CN111934185A - Random laser manufacturing method based on coupling of silver nanorod metamaterial and luminophor - Google Patents
Random laser manufacturing method based on coupling of silver nanorod metamaterial and luminophor Download PDFInfo
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- CN111934185A CN111934185A CN202010775854.2A CN202010775854A CN111934185A CN 111934185 A CN111934185 A CN 111934185A CN 202010775854 A CN202010775854 A CN 202010775854A CN 111934185 A CN111934185 A CN 111934185A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/14—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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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
- H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
- H01S3/10—Controlling the intensity, frequency, phase, polarisation or direction of the emitted radiation, e.g. switching, gating, modulating or demodulating
- H01S3/102—Controlling the intensity, frequency, phase, polarisation or direction of the emitted radiation, e.g. switching, gating, modulating or demodulating by controlling the active medium, e.g. by controlling the processes or apparatus for excitation
Abstract
The invention discloses a method for manufacturing a random laser based on coupling of a silver nanorod metamaterial and a luminous body. The surface plasmon nanometer resonant cavity mode is excited by changing the length of the silver nanorods, and the random laser emission wavelength can be regulated and controlled by the selectivity enhancement of the longitudinal high-order nanometer resonant cavity mode. The random laser has the characteristics of low threshold and high output power, can realize effective regulation and control of the emission wavelength of the random laser in a wider wavelength range, enriches the research field and research direction of the random laser, and can be applied to the aspects of sensing, photonic crystals and the like.
Description
Technical Field
The invention relates to the field of noble metal nano metamaterial and random laser, in particular to a surface plasmon random laser with adjustable emission wavelength based on coupling of a silver nanorod metamaterial and fluorescent molecules.
Background
Unlike conventional lasers, random lasers do not require a resonator formed by mirrors to obtain photons to achieve lasing, and rely on random scattered light in a disordered gain medium to produce random laser light. In 1968, Letokhov et al first calculated optical properties in random gain media that have both amplifying and scattering effects on light. In 1996, Cao et al observed stimulated emission in ZnO semiconductor random media, and well explained the emission spectrum and spatial distribution characteristics of random lasers with photon localization theory. In recent years, random lasers have been widely studied and applied in many aspects, such as speckle-free imaging, illumination, raman lasers, and medical diagnostics, due to their special properties of relatively simple technical requirements (no need for optical cavities), small size, and low spatial coherence. Due to the lack of a complete optical resonant cavity, the regulation and control of random laser wavelength become very difficult, so that the application development of random laser in medical diagnosis, sensing, photonic crystals and other aspects is hindered, and the research of the random laser emission wavelength regulation and control is of great significance.
Many reports on the modulation of random laser emission wavelengths have now demonstrated that this study can be implemented in a variety of systems, such as photonic glass, polymer optical fibers, and metal nanoparticles. In 2008, Gottardo et al in european nonlinear spectroscopy laboratory reported a tunable random laser based on polystyrene spheres, where monodisperse polystyrene spheres were selected as a component of a three-dimensional solid random system, the change of resonance wavelength was controlled by changing the diameter of the spheres, and Mie resonance of polystyrene spheres had a great effect on the laser emission wavelength, and when the change of the diameter of the spheres was controlled within 10%, the shift of the center wavelength of the random laser was still as high as 35 nm.
The plasmon random laser based on the noble metal nano material has strong light scattering enhancement capability and good constraint effect due to the plasmon resonance effect, and has a lower threshold value and higher output power. Therefore, the emission characteristic regulation and control of the plasmon random laser based on the coupling of the nano structure and the luminophor has great research value. In 2011, Zhai Tianrui et al, Beijing industry university, studied a waveguide-plasmon random laser lasing scheme, which was to coat a layer of dye-doped polymer on a substrate of a randomly distributed gold nano-island structure, and change the plasmon resonance peak by changing the average diameter of the gold nano-island, thereby realizing laser wavelength regulation and control, with a regulation and control range up to 17nm, but had disadvantages in characteristics such as laser threshold, regulation and control efficiency.
The surface plasmon resonance cavity of the nano metal metamaterial structure formed by the noble metal nano array has the characteristics of small mode volume and small radiation loss, has a great enhancement effect on the light field intensity of the nano metal surface, can effectively improve the photoluminescence efficiency of a luminous body, and can adjust the excited surface plasmon nano resonance cavity mode by changing the size of the nano metamaterial. The invention provides a random laser with low threshold and high output power by combining the new mechanism, can realize effective regulation and control of random laser emission wavelength in a wider range, and has important application value in the fields of sensing, photonic crystals and the like.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a method for manufacturing a random laser based on the coupling of a silver nanorod metamaterial and a luminous body.
The invention is realized by the following technical scheme:
a random laser manufacturing method based on coupling of a silver nanorod metamaterial and a luminous body adopts Nile red fluorescent dye as an optical gain medium, a silver nanorod metamaterial structure embedded in a porous alumina template as a surface plasmon resonance cavity, a PMMA film as a medium layer between the silver nanorod metamaterial and the luminous body, and an aluminum sheet as a substrate.
The manufacturing method of the random laser based on the coupling of the silver nanorod metamaterial and the luminophor comprises the following preparation steps:
(1) preparing a porous anodic aluminum oxide template by a secondary anodic oxidation method;
(2) placing the through hole alumina template dried in the step (1) in a cavity of an ion sputtering coating machine, and sputtering for 6min at 40mA current in an argon environment to obtain a gold film electrode;
(3) assembling a silver nanorod metamaterial structure in the porous alumina template in the step (2) by an electrochemical deposition method, wherein the metamaterial structure is formed by hexagonal close-packed periodic silver nanorod arrays, the adopted electrochemical deposition process is carried out in an electrochemical system of two electrodes, and a constant voltage of-0.1V is applied to the alumina template electrode;
(4) dissolving PMMA5g in 95g of ethyl acetate, and after the complete dissolution, taking 50mg of nile red fluorescent dye and fully dissolving in 10mL of the PMMA mixed solution;
(5) and (3) removing a gold film electrode on the surface of the silver nanorod metamaterial in a mechanical polishing mode, exposing one end of a silver nanorod embedded in the porous alumina to the air, placing the silver nanorod metamaterial structure on an aluminum sheet substrate, dropwise coating 1 mu L of the Nile red/PMMA mixed solution obtained in the step (4) on one end, where the gold film is removed, of the alumina template, and pumping the solution through a laser after the solution is dried to obtain the random laser based on the coupling of the silver nanorod metamaterial and the luminophor.
In the step (2), the diameter of the hole of the dried alumina template after the full through hole is 70nm, and the thickness of the gold film electrode obtained by sputtering is about 70 nm.
In the step (3), the electrolyte formula used in the electrochemical deposition of the silver nanorods is as follows: AgNO3(10g/L)、EDTA(5g/L)、Na2SO3(50g/L) and K2HPO4(20g/L), the growth length of the nano-rods can be controlled by changing the deposition time.
The filling rate of the nano rods is controlled by controlling voltage by utilizing an electrochemical deposition method, so that the nano rods are incompletely and uniformly filled into holes of an alumina template, and meanwhile, the nano rods can generate uneven stress at a crystal boundary to cause incomplete arrangement of a hexagonal ordered close-packed structure during assembly, so that a defective silver nano rod metamaterial structure is prepared, and disordered multiple light scattering can be generated between a gain layer and the silver nano rod metamaterial structure when an external light source pumps.
The surface plasmon nanometer resonant cavity mode of the silver nanorod metamaterial can change along with the change of the length of the nanorod, when the length of the nanorod is increased, the longitudinal surface plasmon nanometer resonant cavity mode of the same order can generate red shift, and here, silver nanorod metamaterial samples with the nanorod lengths of 244nm, 265nm, 333nm and 480nm are prepared.
The threshold value of the prepared random laser is about 76.5 muJ, the half-peak width of the whole emission spectrum is about 8.5nm, the half-peak width of the main peak is 0.5nm, the surface plasmon nanometer resonant cavity mode is excited by changing the length of the silver nanorods, and the random laser emission wavelength can be regulated and controlled by depending on the selectivity enhancement of the longitudinal surface plasmon nanometer resonant cavity mode, wherein the random laser wavelengths generated after the silver nanorod metamaterial samples with four different lengths are coupled with Nile red dye are respectively 622nm, 628nm, 634nm and 649 nm.
The invention has the advantages that:
according to the good confinement effect of the surface plasmon nanometer resonant cavity of the silver nanorod metamaterial on light at the nanoscale and the optical field enhancement effect, when the surface plasmon nanometer resonant cavity mode of the silver nanorod metamaterial is close to the emission wavelength of Nile red fluorescent dye, the luminous intensity of Nile red and the light scattering of the silver nanorod metamaterial can be greatly enhanced, and the surface plasmon nanometer local electromagnetic field can excite excited state molecules to transfer energy to the mode with the same frequency, phase and polarization, so that the laser effect is caused. In addition, the silver nanorod metamaterial has high sensitivity to the change of the size of the silver nanorod metamaterial, and when the length of the nanorod is changed, the surface plasmon nanometer resonant cavity mode displayed by the silver nanorod is changed correspondingly, so that the length of the nanorod is changed, and the random laser emission wavelength can be regulated and controlled.
The invention is different from the common solid random laser, the threshold value of the common solid random laser is higher, the output power is relatively lower, and the defects limit the application of the common solid random laser. The random laser based on the silver nanorod metamaterial overcomes the defects, has an ultralow laser threshold and high output power, the lowest threshold can reach 76.5 mu J, the output light intensity can still be improved by nearly ten times under the condition that the pumping energy is increased by a small amplitude, in addition, the emission wavelength can be effectively regulated and controlled in a wider range, and when the length of a silver nanorod is changed from 244nm to 480nm, the emission wavelength of random laser is also shifted from 622nm to 649nm, so that the application of the random laser in the aspects of sensing, photonic crystals and the like becomes possible.
The random laser has the characteristics of low threshold and high output power, can realize effective regulation and control of the emission wavelength of the random laser in a wider wavelength range, enriches the research field and research direction of the random laser, and can be applied to the aspects of sensing, photonic crystals and the like.
Drawings
FIG. 1 is a scanning electron microscope image of the surface morphology of the silver nanorod metamaterial structure of the present invention.
FIG. 2 is a structural mechanism diagram of a random laser based on the coupling of silver nanorod metamaterials and luminophores in the invention.
FIG. 3a is a fluorescence spectrum of the nile red fluorescent dye of the present invention.
FIG. 3b is a random laser spectrum based on the coupling of silver nanorod metamaterials with luminophores in the invention.
Fig. 4 is a random laser threshold map in the present invention.
FIG. 5 is a random laser spectrum of the silver nanorod metamaterial coupled with a Nile red emitter when the nanorod length increases from 244nm to 480nm in the present invention.
Detailed Description
As shown in fig. 2, the method for manufacturing a random laser based on coupling of a silver nanorod metamaterial and a luminophore specifically comprises the following steps:
(1) at 500 ℃ and 10-2Annealing the high-purity aluminum sheet for 5 hours under the Pa experiment condition to obtain an aluminum sheet beneficial to anodic oxidation;
(2) preparing ordered and hexagonal close-packed anodic aluminum oxide sheets by a secondary anodic oxidation method, washing and drying the anodic aluminum oxide sheets, and removing unoxidized aluminum on the back surfaces of the anodic aluminum oxide sheets by using a copper chloride solution to obtain an aluminum oxide template;
(3) floating the alumina template in the step (2) on the liquid level of a phosphoric acid solution at 30 ℃ to remove the barrier layer, then placing the alumina template in the same phosphoric acid solution again to enlarge the hole at the bottom of the phosphoric acid solution for 20min to obtain a full-through-hole alumina template, and then washing the full-through-hole alumina template with deionized water for multiple times, and immediately using clean filter paper to absorb water and dry the full-through-hole alumina template;
(4) placing the dried aluminum oxide template with complete through holes in the step (3) in a cavity of an ion sputtering film plating machine, and sputtering for 6min at 40mA current in an argon environment to obtain a gold film electrode;
(5) assembling a silver nanorod metamaterial structure 2 in the porous alumina template in the step (3) by an electrochemical deposition method, wherein the metamaterial structure is formed by hexagonal close-packed periodic silver nanorod arrays;
(6) weighing PMMA5g by using a high-precision electronic balance, dissolving the PMMA in 95g of ethyl acetate, placing the PMMA in an ultrasonic cleaning machine for full oscillation and dissolution in order to ensure full dissolution of PMMA, and weighing 50mg of Nile red fluorescent dye to be fully dissolved in 10mL of the PMMA mixed solution to obtain Nile red/PMMA mixed solution 3;
(7) and removing a gold film electrode on the surface of the silver nanorod metamaterial in a mechanical polishing mode, exposing one end of a silver nanorod embedded in porous alumina to the air, placing the silver nanorod metamaterial structure on an aluminum sheet substrate 1, dripping 1 mu L of the Nile red/PMMA mixed solution obtained in the step (4) on one end of an alumina template, where the gold film is removed, by using a liquid transfer gun, and pumping the solution through a laser after the solution is dried to obtain the random laser based on the coupling of the silver nanorod metamaterial structure 2 and a luminous body.
In the step (2), after each anodic oxidation, the next experimental operation can be carried out only after the aluminum oxide sheet is soaked in deionized water for 24 hours, and the mass fraction of the copper chloride solution is 20-25%.
In the step (3), the mass fraction of the phosphoric acid solution is 5%.
In the step (4), the diameter of the hole of the dried alumina template after the full through hole is 70nm, and the thickness of the gold film electrode obtained by sputtering is about 70 nm.
In the step (5), the adopted electrochemical deposition process is carried out in an electrochemical system with two electrodes, a constant voltage of-0.1V is applied to the alumina template electrode, and the formula of an electrolyte used for electrochemically depositing the silver nanorods is as follows: AgNO3(10g/L)、EDTA(5g/L)、Na2SO3(50g/L) and K2HPO4(20g/L), the growth length of the nano-rods can be controlled by changing the deposition time.
The filling rate of the template holes is not too high by controlling the electrochemical deposition, and because the stress of the alumina template at the crystal lattice is not uniform, partial nano-rods are not generated in the nano-holes or the nano-rods are not uniformly and symmetrically arranged, so that multiple scattering can be formed to generate random laser when an external light source pumps.
The surface plasmon nanometer resonant cavity mode of the silver nanorod metamaterial can change along with the change of the length of the nanorods, when the lengths of the nanorods are increased, the longitudinal surface plasmon nanometer resonant cavity mode of the same order can generate red shift, and when the nanorods are increased to a certain length, a new high-order longitudinal surface plasmon nanometer resonant cavity mode can appear at a short wavelength, and here, silver nanorod metamaterial samples with the nanorod lengths of 244nm, 265nm, 333nm and 480nm are prepared.
The threshold value of the prepared random laser is about 76.5 muJ, the half-peak width of the whole emission spectrum is about 8.5nm, the half-peak width of the main peak is 0.5nm, the surface plasmon nanometer resonant cavity mode is excited by changing the length of the silver nanorods, and the random laser emission wavelength can be regulated and controlled by depending on the selectivity enhancement of the longitudinal surface plasmon nanometer resonant cavity mode, wherein the random laser wavelengths generated after the silver nanorod metamaterial samples with four different lengths are coupled with Nile red dye are respectively 622nm, 628nm, 634nm and 649 nm.
The invention relates to a random laser based on coupling of a silver nanorod metamaterial and a luminophor, and a silver nanorod metamaterial structure is prepared by a secondary anodic oxidation and electrochemical deposition method, wherein the surface appearance of the silver nanorod metamaterial structure is shown in figure 1. The method is characterized in that a nile red fluorescent dye is selected as a luminescent gain medium in the experiment, a solvent selected in the experiment is deionized water or a mixed solution of ethyl acetate and PMMA, the mass fraction of the PMMA is 5%, and the concentration of nile red is 5 mg/mL.
Fig. 2 is a structural mechanism diagram of a random laser based on coupling of a silver nanorod metamaterial and a luminophor, wherein an aluminum sheet is used as a substrate of the laser, a layer of glass slide 4 is covered on a nile red/PMMA layer to prevent oxidation of a sample, and it can be seen that a nile red/PMMA active medium layer is tightly coupled with the silver nanorod metamaterial, so that the active medium layer can play a waveguide role as a plasmon gain medium, and meanwhile, the radiation intensity of nile red is greatly enhanced due to the surface plasmon nanometer resonant cavity resonance of the silver nanorod metamaterial. FIG. 3a is a fluorescence spectrum of Nile Red with a full width at half maximum of about 60nm and an emission wavelength of 635 nm. FIG. 3b is a random laser spectrum generated after the silver nanorod metamaterial is coupled with the Nile red/PMMA gain layer, and it can be seen from the graph that the spectrum is sharper after the silver nanorod metamaterial and the Nile red/PMMA gain layer are coupled, the half-peak width of the whole emission spectrum is about 8.5nm, and the main peak width is about 0.5 nm. Fig. 4 is a threshold map for a random laser, which can be seen to be approximately 75.6 muj. FIG. 5 is a random laser emission spectrum of the silver nanorod metamaterial coupled with Nile red when the nanorod length is increased from 244nm to 480nm, and it can be seen from the graph that as the nanorod length is increased, the longitudinal surface plasmon nanometer resonant cavity mode of the silver nanorod metamaterial can undergo wavelength red shift, so that the emission spectrum of Nile red is selectively enhanced, and the emission wavelength of the random laser spectrum is shifted from 622nm to 649 nm.
The surface plasmon characteristics of the silver nanorod metamaterial are extremely sensitive to the change of the size of the metamaterial, and the excited surface plasmon nanometer resonant cavity mode can be effectively controlled by controlling the length of the nanorod in a relatively simple mode, so that the emission wavelength of the random laser can be regulated. The invention realizes the effective regulation and control of random laser emission wavelength in a wider wavelength range, and can be applied to the fields of sensing, photonic crystals, medicine and the like.
Claims (7)
1. A manufacturing method of a random laser based on coupling of a silver nanorod metamaterial and a luminophor is characterized by comprising the following steps: the random laser is manufactured by adopting a Nile red fluorescent dye as a light gain medium, a silver nanorod metamaterial structure embedded in a porous anodic alumina template as a surface plasmon resonance cavity, a PMMA film as a medium layer between a silver nanorod metamaterial and a luminous body and an aluminum sheet as a substrate.
2. The method for manufacturing the random laser based on the coupling of the silver nanorod metamaterial and the luminophor according to claim 1, wherein the method comprises the following steps: the specific steps for manufacturing the random laser are as follows:
(1) preparing a porous anodic aluminum oxide template by a secondary anodic oxidation method;
(2) placing the porous anodic alumina template dried in the step (1) in a cavity of an ion sputtering coating machine, and sputtering for 6min at 40mA current in an argon environment to obtain a gold film electrode;
(3) assembling a silver nanorod metamaterial structure in the porous anodic alumina template in the step (2) by an electrochemical deposition method, wherein the silver nanorod metamaterial structure is formed by hexagonal close-packed periodic silver nanorod arrays, the electrochemical deposition method is carried out in an electrochemical system with two electrodes, and a constant voltage of-0.1V is applied to the electrodes of the porous anodic alumina template;
(4) dissolving PMMA5g in 95g of ethyl acetate, and after the complete dissolution, taking 50mg of nile red fluorescent dye and fully dissolving the nile red fluorescent dye in 10mL of the PMMA mixed solution to obtain a nile red/PMMA mixed solution;
(5) and (3) removing a gold film electrode on the surface of the silver nanorod metamaterial structure in a mechanical polishing mode, exposing one end of a silver nanorod embedded in the porous anodic alumina template to air, placing the silver nanorod metamaterial structure on an aluminum sheet substrate, dropwise coating 1 mu L of the Nile red/PMMA mixed solution obtained in the step (4) on one end of the porous anodic alumina template, where the gold film is removed, and pumping the solution through a laser after the solution is dried to obtain the random laser based on the coupling of the silver nanorod metamaterial and the luminophor.
3. The method for manufacturing the random laser based on the coupling of the silver nanorod metamaterial and the luminophor according to claim 2, wherein the method comprises the following steps: in the step (2), the pore diameter of the dried porous anodic alumina template is 70nm, and the thickness of the gold film electrode obtained by sputtering is 70 nm.
4. The method for manufacturing the random laser based on the coupling of the silver nanorod metamaterial and the luminophor according to claim 2, wherein the method comprises the following steps: in the step (3), the electrolyte formula used in the electrochemical deposition of the silver nanorod metamaterial structure is as follows: AgNO3(10g/L)、EDTA(5g/L)、Na2SO3(50g/L) and K2HPO4(20g/L), and controlling the growth length of the silver nanorod metamaterial structure by changing the deposition time.
5. The method for manufacturing the random laser based on the coupling of the silver nanorod metamaterial and the luminophor according to claim 4, wherein the method comprises the following steps: the filling rate of the silver nanorod metamaterial structure is controlled by controlling voltage by utilizing an electrochemical deposition method, so that the silver nanorod metamaterial structure is incompletely and uniformly filled into the pores of the porous anodic alumina template, and meanwhile, the stress generated by the silver nanorod metamaterial structure at a crystal boundary is not uniform, so that the incomplete arrangement is a hexagonal ordered close-packed structure during assembly.
6. The method for manufacturing the random laser based on the coupling of the silver nanorod metamaterial and the luminophor according to claim 2, wherein the method comprises the following steps: the surface plasmon nanometer resonant cavity mode of the silver nanorod metamaterial structure changes along with the change of the length of the silver nanorod metamaterial structure, and when the length of the silver nanorod metamaterial structure is increased, the longitudinal surface plasmon nanometer resonant cavity mode of the same order is subjected to red shift.
7. The method for manufacturing the random laser based on the coupling of the silver nanorod metamaterial and the luminophor according to claim 6, wherein the method comprises the following steps: the laser threshold of the random laser is 76.5 muJ, the half-peak width of the whole emission spectrum is about 8.5nm, the half-peak width of the main peak is 0.5nm, the surface plasmon nanometer resonant cavity mode is adjusted and excited by changing the length of the silver nanorod metamaterial structure, and the random laser emission wavelength is adjusted and controlled by means of the selectivity enhancement of the longitudinal surface plasmon nanometer resonant cavity mode.
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