CN103896627B - Preparation method of one-dimensional photonic crystal thin film based on nano multilayer hollow capsule - Google Patents

Preparation method of one-dimensional photonic crystal thin film based on nano multilayer hollow capsule Download PDF

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CN103896627B
CN103896627B CN201410073201.4A CN201410073201A CN103896627B CN 103896627 B CN103896627 B CN 103896627B CN 201410073201 A CN201410073201 A CN 201410073201A CN 103896627 B CN103896627 B CN 103896627B
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solution
multilayer hollow
photonic crystal
dimensional photonic
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CN103896627A (en
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葛丽芹
任姣雨
姚翀
朱彦熙
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Southeast University
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Abstract

The invention discloses a preparation method of a one-dimensional photonic crystal thin film based on a nano multilayer hollow capsule. A SiO2 nano multilayer hollow capsule is taken as a substrate, a spinning technology is combined, and TiO2 and GO are assembled to the surface of the SiO2 nano multilayer hollow capsule, so that the one-dimensional photonic crystal thin film is obtained. According to the preparation method of the one-dimensional photonic crystal thin film based on the nano multilayer hollow capsule, the nano multilayer hollow capsule prepared by adopting a layer-by-layer self-assembly method is taken as the substrate, a photonic band gap can shift by high amplitude by changing the shape of the hollow capsule, so that sensitivity of one-dimensional photonic crystal detection can be improved, and the prepared one-dimensional photonic crystal thin film based on the nano multilayer hollow capsule is more sensitive than a common one-dimensional photonic crystal thin film. The preparation method of the one-dimensional photonic crystal thin film based on the nano multilayer hollow capsule is simple and efficient, operation is easy, and time needed is short.

Description

A kind of preparation method based on nanometer multilayer hollow capsules one-dimensional photonic crystal film
Technical field
The present invention relates to photonic crystal preparing technical field, be specifically related to a kind of preparation method based on nanometer multilayer hollow capsules one-dimensional photonic crystal film.
Background technology
Photonic crystal is the novel dielectric structure material that a kind of specific refractory power changes in space periodicity, the i.e. periodic arrangement of a kind of dielectric medium in another dielectric medium, forms the periodic modulation of dielectric constant, also referred to as photonic bandgap material.Wherein, 1-D photon crystal is the simplest photonic crystal.1-D photon crystal is formed by two or more dielectric material alternative stacked, perpendicular on the direction of medium layer, specific inductivity is periodic function, and on the direction being parallel to medium layer plane, specific inductivity remains unchanged, and it forms photonic band gap structure in one direction.1-D photon crystal because of its prepare that material is various, method is simple, with low cost, and there is excellent optical property, high mechanical strength, high stability, porousness, easily introduce defect layer, to ambiance, pH, different guest molecules, there is sensitive optic response, and possess the advantage such as character of two dimension, three-D photon crystal simultaneously, there is higher researching value and application prospect widely.
Hollow capsules is the important kind of nano-functional material, and its research and preparation have attracted numerous scholar.Its special property shown, as low density, high-specific surface area, fabulous stability and Surface Permeability etc. make it be widely used in the fields such as filler, matrix material, dyestuff, makeup and photonic crystal.Some macroporous inorganic hollow capsules are also applied in catalysis, isolation technique, medicine, sustained release dosage etc.The method preparing hollow capsules has seeded polymerization, macromonomer method and LBL self-assembly method.
LBL self-assembly method is referred to as LBL method.Early 1990s, polyelectrolyte is used for coated colloidal particle by Cuarso etc., utilizes electrostatic interaction and steric effect to strengthen its stability, and becomes the macromolecule layer outer cladding technology of complete set.First at colloidal particle surface electrostatic self-assembly one deck polyelectrolyte, be then placed in and the polyelectrolyte solution of its surface with opposite charges, utilize electrostatic attraction between xenogenesis electric charge to produce motivating force, make polyelectrolyte be adsorbed onto colloidal particle surface.Particle after coated can repeat aforesaid method and carry out repeatedly coated after eccentric cleaning, to obtain desirable hollow capsules material.
One-dimensional photonic crystal film is that guest molecule changes the specific refractory power or layer thickness that form 1-D photon crystal material for detecting the principle of guest molecule, thus causing the movement of 1-D photon crystal forbidden photon band, external manifestation is exactly the change of 1-D photon crystal schemochrome.But the one-dimensional photonic crystal film of preparation forbidden photon band when detecting moves less or not mobile.Therefore, existing one-dimensional photonic crystal film detection sensitivity need to improve.
Summary of the invention
The object of this invention is to provide a kind of preparation method based on nanometer multilayer hollow capsules one-dimensional photonic crystal film, solve the defect that in prior art, one-dimensional photonic crystal film detection sensitivity has much room for improvement.
For solving the problem, the present invention by the following technical solutions:
Based on a preparation method for nanometer multilayer hollow capsules one-dimensional photonic crystal film, with SiO 2nanometer multilayer hollow capsules is substrate, comprises the steps:
Step one, utilize LBL self-assembly legal system for SiO 2nanometer multilayer hollow capsules;
Step 2, silicon chip are cleaned and are dried up, and utilize the SiO that step one is prepared by spin-coating method 2nanometer multilayer hollow capsules is fixed on silicon chip surface, obtains the substrate of one-dimensional photonic crystal film, and wherein, spin coating rotating speed is 3000 ~ 6000rpm, and spin-coating time is 30s ~ 1min;
Step 3, prepare TiO respectively 2colloidal solution and graphene oxide (GO) colloidal solution, wherein, TiO 2colloidal solution concentration is 7.8 ~ 39mg/ml, GO colloidal solution concentration is 0.1 ~ 0.5mg/ml;
Step 4, the TiO utilizing spin-coating method successively step 3 to be prepared 2colloidal solution and GO colloidal solution are coated onto substrate surface prepared by step 2, obtain described based on SiO 2nanometer multilayer hollow capsules one-dimensional photonic crystal film, wherein, every layer of spin coating rotating speed is 3000 ~ 6000rpm, and spin-coating time is 30s ~ 1min.
Described LBL self-assembly legal system is for SiO 2nanometer multilayer hollow capsules comprises the steps:
Step one, be solvent with water, configure polyallylamine hydrochlorides (PAH) solution and sodium polystyrene sulfonate (PSS) solution respectively, wherein, PAH strength of solution is 1 ~ 3mg/ml, PSS strength of solution is 1 ~ 3mg/ml;
Step 2, be the SiO of 100 ~ 500nm by 1 ~ 3ml diameter 2particle washing, repeatedly centrifugal, obtain clean SiO 2for template;
Step 3, the SiO that step 2 is obtained 2be immersed in 5 ~ 10min in PAH solution, the centrifugal 2 ~ 5min of 1000 ~ 1500rpm, is immersed in 5 ~ 10min in PSS solution afterwards again, the centrifugal 2 ~ 5min of 1000 ~ 1500rpm; Repeat PAH solution soaking, centrifugal, PSS solution soaking, centrifugal 4 ~ 5 times, obtain SiO 2/ (PAH/PSS) 4 ~ 5; Afterwards by SiO 2/ (PAH/PSS) 4 ~ 5being immersed in volume fraction is the centrifugal 2 ~ 3min of 5 ~ 10min in 4% ~ 5%HF solution, 7000 ~ 8000rpm; Repeat HF solution soaking, centrifugal 4 ~ 5 times to wash away SiO 2, obtain described SiO 2nanometer multilayer hollow capsules.
Described silicon chip is cleaned to dry up and is comprised the steps: silicon chip to be immersed acetone soln sonic oscillation 30 ~ 60min that volume percent is 90% ~ 100%, and immersing volume percent afterwards is again sonic oscillation 30 ~ 60min in the ethanolic soln of 90% ~ 100%; Finally immersing volume ratio is the H of 3:7 ~ 1:3 2sO 4/ H 2o 24 ~ 12h, N is soaked in mixing solutions 2dry up the silicon chip obtaining cleaning up.
Described TiO 2the preparation of colloidal solution comprises the steps: that taking 4g tetrabutyl titanate adds in 16ml ethanol, and slowly drip 4ml glacial acetic acid under magnetic agitation, stirred at ambient temperature 5 ~ 6h, obtains the TiO that concentration is 39mg/ml 2colloidal solution, dilutes 1 ~ 5 times, obtains the TiO that concentration is 7.8 ~ 39mg/ml 2colloidal solution.
To be coated with one deck TiO 2colloidal solution and one deck GO colloidal solution are a spin coating cycle, and the described spin coating cycle is 2 ~ 4 cycles.
Beneficial effect of the present invention:
1, the present invention with the standby nanometer multilayer hollow capsules of LBL self-assembly legal system for substrate, by the change of hollow capsules form, cause the movement of forbidden photon band by a larger margin, thus promote the sensitivity of 1-D photon crystal detection, that thus prepares is more sensitiveer than common one-dimensional photonic crystal film based on nanometer multilayer hollow capsules one-dimensional photonic crystal film.
2, the inventive method is simply effective, easy and simple to handle, and required time is shorter.
3, the preparation facilities of the present invention's use is simple: do not need what special equipment, common spin coater just can meet the demands.
What 4, prepared by the present invention stores transport easily based on nanometer multilayer hollow capsules one-dimensional photonic crystal film: as long as just can be for subsequent use in clean orifice plate by being placed on based on nanometer multilayer hollow capsules one-dimensional photonic crystal film of preparing; Special protection can not needed through long-distance transport yet.
5, the present invention prepare based on nanometer multilayer hollow capsules one-dimensional photonic crystal film applied range: for preparing has excellent optical property, high mechanical strength, high stability, porousness based on nanometer multilayer hollow capsules one-dimensional photonic crystal film, easily introduces defect layer, to ambiance, pH, different guest molecules, there is sensitive optic response, be with a wide range of applications.
Accompanying drawing explanation
Fig. 1 is the reflection spectrum based on nanometer multilayer hollow capsules one-dimensional photonic crystal film that embodiment 1 is prepared.
Fig. 2 be embodiment 1 prepare based on the result figure of nanometer multilayer hollow capsules one-dimensional photonic crystal film for detection of acidic solution.
Fig. 3 is the result figure of common one-dimensional photonic crystal film for detection of acidic solution.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.The following example only for illustration of the present invention, but is not used for limiting practical range of the present invention.
Based on a preparation method for nanometer multilayer hollow capsules one-dimensional photonic crystal film, with SiO 2nanometer multilayer hollow capsules is substrate, comprises the steps:
Step one, utilize LBL self-assembly legal system for SiO 2nanometer multilayer hollow capsules;
Step 2, silicon chip is immersed acetone soln sonic oscillation 30 ~ 60min that volume percent is 90% ~ 100%, immersing volume percent afterwards is again sonic oscillation 30 ~ 60min in the ethanolic soln of 90% ~ 100%; Finally immersing volume ratio is the H of 3:7 ~ 1:3 2sO 4/ H 2o 24 ~ 12h, N is soaked in mixing solutions 2dry up the silicon chip obtaining cleaning up; Utilize the SiO that step one is prepared by spin-coating method 2nanometer multilayer hollow capsules is fixed on silicon chip surface, obtains the substrate of one-dimensional photonic crystal film, and wherein, spin coating rotating speed is 3000 ~ 6000rpm, and spin-coating time is 30s ~ 1min;
Step 3, prepare TiO respectively 2colloidal solution and GO colloidal solution, wherein, TiO 2colloidal solution concentration is 7.8 ~ 39mg/ml, GO colloidal solution concentration is 0.1 ~ 0.5mg/ml; Wherein, TiO 2colloidal solution is prepared as follows: take 4g tetrabutyl titanate and add in 16ml ethanol, and slowly drip 4ml glacial acetic acid under magnetic agitation, stirred at ambient temperature 5 ~ 6h, obtains the TiO that concentration is 39mg/ml 2colloidal solution, then dilutes 1 ~ 5 times as required, obtains the TiO that concentration is 7.8 ~ 39mg/ml 2colloidal solution; Being prepared as follows of GO colloidal solution: by soluble in water for graphene oxide (GO), is made into the GO colloidal solution that concentration is 0.1 ~ 0.5mg/ml;
Step 4, the TiO utilizing spin-coating method successively step 3 to be prepared 2colloidal solution and graphene oxide colloidal solution are coated onto substrate surface prepared by step 2, obtain described based on SiO 2nanometer multilayer hollow capsules one-dimensional photonic crystal film, wherein, every layer of spin coating rotating speed is 3000 ~ 6000rpm, and spin-coating time is 30s ~ 1min, to be coated with one deck TiO 2colloidal solution and one deck graphene oxide colloidal solution are a spin coating cycle, and the spin coating cycle is 2 ~ 4 cycles.
Described LBL self-assembly legal system is for SiO 2nanometer multilayer hollow capsules, comprises the steps:
Step one, be solvent with water, configure PAH solution and PSS solution respectively, wherein, PAH strength of solution is 1 ~ 3mg/ml, PSS strength of solution is 1 ~ 3mg/ml;
Step 2, be the SiO of 100 ~ 500nm by 1 ~ 3ml diameter 2particle is soluble in water, the centrifugal 2 ~ 5min of 1000 ~ 1500rpm, repeat washing, centrifugal 4 ~ 5 times, obtain clean SiO 2for template;
Step 3, the SiO that step 2 is obtained 2be immersed in 5 ~ 10min in PAH solution, the centrifugal 2 ~ 5min of 1000 ~ 1500rpm, is immersed in 5 ~ 10min in PSS solution afterwards again, the centrifugal 2 ~ 5min of 1000 ~ 1500rpm; Repeat PAH solution soaking, centrifugal, PSS solution soaking, centrifugal 4 ~ 5 times, obtain SiO 2/ (PAH/PSS) 4; Afterwards by SiO 2/ (PAH/PSS) 4being immersed in volume fraction is the centrifugal 2 ~ 3min of 5 ~ 10min in 4% ~ 5%HF solution, 7000 ~ 8000rpm; Repeat HF solution soaking, centrifugal 4 ~ 5 times to wash away SiO 2, obtain described SiO 2nanometer multilayer hollow capsules.
The silicon chip that following examples adopt founds crystal silicon material company limited by Zhejiang to be provided; SiO 2particle is provided by biological electronics National Key Laboratory of Southeast China University.
Embodiment 1
1) make solvent with water, configure PAH solution and PSS solution respectively, two kinds of strength of solution are 1mg/ml.
2) by 2ml SiO 2particle is soluble in water, the centrifugal 3min of 1300rpm, repeat washing, centrifugal 5 times, obtain clean SiO 2for template.
3) by SiO 2be immersed in the centrifugal 3min of 5min, 1300rpm in PAH solution; And then be immersed in the centrifugal 3min of 5min, 1300rpm in PSS solution; Repeat PAH solution soaking, centrifugal, PSS solution soaking, centrifugal 4 times, obtain SiO 2/ (PAH/PSS) 4; Then being immersed in volume fraction is the centrifugal 3min of 5min, 7500rpm in 4%HF solution, repeat HF solution soaking, centrifugal 5 times to wash away SiO 2, obtain SiO 2nanometer multilayer hollow capsules.
4) silicon chip is immersed the acetone soln sonic oscillation 30min that volume percent is 95%, and then to immerse volume percent be sonic oscillation 30min in the ethanolic soln of 95%, finally immersing volume ratio is the H of 1:3 2sO 4/ H 2o 212h is soaked, N in mixing solutions 2dry up the bare silicon wafer obtaining cleaning up.
5) by SiO 2nanometer multilayer hollow capsules drips completely whole silicon chip, and by spin-coating method, spin coating rotating speed is 4500rpm, and spin-coating time is 45s, by SiO 2nanometer multilayer hollow capsules is fixed on silicon chip surface, as the substrate of one-dimensional photonic crystal film.
6) taking 4g tetrabutyl titanate adds in 16ml ethanol, and slowly drip 4ml glacial acetic acid under magnetic agitation, stirred at ambient temperature 5h, obtains the pale yellow transparent TiO that concentration is 39mg/ml 2colloidal solution.GO is soluble in water, be made into the GO colloidal solution that concentration is 0.1mg/ml.
7) successively by TiO 2colloidal solution and GO colloidal solution are spun to substrate surface, and spin speed is 4500rpm, and spin-coating time is 45s, and the spin coating cycle is 3 cycles, prepares based on SiO 2nanometer multilayer hollow capsules one-dimensional photonic crystal film.
As shown in Figure 1, for the present embodiment prepare based on SiO 2the reflection spectrum that nanometer multilayer hollow capsules one-dimensional photonic crystal film is corresponding.As can be seen from the figure, the one-dimensional photonic crystal film forbidden photon band scope prepared of the present embodiment with common one-dimensional photonic crystal film (with the present embodiment prepare based on SiO 2the difference of nanometer multilayer hollow capsules one-dimensional photonic crystal film is not mix SiO 2nanometer multilayer hollow capsules) compare, do not change.
Fig. 2 and Fig. 3 be respectively the present embodiment prepare based on SiO 2nanometer multilayer hollow capsules one-dimensional photonic crystal film and common one-dimensional photonic crystal film (with the present embodiment prepare based on SiO 2the difference of nanometer multilayer hollow capsules one-dimensional photonic crystal film is not mix SiO 2nanometer multilayer hollow capsules) for the result figure of detection of acidic solution.Respectively two kinds of one-dimensional photonic crystal film are immersed 10 ~ 30min in acidic solution (pH=4), compare the reflection spectrum before and after their experiments.Can find out based on SiO from Fig. 2 and Fig. 3 2nanometer multilayer hollow capsules one-dimensional photonic crystal film is more sensitiveer than the one-dimensional photonic crystal film of not mixing nanometer multilayer hollow capsules.
Embodiment 2
1) make solvent with water, configure PAH solution and PSS solution respectively, PAH strength of solution is 1mg/ml, PSS strength of solution is 1mg/ml.
2) by 1ml SiO 2particle is soluble in water, the centrifugal 5min of 1000rpm, repeat washing, centrifugal 4 times, obtain clean SiO 2for template.
3) by SiO 2be immersed in the centrifugal 5min of 5min, 1000rpm in PAH solution; And then be immersed in the centrifugal 5min of 5min, 1000rpm in PSS solution; Repeat PAH solution soaking, centrifugal, PSS solution soaking, centrifugal 4 times, obtain SiO 2/ (PAH/PSS) 4; Then being immersed in volume fraction is the centrifugal 3min of 5min, 7000rpm in 4%HF solution, repeat HF solution soaking, centrifugal 4 times to wash away SiO 2, obtain SiO 2nanometer multilayer hollow capsules.
4) silicon chip is immersed the acetone soln sonic oscillation 30min that volume percent is 90%, and then to immerse volume percent be sonic oscillation 30min in the ethanolic soln of 90%, finally immersing volume ratio is the H of 1:3 2sO 4/ H 2o 24h is soaked, N in mixing solutions 2dry up the bare silicon wafer obtaining cleaning up.
5) by SiO 2nanometer multilayer hollow capsules drips completely whole silicon chip, and by spin-coating method, spin coating rotating speed is 3000rpm, and spin-coating time is 1min, by SiO 2nanometer multilayer hollow capsules is fixed on silicon chip surface, as the substrate of one-dimensional photonic crystal film.
6) taking 4g tetrabutyl titanate adds in 16ml ethanol, and slowly drip 4ml glacial acetic acid under magnetic agitation, stirred at ambient temperature 6h, obtains the TiO that concentration is 39mg/ml 2colloidal solution.GO is soluble in water, be made into the GO colloidal solution that concentration is 0.1mg/ml.
7) successively by TiO 2colloidal solution and GO colloidal solution are spun to substrate surface, and spin speed is 3000rpm, and spin-coating time is 1min, and the spin coating cycle is 2 cycles, prepares based on SiO 2nanometer multilayer hollow capsules one-dimensional photonic crystal film.
Embodiment 3
1) make solvent with water, configure PAH solution and PSS solution respectively, PAH strength of solution is 3mg/ml, PSS strength of solution is 3mg/ml.
2) by 3ml SiO 2particle is soluble in water, the centrifugal 2min of 1500rpm, repeat washing, centrifugal 4 times, obtain clean SiO 2for template.
3) by SiO 2be immersed in the centrifugal 2min of 10min, 1500rpm in PAH solution; And then be immersed in the centrifugal 2min of 10min, 1500rpm in PSS solution; Repeat PAH solution soaking, centrifugal, PSS solution soaking, centrifugal 5 times, obtain SiO 2/ (PAH/PSS) 4; Then being immersed in volume fraction is the centrifugal 3min of 10min, 8000rpm in 5%HF solution, repeat HF solution soaking, centrifugal 5 times to wash away SiO 2, obtain SiO 2nanometer multilayer hollow capsules.
4) silicon chip is immersed the acetone soln sonic oscillation 60min that volume percent is 100%, and then to immerse volume percent be sonic oscillation 60min in the ethanolic soln of 100%, finally immersing volume ratio is the H of 3:7 2sO 4/ H 2o 212h is soaked, N in mixing solutions 2dry up the bare silicon wafer obtaining cleaning up.
5) by SiO 2nanometer multilayer hollow capsules drips completely whole silicon chip, and by spin-coating method, spin coating rotating speed is 6000rpm, and spin-coating time is 30s, by SiO 2nanometer multilayer hollow capsules is fixed on silicon chip surface, as the substrate of one-dimensional photonic crystal film.
6) taking 4g tetrabutyl titanate adds in 16ml ethanol, and slowly drip 4ml glacial acetic acid under magnetic agitation, stirred at ambient temperature 5h, obtains the TiO that concentration is 39mg/ml 2colloidal solution, then dilutes 5 times, obtains the TiO that concentration is 7.8mg/ml 2colloidal solution.GO is soluble in water, be made into the GO colloidal solution that concentration is 0.5mg/ml.
7) successively by TiO 2colloidal solution and GO colloidal solution are spun to substrate surface, and spin speed is 6000rpm, and spin-coating time is 30s, and the spin coating cycle is 4 cycles, prepares based on SiO 2nanometer multilayer hollow capsules one-dimensional photonic crystal film.

Claims (4)

1. based on a preparation method for nanometer multilayer hollow capsules one-dimensional photonic crystal film, it is characterized in that, with SiO 2nanometer multilayer hollow capsules is substrate, comprises the steps:
Step one, utilize LBL self-assembly legal system for SiO 2nanometer multilayer hollow capsules; Described LBL self-assembly legal system is for SiO 2nanometer multilayer hollow capsules comprises the steps: to take water as solvent, and configure PAH solution and PSS solution respectively, wherein, PAH strength of solution is 1 ~ 3mg/ml, PSS strength of solution is 1 ~ 3mg/ml; Be the SiO of 100 ~ 500nm by 1 ~ 3ml diameter 2particle washing, repeatedly centrifugal, obtain clean SiO 2for template; By the SiO obtained 2be immersed in 5 ~ 10min in PAH solution, the centrifugal 2 ~ 5min of 1000 ~ 1500rpm, is immersed in 5 ~ 10min in PSS solution afterwards again, the centrifugal 2 ~ 5min of 1000 ~ 1500rpm; Repeat PAH solution soaking, centrifugal, PSS solution soaking, centrifugal 4 ~ 5 times, obtain SiO 2/ (PAH/PSS) 4 ~ 5; Afterwards by SiO 2/ (PAH/PSS) 4 ~ 5being immersed in volume fraction is the centrifugal 2 ~ 3min of 5 ~ 10min in 4% ~ 5%HF solution, 7000 ~ 8000rpm; Repeat HF solution soaking, centrifugal 4 ~ 5 times to wash away SiO 2, obtain described SiO 2nanometer multilayer hollow capsules;
Step 2, silicon chip are cleaned and are dried up, and utilize the SiO that step one is prepared by spin-coating method 2nanometer multilayer hollow capsules is fixed on silicon chip surface, obtains the substrate of one-dimensional photonic crystal film, and wherein, spin coating rotating speed is 3000 ~ 6000rpm, and spin-coating time is 30s ~ 1min;
Step 3, prepare TiO respectively 2colloidal solution and GO colloidal solution, wherein, TiO 2colloidal solution concentration is 7.8 ~ 39mg/ml, GO colloidal solution concentration is 0.1 ~ 0.5mg/ml;
Step 4, the TiO utilizing spin-coating method successively step 3 to be prepared 2colloidal solution and GO colloidal solution are coated onto substrate surface prepared by step 2, obtain described based on SiO 2nanometer multilayer hollow capsules one-dimensional photonic crystal film, wherein, every layer of spin coating rotating speed is 3000 ~ 6000rpm, and spin-coating time is 30s ~ 1min.
2. the preparation method based on nanometer multilayer hollow capsules one-dimensional photonic crystal film according to claim 1, it is characterized in that, silicon chip described in step 2 is cleaned to dry up and is comprised the steps: silicon chip to be immersed acetone soln sonic oscillation 30 ~ 60min that volume percent is 90% ~ 100%, and immersing volume percent afterwards is again sonic oscillation 30 ~ 60min in the ethanolic soln of 90% ~ 100%; Finally immersing volume ratio is the H of 3:7 ~ 1:3 2sO 4/ H 2o 24 ~ 12h, N is soaked in mixing solutions 2dry up the silicon chip obtaining cleaning up.
3. the preparation method based on nanometer multilayer hollow capsules one-dimensional photonic crystal film according to claim 1, is characterized in that, TiO described in step 3 2the preparation of colloidal solution comprises the steps: that taking 4g tetrabutyl titanate adds in 16ml ethanol, and slowly drip 4ml glacial acetic acid under magnetic agitation, stirred at ambient temperature 5 ~ 6h, obtains the TiO that concentration is 39mg/ml 2colloidal solution, dilutes 1 ~ 5 times, obtains the TiO that concentration is 7.8 ~ 39mg/ml 2colloidal solution.
4. the preparation method based on nanometer multilayer hollow capsules one-dimensional photonic crystal film according to claim 1, is characterized in that, to be coated with one deck TiO in step 4 2colloidal solution and one deck GO colloidal solution are a spin coating cycle, and the described spin coating cycle is 2 ~ 4 cycles.
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