CN107829143A - The preparation method of counter opal structure silver sulfide photonic crystal - Google Patents
The preparation method of counter opal structure silver sulfide photonic crystal Download PDFInfo
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- CN107829143A CN107829143A CN201711377664.XA CN201711377664A CN107829143A CN 107829143 A CN107829143 A CN 107829143A CN 201711377664 A CN201711377664 A CN 201711377664A CN 107829143 A CN107829143 A CN 107829143A
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- photonic crystal
- silver sulfide
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- opal structure
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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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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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
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
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Abstract
The present invention relates to the preparation of feature counter opal structure silver sulfide photonic crystal.A kind of preparation method of counter opal structure silver sulfide photonic crystal, the preparation method is to assemble photonic crystal template using vertical sedimentation by raw material of the polystyrene microsphere containing silver sulfide quantum dot, and the silver sulfide photonic crystal of counter opal structure is then prepared using sacrifice template method.The present invention prepares the counter opal structure silver sulfide photonic crystal of different band gap by sacrificing template method using photonic crystal of opals structure as template.With purple light excited silver sulfide photonic crystal, the red fluorescence of various luster can be sent.Method of the invention is simple to operate, cost is cheap, is adapted to the extensive counter opal structure silver sulfide photonic crystal for preparing and having photon band gap modulating performance.
Description
Technical field
The present invention relates to the preparation of feature counter opal structure silver sulfide photonic crystal.
Background technology
Photonic crystal refers to what the different material of dielectric constant (refractive index) was arranged to make up in space periodicity.Photonic crystal
It is most essential to be characterized in forbidden photon band and photon local.Forbidden photon band can control the propagation of light wherein, and defect state
The property of forbidden photon band can be influenceed by introducing, and be that photoelectricity is integrated, integreted phontonics, a kind of key basic material of optic communication.
In recent years, with regulation and control of the people to semi-conducting material microscopic dimensions and surface modification, the silver sulfide amount prepared
It is sub-, higher fluorescence intensity be present near infrared region.Silver sulfide quantum dot has following common advantageous property：Silver sulfide amount
Son point preparation method is simple, and raw material is easy to get, so that production cost substantially reduces；It has good biocompatibility and low toxicity
Property, it can be applied in imaging biological cells with reference to its good luminosity；On the whole, silver sulfide quantum dot is related in the energy
Device, environmental correclation application, biological association area and composite association area.
Silver sulfide quantum dot and photonic crystal are combined, silver sulfide quantum dot is transformed into the solid-state of periodic structure, more
Be advantageous to post-process.Different periodic structures has different photon band gaps.Silver sulfide quantum dot as a kind of photoelectric material,
With the property that regulation and control light is just provided with after photon band gap.Silver sulfide quantum dot and photonic crystal are combined and prepare different band gap
Silver sulfide quantum dot photonic crystal, not only inherit the original advantageous property of silver sulfide quantum dot well, while pass through light
The regulation and control of sub- crystal bandgap, silver sulfide quantum dot photonic crystal is set to show the property more excellent compared to silver sulfide quantum dot
Matter, such as the enhancing of fluorescence property, strengthen electron transfer efficiency in photoelectrochemical process etc..
The content of the invention
It is an object of the invention to provide a kind of preparation method of counter opal structure silver sulfide photonic crystal, with it is quick,
Efficiently, counter opal structure silver sulfide photonic crystal is synthesized in large area.
To reach above-mentioned purpose, the present invention provides following technical scheme：A kind of counter opal structure silver sulfide photonic crystal
Preparation method, the preparation method is uses vertical sedimentation by raw material of the polystyrene microsphere containing silver sulfide quantum dot
Photonic crystal template is assembled, the silver sulfide photonic crystal of counter opal structure is then prepared using sacrifice template method；Specific steps
For：
(1) polystyrene microsphere is assembled into photonic crystal template by vertical sedimentation in climatic chamber；
(2) the photonic crystal template is handled into 20-120s with plasma technique；
(3) silver sulfide quantum dot solution is uniformly added drop-wise to photonic crystal template surface；The silver sulfide Quantum Solution
Percent by volume is 20-80%；Solvent in the silver sulfide quantum dot solution is ethanol or ethyl acetate；
(4) the photonic crystal template after dropwise addition silver sulfide quantum dot solution is placed on cold compartment of refrigerator 1-6h；
(5) 8-30h in 50-80 DEG C of baking oven is positioned over after；
(6) the photonic crystal template is dissolved with tetrahydrofuran immersion, obtains the sulphur of the counter opal structure of different band gap
Change silver-colored layer of photonic crystals.
Further, the method that emulsion polymerization is taken in the preparation of the polystyrene microsphere, specific preparation method are：80-
The methyl methacrylate of 0.8-1.2 mass parts, the acrylic acid and 17-21 matter of 0.8-1.2 mass parts are added in 100 parts by volume water
The styrene of part is measured, then adds emulsifying agent neopelex 0-0.004 mass parts and 0.5-0.55 mass parts buffering
Agent sodium acid carbonate obtains reaction solution；The reaction solution is kept into for 0.5-2 hours at 60-80 DEG C, then adds 0.45-0.5 mass
Part ammonium persulfate aqueous solution, react 10-15h in 70-90 DEG C under continuous stirring condition, centrifuge and can obtain the polyphenyl
Ethene microballoon.Polystyrene microsphere has core shell structure, using polystyrene as core, with poly- (acrylic acid-methacrylic acid methyl esters)
For shell.Microballoon with soft shell stone in an assembling process, is more beneficial for being closely spaced, so as to form the photon of better quality
Crystal film.Otherwise, crystal film with photon arrangement is not close, so as to influence the preparation matter of counter opal structure silver sulfide photonic crystal
Amount.The particle size range that polystyrene microsphere is made is 150-300nm., can group using the polystyrene microsphere of the particle size range
The crystal film with photon of different band gap in visible-range is dressed up, so as to prepare the counter opal structure silver sulfide photon of different band gap
Crystal.The particle diameter of microballoon is excessive or too small, is not only difficult to assemble, and the band gap that will also result in the crystal film with photon of assembling does not conform to
It is suitable.
Further, in step (1), polystyrene microsphere is dispersed in water obtained polystyrene microsphere emulsion, and it is dilute
Release to translucent；Then super hydrophilic solid substrate is vertically placed in the polystyrene microsphere emulsion, it is permanent at 20-80 DEG C
Temperature, constant humidity under 20-80% humidity, to the emulsion evaporating completely, the polystyrene microsphere can solid substrate surface from
It is assembled into photonic crystal template.
Further, super hydrophilic solid substrate refers to water and solid substrate of the contact angle on solid substrate surface less than 10 °.
Solid substrate is selected from simple glass, quartz plate or silicon chip.Using super hydrophilic solid substrate, be advantageous to polystyrene microsphere at it
Crystal film with photon of the surface-assembled into high quality.So as to be advantageous to the preparation of counter opal structure silver sulfide photonic crystal.
Further, silver sulfide layer of photonic crystals thickness is prepared as 2-5 μm, and the fluorescence for alloing to be excited passes through.
The beneficial effects of the present invention are：The present invention is using photonic crystal of opals structure as template, by sacrificing template
Prepare the counter opal structure silver sulfide photonic crystal of different band gap.With purple light excited silver sulfide photonic crystal, difference can be sent
The red fluorescence of gloss.Method of the invention is simple to operate, cost is cheap, is adapted to extensive prepare to have photon band gap modularity
The counter opal structure silver sulfide photonic crystal of energy.
Described above is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, described in detail below with presently preferred embodiments of the present invention as after.
Embodiment
With reference to embodiment, the embodiment of the present invention is described in further detail.Following examples are used for
Illustrate the present invention, but be not limited to the scope of the present invention.
Embodiment 1
1. the preparation of core shell structure polystyrene microsphere
The methyl methacrylate of 1.2 mass parts, the acrylic acid of 0.8 mass parts and 17 mass parts are added in 90 mass parts water
Styrene, then add 0.002 mass parts emulsifying agent neopelex, and 0.50 mass parts buffer sodium acid carbonate
Obtain reaction solution；Reaction solution is kept at 70 DEG C 1 hour, the ammonium persulfate aqueous solution of 0.50 mass parts is then added, continuously stirs
12h is reacted in 80 DEG C, you can it is 150-300nm polystyrene microspheres that the particle diameter with core shell structure, which is prepared, under the conditions of mixing.
2. the preparation of photonic crystal template
Polystyrene microsphere emulsion obtained above is poured into small beaker, super hydrophilic solid substrate is vertically placed on dress
In the small beaker for having certain density polystyrene emulsion, (temperature is positioned in climatic chamber：20 DEG C, humidity：60%),
Treat the dry photonic crystal template for becoming band gap in 400-800nm or so of emulsion evaporating completely.
3. the preparation of counter opal structure silver sulfide photonic crystal
(1) photonic crystal template of the band gap in 400-800nm is handled into 60s with plasma；
(2) by silver sulfide solution (the pure silver sulfide of volume ratio：Ethanol=1:1) uniformly it is added drop-wise to photonic crystal template table
Face；
(3) it is placed on cold compartment of refrigerator 3h；
(4) it is positioned over 24h in 80 DEG C of baking oven；
(5) dissolving photonic crystal template is soaked with tetrahydrofuran, obtains the counter opal knot of different band gap (400-800nm)
The silver sulfide photonic crystal of structure, through the purple light excited red fluorescence for sending different color and lusters.
Each technical characteristic of embodiment described above can be combined arbitrarily, to make description succinct, not to above-mentioned reality
Apply all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, the scope that this specification is recorded all is considered to be.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Can not therefore it be construed as limiting the scope of the patent.It should be pointed out that come for one of ordinary skill in the art
Say, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (5)
- A kind of 1. preparation method of counter opal structure silver sulfide photonic crystal, it is characterised in that including：(1) polystyrene microsphere is assembled into photonic crystal template by vertical sedimentation in climatic chamber；(2) the photonic crystal template is handled into 20-120s with plasma technique；(3) silver sulfide quantum dot solution is uniformly added drop-wise to photonic crystal template surface；The volume of the silver sulfide Quantum Solution Percentage is 20-80%；Solvent in the silver sulfide quantum dot solution is ethanol or ethyl acetate；(4) the photonic crystal template after dropwise addition silver sulfide quantum dot solution is placed on cold compartment of refrigerator 1-6h；(5) 8-30h in 50-80 DEG C of baking oven is positioned over after；(6) the photonic crystal template is dissolved with tetrahydrofuran immersion, obtains the silver sulfide of the counter opal structure of different band gap Layer of photonic crystals.
- 2. preparation method according to claim 1, it is characterised in that in the step (1), the preparation of the polystyrene microsphere The method for taking emulsion polymerization, including：The methyl methacrylate of 0.8-1.2 mass parts is added in 80-100 parts by volume water, The acrylic acid of 0.8-1.2 mass parts and the styrene of 17-21 mass parts, then add emulsifying agent neopelex 0- 0.004 mass parts and 0.5-0.55 mass parts buffer sodium acid carbonates obtain reaction solution；The reaction solution is kept at 60-80 DEG C 0.5-2h, the ammonium persulfate aqueous solution of 0.45-0.5 mass parts is then added, react 10- in 70-90 DEG C under continuous stirring condition 15h, centrifuge and can obtain the polystyrene microsphere.
- 3. preparation method according to claim 2, it is characterised in that the step (1) includes, and the polystyrene is micro- Ball is dispersed in water obtained polystyrene microsphere emulsion, and is diluted to translucent；Then super hydrophilic solid substrate is placed vertically In the polystyrene microsphere emulsion, constant temperature at 20-80 DEG C, constant humidity under 20-80% is described to the emulsion evaporating completely Polystyrene microsphere can be in solid substrate surface self-organization into crystal film with photon.
- 4. preparation method according to claim 3, it is characterised in that the super hydrophilic solid substrate refers to water and solid-based The contact angle on material surface is less than 10 ° of solid substrate.
- 5. preparation method according to claim 1, it is characterised in that in the step (6), prepare the silver sulfide photon Crystal layer thickness is 2-5 μm, and the fluorescence for alloing to be excited passes through.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113567432A (en) * | 2021-07-30 | 2021-10-29 | 吉林大学 | Sensitive element imitating butterfly wing scale pit structure, preparation method and humidity sensor |
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|---|---|---|---|---|
| CN102409403A (en) * | 2011-11-14 | 2012-04-11 | 中国科学院化学研究所 | Preparation method of self-supporting monocrystal photonic crystal |
| CN102433588A (en) * | 2010-09-29 | 2012-05-02 | 中国科学院化学研究所 | Preparation method of crack-free optical crystal |
| CN105525343A (en) * | 2015-12-18 | 2016-04-27 | 中国科学院理化技术研究所 | Preparation method and application of carbon dot photonic crystal having opal structure or inverse opal structure |
| CN106381520A (en) * | 2016-08-29 | 2017-02-08 | 浙江理工大学 | Method for preparing photonic crystal with inverse opal structure through ultraviolet radiation |
-
2017
- 2017-12-19 CN CN201711377664.XA patent/CN107829143A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102433588A (en) * | 2010-09-29 | 2012-05-02 | 中国科学院化学研究所 | Preparation method of crack-free optical crystal |
| CN102409403A (en) * | 2011-11-14 | 2012-04-11 | 中国科学院化学研究所 | Preparation method of self-supporting monocrystal photonic crystal |
| CN105525343A (en) * | 2015-12-18 | 2016-04-27 | 中国科学院理化技术研究所 | Preparation method and application of carbon dot photonic crystal having opal structure or inverse opal structure |
| CN106381520A (en) * | 2016-08-29 | 2017-02-08 | 浙江理工大学 | Method for preparing photonic crystal with inverse opal structure through ultraviolet radiation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113567432A (en) * | 2021-07-30 | 2021-10-29 | 吉林大学 | Sensitive element imitating butterfly wing scale pit structure, preparation method and humidity sensor |
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Application publication date: 20180323 |