CN102605416A - Preparation method of controllable linear defects in colloidal photonic crystals - Google Patents
Preparation method of controllable linear defects in colloidal photonic crystals Download PDFInfo
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- CN102605416A CN102605416A CN2012100379875A CN201210037987A CN102605416A CN 102605416 A CN102605416 A CN 102605416A CN 2012100379875 A CN2012100379875 A CN 2012100379875A CN 201210037987 A CN201210037987 A CN 201210037987A CN 102605416 A CN102605416 A CN 102605416A
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Abstract
The invention discloses a preparation method of controllable linear defects in colloidal photonic crystals. The method comprises the steps that: a TiO2 nano-rod array is prepared with a controllable distribution density; colloidal-state particles are dispersed in a disperse medium, such that a dispersion liquid is prepared; the TiO2 nano-rod array is placed in a vessel, such that the TiO2 nano-rods are oriented upwards; the dispersion liquid is added into the vessel containing the TiO2 nano-rod array; the vessel is stood, such that the colloidal-state particles are settled freely, and the photonic crystals with controllable linear defects are obtained. With the method, photonic crystals with controllable linear defects are prepared, and the distribution density of the linear defects is controllable. The distribution density of the linear defects in the photonic crystals can be controlled by adjusting the distribution density of the TiO2 nano-rods in the TiO2 nano-rod array. The preparation method provided by the invention is advantaged in simple technology, high efficiency, and low cost.
Description
Technical field
The present invention relates to the assembling technology field of photonic crystal, the preparation method of controlled L&S line defect in particularly a kind of colloidal photon crystal.
Background technology
Photonic crystal is meant the artificial periodic dielectric structure of (PBG) characteristic that has photon band gap.So-called photon band gap is meant that the ripple of a certain range of frequency can not propagate in this periodic structure, there be " forbidden band " in promptly this structure itself.Through specific defective is introduced in the crystalline bandgap structure, can control the photon stream and the various micron order optics of manufacturing of crystals.
Photonic crystal has a lot of particular performances, thereby is widely used in fields such as optics, telecommunications, computingmachine, Chemical Manufacture, drug development and biotechnology, for example can be used as the laser apparatus of no threshold value; Loss-free speculum and crooked light path; The optical microcavity of high-quality-factor, low nonlinear switching and the magnifying glass that drives energy, wavelength resolution is high and ultra prism that volume is minimum; Photonic crystal fiber with dispersion compensation functions, and the efficient of raising photodiode etc.
The photonic crystal that preparation has a L&S line defect in the prior art mainly adopts vacuum plating, laser ablation, electron beam lithography, reactive ion beam etching (RIBE), method such as etching and epitaxy successively.Because complex process, the cost of photonic crystal that apparatus expensive, method for preparing have L&S line defect is very high, is unfavorable for widespread use and popularization.
At present, be starved of the preparation method of controlled L&S line defect in the colloidal photon crystal that a kind of technology is simple and cost is low.
Summary of the invention
The preparation method who the purpose of this invention is to provide controlled L&S line defect in a kind of colloidal photon crystal.
The preparation method of controlled L&S line defect comprises the steps: in the colloidal photon crystal provided by the invention
Distribution density controllably prepares TiO
2Nanometer stick array;
The particles dispersed of colloidal state is prepared dispersion liquid in dispersion medium;
With said TiO
2Nanometer stick array is put into container, makes TiO
2Being oriented straight up of nanometer rod;
Said dispersion liquid joined fill said TiO
2In the said container of nanometer stick array; And
Leave standstill the photonic crystal that said container makes the particle free setting of said colloidal state obtain having controlled L&S line defect.
Preferably, said controllable density ground preparation TiO
2Nanometer stick array further comprises the steps:
1) be 1 in molar ratio with tetra-n-butyl titanate, water and methyl ethyl diketone: (1～1.2): the ratio of (0.3～0.4) is dissolved in the ethanol; Add Vinylpyrrolidone polymer then; Forming titanium concentration is 0.1～0.3mol/L, and Vinylpyrrolidone polymer concentration is the TiO of 30～60mg/L
2Precursor sol;
2) with said TiO
2Precursor sol is spun on the substrate with the speed of 6000～8000rpm under 5～20 ℃, and the spin coating time is 30～40s, on substrate, forms TiO
2Presoma nanometer lattice row dissolved glue film is put into retort furnace with substrate then and is heat-treated at 400～1000 ℃;
3) substrate after the thermal treatment is put into titanate and carry out hydrothermal treatment consists with sour mixed aqueous solution; The concentration of titanate is 0.02～0.05mol/L in the mixed aqueous solution; The concentration of acid is 0.9～3.0mol/L in the mixed aqueous solution; The hydrothermal treatment consists temperature is 80～220 ℃, and the hydrothermal treatment consists time is 0.5～5h, obtains the TiO on substrate
2Nanometer stick array.
Preferably, said titanate is titanous chloride, titanium tetrachloride, titanium sulfate, titanium fluoride or tetra-n-butyl titanate.
Preferably, said acid is hydrochloric acid, nitric acid, sulfuric acid, oleic acid or acetic acid.
Preferably, the material of said substrate comprises FTO conductive glass, ITO, quartz, silicon or metal.
Preferably, said crystal grain comprises SiO
2, ZrO
2, TiO
2, PSt, SiO
2/ Fe
3O
4, PS (PSt)/Fe
3O
4, polymethylmethacrylate (PMMA)/Fe
3O
4And poly (glycidyl methacrylate) (PGMA)/Fe
3O
4In the crystal grain one or more.
Preferably, said particle grain size is 0.1～1.0 μ m.
Preferably, said dispersion medium comprises the arbitrary proportion mixing solutions of zero(ppm) water or ethanol and water, and the particulate mass percent concentration is 0.5～1.5% in the said dispersion liquid.
Preferably, said TiO
2The diameter of nanometer rod is 0.2～1 times of said grain diameter.
The time of preferably, leaving standstill said container was 1～2 week.
The present invention has following beneficial effect:
Said method can prepare the photonic crystal with L&S line defect, and the distribution density of L&S line defect is controlled.Through regulating TiO
2TiO in the nanometer stick array
2The distribution density of nanometer rod is the distribution density of L&S line defect in the may command photonic crystal.Said method preparation technology is simple, and efficient is high, and cost is low.
Embodiment
Below in conjunction with embodiment summary of the invention of the present invention is further described.
Embodiment 1
Preparing method with controlled L&S line defect in PS (PSt) colloidal photon crystal is that example is explained preparation method of the present invention.
In the present embodiment, the preparation method of controlled L&S line defect comprises the steps: in the PSt colloidal photon crystal
Distribution density controllably prepares TiO
2Nanometer stick array;
The PSt particles dispersed of colloidal state prepared in dispersion medium contain PSt particulate dispersion liquid;
With said TiO
2Nanometer stick array is put into container, makes TiO
2Being oriented straight up of nanometer rod;
The said PSt of containing particulate dispersion liquid joined fill said TiO
2In the said container of nanometer stick array; And
Leave standstill the PSt photonic crystal that said container makes the PSt particle free setting of said colloidal state obtain having controlled L&S line defect.
Said controllable density ground preparation TiO
2Nanometer stick array further comprises the steps:
1) be that 1: 1.2: 0.35 ratio is dissolved in the ethanol with tetra-n-butyl titanate, water and methyl ethyl diketone in for example mol ratio, add Vinylpyrrolidone polymer then, forming titanium concentration for example is 0.3mol/L, and Vinylpyrrolidone polymer concentration for example is the TiO of 60mg/L
2Precursor sol;
2) with said TiO
2Precursor sol is for example under 10 ℃, for example is spun on the FTO conducting glass substrate with the speed of for example 7000rpm, and the spin coating time is for example 40s, on said FTO conducting glass substrate, forms TiO
2Presoma nanometer lattice row dissolved glue film, then with said FTO conducting glass substrate put into retort furnace for example 600 ℃ heat-treat;
3) putting into the FTO conducting glass substrate after the thermal treatment for example, the mixed aqueous solution of tetra-n-butyl titanate and hydrochloric acid carries out hydrothermal treatment consists; The concentration of tetra-n-butyl titanate is for example 0.02mol/L in the mixed aqueous solution; The concentration of hydrochloric acid is for example 1.3mol/L in the mixed aqueous solution, and hydrothermal treatment consists is for example being carried out in the water heating kettle, and the hydrothermal treatment consists temperature is for example 140 ℃; The hydrothermal treatment consists time is for example 0.5h, obtains the TiO on the FTO conducting glass substrate
2Nanometer stick array.
The TiO of preparation
2In the nanometer stick array, TiO
2The diameter of nanometer rod is about 83nm, TiO
2The distribution density of nanometer rod is 3.4*10
9Cm
-2In the present embodiment, TiO
2TiO in the nanometer stick array
2The distribution density of nanometer rod is defined as TiO in the substrate unit surface
2The number of nanometer rod.
In the present embodiment, the PSt particle grain size is for example 100nm; Dispersion medium is for example zero(ppm) water; The PSt coating of particles is spherical for for example.Adopt ultra-sonic dispersion to make PSt particle homodisperse in zero(ppm) water.PSt particulate mass percent concentration is for example 1.0% in the said dispersion liquid.
In the present embodiment, leaving standstill said container makes the time of the PSt particle free setting of colloidal state be for example 2 weeks.The PSt photonic crystal for preparing has L&S line defect, and the distribution density of its L&S line defect is 3.4*10
9Cm
-2In the present embodiment, the distribution density of the L&S line defect of photonic crystal is defined as the number perpendicular to L&S line defect in the unit surface of L&S line defect.The distribution density of L&S line defect is by TiO in the PSt photonic crystal
2TiO in the nanometer stick array
2The distribution density decision of nanometer rod, and the distribution density of L&S line defect equals TiO in the PSt photonic crystal
2TiO in the nanometer stick array
2The distribution density of nanometer rod.
Embodiment 2
With SiO
2The preparation method of controlled L&S line defect explains preparation method of the present invention for example in the colloidal photon crystal.
In the present embodiment, SiO
2The preparation method of controlled L&S line defect comprises the steps: in the colloidal photon crystal
Distribution density controllably prepares TiO
2Nanometer stick array;
SiO with colloidal state
2Particles dispersed prepares in dispersion medium and contains SiO
2The particulate dispersion liquid;
With said TiO
2Nanometer stick array is put into container, makes TiO
2Being oriented straight up of nanometer rod;
With the said SiO that contains
2The particulate dispersion liquid joins and fills said TiO
2In the said container of nanometer stick array; And
Leave standstill said container and make the SiO of said colloidal state
2Particle free setting obtains having the SiO of controlled L&S line defect
2Photonic crystal.
Said distribution density controllably prepares TiO
2Nanometer stick array further comprises the steps:
1) be that 1: 1.1: 0.4 ratio is dissolved in the ethanol with tetra-n-butyl titanate, water and methyl ethyl diketone in for example mol ratio, add Vinylpyrrolidone polymer then, forming titanium concentration for example is 0.2mol/L, and Vinylpyrrolidone polymer concentration for example is the TiO of 40mg/L
2Precursor sol;
2) with said TiO
2Precursor sol is for example under 15 ℃, for example is spun on ITO (the Indium Tin Oxides) substrate with the speed of for example 6500rpm, and the spin coating time is for example 30s, on said ito substrate, forms TiO
2Presoma nanometer lattice row dissolved glue film, then with said ito substrate put into retort furnace for example 400 ℃ heat-treat;
3) putting into the ito substrate after the thermal treatment for example, titanium tetrachloride and vitriolic mixed aqueous solution carry out hydrothermal treatment consists; The concentration of titanium tetrachloride is for example 0.02mol/L in the mixed aqueous solution; Vitriolic concentration is for example 0.9mol/L in the mixed aqueous solution, and hydrothermal treatment consists is for example being carried out in the water heating kettle, and the hydrothermal treatment consists temperature is for example 110 ℃; The hydrothermal treatment consists time is for example 1.5h, obtains the TiO on ito substrate
2Nanometer stick array.
The TiO of preparation
2In the nanometer stick array, TiO
2The diameter of nanometer rod is about 42nm, TiO
2The distribution density of nanometer rod is 3.6*10
6Cm
-2In the present embodiment, TiO
2TiO in the nanometer stick array
2The distribution density of nanometer rod is defined as TiO in the substrate unit surface
2The number of nanometer rod.
In the present embodiment, SiO
2Particle grain size is for example 100nm; Dispersion medium is for example zero(ppm) water; SiO
2Coating of particles is spherical for for example.Adopt ultra-sonic dispersion to make SiO
2Particle is homodisperse in zero(ppm) water.SiO in the said dispersion liquid
2The particulate mass percent concentration is for example 1.5%.
In the present embodiment, leave standstill the SiO that said container makes colloidal state
2The time of particle free setting is for example 1.5 weeks.The SiO for preparing
2Photonic crystal has L&S line defect, and the distribution density of its L&S line defect is 3.6*10
6Cm
-2In the present embodiment, the distribution density of the L&S line defect of photonic crystal is defined as the number perpendicular to L&S line defect in the unit surface of L&S line defect.SiO
2The distribution density of L&S line defect is by TiO in the photonic crystal
2TiO in the nanometer stick array
2The distribution density decision of nanometer rod, and SiO
2The distribution density of L&S line defect equals TiO in the photonic crystal
2TiO in the nanometer stick array
2The distribution density of nanometer rod.
Embodiment 3
With SiO
2/ Fe
3O
4The preparation method of controlled L&S line defect explains preparation method of the present invention for example in the colloidal photon crystal.
In the present embodiment, SiO
2/ Fe
3O
4The preparation method of controlled L&S line defect comprises the steps: in the colloidal photon crystal
Distribution density controllably prepares TiO
2Nanometer stick array;
SiO with colloidal state
2/ Fe
3O
4Composite material granular is dispersed in to prepare in the dispersion medium and contains SiO
2/ Fe
3O
4The particulate dispersion liquid;
With said TiO
2Nanometer stick array is put into container, makes TiO
2Being oriented straight up of nanometer rod;
With the said SiO that contains
2/ Fe
3O
4The particulate dispersion liquid joins and fills said TiO
2In the said container of nanometer stick array; And
Leave standstill said container and make the SiO of said colloidal state
2/ Fe
3O
4Particle free setting obtains having the SiO of controlled L&S line defect
2/ Fe
3O
4Photonic crystal.
Said distribution density controllably prepares TiO
2Nanometer stick array further comprises the steps:
1) be that 1: 1: 0.35 ratio is dissolved in the ethanol with tetra-n-butyl titanate, water and methyl ethyl diketone in for example mol ratio, add Vinylpyrrolidone polymer then, forming titanium concentration for example is 0.3mol/L, and Vinylpyrrolidone polymer concentration for example is the TiO of 40mg/L
2Precursor sol;
2) with said TiO
2Precursor sol is for example under 5 ℃, for example is spun on the metal substrate with the speed of for example 8000rpm, and the spin coating time is for example 30s, on said silicon substrate, forms TiO
2Presoma nanometer lattice row dissolved glue film, then with said metal substrate put into retort furnace for example 1000 ℃ heat-treat;
3) putting into the metal substrate after the thermal treatment for example, the mixed aqueous solution of titanous chloride and hydrochloric acid carries out hydrothermal treatment consists; The concentration of titanous chloride is for example 0.05mol/L in the mixed aqueous solution; The concentration of hydrochloric acid is for example 3mol/L in the mixed aqueous solution, and hydrothermal treatment consists is for example being carried out in the water heating kettle, and the hydrothermal treatment consists temperature is for example 220 ℃; The hydrothermal treatment consists time is for example 1h, obtains the TiO on metal substrate
2Nanometer stick array.
The TiO of preparation
2In the nanometer stick array, TiO
2The diameter of nanometer rod is about 200nm, TiO
2The distribution density of nanometer rod is 8.3*10
13Cm
-2In the present embodiment, TiO
2TiO in the nanometer stick array
2The distribution density of nanometer rod is defined as TiO in the substrate unit surface
2The number of nanometer rod.
In the present embodiment, SiO
2/ Fe
3O
4Particle grain size is for example 1.0 μ m; Dispersion medium is the arbitrary proportion mixing solutions of ethanol and water for example; SiO
2/ Fe
3O
4Coating of particles is spherical for for example.Adopt ultra-sonic dispersion to make SiO
2/ Fe
3O
4Particle is homodisperse in dispersion medium.SiO in the said dispersion liquid
2/ Fe
3O
4The particulate mass percent concentration is for example 0.5%.
In the present embodiment, leave standstill the SiO that said container makes colloidal state
2/ Fe
3O
4The time of particle free setting is for example 1.5 weeks.The SiO for preparing
2/ Fe
3O
4Photonic crystal has L&S line defect, and the distribution density of its L&S line defect is 8.3*10
13Cm
-2In the present embodiment, the distribution density of the L&S line defect of photonic crystal is defined as the number perpendicular to L&S line defect in the unit surface of L&S line defect.SiO
2/ Fe
3O
4The distribution density of L&S line defect is by TiO in the photonic crystal
2TiO in the nanometer stick array
2The distribution density decision of nanometer rod, and SiO
2/ Fe
3O
4The distribution density of L&S line defect equals TiO in the photonic crystal
2TiO in the nanometer stick array
2The distribution density of nanometer rod.
Should be appreciated that the above detailed description of technical scheme of the present invention being carried out by preferred embodiment is schematic and nonrestrictive.Those of ordinary skill in the art is reading on the basis of specification sheets of the present invention and can make amendment to the technical scheme that each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement; And these are revised or replacement, do not make the spirit and the scope of the essence disengaging various embodiments of the present invention technical scheme of relevant art scheme.
Claims (10)
1. the preparation method of controlled L&S line defect in the colloidal photon crystal is characterized in that, this method comprises the steps:
Distribution density controllably prepares TiO
2Nanometer stick array;
The particles dispersed of colloidal state is prepared dispersion liquid in dispersion medium;
With said TiO
2Nanometer stick array is put into container, makes TiO
2Being oriented straight up of nanometer rod;
Said dispersion liquid joined fill said TiO
2In the said container of nanometer stick array; And
Leave standstill the photonic crystal that said container makes the particle free setting of said colloidal state obtain having controlled L&S line defect.
2. the preparation method of controlled L&S line defect is characterized in that in the colloidal photon crystal as claimed in claim 1, said controllable density ground preparation TiO
2Nanometer stick array further comprises the steps:
1) be 1 in molar ratio with tetra-n-butyl titanate, water and methyl ethyl diketone: (1～1.2): the ratio of (0.3～0.4) is dissolved in the ethanol; Add Vinylpyrrolidone polymer then; Forming titanium concentration is 0.1～0.3mol/L, and Vinylpyrrolidone polymer concentration is the TiO of 30～60mg/L
2Precursor sol;
2) with said TiO
2Precursor sol is spun on the substrate with the speed of 6000～8000rpm under 5～20 ℃, and the spin coating time is 30～40s, on substrate, forms TiO
2Presoma nanometer lattice row dissolved glue film is put into retort furnace with substrate then and is heat-treated at 400～1000 ℃;
3) substrate after the thermal treatment is put into titanate and carry out hydrothermal treatment consists with sour mixed aqueous solution; The concentration of titanate is 0.02～0.05mol/L in the mixed aqueous solution; The concentration of acid is 0.9～3.0mol/L in the mixed aqueous solution; The hydrothermal treatment consists temperature is 80～220 ℃, and the hydrothermal treatment consists time is 0.5～5h, obtains the TiO on substrate
2Nanometer stick array.
3. the preparation method of controlled L&S line defect is characterized in that in the colloidal photon crystal as claimed in claim 2, and said titanate is titanous chloride, titanium tetrachloride, titanium sulfate, titanium fluoride or tetra-n-butyl titanate.
4. the preparation method of controlled L&S line defect is characterized in that in the colloidal photon crystal as claimed in claim 2, and said acid is hydrochloric acid, nitric acid, sulfuric acid, oleic acid or acetic acid.
5. the preparation method of controlled L&S line defect is characterized in that in the colloidal photon crystal as claimed in claim 2, and the material of said substrate comprises FTO conductive glass, ITO, quartz, silicon or metal.
6. the preparation method of controlled L&S line defect is characterized in that in the colloidal photon crystal as claimed in claim 1, and said crystal grain comprises SiO
2, ZrO
2, TiO
2, PSt, SiO
2/ Fe
3O
4, PSt/Fe
3O
4, PMMA/Fe
3O
4And PGMA/Fe
3O
4In the crystal grain one or more.
7. the preparation method of controlled L&S line defect is characterized in that in the colloidal photon crystal as claimed in claim 1, and the particle diameter of said crystal grain is 0.1～1 μ m.
8. the preparation method of controlled L&S line defect in the colloidal photon crystal as claimed in claim 1; It is characterized in that; Said dispersion medium comprises the arbitrary proportion mixing solutions of zero(ppm) water or ethanol and water, and the particulate mass percent concentration is 0.5～1.5% in the said dispersion liquid.
9. the preparation method of controlled L&S line defect is characterized in that in the colloidal photon crystal as claimed in claim 1, said TiO
2The diameter of nanometer rod is 0.2～1 times of said grain diameter.
10. the preparation method of controlled L&S line defect is characterized in that in the colloidal photon crystal as claimed in claim 1, and the time of leaving standstill said container was 1～2 week.
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Cited By (1)
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| CN108341600A (en) * | 2018-03-14 | 2018-07-31 | 江苏大学 | One kind preparing single layer SiO in glass surface2The method of microballoon film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108341600A (en) * | 2018-03-14 | 2018-07-31 | 江苏大学 | One kind preparing single layer SiO in glass surface2The method of microballoon film |
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