CN116073219B - Preparation method of all-inorganic perovskite liquid laser based on micro-flow channel - Google Patents

Preparation method of all-inorganic perovskite liquid laser based on micro-flow channel Download PDF

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CN116073219B
CN116073219B CN202310366590.9A CN202310366590A CN116073219B CN 116073219 B CN116073219 B CN 116073219B CN 202310366590 A CN202310366590 A CN 202310366590A CN 116073219 B CN116073219 B CN 116073219B
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CN116073219A (en
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陈沛然
吴昱廷
刘胜利
任银娟
王跃
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Nanjing University of Posts and Telecommunications
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Nanjing University of Posts and Telecommunications
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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
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/02—Constructional details
    • H01S3/022—Constructional details of liquid lasers
    • 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
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
    • H01S3/20—Liquids
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention provides a preparation method of an all-inorganic perovskite liquid laser based on a microfluidic channel, belonging to the technical field of photoelectric information and comprisingThe method comprises the following steps: all-inorganic halogen perovskite CsPbBr for preparing dodecylbenzene sulfonic acid ligand by using hot injection method 3 Quantum dot dispersion; a U-shaped flow channel is carved on the PMMA substrate by utilizing a micro control system; ultrasonic cleaning, drying and N-bonding the substrate and the bonding plate 2 0, plasma treatment; processing the optical fiber; placing the fiber cores into the flow channels, and carrying out vacuum hot-pressing packaging on the bonding plate substrate; and (3) taking the bonding steel needle as a runner inlet and outlet, and injecting the quantum dot dispersion liquid into the micro-flow channel. The prepared perovskite liquid laser realizes whispering gallery mode laser. The method provided by the invention is simple and efficient to operate, realizes excellent laser performance, and effectively makes up the short plates with high laser threshold value, multiple laser angle modes and low working stability under high power of the liquid laser in the prior art in the field of optical communication.

Description

Preparation method of all-inorganic perovskite liquid laser based on micro-flow channel
Technical Field
The invention belongs to the technical field of photoelectric information, and particularly relates to a preparation method of an all-inorganic perovskite liquid laser based on a micro-flow channel.
Background
A optofluidic laser is an emerging technology integrating microcavities, microfluidic channels and liquid gain media. It has wide application in new photon devices, such as on-chip tunable coherent light source, biological control laser and sensitive analysis of biological molecules. Photonic devices based on semiconductor colloidal Quantum Dots (QDs) have attracted considerable attention due to their ease of handling, spectral tunability over a broad wavelength range, and potentially low temperature insensitive laser thresholds.
Liquid lasers exhibit unique characteristics compared to solid state lasers that are tightly stacked with gain materials: due to the combination of the microfluidics technology and photonics, a new scheme is provided for the development of highly integrated micro photoelectric equipment, and the method has great potential in the photoelectric information application fields such as photoelectric information communication, optical encryption, laser detectors and the like.
The liquid phase gain medium is a key element constituting the liquid laser, and the iteration of the liquid phase gain medium is critical to the development of the optofluidic technology. Initially, fluorescent dyes have been widely studied as liquid gain media. In these dye liquid lasers, complex pumping and operating arrangements are required to overcome the irreversible conversion of the dye gain medium to non-fluorescent molecules in the quiescent state. Even so, dye molecules are gradually photodegradation during photoexcitation, resulting in reduced gain efficiency, requiring periodic replacement of the solution. In recent years, some reports have investigated the possibility of using CdSe-based quantum dots for liquid laser gain media, however, due to the relatively low gain factor, the pump threshold of these devices is too high to be suitable for practical use. Therefore, there is a great need to find new liquid phase gain media for developing high performance liquid lasers.
Inorganic lead halide perovskite nanocrystals are a new class of laser materials that has emerged in recent years. The greater gain factor and higher defect tolerance of inorganic lead halide perovskite nanocrystals compared to conventional CdSe-based NCs makes inorganic lead halide perovskite nanocrystals a potential liquid gain medium. However, in the past few years, despite significant progress in the development of solid lasers based on inorganic lead halide perovskite nanocrystals, liquid lasers based on inorganic lead halide perovskite nanocrystals have not been realized at a later date.
The 2014 study proposed an ideal optofluidic laser with monolayer gain, but no excellent results were technically achieved due to the technological limitations of the current semiconductor age. However, the solid-liquid mixed laser model can realize high-quality gallery type laser, and provides new possibility for the flow control technology. In the present day introduced as a new semiconductor perovskite, a perovskite material with high gain, high reabsorption coefficient and long carrier lifetime can better fit the shape model to prepare a liquid laser with higher expected effect. Experiments in 2019 prove that the storage time of the material and the luminous performance of the material can be improved by using dodecylbenzene sulfonic acid as a ligand material for preparing the perovskite quantum dots.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a preparation method of an all-inorganic perovskite liquid laser based on a micro-flow channel.
The invention solves the problems of the prior art that the liquid laser has high laser threshold value, a plurality of laser modes and low working stability under high power, and the specific technical scheme comprises the following steps:
a preparation method of an all-inorganic perovskite liquid laser based on a microfluidic channel comprises the following steps:
step 1: all-inorganic halogen perovskite CsPbBr for preparing dodecylbenzenesulfonic acid ligand 3 Quantum dot dispersion;
step 2: a U-shaped runner is carved on the PMMA substrate;
step 3: ultrasonic cleaning, drying and N-bonding the substrate and the bonding plate 2 0, plasma treatment;
step 4: siO is made of 2 Placing the fiber core into a flow channel, and carrying out vacuum hot-pressing packaging on the substrate by using a bonding plate to manufacture a chip with a micro-flow channel;
step 5: and bonding a steel needle on the microfluidic channel as a runner inlet and outlet, and injecting quantum dot dispersion liquid into the microfluidic channel to prepare a perovskite liquid laser, so as to realize whispering gallery mode laser.
Further, the all-inorganic halogen perovskite CsPbBr 3 The concentration of the quantum dot dispersion liquid is not lower than 133.0 mg mL -1 。
Further, the cross section dimension of the U-shaped flow channel is not more than 250 x 250 mu m 2 。
Further, the step 3 is specifically that the base plate and the bonding plate are ultrasonically cleaned by deionized water for 3 times at 50 ℃ for 15 minutes each time; drying in a vacuum drying oven at 80 ℃ for 30 minutes; post-utilization Plasma device N 2 0 gas treatment for 180 seconds, gas flow rate 60 sccm, vacuum pressure 30 mTorr, plasma power 170W.
Further, the SiO 2 The fiber core is made of SiO 2 After the coating layer is removed from the optical fiber, a flame stretching method is used for preparing SiO with smooth surface 2 A core.
Further, the heating rate of the vacuum hot-pressing package is 9 ℃/min, the hot-pressing temperature is 117 ℃, the hot-pressing time is 33 seconds, the cooling rate is 5 ℃/min, and the temperature is reduced to 67 ℃ and taken out.
Further, the all-inorganic halogen perovskite is a rectangular single crystal.
Further, the SiO 2 The radius of the fiber core is 12 mu m-44 mu m.
Compared with the prior art, the method provided by the invention is simple and efficient to operate and easy to realize by using simple equipment; 2. the invention prepares the liquid laser, and effectively makes up the short plate with high laser threshold and low working stability under high power of the liquid laser in the prior art.
Drawings
FIG. 1 is a schematic flow chart of the micro-fluidic chip prepared on a PMMA substrate by using a micro-control system.
FIG. 2 is a schematic diagram of CsPbBr injected with dodecylbenzenesulfonic acid (DBSA) ligand according to the invention 3 Photo of microfluidic chip of quantum dot dispersion.
Fig. 3 is a photograph of a liquid laser prepared by excitation with a femtosecond laser according to the present invention.
Fig. 4 is a graph showing the laser spectrum of the invention excited by the femtosecond laser and the laser threshold characterization of the invention under the pumping condition.
FIG. 5 is a representation of the laser threshold of the invention under pumping conditions, showing the invention at a pump of 22.7 [ mu ] J cm -2 Laser is realized.
Fig. 6 is a spectrum obtained by changing different sized fibers in a microfluidic chip according to the present invention, with corresponding changes in free spectral range and number of laser modes noted. The free spectral radius was 0.67nm when the fiber radius was 44 μm, respectively. The free spectral radius was 1.83nm at a fiber radius of 16 μm. The free spectral radius was 2.44nm at a fiber radius of 12 μm.
Fig. 7 is a graph showing the change in luminous intensity obtained by a liquid laser and a general solid-state thin-film fiber laser prepared by the same-power femtosecond laser excitation according to the present invention. The upper curve is the normalized luminous intensity of the liquid laser, and the lower curve is the normalized luminous intensity of the solid laser.
Detailed Description
The present invention is further illustrated in the accompanying drawings and detailed description which are to be understood as being merely illustrative of the invention and not limiting of its scope, and various modifications of the invention, which are equivalent to those skilled in the art upon reading the invention, will fall within the scope of the invention as defined in the appended claims.
As shown in fig. 1, an all-inorganic perovskite liquid laser based on a microfluidic channel is prepared by the following method:
step 1: all-inorganic halogen perovskite CsPbBr for preparing dodecylbenzenesulfonic acid ligand 3 Quantum dot dispersion;
step 2: a U-shaped runner is carved on the PMMA substrate;
step 3: ultrasonic cleaning, drying and N-bonding the substrate and the bonding plate 2 0, plasma treatment;
step 4: siO is made of 2 Placing the fiber core into a flow channel, and carrying out vacuum hot-pressing packaging on the substrate by using a bonding plate to manufacture a chip with a micro-flow channel;
step 5: and bonding a steel needle on the microfluidic channel as a runner inlet and outlet, and injecting quantum dot dispersion liquid into the microfluidic channel to prepare a perovskite liquid laser, so as to realize whispering gallery mode laser.
And preparing a micro-flow chip on the PMMA substrate by utilizing a micro control system (LSmicro 2020 CNC), installing a milling cutter with a proper size, setting a z-axis undercut distance, namely the engraving depth, and then setting x-axis and y-axis engraving a sample with a proper size, as shown in figure 2. The cross section size of the U-shaped runner is not more than 250 x 250 mu m 2 。
All-inorganic halogen perovskite CsPbBr for preparing dodecylbenzenesulfonic acid (DBSA) ligand by using hot injection method 3 A quantum dot dispersion, the all-inorganic halogen perovskite being a rectangular single crystal; the heat injection method is as follows: cs (cells) 2 CO 3 （0.0593 g， 0.182 mmol），Pb(OAc) 2 (0.206 g,0.54 mmol) ODE (10 mL) and dodecylbenzenesulfonic acid (1.2045 g,3.689 mmoL) were injected into a 100mL three-necked flask, and the mixture was stirred at 120Deaeration was carried out at C for half an hour under argon flow. The clear solution was maintained below 120 ℃ for an additional 30 minutes, and then a toluene solution (748 mg,1.37 mmol,2 mL) of pre-dissolved tetraoctylammonium bromide was rapidly injected into the solution of the above precursor. After 5 a s a water bath was cooled using the reaction mixture.
Ultrasonically cleaning the base plate and the bonding plate with deionized water at 50 ℃ for 3 times, each time for 15 minutes; drying in a vacuum drying oven at 80deg.C for 30 min; after drying, using Plasma equipment N 2 0 gas treatment for 180 seconds, gas flow rate 60 sccm, vacuum pressure 30 mTorr, plasma power 170W. The heating rate in the vacuum hot pressing process is 9 ℃/min, the hot pressing temperature is 117 ℃, the hot pressing time is 33 seconds, the cooling rate is 5 ℃/min, and the temperature is reduced to 67 ℃ and taken out.
SiO 2 The fiber core is made of SiO 2 After the coating layer is removed from the optical fiber, a flame stretching method is used for preparing SiO with smooth surface 2 A core.
CsPbBr of dodecylbenzenesulfonic acid (DBSA) ligand 3 The quantum dot dispersion is injected into a microfluidic chip, a smooth optical microfluidic fiber core in the microfluidic chip is used as a whispering gallery mode microcavity, and a femtosecond laser is utilized to excite the prepared liquid laser, as shown in fig. 3.
By a micro-area fluorescence test system built by a laboratory, laser performance characterization is performed under pumping conditions, a plurality of luminescence peaks appear under certain pumping intensity, and the luminescence intensity of the invention is continuously improved along with the enhancement of the pumping intensity, as shown in fig. 4.
Through a micro-area fluorescence test system built by a laboratory, laser performance characterization is performed under the pumping condition, and the luminous intensity of the microfluidic chip is found to be 22.7 mu J cm in pumping -2 The micro-fluidic chip was demonstrated to achieve laser light, as shown in figure 5.
The spectra in fig. 6 were obtained by changing different sized fibers in the microfluidic chip, and the corresponding changes in free spectral range and angular mode number are noted in the figure, with a free spectral radius of 0.67nm when the fiber radius is 44 μm, respectively. When the radius of the optical fiber was changed to 16. Mu.m, the free spectral radius was 1.83nm. When the optical fiber radius was changed to 12 μm, the free spectral radius was 2.44nm.
The luminous intensity variation diagram in fig. 7 obtained by using a liquid laser prepared by femtosecond laser excitation with the same power and a common solid-state thin-film fiber laser. Two optical fibers of the same size are used as the resonant cavities of the liquid laser and the solid film laser, respectively, and are continuously excited at room temperature for more than 4 hours (corresponding to about 1.4X10 7 Secondary laser irradiation). For liquid lasers, no significant drop in laser intensity was observed throughout the measurement. However, the laser intensity of the thin film-based solid state laser drops sharply at about 30 minutes and then gradually drops to about 56% of the initial intensity.
The line width of the liquid laser is 0.069nm, the quality factor reaches 7480, and the laser threshold is as low as 22.7 mu J cm -2 And at not less than 173.1 [ mu ] J.cm -2 Can keep the stable output power to work for the minimum 4 hours under the excitation illumination, and is high-quality liquid laser.
Characterization of optical properties:
CsPbBr as described above 3 The fluorescence spectrum of the microfluidic channel chip is characterized by a micro-area fluorescence test system built in a laboratory, the micro-area fluorescence test system is built based on a spectrometer iHR320 produced by Horiba company, an external connection microscope (RX 50M) is used for sample positioning, the excitation light wavelength is 405 nm, and the light spot size is about 10 μm.

Claims (3)

1. A preparation method of an all-inorganic perovskite liquid laser based on a microfluidic channel is characterized by comprising the following steps: the method comprises the following steps:
step 1: all-inorganic halogen perovskite CsPbBr for preparing dodecylbenzenesulfonic acid ligand 3 Quantum dot dispersion liquid, all-inorganic halogen perovskite CsPbBr 3 The concentration of the quantum dot dispersion liquid is not lower than 133.0 mg mL -1 The all-inorganic halogen perovskite is a rectangular single crystal;
step 2: a U-shaped runner is carved on a PMMA substrate, and the cross section size of the U-shaped runner is not more than 250 mu m 2 ；
Step 3: ultrasonically cleaning the substrate and bonding plate with deionized water at 50deg.C for 3 times eachSecondary 15 minutes; drying in a vacuum drying oven at 80 ℃ for 30 minutes; post-utilization Plasma device N 2 0 gas treatment for 180 seconds, gas flow rate of 60 sscm, vacuum pressure of 30 mTorr, and plasma power of 170W;
step 4: siO is made of 2 Placing fiber cores into the flow channels, vacuum thermocompression packaging the substrate with bonding plate to obtain chip with microfluidic channels, and performing vacuum thermocompression packaging on the substrate with bonding plate to obtain SiO 2 The radius of the fiber core is 12 mu m-44 mu m;
step 5: and bonding a steel needle on the microfluidic channel as a runner inlet and outlet, and injecting quantum dot dispersion liquid into the microfluidic channel to prepare a perovskite liquid laser, so as to realize whispering gallery mode laser.
2. The method for preparing the micro-fluidic channel-based all-inorganic perovskite liquid laser is characterized in that: the SiO is 2 The fiber core is made of SiO 2 After the coating layer is removed from the optical fiber, a flame stretching method is used for preparing SiO with smooth surface 2 A core.
3. The method for preparing the micro-fluidic channel-based all-inorganic perovskite liquid laser is characterized in that: the heating rate of the vacuum hot-pressing package is 9 ℃/min, the hot-pressing temperature is 117 ℃, the hot-pressing time is 33 seconds, the cooling rate is 5 ℃/min, and the temperature is reduced to 67 ℃ and taken out.
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