CN102492300A - Preparation method of monodispersing fibroin particles and preparation method of photonic crystal - Google Patents
Preparation method of monodispersing fibroin particles and preparation method of photonic crystal Download PDFInfo
- Publication number
- CN102492300A CN102492300A CN2011104124508A CN201110412450A CN102492300A CN 102492300 A CN102492300 A CN 102492300A CN 2011104124508 A CN2011104124508 A CN 2011104124508A CN 201110412450 A CN201110412450 A CN 201110412450A CN 102492300 A CN102492300 A CN 102492300A
- Authority
- CN
- China
- Prior art keywords
- fibroin
- preparation
- disperses
- photonic crystal
- particulate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Peptides Or Proteins (AREA)
- Cosmetics (AREA)
Abstract
The invention discloses a preparation method of monodispersing fibroin particles, which includes the following steps: (a) preparing fibroin: degumming silk to obtain the fibroin; (b) preparing fibroin solution, dissolving and purifying the fibroin obtained in the step (a) to obtain the fibroin solution; (c) preparing the monodispersing fibroin particles: mixing the fibroin solution in the step (b) and inorganic salt solution evenly, processing at the low temperature, standing for at least 12 hours at the room temperature, removing liquid supernatant, and centrifugally washing sediment to obtain the monodispersing fibroin particles. The invention further discloses a preparation method of photonic crystal. Adhesion between the monodispersing fibroin particles obtained through salting out is reduced, and the particles are spherical, smooth in surfaces, good in monodispersing performance and applicable to preparation of the photonic crystal.
Description
Technical field
The invention belongs to field of nanometer technology and technical field of polymer chemistry, relate in particular to the preparation method of a kind of single fibroin particulate preparation method of dispersion and photonic crystal.
Background technology
We can see the wing of butterfly at occurring in nature; The feather of peacock all has bright dazzling; The color of riot of color, that is that photonic crystal is according to the formed material with ordered structure of some cycles series arrangement by the specific inductivity material different because their structure is natural photonic crystal in fact; The existence of photon band gap has produced schemochrome in the photonic crystal, makes us see gorgeous color.
Up to now, existing multiple brand-new photonics device based on photonic crystal is proposed in succession, comprises the laser apparatus of no threshold value; Loss-free speculum and crooked light path; The optical microcavity of high-quality-factor, low nonlinear switching and the magnifying glass that drives energy, wavelength resolution is high and ultra prism that volume is minimum; Have the photonic crystal fiber of dispersion compensation functions, and the photodiode of raising the efficiency etc.
Photonic crystal can be processed by precision optical machinery, the preparation of methods such as little processing of electronics and colloid self-assembly.Wherein, The colloid self-assembly is to prepare near infrared and the visible the easiest method of light-wave band three-D photon crystal at present; It is meant is not having structural units such as the atomic group of atom, molecule formation, supramolecule, molecular aggregate, nano particle under the situation of outside interference; Spontaneously found into the process of the aggregate of Thermodynamically stable, Stability Analysis of Structures, organization regulation through the non covalent bond effect, monodisperse silica and granules of polystyrene are the materials of the most widely used preparation photonic crystal at present.
Silk fibroin is a kind of natural macromolecular material, and it is nontoxic, harmless and do not have immunoreation, has excellent biocompatibility and biodegradable.The relevant report of existing at present many preparation silk fibroin micron-particles, main preparation method has phase separation method, salting-out process, reverse microemulsion method and EFI method.
The ratio juris of saltouing is: there is hydrophilic radical on the silk fibroin molecular surface; Make water molecules form hydrated film on the surface; And the electric charge of hydrophilic radical and the charges of different polarity in the water molecules attract to form double electrical layers; Guarantee the solubility equilibria and the stable existence of molecule, the protein surface electric charge is neutralized in the adding of salt and hydrated film is destroyed, and destroys the stability and precipitate of protein in the aqueous solution and separates out; Make silk fibroin water solution from the insoluble conformation transition of random coil, form single fibroin particle that disperses to lower, the more stable beta sheet of energy.
In the prior art; David L.Kaplan seminar of U.S. Tufts University has adopted the method for saltouing, and silk fibroin solution is mixed with potassium phosphate solution, prepares particle diameter and disperses the fibroin particle at 486nm to the list between the 1.4um; Be applied to research to drug release; But the particle surface of its acquisition is coarse, and size distribution is wide, is unfavorable for the orderly self-assembly of particulate.
Summary of the invention
The technical problem that the present invention solves is to provide the preparation method of a kind of single fibroin particulate preparation method of dispersion and photonic crystal; Single fibroin particle that disperses that preparation method of the present invention obtains is spherical in shape; Show smooth; Monodispersity is better, and the adhesive between the particle reduces, and is applicable to the preparation of photonic crystal.
For solving the problems of the technologies described above, technical scheme of the present invention is achieved in that a kind of single fibroin particulate preparation method that disperses, and especially, comprises the steps:
A) preparation of fibroin: with the silk acquisition fibroin that comes unstuck;
B) preparation of silk fibroin protein solution: fibroin dissolving, purifying in the step a) are obtained silk fibroin protein solution;
C) single fibroin particulate that disperses prepares: with silk fibroin protein solution in the step b) and inorganic salt solution uniform mixing, subzero treatment at room temperature leaves standstill and is not less than 12 hours, removes supernatant then, and the throw out centrifuge washing obtains single fibroin particle that disperses.
Preferably, in above-mentioned single the dispersion among the fibroin particulate preparation method, the dissolving of fibroin need be under 80～100 ℃ environment in the said step b).
Preferably, in above-mentioned single the dispersion among the fibroin particulate preparation method, the dissolution time of fibroin is 6～12 hours in the said step b).
Preferably, in above-mentioned single the dispersion among the fibroin particulate preparation method, the inorganic salt in the said step c) are potassiumphosphate.
Preferably, in above-mentioned single the dispersion among the fibroin particulate preparation method, the ionic strength of said potassiumphosphate is 0.8～1.25M, and the pH value is 7～9.
Preferably, in above-mentioned single the dispersion among the fibroin particulate preparation method, the concentration of silk fibroin protein solution is 0.1%～1% in the said step b).
Preferably, in above-mentioned single the dispersion among the fibroin particulate preparation method, to use mass concentration be 0.5% the sodium hydrogencarbonate acquisition fibroin that comes unstuck to silk in the said step a).
Preferably, in above-mentioned single the dispersion among the fibroin particulate preparation method, the temperature of subzero treatment is 4～8 ℃ in the said step c), and the time is 2～4 hours.
The present invention also provides a kind of preparation method of photonic crystal, and especially, said photonic crystal is that material passes through the self-assembling method acquisition with the monodisperse particles, and said monodisperse particles adopts above-mentioned described single fibroin particle that disperses.
Preferably, in the preparation method of above-mentioned photonic crystal, said self-assembling method is a vertical deposition method
The present invention has reduced the adhesive between single dispersion fibroin particle through single fibroin particle that disperses that salting-out process obtains, and particle is spherical in shape, smooth surface, and monodispersity is better, is applicable to the preparation of photonic crystal.
Description of drawings
In order to be illustrated more clearly in the technical scheme of the embodiment of the invention; The accompanying drawing of required use is done to introduce simply in will describing embodiment below; Obviously, the accompanying drawing in describing below only is some embodiments of the present invention, for those of ordinary skills; Under the prerequisite of not paying creative work, can also obtain other accompanying drawing according to these accompanying drawings.
Shown in Figure 1 is the method block diagram for preparing photonic crystal in the embodiment of the invention;
The single fibroin particle photo under sem that disperses that obtains for embodiment 1 shown in Figure 2;
The single fibroin particle grain size distribution figure that disperses that obtains for embodiment 1 shown in Figure 3;
The single fibroin particle photo under sem that disperses that obtains for embodiment 2 shown in Figure 4;
The single fibroin particle grain size distribution figure that disperses that obtains for embodiment 2 shown in Figure 5;
The single fibroin particle photo under sem that disperses that obtains for embodiment 3 shown in Figure 6;
The single fibroin particle grain size distribution figure that disperses that obtains for embodiment 3 shown in Figure 7;
The single fibroin particle photo under sem that disperses that obtains for embodiment 4 shown in Figure 8;
The single fibroin particle grain size distribution figure that disperses that obtains for embodiment 4 shown in Figure 9.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment the preferred embodiment of the invention is described, describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
The embodiment of the invention discloses a kind of single fibroin particulate preparation method that disperses, comprise the steps:
A) preparation of fibroin: with the silk acquisition fibroin that comes unstuck;
B) preparation of silk fibroin protein solution: fibroin dissolving, purifying in the step a) are obtained silk fibroin protein solution;
C) single fibroin particulate that disperses prepares: with silk fibroin protein solution in the step b) and inorganic salt solution uniform mixing, subzero treatment at room temperature leaves standstill and is not less than 12 hours, removes supernatant then, and the throw out centrifuge washing obtains single fibroin particle that disperses.。
What the preparation of above-mentioned single dispersion fibroin particulate was adopted is salting-out process; Its principle is following: there is hydrophilic radical on the silk fibroin molecular surface; Make water molecules form hydrated film on the surface, and the electric charge of hydrophilic radical and the attraction of the charges of different polarity in water molecules formation double electrical layers, the solubility equilibria and the stable existence of assurance molecule; The protein surface electric charge is neutralized in the adding of salt and hydrated film is destroyed; Destroy the stability and precipitate of protein in the aqueous solution and separate out, make silk fibroin water solution, form single fibroin particle that disperses from the insoluble conformation transition of random coil to lower, the more stable beta sheet of energy.
In the step c), it is in order to make the particle slaking, to make its structure change βZhe Die fully into by random coil that room temperature left standstill more than 12 hours.
In above-mentioned single the dispersion among the fibroin particulate preparation method, preferred, to use mass concentration be 0.5% the sodium hydrogencarbonate acquisition fibroin that comes unstuck to silk in the step a).Be easy to expect that said sodium hydrogencarbonate also can adopt yellow soda ash or other basic solns to substitute, and does not limit among the present invention.
In above-mentioned single the dispersion among the fibroin particulate preparation method, preferred, the fibroin in the step b) need pass through high temperature and dissolve for a long time, obtains silk fibroin protein solution through purifying then.The dissolved temperature is preferably 80～100 ℃, and the dissolved time is preferably 6～12 hours, and the means of purifying preferably adopt the dialysis mode, and the concentration of silk fibroin protein solution is preferably 0.1%～1%.Through the silk fibroin protein solution that these means obtain, relative molecular weight narrow distribution.
In above-mentioned single the dispersion among the fibroin particulate preparation method, preferred, the inorganic salt in the step c) are potassiumphosphate.The ionic strength of said potassiumphosphate is 0.8～1.25M, and the pH value is 7～9.Said inorganic salt can also be selected from sodium-chlor, sodium sulfate, sal epsom, ammonium sulfate, potassiumphosphate etc., and its purpose is to make the protein surface electric charge to be neutralized and hydrated film is destroyed, and destroys the stability and precipitate of protein in the aqueous solution and separates out.
In above-mentioned single the dispersion among the fibroin particulate preparation method, preferred, the temperature of subzero treatment is 4～8 ℃ in the said step c), and the time is 2～4 hours.Preferred, the temperature of subzero treatment is 4 ℃, and the time is 2 hours.Subzero treatment is in order to prevent fibroin particulate adhesion reunion.
The embodiment of the invention also discloses a kind of preparation method of photonic crystal, said photonic crystal is that material passes through the self-assembling method acquisition with the monodisperse particles, and said monodisperse particles adopts described single fibroin particle that disperses.
Self-assembling method comprises self-assembly under natural sedimentation, the centrifuge field, filters the sedimentation self-assembly, the self-assembly under the auxiliary settling process of electrophoresis, colloid epitaxy, object restriction and vertical deposition method etc., can be selected from a kind of in the aforesaid method in order to the method for preparing photonic crystal in the embodiment of the invention.Preferably, the preferred vertical deposition method that adopts in the embodiment of the invention.
The vertical deposition method principle is: the vertical immersion of substrate contained in the solution of monodisperse particles; When solvent evaporation; Slowly from the substrate landing, particle is self-assembled into the photonic crystal with periodic arrangement structure to fluid surface at substrate surface under capillary pressure and electrostatic repulsion effect.
Photon crystal material is realized the special regulation and control to light with the formed periodic structure of the regular arrangement of single dispersed latex grain to the refraction of light or diffraction; Size according to periodic arrangement is different; To regulate and control light wavelength different, the Application Areas of corresponding prepared colloid photonic crystal film is different.In using usually, the colloidal crystal film is mainly used in aspects such as wave filter, photoswitch, optical waveguides, optical fiber.
In order to further specify technical scheme of the present invention; Below in conjunction with Fig. 1 and embodiment the preferred embodiment of the invention is described; Describe just to further specifying feature and advantage of the present invention but should be appreciated that these, rather than to the restriction of claim of the present invention.
Single preparation method who disperses fibroin particle and photonic crystal comprises the steps:
A) preparation of fibroin
Remove ionized water 2L, add the 10g sodium hydrogencarbonate, boil the back and add 10g cocoon sheet, boil 45min, wash 3-4 time with deionized water then, put into 40 ℃ of oven for drying, the back of coming unstuck fully obtains fibroin.
B) preparation of silk fibroin protein solution
The fibroin that obtains in the step a) dissolves 6h with LiBr solution in 80 ℃ of baking ovens, using molecular weight cut-off is 14000 dialysis tubing dialysis 3 days, obtains silk fibroin protein solution.
C) single fibroin particulate that disperses prepares
With concentration is that 0.5% silk fibroin protein solution and ionic strength are 1M, and the potassium phosphate solution of pH=8 mixes under magnetic agitation fast, and the time is 5min, and the solution that mixes places 4 ℃ of refrigerator 2h (subzero treatment), at room temperature leaves standstill 12h then.With the speed centrifuge washing of solution with 6000rpm, abandoning supernatant, throw out is with deionized water wash 3 times; And then it is centrifugal with lower speed; Make big solids precipitation obtain smaller particles, be dispersed in the deionized water, obtain single fibroin particulate suspension-s that disperses.
D) preparation of photonic crystal
Substrate is vertically immersed single the dispersion in the fibroin particulate suspension-s that step c) obtains; When solvent evaporation; Fluid surface is slowly from the substrate landing, and single fibroin particle that disperses is self-assembled into the photonic crystal with periodic arrangement structure at substrate surface under capillary pressure and electrostatic repulsion effect.
The thickness of photonic crystal can come accurately control through regulating single concentration of fibroin particulate diameter and solution of disperseing.
Ginseng Fig. 2 and shown in Figure 3, the single fibroin particle photo under sem that disperses that obtains for embodiment 1 shown in Figure 2; The single fibroin particle grain size distribution figure that disperses that obtains for embodiment 1 shown in Figure 3.Can find out that by Fig. 2 single fibroin particle that disperses that embodiment 1 obtains is spherical in shape, smooth surface, and also the viscosity between the particle is less.Can be found out that by Fig. 3 single dispersion fibroin particulate median size that embodiment 1 obtains is 1644nm, monodispersity is 0.055, is adapted to pass through self-assembling method and prepares photonic crystal.
Single preparation method who disperses fibroin particle and photonic crystal comprises the steps:
A) preparation of fibroin
Remove ionized water 2L, add the 10g sodium hydrogencarbonate, boil the back and add 10g cocoon sheet, boil 45min, wash 3-4 time with deionized water then, put into 40 ℃ of oven for drying, the back of coming unstuck fully obtains fibroin.
B) preparation of silk fibroin protein solution
The fibroin that obtains in the step a) dissolves 6h with LiBr solution in 80 ℃ of baking ovens, using molecular weight cut-off is 14000 dialysis tubing dialysis 3 days, obtains silk fibroin protein solution.
C) single fibroin particulate that disperses prepares
With concentration is that 0.1% silk fibroin protein solution and ionic strength are 0.8M, and the potassium phosphate solution of pH=8 mixes under magnetic agitation fast, and the time is 5min, and the solution that mixes places 4 ℃ of refrigerator 2h (subzero treatment), at room temperature leaves standstill 12h then.With the speed centrifuge washing of solution with 6000rpm, abandoning supernatant, throw out is with deionized water wash 3 times; And then it is centrifugal with lower speed; Make big solids precipitation obtain smaller particles, be dispersed in the deionized water, obtain single fibroin particulate suspension-s that disperses.
D) preparation of photonic crystal
Substrate is vertically immersed single the dispersion in the fibroin particulate suspension-s that step c) obtains; When solvent evaporation; Fluid surface is slowly from the substrate landing, and single fibroin particle that disperses is self-assembled into the photonic crystal with periodic arrangement structure at substrate surface under capillary pressure and electrostatic repulsion effect.
The thickness of photonic crystal can come accurately control through regulating single concentration of fibroin particulate diameter and solution of disperseing.
Ginseng Fig. 4 and shown in Figure 5, the single fibroin particle photo under sem that disperses that obtains for embodiment 2 shown in Figure 4; The single fibroin particle grain size distribution figure that disperses that obtains for embodiment 2 shown in Figure 5.Can find out that by Fig. 4 single fibroin particle that disperses that embodiment 2 obtains is spherical in shape, smooth surface, and also the viscosity between the particle is less.Can be found out that by Fig. 5 single dispersion fibroin particulate median size that embodiment 2 obtains is 1292nm, monodispersity is 0.106, is adapted to pass through self-assembling method and prepares photonic crystal.
Single preparation method who disperses fibroin particle and photonic crystal comprises the steps:
A) preparation of fibroin
Remove ionized water 2L, add the 10g sodium hydrogencarbonate, boil the back and add 10g cocoon sheet, boil 45min, wash 3-4 time with deionized water then, put into 40 ℃ of oven for drying, the back of coming unstuck fully obtains fibroin.
B) preparation of silk fibroin protein solution
The fibroin that obtains in the step a) dissolves 6h with LiBr solution in 80 ℃ of baking ovens, using molecular weight cut-off is 14000 dialysis tubing dialysis 3 days, obtains silk fibroin protein solution.
C) single fibroin particulate that disperses prepares
With concentration is that 0.5% silk fibroin protein solution and ionic strength are 1.25M, and the potassium phosphate solution of pH=8 mixes under magnetic agitation fast, and the time is 5min, and the solution that mixes places 4 ℃ of refrigerator 2h (subzero treatment), at room temperature leaves standstill 12h then.With the speed centrifuge washing of solution with 6000rpm, abandoning supernatant, throw out is with deionized water wash 3 times; And then it is centrifugal with lower speed; Make big solids precipitation obtain smaller particles, be dispersed in the deionized water, obtain single fibroin particulate suspension-s that disperses.
D) preparation of photonic crystal
Substrate is vertically immersed single the dispersion in the fibroin particulate suspension-s that step c) obtains; When solvent evaporation; Fluid surface is slowly from the substrate landing, and single fibroin particle that disperses is self-assembled into the photonic crystal with periodic arrangement structure at substrate surface under capillary pressure and electrostatic repulsion effect.
The thickness of photonic crystal can come accurately control through regulating single concentration of fibroin particulate diameter and solution of disperseing.
Ginseng Fig. 6 and shown in Figure 7, the single fibroin particle photo under sem that disperses that obtains for embodiment 3 shown in Figure 6; The single fibroin particle grain size distribution figure that disperses that obtains for embodiment 3 shown in Figure 7.Can find out that by Fig. 6 single fibroin particle that disperses that embodiment 3 obtains is spherical in shape, smooth surface, and also the viscosity between the particle is less.Can be found out that by Fig. 7 single dispersion fibroin particulate median size that embodiment 3 obtains is 1673nm, monodispersity is 0.033, is adapted to pass through self-assembling method and prepares photonic crystal.
Single preparation method who disperses fibroin particle and photonic crystal comprises the steps:
A) preparation of fibroin
Remove ionized water 2L, add the 10g sodium hydrogencarbonate, boil the back and add 10g cocoon sheet, boil 45min, wash 3-4 time with deionized water then, put into 40 ℃ of oven for drying, the back of coming unstuck fully obtains fibroin.
B) preparation of silk fibroin protein solution
The fibroin that obtains in the step a) dissolves 6h with LiBr solution in 80 ℃ of baking ovens, using molecular weight cut-off is 14000 dialysis tubing dialysis 3 days, obtains silk fibroin protein solution.
C) single fibroin particulate that disperses prepares
With concentration is that 1% silk fibroin protein solution and ionic strength are 1.25M, and the potassium phosphate solution of pH=8 mixes under magnetic agitation fast, and the time is 5min, and the solution that mixes places 4 ℃ of refrigerator 2h (subzero treatment), at room temperature leaves standstill 12h then.With the speed centrifuge washing of solution 6000rpm, abandoning supernatant, throw out is with deionized water wash 3 times; And then it is centrifugal with lower speed; Make big solids precipitation obtain smaller particles, be dispersed in the deionized water, obtain single fibroin particulate suspension-s that disperses.
D) preparation of photonic crystal
Substrate is vertically immersed single the dispersion in the fibroin particulate suspension-s that step c) obtains; When solvent evaporation; Fluid surface is slowly from the substrate landing, and single fibroin particle that disperses is self-assembled into the photonic crystal with periodic arrangement structure at substrate surface under capillary pressure and electrostatic repulsion effect.
The thickness of photonic crystal can come accurately control through regulating single concentration of fibroin particulate diameter and solution of disperseing.
Ginseng Fig. 8 and shown in Figure 9, the single fibroin particle photo under sem that disperses that obtains for embodiment 4 shown in Figure 8; The single fibroin particle grain size distribution figure that disperses that obtains for embodiment 4 shown in Figure 9.Can find out that by Fig. 8 single fibroin particle that disperses that embodiment 4 obtains is spherical in shape, smooth surface, and also the viscosity between the particle is less.Can be found out that by Fig. 9 single dispersion fibroin particulate median size that embodiment 4 obtains is 2167nm, monodispersity is 0.080, is adapted to pass through self-assembling method and prepares photonic crystal.
In sum, the present invention has reduced the adhesive between single dispersion fibroin particle through single fibroin particle that disperses that salting-out process obtains, and particle is spherical in shape, smooth surface, and monodispersity is better, is applicable to the preparation of photonic crystal.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be conspicuous concerning those skilled in the art, and defined General Principle can realize under the situation that does not break away from the spirit or scope of the present invention in other embodiments among this paper.Therefore, the present invention will can not be restricted to these embodiment shown in this paper, but will meet and principle disclosed herein and features of novelty the wideest corresponding to scope.
Claims (10)
1. single fibroin particulate preparation method that disperses is characterized in that, comprises the steps:
A) preparation of fibroin: with the silk acquisition fibroin that comes unstuck;
B) preparation of silk fibroin protein solution: fibroin dissolving, purifying in the step a) are obtained silk fibroin protein solution;
C) single fibroin particulate that disperses prepares: with silk fibroin protein solution in the step b) and inorganic salt solution uniform mixing, subzero treatment at room temperature leaves standstill and is not less than 12 hours, removes supernatant then, and the throw out centrifuge washing obtains single fibroin particle that disperses.
2. single fibroin particulate preparation method that disperses according to claim 1, it is characterized in that: the dissolving of fibroin need be under 80～100 ℃ environment in the said step b).
3. single fibroin particulate preparation method that disperses according to claim 2, it is characterized in that: the dissolution time of fibroin is 6～12 hours in the said step b).
4. single fibroin particulate preparation method that disperses according to claim 1, it is characterized in that: the inorganic salt in the said step c) are potassiumphosphate.
5. single fibroin particulate preparation method that disperses according to claim 4, it is characterized in that: the ionic strength of said potassiumphosphate is 0.8～1.25M, the pH value is 7～9.
6. single fibroin particulate preparation method that disperses according to claim 1, it is characterized in that: the concentration of silk fibroin protein solution is 0.1%～1% in the said step b).
7. single fibroin particulate preparation method that disperses according to claim 1 is characterized in that: to use mass concentration be 0.5% the sodium hydrogencarbonate acquisition fibroin that comes unstuck to silk in the said step a).
8. single fibroin particulate preparation method that disperses according to claim 1, it is characterized in that: the temperature of subzero treatment is 4～8 ℃ in the said step c), the time is 2～4 hours.
9. the preparation method of a photonic crystal is characterized in that: said photonic crystal is that material passes through self-assembling method and obtains with the monodisperse particles, and said monodisperse particles adopts any described single fibroin particle that disperses of claim 1 to 8.
10. the preparation method of photonic crystal according to claim 9, it is characterized in that: said self-assembling method is a vertical deposition method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104124508A CN102492300B (en) | 2011-12-12 | 2011-12-12 | Preparation method of monodispersing fibroin particles and preparation method of photonic crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011104124508A CN102492300B (en) | 2011-12-12 | 2011-12-12 | Preparation method of monodispersing fibroin particles and preparation method of photonic crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102492300A true CN102492300A (en) | 2012-06-13 |
| CN102492300B CN102492300B (en) | 2013-11-27 |
Family
ID=46184164
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011104124508A Active CN102492300B (en) | 2011-12-12 | 2011-12-12 | Preparation method of monodispersing fibroin particles and preparation method of photonic crystal |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102492300B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103993060A (en) * | 2014-05-08 | 2014-08-20 | 苏州大学张家港工业技术研究院 | Preparation method for controllable silk fibroin particle |
| CN107699952A (en) * | 2017-09-13 | 2018-02-16 | 大连大学 | A kind of preparation method of fibroin 1-D photon crystal |
| CN107698174A (en) * | 2017-09-13 | 2018-02-16 | 大连大学 | A kind of preparation method of the erasable photonic crystal paper of fibroin |
| CN108059661A (en) * | 2017-12-19 | 2018-05-22 | 上海祁稷新材料发展有限公司 | A kind of preparation method of nano wire fibroin particle |
| CN114808454A (en) * | 2022-05-05 | 2022-07-29 | 苏州大学 | Amorphous colloid array structure yarn-dyed fabric and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4233212A (en) * | 1979-04-17 | 1980-11-11 | Kanebo, Ltd. | Process for producing a fine powder of silk fibroin |
| JPS61276825A (en) * | 1985-05-31 | 1986-12-06 | Kanebo Ltd | Porous silk fibroin powder and production thereof |
| JP2005052162A (en) * | 2003-04-10 | 2005-03-03 | Silk Kogei:Kk | Production method of silk fibroin film |
| CN101891962A (en) * | 2010-07-22 | 2010-11-24 | 苏州大学 | Preparation method of silk fibroin porous three-dimensional material |
| CN101967282A (en) * | 2010-09-21 | 2011-02-09 | 苏州大学 | Sparingly water-soluble transparent silk fibroin film and preparation method thereof |
-
2011
- 2011-12-12 CN CN2011104124508A patent/CN102492300B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4233212A (en) * | 1979-04-17 | 1980-11-11 | Kanebo, Ltd. | Process for producing a fine powder of silk fibroin |
| JPS61276825A (en) * | 1985-05-31 | 1986-12-06 | Kanebo Ltd | Porous silk fibroin powder and production thereof |
| JP2005052162A (en) * | 2003-04-10 | 2005-03-03 | Silk Kogei:Kk | Production method of silk fibroin film |
| CN101891962A (en) * | 2010-07-22 | 2010-11-24 | 苏州大学 | Preparation method of silk fibroin porous three-dimensional material |
| CN101967282A (en) * | 2010-09-21 | 2011-02-09 | 苏州大学 | Sparingly water-soluble transparent silk fibroin film and preparation method thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103993060A (en) * | 2014-05-08 | 2014-08-20 | 苏州大学张家港工业技术研究院 | Preparation method for controllable silk fibroin particle |
| CN107699952A (en) * | 2017-09-13 | 2018-02-16 | 大连大学 | A kind of preparation method of fibroin 1-D photon crystal |
| CN107698174A (en) * | 2017-09-13 | 2018-02-16 | 大连大学 | A kind of preparation method of the erasable photonic crystal paper of fibroin |
| CN107698174B (en) * | 2017-09-13 | 2020-10-09 | 大连大学 | Preparation method of fibroin erasable photonic crystal paper |
| CN108059661A (en) * | 2017-12-19 | 2018-05-22 | 上海祁稷新材料发展有限公司 | A kind of preparation method of nano wire fibroin particle |
| CN114808454A (en) * | 2022-05-05 | 2022-07-29 | 苏州大学 | Amorphous colloid array structure yarn-dyed fabric and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102492300B (en) | 2013-11-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102492300B (en) | Preparation method of monodispersing fibroin particles and preparation method of photonic crystal | |
| Lin et al. | Correlation between hierarchical structure of crystal networks and macroscopic performance of mesoscopic soft materials and engineering principles | |
| Cölfen et al. | Higher‐order organization by mesoscale self‐assembly and transformation of hybrid nanostructures | |
| Lim et al. | Fabrication of one-dimensional colloidal assemblies from electrospun nanofibers | |
| Tian et al. | Bioinspired silica-based superhydrophobic materials | |
| Xu et al. | Wet and functional adhesives from one‐step aqueous self‐assembly of natural amino acids and polyoxometalates | |
| Taubert et al. | Kinetics and particle formation mechanism of zinc oxide particles in polymer-controlled precipitation from aqueous solution | |
| Qi et al. | Reverse micelle based formation of BaCO3 nanowires | |
| Holgado et al. | Electrophoretic deposition to control artificial opal growth | |
| Gao et al. | Block-copolymer-controlled growth of CaCO3 microrings | |
| CN100378190C (en) | Nano-water soluble microgel oil displacing material and its preparation method | |
| Weng et al. | Control of gel morphology and properties of a class of metallo-supramolecular polymers by good/poor solvent environments | |
| Liu et al. | Bioinspired crystallization of CaCO3 coatings on electrospun cellulose acetate fiber scaffolds and corresponding CaCO3 microtube networks | |
| JPWO2016093121A1 (en) | Colloidal eutectic, colloidal eutectic solidified body, and production method thereof | |
| Yu et al. | Large-area and water rewriteable photonic crystal films obtained by the thermal assisted air–liquid interface self assembly | |
| Li et al. | Controlling the morphology of BaCO3 aggregates by carboxymethyl cellulose through polymer induced needle-stacking self-assembly | |
| BRPI0722100A2 (en) | "ADDITIVE PREPARATION METHOD FOR COATINGS DESIGNED TO PROTECT SURFACES AND ADDITIVE FOR COATINGS DESIGNED TO PROTECT SURFACES" | |
| CN1687225A (en) | Method for preparing transparent optical material of polymer in high nano phase | |
| Ge et al. | Niche applications of magnetically responsive photonic structures | |
| Santos et al. | Optical sensor platform based on cellulose nanocrystals (CNC)–4′-(hexyloxy)-4-biphenylcarbonitrile (HOBC) bi-phase nematic liquid crystal composite films | |
| CN107057611A (en) | A kind of preparation method of polyacrylic hydrogels binder | |
| Kuleshova et al. | Automated device for vertical deposition of colloidal opal films | |
| Yin et al. | Gelation phenomenon during antisolvent crystallization of cefotaxime sodium | |
| Wang et al. | Superhydrophilic quaternized calcium alginate based aerogel membrane for oil-water separation and removal of bacteria and dyes | |
| CN103846067B (en) | Magnetic opposite sex Janus microballoon that a kind of particle diameter and pattern are all controlled and preparation method thereof and microfluidic control device used |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |