CN103352255A - Preparation method of photonic crystal with inverse opal structure - Google Patents
Preparation method of photonic crystal with inverse opal structure Download PDFInfo
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- CN103352255A CN103352255A CN2013102511986A CN201310251198A CN103352255A CN 103352255 A CN103352255 A CN 103352255A CN 2013102511986 A CN2013102511986 A CN 2013102511986A CN 201310251198 A CN201310251198 A CN 201310251198A CN 103352255 A CN103352255 A CN 103352255A
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Abstract
The invention discloses a preparation method of a photonic crystal with an inverse opal structure, and belongs to the technical field of the photonic crystal with the inverse opal structure. The preparation method comprises the following technological steps of: firstly adding polymeric microspheres to colloidal sol in proportions, and then dispersing the mixture for 10-60 minutes by using ultrasonic waves so as to form a uniform stable suspension emulsion; transferring the prepared suspended emulsion to a glass container, and vertically placing a clean substrate in the glass container filled with the suspended emulsion; then slantwise placing the glass container on a heating platform, and heating so as to volatilize a solvent; utilizing a binary synergistic effect for ensuring that polymeric microspheres and the colloidal sol grow on the substrate in a self-organizing manner to form a polymer; after ending growth, taking out a sample, and heating in air under an appropriate temperature condition so as to decompose and volatize the polymer; cooling and taking the sample to obtain the photonic crystal with the inverse opal structure, which has good degree of crystallinity and no defects and is large in area.
Description
Technical field
The invention belongs to the photonic crystal with inverse opal structure technical field, a kind of preparation method with photonic crystal of counter opal structure particularly is provided, can prepare the photonic crystal of big area, flawless counter opal structure.
Background technology
Photonic crystal is the structure that is periodic arrangement by the dielectric material of differing dielectric constant in the space.Be similar to the behavior of electronics in semiconductor crystal, when photon is propagated in photonic crystal, be subject to the relatively strong scattering of the nonhomogeneous media of periodic arrangement with arrange hertzian wave with magnitude of medium period, so that the electronic wave in this wavelength region are forbidden propagating and producing photon band gap at photonic crystal.In addition, photonic crystal also has the characteristics such as the spontaneous radiation of inhibition, photon limitation.Relative electronics, photon has all surpassed electronics from far away in the performance of the aspects such as velocity of propagation, information content, anti-interference, efficient, responding ability, energy waste, interconnection and parallel ability.The appearance of photonic crystal makes microminiaturization and the integrated possibility that becomes of the information processing technology " full photon " and photon technology, and it may cause the again revolution of information technology in the near future.
According to the dimension of dielectric medium period profile in the space, photonic crystal can be divided into one dimension, two and three dimensions photonic crystal.The complete processing of one dimension, 2 D photon crystal is comparatively simple, relevant photonic device is developed in succession, such as the photonic crystal resonant cavity of the ultrahigh quality factor, efficient multi-channel photon crystal filter, ultrahigh resolution short wavelength photons crystal laser etc.And the three-D photon crystal preparation is relatively difficult, especially in the visible region scope, the cycle lattice parameter of requirement very little (100-600nm) is based on the micro-nano processing technology on plane, be difficult to prepare so meticulous three-dimensional structure, therefore greatly hindered development and the application of photonic crystal.
The colloidal self-assembly method is that a kind of optics that is applicable to is to the method for near infrared band three-dimensional photon crystal preparation.It utilizes inducing or positive action of the external force such as gravity, centrifugal force, surface tension, pressure, electrical forces, magnetic field force usually, make the mono-dispersion microballoon displacement, add the interaction (electrostatic force or Van der Waals force) on surface between the microballoon, thereby make microballoon be self-assembled into periodic structure.The colloidal self-assembly process generally is easy to form stable face-centred cubic structure, usually is referred to as opal structural; Utilize chemical vapour deposition, electrochemical deposition or sol-gel method etc. to fill the material of differing dielectric constant in the space of opal structural, then remove the opal template, the periodic structure that obtains is referred to as counter opal structure.
Traditional method for preparing counter opal structure generally is divided into three steps: at first utilize polymer microballoon to prepare the opal structural template, then template is immersed corresponding precursor (SiO
2, TiO
2Deng) in solution or colloid in, remove at last template and obtain counter opal structure.The following weak point of this method: the one, because opaline space is less, the colloid that wish is filled is difficult to fill the space fully, causes some defective; The 2nd, in the process that immerses, the opal structural destruction that easily comes off.Although utilize successively vapour deposition process (such as ald), can obtain high quality, flawless photonic crystal with inverse opal structure, this process needs to consume a large amount of human and material resources and financial resources, also needs high-quality opal template simultaneously.Therefore, want to make counter opal structure to obtain to use widely, the needs exploitation is a kind of can to prepare big area, the method for zero defect, high-quality counter opal structure easily.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with photonic crystal of counter opal structure, utilize the binary synergistic effect, at first prepare polymeric colloid microballoon and SiO
2The binary stabilising system of colloidal sol, take this system as raw material, then the periodicity composite structure of a step assembling colloid micro ball and gel removes the colloidal spheres template, can obtain the photonic crystal of high quality, big area, flawless counter opal structure.The method is simple, quick, good reproducibility.The present invention can prepare high quality, big area, zero defect counter opal structure.The concrete technology step is as follows:
(1) at first the polymer microballoon (such as polystyrene microsphere) of finite concentration, certain particle diameter is joined in the certain density colloidal sol according to a certain percentage, then utilize ultrasonic wave to disperse 5-60 minute, make it to form uniform and stable suspended emulsion.
(2) above-mentioned prepared suspended emulsion is transferred in the sizeable Glass Containers, and a substrate cleaning, sizeable (such as glass, silicon single crystal, quartz etc.) vertically is placed in the Glass Containers that above-mentioned suspended emulsion is housed; Then, to warm table, heating is slowly volatilized solvent the Glass Containers slant setting; Utilize the binary synergistic effect, allow polymer microballoon and colloidal sol grow in substrate in the mode of self-organization, form the periodicity composite structure of polymer microballoon and gel.
(3) growth complete after, take out sample, in air and under the suitable temperature condition, heat the regular hour, make the polymer unwinds volatilization; Sample is taken out in cooling, namely obtains the quality perfection, better crystallinity degree, the photonic crystal of zero defect, large-area counter opal structure.
In above-mentioned preparation method, the described polymer microballoon of step (1) can be polystyrene microsphere, poly (methyl methacrylate) micro-sphere etc.; The particle size range of described polymer microballoon is: between the 0.05-4um, and volume distributed median CV＜3%; Described suspended emulsion, the concentration of polymer microballoon are 0.01-1% (w/w: weight percent, solvent are water), the concentration of colloidal sol is 0.005-0.5%(w/w: weight percent, solvent is water), the ratio of both concentration is 2:1(w/w: weight percent, solvent are water).
The described colloidal sol of step (1) can be SiO
2Colloidal sol, TiO
2Colloidal sol, AgI colloidal sol etc. also can be the precursors of colloidal sol, such as tetraethoxysilane (TEOS), and tetrabutyl titanium etc.
The described Glass Containers of step (2) can be cuvette, beaker etc., is preferably square container.The container size is such as the 1cm*1cm*4cm cuvette.
The described substrate of step (2) can be glass, silicon single crystal, quartz, Copper Foil, aluminium foil etc., and it is smooth smooth that substrate is wanted, and its size is decided by Glass Containers and requirement of experiment.In the 1cm*1cm*4cm cuvette, can put into the quartz plate of 0.5cm*4cm.
Step (2) described the Glass Containers slant setting to warm table, obliquity can be selected between 15-90 °, preferably selects 15-75 °.
The described warm table of step (2), temperature range is controlled between 20-80 ℃, in conjunction with actual needs, between preferred 40-75 ℃.
Heated sample under the described temperature condition suitable in air of step (3) makes polymer unwinds volatilization, the temperature range of heating between 300-500 ℃, preferential 375 ℃.
Heated sample under the described temperature condition suitable in air of step (3), the time of heating is decided by the temperature of heating, and in general, temperature is higher, and required time is shorter.Be preferably in 6～20 hours heat-up time, preferred 10 hours.
The counter opal structure that above-mentioned preparation method provided by the invention obtains is ordered 3 D structure, and defective is less, and area is large (even can reach a centimetre magnitude), is combined firmly with substrate; This structure can be widely used in the fields such as high-performance optical device, sensor, catalyzer.
The present invention has following characteristics:
1, the ingenious binary synergistic effect of utilizing polymeric colloid microballoon and sol-gel (or its presoma) of the present invention, a step is self-assembled into big area, flawless periodicity composite structure jointly.Further by heating, the polymeric colloid microsphere template is decomposed, thereby obtain SiO
2, TiO
2Deng counter opal structure.
The particle size range of the polymkeric substance mono-dispersion microballoon of self-assembly that 2, the present invention participates in can be between the 0.05um-2um, thereby can realize the assembling of different size structural unit.
3, the polymer microballoon of the self-assembly that participates in and sol-gel presoma can have very wide concentration range among the present invention.
4, nontoxic pollution-free is carried out in self-assembly in the aqueous solution.
The advantages such as 5, the method is simple, and good reproducibility is easy to operate, and cost is lower.The counter opal structure that obtains is that defective is less, and quality is higher, the crystal region area is larger, can reach centimetre magnitude or larger.
Description of drawings
Fig. 1 is preparation SiO
2Counter opal structure experimental installation schematic diagram.Wherein, temperature control electric warm table 1, thermal conduction platform 2, temperature sensor 3, cuvette 4, polystyrene microsphere and SiO
2 Colloidal suspension emulsion 5, substrate 6.
Fig. 2 is prepared SiO
2The low power electron scanning micrograph of counter opal structure, this photo are perpendicular to the direction of growth (111) shooting.Can find out gained SiO from above-mentioned picture
2Counter opal ordered structure area is larger.
Fig. 3 is prepared SiO
2The electron scanning micrograph of counter opal structure, magnification are 10000 times, and this photo is perpendicular to that the direction of growth (111) takes.Can find out gained SiO from above-mentioned picture
2Counter opal ordered structure area is larger, smooth, smooth.
Fig. 4 is prepared SiO
2The high power electron scanning micrograph of counter opal structure, magnification are 20000 times.Prepared sample is the high-sequential structure, and the ordered structure unit is 330nm, along the growth of (111) direction, in the scope shown in the picture, without any defective.
Fig. 5 is prepared SiO
2The high power electron scanning micrograph of counter opal structure, magnification are 50000 times.Prepared sample is the high-sequential structure, and the ordered structure unit is 330nm, along the growth of (111) direction, in the scope shown in the picture, without any defective.
Fig. 6 is prepared SiO
2The electron scanning micrograph of counter opal structure, this photo takes along the direction of growth (110), and magnification is 5000 times.Can find out from this photo, this structure still is the high-sequential structure on (110) direction, thereby illustrates that this structure is ordered 3 D structure.
Fig. 7 is prepared SiO
2The electron scanning micrograph of counter opal structure, this photo is taken along the direction of growth (110), and magnification is 23000 times, from picture, can find out, be cubic grid structure in (110) direction., high-sequential still, zero defect.
Fig. 8 is prepared SiO
2The transmitted spectrum of counter opal structure and reflection spectrum curve.Wherein (a) is transmitted spectrum, and from spectrogram, the bandgap center position of this anti-protein structure is between 530-570nm, and the forbidden band half-width is about 40nm; (b) be reflection spectrum, the position height of reflection spectrum and projection spectrum overlaps, and illustrates that this structure does not almost have defective.
Embodiment
Embodiment:
Get respectively 0.1 milliliter 10% the polystyrene microsphere suspended emulsion (weight percent, particle diameter: 330nm) and 0.05 milliliter 10% the TEOS aqueous solution (weight percent is with SiO
2Meter) put into the cuvette of 4ml, and in above-mentioned cuvette, add three milliliters of mill-Q water, ultra-sonic dispersion 10 minutes, mentioned solution is mixed.Then the substrate of glass of a slice cleaning is vertically put into above-mentioned cuvette.Cuvette is put on the warm table, under 75 ℃ of conditions, polystyrene microsphere template and SiO
2The colloid matrix in substrate of glass assembling growth, is incubated 48 hours jointly, takes out, and obtains polystyrene microsphere and SiO
2The composite structure of colloid.Above-mentioned composite structure is put on the heat platform, and heating was taken out, thereby has been obtained high quality, flawless SiO after 10 hours in the air under 375 ℃ of conditions
2Counter opal structure.
Need to prove, above-described embodiment just is used for illustrating method feature of the present invention, not to limit patent claim of the present invention, also can be replaced by poly (methyl methacrylate) micro-sphere, the tetrabutyl titanium aqueous solution etc. respectively such as used polystyrene microsphere, TEOS solution in the present embodiment, but its principle still belongs to patent application category of the present invention.
Claims (9)
1. preparation method with photonic crystal of counter opal structure, it is characterized in that: processing step is:
(1) at first polymer microballoon is joined in the presoma of colloidal sol or colloidal sol in proportion, then utilize ultrasonic wave to disperse 5-60 minute, make it to form uniform and stable suspended emulsion;
Suspended emulsion, the concentration of polymer microballoon are the 0.01-1 % by weight, and solvent is water, and the concentration of colloidal sol is the 0.005-0.5 % by weight, and solvent is water, and the ratio of both concentration is 2:1;
(2) above-mentioned prepared suspended emulsion is transferred in the Glass Containers, and the substrate of a cleaning vertically is placed in the Glass Containers that above-mentioned suspended emulsion is housed; Then, to warm table, heating makes solvent evaporates the Glass Containers slant setting; Utilize the binary synergistic effect, allow polymer microballoon and colloidal sol grow in substrate in the mode of self-organization, form polymkeric substance;
(3) growth complete after, take out sample, in air and under the suitable temperature condition, heat, make the polymer unwinds volatilization; Sample is taken out in cooling, namely obtains better crystallinity degree, the photonic crystal of zero defect, large-area counter opal structure.
2. preparation method according to claim 1, it is characterized in that: the described polymer microballoon of step (1) is polystyrene microsphere or poly (methyl methacrylate) micro-sphere; The particle size range of described polymer microballoon is: between the 0.05-4um, and volume distributed median CV＜3%.
3. preparation method according to claim 1, it is characterized in that: the described colloidal sol of step (1) is SiO
2Colloidal sol, TiO
2Colloidal sol, AgI colloidal sol etc., sol precursor can be tetraethoxysilane, tetrabutyl titanium etc., but colloidal sol and presoma thereof and not only be confined to above-mentioned several.
4. preparation method according to claim 1 is characterized in that: when step (1) preparation polymer microballoon and colloidal sol (or sol precursor) suspended emulsion, need ultra-sonic dispersion 5-60min, in order to obtain suspended emulsion stable, homogeneous.
5. preparation method according to claim 1 is characterized in that, the described Glass Containers of step (2) is cuvette or beaker.
6. preparation method according to claim 5 is characterized in that, being shaped as of described cuvette is square.
7. preparation method according to claim 1 is characterized in that, the described choice of the substrates glass of step (2), silicon single crystal, quartz, synthetic glass, aluminium foil, Copper Foil.
8. preparation method according to claim 1 is characterized in that, step (2) described the Glass Containers slant setting to warm table, obliquity is between 15-90 °;
The described warm table of step (2), temperature is controlled between 20-80 ℃.
9. preparation method according to claim 1 is characterized in that, heated sample in air and under the suitable temperature condition in the step (3), the temperature range of heating between 300-500 ℃, 6～10 hours heat-up times.
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| CN105113007A (en) * | 2015-09-25 | 2015-12-02 | 哈尔滨工业大学 | Method of utilizing one-step method to quickly prepare high-quality inverse opal structure photonic crystals |
| CN113213488A (en) * | 2021-05-07 | 2021-08-06 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Aptamer inverse opal photonic crystal sensing material and method for rapidly and ultrasensitively detecting staphylococcus aureus enterotoxin B without markers |
| US11534759B2 (en) | 2021-01-22 | 2022-12-27 | Saudi Arabian Oil Company | Microfluidic chip with mixed porosities for reservoir modeling |
| CN115574999A (en) * | 2022-09-23 | 2023-01-06 | 苏州芯聚半导体有限公司 | Stress discoloration detection substrate, preparation method and application |
| US11610509B2 (en) | 2021-01-04 | 2023-03-21 | Saudi Arabian Oil Company | Fabrication of micromodels for carbonate reservoirs |
| US11660595B2 (en) | 2021-01-04 | 2023-05-30 | Saudi Arabian Oil Company | Microfluidic chip with multiple porosity regions for reservoir modeling |
| US11773715B2 (en) | 2020-09-03 | 2023-10-03 | Saudi Arabian Oil Company | Injecting multiple tracer tag fluids into a wellbore |
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| US11534759B2 (en) | 2021-01-22 | 2022-12-27 | Saudi Arabian Oil Company | Microfluidic chip with mixed porosities for reservoir modeling |
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| CN113213488A (en) * | 2021-05-07 | 2021-08-06 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Aptamer inverse opal photonic crystal sensing material and method for rapidly and ultrasensitively detecting staphylococcus aureus enterotoxin B without markers |
| CN115574999A (en) * | 2022-09-23 | 2023-01-06 | 苏州芯聚半导体有限公司 | Stress discoloration detection substrate, preparation method and application |
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