CN105439462A - Purple hollow silicon oxide photonic crystal structure color thin film and preparation method thereof - Google Patents
Purple hollow silicon oxide photonic crystal structure color thin film and preparation method thereof Download PDFInfo
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- CN105439462A CN105439462A CN201510874389.7A CN201510874389A CN105439462A CN 105439462 A CN105439462 A CN 105439462A CN 201510874389 A CN201510874389 A CN 201510874389A CN 105439462 A CN105439462 A CN 105439462A
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Abstract
The invention discloses a purple hollow silicon oxide photonic crystal structure color thin film and a preparation method thereof and belongs to the technical field of preparation of photonic crystal structure color thin films. According to the method, organic microsphere polystyrene (PS) with the particle size being 200+/-5 nm serves as a template, -NH2 is firstly modified on the surface of the template, then the surface of the template is coated with a uniform silicon oxide layer through the improved method shown in the specification, finally, a photonic crystal structure of an opal structure is formed on the surface of a glass substrate in a self-assembly mode, then, PS microspheres are forged under protection of reduction atmosphere to be carbonized, black matter generated by the carbonized PS microspheres exist in all hollow silicon oxide shell layers to absorb most part of incoherent scattered light, and the purple photonic crystal structure color thin film assembled by the high-saturability silicon oxide hollow spheres is obtained. The method is simple in process, raw materials are easy to obtain, and the method can be widely applied in the aspects of display, printing, paint, cosmetics, photonic crystal and the like.
Description
Technical field
The invention belongs to photonic crystal structure color film preparing technical field, be specifically related to hollow silicon oxide photonic crystal structure color film of a kind of purple and preparation method thereof.
Background technology
Schemochrome by object microtexture and visible ray interferes, the phenomenon such as scattering or diffraction develops the color, this is a kind of physics colour generation, and it has the advantages such as bright-colored, will never fade, environmental friendliness, preparation cycle are short.Wherein by the orderly self-assembly method of colloid micro ball, the opal photonic crystal that the high low-refraction formed alternately changes, also there is photon band gap feature, when incident light frequency drops in bandgap range, this incident light will by this photonic crystal, these visible rays that can not continue to propagate can be reflected by photonic crystal, finally form coherent diffraction at the photon crystal surface with periodic structure, and produce bright and colourful schemochrome.By the research to occurring in nature and artificial preparation schemochrome, there is good application in display, decoration, the field such as false proof at present.In recent years, the photonic crystal that hollow ball is assembled into was subject to the extensive of investigator, if Deng is at SynthesisofMonodispersePolystyreneVinyl-SiO
2core-ShellParticlesandHollowSiO
2put forward a kind of preparation method of silicon oxide hollow ball photonic crystal structure color film in Spheres, mainly pass through PSSiO
2the self-assembly of nucleocapsid structure microballoon on substrate, then the technology of the few organics removal core of ton obtains in glass baseplate surface assembling under air, and this photonic crystal structure color has good structure.But the photonic crystal of silicon oxide hollow ball assembling is thinner due to shell, result in effective refractive index modulation less, thus the photonic crystal that hollow silicon oxide assembles to have reflection strength less.This seriously will limit the application of hollow ball photonic crystal in schemochrome.
Summary of the invention
The object of the present invention is to provide hollow silicon oxide photonic crystal structure color film of a kind of purple and preparation method thereof, the method is simple, environmentally safe, and obtained purple hollow silicon oxide photonic crystal structure color film color saturation is high, not fugitive color.
The present invention is achieved through the following technical solutions:
A preparation method for the hollow silicon oxide photonic crystal structure color film of purple, comprises the following steps:
1) by particle diameter be the polystyrene microsphere powder ultrasonic disperse of 200 ± 5nm in the mixed solution of ethanol and deionized water, then add ammoniacal liquor, fully add silicon source in the backward mixed system of mixing, after stirring reaction, centrifuging and taking precipitates, and precipitates through washing, drying, obtained PSSiO
2nucleocapsid structure microballoon;
2) by PSSiO
2nucleocapsid structure microballoon is scattered in dehydrated alcohol, obtained containing SiO
2the emulsion of microballoon;
3) glass substrate is dipped vertically into containing SiO
2in the emulsion of microballoon, be dried to containing SiO at 40 ~ 50 DEG C
2after dehydrated alcohol in the emulsion of microballoon volatilizees completely, obtain nucleocapsid structure photon crystal film at glass substrate surface;
4) nucleocapsid structure photon crystal film is calcined 1 ~ 4 hour under 500 ~ 600 DEG C of reducing atmospheres, the obtained hollow silicon oxide photonic crystal structure color film of high color saturation purple.
Step 1) in the amount ratio of polystyrene microsphere powder, ethanol and deionized water be 0.03g:(25 ~ 40) mL:(1 ~ 3) mL.
The ammoniacal liquor that 0.3 ~ 0.5mL massfraction is 30% is added in the mixed solution of every 30 ~ 45mL ethanol and deionized water.
Step 1) described silicon source adds tetraethoxy in mixed system, add-on is that every 0.03g polystyrene microsphere powder adds 150 ~ 200 μ L tetraethoxys.
Step 1) add ammoniacal liquor after abundant mixing be at room temperature adopt magnetic agitation 30 ~ 60min; The stirring reaction added behind silicon source is at room temperature magnetic agitation 7 ~ 10h.
Step 1) described in centrifugal be carry out under 4000 ~ 8000r/min, centrifugation time is 3-6min.
Step 1) the described washing to precipitation precipitation first washed 2 ~ 4 times through deionization, then through washes of absolute alcohol 2 ~ 4 times.
Step 2) middle PSSiO
2the amount ratio of nucleocapsid structure microballoon and dehydrated alcohol is (0.1 ~ 0.25) g:10mL.
Glass substrate is before use through cleaning: first in the hydrogen peroxide solution that mass concentration is 30%, soak 10h, respectively clean 2 ~ 3 times with deionized water and dehydrated alcohol.
The invention also discloses the hollow silicon oxide photonic crystal structure color film of purple adopting aforesaid method obtained.
Compared with prior art, the present invention has following useful technique effect:
The preparation method of the hollow silicon oxide photonic crystal structure color film of purple disclosed by the invention, first with particle diameter be organic polystyrene (PS) the microballoon powder of 200 ± 5nm for template, first modify-NH on its surface
2, then utilization improves
method is at the uniform silicon oxide layer of its Surface coating one deck, then formed the photon crystal structure of opal structural at glass substrate surface by self-assembly, again by the calcining under protection of reducing atmosphere by the carbonization of PS microballoon, the atrament generated due to the PS microballoon of carbonization is present in each hollow silicon oxide shell inside, thus absorb most of non-coherent scattering light, partially carbonized PS is present in hollow ball inside, greatly improve hollow ball color saturation, thus solve hollow ball and be assembled into the low shortcoming of photonic crystal color visibility, obtain a kind of purple photonic crystal structure color film that there is high saturation silicon oxide hollow ball and assemble.Present invention process process is simple, environmentally safe, and energy large-scale commercial production, has broad application prospects.
The purple film color obtained through the present invention is beautiful, saturation ratio is high, not fugitive color, solves chemical organic compounds pigment fugitive color, harmful shortcoming.
Accompanying drawing explanation
Fig. 1 is the optical microscope photograph that embodiment 1 gained has the hollow silicon oxide photonic crystal structure color film of purple;
Fig. 2 is the transmission photo of the hollow silicon oxide microsphere of embodiment 1 gained.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
Embodiment 1
A preparation method for the hollow silicon oxide photonic crystal structure color film of purple, comprises the following steps:
(1) by polystyrene (PS) microballoon powder, ethanol and the deionized water amount ratio according to 0.03g:30mL:1mL, taking particle diameter is that the PS microballoon powder ultrasonic disperse of 200 ± 5nm is in the mixed solution of dehydrated alcohol and deionized water, after dispersion completely, the ratio of 0.3mL ammoniacal liquor is added according to every 30mL mixed solution, ammoniacal liquor is added in mixed solution, room temperature lower magnetic force is uniformly mixed 30min, 150 μ L tetraethoxys are added again fast as silicon source in reaction system, after room temperature lower magnetic force stirring reaction 8h through washing, centrifugal, dry, can PSSiO be obtained
2nucleocapsid structure microballoon.
(2) precise step (1) obtains PSSiO
2nucleocapsid structure microballoon 0.1g, ultrasonic disperse is in 10ml dehydrated alcohol, obtained containing SiO
2the emulsion of microballoon, and in 40 DEG C of baking ovens, utilize vertical deposition method plated film on a glass substrate.
(3) the nucleocapsid structure photon crystal film of preparation is calcined 1h under 500 DEG C of reducing atmospheres, organic micro-spheres carbonization, the hollow silicon oxide photonic crystal structure color film of purple of existing high color saturation can be obtained.
See Fig. 1, the schemochrome unit as can be seen from Figure 1 after calcining presents the purple with high saturation, and color is beautiful.
See Fig. 2, the hollow silicon oxide microsphere as can be seen from Figure 2 utilizing the method to prepare has homogeneous particle diameter, and the state of the high dispersing be in, be conducive to the carrying out of self assembling process; As can be seen from the figure, after calcined, organic layer is removed, and hollow silicon oxide ball successfully obtains.
Embodiment 2
A preparation method for the hollow silicon oxide photonic crystal structure color film of purple, comprises the following steps:
(1) by polystyrene (PS) microballoon powder, ethanol and the deionized water amount ratio according to 0.03g:35mL:2mL, taking particle diameter is that the PS microballoon powder ultrasonic disperse of 200 ± 5nm is in the mixed solution of dehydrated alcohol and deionized water, after dispersion completely, the ratio of 0.4mL ammoniacal liquor is added according to every 35mL mixed solution, ammoniacal liquor is added in mixed solution, room temperature lower magnetic force is uniformly mixed 40min, 170 μ L tetraethoxys are added again fast as silicon source in reaction system, after room temperature lower magnetic force stirring reaction 10h through washing, centrifugal, dry, can PSSiO be obtained
2nucleocapsid structure microballoon, hollow silicon oxide core microballoon, its diameter is 240 ± 5nm, and shell thickness is 25 ± 5nm.
(2) precise step (1) obtains PSSiO
2nucleocapsid structure microballoon 0.15g, ultrasonic disperse, in 10mL dehydrated alcohol, has obtained SiO
2the emulsion of microballoon, and in 45 DEG C of baking ovens, utilize vertical deposition method plated film on a glass substrate.
(3) the nucleocapsid structure photon crystal film of preparation is calcined 4h under 550 DEG C of reducing atmospheres, because the carbonization of organic micro-spheres, the hollow silicon oxide photonic crystal structure color film of purple of existing high color saturation can be obtained.
Embodiment 3
A preparation method for the hollow silicon oxide photonic crystal structure color film of purple, comprises the following steps:
(1) by polystyrene (PS) microballoon powder, ethanol and the deionized water amount ratio according to 0.03g:40mL:3mL, taking particle diameter is that the PS microballoon powder ultrasonic disperse of 200 ± 5nm is in the mixed solution of dehydrated alcohol and deionized water, after dispersion completely, the ratio adding 0.5mL ammoniacal liquor according to every 45ml mixed solution adds ammoniacal liquor in mixed solution, room temperature lower magnetic force is uniformly mixed 30min, 200 μ L tetraethoxys are added again fast as silicon source in reaction system, after room temperature lower magnetic force stirring reaction 7h through washing, centrifugal, dry, can PSSiO be obtained
2nucleocapsid structure microballoon.
(2) precise step (1) obtains PSSiO
2nucleocapsid structure microballoon 0.18g, ultrasonic disperse has obtained SiO in 10mL dehydrated alcohol
2the emulsion of microballoon, and in 40 ~ 50 DEG C of baking ovens, utilize vertical deposition method plated film on a glass substrate.
(3) the nucleocapsid structure photon crystal film of preparation is calcined 2h under 600 DEG C of reducing atmospheres, because the carbonization of organic micro-spheres, the hollow silicon oxide photonic crystal structure color film of purple of existing high color saturation can be obtained.
In sum, first the present invention adopts without emulsion polymerization, prepares the PS microballoon of 200 ± 5nm of uniform particle sizes, then by improve
method can obtain at its coated with uniform one deck silicon oxide the PSSiO that particle diameter is 240 ± 5nm
2nucleocapsid structure microballoon, the carbonization finally by PS organic under protection of reducing atmosphere can obtain having the hollow silicon oxide photon crystal film of high brightness purple.This method solve the problem that hollow ball photonic crystal colour intensity is low, this purple film color is beautiful simultaneously, and not fugitive color, solves chemical organic compounds pigment fugitive color, harmful shortcoming.Present invention process process is simple, enormously simplify experimentation, and has higher saturation ratio by the purple hollow silicon oxide photonic crystal structure color film that this method obtains, and in display, printing, coating, makeup, the aspects such as photonic crystal are widely used.
Claims (10)
1. a preparation method for the hollow silicon oxide photonic crystal structure color film of purple, is characterized in that, comprise the following steps:
1) by particle diameter be the polystyrene microsphere powder ultrasonic disperse of 200 ± 5nm in the mixed solution of ethanol and deionized water, then add ammoniacal liquor, fully add silicon source in the backward mixed system of mixing, after stirring reaction, centrifuging and taking precipitates, and precipitates through washing, drying, obtained PSSiO
2nucleocapsid structure microballoon;
2) by PSSiO
2nucleocapsid structure microballoon is scattered in dehydrated alcohol, obtained containing SiO
2the emulsion of microballoon;
3) glass substrate is dipped vertically into containing SiO
2in the emulsion of microballoon, be dried to containing SiO at 40 ~ 50 DEG C
2after dehydrated alcohol in the emulsion of microballoon volatilizees completely, obtain nucleocapsid structure photon crystal film at glass substrate surface;
4) nucleocapsid structure photon crystal film is calcined 1 ~ 4 hour under 500 ~ 600 DEG C of reducing atmospheres, the obtained hollow silicon oxide photonic crystal structure color film of purple.
2. the preparation method of the hollow silicon oxide photonic crystal structure color film of purple according to claim 1, it is characterized in that, step 1) in the amount ratio of polystyrene microsphere powder, ethanol and deionized water be 0.03g:(25 ~ 40) mL:(1 ~ 3) mL.
3. the preparation method of the hollow silicon oxide photonic crystal structure color film of purple according to claim 1, is characterized in that, adds the ammoniacal liquor that 0.3 ~ 0.5mL massfraction is 30% in the mixed solution of every 30 ~ 45mL ethanol and deionized water.
4. the preparation method of the hollow silicon oxide photonic crystal structure color film of purple according to claim 1, it is characterized in that, step 1) described silicon source adds tetraethoxy in mixed system, add-on is that every 0.03g polystyrene microsphere powder adds 150 ~ 200 μ L tetraethoxys.
5. the preparation method of the hollow silicon oxide photonic crystal structure color film of purple according to claim 1, is characterized in that, step 1) add ammoniacal liquor after abundant mixing be at room temperature adopt magnetic agitation 30 ~ 60min; The stirring reaction added behind silicon source is at room temperature magnetic agitation 7 ~ 10h.
6. the preparation method of the hollow silicon oxide photonic crystal structure color film of purple according to claim 1, is characterized in that, step 1) described in centrifugal be carry out under 4000 ~ 8000r/min, centrifugation time is 3 ~ 6min.
7. the preparation method of the hollow silicon oxide photonic crystal structure color film of purple according to claim 1, is characterized in that, step 1) the described washing to precipitation precipitation first washed 2 ~ 4 times through deionization, then through washes of absolute alcohol 2 ~ 4 times.
8. the preparation method of the hollow silicon oxide photonic crystal structure color film of purple according to claim 1, is characterized in that, step 2) middle PSSiO
2the amount ratio of nucleocapsid structure microballoon and dehydrated alcohol is (0.1 ~ 0.25) g:10mL.
9. the preparation method of the hollow silicon oxide photonic crystal structure color film of purple according to claim 1, it is characterized in that, glass substrate is before use through cleaning: first in the hydrogen peroxide solution that mass concentration is 30%, soak 10h, respectively clean 2 ~ 3 times with deionized water and dehydrated alcohol.
10. adopt the hollow silicon oxide photonic crystal structure color film of purple that the method in claim 1 ~ 9 described in any one is obtained.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108919386A (en) * | 2018-06-20 | 2018-11-30 | 中山大学 | The method for preparing magnetic amorphous photonic crystal based on ferroso-ferric oxide/silicon dixoide nucleocapsid structure nano particles |
| CN114605807A (en) * | 2022-02-18 | 2022-06-10 | 大连理工大学 | Polycarbonate diol-based structural color elastomer and preparation method thereof |
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| CN103288491A (en) * | 2013-05-29 | 2013-09-11 | 陕西科技大学 | Preparation method of blue-green photonic crystal structure color film |
| CN103288492A (en) * | 2013-05-29 | 2013-09-11 | 陕西科技大学 | Preparation method of red photonic crystal structured colored glaze |
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| CN103288491A (en) * | 2013-05-29 | 2013-09-11 | 陕西科技大学 | Preparation method of blue-green photonic crystal structure color film |
| CN103288492A (en) * | 2013-05-29 | 2013-09-11 | 陕西科技大学 | Preparation method of red photonic crystal structured colored glaze |
Non-Patent Citations (1)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108919386A (en) * | 2018-06-20 | 2018-11-30 | 中山大学 | The method for preparing magnetic amorphous photonic crystal based on ferroso-ferric oxide/silicon dixoide nucleocapsid structure nano particles |
| CN114605807A (en) * | 2022-02-18 | 2022-06-10 | 大连理工大学 | Polycarbonate diol-based structural color elastomer and preparation method thereof |
| CN114605807B (en) * | 2022-02-18 | 2022-12-13 | 大连理工大学 | Polycarbonate diol-based structural color elastomer and preparation method thereof |
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