CN107699953A - A kind of method for using modified silk albumen to prepare polystyrene inverse opal photonic crystal for filling liquid - Google Patents
A kind of method for using modified silk albumen to prepare polystyrene inverse opal photonic crystal for filling liquid Download PDFInfo
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- CN107699953A CN107699953A CN201710821014.3A CN201710821014A CN107699953A CN 107699953 A CN107699953 A CN 107699953A CN 201710821014 A CN201710821014 A CN 201710821014A CN 107699953 A CN107699953 A CN 107699953A
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- photonic crystal
- polystyrene
- inverse opal
- filling liquid
- opal photonic
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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
- C30B29/54—Organic compounds
- C30B29/58—Macromolecular 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
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/002—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials
- G02B1/005—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of materials engineered to provide properties not available in nature, e.g. metamaterials made of photonic crystals or photonic band gap materials
Abstract
The invention belongs to photonic crystal technical field, and in particular to a kind of method for using modified silk albumen to prepare polystyrene inverse opal photonic crystal for filling liquid.Technical scheme mainly includes：Degumming twice, a salt solution, and flowing water dialysis 72h are carried out to silk cocoon layer, after dialysis, is modified using glutaraldehyde as crosslinking agent.Monodisperse polystyrene nanoparticle polymer emulsion is prepared with the method for emulsifier-free emulsion polymerization, it is self-assembly of colloidal photon crystal, the photonic crystal space of nanoparticle formation is filled with using modified silk albumen as filling liquid afterwards, taken off after natural evaporation, it is immersed in tetrahydrofuran and removes diameter polystyrene spheres, polystyrene inverse opal photonic crystal is made.It is biomedical that the present invention uses modified silk albumen to be used as polystyrene inverse opal photonic crystal prepared by filling liquid, a kind of very valuable biomaterial in the application field such as bio-photon or electronics, has a good application prospect.
Description
Technical field
Modified silk albumen is used to prepare polystyrene inverse opal photonic crystal for filling liquid the present invention relates to a kind of
Method, belong to photonic crystal technical field.
Background technology
Photonic crystal is the material regular interval arrangement form of two kinds of differing dielectric constants, has selectivity anti-for light
Penetrate.Form material organic/inorganic substance, high-molecular organic material of photonic crystal etc..Photonic crystal can be by controlling different lattices
Constant carrys out the color of control structure, can also penetrate into structure by using different (being usually liquid) fillers and produce change.Silk
Albumen is the albumen extracted from silk fiber, has non-toxic, nonirritant, good breathable moisture permeability and excellent biology
The advantages that compatibility.In biological technical field, fibroin film can as immobilised enzymes carrier and prepare biology sensor.But
Film prepared by fibroin solutions is soluble in water, is difficult to apply to most of fields, application has limitation.
The content of the invention
The purpose of the present invention is to prepare polystyrene inverse opal photonic crystal by filling liquid of modified silk albumen.This hair
The polystyrene inverse opal photonic crystal of bright preparation preserves, safety easy to carry, and Production Time is short, and application value is big, prospect
Preferably.
The purpose of the present invention is achieved by the following technical programs：One kind uses modified silk albumen to be prepared for filling liquid
The method of polystyrene inverse opal photonic crystal, comprises the following steps：
(1) extraction of fibroin：Degumming twice, a salt solution, and flowing water dialysis 72h are carried out to silk cocoon layer, is obtained
Volumetric concentration is 6.0%-8.0% fibroin solutions, volumetric concentration then is diluted into 1.8%-2.2%, after dilution
Fibroin solutions stored at 2-8 DEG C；
(2) modification of fibroin：To step (1) prepare fibroin solutions in add its volume 0.25%~
0.5% glutaraldehyde cross-linking agent is modified, and obtains modified silk albumen；
(3) preparation of polystyrene colloid crystal：
S1 prepares Monodispersity polystyrene nanosphere polymer emulsion using the method for emulsifier-free emulsion polymerization, nanosphere it is straight
Footpath is 200~500nm；
S2 prepares the polystyrene colloid of high-sequential using sheet glass as substrate by natural evaporation solvent self-assembling method
Crystal；
(4) preparation of polystyrene inverse opal photonic crystal：Step (2) is added dropwise on polystyrene colloid crystal to prepare
Modified silk protein solution, naturally osmotic, air-dry after film is taken off；The film of gained is immersed into tetrahydrofuran and removes polyphenyl second
Alkene nanosphere body, film is then taken out with natural evaporation tetrahydrofuran, obtains polystyrene inverse opal photonic crystal.
Further, 0.5wt% Carbon Dioxide sodium solutions are used in described scouring processes, are used in salt solution preocess
50wt% anhydrous calcium chloride solution.
Further, described usually time is 30min.
Further, the described salt solution time is 5min.
Further, the glass flake substrate is handled by order below：The first step is in acetone soln at ultrasonic wave
Manage 30min；Second step ultrasonication 30min in ethanol solution；3rd step ultrasonication 1h in prianha solution,
Described prianha solution is the 98wt% concentrated sulfuric acids and hydrogen peroxide according to volume ratio 3：1 is mixed；4th step is in deionized water
Ultrasonication 30min, is dried with lens wiping paper.
Further, the time in described step (3) needed for natural evaporation solvent self assembly is 3h.
Further, modified silk protein solution naturally osmotic and air-dried required time are 3h in described step (4).
Further, film is immersed into tetrahydrofuran in the step (4) and removes polystyrene nanospheres body, then taken out
Film is with natural evaporation tetrahydrofuran, required time 4h.
Beneficial effects of the present invention are as follows：
(1) preparation method used in the present invention relative to traditional polystyrene inverse opal photonic crystal preparation side
Preparation time is shortened for method, it is simple to operate and repeated preferable.Traditional Method needs 2-3 week just to prepare one,
And method used in the present invention can be prepared in batches in 5-8h.
(2) the filling solution selected in the present invention is the natural silk egg of the Economical Purification extracted from silk fiber
In vain, glutaraldehyde is added according still further to volume ratio 0.25%-0.5% to be modified in fibroin solutions.Modified silk egg
White solution is not readily dissolved in water in preparation film forming phase than unmodified fibroin, can be used for the detection of water-soluble substances.Pass
System technique not only more difficult control of the concentration of fibroin solutions in preparation process, it is all difficult to prepare that concentration is too low or too high
Go out regularly arranged polystyrene spheres, instant invention overcomes the change in concentration of the modified silk protein solution in preparation process to knot
The harmful effect of fruit, and obtain suitable modified silk protein concentration scope 1.8vt%-2.2vt%.In addition, glutaraldehyde is dense
Spend height can cause film its colour changed into yellow become fragile it is frangible be not easy to peel and elute polystyrene spheres be more difficult to relative to unmodified
Elution, the present invention are anti-in 0.25%-0.5%, obtained polystyrene by the control of the volume ratio of glutaraldehyde and modified silk albumen
It is opal photonic crystal steady quality, non-breakable and not soluble in water.
(3) the modified silk albumen desciccator diaphragm prepared by the present invention is beneficial to preserve and carrying is convenient to safety, made
Time is short, preparation process is simple to operation, is not readily dissolved in water, and application field is wider for unmodified fibroin
It is general.
Brief description of the drawings
Fig. 1 is the preparation flow figure of polystyrene inverse opal photonic crystal；
Fig. 2 is the polystyrene colloid crystallogram that the present invention is prepared；
Fig. 3 is the polystyrene inverse opal photonic crystal photo that THF of the present invention soaked gained；
Fig. 4 is polystyrene inverse opal photonic crystal electron microscope.
Embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not with any shape
Formula is limited to embodiment content.Test method described in embodiment is conventional method unless otherwise specified；Such as without special theory
It is bright, the reagent and biomaterial, commercially obtain.
Embodiment 1
The extraction of fibroin
(1) 0.5wt% Carbon Dioxide sodium solution 300ml is prepared, is boiled, 9.0g silk cocoons layer is put into and carries out first time degumming
30min, the endless bright silk albumen that will be obtained, 1h is dried after wringing out at 55 DEG C.
(2) second of complete degumming process is carried out according to the method for first time degumming, obtains the fibroin of complete degumming,
It is standby to dry 1h after wringing out at 55 DEG C again.
(3) 50wt% anhydrous calcium chloride solution 40ml is prepared, boils, is put into the drying fibroin of complete degumming, it is molten
Solution, boils 5min, the fibroin of complete degumming is become solution.
(4) obtained solution is transferred in bag filter, flowing water dialysis 72h, is finally 7% by obtained volumetric concentration
Fibroin solutions are diluted to obtain the fibroin solutions that volumetric concentration is 2.0%, deposit in refrigerator 4 DEG C it is fresh-keeping.
Embodiment 2
The glutaraldehyde cross-linking agent that its volume 0.25% is added in the fibroin solutions prepared to step (1) is modified,
Obtain modified silk albumen.
Embodiment 3
The preparation of PS colloids
(1) chromic acid lotion immersion used in glass apparatus 6h, running water rinse, 2vt% hydrofluoric acid clean, finally according to
It is secondary to be respectively washed three to five times with distilled water and ethanol.
(2) polymerisation is carried out in round bottom three-necked bottle：Monomer styrene and deionized water are first entered into reaction bulb, magnetic
Logical nitrogen flooding oxygen 15min under the stirring of power agitator, is then warming up to 70 DEG C, and initiator persulfuric acid is added after reaching equalized temperature
Potassium, under nitrogen protection constant temperature polymerization 12h.Room temperature is cooled to, obtains polymer emulsion.
(3) polymer emulsion 300nm apertures miillpore filter Purification by suction filtration, washed repeatedly with distilled water in purge process,
It is standby by being preserved in liquid form respectively after obtained colloidal solid again ultrasonic disperse when the electrical conductivity of filtrate no longer changes
With.
(4) processing of 2.5x × 2.5cm sheet glass (silicon chip)：The first step, the ultrasonication 30min in acetone soln；
Second step, the ultrasonication 30min in ethanol solution；3rd step, the ultrasonication 1h in prianha solution；Pay attention to mixed
Hydrogen peroxide is slowly added to the concentrated sulfuric acid during conjunction, side stirring just adds；4th step, last deionized water ultrasonication 30min, use
Lens wiping paper is dried stand-by.
(5) the PS emulsions of 1.0ml preparations are dripped on treated 2.5 × 2.5cm sheet glass, and natural evaporation is assembled in closed
3h is carried out under room temperature condition, as shown in Figure 2.
Embodiment 4
The preparation of polystyrene inverse opal photonic crystal
(1) the modified silk albumen of volumetric concentration 2.0% is added dropwise on prepared PS colloidal crystals, makes modified silk egg
White naturally osmotic is in colloidal crystal and makes solvent evaporation be assembled under the conditions of closed room temperature to carry out 3h and can take off.
(2) inverse opal film of gained is immersed in 4h in tetrahydrofuran and removes PS spheroids, then make THF at normal temperatures
Naturally volatilize, you can obtain polystyrene inverse opal photonic crystal, as shown in Figure 3.The pipe/polyhenylethylene nano prepared is micro-
Ball carries out metal spraying scanning front with ESEM, obtains scanning electron microscope (SEM) photograph, as shown in Figure 4.It can be seen that polyphenyl second prepared by this method
Alkene f inverse opal photonic crystal structures have periodic arrangement, and nanometer bulb diameter is in 200-250nm.
Embodiment 5
The preparation of polystyrene inverse opal photonic crystal
The present embodiment is in addition to the volumetric concentration of modified silk albumen is 3%, and other conditions are same as Example 4, by this
The anti-albumen photon crystal arrangement of polystyrene prepared by volumetric concentration is mixed and disorderly.
Embodiment 6
The preparation of polystyrene inverse opal photonic crystal
The glutaraldehyde that uses when in the present embodiment prepared by modified protein, the volume ratio of itself and fibroin solutions is 3%, system
Standby obtained polystyrene inverse opal photonic crystal jaundice embrittlement, it is of poor quality.
Claims (8)
1. a kind of method for using modified silk albumen to prepare polystyrene inverse opal photonic crystal for filling liquid, its feature exists
In comprising the following steps：
(1) extraction of fibroin：Degumming twice, a salt solution, and flowing water dialysis 72h are carried out to silk cocoon layer, obtains volume
Concentration is 6.0%-8.0% fibroin solutions, volumetric concentration then is diluted into 1.8%-2.2%, by the silkworm after dilution
Silk protein solution stores at 2-8 DEG C；
(2) modification of fibroin：Its volume 0.25%~0.5% is added in the fibroin solutions prepared to step (1)
Glutaraldehyde cross-linking agent is modified, and obtains modified silk albumen；
(3) preparation of polystyrene colloid crystal：
S1 prepares Monodispersity polystyrene nanosphere polymer emulsion using the method for emulsifier-free emulsion polymerization, nanosphere it is a diameter of
200~500nm；
S2 prepares the polystyrene colloid crystal of high-sequential using sheet glass as substrate by natural evaporation solvent self-assembling method；
(4) preparation of polystyrene inverse opal photonic crystal：Changing for step (2) preparation is added dropwise on polystyrene colloid crystal
Property fibroin solutions, naturally osmotic, air-dry after film is taken off；The film of gained is immersed into tetrahydrofuran removing polystyrene to receive
Rice spheroid, then takes out film with natural evaporation tetrahydrofuran, obtains polystyrene inverse opal photonic crystal.
2. modified silk albumen is used to prepare polystyrene inverse opal photonic crystal for filling liquid as claimed in claim 1
Method, it is characterised in that 0.5wt% Carbon Dioxide sodium solutions are used in described scouring processes, are used in salt solution preocess
50wt% anhydrous calcium chloride solution.
3. modified silk albumen is used to prepare polystyrene inverse opal photonic crystal for filling liquid as claimed in claim 1
Method, it is characterised in that described usually time is 30min.
4. modified silk albumen is used to prepare polystyrene inverse opal photonic crystal for filling liquid as claimed in claim 1
Method, it is characterised in that the described salt solution time is 5min.
5. modified silk albumen is used to prepare polystyrene inverse opal photonic crystal for filling liquid as claimed in claim 1
Method, it is characterised in that：The glass flake substrate is handled by order below：First step ultrasonication in acetone soln
30min；Second step ultrasonication 30min in ethanol solution；3rd step ultrasonication 1h in prianha solution, institute
The prianha solution stated is the 98wt% concentrated sulfuric acids and hydrogen peroxide according to volume ratio 3：1 is mixed；4th step surpasses in deionized water
Sonicated 30min, is dried with lens wiping paper.
6. modified silk albumen is used to prepare polystyrene inverse opal photonic crystal for filling liquid as claimed in claim 1
Method, it is characterised in that the time in described step (3) needed for natural evaporation solvent self assembly is 3h.
7. modified silk albumen is used to prepare polystyrene inverse opal photonic crystal for filling liquid as claimed in claim 1
Method, it is characterised in that modified silk protein solution naturally osmotic and air-dried required time are 3h in described step (4).
8. modified silk albumen is used to prepare polystyrene inverse opal photonic crystal for filling liquid as claimed in claim 1
Method, it is characterised in that film is immersed into tetrahydrofuran in the step (4) and removes polystyrene nanospheres body, soak time
For 4h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109943080A (en) * | 2019-04-03 | 2019-06-28 | 北京理工大学 | The preparation method of the wire protein fiber element flexible material of photonic crystal functionalization coloring |
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| CN102517651A (en) * | 2011-11-28 | 2012-06-27 | 苏州大学 | Color fixing method of natural colorful mulberry silk |
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2017
- 2017-09-13 CN CN201710821014.3A patent/CN107699953A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102517651A (en) * | 2011-11-28 | 2012-06-27 | 苏州大学 | Color fixing method of natural colorful mulberry silk |
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| 《发光学报》: ""聚乙二醇/二氧化钛一维光子晶体的制备及其性质研究"", 《发光学报》 * |
| YING YING DIAO ET AL.: ""Multiple Structural Coloring of Silk-Fibroin Photonic Crystals and Humidity-Responsive Color Sensing"", 《ADV.FUNCT.MATER.》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109943080A (en) * | 2019-04-03 | 2019-06-28 | 北京理工大学 | The preparation method of the wire protein fiber element flexible material of photonic crystal functionalization coloring |
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