CN113300206A - Wavelength tunable laser generation method based on perovskite thin film - Google Patents
Wavelength tunable laser generation method based on perovskite thin film Download PDFInfo
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- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
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Abstract
The invention relates to the technical field of laser, and discloses a wavelength tunable laser generation method based on a perovskite film, which comprises the following steps: mixing methyl amine iodide and methyl amine bromide in a molar ratio of 1-x: x, blending, and adding an isopropanol solvent to form a post-treatment solution; coating the post-treatment solution on the surface of the perovskite film in a spin coating manner, then carrying out annealing treatment, and then cooling to room temperature; packaging the perovskite thin film; controlling the temperature of the perovskite thin film to be a certain constant temperature between-80 ℃ and 25 ℃; the pumping light is focused and then irradiates the surface of the perovskite film to form pumping light spots; the modulated light forms an irradiation light spot which is completely overlapped with the pumping light spot on the surface of the perovskite film after being focused; the modulation frequency, the duty ratio and the light intensity of the modulated light are controlled, and the continuous adjustability of the output wavelength is realized. The wavelength of the output laser can be continuously adjusted by adjusting the modulation frequency of the light, and the laser has good repeatability and stability.
Description
Technical Field
The invention relates to the technical field of laser, in particular to a wavelength tunable laser generation method based on a perovskite thin film.
Background
A wavelength tunable laser is a laser that can continuously vary the laser output wavelength over a range. The laser can be widely applied to the fields of spectral analysis, communication, biomedicine and the like. According to the actual requirement, the control unit of the laser is adjusted to change the output wavelength of the laser.
The perovskite material has good optical absorption coefficient and higher luminous quantum efficiency, so that the material has great application prospect in the fields of luminescent devices, laser devices and the like, and is widely concerned by researchers. It has been found that the band gap of perovskite materials is related to the proportion of the halogen component. Research shows that laser materials with different output wavelengths can be prepared by changing the proportion of halogen components, people can realize the control of the output wavelengths by replacing the laser materials with different components, and obviously, the method has great limitation. The method brings inconvenience to people in the actual use process, increases the cost of the system, cannot realize continuous adjustment of the wavelength, and even can damage and pollute the laser system.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a perovskite film-based wavelength tunable laser generation method, which realizes the continuous adjustment of the wavelength of output laser by adjusting the modulation frequency of light and has good repeatability and stability.
The technical scheme is as follows: the invention provides a perovskite film-based wavelength tunable laser generation method, which comprises the following steps: s1: carrying out post-treatment on the prepared perovskite thin film with the substrate: preparation of post-treatment solution: mixing methyl amine iodide and methyl amine bromide in a molar ratio of 1-x: x, adding an isopropanol solvent to form a post-treatment solution with the molar concentration of 25-35 mmol/L after blending; wherein x is in the range of 0.2 to 0.8; coating the post-treatment solution on the surface of the perovskite thin film in a spin coating manner, then carrying out annealing treatment, and then cooling to room temperature; s2: packaging the perovskite thin film obtained in the step S1; s3: controlling the temperature of the perovskite thin film to be a certain constant temperature between-80 ℃ and 25 ℃; s4: the pump light is focused and then irradiates the surface of the perovskite film to form a pump light spot; s5: the modulated light forms irradiation light spots completely coincident with the pumping light spots on the surface of the perovskite thin film after being focused; s6: and controlling the modulation frequency, the duty ratio and the light intensity of the modulated light to realize the continuous adjustability of the output wavelength.
Preferably, in S1, the annealing conditions are: heating at 95-105 deg.C for 2-7 min.
Preferably, the main component of the perovskite thin film is CH3NH3Pb(I1-xBrx)3Wherein the value of x ranges from 0.2 to 0.8.
Preferably, the CH3NH3Pb(I1-xBrx)3The preparation method adopts a spin coating method and comprises the following specific steps: cleaning the substrate; CH (CH)3NH3Pb(I1-xBrx)3Preparing a precursor solution: iodinating an amine (CH) with a methyl group3NH3I) Iodine, iodineLead dissolving (PbI)2) Methyl amine bromide (CH)3NH3Br) and lead bromide (PbBr)2) In a molar ratio of 1-x: 1-x: x: x, adding the mixture in a volume ratio of 6: 4-9: 1 of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO), stirring for more than 12 hours at normal temperature to prepare 0.8-1.2 mol/L CH3NH3Pb(I1-xBrx)3Precursor solution; wherein x is in the range of 0.2 to 0.8; perovskite film formation: spin coating the CH on a substrate3NH3Pb(I1-xBrx)3The precursor solution is spin-coated with the CH within 15-25 seconds after the spin coating process begins3NH3Pb(I1-xBrx)3Chlorobenzene is quickly dripped on a substrate of the precursor solution; after the spin coating is finished, annealing the substrate, and then cooling to room temperature to obtain CH3NH3Pb(I1-xBrx)3A film.
Preferably, in the perovskite film forming process, the annealing treatment conditions are as follows: heating for 30-90 s at 60-70 ℃, and then transferring to 95-105 ℃ for heating for 15-25 min.
Preferably, in S2, the specific steps of packaging are as follows: and (2) dissolving polymethyl methacrylate (PMMA) in chlorobenzene to prepare a PMMA solution, and spin-coating the PMMA solution on the perovskite thin film obtained from S1 to dry.
Preferably, in S4, the pumping spot is a linear spot, and the linear spot perpendicularly intersects with the edge of the substrate, and the linear spot excites the amplified spontaneous emission or laser generated by the perovskite thin film to be collected through a lateral direction.
Preferably, in S4, the pump spot is a circular spot, and the amplified spontaneous emission or laser generated by exciting the perovskite thin film is collected by back scattering.
Preferably, in S5, the modulated light is modulated by a TTL signal, and becomes quasi-continuous light after being modulated.
Preferably, the substrate is a glass or quartz substrate.
Has the advantages that: compared with the prior art, the method has the advantages of low cost and simple operation. The wavelength modulation of amplified spontaneous emission or laser generated by the perovskite thin film can be realized only by light modulation without replacing perovskite materials, and the photoinduced phase separation effect of the mixed halide perovskite is utilized, namely, halogen ions in the thin film can be separated under the illumination of light, so that the band gap of the material is indirectly changed. And in the post-treatment process, the optical property of the film is regulated and controlled, so that the band gap of the film can be continuously adjusted. Finally, phase separation is stabilized in a certain state by modulation of continuous light, stable light output is realized, and good repeatability and stability are achieved.
Drawings
FIG. 1 is a schematic diagram of the system of the present invention;
FIG. 2 is a graph showing a relationship between amplified spontaneous emission and modulated light duty ratio of the perovskite thin film produced in embodiment 1;
FIG. 3 is a graph showing the amplified spontaneous emission stability of the perovskite thin film prepared in embodiment 1;
fig. 4 is a graph showing the relationship between the amplified spontaneous emission and the modulated light duty ratio of the perovskite thin film prepared in embodiment 2.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Embodiment 1:
the embodiment provides a wavelength tunable laser generation method based on a perovskite thin film, which mainly comprises the following steps:
1. a preparation method of perovskite film.
The main component of the perovskite thin film is CH3NH3Pb(I0.5Br0.5)3The coating is prepared by a spin coating method. The method comprises the following specific steps:
cleaning the glass substrate. Square glass with side length of 15 mm is sequentially put into a glass cleaning agent, ethanol, acetone and deionized water to be respectively ultrasonically cleaned for 15 minutes, and the glass is dried by flowing nitrogen after being cleaned.
Preparing perovskite precursor solution. Iodinating an amine (CH) with a methyl group3NH3I) Lead iodide (PbI)2) Methyl amine bromide (CH)3NH3Br) and lead bromide (PbBr)2) After blending according to the molar ratio of 0.5:0.5:0.5:0.5, adding a blending solvent of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) with the volume ratio of 4:1, stirring for more than 12 hours at normal temperature to prepare 1 mol/L CH3NH3Pb(I0.5Br0.5)3And (3) precursor solution.
③ the film forming process of perovskite. The glass substrate was placed in a spin coater and 50. mu.l of CH was added3NH3Pb(I0.5Br0.5)3And dripping the precursor solution on the substrate to ensure that the solution uniformly covers the surface of the substrate. Spin coating speed and time of the spin coater were 4000 revolutions and 30 seconds, respectively. 200. mu.l of chlorobenzene was quickly dropped on the substrate at 20 seconds after the start of the spin coating process. After the spin coating process is finished, the substrate is placed on a heating table to perform annealing operation, and after the substrate is heated at 65 ℃ for 1 minute, the substrate is transferred to 100 ℃ to be heated for 20 minutes. Finally, the prepared CH3NH3Pb(I0.5Br0.5)3And taking down the film and cooling.
Fourthly, post-treatment. Blending methyl amine iodide and methyl amine bromide in a molar ratio of 0.5:0.5, and adding an isopropanol solvent to form a post-treatment solution. The molar concentration of the solution was 30 mmol/L. Prepared CH3NH3Pb(I0.5Br0.5)3The film was placed in a spin coater, 100. mu.l of the post-treatment solution was added dropwise to CH3NH3Pb(I0.5Br0.5)3On a film to make the solution cover CH uniformly3NH3Pb(I0.5Br0.5)3The surface of the film. After waiting about 10 seconds, a spin coating operation was performed. Spin coating speed and time of the spin coater were 4000 revolutions and 30 seconds, respectively. And after the rotary coating process is finished, placing the substrate on a heating table to perform annealing operation, heating at 100 ℃ for 5 minutes, and then taking down and cooling.
And fifthly, packaging. Polymethyl methacrylate (PMMA) was dissolved in chlorobenzene to prepare a PMMA solution of 100 mg/ml. Post-treated CH3NH3Pb(I0.5Br0.5)3The film was placed in a spin coater and 100. mu.l of PMMA solution was added dropwise to the film to allow the solution to cover the CH uniformly3NH3Pb(I0.5Br0.5)3After the surface of the film, a spin coating operation is performed. Spin coating speed and time of the spin coater were 4000 revolutions and 30 seconds, respectively. After the rotary coating process is finished, the film is taken down and dried, and finally the packaged CH is prepared3NH3Pb(I0.5Br0.5)3A film.
2. And (5) building a laser generation system.
Is prepared from3NH3Pb(I0.5Br0.5)3Film fixed in cryostat, CH3NH3Pb(I0.5Br0.5)3The temperature of the film was controlled at 240K.
And 532 nm pulse laser is adopted as the pumping light, the repetition frequency is 100 Hz, and the pulse width is about 1 ns. Pulsed light is irradiated on CH after being focused3NH3Pb(I0.5Br0.5)3On the surface of the film, a circular pumping light spot is formed, and the light intensity is about 100 micro-joules per square centimeter.
And controlling the wavelength control unit by adopting modulation light. The modulated light adopts 532 nm continuous laser, and is modulated by the photoacoustic modulator TTL, and then irradiates on the surface of the perovskite film to form irradiation light spots, and the irradiation light spots are completely coincided with the circular pumping light spots.
By controlling the modulation frequency and the light intensity of the quasi-continuous light, the continuous adjustability of the output wavelength can be realized.
1. The modulated light has an intensity of about 2 milliwatts per square centimeter and a modulation frequency of 5 Hz. It can be seen that by controlling the conditions under which light is modulated, tunability of the output wavelength can be achieved. FIG. 2 is a graph of the relationship between amplified spontaneous emission and modulated light duty cycle of a perovskite thin film, the spectra being measured under steady conditions after several periods of irradiation.
2. The light intensity of the modulated light is about 5 milliwatts per square centimeter, the modulation frequency is 1 Hz, the duty ratio is 12 percent, and the stable output of two continuous hours is realized. FIG. 3 is a schematic representation of the stability of amplified spontaneous emission of perovskite thin films.
Embodiment 2:
the embodiment provides a wavelength tunable laser generation method based on a perovskite thin film, which mainly comprises the following steps:
1. a preparation method of perovskite film.
The main component of the perovskite thin film is CH3NH3Pb(I0.78Br0.22)3The coating is prepared by a spin coating method.
Cleaning the glass substrate. Square glass with side length of 15 mm is sequentially put into a glass cleaning agent, ethanol, acetone and deionized water to be respectively ultrasonically cleaned for 15 minutes, and the glass is dried by flowing nitrogen after being cleaned.
② in the preparation of perovskite precursor solution, methyl amine iodide (CH)3NH3I) Lead iodide (PbI)2) Methyl amine bromide (CH)3NH3Br) and lead bromide (PbBr)2) After blending according to the molar ratio of 0.78:0.78:0.22:0.22, adding a blending solvent of N, N-Dimethylformamide (DMF) and dimethyl sulfoxide (DMSO) according to the volume ratio of 7:3, stirring for more than 12 hours at normal temperature to prepare 1 mol/L CH3NH3Pb(I0.78Br0.22)3And (3) precursor solution.
③ the film forming process of perovskite. The glass substrate was placed in a spin coater and 50. mu.l of CH was added3NH3Pb(I0.78Br0.22)3And dripping the precursor solution on the substrate to ensure that the solution uniformly covers the surface of the substrate. Spin coating speed and time of the spin coater were 4000 revolutions and 30 seconds, respectively. 200. mu.l of chlorobenzene was quickly dropped on the substrate at 20 seconds after the start of the spin coating process. After the spin coating process is finished, the substrate is placed on a heating table to perform annealing operation, and after the substrate is heated at 70 ℃ for 1 minute, the substrate is transferred to 95 ℃ to be heated for 20 minutes. Finally, willPrepared CH3NH3Pb(I0.78Br0.22)3And taking down the film and cooling.
Fourthly, post-treatment. Blending methyl amine iodide and methyl amine bromide in a molar ratio of 0.78:0.22, and adding an isopropanol solvent to form a post-treatment solution. The molar concentration of the solution was 35 mmol/L. Prepared CH3NH3Pb(I0.78Br0.22)3The film was placed in a spin coater, 100. mu.l of the post-treatment solution was added dropwise to CH3NH3Pb(I0.78Br0.22)3On a film to make the solution cover CH uniformly3NH3Pb(I0.78Br0.22)3The surface of the film. After waiting about 10 seconds, a spin coating operation was performed. Spin coating speed and time of the spin coater were 4000 revolutions and 30 seconds, respectively. And after the rotary coating process is finished, placing the substrate on a heating table to perform annealing operation, heating at 100 ℃ for 4 minutes, and then taking down and cooling.
And fifthly, packaging. Polymethyl methacrylate (PMMA) was dissolved in chlorobenzene to prepare a PMMA solution of 100 mg/ml. Post-treated CH3NH3Pb(I0.78Br0.22)3The film was placed in a spin coater and 100. mu.l of PMMA solution was added dropwise to the film to allow the solution to cover the CH uniformly3NH3Pb(I0.78Br0.22)3After the surface of the film, a spin coating operation is performed. Spin coating speed and time of the spin coater were 4000 revolutions and 30 seconds, respectively. After the rotary coating process is finished, the film is taken down and dried, and finally the packaged CH is prepared3NH3Pb(I0.78Br0.22)3A film.
2. And (5) building a laser generation system.
Is prepared from3NH3Pb(I0.78Br0.22)3Film fixed in cryostat, CH3NH3Pb(I0.78Br0.22)3The temperature of the film was controlled at 300K.
② pump light adopts 532 nm pulse laserThe repetition frequency is 50 Hz and the pulse width is about 1 ns. Pulsed light is irradiated on CH after being focused3NH3Pb(I0.78Br0.22)3On the surface of the film, a circular pumping spot is formed with an intensity of about 150 microjoules per square centimeter.
And controlling the wavelength control unit by adopting modulation light. The modulated light adopts 532 nm continuous laser, and is modulated by the photoacoustic modulator TTL, and then irradiates on the surface of the perovskite film to form irradiation light spots, and the irradiation light spots are completely coincided with the circular pumping light spots.
The modulated light has an intensity of about 80 milliwatts per square centimeter and a modulation frequency of 5 Hz. It can be seen that by controlling the conditions under which light is modulated, tunability of the output wavelength can be achieved. FIG. 4 is a graph of the relationship between amplified spontaneous emission and modulated light duty cycle of a perovskite thin film, the spectra being measured under steady conditions after several periods of irradiation.
Embodiment 3:
the quartz grating is selected as the substrate, and the laser radiation output can be realized by selecting any one of the two implementation modes. The half-wave width of the output laser peak is narrower compared with the amplified spontaneous emission, so that the laser has better monochromaticity.
The above embodiments are merely illustrative of the technical concepts and features of the present invention, and the purpose of the embodiments is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A wavelength tunable laser generation method based on a perovskite thin film is characterized by comprising the following steps:
s1: carrying out post-treatment on the prepared perovskite thin film with the substrate:
preparation of post-treatment solution: mixing methyl amine iodide and methyl amine bromide in a molar ratio of 1-x: x, adding an isopropanol solvent to form a post-treatment solution with the molar concentration of 25-35 mmol/L after blending; wherein x is in the range of 0.2 to 0.8;
coating the post-treatment solution on the surface of the perovskite thin film in a spin coating manner, then carrying out annealing treatment, and then cooling to room temperature;
s2: packaging the perovskite thin film obtained in the step S1;
s3: controlling the temperature of the perovskite thin film to be a certain constant temperature between-80 ℃ and 25 ℃;
s4: the pump light is focused and then irradiates the surface of the perovskite film to form a pump light spot;
s5: the modulated light forms irradiation light spots completely coincident with the pumping light spots on the surface of the perovskite thin film after being focused;
s6: and controlling the modulation frequency, the duty ratio and the light intensity of the modulated light to realize the continuous adjustability of the output wavelength.
2. The method for wavelength tunable laser generation of perovskite thin film as claimed in claim 1, wherein in S1, the annealing conditions are: heating at 95-105 deg.C for 2-7 min.
3. The method of claim 1, wherein the perovskite thin film comprises a major component of CH3NH3Pb(I1-xBrx)3Wherein the value of x ranges from 0.2 to 0.8.
4. The perovskite thin film based wavelength tunable laser generation method of claim 3, wherein the CH3NH3Pb(I1-xBrx)3The preparation method adopts a spin coating method and comprises the following specific steps:
cleaning the substrate;
CH3NH3Pb(I1-xBrx)3preparing a precursor solution: mixing methyl amine iodide, lead iodide, methyl amine bromide and lead bromide in a molar ratio of 1-x: 1-x: x: x, adding the mixture in a volume ratio of 6: 4-9: 1N, N-dimethylformamide and dimethylStirring the mixed solvent of the base sulfoxide for more than 12 hours at normal temperature to prepare 0.8-1.2 mol/L CH3NH3Pb(I1-xBrx)3Precursor solution;
perovskite film formation:
spin coating the CH on a substrate3NH3Pb(I1-xBrx)3The precursor solution is spin-coated with the CH within 15-25 seconds after the spin coating process begins3NH3Pb(I1-xBrx)3Chlorobenzene is quickly dripped on a substrate of the precursor solution; after the spin coating is finished, annealing the substrate, and then cooling to room temperature to obtain CH3NH3Pb(I1-xBrx)3A film.
5. The method for wavelength tunable laser generation of perovskite thin film as claimed in claim 4, wherein the annealing conditions during the perovskite film formation are as follows: heating for 30-90 s at 60-70 ℃, and then transferring to 95-105 ℃ for heating for 15-25 min.
6. The method for producing wavelength tunable laser based on perovskite thin film as claimed in any one of claims 1 to 5, wherein in S2, the steps of packaging are as follows:
and (3) dissolving the polymethyl methacrylate in chlorobenzene to prepare a polymethyl methacrylate solution, and spin-coating the polymethyl methacrylate solution on the perovskite thin film obtained in S1 to dry.
7. The method for generating perovskite thin film-based wavelength tunable laser according to any one of claims 1 to 5, wherein in S4, the pumping light spot is a linear light spot, and the linear light spot is perpendicularly intersected with the edge of the substrate, and the linear light spot excites amplified spontaneous emission or laser generated by the perovskite thin film to be collected through lateral direction.
8. The method for generating perovskite thin film-based wavelength tunable laser according to any one of claims 1 to 5, wherein in S4, the pump spot is a circular spot, and the amplified spontaneous emission or laser generated by exciting the perovskite thin film by the circular pump spot is collected by back scattering.
9. The method for producing a perovskite thin film-based wavelength tunable laser as claimed in any one of claims 1 to 5, wherein the modulated light is modulated by TTL signal and becomes quasi-continuous light in S5.
10. The perovskite thin film based wavelength tunable laser generation method of any one of claims 1 to 5, wherein the substrate is a glass or quartz substrate.
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| US20190062175A1 (en) * | 2017-08-30 | 2019-02-28 | Florida State University Research Foundation, Inc. | Bandgap-tunable perovskite materials and methods of making the same |
| CN109473557A (en) * | 2018-11-05 | 2019-03-15 | 长春工业大学 | A kind of preparation method of hybrid inorganic-organic perovskite optoelectronic film sensor |
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| US20190062175A1 (en) * | 2017-08-30 | 2019-02-28 | Florida State University Research Foundation, Inc. | Bandgap-tunable perovskite materials and methods of making the same |
| CN109473557A (en) * | 2018-11-05 | 2019-03-15 | 长春工业大学 | A kind of preparation method of hybrid inorganic-organic perovskite optoelectronic film sensor |
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Application publication date: 20210824 Assignee: Shanghai Houfei Energy Technology Co.,Ltd. Assignor: HUAIYIN INSTITUTE OF TECHNOLOGY Contract record no.: X2022320000360 Denomination of invention: Wavelength tunable laser generation based on perovskite thin films Granted publication date: 20220318 License type: Common License Record date: 20221210 |