CN111987583B - Random laser and preparation method and application thereof - Google Patents
Random laser and preparation method and application thereof Download PDFInfo
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- CN111987583B CN111987583B CN202010906495.XA CN202010906495A CN111987583B CN 111987583 B CN111987583 B CN 111987583B CN 202010906495 A CN202010906495 A CN 202010906495A CN 111987583 B CN111987583 B CN 111987583B
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Abstract
The invention provides a random laser, which comprises a gain medium, wherein the gain medium is a graphite diyne nano sheet. The random laser adopts the graphite diyne nanosheet as a gain medium, the graphite diyne nanosheet shows excellent light emission performance in a visible light region, photon transition obeys the three-level energy structure regulation, and meanwhile, photons with broadband emission spectra of 450-700 nm and wavelengths shorter than 400nm are an effective excitation source. The invention also provides a preparation method and application of the random laser.
Description
Technical Field
The invention relates to the technical field of random lasers, in particular to a random laser, and further relates to a preparation method and application of the random laser.
Background
The solid-state laser of the semiconductor laser pump is a laser generating device which takes a laser diode sequence as a pump source and takes a solid laser material as a gain medium. The all-solid-state laser has the advantages of small volume, light weight, high efficiency, stable performance, good reliability, long service life, high beam quality and the like, and has huge market demand. The all-solid-state laser technology is one of the few high technical fields which have integral advantages from a material source to laser system integration internationally in China at present, has a good foundation for accelerating development in partial fields, and has a huge demand gap in coherent laser sources provided by disordered gain media under the condition of no reflector.
The random laser is a novel optical fiber laser, compared with a conventional solid-state laser, the angle distribution of the random laser can completely cover a solid angle of 4 pi, and due to the advantages of no resonance mode, better stability, higher reliability, simpler structure and the like, the random laser is greatly developed in the aspect of searching various new light sources such as high power/high efficiency, wide spectrum emission, low coherence and the like in recent years. The random laser is a non-traditional micro-cavity laser with the diameter of only micron magnitude, and is characterized in that the stimulated radiation phenomenon can be formed in a disordered medium with gain. In the traditional laser, a feedback mechanism is derived from the limiting effect of a laser cavity on an optical wave; in random lasers, it is the multiple scattering caused by the disorder of the medium that provides a feedback mechanism for the system. Random lasers can be embedded in the photonic crystal as light sources, and dispersed in the fluid to measure the fluid distribution; the light source can also be used as a light source in a planar light display, and is widely applied.
In addition, semiconductor nanoplatelets, such as CdSe, PbSe, ZnO and perovskite quantum dots, have been vividly studied as effective gain media, however, their biomedical toxicity, narrow tuning of light frequencies, and inherent instability of materials remain obstacles to overcome. A semiconductor nano sheet with high biocompatibility, wide adjustment and good stability is developed and applied to a random laser to become a hot spot and a difficult point.
Disclosure of Invention
In view of the above, the present invention provides a random laser, a method for manufacturing the random laser, and an application of the random laser as a light source, and provides a novel random laser to solve the defects of narrow adjustment of light frequency, inherent instability, and the like of the existing laser.
In a first aspect, the invention provides a random laser, comprising a gain medium, wherein the gain medium is a graphite diyne nanosheet.
The random laser adopts the graphite diyne nanosheet as a gain medium, the graphite diyne nanosheet shows excellent light emission performance in a visible light region, photon transition obeys the three-level energy structure regulation, and meanwhile, photons with broadband emission spectra of 450-700 nm and wavelengths shorter than 400nm are an effective excitation source. Graphite diyne nanosheets, as a disordered gain medium, can be manufactured at low cost and coated on substrates of any shape. Injection of a small gain medium into specific biological tissues can also impart unique emission characteristics and thus can be applied for biological imaging and diagnostics. The laser mode and frequency limitations in conventional lasers due to 2 pi mirror bounce have been broken by random lasers. In this case, the light will experience multiple scattering in the system, filling in spectral blanks, white laser sources, speckle-free imaging, etc.
Preferably, the gain medium is a graphite diyne film, and the graphite diyne film comprises graphite diyne nanosheets;
the area of the graphite diyne film is 1-5 cm2。
More preferably, the area of the graphite diyne film is 3cm2。
Preferably, the lattice fringes of the graphite diyne nanosheet are 0.294nm, and the Raman spectrum of the graphite diyne nanosheet has four characteristic peaks, each of which is 1378cm-1、1575cm-1、1920cm-1And 2168cm-1。
Preferably, the graphite diyne nanosheet has an X-ray photoelectron spectrum with four peaks, 284.4eV, 284.9eV, 286.2eV and 288.5eV, respectively.
In a second aspect, the present invention provides a method for preparing a random laser, comprising the following steps:
synthesizing graphite diyne: providing hexaethynylbenzene as a synthetic monomer, dissolving hexaethynylbenzene in an organic solvent to obtain a hexaethynylbenzene solution, providing a substrate, placing the substrate in the organic solvent to obtain a substrate solution, heating the substrate solution and maintaining the temperature at 55-65 ℃, and adding the hexaethynylbenzene solution into the heat-insulated substrate solution for reaction for 1-5 days at one time to obtain graphite diyne attached to the substrate;
stripping the graphite diyne film: transferring the graphite diyne attached to the substrate into a ferric chloride solution for wet stripping to obtain a graphite diyne film;
preparing a random laser: preparing a random laser by taking a graphite diyne film as a gain medium;
the substrate is a copper substrate.
The preparation method of the random laser comprises the steps of synthesizing large-area graphite diyne, stripping the graphite diyne film, preparing the random laser and the like. The most important of them is the synthesis of large-area graphite diyne. By correcting the mode of adding the monomer hexaethynylbenzene in the Glaser coupling reaction process, the original dropwise slow addition is replaced by the rapid one-time addition, the monomer concentration in unit time is ensured to be large enough, so that the coupling can be rapidly carried out on the copper substrate, and the large-size graphite diyne film is prepared by wet stripping. The nano-sheet has excellent light emission performance in a visible light region, photon transition obeys the three-level energy structure regulation, a covered broadband emission spectrum is displayed between 450-700 nm, and photons with the wavelength shorter than 400nm are an effective excitation source. The graphite diyne film prepared by the method has the advantages of simple preparation process, strong operability and the like, the thickness of the graphite diyne film can be properly adjusted according to requirements, the longer the reaction time is, the larger the film thickness is, but the film thickness cannot exceed five days, otherwise, the copper foil is decomposed due to the overlong reaction time and overhigh temperature, and finally the extraction and separation of the film are influenced.
Preferably, in the step of synthesizing graphite diyne, the organic solvent is one or more of pyridine, pyridine/methanol, ammonia/ethanol and ethylamine solution in combination. More preferably, the organic solvent is pyridine.
Preferably, in the step of synthesizing graphite diyne, the concentration of the hexaethynylbenzene in the hexaethynylbenzene solution is 0.0005-0.002M. More preferably, the concentration of hexaethynylbenzene in the hexaethynylbenzene solution is 0.001M.
Preferably, the base solution is maintained at 60 ℃ during the step of synthesizing graphite diyne.
Preferably, the hexaethynylbenzene solution is added to the incubated base solution at once for 3 days.
In a third aspect, the invention provides a use of the random laser of the first aspect in a light source device.
The application of the random laser in the light source equipment eliminates the mode and frequency limitation of the laser caused by the rebound of a 2 pi reflecting mirror in the conventional laser, and under the condition, light can undergo multiple scattering in a system, so that spectrum blanks, white laser sources, speckle-free imaging and the like can be filled.
Advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of embodiments of the invention.
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In order to more clearly illustrate the contents of the present invention, a detailed description thereof will be given below with reference to the accompanying drawings and specific embodiments.
FIG. 1 shows the optical characterization results of the graphite diyne provided by the present invention; wherein a is a linear absorption spectrum chart of the graphite diyne nanosheet; b is an emission spectrum of the graphite diyne nanosheet under different excitation wavelengths; c is the emission spectrum under 360nm excitation (the left side corresponds to 430nm, 407nm and 455nm from top to bottom, and the right side corresponds to 360 nm); d is a photoluminescence lifetime graph under 360nm excitation;
FIG. 2 is a kinetic diagram of a photoelectric carrier of graphite diyne nano-sheets provided by the invention; wherein a is an experimental transient absorption characterization chart of a graphite diyne nanosheet solution, and an inset shows a proposed photocarrier transition process; b is an overall fitting spectrogram; c is a kinetic graph of experimental results;
FIG. 3 is a graph of the random laser performance of graphite diyne nanosheets provided by the present invention;
FIG. 4 is a graph of the integrated emission intensity provided by the present invention as a function of pump wavelength at (a)390nm, (b)400nm, and (c)410nm, respectively; d is a 1931 three primary colors space chromaticity diagram of the multicolor graphite diyne random laser; and e is the photographic image of the graphite diyne random laser to be detected.
Detailed Description
While the following is a description of the preferred embodiments of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
In a first aspect, the invention provides a random laser, comprising a gain medium, wherein the gain medium is a graphite diyne nanosheet.
Preferably, the gain medium is a graphite diyne film, and the graphite diyne film comprises graphite diyne nanosheets;
the area of the graphite diyne film is 1-5 cm2。
More preferably, the area of the graphite diyne film is 3cm2。
Preferably, the lattice fringes of the graphite diyne nanosheet are 0.294nm, and the Raman spectrum of the graphite diyne nanosheet has four characteristic peaks, each of which is 1378cm-1、1575cm-1、1920cm-1And 2168cm-1。
Preferably, the graphite diyne nanosheet has an X-ray photoelectron spectrum with four peaks, 284.4eV, 284.9eV, 286.2eV and 288.5eV, respectively.
In a second aspect, the present invention provides a method for preparing a random laser, comprising the following steps:
synthesizing graphite diyne: providing hexaethynylbenzene as a synthetic monomer, dissolving hexaethynylbenzene in an organic solvent to obtain a hexaethynylbenzene solution, providing a substrate, placing the substrate in the organic solvent to obtain a substrate solution, heating the substrate solution and maintaining the temperature at 55-65 ℃, and adding the hexaethynylbenzene solution into the heat-insulated substrate solution for reaction for 1-5 days at one time to obtain graphite diyne attached to the substrate;
stripping the graphite diyne film: transferring the graphite diyne attached to the substrate into a ferric chloride solution for wet stripping to obtain a graphite diyne film;
preparing a random laser: preparing a random laser by taking a graphite diyne film as a gain medium;
the substrate is a copper substrate.
Preferably, in the step of synthesizing graphite diyne, the organic solvent is one or more of pyridine, pyridine/methanol, ammonia/ethanol and ethylamine solution in combination. More preferably, the organic solvent is pyridine.
Preferably, in the step of synthesizing graphite diyne, the substrate is sequentially placed in dilute hydrochloric acid, acetone and ethanol for ultrasonic treatment before being placed in an organic solvent.
Preferably, in the step of synthesizing graphite diyne, the concentration of the hexaethynylbenzene in the hexaethynylbenzene solution is 0.0005-0.002M. More preferably, the concentration of hexaethynylbenzene in the hexaethynylbenzene solution is 0.001M.
Preferably, the base solution is maintained at 60 ℃ during the step of synthesizing graphite diyne.
Preferably, the hexaethynylbenzene solution is added to the incubated base solution at once for 3 days.
In a third aspect, the invention provides a use of the random laser of the first aspect in a light source device.
The random laser and its preparation are described in detail below by way of specific examples.
Preparation examples
A preparation method of a random laser comprises the following steps:
synthesizing large-area graphite diyne with copper foil as a substrate: taking hexaethynylbenzene as a synthetic monomer, sequentially carrying out ultrasonic treatment on a copper foil in dilute hydrochloric acid, acetone and ethanol in advance, and placing the copper foil in a pyridine solution. The pyridine solution of hexaethynylbenzene with the concentration of 0.001M is quickly added into a reaction system at 60 ℃ for three days (the reaction time can be properly adjusted according to the thickness of the graphite alkyne to be obtained, the longer the reaction time is, the larger the film thickness is, but the film thickness can not exceed five days, otherwise, the copper foil is decomposed due to the overlong reaction time and overhigh temperature, and finally the extraction and separation of the film are influenced), and the graphite diyne attached to the copper foil is obtained by post-treatment.
And (3) wet stripping of the graphite diyne film: and then carrying out wet stripping in a ferric chloride solution to obtain the graphite diyne film.
And preparing a random laser taking graphite diyne as a gain medium.
Effect embodiment:
and (3) characterization of graphite diyne nanosheets. The linear optical absorption spectrum of the graphite diyne nano-sheet is shown in figure 1 a. Three weak absorption shoulders were observed at 260nm, 318nm and 367 nm. As shown in fig. 1b, the graphite diyne solution is highly transparent to light with a wavelength of more than 420nm, consistent with photoluminescence excitation spectra. Photoluminescence is well characterized by excitation at different wavelengths of 280 to 400nm, which cover the absorption band well. The emission spectra remained consistent with previous reports and the reproducibility remained after half a month. However, the emission band is independent of the excitation wavelength, unlike previous reports on fluorinated graphite diyne. The blue/red shift of the excitation frequency emission is often observed in two-dimensional materials, which depends to a large extent on particle size and microenvironment. As shown in fig. 1c, the maximum emission intensity was reached at an excitation wavelength of 360nm, and the three emission peaks (407, 430, and 455nm) had very similar photoluminescence spectra, normalized to unity, indicating that the three peaks experienced the same energy transition in the graphite diyne. The photoluminescence lifetime characteristics further confirm the foregoing conclusions, as shown in figure 1 d. The lifetimes of the three peaks are all close to 1.6ns, and no relevant report of the emission lifetime of graphite diyne exists in the past. However, this value has a smaller gain compared to other carbon-based two-dimensional materials or quantum dot materials, such as carbon nanodots (5-9ns) and graphene quantum dots (3-5 ns).
The kinetics of carriers in visible region graphite diyne solution were characterized by a commercial transient absorption spectrometer (Helios fire, ultra fast Systems, usa). The pump source is delivered by the OPA system at 400 nm. In the femtosecond titanium: under the excitation of a sapphire oscillator, the resolution of a broadband probe wavelength band delay line generated by a calcium difluoride crystal is 15 femtoseconds, and the resolution of a pulse laser source is 90 femtoseconds. The spatial resolution of the pump/probe beam is about 50 microns. The graphite diyne solution was dispersed in an isopropanol solution and then fixed in a cuvette of 10mm thickness for carrier kinetic measurements. The dynamics of visible-state photocarriers in the graphite diyne nanosheet solution are researched as follows, the time resolution of a spectrometer for transient absorption is about 90 femtoseconds, the excitation wavelength is 400nm, and the wavelength range of a probe is from 440 to 780 nm. The experimental results are shown in fig. 2a, where a band can be observed at 450 to 600nm for strong excited state absorption, and the deep blue color below 450nm is due to the ground state bleaching effect of the pump light. The ensemble of experimental results fitted with two main transient absorption spectra and two main kinetics, as shown in fig. 2b, 2c, 380mV stokes shift to a stable emission peak (fig. 2 b). The main kinetics cannot be mediated by a single attenuationThe subtraction process is suitably fitted, as shown in FIG. 2c, with two exponentially decaying component processes fitted to the lifetime τ12.98ps and τ2140.4ps corresponds to kinetics 1, and τ112.4ps and τ2180.1ps corresponds to kinetics 2, the two-step transition state is shown in figure 2 a. The ground state carriers can rise to a state where the excited state is pumped with 400nm (3.1eV) photons and then rapidly heat in time to an intermediate state for a period of 3-12 ps. As shown in fig. 3, a multimodal distribution of excited state absorption and emission, a sub-fine structure may exist in an intermediate state (fig. 2 a). The return of the excited carriers to the ground state requires 140-180ps, and the light emission energy is about 2.38 eV. The lifetime of the photoluminescence spectrum is different from a stable photoluminescence process due to the absence of relaxed probe light.
The random laser performance of the graphdiyne solution is shown in fig. 3, with three excitation wavelengths (390, 400 and 410nm) near the effective photoluminescence excitation peak used as pump sources. The pump intensity increased and a broad range of sharp discharge peak backgrounds appeared indicating successful generation of random lasers. The random laser performance is similar to the experimental results of recently reported MXene quantum dots, boron nitride nanosheets and zinc oxide nanowires. The random laser threshold is functionally related to the pump wavelength and the integrated intensity three pump wavelengths are shown in fig. 4a-c as the functional intensity of the pump. The threshold values of three pump wavelengths of the random laser are respectively 7.3, 16.4 and 23.0kW/cm2This sequence is consistent with previous photoluminescence excitation spectra, decreasing with increasing wavelengths under high efficiency excitation (fig. 1 c). Effective excitation above 400nm is very minimal and higher excitation intensities are required to reach the laser threshold. The spectrum of a random laser based on graphite diyne covers most of the visible region from 450 to 700 nm. The chromaticity of the spectrum of the random laser light at different pump wavelengths and intensities is shown in fig. 4d, corresponding to fig. 3, and the color of the random laser light can be changed from light green to light red by adjusting the pump parameters through engineering techniques. As shown in fig. 4e, the image of the graphitic diyne random laser shows the product under test.
According to the theory of random laser, the graphite diyne nanosheet is used as an active gain medium, and photons emitted in the solution can be randomly amplified. Provided that the photon amplification of the random laser is greater than the optical loss in the random nanostructure. Graphite diyne has a particle size of about 389nm, and the specific wavelength is small, and mie scattering does not provide effective optical feedback for generating random laser light. The eigen foam can realize strong photo-thermal property under strong excitation, thereby providing effective feedback graphite diyne. It was deduced from the Rayleigh-Plesset equation that the low surface tension of the solution favors the formation of large bubbles and high intensity light scattering. The surface tension of chlorobenzene at the spectrum is 33.6mN/m of the chaotic behavior of random laser. The resulting bubble instability changes over time due to brownian motion of the gain medium, and spectral diversity is created by multiple scattering in the highly free system of the mode competition.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (5)
1. A preparation method of a random laser is characterized by comprising the following steps:
synthesizing graphite diyne: providing hexaethynylbenzene as a synthetic monomer, dissolving hexaethynylbenzene in an organic solvent to obtain a hexaethynylbenzene solution, providing a substrate, placing the substrate in the organic solvent to obtain a substrate solution, heating the substrate solution and maintaining the temperature at 55-65 ℃, and adding the hexaethynylbenzene solution into the heat-insulated substrate solution for reaction for 1-5 days at one time to obtain graphite diyne attached to the substrate;
stripping the graphite diyne film: transferring the graphite diyne attached to the substrate into a ferric chloride solution for wet stripping to obtain a graphite diyne film;
preparing a random laser: preparing a random laser by taking a graphite diyne film as a gain medium;
the substrate is a copper substrate.
2. The method of claim 1, wherein in the step of synthesizing graphitic diyne, the organic solvent is one or more of pyridine, pyridine/methanol, ammonia/ethanol, and ethylamine solution.
3. The method for preparing a random laser according to claim 1, wherein in the step of synthesizing the graphitic diyne, the substrate is sequentially placed in dilute hydrochloric acid, acetone and ethanol for ultrasonic treatment before being placed in an organic solvent.
4. The method of claim 1, wherein the hexaethynylbenzene solution has a hexaethynylbenzene concentration of 0.0005M to 0.002M during the step of synthesizing graphitic diyne.
5. The method for preparing a random laser according to claim 1, wherein, in the step of synthesizing the graphitic diyne, the hexaethynylbenzene solution has a hexaethynylbenzene concentration of 0.001M, the base solution is maintained at 60 ℃, and the hexaethynylbenzene solution is added to the incubated base solution at one time for reaction for 3 days.
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