CN102808317A - Method for preparing silicon dioxide nanosphere assembled polymer fiber - Google Patents
Method for preparing silicon dioxide nanosphere assembled polymer fiber Download PDFInfo
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- CN102808317A CN102808317A CN2012103031356A CN201210303135A CN102808317A CN 102808317 A CN102808317 A CN 102808317A CN 2012103031356 A CN2012103031356 A CN 2012103031356A CN 201210303135 A CN201210303135 A CN 201210303135A CN 102808317 A CN102808317 A CN 102808317A
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Abstract
The invention relates to a method for preparing a silicon dioxide nanosphere assembled polymer fiber. The method comprises the following steps of: preparing a monodispersed silicon dioxide nanosphere from tetraethyl orthosilicate, ethanol, high-purity water and ammonia water by a sol-gel method; and putting a polymer fiber into a glass capillary, injecting the silicon dioxide nanosphere which is dispersed into a mixed solvent of the ethanol and the high-purity water into the glass capillary, fixing the glass capillary in a drying oven, and adjusting temperature to evaporate the solvent so as to obtain the silicon dioxide nanosphere assembled polymer fiber. The preparation process is simple, a chemical dye is not needed, the obtained polymer fiber has high optical property and flexibility, and the method has great significance for preparing a structural color fiber, makes great contribution to environment-friendly dyeing and finishing and is wide in application prospect.
Description
Technical field
The invention belongs to macromolecular fibre assembling field, particularly a kind of method of silica nanosphere assembling macromolecular fibre.
Background technology
The self assembly of nano material is under suitable physics, electrochemical conditions; Atom, molecule, particle and other construction units; Interaction through non-covalent bonds such as hydrogen bond, van der waals bond, electrostatic force, hydrophilic-hydrophobic interaction; Under the driving of the minimum property of system capacity principle, spontaneously formation has the process of nano structural material.Self-assembling technique the preparation that beginning just is applied to nano material always occurs from nano material, like nanocluster, nanotube, nano-rings, nano wire and functionalized nano material etc.Self assembly is the new method of constructing functional material with molecular level, has realized that the uniformity of molecule on the microstructure aspect is arranged in order, and this provides a kind of method of convenient and efficient for the preparation of photonic crystal.
At present; The schemochrome fiber is a kind of fiber with sandwich construction, belongs to 2 D photon crystal, selects the high polymer fibre and the thickness that calculates each layer of certain refractive index through strictness; Make each fibre thin layer produce the long mutually interference effect that strengthens, reflect the light of the very strong colour of certain wavelength light.Fiber based on the photonic crystal opal structural promptly passes through certain method, technological means, on fiber, adheres to the nanosphere such as the SiO that can be used as photonic crystal
2, PS or PMMA etc., under the irradiation of light, to physical optics effects such as scattering of light, diffraction and interference, make its Show Color through photonic crystal, i.e. schemochrome, fiber also demonstrates the corresponding structure look so.This fiber that has adhered to photonic crystal and colour developing is the photon crystal structure color fibre.
In recent years, Chinese scholars has been carried out extensive and deep research utilizing self-assembling technique to prepare photonic crystal and make it display structure look this respect.Ke Qin Zhang etc. are at Journal of Fiber Bioengineering and Informatics 2010; 2; Reported among the 214-218 that the method through the colloid self assembly has prepared the schemochrome fiber based on photonic crystal in open space, the photon crystal structure color fibre of preparing has excellent optical property placing observation under the light microscope; But owing to be in open space, to assemble, its photon crystal structure is difficult to keep the continuity of long distance.Zhifu Liu etc. are at Chemistry Communications 2011; 47; Design microfluidic device in being reported among the 12801-12803 between microvoid, the method through self assembly has prepared the schemochrome glass fibre by the silica assembling, under light microscope, has bluish-green schemochrome; But the schemochrome glass fibre of its preparation lacks pliability, as the fiber with special performance very big limitation is arranged in practical application.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of silica nanosphere assembling macromolecular fibre; It is simple that the present invention prepares process, need not chemical dye, and energy consumption is low; Be a kind of dyeing and finishing method of green non-pollution, energy-saving and emission-reduction and environmental protection are had big meaning; The macromolecular fibre of preparation not only has excellent optical property, and good pliability is arranged, and makes its fiber as a kind of unique properties step essential step to practical application; The present invention is significant for the implementation structure color fibre, for realizing that green dyeing and finishing also has significant contribution.
The present invention the method for a kind of silica nanosphere assembling macromolecular fibre, comprising:
(1) prepare two kinds of washing lotions of soda acid respectively, cleaning glass capillary and macromolecular fibre, and use distilled water flushing, oven dry;
(2) at room temperature, ethanol, high purity water, ammoniacal liquor were mixed the back magnetic agitation 5 ~ 20 minutes; The mixed solution that adds positive tetraethyl orthosilicate and ethanol again, regulating temperature is 25 ~ 60 ℃, isothermal reaction 0.5 ~ 2 hour; Obtain monodispersed silica nanosphere; Naturally after the cooling with the silica nanosphere separating, washing, and be distributed in the ethanol, obtain dispersion liquid;
(3) dispersion liquid is mixed with high purity water, be transported to mixed liquor in the capillary glass tube that is placed with macromolecular fibre through micro syringe pump with syringe; Heating evaporation falls the second alcohol and water, and the back oven dry that evaporates makes the silica nanosphere self assembly on the macromolecular fibre surface.
Pickle in the said step (1) is that volume ratio is the concentrated sulfuric acid, hydrogen peroxide solution, the distilled water of 3:1:20; Alkali wash water is that volume ratio is ammoniacal liquor, hydrogen peroxide solution, the distilled water of 3:1:20; The wash temperature of soda acid two kinds of washing lotion cleaning glass capillary and macromolecular fibre is 80 ~ 120 ℃, and wash time is 20 ~ 60min.
Macromolecular fibre in the said step (1) is polypropylene fibre or polyamide fiber.
The volume ratio of the ethanol in the said step (2), high purity water, ammoniacal liquor, positive tetraethyl orthosilicate is 100:9:3.5:3 ~ 100:9:3.5:7.
Ethanol in the said step (2) is 28:3 ~ 28:7 with the volume ratio of positive tetraethyl orthosilicate TEOS.
Magnetic agitation speed in the said step (2) is 400 ~ 600rpm.
The concentration that silica nanosphere in the said step (2) is scattered in the ethanol is 8 ~ 32mg/mL.
The dispersion liquid in the said step (3) and the volume ratio of high purity water are 6:4 ~ 8:2.
Evaporating temperature in the said step (3) is 65 ~ 85 ℃, and bake out temperature is 65 ~ 120 ℃, and drying time is 6 ~ 15 hours.
The invention provides a kind of method with silica nanosphere assembling macromolecular fibre.Silica nanosphere mode self assembly through heating evaporation in the glass capillary microchannel is surperficial at macromolecular fibre, the schemochrome of realization macromolecular fibre.The present invention adopts
sol-gel process, is the monodispersed silica nanosphere of feedstock production with positive tetraethyl orthosilicate, ethanol, high purity water, ammoniacal liquor; Secondly, the silica nanosphere that utilizes micro syringe pump will be dissolved in the second alcohol and water is expelled in the glass capillary that is placed with macromolecular fibre; Glass tube is fixed in the baking oven, regulates temperature evaporation water and ethanol, finally obtain the macromolecular fibre of silica nanosphere assembling.The ratio, the temperature of thermal evaporation of particle diameter, water and ethanol through the adjustment silica nanosphere can be arranged in the silica of the different numbers of plies macromolecular fibre surface, make its display structure look.
The present invention implements like this: earlier respectively with the soda acid washing lotion glass cleaning capillary for preparing and macromolecular fibre and oven dry; Measure ethanol, water, ammoniacal liquor then by a certain percentage, mix and pour in the there-necked flask, after stirring; The mixed liquor that adds a certain amount of TEOS and ethanol; Regulate temperature, isothermal reaction obtains silica nanosphere, and it is distributed to obtains dispersion liquid in the alcohol solvent; At last; Use capillary glass tube to be assembling substrates as microchannel, macromolecular fibre; Utilize micro syringe pump that the mixed solution of dispersion liquid and water is transported to the microchannel that places baking oven, regulate oven temperature ethanol evaporation and water, obtain the macromolecular fibre of silica nanosphere assembling.
Beneficial effect
It is simple that the present invention prepares process, need not chemical dye, and energy consumption is low, is a kind of dyeing and finishing method of green non-pollution, and energy-saving and emission-reduction and environmental protection are had big meaning; The macromolecular fibre of preparation not only has excellent optical property, and good pliability is arranged, and makes its fiber as a kind of unique properties step essential step to practical application; The present invention is significant for the implementation structure color fibre, for realizing that green dyeing and finishing also has significant contribution.
Description of drawings
Low power (a) high power (b) stereoscan photograph that macromolecular fibre monolayer surface silica nanosphere is arranged among Fig. 1 embodiment 1;
Macromolecular fibre surface multilayer silica nanosphere stereoscan photograph (a) among Fig. 2 embodiment 2, optical microscope photograph (b) (multiplication factor: 100 times);
Among Fig. 3 embodiment 3 in the capillary glass tube microchannel liquid level change spectrogram in time;
The stereoscan photograph that macromolecular fibre monolayer surface silica nanosphere is arranged among Fig. 4 embodiment 4;
The optical microscope photograph (multiplication factor: 400 times) that macromolecular fibre surface multilayer silica nanosphere is arranged among Fig. 5 embodiment 5.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Respectively with the concentrated sulfuric acid, hydrogen peroxide solution, distilled water; Volume ratio is that 3:1:20 and ammoniacal liquor, hydrogen peroxide solution, distilled water volume ratio are two kinds of washing lotions of 3:1:20 preparation soda acid, and cleaning glass capillary and polypropylene fibre under 80 ℃ of conditions, scavenging period are 60min; And use distilled water flushing, dry; Under the room temperature; Measure ethanol, 9mL water, the 3.5mL ammoniacal liquor of 72mL and be placed in the there-necked flask; The mixing speed of regulating magnetic stirring apparatus is 500rpm, and magnetic agitation 15 minutes adds the mixed solution of 7mL TEOS and 28mL ethanol again; Regulating the oil bath pan temperature is 25 ℃, and isothermal reaction is cooling naturally after 2 hours.With the product centrifugation, washing obtains monodispersed silica nanosphere, and it is distributed to the dispersion liquid that obtains 16mg/mL in the 50mL alcohol solvent then.
The dispersion liquid that above-mentioned steps is obtained is water-soluble and the solution that obtains placed syringe in the ratio of 7:3.Again polypropylene fibre is put into the glass capillary microchannel; Utilize micro syringe pump the liquid in the syringe to be transported to the glass capillary microchannel that places baking oven; Regulating oven temperature is 70 ℃, and evaporating off water and ethanol self-assemble on the polypropylene fibre silica nanosphere; Take off glass tube behind the liquid evaporate to dryness in glass tube, be placed on 80 ℃ of oven dry taking-ups after 10 hours in the baking oven, obtain the polypropylene fibre of silica nanosphere assembling.Fig. 1 is the stereoscan photograph that macromolecular fibre monolayer surface silica nanosphere is arranged, and can know that by figure silica nanosphere is assembled in the surface of polypropylene fibre with the mode of face-centered cubic packing, and is evenly distributed.
Embodiment 2
Respectively with the concentrated sulfuric acid, hydrogen peroxide solution, distilled water; Volume ratio is that 3:1:20 and ammoniacal liquor, hydrogen peroxide solution, distilled water volume ratio are two kinds of washing lotions of 3:1:20 preparation soda acid, and cleaning glass capillary and polypropylene fibre under 90 ℃ of conditions, scavenging period are 50min; And use distilled water flushing, dry; At room temperature; Measure ethanol, 9mL water, the 3.5mL ammoniacal liquor of 72mL and be placed in the there-necked flask; The mixing speed of regulating magnetic stirring apparatus is 400rpm, and magnetic agitation 20 minutes adds the mixed solution of 3mL TEOS and 28mL ethanol again; Regulating the oil bath pan temperature is 30 ℃, and isothermal reaction is cooling naturally after 1.5 hours.With the product centrifugation, washing obtains monodispersed silica nanosphere, and it is distributed to the dispersion liquid that obtains 16mg/mL in the 30mL alcohol solvent then.
The dispersion liquid that above-mentioned steps is obtained is water-soluble and the solution that obtains placed syringe by the volume ratio of 8:2.Again polypropylene fibre is put into the glass capillary microchannel; Utilize micro syringe pump the liquid in the syringe to be transported to the glass capillary microchannel that places baking oven; Regulating oven temperature is 75 ℃, and evaporating off water and ethanol self-assemble on the polypropylene fibre silica nanosphere; Take off glass tube behind the liquid evaporate to dryness in glass tube, be placed on 65 ℃ of oven dry taking-ups after 15 hours in the baking oven, obtain the polypropylene fibre of silica nanosphere assembling.Fig. 2 is stereoscan photograph and the corresponding with it optical microscope photograph that macromolecular fibre surface multilayer silica nanosphere is arranged.
Respectively with the concentrated sulfuric acid, hydrogen peroxide solution, distilled water; Volume ratio is that 3:1:20 and ammoniacal liquor, hydrogen peroxide solution, distilled water volume ratio are two kinds of washing lotions of 3:1:20 preparation soda acid, and cleaning glass capillary and polypropylene fibre under 100 ℃ of conditions, scavenging period are 40min; And use distilled water flushing, dry; At room temperature; Measure ethanol, 9mL water, the 3.5mL ammoniacal liquor of 72mL and be placed in the there-necked flask; The mixing speed of regulating magnetic stirring apparatus is 600rpm, and magnetic agitation 10 minutes adds the mixed solution of 3mL TEOS and 28mL ethanol again; Regulating the oil bath pan temperature is 40 ℃, and isothermal reaction is cooling naturally after 1.5 hours.With the product centrifugation, washing obtains monodispersed silica nanosphere, and it is distributed to the dispersion liquid that obtains 8mg/mL in the 30mL alcohol solvent then.
The dispersion liquid that above-mentioned steps is obtained is water-soluble and the solution that obtains placed syringe by the volume ratio of 6:4.Again polypropylene fibre is put into the glass capillary microchannel; Utilize micro syringe pump the liquid in the syringe to be transported to the glass capillary microchannel that places baking oven; Regulating oven temperature is 85 ℃, and evaporating off water and ethanol self-assemble on the polypropylene fibre silica nanosphere; Take off glass tube behind the liquid evaporate to dryness in glass tube, be placed on 100 ℃ of oven dry taking-ups after 8 hours in the baking oven, obtain the polypropylene fibre of silica nanosphere assembling.Fig. 3 is a liquid level variation diagram in time in the glass capillary.
Embodiment 4
Respectively with the concentrated sulfuric acid, hydrogen peroxide solution, distilled water; Volume ratio is that 3:1:20 and ammoniacal liquor, hydrogen peroxide solution, distilled water volume ratio are two kinds of washing lotions of 3:1:20 preparation soda acid, and cleaning glass capillary and polyamide fiber under 110 ℃ of conditions, scavenging period are 30min; And use distilled water flushing, dry; At room temperature; Measure ethanol, 9mL water, the 3.5mL ammoniacal liquor of 72mL and be placed in the there-necked flask; The mixing speed of regulating magnetic stirring apparatus is 600rpm, and magnetic agitation 5 minutes adds the mixed solution of 7mL TEOS and 28mL ethanol again; Regulating the oil bath pan temperature is 50 ℃, and isothermal reaction is cooling naturally after 1 hour.With the product centrifugation, washing obtains monodispersed silica nanosphere, and it is distributed to the dispersion liquid that obtains 32mg/mL in the 50mL alcohol solvent then.
The dispersion liquid that above-mentioned steps is obtained is water-soluble and the solution that obtains placed syringe by the volume ratio of 6:4.Again polyamide fiber is put into the glass capillary microchannel; Utilize micro syringe pump the liquid in the syringe to be transported to the glass capillary microchannel that places baking oven; Regulating oven temperature is 80 ℃, and evaporating off water and ethanol self-assemble on the polyamide fiber silica nanosphere; Take off glass tube behind the liquid evaporate to dryness in glass tube, be placed on 120 ℃ of oven dry taking-ups after 6 hours in the baking oven, obtain the polyamide fiber of silica nanosphere assembling.Fig. 4 is the stereoscan photograph that macromolecular fibre monolayer surface silica nanosphere is arranged.
Embodiment 5
Respectively with the concentrated sulfuric acid, hydrogen peroxide solution, distilled water; Volume ratio is that 3:1:20 and ammoniacal liquor, hydrogen peroxide solution, distilled water volume ratio are two kinds of washing lotions of 3:1:20 preparation soda acid, and cleaning glass capillary and polyamide fiber under 120 ℃ of conditions, scavenging period are 20min; And use distilled water flushing, dry; At room temperature; Measure ethanol, 9mL water, the 3.5mL ammoniacal liquor of 72mL and be placed in the there-necked flask; The mixing speed of regulating magnetic stirring apparatus is 400rpm, and magnetic agitation 20 minutes adds the mixed solution of 3mL TEOS and 28mL ethanol again; Regulating the oil bath pan temperature is 60 ℃, and isothermal reaction is cooling naturally after 0.5 hour.With the product centrifugation, washing obtains monodispersed silica nanosphere, and it is distributed to the dispersion liquid that obtains 32mg/mL in the 30mL alcohol solvent then.
The dispersion liquid that above-mentioned steps is obtained is water-soluble and the solution that obtains placed syringe by the volume ratio of 6:4.Again polyamide fiber is put into the glass capillary microchannel; Utilize micro syringe pump the liquid in the syringe to be transported to the glass capillary microchannel that places baking oven; Regulating oven temperature is 85 ℃, and evaporating off water and ethanol self-assemble on the polyamide fiber silica nanosphere; Take off glass tube behind the liquid evaporate to dryness in glass tube, be placed on 90 ℃ of oven dry taking-ups after 10 hours in the baking oven, obtain the polyamide fiber of silica nanosphere assembling.Fig. 5 is the optical microscope photograph that macromolecular fibre surface multilayer silica nanosphere is arranged.
Claims (9)
1. the method for silica nanosphere assembling macromolecular fibre comprises:
(1) prepare two kinds of washing lotions of soda acid respectively, cleaning glass capillary and macromolecular fibre, and use distilled water flushing, oven dry;
(2) at room temperature, ethanol, high purity water, ammoniacal liquor were mixed the back magnetic agitation 5 ~ 20 minutes; The mixed solution that adds positive tetraethyl orthosilicate and ethanol again, regulating temperature is 25 ~ 60 ℃, isothermal reaction 0.5 ~ 2 hour; Obtain monodispersed silica nanosphere; Naturally after the cooling silica nanosphere centrifugation is washed, and be distributed in the ethanol, obtain dispersion liquid;
(3) dispersion liquid is mixed with high purity water, be transported to mixed liquor in the capillary glass tube that is placed with macromolecular fibre through micro syringe pump with syringe; Heating evaporation falls the second alcohol and water, and the back oven dry that evaporates makes the silica nanosphere self assembly on the macromolecular fibre surface.
2. the method for a kind of silica nanosphere assembling macromolecular fibre according to claim 1, it is characterized in that: the pickle in the step (1) is the concentrated sulfuric acid, hydrogen peroxide solution, the distilled water of volume ratio 3:1:20; Alkali wash water is ammoniacal liquor, hydrogen peroxide solution, the distilled water of volume ratio 3:1:20; The wash temperature of cleaning glass capillary and macromolecular fibre is 80 ~ 120 ℃, and wash time is 20 ~ 60min.
3. the method for a kind of silica nanosphere assembling macromolecular fibre according to claim 1, it is characterized in that: the macromolecular fibre in the said step (1) is polypropylene fibre and polyamide fiber.
4. the method for a kind of silica nanosphere assembling macromolecular fibre according to claim 1 is characterized in that: the volume ratio of the ethanol in the said step (2), high purity water, ammoniacal liquor, positive tetraethyl orthosilicate is 100:9:3.5:3 ~ 100:9:3.5:7.
5. the method for a kind of silica nanosphere assembling macromolecular fibre according to claim 1 is characterized in that: the ethanol in the said step (2) is 28:3 ~ 28:7 with the volume ratio of positive tetraethyl orthosilicate TEOS.
6. the method for a kind of silica nanosphere assembling macromolecular fibre according to claim 1, it is characterized in that: the magnetic agitation speed in the said step (2) is 400 ~ 600rpm.
7. the method for a kind of silica nanosphere assembling macromolecular fibre according to claim 1, it is characterized in that: the concentration that the silica nanosphere in the said step (2) is scattered in the ethanol is 8 ~ 32mg/mL.
8. the method for a kind of silica nanosphere assembling macromolecular fibre according to claim 1, it is characterized in that: the dispersion liquid in the said step (3) and the volume ratio of high purity water are 6:4 ~ 8:2.
9. the method for a kind of silica nanosphere assembling macromolecular fibre according to claim 1, it is characterized in that: the evaporating temperature in the said step (3) is 65 ~ 85 ℃, and bake out temperature is 65 ~ 120 ℃, and drying time is 6 ~ 15 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104213399A (en) * | 2014-08-26 | 2014-12-17 | 上海应用技术学院 | High-refractive-index structure color fiber with self assembly of ZnS nano balls and preparation method of high-refractive-index structure color fiber with self assembly of ZnS nano balls |
| CN106637953A (en) * | 2016-12-14 | 2017-05-10 | 陕西科技大学 | Modification method of p-aramid fiber chopped fiber |
| CN109338717A (en) * | 2018-09-28 | 2019-02-15 | 西安理工大学 | Compliant conductive fiber based on silver nanowires and preparation method thereof |
| CN110004520A (en) * | 2019-04-17 | 2019-07-12 | 电子科技大学 | A kind of simple method for preparing uniform micron order fiber |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104213399A (en) * | 2014-08-26 | 2014-12-17 | 上海应用技术学院 | High-refractive-index structure color fiber with self assembly of ZnS nano balls and preparation method of high-refractive-index structure color fiber with self assembly of ZnS nano balls |
| CN106637953A (en) * | 2016-12-14 | 2017-05-10 | 陕西科技大学 | Modification method of p-aramid fiber chopped fiber |
| CN109338717A (en) * | 2018-09-28 | 2019-02-15 | 西安理工大学 | Compliant conductive fiber based on silver nanowires and preparation method thereof |
| CN109338717B (en) * | 2018-09-28 | 2021-04-06 | 西安理工大学 | Flexible conductive fiber based on silver nanowires and preparation method thereof |
| CN110004520A (en) * | 2019-04-17 | 2019-07-12 | 电子科技大学 | A kind of simple method for preparing uniform micron order fiber |
| CN110004520B (en) * | 2019-04-17 | 2020-10-09 | 电子科技大学 | Method for simply preparing uniform micron-sized fibers |
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Application publication date: 20121205 |