CN106329306A - Nanometer aperture structure based disordered gain medium preparing method - Google Patents
Nanometer aperture structure based disordered gain medium preparing method Download PDFInfo
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- CN106329306A CN106329306A CN201610861230.6A CN201610861230A CN106329306A CN 106329306 A CN106329306 A CN 106329306A CN 201610861230 A CN201610861230 A CN 201610861230A CN 106329306 A CN106329306 A CN 106329306A
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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
- H01S3/169—Nanoparticles, e.g. doped nanoparticles acting as a gain material
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Abstract
The invention provides a nanometer aperture structure based disordered gain medium preparing method, which adopts a simply operative spin coating and film forming method. In the method, methanol and THF are used as mixed solvent; PMMA and PS are used as film base materials. Through the spin-coating method, a phase separation structure is formed in the film. After removal of PS with selective solvent of cyclohexane, a two-dimensional disordered dielectric sample consisting of PMMA and air nanometer apertures is obtained. The nanometer aperture structure based disordered gain medium obtained by this method has uniform sized and good dispersion performance provided dispersion units. Through the change in preparing technology parameters to further control the parameters of the size, the shape, and the filling rate, it is possible to realize the control of random laser output modes.
Description
Technical field
The invention belongs to organic nano material preparing technical field, particularly to a kind of based on nanoaperture structure unordered
The preparation method of gain media.
Background technology
Random Laser refers to the stimulated radiation phenomenon that photon multiple scattering in random media is formed, and it shakes
Swing pattern and be decided by multiple scattering event, and export a nondirectional relative photo.Due to photon travel path in media as well
Being random, " Random Laser (Random Laser) " this title was suggested first in nineteen ninety-five.Subsequently, various countries scientist exists
Multiple random media all observes Random Laser radiation phenomenon, to the complicated physics occurred in random media
The understanding of process is the most clear.Random Laser is due to the physical mechanism of its uniqueness and is widely applied prospect, is swashing in recent years
Optical physics is of great interest with photoelectron technical field.
In recent years, cause the great interest of scientists about Random Laser applied research in optoelectronic areas,
And study hotspot is concentrated mainly in the preparation method of random media.The class of the most relatively common random media
Type mainly has laser crystal powder, and the colloidal suspension solution that laser dye forms with metal oxide particle, mixed with laser dye
With polymer flake or the thin film of scattering particles, semiconductive thin film or cluster sample, laser dye and liquid crystal compound etc..So
And, these preparation methoies above-mentioned suffer from many deficiencies in application, and such as random configuration is uncontrollable, poor stability, collection
One-tenth degree is low.From the operation principle of Random Laser, the characteristic of radiant light is decided by photon multiple scattering mistake in media as well
Journey, and multiple scattering is affected by the morphological parameters of scattering particles.Therefore, the control to radiant light to be realized, be necessary for passing through
Change the aspect parameters such as the shape of scattering particles, size and packed density to realize.On the other hand, according to Mie scattering theory,
Photon generation effective with multiple scattering process to be made, the yardstick of its scattering particles can must be compared with optical wavelength.We are felt
The optical region of the active optical component of interest, corresponding scattering particles yardstick should be nanometer scale.
At present, the preparation method of nanostructured is a lot, such as beamwriter lithography, reactive ion etching, electron beam evaporation and stripping
From technology such as technology and femtosecond laser direct write.But, costly, cost is high, complex process for the equipment needed for these technology,
It is unfavorable for that the large-scale promotion of nanometer active optical component, the preparation technology of nanoaperture structure then can solve the problem that above-mentioned asking
Topic.
Summary of the invention
Instant invention overcomes shortcoming of the prior art, it is provided that a kind of random media based on nanoaperture structure
Preparation method, the method step is simple, with low cost, green general-purpose.Utilize nanoporous film prepared by this technology, its hole
Gap pattern is homogeneous, good dispersion, and the structural parameters such as the size of hole and filling rate can be joined by the technique in preparation process
Number control effectively.The random media obtained, the luminous intensity of its Random Laser is higher, and mode stability is good, can
For preparing active optical waveguide device, it is possible to the aspects such as optics shows, optical sensing are used widely.
In order to solve above-mentioned technical problem, the present invention is achieved by the following technical solutions:
The preparation method of a kind of random media based on nanoaperture structure, comprises the following steps:
A, substrate clean；
B, by methanol and THF using the ratio mix homogeneously of 4:1 as solvent；Take PMMA and the PS mixing conduct of identical weight
Solute, the mean molecule quantity of PMMA and PS is respectively 100000 and 70000, with the proportional arrangement solution that mass percent is 4%,
And stir；
C, laser dye rhodamine 6G (Rh6G) is added in step b gained solution, and add 1-2ml hydroxyethyl methacrylate
Ethyl ester controls at 5*10 as cosolvent, dye strength-3About mol/L, magnetic agitation 20-30 minute, obtain orange transparent molten
Liquid；
D, utilizing spin coating instrument to be spin-coated on silicon chip by step c gained solution, ambient temperature controls at about 20～25 DEG C, phase
To humidity less than 40%；
E, step d gained thin film is put in vacuum drying oven, is dried 15 minutes with 70 DEG C, thin film is carried out heat cure,
I.e. can get film sample；
F, the film sample of step e gained is put in cyclohexane solution, and be heated to 60 DEG C, take out after 1 minute, can be by
PS in sample removes；Again sample is dried 15 minutes with 70 DEG C, final acquisition PMMA and the film sample of air void structure.
Further, described substrate cleans and includes deionized water rinsing, and concentrated sulphuric acid removes metal-oxide, and acetone goes oil removing
Fat, ammonia removes remaining concentrated sulphuric acid, hydrogen peroxide flushing and drying.
Further, described spin coating process first with 500～700rpm low speed prerotation, the time is several seconds, and turning in advance
Journey instills solution on silicon chip, it is therefore an objective to tentatively got rid of by unnecessary solution；Then carry out high speed rotating, rotating speed 2000～
Selecting between 4000rpm, the persistent period is about 40 seconds, controls film thickness by changing rotating speed and persistent period.
Compared with prior art, the invention has the beneficial effects as follows:
A kind of preparation method based on nanoaperture structural disorder gain media of the present invention, uses operation easy
Spin-coating film method, uses methanol and oxolane (THF) as mixed solvent, utilizes PMMA and PS as film substrate, pass through
Spin-coating method forms phase separation structure in the film, can obtain by PMMA and air after being removed by PS with selective solvent hexamethylene
Nanoaperture composition two-dimentional Disordered Media sample, the method low cost, simplicity, environmental protection, it is adaptable to multiple different substrate materials and send out
The preparation of the random media of light center.Using the nanoaperture random media that this method obtains, its scattering unit is big
Little more uniform, good dispersion, it is possible to control the pattern ginsengs such as its size, shape and filling rate by changing preparation technology parameter
Number, thus realize the control to Random Laser output mode.The random media of this high-luminous-efficiency can be used for preparation to be had
Source fiber waveguide device, it is possible to the aspects such as optics shows, optical sensing are used widely.
Accompanying drawing explanation
Accompanying drawing is used for providing a further understanding of the present invention, is used for together with embodiments of the present invention explaining the present invention,
It is not intended that limitation of the present invention, in the accompanying drawings:
Fig. 1 is the scanning electron microscope diagram preparing nanoporous film；
Fig. 2 is the random media of preparation spectral radiance map under different pulsed laser energies excite；
Fig. 3 is the input-output curve of the random media Random Laser radiation of preparation；
Detailed description of the invention
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are illustrated, it will be appreciated that preferred reality described herein
Execute example be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Prepared by random media based on nanoaperture structure, specifically comprise the following steps that
1, select silicon chip a diameter of 1 inch, crystal orientation is [111] type, shows that irregularity degree is less than 1 micron.Use deionization
Water rinse substrate repeatedly, removes the dust of physical absorption above substrate；Substrate is put in concentrated sulphuric acid and boils, in order to remove substrate
The organic impurities on surface and metal-oxide；By deionized water rinse substrate repeatedly；Then use acetone ultrasonic cleaning, remove various
Oils and fats；Substrate is put in ammonia and boils, remove the concentrated sulphuric acid of remaining；Clear with deionized water flushing ammonia repeatedly with hydrogen peroxide
Washed substrate；Substrate is put in baking oven and dry, standby.
2, methanol and oxolane 40ml and 10ml mix homogeneously are taken respectively as solvent；Take PMMA and PS each 0.8g mixing
As solute, the mean molecule quantity of PMMA and PS is respectively 100000 and 70000.Magnetic agitation is completely dissolved to PMMA and PS.
3,0.12g rhodamine 6G (Rh6G) is added in step 2 gained solution, and add 2ml hydroxyethyl methylacrylate
(HEMA) as cosolvent, magnetic agitation is fully dissolved for 30 minutes to dyestuff, obtains orange clear solution.
4, utilizing spin coating instrument to be spin-coated on silicon chip by step 3 gained solution, ambient temperature controls at about 20～25 DEG C, phase
To humidity less than 40%.Spin coating process is first with the low speed prerotation of 500rpm, and the time is usually several seconds, and past during prerotation
Solution is instilled, it is therefore an objective to tentatively got rid of by unnecessary solution on silicon chip；Then carrying out high speed rotating, rotating speed is 3000rpm, continues
Time is usually 40 seconds.The silicon chip being fixed on disk axes in this stage rapidly rotates, and the flowing of air simultaneously makes solvent
Volatilization aggravation, forms one layer of uniform thin polymer film on substrate.
5, step 4 gained thin film is put in vacuum drying oven, is dried 15 minutes with 70 DEG C, thin film is carried out heat cure,
I.e. can get adhesiveness and the preferable film sample of mechanical strength.
6, the film sample of step 5 gained is put in cyclohexane solution, and be heated to 60 DEG C, take out after 1 minute, can be by
Polystyrene (PS) in sample is removed.Sample is dried 15 minutes with 70 DEG C, final PMMA and the air void structure of obtaining
Film sample.The SEM pattern of sample is as shown in Figure 1.
7, utilize the Nd:YAG laser of frequency multiplication as excitation light, sample is carried out photoluminescence experiment, can obtain random sharp
The spectrogram of light radiation and input-output curve, the most as shown in Figure 2,3, the upper, middle and lower line of Fig. 2 is 0.018mJ respectively,
0.012mJ, 0.006mJ.
If adding appropriate laser dye during organic solution configures, dye molecule is made to embed polymethyl
In acid formicester (PMMA) substrate, i.e. it is available for producing the random media of Random Laser.Using nanoaperture as unordered
The scattering center of medium, the generation for Random Laser provides multiple scattering event.
PHASE SEPARATION principle and traditional spin-coating film technique is used to prepare Nanoporous Polymer Films.This technique is only
Including the coating of simple solution and two processes of evaporation, it requires that the material of shape film forming layer must be able to be dissolved in certain solvent.
Owing to spin-coating film Processes and apparatus relatively other film technique is simply a lot, it has been widely used in microcircuit manufacture, light
Multiple fields such as prepared by dish plated film, optical device, anti-reflection film making.From the point of view of most polymer, as long as selecting suitably
Solvent just can be dissolved and be formed uniform and stable solution；And the molecular weight of polymer is general the biggest, its solution has
There are the best viscous force and film forming characteristics.
The preparation of Nanoporous Polymer Films is different from again simply revolves film, being mainly characterized by two kinds of polymer of it
Being codissolved in a kind of solvent, film forming latter two polymer occurs to be separated, thus forming a wherein phase is Discrete Distribution, and another phase is
The special construction of continuous distribution.Then, being immersed by thin film in selective solvent, this solvent can only dissolve one of which polymer
And another kind can not be dissolved.When being the formation of Nanoporous Polymer Films after the polymer getting rid of wherein Discrete Distribution, from
And obtain the Disordered Media structure of a kind of two dimension.As long as we add suitable laser dye during the configuration of polymer solution
Material, dye molecule group will be embedded in polymer, thus forms the random media that can produce Random Laser output.
Use laser to excite sample, then dye molecule can form induced transition as the centre of luminescence and produce random
Laser exports.The method low cost, easy and simple to handle, it is adaptable to other organic host materials and the active nano-device of gain substance
Preparation.
Using the random media that this method prepares, its scattering particles regular shape, uniformity are good, size is controlled.This
The unordered gain material of nanoaperture planting high-luminous-efficiency can be as novel active light functional material, at organic optical waveguide device
The aspects such as part, optics show, optical sensing are all with a wide range of applications.Develop unordered gain based on nanoaperture structure
The simple technology of preparing of medium, the development to subjects such as chemistry, material and photoelectrons all has important promotion meaning.
The random media of this high-luminous-efficiency can be used for preparing active optical waveguide device, it is possible to optics shows, light
Learn the aspects such as sensing to be used widely.
Finally it is noted that these are only the preferred embodiments of the present invention, it is not limited to the present invention, although
Being described in detail the present invention with reference to embodiment, for a person skilled in the art, it still can be to aforementioned
Technical scheme described in each embodiment is modified, or wherein portion of techniques feature carries out equivalent, but all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included in the protection of the present invention
Within the scope of.
Claims (3)
1. the preparation method of a random media based on nanoaperture structure, it is characterised in that comprise the following steps:
A, substrate clean；
B, by methanol and THF using the ratio mix homogeneously of 4:1 as solvent；PMMA and PS taking identical weight mixes as molten
Matter, the mean molecule quantity of PMMA and PS is respectively 100000 and 70000, with the proportional arrangement solution that mass percent is 4%, and
Stir；
C, laser dye rhodamine 6G (Rh6G) is added in step b gained solution, and add 1-2ml hydroxyethyl methylacrylate
As cosolvent, dye strength controls at 5*10-3About mol/L, magnetic agitation 20-30 minute, obtain orange clear solution；
D, utilizing spin coating instrument to be spin-coated on silicon chip by step c gained solution, ambient temperature controls at about 20～25 DEG C, the wettest
Degree is less than 40%；
E, step d gained thin film is put in vacuum drying oven, is dried 15 minutes with 70 DEG C, thin film is carried out heat cure,
Obtain film sample；
F, the film sample of step e gained is put in cyclohexane solution, and be heated to 60 DEG C, take out after 1 minute, can be by sample
In PS remove；Again sample is dried 15 minutes with 70 DEG C, final acquisition PMMA and the film sample of air void structure.
The preparation method of a kind of random media based on nanoaperture structure, its feature exists
In, described substrate cleans and includes deionized water rinsing, and concentrated sulphuric acid removes metal-oxide, and acetone removes oils and fats, and ammonia is removed residual
Remaining concentrated sulphuric acid, hydrogen peroxide rinses and dries.
The preparation method of a kind of random media based on nanoaperture structure, its feature exists
In, described spin coating process first with 500～700rpm low speed prerotation, the time is several seconds, and toward on silicon chip during prerotation
Instill solution, it is therefore an objective to tentatively got rid of by unnecessary solution；Then carrying out high speed rotating, rotating speed is between 2000～4000rpm
Selecting, the persistent period is about 40 seconds, controls film thickness by changing rotating speed and persistent period.
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Cited By (4)
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| CN109137123A (en) * | 2018-08-14 | 2019-01-04 | 郑州大学 | A method of preparing polycarbazole derivates nanometer fiber |
| CN109687282A (en) * | 2019-02-11 | 2019-04-26 | 中国科学院微电子研究所 | Three-dimensional metamaterial surface phasmon laser |
| CN109873289A (en) * | 2019-04-04 | 2019-06-11 | 北京师范大学 | A kind of optical fiber source that output can switch between laser and Random Laser |
| CN115894090B (en) * | 2022-11-17 | 2024-03-22 | 中国工程物理研究院激光聚变研究中心 | Method for preparing high-reflection-resistance sub-wavelength structure on surface of brittle and hard material |
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| CN115894090B (en) * | 2022-11-17 | 2024-03-22 | 中国工程物理研究院激光聚变研究中心 | Method for preparing high-reflection-resistance sub-wavelength structure on surface of brittle and hard material |
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