours.
4. The method for preparing the perovskite micro-ring resonator array as claimed in claim 1, wherein the size of the glass substrate in the step (3) is 25 × 25mm, the thickness is 100-1000 μm, the volume of the MAPbBr3 precursor solution is 10-30 μ L, the heating temperature of the heating stage is 60-80 ℃, and the heating time is 2-10 min.
5. A perovskite microring resonator array prepared by the method of any one of claims 1 to 4.
6. Use of an array of perovskite microring resonators as claimed in claim 5 in a laser resonator.
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