CN108441962A - The preparation method of opal structural silver sulfide photonic crystal - Google Patents
The preparation method of opal structural silver sulfide photonic crystal Download PDFInfo
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- CN108441962A CN108441962A CN201711378718.4A CN201711378718A CN108441962A CN 108441962 A CN108441962 A CN 108441962A CN 201711378718 A CN201711378718 A CN 201711378718A CN 108441962 A CN108441962 A CN 108441962A
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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 preparations of functional protein stone structure silver sulfide photonic crystal.The preparation method of a kind of opal structural silver sulfide photonic crystal of the present invention, which is characterized in that the silver sulfide photonic crystal that opal structural is made in microsphere template is assembled by vertical sedimentation；Wherein, with polystyrene microsphere for the microsphere template, after being assembled into photonic crystal using vertical sedimentation, silver sulfide quantum dot solution is added dropwise in the photon crystal surface, the silver sulfide photonic crystal of the opal structural is made after solidification；Alternatively, with the silicon dioxide microsphere containing silver sulfide quantum dot for the microsphere template, the silver sulfide photonic crystal of the opal structural is then assembled into using vertical sedimentation.The present invention is prepared for the opal structural silver sulfide photonic crystal with tuneable photonic band gap.Method extensive opal structural silver sulfide photonic crystal of the preparation with photon band gap modulating performance easy to operate, of low cost, suitable of the present invention.
Description
Technical field
The present invention relates to the preparations of functional protein stone structure silver sulfide photonic crystal.
Background technology
Photonic crystal refers to that the different material of dielectric constant (refractive index) is 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 influenced by introducing, be integrated photoelectricity, integreted phontonics, optic communication a kind of key basic material.
In recent years, the regulation and control with people to semi-conducting material microscopic dimensions and surface modification, the vulcanization silver content prepared
Sub-, near infrared region, there are higher fluorescence intensities.Silver sulfide quantum dot has following common advantageous property：Vulcanize silver content
Son point preparation method is simple, and raw material is easy to get, to make production cost substantially reduce；It is with good biocompatibility and low toxicity
Property, it can be applied in imaging biological cells in conjunction with its good luminosity；On the whole, silver sulfide quantum dot is in energy correlation
Device, environmental correclation application, biological related field and composite material related field.
Silver sulfide quantum dot and photonic crystal are combined, so that silver sulfide quantum dot is transformed into the solid-state of periodic structure, more
Be conducive to post-process.Different periodic structures has different photon band gaps.Silver sulfide quantum dot as a kind of photoelectric material,
With the property for being just provided with regulation and control light 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 passing through light
The regulation and control of sub- crystal bandgap make silver sulfide quantum dot photonic crystal show the property more excellent compared to silver sulfide quantum dot
Matter enhances the electron transfer efficiency etc. in photoelectrochemical process such as the enhancing of fluorescence property.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of opal structural silver sulfide photonic crystal, fast to meet
Speed, efficient, large area prepare the demand of opal structural silver sulfide photonic crystal.
In order to achieve the above objectives, the present invention provides the following technical solutions：A kind of opal structural silver sulfide photon
The preparation method of crystal, which is characterized in that microsphere template is assembled by vertical sedimentation, opal structural is made
Silver sulfide photonic crystal；Wherein, using polystyrene microsphere as microsphere template, after being assembled into photonic crystal using vertical sedimentation,
Silver sulfide quantum dot solution is added dropwise in photon crystal surface, the silver sulfide photonic crystal of opal structural is made after solidification；Alternatively,
Using the silicon dioxide microsphere containing silver sulfide quantum dot as microsphere template, opal structural is then assembled into using vertical sedimentation
Silver sulfide photonic crystal.
Further, using polystyrene microsphere as template, include the following steps：
(1) polystyrene microsphere template is assembled into photonic crystal by vertical sedimentation in climatic chamber
Layer；
(2) layer of photonic crystals plasma technique is handled into 20-120s；
(3) silver sulfide quantum dot solution is dropped evenly into photonic crystal layer surface；The volume hundred of silver sulfide Quantum Solution
Divide than being 20-80%, the solvent in silver sulfide quantum dot solution is ethyl alcohol or ethyl acetate；
(4) layer of photonic crystals after dropwise addition silver sulfide quantum dot solution is placed on cold compartment of refrigerator 1-6h；
(5) after by the layer of photonic crystals be positioned in 50-80 DEG C of baking oven 8-30h solidifications to get.
Further, the method that emulsion polymerization is taken in the preparation of the polystyrene microsphere template, specific preparation method are：
The methyl methacrylate of 0.8-1.2 mass parts, the acrylic acid and 17- of 0.8-1.2 mass parts are added in 80-100 parts by volume water
Emulsifier neopelex 0-0.004 mass parts and 0.5-0.55 mass parts are then added in the styrene of 21 mass parts
Buffer sodium bicarbonate obtains reaction solution；The reaction solution is kept at 60-80 DEG C 0.5-2 hours, 0.45-0.5 is then added
The ammonium persulfate aqueous solution of mass parts, 10-15h is reacted under continuous stirring condition in 70-90 DEG C, and centrifugation can be obtained described
Polystyrene microsphere template.Polystyrene microsphere obtained has nucleocapsid, using polystyrene as core, with poly- (acrylic acid-first
Base methyl acrylate) it is shell.Microballoon with soft shell stone in an assembling process, is more advantageous to and is closely spaced, to be formed
The crystal film with photon of better quality.Otherwise, crystal film with photon arrangement is not close, to influence opal structural silver sulfide photon
The preparation quality of crystal.In addition, the grain size of polystyrene microsphere obtained is 150-300nm.Utilize the polyphenyl of the particle size range
Ethylene microballoon can be assembled into the crystal film with photon of different band gap in visible-range.The grain size of microballoon is excessive or too small, no
It is only difficult to assemble, the band gap that will also result in the crystal film with photon of assembling is improper.
Further, using the silicon dioxide microsphere containing silver sulfide quantum dot as template, include the following steps：
(1) by the silicon dioxide microsphere template containing silver sulfide quantum dot by vertical sedimentation the group in climatic chamber
Dress up layer of photonic crystals；
(2) layer of photonic crystals plasma technique is handled into 20-120s；
(3) layer of photonic crystals is placed on cold compartment of refrigerator 1-6h after；
(4) and then by layer of photonic crystals be positioned in 50-80 DEG C of baking oven 8-30h solidifications to get
Further, the specific preparation method of the silicon dioxide microsphere template containing silver sulfide quantum dot is：3- will be contained
The ethanol solution of the water of 10 mass parts and the ammonia of 0.65-2 mass parts is added in reactor, is kept for 20-30 DEG C and stirred；Containing just
The ethanol solution and silver sulfide solution of silester are added in above-mentioned reactor, and the percent by volume of silver sulfide Quantum Solution is
20-80%, the solvent in silver sulfide quantum dot solution are ethyl alcohol or ethyl acetate；It is maintained at positive silicic acid in whole system simultaneously
A concentration of 0.15-0.2mol/L of ethyl ester；Stirring 2-3 hours, centrifuge washing obtain grain size and contain silver sulfide for 150-300nm
Silicon dioxide microsphere template.
Further, it is by the step of vertical sedimentation assembling microsphere template：The microsphere template is dispersed in water
Microsphere template dispersion liquid is made, and is diluted to translucent；Then super hydrophilic solid substrate is vertically placed on the microsphere template
In dispersion liquid, constant temperature at 20-80 DEG C, constant humidity under 20-80%, until the dispersion liquid evaporating completely, the microsphere template can be
Solid substrate surface self-organization is at crystal film with photon.
Further, super hydrophilic solid substrate refers to the solid substrate that water is less than 10 ° with the contact angle on solid substrate surface.
Further, the silver sulfide photonic crystal layer thickness being prepared is 2-5 μm, keeps the fluorescence being excited saturating
It crosses.
The beneficial effects of the present invention are：The present invention is prepared for the opal structural silver sulfide light with tuneable photonic band gap
Sub- crystal is obtained with glossiness feux rouges via purple light excited.The method big rule easy to operate, of low cost, suitable of the present invention
Mould prepares the opal structural silver sulfide photonic crystal with photon band gap modulating performance.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, it is described in detail as after with presently preferred embodiments of the present invention below.
Specific implementation mode
With reference to embodiment, the embodiment of the present invention is furthur described in detail.Following embodiment is used for
Illustrate the present invention, but is not limited to the scope of the present invention.
Embodiment 1
(1) polystyrene microsphere is prepared
The methyl methacrylate of 1.2 mass parts, the acrylic acid of 1 mass parts and 16.8 mass parts are added in 90 mass parts water
Styrene, then be added 0.002 mass parts emulsifier neopelex, 0.50 mass parts buffer sodium bicarbonate,
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 the 150-300nm polystyrene microspheres of nucleocapsid are prepared under the conditions of mixing.
(2) polystyrene microsphere is dispersed in water obtained dispersion liquid, and be diluted to translucent；Then sheet glass is vertical
It is positioned in above-mentioned dispersion liquid, keeps 20 DEG C of constant temperature, 60% constant humidity, until dispersion liquid evaporating completely, polystyrene microsphere is in glass
Surface self-organization is at layer of photonic crystals.
(3) layer of photonic crystals plasma technique is handled into 20-120s；
(4) by silver sulfide quantum dot solution (the pure silver sulfide of volume ratio：Ethyl alcohol=1:1) uniformly it is added drop-wise to layer of photonic crystals
Surface.
(5) layer of photonic crystals after dropwise addition silver sulfide quantum dot solution is placed on cold compartment of refrigerator 1-6h；
(6) layer of photonic crystals is positioned in 50-80 DEG C of baking oven after 8-30h solidifications to get.
Embodiment 2
(1) silicon dioxide microsphere containing silver sulfide quantum dot is prepared
The ethanol solution of water containing 10mol and 2mol ammonia is added in reactor, kept for 25 DEG C and is stirred；Contain positive silicon
Ethanol solution and silver sulfide quantum dot solution (the pure silver sulfide of volume ratio of acetoacetic ester：Ethyl alcohol=1:1) it is added to immediately above-mentioned anti-
The concentration answered in device, while being maintained at ethyl orthosilicate in synthetic system is 0.22mol/L；Mixed system stirs 2-3 hours；Instead
Suspension after answering is centrifuged and is washed with deionized for several times, and it is 150-300nm Containing Sulfur silver quantum dots that grain size, which is prepared,
Silicon dioxide microsphere.
(2) above-mentioned silicon dioxide microsphere is dispersed in water obtained dispersion liquid, and be diluted to translucent；Then by sheet glass
It is vertically placed in above-mentioned dispersion liquid, keeps 20 DEG C of constant temperature, 60% constant humidity, until dispersion liquid evaporating completely, the dioxy of Containing Sulfur silver
SiClx microballoon is self-assembled into layer of photonic crystals in glass surface.
(3) layer of photonic crystals plasma technique is handled into 20-120s；
(4) layer of photonic crystals is placed on cold compartment of refrigerator 1-6h after；
(5) and then by layer of photonic crystals be positioned in 50-80 DEG C of baking oven 8-30h solidifications to get
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies 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, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, 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
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (8)
1. a kind of preparation method of opal structural silver sulfide photonic crystal, which is characterized in that assembled by vertical sedimentation micro-
The silver sulfide photonic crystal of opal structural is made in ball template；Wherein, with polystyrene microsphere for the microsphere template, using perpendicular
After straight sedimentation is assembled into photonic crystal, silver sulfide quantum dot solution is added dropwise in the photon crystal surface, institute is made after solidification
State the silver sulfide photonic crystal of opal structural；Alternatively, with the silicon dioxide microsphere containing silver sulfide quantum dot for the microballoon
Then template is assembled into the silver sulfide photonic crystal of the opal structural using vertical sedimentation.
2. preparation method according to claim 1, which is characterized in that including：
(1) polystyrene microsphere template is assembled into layer of photonic crystals by vertical sedimentation in climatic chamber；
(2) layer of photonic crystals plasma technique is handled into 20-120s；
(3) silver sulfide quantum dot solution is dropped evenly into the photonic crystal layer surface；The body of the silver sulfide Quantum Solution
Product percentage is 20-80%, and the solvent in the silver sulfide quantum dot solution is ethyl alcohol or ethyl acetate；
(4) layer of photonic crystals after the dropwise addition silver sulfide quantum dot solution is placed on cold compartment of refrigerator 1-6h；
(5) after by the layer of photonic crystals be positioned in 50-80 DEG C of baking oven 8-30h solidifications to get.
3. preparation method according to claim 2, which is characterized in that in the step (1), the polystyrene microsphere mould
The method that emulsion polymerization is taken in the preparation of plate, specific preparation method are：0.8-1.2 mass parts are added in 80-100 parts by volume water
Emulsifier 12 is then added in methyl methacrylate, the styrene of the acrylic acid and 17-21 mass parts of 0.8-1.2 mass parts
Sodium alkyl benzene sulfonate 0-0.004 mass parts and 0.5-0.55 mass parts buffer sodium bicarbonates obtain reaction solution；By the reaction
Liquid is kept at 60-80 DEG C 0.5-2 hours, and the ammonium persulfate aqueous solution of 0.45-0.5 mass parts, continuous stirring condition is then added
Under in 70-90 DEG C react 10-15h, centrifugation can be obtained the polystyrene microsphere template.
4. preparation method according to claim 1, which is characterized in that include the following steps：
(1) by described the silicon dioxide microsphere template containing silver sulfide quantum dot by vertical sedimentation the group in climatic chamber
Dress up layer of photonic crystals；
(2) layer of photonic crystals plasma technique is handled into 20-120s；
(3) layer of photonic crystals is placed on cold compartment of refrigerator 1-6h after；
(4) then by the layer of photonic crystals be positioned in 50-80 DEG C of baking oven 8-30h solidifications to get
5. wanting the preparation method described in 4 according to right, which is characterized in that the silicon dioxide microsphere containing silver sulfide quantum dot
The specific preparation method of template is：The ethanol solution of water containing 3-10 mass parts and the ammonia of 0.65-2 mass parts is added to reaction
In device, is kept for 20-30 DEG C and stirred；Ethanol solution containing ethyl orthosilicate and silver sulfide solution are added to above-mentioned reactor
In, the percent by volume of the silver sulfide Quantum Solution is 20-80%, and the solvent in the silver sulfide quantum dot solution is ethyl alcohol
Or ethyl acetate；It is maintained at a concentration of 0.15-0.2mol/L of ethyl orthosilicate in whole system simultaneously；Stirring 2-3 hours,
Centrifuge washing obtains the silicon dioxide microsphere template containing silver sulfide.
6. according to claim 2 or 4 any one of them preparation methods, which is characterized in that, will be described micro- in the step (1)
Ball template is dispersed in water obtained microsphere template dispersion liquid, and is diluted to translucent；Then super hydrophilic solid substrate is put vertically
It is placed in the microsphere template dispersion liquid, constant temperature at 20-80 DEG C, constant humidity under 20-80%, until the dispersion liquid evaporating completely, institute
Stating microsphere template can be in solid substrate surface self-organization at crystal film with photon.
7. wanting 6 or the preparation method according to right, which is characterized 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.
8. wanting 2 or 4 any one of them preparation methods according to right, which is characterized in that prepare the silver sulfide layer of photonic crystals
Thickness is 2-5 μm, and the fluorescence being excited is allow to penetrate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116970387A (en) * | 2023-07-25 | 2023-10-31 | 南京邮电大学 | Composite nano material for detecting hydrolyzed milk powder and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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2017
- 2017-12-19 CN CN201711378718.4A patent/CN108441962A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116970387A (en) * | 2023-07-25 | 2023-10-31 | 南京邮电大学 | Composite nano material for detecting hydrolyzed milk powder and preparation method and application thereof |
| CN116970387B (en) * | 2023-07-25 | 2024-05-10 | 南京邮电大学 | Composite nano material for detecting hydrolyzed milk powder and preparation method and application thereof |
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Application publication date: 20180824 |