CN116987401A - Organic single crystal dye laser, and preparation method and application thereof - Google Patents
Organic single crystal dye laser, and preparation method and application thereof Download PDFInfo
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B57/00—Other synthetic dyes of known constitution
- C09B57/02—Coumarine dyes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0025—Crystal modifications; Special X-ray patterns
-
- 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
- H01S3/05—Construction or shape of optical resonators; Accommodation of active medium therein; Shape of active medium
- H01S3/06—Construction or shape of active medium
- H01S3/0602—Crystal lasers or glass 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
- H01S3/16—Solid materials
- H01S3/168—Solid materials using an organic dye dispersed in a solid matrix
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Electromagnetism (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Lasers (AREA)
Abstract
The application provides an organic single crystal dye laser, a preparation method and application thereof. The organic single crystal dye laser comprises a dye single crystal, wherein the dye single crystal is obtained by self-assembly of organic dye molecules; in the dye single crystal, the organic dye molecules have loose molecular arrangement structures, and can inhibit intermolecular charge transfer, so that stimulated radiation is more likely to be realized. The organic single crystal dye laser has loose molecular stacking and weak pi-pi interaction, can inhibit intermolecular charge transfer and maintain excellent optical gain of dye molecules, thereby realizing low-threshold laser emission; the organic dye monocrystal provided by the application is assembled into a microwire, can be used as a high-quality optical resonant cavity, and provides optical feedback and mode amplification for stimulated radiation of organic dye molecules. The organic single crystal dye laser of the application realizes the optical pumping laser radiation of single crystal dye for the first time. The application also provides application of the organic single crystal dye laser.
Description
Technical Field
The application belongs to the technical field of organic micro-nano lasers, and particularly relates to a novel organic single crystal dye laser, a preparation method thereof and application thereof in laser performance.
Background
Since the advent of the first ruby laser, rapid advances have been made in the design and development of lasers. In 1966, researchers invented dye lasers using organic dye solutions as gain media. Organic dye molecules with broad emission bands are particularly useful for constructing tunable and pulsed lasers and exhibit many advanced applications in astronomy, manufacturing, medicine, spectroscopy, etc. In order to further satisfy the integration of optical devices and the safety of laser devices during transportation and storage, solid-state dye lasers have received widespread attention and development. However, the existing solid dye laser mainly relies on dye-doped polymers as gain media, and has the problems of high defect density, low optical gain, poor stability and the like. The single crystal structure has the advantages of few defects, high optical gain, good stability, large refractive index and optical anisotropy, and provides a wide prospect for the design of high-performance solid-state lasers. Although organic lasers in the single crystalline state have been implemented in some organic semiconductor materials, these materials are primarily limited to a few aromatic oligomers, and in recent years, organic single crystalline semiconductor lasers have approached their performance and functional limits. In contrast, laser dye molecules are of a wide variety, such as coumarin, rhodamine, and cyanine derivatives, among others. The realization of dye single crystal laser is expected to further widen the gain system of the organic single crystal laser. However, the realization of stimulated radiation in the single crystalline state with organic dye molecules is still a great challenge today, mainly for reasons such as: the dye molecule self-assembly process follows thermodynamic or kinetic approach (thermodynamic products are more stable and kinetic products are formed faster), and in general, kinetic aggregates spontaneously recombine to a thermodynamic stable state through molecular thermal motion, so that the thermodynamic products are more easily obtained, but the thermodynamic dye aggregates often generate intermolecular charge transfer due to the tight molecular arrangement, further suffer from serious intermolecular quenching, and are difficult to provide enough optical gain, so that the realization of dye single crystal lasers is unfavorable.
Disclosure of Invention
In order to solve the defects in the prior art, the application provides an organic single crystal dye laser, a preparation method thereof and application thereof in laser performance; the organic single crystal dye laser is a laser which can inhibit charge transfer of a molecular self-assembly body to promote stimulated radiation process, and can be used for preparing an organic micro-nano laser.
The application provides the following technical scheme:
the application provides an organic single crystal dye laser which comprises a dye single crystal, wherein the dye single crystal is obtained through self-assembly of organic dye molecules.
According to an embodiment of the present application, the dye single crystal has a high crystallinity.
According to an embodiment of the application, the dye single crystal has a low threshold of laser emission.
According to the embodiment of the present application, in the dye single crystal, the organic dye molecules have a loose molecular arrangement structure, and intermolecular charge transfer can be suppressed, so that stimulated radiation is more likely to be realized.
Preferably, in the molecular arrangement structure, the minimum period units are formed by stacking the organic dye molecules in parallel. Further, the distance between molecules piled up in parallel is larger thanFor example +.>
According to an embodiment of the present application, the dye single crystal has a micro-nano structure. Preferably, the micro-nano structure has typical optical waveguide characteristics that confine the propagating photons and create optical resonance.
Preferably, the micro-nano structure may be a micro-wire structure. Further, the length of the micro-wire structure may be 3-30 μm, the width of the micro-wire structure may be 0.8-2.5 μm, and the thickness of the micro-wire structure may be 0.3-1 μm. Illustratively, the length of the microwire structure may be 3.6-15.8 μm, the width of the microwire structure may be 1-2.2 μm, and the thickness of the microwire structure may be 0.5-0.8 μm.
According to an embodiment of the application, the organic dye molecule is selected from organic dyes having an optical gain.
Preferably, the organic dye molecule is selected from coumarin-153 (C153), for example.
According to an embodiment of the present application, the coumarin-153 has the structure shown in formula 1:
according to an embodiment of the application, the organic dye molecule self-assembly comprises: the organic dye molecules self-assemble to obtain the dye single crystal under weak intermolecular forces (such as pi-pi bonds, hydrogen bonds and the like).
According to an exemplary aspect of the present application, the organic single crystal dye laser includes a dye single crystal, the dye single crystal being self-assembled by the organic dye molecule, the organic dye molecule being selected from coumarin-153.
Preferably, the dye monocrystal is triclinic system, and the unit cell parameter is α＝80.231°，β＝78.024°，γ＝74.093°。
Preferably, the dye single crystal has an optical gain. Further, the organic single crystal dye laser emits cyan light under excitation of ultraviolet light (330-380 nm), for example, with a maximum emission wavelength of 516nm.
Preferably, the organic single crystal dye laser has a fluorescence quantum yield of 59.8% under excitation at 405 nm.
Preferably, in the dye single crystal, the molecular arrangement structure of the organic dye molecule is substantially as shown in a or B of fig. 4.
Further, in the molecular arrangement structure, the minimum period unit is that the organic dye molecules are stacked in parallel. Preferably, in the dye single crystal, the distance between molecules stacked in parallel is
Preferably, the dye single crystal has a micro-wire structure. Further, the length of the micro-wire structure may be 3-30 μm, the width of the micro-wire structure may be 0.8-2.5 μm, and the thickness of the micro-wire structure may be 0.3-1 μm. Illustratively, the microwires may have a length of 3.6-15.8 μm, the microwires may have a width of 1-2.2 μm, and the microwires may have a thickness of 0.5-0.8 μm.
Preferably, the microwire structure has typical optical waveguide characteristics, confining the propagating photons and producing optical resonance. Illustratively, the dye single crystal has an optically resonant microcavity, specifically a fabry-perot microcavity.
The application also provides a preparation method of the organic single crystal dye laser, which comprises the following steps:
1) Dissolving organic dye molecules in an organic solvent to obtain a saturated organic solution;
2) And (3) dropwise adding the saturated organic solution prepared in the step (1) onto a substrate, and self-assembling organic dye molecules in an anti-solvent atmosphere to obtain the organic single crystal dye laser.
According to an embodiment of the application, in step 1), the organic solvent is selected from small molecule organic solvents that dissolve the organic dye molecules.
Preferably, the organic solvent is selected from n-hexane, dichloromethane, tetrahydrofuran, toluene, acetonitrile, chloroform, preferably n-hexane.
According to an embodiment of the application, in step 1), the molar concentration of the organic dye molecules in the organic solvent is 1-10mmol/L, preferably 2-4mmol/L.
According to an embodiment of the present application, in step 1), the preparation method of the saturated organic solution specifically includes: dissolving organic dye molecules in an organic solvent, and respectively stirring at different temperatures to obtain organic solutions at different temperatures; and filtering again to obtain saturated organic solution.
Preferably, the temperature of the stirring is 30-80 ℃, preferably 40 ℃.
Preferably, the speed of stirring is 800-2000rpm, preferably 1000-2000rpm, for example 1500rpm.
Preferably, the stirring time is 15-60min, preferably 30min.
Preferably, the filtration may be performed in devices known in the art. Illustratively, the filtration is performed in a polytetrafluoroethylene filter having a diameter of 0.1-1 μm, for example 0.2 μm.
According to an embodiment of the application, in step 2), the anti-solvent atmosphere is selected from at least one of acetone, n-hexane, ethanol, preferably ethanol.
According to an embodiment of the application, in step 2), the substrate is selected from substrates known in the art as base materials, for example from glass plates, silicon plates, quartz plates.
According to an embodiment of the application, in step 2), the temperature of the substrate is 10-30 ℃, for example 20 ℃.
According to an embodiment of the application, in step 2), the self-assembly of the organic dye molecules is an organic solvent evaporation induced self-assembly.
Preferably, the temperature of the self-assembly is 30-80 ℃, for example 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃ or 80 ℃.
According to an embodiment of the present application, in step 2), the size of the organic single crystal dye laser is controlled by the volume of the saturated solution added dropwise.
The application also provides application of the organic single crystal dye laser, for example, application in the fields of organic micro-nano laser, integrated optical circuits, organic lasers and the like.
The application also provides a micro-nano laser which comprises the organic single crystal dye laser.
The application also provides an integrated optical circuit, which comprises a coherent light source, wherein the coherent light source comprises the organic single crystal dye laser.
The application provides an organic laser, preferably a low threshold organic laser, comprising the organic single crystal dye laser described above.
The application has the beneficial effects that:
the organic single crystal dye laser has the following advantages:
1. the organic single crystal dye laser provided by the application has a micro-nano structure, such as a micron line structure, can be used as a high-quality optical resonant cavity, provides optical feedback and mode selection for stimulated radiation of dye single crystals, and can effectively output coherent optical signals in a directional manner;
2. the organic dye monocrystal provided by the application has larger molecular spacing and weaker intermolecular interaction, inhibits the intermolecular charge transfer process, maintains the sufficient optical gain property of the dye in an aggregation state, and is beneficial to establishing particle number inversion so as to realize final laser radiation (such as low-threshold laser emission);
3. the inventor researches find that in the excited state process of the organic single crystal dye laser, a larger potential barrier exists between the intramolecular charge transfer state and the intermolecular charge transfer state energy level, and the intermolecular charge transfer state of unfavorable stimulated radiation is not generated, so that the organic single crystal dye laser has a faster radiation transition rate;
4. the inventor researches find that the dye monocrystal is a kinetic product obtained by accelerating the self-assembly process, and the assembly process of molecules can be regulated and controlled by controlling the experimental temperature, so that the formation of thermodynamic dye monocrystal which is formed by closely accumulating molecules and is unfavorable for stimulated radiation is avoided;
5. the inventor researches find that the organic single crystal dye laser can effectively inhibit intermolecular charge transfer due to the weakened intermolecular pi-pi acting force, so that stimulated radiation (such as low-threshold laser emission) can be realized in a gain interval (for example, 505-515 nm) of the dye, and great potential of dye single crystals with kinetic control in the aspect of constructing the organic single crystal laser is shown.
6. The inventors have realized for the first time optically pumped laser radiation in the organic dye single crystal and adjusted the mode spacing of the laser by changing the size of the organic dye single crystal. The organic dye single crystal laser can be used for realizing a small-size micro-nano coherent light source and integrating a photonics loop to obtain improved laser performance.
Drawings
Fig. 1 is a flow chart showing a process for preparing an organic single crystal dye laser of example 1.
FIG. 2 is a graph showing the morphology characterization of the organic single crystal dye laser of example 1.
FIG. 3 is a graph showing the X-ray diffraction results of the organic single crystal dye laser in example 1.
Fig. 4 is a molecular arrangement structure diagram of the organic single crystal dye laser in example 1.
Fig. 5 is a graph of the micro-domain raman results of the organic single crystal dye laser of example 1.
FIG. 6 is a graph showing fluorescence emission spectra of the organic single crystal dye laser in example 1.
FIG. 7 shows fluorescence quantum yields of the organic single crystal dye laser in example 1.
FIG. 8 is a graph showing the fluorescence decay curve of the organic single crystal dye laser of example 1.
FIG. 9 is a graph showing the fluorescence lifetime results of the organic single crystal dye laser of example 1 at different fluorescence wavelengths.
Fig. 10 is a schematic energy level diagram of the organic single crystal dye laser and the corresponding excited state process in example 1.
FIG. 11 is a simulation result of electric field distribution of the organic single crystal dye laser in example 1.
FIG. 12 is a graph showing the results of characterization of the laser properties of the organic single crystal dye laser in example 1.
Detailed Description
The technical scheme of the application will be further described in detail below with reference to specific embodiments. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the application. All techniques implemented based on the above description of the application are intended to be included within the scope of the application.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
Example 1
The preparation method of the organic single crystal dye laser comprises the following steps:
1) The organic dye molecule C153 (purchased from Tci tai (Shanghai) to industry development limited, model: c2858 Dissolving in n-hexane solvent to obtain dye solution with concentration of 2 mmol/L;
2) Placing the dye solution in the step 1) on a hot table at 40 ℃, stirring at 1500rpm for 30min, and standing;
3) Filtering the solution obtained in the step 2) by using a polytetrafluoroethylene filter with the diameter of 0.2 mu m to obtain a saturated solution of organic dye molecules C153;
4) Dripping the saturated solution at 40 ℃ prepared in the step 3) on a glass sheet at room temperature (20 ℃) and placing the glass sheet in an ethanol atmosphere, and self-assembling organic dye molecules C153 after the n-hexane solvent is completely volatilized to obtain dye single crystals with a micro-wire structure, namely the organic single crystal dye laser of the embodiment;
the size of the dye single crystal can be achieved by controlling the volume of the saturated solution added dropwise in the step 4), the volumes of the saturated solution added dropwise on the glass sheet are respectively 10 mu L, 15 mu L, 20 mu L, 25 mu L, 30 mu L, 40 mu L and 50 mu L, and the sizes of the micro-wire structures corresponding to the prepared dye single crystals are respectively 3.6 mu m, 1 mu m, 560nm, 5.1 mu m, 1.1 mu m, 500nm, 7.3 mu m, 1.4 mu m, 510nm, 9.1 mu m, 1.3 mu m, 560nm, 10 mu m, 2 mu m, 600nm, 12.5 mu m, 1.2 mu m, 700nm and 15.8 mu m, 2.2 mu m, 800nm.
Fig. 1 is a flow chart showing a process for preparing an organic single crystal dye laser of example 1. As can be seen from fig. 1, in a hot solution (e.g., 40 ℃) of organic dye molecules C153, the dye molecules are uniformly dispersed in the solvent at a large interval. After the organic dye hot solution liquid drop is cast on a substrate at room temperature, the liquid drop of the hot solution is subject to quick molecular nucleation under the drive of volatilization and cooling, so as to form crystal nuclei with loose molecular accumulation, and then the crystal nuclei are further induced to grow into dynamic dye single crystals by molecular epitaxy, and the dynamic dye single crystals with larger molecular interval provide possibility for maintaining enough optical gain of dye molecules.
Test example 1
The organic single crystal dye laser of example 1 was subjected to the following morphological structure analysis and fluorescence property characterization:
1. topography characterization test
Fig. 2 is a graph showing the morphology of the organic single crystal dye laser in example 1, and the dimensions of the organic single crystal dye laser are respectively: a is 12.5 μm 1.2 μm 700nm; b is 7.3 μm x 1.4 μm x 510nm; c and D are each 10 μm by 2 μm by 600nm. A, B, C, D in FIG. 2 is a topographical characterization of the organic single crystal dye laser obtained in example 1. Wherein A in FIG. 2 is a scanning electron microscope image, and the scale is 2 μm; b in fig. 2 is a photoluminescence chart, and the scale is 2 μm; c in FIG. 2 is a transmission electron microscope image, and the scale is 500nm; d in FIG. 2 is a selected area electron diffraction pattern, and the scale is 2 1/nm.
As can be seen from a in fig. 2, the organic single crystal dye laser of example 1 is a one-dimensional microwire structure having a smooth and flat surface and regular end faces, the length of the microwire is 12.5 μm, the width of the microwire is 1.2 μm, and the thickness of the microwire is 700nm. As can be seen from B in fig. 2, the organic single crystal dye laser emits bright green light under the irradiation of ultraviolet light (the bright color in the figure is the bright green light in the color chart), and has typical optical waveguide characteristics, such as bright luminescence at the end and weaker luminescence of the body of the micro-wire, which indicates that the micro-wire can better limit photons transmitted by the domain and generate optical resonance. As can be seen from C and D in FIG. 2, the organic single crystal dye laser of example 1Transmission Electron Microscopy (TEM) and corresponding selective electron diffraction (SAED) of the device indicate that the micrometer lines of the organic dye single crystal are along [012 ]]The values of the inter-plane distances of the (012) and (210) are respectivelyAnd->This is consistent with the results of X-ray diffraction (XRD) of the organic single crystal dye laser.
2. Molecular arrangement structure
(1) Fig. 3 is an X-ray diffraction result graph of the organic single crystal dye laser of example 1, the size of the organic single crystal dye laser is 10 μm×2 μm×600nm. As can be seen from fig. 3, the organic single crystal dye laser of the micro-wire structure has high crystallinity, and the XRD spectrum can be well indexed to the triclinic system, and the unit cell parameters thereof areα= 80.231 °, β= 78.024 °, γ= 74.093 °. The crystal structure of the organic single crystal dye laser was clarified in combination with the analysis of fig. 2 and B, C and fig. 3, which provides conditions for further detailed analysis of the molecular arrangement.
(2) Fig. 4 is a molecular arrangement structure diagram of an organic single crystal dye laser of example 1, the size of the organic single crystal dye laser is 10 μm×2 μm×600nm. In fig. 4 a is a face-to-face molecular arrangement of the smallest periodic unit of the organic single crystal dye laser, and in fig. 4B is a parallel face-to-face molecular arrangement with a smallest pi-pi spacing. As can be seen from fig. 4 a, the repeat unit along the face-to-face pi-pi stacking direction consists of three parallel organic dye molecules C153, and there are three pi-pi intermolecular interactions in the crystalline phase of the organic single crystal dye laser, corresponding to two antiparallel and one parallel molecular stacking modes. Since the distance of parallel molecular stacking is the smallest, the luminescence effect on the organic dye molecule C153 is the largest, and as can be seen from FIG. 4B, the intermolecular distance of parallel molecular stacking of the kinetic dye single crystal isThis intermolecular distance is +.about.of the closely packed thermodynamic C153 dye single crystal>And is relatively large. The loose molecular packing mode in the dynamic dye single crystal is beneficial to inhibiting intermolecular charge transfer in the organic single crystal dye laser, so that stimulated radiation is more likely to be realized.
(3) Fig. 5 is a graph of the micro-domain raman results of the organic single crystal dye laser of example 1, the size of the organic single crystal dye laser being 10 μm by 2 μm by 600nm. As can be seen from FIG. 5, the organic single crystal dye laser is at 1159cm -1 There is a C-C single bond stretching vibration peak, while the stretching vibration peak of C=C double bond is located at 1608.19cm -1 C=c stretching vibration peak (1597.78 cm compared to thermodynamic C153 dye single crystal -1 ) Blue shift, further indicating that organic single crystal dye lasers have weaker pi-pi stacking interactions.
3. Fluorescent performance test:
(1) Fig. 6 is a fluorescence emission spectrum of the organic single crystal dye laser of example 1, the size of the organic single crystal dye laser is 10 μm×2 μm×600nm. As can be seen from fig. 6, the organic single crystal dye laser emits cyan light under excitation of ultraviolet light (330-380 nm), and its maximum emission wavelength is 516nm.
(2) Fig. 7 shows the fluorescence quantum yield of the organic single crystal dye laser of example 1, the size of the organic single crystal dye laser being 10 μm by 2 μm by 600nm. The fluorescence emission spectra without sample and with sample (the two overlap more at 405 nm) are compared by the formula Φ PL ＝A em /(A ex,no sample –A ex,with sample ) The quantum yield of the organic single crystal dye laser can be obtained, wherein A is em Is the integral area of the sample emission spectrum, A ex,with sample And A ex,no sample The integrated area at 405nm excitation light with and without sample, respectively. As can be seen from FIG. 7, the quantum yield of the organic single crystal dye laser is59.8%, which is far higher than the quantum yield of single crystals of organic dyes for intermolecular charge transfer, which is very advantageous for light amplification.
(3) Fig. 8 is a fluorescence attenuation curve of the organic single crystal dye laser of example 1, the size of the organic single crystal dye laser is 10 μm×2 μm×600nm. As can be seen from FIG. 8, the fluorescence intensity of the organic single crystal dye laser decays exponentially with time, and further fitting analysis shows that the fluorescence lifetime τ is 1.53ns, which is much smaller than that of the dye single crystal with intermolecular charge transfer. With the results of fig. 7 and 8, the radiation transition rate k is calculated according to the formula r ＝Φ PL And (tau) calculating to obtain the radiation transition rate of the organic single crystal dye laser to be 0.39ns -1 This faster radiation transition favors the occurrence of stimulated radiation.
(4) Fig. 9 is a graph showing the fluorescence lifetime results of the organic single crystal dye laser of example 1 at different fluorescence wavelengths, the size of the organic single crystal dye laser being 10 μm by 2 μm by 600nm. As can be seen from fig. 9, the fluorescence lifetimes of the organic single crystal dye lasers are different for different fluorescence wavelengths, and as the fluorescence wavelength increases, the fluorescence lifetime of the organic single crystal dye lasers increases (e.g., the fluorescence wavelengths are 480nm, 500nm, 520nm, 540nm, 560nm, 580nm, and the corresponding fluorescence lifetimes are 1.22ns, 1.44ns, 1.63ns, 1.83ns, 2.23ns, 2.47 ns), indicating that the emission of the organic single crystal dye lasers at 516nm results from monomer emission in the intramolecular charge transfer state (the localized monomer emission appears to have a fluorescence lifetime that remains relatively unchanged with increasing fluorescence wavelength).
(5) Based on this, the inventors propose an excited state physical model of the organic single crystal dye laser, as shown in fig. 10, which is an energy level diagram and a corresponding excited state process of the organic single crystal dye laser of example 1. As can be seen from fig. 10, the organic dye molecule C153 vertically transitions from the ground state to the local state under light excitation, and rapidly drops back to the intramolecular charge transfer state. Organic single crystal dye lasers have loose molecular stacks and weak pi-pi stacking interactions, making it difficult for intramolecular charge transfer monomer states to transfer charge to unexcited neighboring molecules, thereby inhibiting intermolecular charge transfer state formation. Because the intramolecular charge transfer state has a smaller degree of charge separation than the intermolecular charge transfer state, corresponding to a larger overlap of wave functions between the ground state and the excited state, the dynamic organic dye single crystal has a larger probability of radiative transition, and is expected to provide effective optical gain for realizing a single crystal dye laser.
From the above characterization results, it is apparent that the organic single crystal dye laser obtained in example 1 has excellent optical gain.
Test example 2
The organic single crystal dye laser of example 1 (10 μm by 2 μm by 600nm size) was subjected to electric field distribution simulation as follows:
test instrument: COMSOL electric field distribution simulation software.
The testing process comprises the following steps:
(1) Drawing a two-dimensional rectangular structure with the length of 10 mu m and the width of 2 mu m in simulation software, representing the dye monocrystal with the prepared micrometer line structure, and setting the refractive index to be 1.56;
(2) Drawing a large rectangular structure with the length of 16 mu m and the width of 12 mu m, representing the external environment-air around the micrometer linear monocrystal, and setting the refractive index of the large rectangular structure to be 1;
(3) Inputting a characteristic frequency formula corresponding to the laser wavelength 510nm of the nanowire monocrystal: c_const/510[ nm ]; the software starts to calculate the electric field distribution intensity.
Fig. 11 shows the electric field distribution simulation result of the organic single crystal dye laser in example 1. As can be seen from fig. 11, the optical mode along the axial direction of the organic dye single crystal micrometer axis (as indicated by the arrow direction marked in fig. 11) clearly shows that the rectangle containing an elliptical spot at the center of fig. 11 (which is 10 μm long and 2 μm wide) is reflected back and forth along the two end faces of the micrometer line structure, and thus it can be seen that the high quality optical resonant microcavity of the organic single crystal dye laser is a typical fabry-perot microcavity.
Test example 3
The organic single crystal dye laser of example 1 was subjected to a femtosecond light excitation test at a femtosecond light pump.
Femtosecond light excitation test instrument: the built space resolution micro-region spectrum test system comprises a titanium-doped sapphire laser with the wavelength of 800nm (pulse width of 100-200fs and repetition frequency of 1 KHz); nonlinear optical crystal beta-BaB 2 O 4 (BBO); a microscope system; and a spectrometer.
The test process of the femtosecond light excitation comprises the following steps: the laser with 800nm wavelength is output by a titanium-doped sapphire laser, and the laser beam passes through a nonlinear optical crystal beta-BaB 2 O 4 (BBO) a femtosecond pulsed laser with a frequency multiplication of 400 nm. All lasers pass through a 720nm short-pass filter together to obtain purer femtosecond laser with the wavelength of 400 nm. The 400nm femtosecond laser enters a microscope system after being reflected, is focused into a light spot of about 20 mu m by a 50-time objective lens and is used as a light source for exciting the organic single crystal dye laser of the embodiment 1, then the same objective lens is used for collecting signal light emitted by the organic single crystal dye laser of the embodiment 1, and the collected signal light is analyzed by a spectrometer after the excitation light is filtered by a 420nm long-pass filter.
Test conditions: the spectrometer software needs to run at the low temperature of 75 ℃ below zero, the temperature of a circulating water cooling system of the titanium-doped sapphire laser is set to 21 ℃, and the organic single crystal dye laser in the embodiment 1 is tested at room temperature.
FIG. 12 is a graph showing the results of characterization of the laser properties of the organic single crystal dye laser in example 1. Wherein the scale of the inset in a in fig. 12 is 5 μm, which corresponds to the dimensions of the organic single crystal dye laser: 10 μm x 2 μm x 600nm. As can be seen from a in fig. 12, when a single organic single crystal dye laser is subjected to femtosecond light excitation, a very bright light emitting behavior occurs at both ends of the organic single crystal dye laser, indicating that the emitted light is significantly modulated by the high quality fabry-perot resonator. With the power of the femtosecond optical pump being 80 mu J/cm 2 Up to 186. Mu.J/cm 2 The optical mode around 510nm in the emission spectrum of the organic single crystal dye laser is greatly amplified. Further analysis of the spectral intensity and spectral full width at half maximum versus pump power from B in FIG. 12 shows that the corresponding curve exhibits significant nonlinear behavior and accompaniesThe rapid narrowing of the full width at half maximum of the emission spectrum further proves that the organic single crystal dye laser successfully realizes the emission of laser light.
As can be seen from fig. 12C, as the size of the organic single crystal dye laser increases, the laser mode spacing distance L decreases, where l=15.8 micrometers represents that the laser size is 15.8 μm×2.2 μm×800nm, and the corresponding laser mode spacing distance is 1.75nm; l=9.1 microns represents a laser size of 9.1 μm x 1.3 μm x 560nm with a corresponding laser mode separation distance of 3nm; l=7.3 microns represents a laser size of 7.3 μm x 1.4 μm x 510nm with a corresponding laser mode separation distance of 3.77nm. In fig. 12, the abscissa is the inverse of the length of the organic single crystal dye laser, and the relationship between the mode spacing in the organic single crystal dye lasers of different sizes and the length of the organic single crystal dye laser can be further analyzed, where the sizes are 15.8 μm by 2.2 μm by 800nm, 12.5 μm by 1.2 μm by 700nm, 10 μm by 2 μm by 600nm, 9.1 μm by 1.3 μm by 560nm, 7.3 μm by 1.4 μm by 510nm, and 5.1 μm by 1.1 μm by 500nm, and the corresponding mode spacing is: 1.5nm, 1.8nm, 2.8nm, 3nm, 3.7nm, and 5.3nm, it was confirmed that the laser mode in the organic single crystal dye laser was a fabry-perot resonant mode.
As can be seen from fig. 12, we have realized laser emission for the first time in an organic dye single crystal based on excellent optical gain and high quality optical resonator of loose stack of dye molecules, and successfully constructed a low threshold organic single crystal dye laser. By means of a temperature-controlled molecular dynamics self-assembly strategy, we prepared an organic single crystal dye laser with weak pi-pi interactions to inhibit intermolecular charge transfer.
From the above results, it is understood that the organic single crystal dye laser obtained in example 1 can be used in the organic micro-nano laser field, even in the integrated photonics field and the organic driving laser field, due to the excellent optical gain and the high quality of the optical resonator
The application realizes the monocrystal dye laser by adjusting molecular accumulation, thus the application is expected to develop high-performance photon materials based on molecular arrangement engineering. The organic single crystal dye laser has great prospect in photoelectric application.
The above description of exemplary embodiments of the application has been provided. However, the scope of the present application is not limited to the above embodiments. Any modifications, equivalent substitutions, improvements, or the like, which are within the spirit and principles of the present application, should be made by those skilled in the art, and are intended to be included within the scope of the present application.
Claims (10)
1. An organic single crystal dye laser, characterized in that the organic single crystal dye laser comprises a dye single crystal obtained by self-assembly of organic dye molecules;
in the dye single crystal, the organic dye molecules have loose molecular arrangement structures, and can inhibit intermolecular charge transfer, so that stimulated radiation is more likely to be realized.
2. The laser of claim 1, wherein in the molecular arrangement, the smallest periodic units are stacked in parallel by the organic dye molecules. Further, the distance between molecules piled up in parallel is larger than
Preferably, the dye single crystal has a micro-nano structure. Preferably, the micro-nano structure has typical optical waveguide characteristics that confine the propagating photons and create optical resonance.
Preferably, the organic dye molecule is selected from organic dyes having optical gain.
Preferably, the organic dye molecule is selected from coumarin-153.
Preferably, the coumarin-153 has a structure as shown in formula 1:
preferably, the organic dye molecule self-assembly comprises: and under weak intermolecular force, the organic dye molecules self-assemble to obtain the dye monocrystal.
3. The laser according to claim 1 or 2, characterized in that the organic single crystal dye laser comprises a dye single crystal, which is self-assembled by the organic dye molecules selected from coumarin-153.
Preferably, the dye monocrystal is triclinic system, and the unit cell parameter is α＝80.231°，β＝78.024°，γ＝74.093°。
4. A laser as claimed in any one of claims 1 to 3 wherein the single crystal of dye has an optical gain. Further, the organic single crystal dye laser emits green light under the excitation of ultraviolet light.
Preferably, the organic single crystal dye laser has a fluorescence quantum yield of 59.8% under excitation at 405 nm.
Preferably, in the dye single crystal, the molecular arrangement structure of the organic dye molecule is substantially as shown in a or B of fig. 4.
Further, in the molecular arrangement structure, the minimum period unit is 5 organic dye molecules stacked in parallel. Preferably, in the dye single crystal, the distance between molecules stacked in parallel is
Preferably, the dye single crystal has a micro-wire structure. Further, the length of the micro-wire structure is 3-30 μm, the width of the micro-wire structure is 0.8-2.5 μm, and the thickness of the micro-wire structure is 0.3-1 μm.
Preferably, the microwire structure has typical optical waveguide characteristics, confining the propagating photons and producing optical resonance. Illustratively, the dye single crystal has an optically resonant microcavity, specifically a fabry-perot microcavity.
5. A method for preparing an organic single crystal dye laser as claimed in any one of claims 1 to 4, comprising the steps of:
1) Dissolving organic dye molecules in an organic solvent to obtain a saturated organic solution;
2) And (3) dropwise adding the saturated organic solution prepared in the step (1) onto a substrate, and self-assembling organic dye molecules in an anti-solvent atmosphere to obtain the organic single crystal dye laser.
Preferably, in step 1), the organic solvent is selected from small molecule organic solvents that can dissolve the organic dye molecules.
Preferably, the organic solvent is selected from n-hexane, dichloromethane, tetrahydrofuran, toluene, acetonitrile, chloroform.
Preferably, in step 1), the molar concentration of the organic dye molecules in the organic solvent is 1-10mmol/L.
Preferably, in step 1), the preparation method of the saturated organic solution specifically includes: dissolving organic dye molecules in an organic solvent, and respectively stirring at different temperatures to obtain organic solutions at different temperatures; and filtering again to obtain saturated organic solution.
Preferably, the temperature of the stirring is 30-80 ℃.
Preferably, the speed of stirring is 800-2000rpm.
Preferably, the stirring time is 15-60min.
6. The method according to claim 5, wherein in step 2), the antisolvent atmosphere is at least one selected from the group consisting of acetone, n-hexane, and ethanol.
Preferably, in step 2), the temperature of the substrate is 10-30 ℃.
Preferably, in step 2), the organic dye molecules self-assemble into self-assemblies induced by volatilization of the organic solvent.
Preferably, the temperature of the self-assembly is 30-80 ℃.
7. Use of an organic single crystal dye laser as claimed in any one of claims 1 to 4.
8. A micro-nano laser comprising the organic single crystal dye laser of any one of claims 1-4.
9. An integrated optical circuit comprising a coherent light source comprising the organic single crystal dye laser of any one of claims 1-4.
10. An organic laser, preferably a low threshold organic laser, comprising an organic single crystal dye laser according to any one of claims 1-4.
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| CN101712811A (en) * | 2008-10-06 | 2010-05-26 | 天津市化学试剂研究所 | Purifying method of laser dye cumarin-4 |
| WO2015030427A1 (en) * | 2013-08-27 | 2015-03-05 | 동우 화인켐 주식회사 | Photoluminescence coating composition and photoluminescence film using same |
| CN108732662A (en) * | 2017-04-20 | 2018-11-02 | 中国科学院化学研究所 | A kind of micro- disk of organic flexible/metal nanometer line hetero-junctions and preparation method thereof |
| CN109212640A (en) * | 2017-07-04 | 2019-01-15 | 中国科学院化学研究所 | Organic/metal nanometer line hetero-junctions of one kind and its preparation method and application |
| CN111647949A (en) * | 2020-04-26 | 2020-09-11 | 中国科学院化学研究所 | Organic single crystal micro-strip for organic electric pumping laser and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101712811A (en) * | 2008-10-06 | 2010-05-26 | 天津市化学试剂研究所 | Purifying method of laser dye cumarin-4 |
| WO2015030427A1 (en) * | 2013-08-27 | 2015-03-05 | 동우 화인켐 주식회사 | Photoluminescence coating composition and photoluminescence film using same |
| CN108732662A (en) * | 2017-04-20 | 2018-11-02 | 中国科学院化学研究所 | A kind of micro- disk of organic flexible/metal nanometer line hetero-junctions and preparation method thereof |
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