CN104716553A - Optical pumping SiO2-Rh6G gel random laser and manufacturing method thereof - Google Patents

Optical pumping SiO2-Rh6G gel random laser and manufacturing method thereof Download PDF

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CN104716553A
CN104716553A CN201510131799.2A CN201510131799A CN104716553A CN 104716553 A CN104716553 A CN 104716553A CN 201510131799 A CN201510131799 A CN 201510131799A CN 104716553 A CN104716553 A CN 104716553A
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rh6g
sio
gel
rubber material
gel rubber
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CN104716553B (en
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李廷帅
刘西云
徐民
黄蹬峰
易涛
刘慎业
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University of Electronic Science and Technology of China
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Abstract

The invention discloses an optical pumping SiO2-Rh6G gel random laser and a manufacturing method thereof. The optical pumping SiO2-Rh6G gel random laser comprises a pumping light source, a spiral attenuating slice, a focusing convex lens and a SiO2-Rh6G gel material. Emergent light of the pumping light source passes through the spiral attenuating slice and then passes through the focusing convex lens to be converged into a focusing light beam, the focusing light beam perpendicularly lights the surface of the SiO2-Rh6G gel material, the emergent light then is multiply scattered and gained by the SiO2-Rh6G gel material, and finally an emission spectrum of the random laser can be obtained. The optical pumping SiO2-Rh6G gel random laser uses the SiO2-Rh6G gel material which is excellent in performance and low in cost as unordered scattering gain media, so that the problems that a random laser in the prior art is higher in emission threshold, lower in efficiency and higher in using cost are solved. In addition, the optical pumping SiO2-Rh6G gel random laser is wide in application prospect in scientific research and industrial production.

Description

Optical pumping SiO 2-Rh6G gel accidental laser and preparation method thereof
Technical field
The invention belongs to optical laser technical field, be specifically related to a kind of optical pumping SiO 2the design of-Rh6G gel accidental laser and preparation method thereof.
Background technology
Nineteen sixty-eight, the former Russian scholar Letokhov propose first in random gain media exist light be excited amplify phenomenon, and calculate its optical characteristics by solving diffusion equation.But people but generally believed that the multiple scattering in random gain media was unfavorable for Laser emission at that time, therefore in 25 subsequently year, this theory was not taken seriously always.Until 1994, the people such as N.M.Lawandy are doped with TiO with laser pumping 2the Rh6G colloidal solution of scattering particles, observes Random Laser phenomenon, and the initiative theory of Letokhov just starts the extensive concern obtaining people.Accidental laser is a kind of unconventional laser, and it does not need conventional resonant cavity, but relies on the multiple scattering of photon in random media to obtain the gain effect of light.The generation mechanism of this uniqueness not only allows it have the tempting prospect of the advantage of engineering and theoretical research, and has huge potential application in various fields such as laser paint, laser display, biological tissue's detections.
In recent years, various novel accidental laser experiment is in the news in succession, and the innovative point of these experiments is mainly based on novel scattering mechanism and different luminescent materials, and the transmitting threshold value of these accidental lasers is higher, efficiency is lower and use cost is higher.Relate to SiO at present 2the research of gel accidental laser is not also a lot, particularly optical pumping SiO 2-Rh6G gel accidental laser have not been reported.
Summary of the invention
The object of the invention is that transmitting threshold value in order to solve accidental laser in prior art is higher, efficiency is lower and the problem that use cost is higher, proposes a kind of optical pumping SiO 2-Rh6G gel accidental laser and preparation method thereof.
Technical scheme of the present invention is: a kind of optical pumping SiO 2-Rh6G gel accidental laser, comprises pump light source, spiral attenuator, focuses on convex lens and SiO 2-Rh6G gel rubber material; The emergent light of pump light source is again through focusing on convex lens after spiral attenuator, and making it converge is a focused beam, and then focused beam impinges perpendicularly on SiO 2-Rh6G gel rubber material surface, then through SiO 2the multiple scattering of-Rh6G gel rubber material and gain, finally obtain the emission spectrum of accidental laser.
Preferably, accidental laser also comprises speculum, and speculum is positioned at and focuses on convex lens and SiO 2between-Rh6G gel rubber material, for adjusting the direction of focused beam.
Preferably, pump light source is pulse laser, the green laser of its emergent light to be wavelength be 532nm; The attenuation rate of described spiral attenuator is chosen as 10% ~ 90% according to the energy of pump light source, and the focal length focusing on convex lens is 200mm ~ 800mm, and speculum is silver-plated completely reflecting mirror.
Preferably, SiO 2-Rh6G gel rubber material be have launch Random Laser characteristic mix Rh6G porous SiO 2gel rubber material, as the material of scattering medium, SiO 2the pore size of-Rh6G gel rubber material is 300nm ~ 900nm.
Preferably, the emission spectrum of accidental laser is observed by fiber spectrometer, and observed direction is and SiO 2the direction that-Rh6G gel rubber material surface is fixing in random selecting one on the anchor ring of 60 degree, fiber spectrometer is connected by data acquisition line concentration with computer.
Present invention also offers a kind of optical pumping SiO 2the using method of-Rh6G gel accidental laser, is characterized in that, comprise the following steps:
S1, by the emergent light of pump light source through spiral attenuator, can 0.2mJ ~ 0.9mJ be decayed to;
S2, by the pump light after energy attenuation by focus on convex lens, making it converge is a focused beam;
S3, by SiO 2-Rh6G gel rubber material is placed in focused beam focus place, makes pump light impinge perpendicularly on SiO 2-Rh6G gel rubber material surface.
Present invention also offers a kind of SiO 2the preparation method of-Rh6G gel rubber material, comprises the following steps:
Under A1, normal temperature, organosilan is dissolved in organic solvent, and slowly instills diluted acid, be then placed on magnetic stirring apparatus and stir, make organosilan and organic solvent reaction thoroughly, obtain the hydrosol; The volume ratio of described organosilan, organic solvent and diluted acid is (16 ~ 20): (30 ~ 50): (0.2 ~ 0.3); The concentration of described diluted acid is 0.01mol/L ~ 0.1mol/L;
Under A2, normal temperature, Rh6G powder is dissolved in organic solvent, obtains the Rh6G solution that mass concentration is 0.001g/ml ~ 0.008g/ml;
Under A3, normal temperature, Rh6G solution is mixed with the hydrosol after stirring, more slowly drips ammoniacal liquor; Dropwise latter standing aging 24 hours ~ 48 hours, obtain SiO 2-Rh6G gel; The volume ratio of described Rh6G solution, the hydrosol, ammoniacal liquor is (6 ~ 12): (50 ~ 60): (0.1 ~ 0.2).
Further, in steps A 1, organosilan is the one in tetraethyl orthosilicate, methyl silicate, methyltrimethoxy silane, multi-polysiloxane; Organic solvent is the one in absolute methanol, absolute ethyl alcohol, propyl alcohol; Diluted acid is the one in watery hydrochloric acid, dilute sulfuric acid, oxalic acid, citric acid.
Further, in steps A 2, organic solvent is the one in absolute ethyl alcohol, absolute methanol, DMF.
Further, in steps A 3, the mass fraction of ammoniacal liquor is 20% ~ 50%.
The invention has the beneficial effects as follows: the excellent and SiO that price is relatively low of utility of the present invention 2-Rh6G gel rubber material, as the disordered chain medium of accidental laser, utilizes SiO 2-Rh6G gel rubber material has continuous random network configuration and is conducive to the nanoscale particle of photon multiple scattering and gain and the characteristic of space distribution, it is made to be under 532nm pulse laser excites at wavelength, form laser by the Anderson localization characteristic of photon and shake resonant cavity, thus produce the Random Laser emission spectrum of visible light wave range.The transmitting threshold value that present invention efficiently solves accidental laser in prior art is higher, efficiency is lower and the problem that use cost is higher, has broad application prospects in scientific research and industrial production.
Accompanying drawing explanation
The optical pumping SiO that Fig. 1 provides for the embodiment of the present invention 2-Rh6G gel accidental laser structural representation.
Fig. 2 is optical pumping SiO 2the photic emission spectra curve chart of-Rh6G gel rubber material accidental laser.
Fig. 3 is optical pumping SiO provided by the invention 2the using method flow chart of-Rh6G gel accidental laser.
Fig. 4 is optical pumping SiO provided by the invention 2preparation method's flow chart of-Rh6G gel rubber material.
Description of reference numerals: 1-pump light source, 2-spiral attenuator, 3-focusing convex lens, 4-speculum, 5-SiO 2-Rh6G gel rubber material, 6-fiber spectrometer, 7-computer.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are further described.
Rh6G is rhodamine 6G, has another name called rose-red 6G, rhodamine 590 or rhodamine 6G; Its proterties is red or yellowish-brown powder, water-soluble in scarlet colour band green fluorescence, is dissolved in alcohol and takes on a red color band yellow fluorescence or yellowish red color band green fluorescence, can be used as adsorption indicator or biological stain.
The invention provides a kind of optical pumping SiO 2-Rh6G gel accidental laser, its structure as shown in Figure 1, comprises pump light source 1, spiral attenuator 2, focuses on convex lens 3 and SiO 2-Rh6G gel rubber material 5; The emergent light of pump light source 1 is again through focusing on convex lens 3 after spiral attenuator 2, and making it converge is a focused beam, and then focused beam impinges perpendicularly on SiO 2-Rh6G gel rubber material 5 surface, then through SiO 2the multiple scattering of-Rh6G gel rubber material 5 and gain, finally obtain the emission spectrum of accidental laser.
Wherein, pump light source 1 is pulse laser, and the green laser of its emergent light to be wavelength be 532nm, the emanated energy of this laser is larger.
In order to avoid thermal effect is to SiO 2the luminescence queenching phenomenon that the damage of-Rh6G gel rubber material 5 and thermal effect may cause, by the emergent light of pump light source 1 through spiral attenuator 2, can be reduced to 0.2mJ ~ 0.9mJ.The attenuation rate of spiral attenuator 2 is chosen as 10% ~ 90% according to the energy of pump light source 1.
Focus on convex lens 3 for strengthening the intensity of the pump light after energy attenuation, and pooled a focused beam.According to the spot size of the pump light after energy attenuation, the focal length focusing on convex lens 3 is chosen as 200mm ~ 800mm, and the focal length focusing on convex lens 3 in the present embodiment is preferably 500mm.
SiO 2-Rh6G gel rubber material 5 for have launch Random Laser characteristic mix Rh6G porous SiO 2gel rubber material, as the material of scattering medium, its pore size is 300nm ~ 900nm.SiO 2-Rh6G gel rubber material 5 has continuous random network configuration and is conducive to the nanoscale particle of photon multiple scattering and gain and the characteristic of space distribution, for the multiple scattering of photon and gain create favourable condition, thus improve the intensity of Random Laser and reduce pumping threshold.Meanwhile, because the structure that gel is special makes it also have numerous functions such as fire prevention, sound insulation, printing opacity, and its manufacture craft is simple, cost is low, makes it have broad application prospects in calorifics, acoustics, optics, particle detection.In the present invention, SiO 2-Rh6G gel rubber material 5, under pulse laser excites, forms laser by the Anderson localization characteristic of photon and shakes resonant cavity, thus produce the Random Laser emission spectrum of visible light wave range.
Optical pumping SiO 2the photic emission spectra of-Rh6G gel rubber material accidental laser as shown in Figure 2, wherein can observe the narrow linewidth emission peak that two have complete below the peak half-breadth 3nm of Random Laser characteristic, therefore optical pumping SiO in the visible region of wavelength 560nm ~ 580nm 2the emission spectrum wave band of-Rh6G gel rubber material accidental laser is 560nm ~ 580nm.Optical pumping SiO 2the emission spectrum of-Rh6G gel rubber material accidental laser is observed by fiber spectrometer 6, and observed direction is and SiO 2the direction that-Rh6G gel rubber material 5 surface is fixing in random selecting one on the anchor ring of 60 degree, fiber spectrometer 6 is connected by data acquisition line concentration with computer 7.
For convenience of observation, can at focusing convex lens 3 and SiO 2a speculum 4 is set between-Rh6G gel rubber material 5 to adjust the direction of focused beam.In the present embodiment, speculum 4 is silver-plated completely reflecting mirror, is reflected by the focused beam that focusing convex lens 3 converge, and makes its incident direction change 90 degree and impinge perpendicularly on SiO 2-Rh6G gel rubber material 5 surface.
Present invention also offers a kind of optical pumping SiO 2the using method of-Rh6G gel accidental laser, as shown in Figure 3, comprises the following steps:
S1, by the emergent light of pump light source 1 through spiral attenuator 2, can 0.2mJ ~ 0.9mJ be decayed to;
S2, by the pump light after energy attenuation by focus on convex lens 3, making it converge is a focused beam;
S3, by SiO 2-Rh6G gel rubber material 5 is placed in focused beam focus place, makes pump light impinge perpendicularly on SiO 2-Rh6G gel rubber material 5 surface.
For convenience of observation, can at focusing convex lens 3 and SiO 2a speculum 4 is set between-Rh6G gel rubber material 5 to adjust the direction of focused beam.
It is pointed out that the spiral attenuator 2 by selecting differential declines rate, the output energy of pump light can be changed, and then the Random Laser emission spectrum of varying strength can be observed in same observed direction.
Present invention also offers a kind of SiO 2the preparation method of-Rh6G gel rubber material, as shown in Figure 4, comprises the following steps:
Under A1, normal temperature, organosilan is dissolved in organic solvent, and slowly instills diluted acid, be then placed on magnetic stirring apparatus and stir, make organosilan and organic solvent reaction thoroughly, obtain the hydrosol; The volume ratio of above-mentioned organosilan, organic solvent and diluted acid is (16 ~ 20): (30 ~ 50): (0.2 ~ 0.3); The concentration of above-mentioned diluted acid is 0.01mol/L ~ 0.1mol/L.
Above-mentioned organosilan is the one in tetraethyl orthosilicate, methyl silicate, methyltrimethoxy silane, multi-polysiloxane; Above-mentioned organic solvent is the one in absolute methanol, absolute ethyl alcohol, propyl alcohol.The object adding diluted acid promotes that organosilan is hydrolyzed, generation colloidal sol, above-mentioned diluted acid to be pH value be 1 ~ 2 watery hydrochloric acid, dilute sulfuric acid, oxalic acid, one in citric acid.
The object of this step obtains the hydrosol, can be not limited to above-mentioned raw materials and be prepared, as long as can obtain above-mentioned SiO with following Rh6G powdered reaction by above-mentioned raw materials 2-Rh6G gel.
In this step, to the speed of agitator of magnetic stirring apparatus and time, there is no particular limitation, as long as can reach organosilan and organic solvent reacts object thoroughly.In the embodiment of the present invention, the magnetic stirrer range of speeds of employing is 250r/min ~ 750r/min, and mixing time is 2 hours ~ 6 hours.
Under A2, normal temperature, Rh6G powder is dissolved in organic solvent, obtains the Rh6G solution that mass concentration is 0.001g/ml ~ 0.008g/ml.
The object of this step is the ethanol solution obtaining Rh6G.Above-mentioned organic solvent is the one in absolute ethyl alcohol, absolute methanol, DMF etc.
Under A3, normal temperature, Rh6G solution is mixed with the hydrosol after stirring, more slowly drips ammoniacal liquor; Dropwise latter standing aging 24 hours ~ 48 hours, obtain SiO 2-Rh6G gel; The volume range of above-mentioned Rh6G solution, the hydrosol, ammoniacal liquor is (6 ~ 12): (50 ~ 60): (0.1 ~ 0.2).
The object of this step is that the aging reaction of the hydrosol that the Rh6G solution that obtained by steps A 2 and steps A 1 are obtained obtains SiO 2-Rh6G gel.The object of slow instillation ammoniacal liquor is that the mixed solution pH value of above-mentioned Rh6G solution and the hydrosol is adjusted to 7 ~ 8, promotes the polycondensation of particulate, reduces the time of gel-forming.The mass fraction of above-mentioned ammoniacal liquor is 20% ~ 50%.In this step, be not particularly limited the drop rate of ammoniacal liquor, as long as can achieve the above object, in the embodiment of the present invention, the drop rate of ammoniacal liquor is 3 droplets/minute.
Below with embodiment 1 ~ embodiment 3 to above-mentioned SiO 2the preparation method of-Rh6G gel rubber material illustrates.
Embodiment 1:
Under A1, normal temperature, 16ml tetraethyl orthosilicate is dissolved in 30ml absolute ethyl alcohol, and slowly instills 0.2ml watery hydrochloric acid, be then placed on magnetic stirring apparatus and stir 2 hours with 250r/min, make tetraethyl orthosilicate and absolute ethyl alcohol reaction thoroughly namely obtain the hydrosol; The concentration of above-mentioned watery hydrochloric acid is 0.01mol/L;
Under A2, normal temperature, 0.01g Rh6G powder is dissolved in 10ml absolute ethyl alcohol, obtains the Rh6G solution that mass concentration is 0.001g/ml;
Under A3, normal temperature, 6ml Rh6G solution is mixed with the above-mentioned hydrosol of 50ml, more slowly drip 0.1ml ammoniacal liquor; Dropwise latter standing aging 24 hours, obtain SiO 2-Rh6G gel; The drop rate of above-mentioned ammoniacal liquor is 3 droplets/minute, and mass fraction is 20%.
Embodiment 2:
Under A1, normal temperature, 20ml methyl silicate is dissolved in 50ml absolute methanol, and slowly instills 0.3ml dilute sulfuric acid, be then placed on magnetic stirring apparatus and stir 6 hours with 750r/min, make methyl silicate and absolute methanol reaction thoroughly namely obtain the hydrosol; The concentration of above-mentioned dilute sulfuric acid is 0.1mol/L;
Under A2, normal temperature, 0.08g Rh6G powder is dissolved in 10ml absolute methanol, obtains the Rh6G solution that mass concentration is 0.008g/ml;
Under A3, normal temperature, 12ml Rh6G solution is mixed with the above-mentioned hydrosol of 60ml, more slowly drip 0.2ml ammoniacal liquor; Dropwise latter standing aging 48 hours, obtain SiO 2-Rh6G gel; The drop rate of above-mentioned ammoniacal liquor is 3 droplets/minute, and mass fraction is 50%.
Embodiment 3:
Under A1, normal temperature, 18ml methyltrimethoxy silane is dissolved in 40ml propyl alcohol, and slowly instills 0.25ml oxalic acid; Then be placed on magnetic stirring apparatus and stir 4 hours with 600r/min, make methyltrimethoxy silane and propyl alcohol reaction thoroughly namely obtain the hydrosol; The concentration of above-mentioned oxalic acid is 0.05mol/L;
Under A2, normal temperature, 0.05g Rh6G powder is dissolved in 10ml DMF, obtains the Rh6G solution that mass concentration is 0.005g/ml;
Under A3, normal temperature, 10ml Rh6G solution is mixed with the above-mentioned hydrosol of 55ml, more slowly drip 0.15ml ammoniacal liquor; Dropwise latter standing aging 36 hours, obtain SiO 2-Rh6G gel; The drop rate of above-mentioned ammoniacal liquor is 3 droplets/minute, and mass fraction is 30%.
Those of ordinary skill in the art will appreciate that, embodiment described here is to help reader understanding's principle of the present invention, should be understood to that protection scope of the present invention is not limited to so special statement and embodiment.Those of ordinary skill in the art can make various other various concrete distortion and combination of not departing from essence of the present invention according to these technology enlightenment disclosed by the invention, and these distortion and combination are still in protection scope of the present invention.

Claims (10)

1. an optical pumping SiO 2-Rh6G gel accidental laser, is characterized in that, comprises pump light source (1), spiral attenuator (2), focuses on convex lens (3) and SiO 2-Rh6G gel rubber material (5); The emergent light of described pump light source (1) is again through focusing on convex lens (3) after spiral attenuator (2), and making it converge is a focused beam, and then focused beam impinges perpendicularly on SiO 2-Rh6G gel rubber material (5) surface, then through SiO 2the multiple scattering of-Rh6G gel rubber material (5) and gain, finally obtain the emission spectrum of accidental laser.
2. optical pumping SiO according to claim 1 2-Rh6G gel accidental laser, is characterized in that, described accidental laser also comprises speculum (4); Described speculum (4) is positioned at and focuses on convex lens (3) and SiO 2between-Rh6G gel rubber material (5), for adjusting the direction of focused beam.
3. optical pumping SiO according to claim 1 2-Rh6G gel accidental laser, is characterized in that, described pump light source (1) is pulse laser, the green laser of its emergent light to be wavelength be 532nm; The attenuation rate of described spiral attenuator (2) is chosen as 10% ~ 90% according to the energy of pump light source (1); The focal length of described focusing convex lens (3) is 200mm ~ 800mm.
4. optical pumping SiO according to claim 1 2-Rh6G gel accidental laser, is characterized in that, described SiO 2-Rh6G gel rubber material (5) for have launch Random Laser characteristic mix Rh6G porous SiO 2gel rubber material, as the material of scattering medium; Described SiO 2the pore size of-Rh6G gel rubber material (5) is 300nm ~ 900nm.
5. optical pumping SiO according to claim 2 2-Rh6G gel accidental laser, is characterized in that, the emission spectrum of described accidental laser is observed by fiber spectrometer (6), and observed direction is and SiO 2the direction that-Rh6G gel rubber material (5) surface is fixing in random selecting one on the anchor ring of 60 degree; Described fiber spectrometer (6) is connected by data acquisition line concentration with computer (7).
6. an optical pumping SiO 2the using method of-Rh6G gel accidental laser, is characterized in that, comprise the following steps:
S1, by the emergent light of pump light source (1) through spiral attenuator (2), can 0.2mJ ~ 0.9mJ be decayed to;
S2, by the pump light after energy attenuation by focus on convex lens (3), making it converge is a focused beam;
S3, by SiO 2-Rh6G gel rubber material (5) is placed in focused beam focus place, makes pump light impinge perpendicularly on SiO 2-Rh6G gel rubber material (5) surface.
7. a SiO 2the preparation method of-Rh6G gel rubber material, is characterized in that, comprises the following steps:
Under A1, normal temperature, organosilan is dissolved in organic solvent, and slowly instills diluted acid, be then placed on magnetic stirring apparatus and stir, make organosilan and organic solvent reaction thoroughly, obtain the hydrosol; The volume ratio of described organosilan, organic solvent and diluted acid is (16 ~ 20): (30 ~ 50): (0.2 ~ 0.3); The concentration of described diluted acid is 0.01mol/L ~ 0.1mol/L;
Under A2, normal temperature, Rh6G powder is dissolved in organic solvent, obtains the Rh6G solution that mass concentration is 0.001g/ml ~ 0.008g/ml;
Under A3, normal temperature, Rh6G solution is mixed with the hydrosol after stirring, more slowly drips ammoniacal liquor; Dropwise latter standing aging 24 hours ~ 48 hours, obtain SiO 2-Rh6G gel; The volume ratio of described Rh6G solution, the hydrosol, ammoniacal liquor is (6 ~ 12): (50 ~ 60): (0.1 ~ 0.2).
8. SiO according to claim 7 2the preparation method of-Rh6G gel rubber material, is characterized in that, in described steps A 1, organosilan is the one in tetraethyl orthosilicate, methyl silicate, methyltrimethoxy silane, multi-polysiloxane; Organic solvent is the one in absolute methanol, absolute ethyl alcohol, propyl alcohol; Diluted acid is the one of watery hydrochloric acid, dilute sulfuric acid, oxalic acid, citric acid.
9. SiO according to claim 7 2the preparation method of-Rh6G gel rubber material, is characterized in that, in described steps A 2, organic solvent is the one in absolute ethyl alcohol, absolute methanol, DMF.
10. the preparation method of SiO2-Rh6G gel rubber material according to claim 7, is characterized in that, in described steps A 3, the mass fraction of ammoniacal liquor is 20% ~ 50%.
CN201510131799.2A 2015-03-25 2015-03-25 Optical pumping SiO2- Rh6G gel accidental lasers and preparation method thereof Expired - Fee Related CN104716553B (en)

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