CN103265713A - Preparation method for multi-color film - Google Patents
Preparation method for multi-color film Download PDFInfo
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- CN103265713A CN103265713A CN2013101528956A CN201310152895A CN103265713A CN 103265713 A CN103265713 A CN 103265713A CN 2013101528956 A CN2013101528956 A CN 2013101528956A CN 201310152895 A CN201310152895 A CN 201310152895A CN 103265713 A CN103265713 A CN 103265713A
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Abstract
The invention provides a preparation method for a multi-color film, relating to a preparation method for a film. The objective of the invention is to overcome the problem that an inverse opal photonic crystal has a single response to a single outside stimulus, i.e., a single change in color, in the prior art. The preparation method comprises the following steps: 1, preparing a SiO2 seed; 2, preparing a SiO2 colloidal microsphere; 3, carrying out washing and drying; 4, preparing a SiO2 colloidal crystal template; 5, preparing a PMMA composite film; and 6, carrying out stretching. The multi-color film prepared in the invention is a photonic crystal with an inverse opal structure and has an ordered porous structure; meanwhile, the multi-color film has a certain orientation degree in a certain direction, so characteristics of the film in the field of a three dimensional structure are maintained. The preparation method provided by the invention is used for preparing the multi-color film.
Description
Technical field
The present invention relates to the preparation method of film.
Background technology
Since Yablonovitch and John since proposing the concept of photonic crystal simultaneously in 1987, in the time in 20 years, the research of photonic crystal is subjected to people's great attention always.Photonic crystal be by two or more materials with differing dielectric constant (specific refractory power) in the space according to the formed material with ordered structure of certain cycle series arrangement.Hertzian wave can be subjected to the modulation of the cycle potential field that is made of dielectric medium when propagating in this material that has in the periodic structure, thereby form the photonic band gap that is similar to the semiconductor energy band structure.If do not have overlappingly between the photonic band gap, will form photon band gap.The photon that frequency drops in the band gap can't be propagated in photonic crystal, the forbidden photon band material so photonic crystal is otherwise known as.Photonic crystal has shown great application prospect as the important advanced optical material of a class at aspects such as low threshold laser, straight (sharp) angle optical waveguides, photodiodes, becomes a kind of important materials that makes up photonic device.In actual applications, it is most important for the design and use of photonic device to make the forbidden photon band of response to external motivating force (electricity, light, chemical environment etc.).Photonic crystal with the forbidden photon band that can be regulated and control by external stimulus is called can modulate photonic crystal.At present, the research that can modulate photonic crystal becomes important direction and the focus of photonic crystal research field.In photonic crystal, the width of photon band gap and position are mainly determined by the lattice parameter of dielectric specific refractory power (or specific inductivity) and photonic crystal.Externally under the excitation of environment, changing wherein, any one parameter can play the purpose of regulating forbidden photon band.Under the single stimulation in the external world, a kind of response only can take place in photonic crystal usually, and color also only a kind of change can take place, and multiple color can not co-exist on a kind of photon crystal material simultaneously.
Therefore present inverse opal photonic crystal exists under the single external stimulus single response can only take place, i.e. the problem of solid color variation.
Summary of the invention
The present invention will solve present inverse opal photonic crystal and exist under the single external stimulus single response can only take place, i.e. the problem that changes of solid color, and a kind of preparation method of colorful film is provided.
A kind of preparation method of colorful film specifically prepares according to following steps:
One, L-arginine and deionized water are mixed, put into water-bath then, L-arginine and deionization are stirred, add hexanaphthene again, obtain mixing solutions; Regulating bath temperature is 55 ℃～65 ℃, and the control stirring velocity is 280rpm～320rpm, and mixing solutions is stirred, and the constant water bath temperature is 58 ℃～62 ℃ then, and adds tetraethoxy, and restir 18h～24h obtains SiO
2Seed, wherein, the volume ratio of the arginic quality of L-and deionized water is (12～14) mg: (9～11) mL, the volume of hexanaphthene are 16mL～20mL, the volume of tetraethoxy is 20mL～24mL;
Two, be that 25%～30% ammoniacal liquor mixes with dehydrated alcohol and mass concentration, put into temperature then and be 20 ℃～30 ℃ water-bath, add the SiO that step 1 obtains again
2Seed, the control stirring velocity is 180rpm～220rpm, keeps 12min～18min, adds mixed liquor A and mixed liquid B again, the control drop rate is 0.2mL/min～0.5mL/min, obtains SiO
2Colloid micro ball; Wherein the volume ratio of above-mentioned dehydrated alcohol and ammoniacal liquor is (9～11): 1, SiO
2The volume of seed is 0.5mL～0.7mL, mixed liquor A is made up of tetraethoxy and dehydrated alcohol, wherein the volume ratio of positive tetraethyl orthosilicate and dehydrated alcohol is (1～3): (3～5), mixed liquid B is that 25%～30% ammoniacal liquor and dehydrated alcohol are formed by deionized water, mass concentration, and wherein deionized water, mass concentration are that 25%～30% ammoniacal liquor and the volume ratio of dehydrated alcohol are (1～3): (2～4): (6～8);
Three, the SiO that step 2 is obtained
2Absolute ethanol washing is used in colloid micro ball deionized water centrifuge washing 3～5 times again, and centrifuge washing is 4～6 times then, and is dry again, obtains dry SiO
2Colloid micro ball;
Four, the SiO of the drying that step 3 is obtained
2Colloid micro ball is dissolved in the dehydrated alcohol, is mixed with mass concentration and is 30%～40% SiO
2Colloid emulsion vertically inserts SiO with substrate then
2In the colloid emulsion, the control temperature is 28 ℃～32 ℃, SiO
2Take out substrate after the absolute ethanol volatilizes in the colloid emulsion, obtain SiO
2Colloidal crystal template, wherein substrate is glass substrate;
Five, PMMA/MMA solution evenly is cast in the SiO that step 4 obtains
2On the colloidal crystal template, the control temperature is 60 ℃～80 ℃, keeps 12h～24h, obtains the PMMA composite membrane;
Six, it is 1%～3% HF that the PMMA composite membrane that step 5 is obtained is put into mass concentration, keeps 10h～12h, takes out the PMMA composite membrane, is immersed in new mass concentration again and is among 1%～3% the HF, keeps 8h～10h; Dry up with the ultrapure water washing and with nitrogen, then the PMMA composite membrane is loaded on the film stretching instrument, the temperature that the film stretching instrument is set is 75 ℃～85 ℃, prepares colorful film.
The invention has the beneficial effects as follows: the present invention adopts self-assembling technique, with PMMA/MMA solution casting SiO
2Colloidal crystal template corrodes then and removes SiO
2Colloidal crystal template stretches and prepares colorful film, and this film has not only possessed the order of colloidal crystal counter opal structure, has certain orientation degree in a certain direction simultaneously, has kept its characteristic in the three-dimensional structure field; Secondly the optical property of the caused uniqueness of this colorful film counter opal structure, it presents iris under visible light, not only have broad application prospects in the photonic crystal field, but also had the characteristic of polymkeric substance.
The present invention is for the preparation of colorful film.
Description of drawings
Fig. 1 is the digital photograph of the colorful film of embodiment one preparation, and wherein a represents redness, and the b representative is orange, and c represents yellow, and d represents green, and e represents cyan;
Fig. 2 is the reflected light spectrogram of the colorful film of embodiment one preparation, and wherein a represents redness, and the b representative is orange, and c represents yellow, and d represents green, and e represents cyan.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of a kind of colorful film of present embodiment specifically prepares according to following steps:
One, L-arginine and deionized water are mixed, put into water-bath then, L-arginine and deionization are stirred, add hexanaphthene again, obtain mixing solutions; Regulating bath temperature is 55 ℃～65 ℃, and the control stirring velocity is 280rpm～320rpm, and mixing solutions is stirred, and the constant water bath temperature is 58 ℃～62 ℃ then, and adds tetraethoxy, and restir 18h～24h obtains SiO
2Seed, wherein, the volume ratio of the arginic quality of L-and deionized water is (12～14) mg: (9～11) mL, the volume of hexanaphthene are 16mL～20mL, the volume of tetraethoxy is 20mL～24mL;
Two, be that 25%～30% ammoniacal liquor mixes with dehydrated alcohol and mass concentration, put into temperature then and be 20 ℃～30 ℃ water-bath, add the SiO that step 1 obtains again
2Seed, the control stirring velocity is 180rpm～220rpm, keeps 12min～18min, adds mixed liquor A and mixed liquid B again, the control drop rate is 0.2mL/min～0.5mL/min, obtains SiO
2Colloid micro ball; Wherein the volume ratio of above-mentioned dehydrated alcohol and ammoniacal liquor is (9～11): 1, SiO
2The volume of seed is 0.5mL～0.7mL, mixed liquor A is made up of tetraethoxy and dehydrated alcohol, wherein the volume ratio of positive tetraethyl orthosilicate and dehydrated alcohol is (1～3): (3～5), mixed liquid B is that 25%～30% ammoniacal liquor and dehydrated alcohol are formed by deionized water, mass concentration, and wherein deionized water, mass concentration are that 25%～30% ammoniacal liquor and the volume ratio of dehydrated alcohol are (1～3): (2～4): (6～8);
Three, the SiO that step 2 is obtained
2Absolute ethanol washing is used in colloid micro ball deionized water centrifuge washing 3～5 times again, and centrifuge washing is 4～6 times then, and is dry again, obtains dry SiO
2Colloid micro ball;
Four, the SiO of the drying that step 3 is obtained
2Colloid micro ball is dissolved in the dehydrated alcohol, is mixed with mass concentration and is 30%～40% SiO
2Colloid emulsion vertically inserts SiO with substrate then
2In the colloid emulsion, the control temperature is 28 ℃～32 ℃, SiO
2Take out substrate after the absolute ethanol volatilizes in the colloid emulsion, obtain SiO
2Colloidal crystal template, wherein substrate is glass substrate;
Five, PMMA/MMA solution evenly is cast in the SiO that step 4 obtains
2On the colloidal crystal template, the control temperature is 60 ℃～80 ℃, keeps 12h～24h, obtains the PMMA composite membrane;
Six, it is 1%～3% HF that the PMMA composite membrane that step 5 is obtained is put into mass concentration, keeps 10h～12h, takes out the PMMA composite membrane, is immersed in new mass concentration again and is among 1%～3% the HF, keeps 8h～10h; Dry up with the ultrapure water washing and with nitrogen, then the PMMA composite membrane is loaded on the film stretching instrument, the temperature that the film stretching instrument is set is 75 ℃～85 ℃, prepares colorful film.
Present embodiment adopts self-assembling technique, with PMMA/MMA solution casting SiO
2Colloidal crystal template corrodes then and removes SiO
2Colloidal crystal template stretches and prepares colorful film, and this film has not only possessed the order of colloidal crystal counter opal structure, has certain orientation degree in a certain direction simultaneously, has kept its characteristic in the three-dimensional structure field; Secondly the optical property of the caused uniqueness of this colorful film counter opal structure, it presents iris under visible light, not only have broad application prospects in the photonic crystal field, but also had the characteristic of polymkeric substance.
Embodiment two: what present embodiment and embodiment one were different is: the control stirring velocity is 300rpm in the step 1.Other is identical with embodiment one.
Embodiment three: what present embodiment and embodiment one were different is: the volume ratio of the arginic quality of L-and deionized water is 13mg: 10mL in the step 1.Other is identical with embodiment one.
Embodiment four: what present embodiment and embodiment one were different is: SiO in the step 4
2The mass concentration of colloid emulsion is 32%～38%.Other is identical with embodiment one.
Embodiment five: what present embodiment and embodiment one were different is: the control temperature is 30 ℃ in the step 4.Other is identical with embodiment one.
Embodiment six: what present embodiment and embodiment one were different is: the mass concentration of PMMA/MMA solution is 25%～35% in the step 5.Other is identical with embodiment one.
Embodiment seven: what present embodiment was different with one of embodiment one to six is: the mass concentration of PMMA/MMA solution is 30% in the step 5.Other is identical with one of embodiment one to six.
Embodiment eight: what present embodiment and embodiment one were different is: the control temperature is 65 ℃～75 ℃ in the step 5, keeps 14h～22h.Other is identical with embodiment one.
Embodiment nine: what present embodiment and embodiment one were different is: the temperature of film stretching instrument is 78 ℃～82 ℃ in the step 6.Other is identical with embodiment one.
Embodiment ten: what present embodiment was different with one of embodiment one to nine is: the temperature of film stretching instrument is 80 ℃ in the step 6.Other is identical with one of embodiment one to nine.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment one:
The preparation method of a kind of colorful film of present embodiment specifically prepares according to following steps:
One, L-arginine and deionized water are mixed, put into water-bath then, L-arginine and deionization are stirred, add hexanaphthene again, obtain mixing solutions; Regulating bath temperature is 60 ℃, and the control stirring velocity is 300rpm, and mixing solutions is stirred, and the constant water bath temperature is 60 ℃ then, and adds tetraethoxy, and restir 20h obtains SiO
2Seed, wherein, the arginic quality of L-is 364mg, and the volume of deionized water is 276mL, and the volume of hexanaphthene is 18mL, and the volume of tetraethoxy is 22mL;
Two, be that 30% ammoniacal liquor mixes with dehydrated alcohol and mass concentration, put into temperature then and be 25 ℃ water-bath, add the SiO that step 1 obtains again
2Seed, the control stirring velocity is 200rpm, keeps 15min, adds mixed liquor A and mixed liquid B again, the control drop rate is 0.2mL/min, obtains SiO
2Colloid micro ball; Wherein the volume of above-mentioned dehydrated alcohol is 160mL, and the volume of ammoniacal liquor is 15mL, SiO
2The volume of seed is 0.62mL, mixed liquor A is made up of tetraethoxy and dehydrated alcohol, wherein the volume of tetraethoxy is that the volume of 21.92mL, dehydrated alcohol is 43.84mL, mixed liquid B is that 30% ammoniacal liquor and dehydrated alcohol are formed by deionized water, mass concentration, and wherein the volume of deionized water is that 5.48mL, mass concentration are that the volume of 30% ammoniacal liquor is that the volume of 8.22mL, dehydrated alcohol is 19.18mL;
Three, the SiO that step 2 is obtained
2Absolute ethanol washing is used in colloid micro ball deionized water centrifuge washing 4 times again, and centrifuge washing is 5 times then, and is dry again, obtains dry SiO
2Colloid micro ball;
Four, the SiO of the drying that step 3 is obtained
2Colloid micro ball is dissolved in the dehydrated alcohol, is mixed with mass concentration and is 35% SiO
2Colloid emulsion vertically inserts SiO with substrate then
2In the colloid emulsion, the control temperature is 30 ℃, SiO
2Take out substrate after the absolute ethanol volatilizes in the colloid emulsion, obtain SiO
2Colloidal crystal template, wherein substrate is glass substrate;
Five, PMMA/MMA solution evenly is cast in the SiO that step 4 obtains
2On the colloidal crystal template, the control temperature is 80 ℃, keeps 24h, obtains the PMMA composite membrane;
Six, it is 2% HF that the PMMA composite membrane that step 5 is obtained is put into mass concentration, keeps 10h, takes out the PMMA composite membrane, is immersed in new mass concentration again and is among 2% the HF, keeps 8h; Dry up with the ultrapure water washing and with nitrogen, then the PMMA composite membrane is loaded on the film stretching instrument, the temperature that the film stretching instrument is set is 80 ℃, prepares colorful film.
The digital photograph of the colorful film of present embodiment preparation as shown in Figure 1, wherein a represent redly, b represents orange, c represents yellow, and d represents green, and e represents cyan, f represents blue, and as can be seen from the figure it presents iris under visible light, and this film has unique optical property.
The reflected light spectrogram of the colorful film of present embodiment preparation as shown in Figure 2, wherein a represent redly, b represents orange, c represents yellow, and d represents green, and e represents cyan, f represents blue, and as can be seen from the figure the color of colorful film film changes in gradient, and color has been covered with whole visible region substantially.
The present invention adopts self-assembling technique, with PMMA/MMA solution casting SiO
2Colloidal crystal template corrodes then and removes SiO
2Colloidal crystal template stretches and prepares colorful film, and this film has not only possessed the order of colloidal crystal counter opal structure, has certain orientation degree in a certain direction simultaneously, has kept its characteristic in the three-dimensional structure field; Secondly the optical property of the caused uniqueness of this colorful film counter opal structure, it presents iris under visible light, not only have broad application prospects in the photonic crystal field, but also had the characteristic of polymkeric substance.
Claims (10)
1. the preparation method of a colorful film is characterized in that specifically preparing a kind of preparation method of colorful film according to following steps:
One, L-arginine and deionized water are mixed, put into water-bath then, L-arginine and deionization are stirred, add hexanaphthene again, obtain mixing solutions; Regulating bath temperature is 55 ℃～65 ℃, and the control stirring velocity is 280rpm～320rpm, and mixing solutions is stirred, and the constant water bath temperature is 58 ℃～62 ℃ then, and adds tetraethoxy, and restir 18h～24h obtains SiO
2Seed, wherein, the volume ratio of the arginic quality of L-and deionized water is (12～14) mg: (9～11) mL, the volume of hexanaphthene are 16mL～20mL, the volume of tetraethoxy is 20mL～24mL;
Two, be that 25%～30% ammoniacal liquor mixes with dehydrated alcohol and mass concentration, put into temperature then and be 20 ℃～30 ℃ water-bath, add the SiO that step 1 obtains again
2Seed, the control stirring velocity is 180rpm～220rpm, keeps 12min～18min, adds mixed liquor A and mixed liquid B again, the control drop rate is 0.2mL/min～0.5mL/min, obtains SiO
2Colloid micro ball; Wherein the volume ratio of above-mentioned dehydrated alcohol and ammoniacal liquor is (9～11): 1, SiO
2The volume of seed is 0.5mL～0.7mL, mixed liquor A is made up of tetraethoxy and dehydrated alcohol, wherein the volume ratio of positive tetraethyl orthosilicate and dehydrated alcohol is (1～3): (3～5), mixed liquid B is that 25%～30% ammoniacal liquor and dehydrated alcohol are formed by deionized water, mass concentration, and wherein deionized water, mass concentration are that 25%～30% ammoniacal liquor and the volume ratio of dehydrated alcohol are (1～3): (2～4): (6～8);
Three, the SiO that step 2 is obtained
2Absolute ethanol washing is used in colloid micro ball deionized water centrifuge washing 3～5 times again, and centrifuge washing is 4～6 times then, and is dry again, obtains dry SiO
2Colloid micro ball;
Four, the SiO of the drying that step 3 is obtained
2Colloid micro ball is dissolved in the dehydrated alcohol, is mixed with mass concentration and is 30%～40% SiO
2Colloid emulsion vertically inserts SiO with substrate then
2In the colloid emulsion, the control temperature is 28 ℃～32 ℃, SiO
2Take out substrate after the absolute ethanol volatilizes in the colloid emulsion, obtain SiO
2Colloidal crystal template, wherein substrate is glass substrate;
Five, PMMA/MMA solution evenly is cast in the SiO that step 4 obtains
2On the colloidal crystal template, the control temperature is 60 ℃～80 ℃, keeps 12h～24h, obtains the PMMA composite membrane;
Six, it is 1%～3% HF that the PMMA composite membrane that step 5 is obtained is put into mass concentration, keeps 10h～12h, takes out the PMMA composite membrane, is immersed in new mass concentration again and is among 1%～3% the HF, keeps 8h～10h; Dry up with the ultrapure water washing and with nitrogen, then the PMMA composite membrane is loaded on the film stretching instrument, the temperature that the film stretching instrument is set is 75 ℃～85 ℃, prepares colorful film.
2. the preparation method of a kind of colorful film according to claim 1 is characterized in that the control stirring velocity is 300rpm in the step 1.
3. the preparation method of a kind of colorful film according to claim 1 is characterized in that the volume ratio of the arginic quality of L-and deionized water is 13mg: 10mL in the step 1.
4. the preparation method of a kind of colorful film according to claim 1 is characterized in that SiO in the step 4
2The mass concentration of colloid emulsion is 32%～38%.
5. the preparation method of a kind of colorful film according to claim 1 is characterized in that the control temperature is 30 ℃ in the step 4.
6. the preparation method of a kind of colorful film according to claim 1, the mass concentration that it is characterized in that PMMA/MMA solution in the step 5 is 25%～35%.
7. the preparation method of a kind of colorful film according to claim 6, the mass concentration that it is characterized in that PMMA/MMA solution in the step 5 is 30%.
8. the preparation method of a kind of colorful film according to claim 1 is characterized in that the control temperature is 65 ℃～75 ℃ in the step 5, keeps 14h～22h.
9. the preparation method of a kind of colorful film according to claim 1, the temperature that it is characterized in that film stretching instrument in the step 6 is 78 ℃～82 ℃.
10. the preparation method of a kind of colorful film according to claim 9, the temperature that it is characterized in that film stretching instrument in the step 6 is 80 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467773A (en) * | 2013-09-13 | 2013-12-25 | 东南大学 | Photonic crystal film with dual regulation and control on structural colors and wettability and preparation method thereof |
| CN104614808A (en) * | 2015-02-13 | 2015-05-13 | 苏州中科纳福材料科技有限公司 | Optical functional material with hue and gloss and production and application thereof |
| CN104698536A (en) * | 2015-02-13 | 2015-06-10 | 苏州中科纳福材料科技有限公司 | Optical functional material with gloss and color and preparation and application thereof |
| CN105113006A (en) * | 2015-09-21 | 2015-12-02 | 陕西科技大学 | Mono-dispersed spherical zinc sulfide photonic crystal with rough surface and preparation method thereof |
| CN111044496A (en) * | 2019-12-21 | 2020-04-21 | 东南大学 | Preparation method and application of silicon dioxide-based super-resolution imaging probe |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090046350A1 (en) * | 2004-05-14 | 2009-02-19 | Peter Herman | Photonic crystal mirrors for high-resolving-power fabry perots |
| CN101655610A (en) * | 2009-09-11 | 2010-02-24 | 中国科学院长春应用化学研究所 | Preparation method of inverse opal hydrogel photonic crystal with hybridized structure |
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- 2013-04-27 CN CN201310152895.6A patent/CN103265713B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090046350A1 (en) * | 2004-05-14 | 2009-02-19 | Peter Herman | Photonic crystal mirrors for high-resolving-power fabry perots |
| CN101655610A (en) * | 2009-09-11 | 2010-02-24 | 中国科学院长春应用化学研究所 | Preparation method of inverse opal hydrogel photonic crystal with hybridized structure |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467773A (en) * | 2013-09-13 | 2013-12-25 | 东南大学 | Photonic crystal film with dual regulation and control on structural colors and wettability and preparation method thereof |
| CN103467773B (en) * | 2013-09-13 | 2015-09-02 | 东南大学 | Photon crystal film of a kind of schemochrome and the two regulation and control of wetting property and preparation method thereof |
| CN104614808A (en) * | 2015-02-13 | 2015-05-13 | 苏州中科纳福材料科技有限公司 | Optical functional material with hue and gloss and production and application thereof |
| CN104698536A (en) * | 2015-02-13 | 2015-06-10 | 苏州中科纳福材料科技有限公司 | Optical functional material with gloss and color and preparation and application thereof |
| CN104614808B (en) * | 2015-02-13 | 2018-01-12 | 苏州中科纳福材料科技有限公司 | A kind of optical functional materialses and its preparation and application with form and aspect and gloss |
| CN104698536B (en) * | 2015-02-13 | 2018-01-12 | 苏州中科纳福材料科技有限公司 | A kind of optical functional materialses and its preparation and application with gloss and form and aspect |
| CN105113006A (en) * | 2015-09-21 | 2015-12-02 | 陕西科技大学 | Mono-dispersed spherical zinc sulfide photonic crystal with rough surface and preparation method thereof |
| CN111044496A (en) * | 2019-12-21 | 2020-04-21 | 东南大学 | Preparation method and application of silicon dioxide-based super-resolution imaging probe |
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| CN103265713B (en) | 2014-11-05 |
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