CN106868592A - A kind of preparation of titanium dioxide inverse opal photonic crystal and method of modifying - Google Patents
A kind of preparation of titanium dioxide inverse opal photonic crystal and method of modifying Download PDFInfo
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- CN106868592A CN106868592A CN201710007765.1A CN201710007765A CN106868592A CN 106868592 A CN106868592 A CN 106868592A CN 201710007765 A CN201710007765 A CN 201710007765A CN 106868592 A CN106868592 A CN 106868592A
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- photonic crystal
- opal photonic
- titanium dioxide
- inverse opal
- polymethyl methacrylate
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B1/00—Single-crystal growth directly from the solid state
- C30B1/10—Single-crystal growth directly from the solid state by solid state reactions or multi-phase diffusion
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/02—Heat treatment
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Abstract
The present invention discloses a kind of preparation method of titanium dioxide inverse opal photonic crystal, and step is as follows:(1)Polymethyl methacrylate opal photonic crystal masterplate is prepared on slide using vertical deposition method;(2)TiO 2 precursor solution is filled into the gap of polymethyl methacrylate opal photonic crystal masterplate using capillary force osmosis, after natural air drying, 500 DEG C are risen with the speed of 50 DEG C/h, sintering obtains titanium dioxide inverse opal photonic crystal, wherein, the TiO 2 precursor solution is by volume 37.5 by butyl titanate, ethanol, water and nitric acid:25:1:1.625 compositions.The inventive method can obtain the complete titanium dioxide inverse opal photonic crystal of large-area high-quality, and operate more simple.The electron mobility and catalytic performance of photonic crystal can be improved after titanium dioxide inverse opal photonic crystal modification silver.
Description
Technical field
Preparation and method of modifying the present invention relates to a kind of titanium dioxide inverse opal photonic crystal.
Background technology
Photonic crystal refers to the artificial periodic dielectric structures with photon band gap characteristic.This periodic arrangement makes
Photonic crystal can form the forbidden photon band similar to semiconductor forbidden band, and then can realize the regulation and control to photon.According to photon
Crystal can be classified as to the geometric properties of light modulation:1-D photon crystal, 2 D photon crystal, three-D photon crystal.It is three-dimensional
Inverse opal photonic crystal is due to big specific surface area, connective, good opening high.Counter opal light in recent years
Sub- crystal has in terms of bio-sensing, catalysis, solar cell and electronic device widely to be applied.Nanostructured titanium dioxide
Titanium has excellent optics, catalysis and conduction property, is widely used in industry, food and field of environment protection.Due to nanometer two
Titanium oxide has high transparency, high index of refraction again, therefore is the ideal material for preparing three-dimensional inverse opal photonic crystal.
" Colloidal Template Method prepares ordered big hole TiO2Material "(Chemical journal, volume 64 the 13rd phase, 1389- in 2006
1392)Disclose a kind of ordered big hole TiO2The preparation method of material, the method is with V (butyl titanate):V (water):V (second
Alcohol):V (hydrochloric acid)=5:2:3:1 sol impregnation polymethyl methacrylate (PMMA) colloidal crystal, by gel, ageing, journey
PMMA is removed after sequence intensification roasting obtain ordered big hole TiO2, ordered big hole TiO prepared by the method2Material exists as shown in Figure 5
More surface defect, it is difficult to obtain the complete ordered big hole TiO of large area2。
Patent document CN102336434A discloses a kind of preparation side of titanium dioxide counter opal structure Ordered Macroporous Materials
Method, it first prepares polystyrene opal structural template using vertical deposition method, then the hydrochloric acid of template immersion titanium tetrachloride is molten
Liquid, slow filling hydrous titanium oxide, 70~90 DEG C of holding is needed in filling process in template, and high-temperature roasting is obtained after filling,
Although this can obtain the more preferable titanium dioxide counter opal structure of the degree of order, the base used vertical deposition method is needed during its preparation
Bottom substrate carries out hydrophilic treated, and protection temperature higher is needed during filling, operates more numerous and diverse.
The content of the invention
The technical problem to be solved in the present invention is to overcome existing defect, there is provided a kind of titanium dioxide inverse opal photon
The preparation method of crystal.
In order to solve the above-mentioned technical problem, the invention provides following technical scheme:
A kind of preparation method of titanium dioxide inverse opal photonic crystal, step is as follows:
(1)Polymethyl methacrylate opal photonic crystal masterplate is prepared on slide using vertical deposition method;
(2)TiO 2 precursor solution is filled into by polymethyl methacrylate opal photonic crystal using liquid infiltration method
In the gap of masterplate, after natural air drying, 500 DEG C are risen with the speed of 50 DEG C/h, it is brilliant that sintering obtains titanium dioxide inverse opal photon
Body, wherein, the TiO 2 precursor solution is by volume 37.5 by butyl titanate, ethanol, water and nitric acid:25:1:
1.625 compositions.
Preferably, the detailed process of vertical deposition method is as follows:Clean slide is inserted vertically into poly-methyl methacrylate
In ester nanosphere emulsion, placed 3 days in 30 DEG C of air dry oven, polymethyl methacrylate egg is obtained on slide
White stone photonic crystal masterplate.
A kind of method of modified titanic oxide inverse opal photonic crystal, the anti-egg of titanium dioxide that will be prepared according to the above method
White stone photonic crystal silver nitrate solution soaks 1 hour, then in 350 DEG C of sintering, obtains the anti-albumen of titanium dioxide of modified by silver
Stone photonic crystal.
Compared with the conventional method, the inventive method can obtain the complete titanium dioxide inverse opal photon of large-area high-quality
Crystal, and operate more simple.By the modification of silver, the electronics that can effectively improve titanium dioxide inverse opal photonic crystal is moved
Shifting rate, improves the conduction and catalytic performance of semi-conducting material.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, with reality of the invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings:
Fig. 1 is the stereoscan photograph of polymethyl methacrylate opal photonic crystal masterplate;
Fig. 2 is the stereoscan photograph of titanium dioxide inverse opal photonic crystal;
Fig. 3 is the transmission electron microscope photo of modified by silver titanium dioxide inverse opal photonic crystal;
Fig. 4 is the photon band gap curve of photonic crystal.
Fig. 5 is the stereoscan photograph of existing titanium dioxide inverse opal photonic crystal.
Specific embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that preferred reality described herein
Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment 1
(1)The preparation of polymethyl methacrylate nano ball
Add 60 ml water in the hole round-bottomed bottles of 100 ml tri-, 8 ml methyl methacrylate liquid, 24 mg potassium peroxydisulfates, it
After add three hole round-bottomed bottles.Oil bath pan is closed after being reacted 90 minutes in 95 DEG C of oil bath pans, polymethyl methacrylate is obtained
Nanosphere emulsion.
(2)The growth of polymethyl methacrylate photonic crystal of opals structure masterplate
60 ml water are added in beaker, 2.5 ml polymethyl methacrylate nano ball emulsion, the slide for taking cleaning is vertical
In insertion beaker.Beaker is put into 30 DEG C of air dry oven, is placed 3 days, in the presence of capillary force on slide
Polymethyl methacrylate opal photonic crystal masterplate is prepared, stereoscan photograph is as shown in Figure 1.
(3)The preparation of titanium dioxide inverse opal photonic crystal
15 ml butyl titanates are dissolved in 10 ml absolute ethyl alcohols, 0.4 ml pure water is added dropwise over, is then added dropwise over again
0.65 ml nitric acid, and stir 1 hour to solution clarification, obtain TiO 2 precursor solution.By settled solution spin coating or drop in
On polymethyl methacrylate opal photonic crystal masterplate, permeated by capillarity and be filled into opal photonic crystal masterplate
Gap in.And by the template after filling in atmosphere natural air drying after, be put into tube furnace, with 50 DEG C per hour of speed liter
Temperature is kept for 3 hours of sintering to 500 DEG C.Room temperature is naturally cooling to afterwards, prepares titanium dioxide inverse opal photonic crystal,
Stereoscan photograph is as shown in Figure 2.Can be seen that the inventive method by Fig. 2 and Fig. 5 can obtain the complete titanium dioxide of large area
Inverse opal photonic crystal, defect is less, and photonic crystal quality is significantly improved.
(4)Modified by silver titanium dioxide inverse opal photonic crystal
850 mg silver nitrates are dissolved in 20 ml ultra-pure waters, the titanium dioxide inverse opal photonic crystal that will be prepared is dipped in
In silver nitrate solution, kept for 1 hour, the titanium dioxide inverse opal photonic crystal that then will be loaded with silver nitrate is put into annealing furnace
In, 350 DEG C are warming up to 100 DEG C per hour of speed, keep sintering 1 hour.Room temperature then is naturally cooling to, silver is prepared
The titanium dioxide inverse opal photonic crystal of modification, transmission electron microscope photo are as shown in figure 3, photon band gap curve is as shown in Figure 4.
Finally it should be noted that:The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
Modified with to the technical scheme described in foregoing embodiments, or equivalent is carried out to which part technical characteristic.
All any modification, equivalent substitution and improvements within the spirit and principles in the present invention, made etc., should be included in of the invention
Within protection domain.
Claims (3)
1. a kind of preparation method of titanium dioxide inverse opal photonic crystal, step is as follows:
(1)Polymethyl methacrylate opal photonic crystal masterplate is prepared on slide using vertical deposition method;
(2)TiO 2 precursor solution is filled into by polymethyl methacrylate opal photonic crystal using liquid infiltration method
In the gap of masterplate, after natural air drying, 500 DEG C are risen with the speed of 50 DEG C/h, it is brilliant that sintering obtains titanium dioxide inverse opal photon
Body, wherein, the TiO 2 precursor solution is by volume 37.5 by butyl titanate, ethanol, water and nitric acid:25:1:
1.625 compositions.
2. preparation method according to claim 1, it is characterised in that the detailed process of vertical deposition method is as follows:By cleaning
Slide be inserted vertically into polymethyl methacrylate nano ball emulsion, in 30 DEG C of air dry oven place 3 days,
Polymethyl methacrylate opal photonic crystal masterplate is obtained on slide.
3. a kind of method of modified titanic oxide inverse opal photonic crystal, the dioxy that will be prepared according to claim 1 methods described
Change titanium inverse opal photonic crystal silver nitrate solution to soak 1 hour, then in 350 DEG C of sintering, obtain the titanium dioxide of modified by silver
Titanium inverse opal photonic crystal.
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Cited By (5)
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CN106835281A (en) * | 2017-01-05 | 2017-06-13 | 南阳师范学院 | A kind of preparation method of Yttrium Orthovanadate three-dimensional inverse opal photonic crystal |
CN107655813A (en) * | 2017-11-09 | 2018-02-02 | 东南大学 | Based on cardiac muscle cell's detection method of counter opal structure hydrogel and its application |
CN107876038A (en) * | 2017-11-29 | 2018-04-06 | 青岛农业大学 | A kind of counter opal TiO of Ag inductions2The preparation method of homojunction photochemical catalyst |
CN113737281A (en) * | 2021-08-31 | 2021-12-03 | 武汉理工大学 | Oxide spherical photonic crystal with inverse opal structure, simple preparation method and application thereof |
CN114113051A (en) * | 2021-12-16 | 2022-03-01 | 南京信息工程大学 | Preparation method and application of PSMA (patterned sapphire substrate) electrochemiluminescence sensor |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106835281A (en) * | 2017-01-05 | 2017-06-13 | 南阳师范学院 | A kind of preparation method of Yttrium Orthovanadate three-dimensional inverse opal photonic crystal |
CN107655813A (en) * | 2017-11-09 | 2018-02-02 | 东南大学 | Based on cardiac muscle cell's detection method of counter opal structure hydrogel and its application |
CN107876038A (en) * | 2017-11-29 | 2018-04-06 | 青岛农业大学 | A kind of counter opal TiO of Ag inductions2The preparation method of homojunction photochemical catalyst |
CN107876038B (en) * | 2017-11-29 | 2020-03-17 | 青岛农业大学 | Ag-induced inverse opal TiO2Preparation method of homojunction photocatalyst |
CN113737281A (en) * | 2021-08-31 | 2021-12-03 | 武汉理工大学 | Oxide spherical photonic crystal with inverse opal structure, simple preparation method and application thereof |
CN113737281B (en) * | 2021-08-31 | 2024-04-26 | 武汉理工大学 | Oxide spherical photonic crystal with inverse opal structure, simple preparation method and application thereof |
CN114113051A (en) * | 2021-12-16 | 2022-03-01 | 南京信息工程大学 | Preparation method and application of PSMA (patterned sapphire substrate) electrochemiluminescence sensor |
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