CN102116899A - Alpha-Fe2O3/Si porous photonic crystal and preparation method and application thereof - Google Patents

Alpha-Fe2O3/Si porous photonic crystal and preparation method and application thereof Download PDF

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CN102116899A
CN102116899A CN 201110051175 CN201110051175A CN102116899A CN 102116899 A CN102116899 A CN 102116899A CN 201110051175 CN201110051175 CN 201110051175 CN 201110051175 A CN201110051175 A CN 201110051175A CN 102116899 A CN102116899 A CN 102116899A
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photonic crystal
porous photonic
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porous
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张正犁
郁可
尹海宏
娄蕾
朱自强
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East China Normal University
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Abstract

The invention provides an alpha-Fe2O3/Si porous photonic crystal comprising an alpha-Fe2O3/Si material and a Si substrate, wherein the alpha-Fe2O3/Si material is periodically arranged on the Si substrate in a hexagonal lattice point way. The invention also provides a preparation method of the alpha-Fe2O3/Si porous photonic crystal, and application of the alpha-Fe2O3/Si porous photonic crystal in optical diffraction. In the invention, two-dimensional photonic crystals are constructed through selecting proper materials to adjust dielectric constants, so that the cost is low and the preparation is rapid and safe.

Description

A kind of α-Fe＜sub〉2＜/sub〉O＜sub〉3＜/sub 〉/the poroid photonic crystal of Si and its production and application
Technical field
The invention belongs to photoelectron material, semiconductor materials and devices technical field, be specifically related to a kind of α-Fe 2O 3/ Si porous photonic crystal and its preparation method and application.
Background technology
Therefore the two-dimensional and periodic nanostructured strengthens aspects such as (SERS) at catalysis, sensing, photonic crystal, battery technology, Raman spectrum in recent years and has caused very big concern owing to have large-area periodic material arrangement and the general bigger surface area of material.In recent years, people utilize the whole bag of tricks, and for example photoetching, little contact, self assembly etc. have prepared multiple two-dimensional periodic structure.Yet in these methods, photoetching is faced with the diffracted error problem of optical system, causes end product quality not high, and its preparation process efficient is low, the cost height, and can only carry out photoetching to specific material, limited its widespread use; And little contact method is owing to need preparation template earlier, and then duplicates by physical method and to obtain final needed material, sometimes needs three even more step, so have deviation unavoidably in this process.And the cost of self-assembly method is low, and the selection of end product is also more extensive, can cover various metals and semiconductor, therefore more and more is subjected to researcher's favor.In addition, in the material of these preparations, great majority research is all paid close attention to it in above-mentioned application aspect various such as sensing, catalysis, the concern optical property is seldom arranged, especially the application of optical diffraction character.In fact, according to previous research, the propagation of light in photonic crystal and the propagation in generic media have a great difference, and for example there is photonic band gap in photonic crystal, can stop the photon of component frequency to pass through; Photonic crystal can also change the direction of propagation of light by defective.Therefore, the optical diffraction performance of photonic crystal is also different with generic media, the report to this is also arranged before, but all deeply do not study.
The defective such as the present invention has overcome high expensive of the prior art, preparation process is complicated and kind wayward, product is limited provides a kind of α-Fe 2O 3/ Si porous photonic crystal and preparation method thereof has that cost is low, preparation process is simply controlled, the wide beneficial effect of kind scope of product.α-Fe of the present invention 2O 3/ Si porous photonic crystal is by α-Fe 2O 3α-Fe that material hexagon periodic arrangement forms at the Si substrate 2O 3/ Si composite construction has adopted the method for self assembly and solution titration in its preparation, at atmospheric pressure with do not have under the condition of catalyst, obtains this structure of large tracts of land in silicon chip substrate.α-Fe of the present invention 2O 3/ Si porous photonic crystal can be used in actual optical diffraction, and it has the diffraction property different from common grating.。The present invention adjusts dielectric constant by selecting appropriate material, thus the structure 2 D photon crystal its optical property is studied, with further promotion its in the application aspect the optics.
Summary of the invention
The invention provides a kind of α-Fe 2O 3/ Si porous photonic crystal is characterized in that, comprises α-Fe 2O 3Material and Si substrate; Wherein, described α-Fe 2O 3Material is hexagon lattice point periodic arrangement on described Si substrate, described α-Fe 2O 3The aperture of material is 200 nm –, 800 nm, and its thickness is 100-200nm, described α-Fe 2O 3Material covers the 25-35% of the described Si substrate gross area.
The present invention also provides a kind of described α-Fe 2O 3The preparation method of/Si porous photonic crystal is characterized in that, may further comprise the steps successively:
A) with the ultrasonic cleaning of described Si substrate, then 500-550 ℃ of heating down;
B) get the PS mono-dispersion microballoon and drip on described Si substrate, it is statically placed in the air, be self-assembled into up to described PS mono-dispersion microballoon and be the periodic template of sexangle;
C) with 10-20 μ L Fe (NO 3) 3Solution drips in step b) on the template that assembles;
D) after 110 ℃ of lower oven dry, the PS mono-dispersion microballoon is removed at high temperature heating again, obtains described α-Fe 2O 3/ Si porous photonic crystal.
α-Fe of the present invention 2O 3The preparation method of/Si porous photonic crystal is characterized in that, described steps d) in high-temperature heating be under 450-550 ℃, to carry out.
α-Fe of the present invention 2O 3The preparation method of/Si porous photonic crystal, it is further characterized in that, with the resulting α-Fe of step d) 2O 3/ Si porous photonic crystal cleans in ultrasonic.
The invention provides a kind of described α-Fe 2O 3The application of/Si porous photonic crystal in optical diffraction is characterized in that, with the light wave of a branch of focusing along perpendicular to described α-Fe 2O 3The direction on/Si porous photonic crystal plane is incident to its surface, and the pattern of diffraction is hexagon; Distance between the point diffraction of light wave arrives described α-Fe with optical screen 2O 3Ratio of distances constant value between the/Si porous photonic crystal is directly proportional with described optical wavelength, with described α-Fe 2O 3The periodicity size of/Si porous photonic crystal is inversely proportional to.
The invention provides a kind of α-Fe 2O 3/ Si porous photonic crystal and preparation method thereof.Periodic α-Fe provided by the present invention 2O 3/ Si porous photonic crystal structure is reported first in the world, and this photonic crystal is by α-Fe 2O 3Alternately form with the Si bi-material, wherein α-Fe 2O 3Material is hexagon lattice point periodic arrangement, and generally in about 200 nm –, 800 nm scopes, thickness is about 100-200 nm to pore size, and the area that covers the Si substrate accounts for greatly the 25%-35% of the gross area.
α-Fe of the present invention 2O 3The preparation method of/Si porous photonic crystal may further comprise the steps:
1. with silicon substrate ultrasonic cleaning 30 minutes, heated 2 hours down at 500-550 ℃ then, to reach the effect that improves surface hydrophilicity.
2. with the certain density PS(polystyrene of preprepared) mono-dispersion microballoon (diameter can be controlled on demand) takes a morsel and drips on substrate, place air a period of time substrate is static, avoid all disturbances, the PS microballoon will automatically be self-assembled into along with the evaporation of moisture and be the periodic template of sexangle.
3. with the Fe (NO about 10-20 μ L 3) 3Solution drips on the template that has assembled with liquid-transfering gun, because the effect of capillary force, solution will infiltrate in the space between the PS microballoon.Because the density of PS microballoon is less than Fe (NO 3) 3Solution, the PS template will float on the solution.
4. 110 ℃ of lower oven dry 2 hours, make Fe (NO 3) 3Moisture evaporation in the solution.
5. 450-550 ℃ of lower heating 3 hours, make Fe (NO 3) 3Precursor liquid changes solid-state α-Fe into 2O 3, the PS microballoon by burning-off, forms the poroid nanostructured of periodicity that needs under this high temperature simultaneously.Finally in ultrasonic, clean 30 min, obtain α-Fe of the present invention 2O 3/ Si porous photonic crystal, α-Fe 2O 3Be rendered as one deck bronzing material at the Si sheet.
The present invention has synthesized periodic α-Fe by the control to some parameters in self-assembly method and the solution titration 2O 3/ Si porous photonic crystal.
With respect to the synthetic similar photon crystal structure of former report, outstanding feature of the present invention is: (1) growing method cost is low, and preparation is quick, safety, and is low for equipment requirements; (2) adopt α-Fe 2O 3With the photonic crystal that the Si bi-material replaces, consist of weak modulation; (3) growth course does not need extra atmosphere and pressure etc., and is nontoxic, good reproducibility, and the growth area is bigger.
α-Fe of the present invention 2O 3The concrete application process of/Si porous photonic crystal is as follows:
With the light wave of a branch of focusing along perpendicular to α-Fe of the present invention 2O 3The direction on/Si porous photonic crystal plane is incident to its surface, and the pattern of diffraction is hexagon.Distance between the point diffraction of light wave arrives α-Fe with optical screen 2O 3Distance between the/Si porous photonic crystal is directly proportional.Distance between the point diffraction of light wave arrives described α-Fe with optical screen 2O 3Ratio of distances constant value between the/Si porous photonic crystal and optical wavelength become consistent variation tendency, with α-Fe 2O 3The periodicity size of/Si porous photonic crystal becomes opposite variation tendency.
Description of drawings
Fig. 1 is α-Fe of the present invention 2O 3The structural representation of/Si porous photonic crystal.
Fig. 2 is α-Fe of the present invention 2O 3The preparation process schematic diagram of/Si porous photonic crystal; Wherein, (a) expression self assembly; (b) after the expression titration; (c) after the expression oven dry; (d) expression obtains α-Fe of the present invention through high-temperature baking and after cleaning 2O 3/ Si porous photonic crystal.
Fig. 3 is α-Fe of the present invention 2O 3The X-ray diffractogram of/Si porous photonic crystal.
Fig. 4 is α-Fe of the present invention 2O 3The SEM photo of/Si porous photonic crystal when diameter is 800 nm, illustration is α-Fe 2O 3The AFM photo of/Si porous photonic crystal multiplication factor.
Embodiment
In conjunction with following specific embodiments and the drawings, the present invention is described in further detail, and protection content of the present invention is not limited to following examples.Under the spirit and scope that do not deviate from inventive concept, variation and advantage that those skilled in the art can expect all are included among the present invention, and are protection domain with the appending claims.
As shown in Figure 1, α-Fe of the present invention 2O 3The structure of/Si porous photonic crystal is α-Fe from top to down successively 2O 3Material and Si substrate; Wherein, α-Fe 2O 3Material is hexagon lattice point periodic arrangement on the Si substrate, α-Fe 2O 3The aperture of material is 470 nm, and its thickness is about 200nm, α-Fe 2O 3Material covers 30% of the Si substrate gross area.
Among the present invention, α-Fe 2O 3The aperture of material can be 200 nm –, 800 nm, and its thickness can be about 100-200nm, α-Fe 2O 3Material can cover the 25-35% of the Si substrate gross area.
As shown in Figure 2,1 expression PS mono-dispersion microballoon, 2 expression Si substrates, 3 expression Fe (NO 3) 3Solution, 4 expression Fe 2O 3
Embodiment 1: α-Fe 2O 3The preparation of/Si porous photonic crystal
1. with silicon substrate ultrasonic cleaning 30 minutes, heated 2 hours down at 500-550 ℃ then, to reach the effect that improves surface hydrophilicity; Among Fig. 2 (a) 2 expression Si substrate.
2. the PS mono-dispersion microballoon that with preprepared 10 μ L, 10% massfraction, diameter is 470 nm drips on substrate, places one time of air substrate is static, avoids all disturbances.Can be observed the PS microballoon and will automatically be self-assembled into along with the evaporation of moisture and be the periodic template of sexangle, the water evaporates process is the self assembly of PS microballoon and finishes substantially when finishing.The xsect of the arrangement mode of PS microballoon is shown in (a) among Fig. 2, and wherein 1 represents the PS mono-dispersion microballoon.
3. with the Fe (NO about 10-20 μ L 3) 3Solution drips on the template that has assembled with liquid-transfering gun, because the effect of capillary force, solution will infiltrate in the space between the PS microballoon, shown in (b) among Fig. 2; Because the density of PS microballoon is less than Fe (NO 3) 3Solution, the PS template will float on Fe (NO 3) 3On the solution, the expression of 3 among figure Fe (NO 3) 3Solution.
4. 110 ℃ of lower oven dry 2 hours, make Fe (NO 3) 3Moisture evaporation in the solution is shown in (c) among Fig. 2.
5. 450-550 ℃ of lower heating 3 hours, make Fe (NO 3) 3Precursor liquid changes solid-state α-Fe into 2O 3, the PS microballoon by burning-off, forms the poroid nanostructured of periodicity that needs under this high temperature simultaneously.In ultrasonic, clean 30 min, finally obtain α-Fe of the present invention 2O 3/ Si porous photonic crystal, 4 expression α-Fe shown in (d) among Fig. 2 2O 3, it is rendered as one deck bronzing material at the Si sheet.
Embodiment 2: α-Fe 2O 3The diffraction application of/Si porous photonic crystal
α-Fe of the present invention 2O 3The preparation method of/Si porous photonic crystal, take polystyrene (PS) bead as template, take Si as substrate, Fe (NO 3) 3Solution is precursor liquid, adopts solution titration growth α-Fe 2O 3Poroid periodic nano-structure.Utilize the α-Fe of this method growth 2O 3Poroid periodic nano-structure is made up of the circular nano-pore of hexagonal array, and its XRD schemes as shown in Figure 3, and low power SEM and high power AFM figure are as shown in Figure 4.As can be seen from Fig. 3, the position of diffraction maximum and α-Fe 2O 3The XRD standard card on the peak corresponding, confirm that product is α-Fe really 2O 3As can be seen from Fig. 4, the nano-pore diameter is between 200-800 nm, and the hole wall height is 200 nm, and the area of hole wall part (color is than shallow portion among Fig. 4) covering Si substrate (color is than the deep branch among Fig. 4) accounts for greatly the 25-35% of the gross area.Can be found out that by SEM figure they are arranged closely, neat zero defect has good periodicity, can find out from AFM figure, and the edge of circular hole is the positive circle of rule.The present invention can be implemented on the silicon substrate large tracts of land and periodically grows, and the material of generation is good stability at normal temperatures, and is high temperature resistant, anti-oxidant.This α-Fe 2O 3Material and Si substrate just consist of a kind of photonic crystal, can be calculated through theory, and it has special optical diffraction performance, the research of periodicity material is had huge value, and having broad application prospects aspect the display device of new generation.
With α-Fe of the present invention 2O 3When/Si porous photonic crystal carries out actual optics diffraction application, with the light wave of a branch of focusing along perpendicular to α-Fe of the present invention 2O 3The direction on/Si porous photonic crystal plane is incident to its surface, and the pattern of diffraction is hexagon.Distance between the point diffraction of light wave arrives α-Fe with optical screen 2O 3Ratio of distances constant value between the/Si porous photonic crystal is directly proportional with optical wavelength, and both are consistent variation tendency; Distance between the point diffraction of light wave arrives α-Fe with optical screen 2O 3Ratio of distances constant value and α-Fe between/the Si porous photonic crystal 2O 3The periodicity size of/Si porous photonic crystal is inversely proportional to, and both are opposite variation tendency.
In the present embodiment, the α-Fe of the present invention that adopts crystal periodicity a to vary in size 2O 3/ Si porous photonic crystal under the light wave of Different lightwave wavelength X, has carried out respectively three groups of diffraction experiments.With light wave along perpendicular to α-Fe 2O 3The direction on/Si porous photonic crystal plane is incident to its surface, and the pattern of diffraction is hexagon.Present embodiment obtains α-Fe 2O 3Between the periodicity of/Si porous photonic crystal size a, optical wavelength λ, the point diffraction apart from r and optical screen between the photonic crystal apart from the numerical relation between ratio (r/d) three of d, as shown in table 1 below:
Table 1
Figure 844185DEST_PATH_IMAGE001
According to table 1, compare the 1st, 2 group of experimental result as seen, as α-Fe 2O 3When the periodicity of/Si porous photonic crystal size a was 780nm, λ reduced along with optical wavelength, between the point diffraction apart from r and optical screen to being the consistent trend that reduces apart from the ratio r/d of d and optical wavelength λ between the photonic crystal; Relatively the 2nd, 3 group of experimental result as seen, when optical wavelength λ is identical when being 400nm, along with α-Fe 2O 3The periodicity of/Si porous photonic crystal size a reduces, and is opposite increase tendency apart from r and optical screen to the ratio r/d apart from d between the photonic crystal between the point diffraction.

Claims (5)

1. α-Fe 2O 3/ Si porous photonic crystal is characterized in that, comprises α-Fe 2O 3Material and Si substrate; Wherein, described α-Fe 2O 3Material is hexagon lattice point periodic arrangement on described Si substrate, described α-Fe 2O 3The aperture of material is 200 nm –, 800 nm, and its thickness is 100-200nm, described α-Fe 2O 3Material covers the 25-35% of the described Si substrate gross area.
2. α-Fe as claimed in claim 1 2O 3The preparation method of/Si porous photonic crystal is characterized in that, may further comprise the steps successively:
A) with the ultrasonic cleaning of described Si substrate, then 500-550 ℃ of heating down;
B) get the PS mono-dispersion microballoon and drip on described Si substrate, it is statically placed in the air, be self-assembled into up to described PS mono-dispersion microballoon and be the periodic template of sexangle;
C) with 10-20 μ L Fe (NO 3) 3Solution drips in step b) on the template that assembles;
D) after 110 ℃ of lower oven dry, the PS mono-dispersion microballoon is removed at high temperature heating again, obtains described α-Fe 2O 3/ Si porous photonic crystal.
3. α-Fe as claimed in claim 2 2O 3The preparation method of/Si porous photonic crystal is characterized in that, described steps d) in high-temperature heating be under 450-550 ℃, to carry out.
4. α-Fe as claimed in claim 2 2O 3The preparation method of/Si porous photonic crystal, it is further characterized in that, with the resulting α-Fe of step d) 2O 3/ Si porous photonic crystal carries out ultrasonic cleaning.
5. α-Fe as claimed in claim 1 2O 3The application of/Si porous photonic crystal in optical diffraction is characterized in that, with the light wave of a branch of focusing along perpendicular to described α-Fe 2O 3The direction on/Si porous photonic crystal plane is incident to its surface, and the pattern of diffraction is hexagon; Distance between the point diffraction of light wave arrives described α-Fe with optical screen 2O 3Ratio of distances constant value between the/Si porous photonic crystal is directly proportional with described optical wavelength, with described α-Fe 2O 3The periodicity size of/Si porous photonic crystal is inversely proportional to.
CN 201110051175 2011-03-03 2011-03-03 Alpha-Fe2O3/Si porous photonic crystal and preparation method and application thereof Pending CN102116899A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106298450A (en) * 2016-08-10 2017-01-04 华东师范大学 A kind of nano patterned Sapphire Substrate and its preparation method and application
CN109655971A (en) * 2018-11-14 2019-04-19 华南师范大学 A method of micro-nano structure is prepared on planar optical waveguide surface

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101570891A (en) * 2009-06-09 2009-11-04 华东师范大学 Alpha-Fe2O3 bowl-shaped photon crystal structure and preparation method thereof
CN101570892A (en) * 2009-06-09 2009-11-04 华东师范大学 Au-ZnO two-dimensional photon crystal structure and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101570891A (en) * 2009-06-09 2009-11-04 华东师范大学 Alpha-Fe2O3 bowl-shaped photon crystal structure and preparation method thereof
CN101570892A (en) * 2009-06-09 2009-11-04 华东师范大学 Au-ZnO two-dimensional photon crystal structure and preparation method thereof

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《华东师范大学学报（自然科学版）》 20100930 吴玮 等 基于聚苯乙烯模板的二维光子晶体的制备 , 第5期 2 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106298450A (en) * 2016-08-10 2017-01-04 华东师范大学 A kind of nano patterned Sapphire Substrate and its preparation method and application
CN106298450B (en) * 2016-08-10 2019-04-30 华东师范大学 A kind of nano patterned Sapphire Substrate and its preparation method and application
CN109655971A (en) * 2018-11-14 2019-04-19 华南师范大学 A method of micro-nano structure is prepared on planar optical waveguide surface

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Application publication date: 20110706