CN103265713B - Preparation method for multi-color film - Google Patents
Preparation method for multi-color film Download PDFInfo
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- CN103265713B CN103265713B CN201310152895.6A CN201310152895A CN103265713B CN 103265713 B CN103265713 B CN 103265713B CN 201310152895 A CN201310152895 A CN 201310152895A CN 103265713 B CN103265713 B CN 103265713B
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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 are since proposing the concept of photonic crystal in 1987 simultaneously, in the time of 20 years, the research of photonic crystal is subject to people's great attention always.Photonic crystal is to arrange according to certain cycle order the material with ordered structure forming in space by the two or more materials with differing dielectric constant (specific refractory power).The modulation of the cycle potential field that hertzian wave can be subject to being made up of dielectric medium while propagation in this material having in periodic structure, thus the photonic band gap that is similar to semiconductor energy band structure formed.If do not have overlappingly between photonic band gap, will form photon band gap.The photon that frequency drops in band gap cannot be propagated in photonic crystal, the forbidden photon band material so photonic crystal is otherwise known as.Photonic crystal, as the important advanced optical material of a class, has shown huge application prospect at aspects such as low threshold laser, straight (sharp) angle optical waveguides, photodiodes, becomes a kind of important materials that builds photonic device.In actual applications, can make the forbidden photon band of response to external motivating force (electricity, light, chemical environment etc.) most important for the design and use of photonic device.The photonic crystal with the forbidden photon band that can be regulated and controled 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.Under the excitation of outside atmosphere, change wherein any one parameter and can play the object that regulates forbidden photon band.Under the single stimulation in the external world, only can there is a kind of response in photonic crystal conventionally, and a kind of change also only can occur color, and multiple color can not co-exist on a kind of photon crystal material simultaneously.
Therefore can only there is single response, the problem that solid color changes in inverse opal photonic crystal existence at present under single external stimulus.
Summary of the invention
The present invention will solve current inverse opal photonic crystal and exist, under single external stimulus, single response can only occur, the problem that solid color changes, and a kind of preparation method of colorful film is provided.
A preparation method for colorful film, specifically prepares according to following steps:
One, L-arginine and deionized water are mixed, then put into water-bath, by even to L-arginine and deionized water and stirring, then add hexanaphthene, obtain mixing solutions; Regulating bath temperature is 55 DEG C～65 DEG C, and control stirring velocity is 280rpm～320rpm, and mixing solutions is stirred, and then constant water bath temperature is 58 DEG C～62 DEG C, and adds tetraethoxy, then stirs 18h～24h, obtains SiO
2seed, wherein, the quality of L-arginine and the volume ratio of deionized water are (12～14) mg: (9～11) mL, the volume of hexanaphthene is 16mL～20mL, the volume of tetraethoxy is 20mL～24mL;
Two, the ammoniacal liquor that is 25%～30% by dehydrated alcohol and mass concentration mixes, and then puts into temperature and be the water-bath of 20 DEG C～30 DEG C, then the SiO that adds step 1 to obtain
2seed, control stirring velocity is 180rpm～220rpm, keeps 12min～18min, then adds mixed liquor A and mixed liquid B, 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 tetraethyl orthosilicate and dehydrated alcohol is (1～3): (3～5), ammoniacal liquor and dehydrated alcohol that mixed liquid B is 25%～30% by deionized water, mass concentration form, and wherein deionized water, ammoniacal liquor that mass concentration is 25%～30% and the volume ratio of dehydrated alcohol are (1～3): (2～4): (6～8);
Three, SiO step 2 being obtained
2colloid micro ball deionized water centrifuge washing 3～5 times, then use absolute ethanol washing, then centrifuge washing 4～6 times, drier, obtain dry SiO
2colloid micro ball;
Four, dry SiO step 3 being obtained
2colloid micro ball is dissolved in dehydrated alcohol, is mixed with mass concentration and is 30%～40% SiO
2colloid emulsion, then vertically inserts SiO by substrate
2in colloid emulsion, controlling temperature is 28 DEG C～32 DEG C, SiO
2after absolute ethanol volatilizes in colloid emulsion, take out substrate, obtain SiO
2colloidal crystal template, wherein substrate is glass substrate;
Five, PMMA/MMA solution is evenly cast in to the SiO that step 4 obtains
2on colloidal crystal template, controlling temperature is 60 DEG C～80 DEG C, keeps 12h～24h, obtains PMMA composite membrane;
Six, it is 1%～3% HF that PMMA composite membrane step 5 being obtained is put into mass concentration, keeps 10h～12h, takes out PMMA composite membrane, then to be immersed in new mass concentration be, in 1%～3% HF, to keep 8h～10h; Dry up with ultrapure water washing and with nitrogen, then PMMA composite membrane is loaded on film stretching instrument, the temperature that film stretching instrument is set is 75 DEG C～85 DEG C, 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, then corrodes 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 in one direction certain orientation degree simultaneously, has retained its characteristic in three-dimensional structure field; Secondly the optical property of the caused uniqueness of this colorful film counter opal structure, it presents iris under visible ray, not only has broad application prospects in photonic crystal field, but also has had the characteristic of polymkeric substance.
The present invention is for the preparation of colorful film.
Brief description of the drawings
Fig. 1 is the digital photograph of the colorful film prepared of embodiment mono-, and wherein a represents redly, and b represents orange, and c represent yellow, and d represents green, and e represents cyan;
Fig. 2 is the reflected light spectrogram of the colorful film prepared of embodiment mono-, and wherein a represents redly, and b represents orange, and c represent 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, then put into water-bath, by even to L-arginine and deionized water and stirring, then add hexanaphthene, obtain mixing solutions; Regulating bath temperature is 55 DEG C～65 DEG C, and control stirring velocity is 280rpm～320rpm, and mixing solutions is stirred, and then constant water bath temperature is 58 DEG C～62 DEG C, and adds tetraethoxy, then stirs 18h～24h, obtains SiO
2seed, wherein, the quality of L-arginine and the volume ratio of deionized water are (12～14) mg: (9～11) mL, the volume of hexanaphthene is 16mL～20mL, the volume of tetraethoxy is 20mL～24mL;
Two, the ammoniacal liquor that is 25%～30% by dehydrated alcohol and mass concentration mixes, and then puts into temperature and be the water-bath of 20 DEG C～30 DEG C, then the SiO that adds step 1 to obtain
2seed, control stirring velocity is 180rpm～220rpm, keeps 12min～18min, then adds mixed liquor A and mixed liquid B, 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 tetraethyl orthosilicate and dehydrated alcohol is (1～3): (3～5), ammoniacal liquor and dehydrated alcohol that mixed liquid B is 25%～30% by deionized water, mass concentration form, and wherein deionized water, ammoniacal liquor that mass concentration is 25%～30% and the volume ratio of dehydrated alcohol are (1～3): (2～4): (6～8);
Three, SiO step 2 being obtained
2colloid micro ball deionized water centrifuge washing 3～5 times, then use absolute ethanol washing, then centrifuge washing 4～6 times, drier, obtain dry SiO
2colloid micro ball;
Four, dry SiO step 3 being obtained
2colloid micro ball is dissolved in dehydrated alcohol, is mixed with mass concentration and is 30%～40% SiO
2colloid emulsion, then vertically inserts SiO by substrate
2in colloid emulsion, controlling temperature is 28 DEG C～32 DEG C, SiO
2after absolute ethanol volatilizes in colloid emulsion, take out substrate, obtain SiO
2colloidal crystal template, wherein substrate is glass substrate;
Five, PMMA/MMA solution is evenly cast in to the SiO that step 4 obtains
2on colloidal crystal template, controlling temperature is 60 DEG C～80 DEG C, keeps 12h～24h, obtains PMMA composite membrane;
Six, it is 1%～3% HF that PMMA composite membrane step 5 being obtained is put into mass concentration, keeps 10h～12h, takes out PMMA composite membrane, then to be immersed in new mass concentration be, in 1%～3% HF, to keep 8h～10h; Dry up with ultrapure water washing and with nitrogen, then PMMA composite membrane is loaded on film stretching instrument, the temperature that film stretching instrument is set is 75 DEG C～85 DEG C, prepares colorful film.
Present embodiment adopts self-assembling technique, with PMMA/MMA solution casting SiO
2colloidal crystal template, then corrodes 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 in one direction certain orientation degree simultaneously, has retained its characteristic in three-dimensional structure field; Secondly the optical property of the caused uniqueness of this colorful film counter opal structure, it presents iris under visible ray, not only has broad application prospects in photonic crystal field, but also has had the characteristic of polymkeric substance.
Embodiment two: present embodiment is different from embodiment one: controlling stirring velocity in step 1 is 300rpm.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one: in step 1, the quality of L-arginine and the volume ratio of deionized water are 13mg: 10mL.Other is identical with embodiment one.
Embodiment four: present embodiment is different from embodiment one: SiO in step 4
2the mass concentration of colloid emulsion is 32%～38%.Other is identical with embodiment one.
Embodiment five: present embodiment is different from embodiment one: controlling temperature in step 4 is 30 DEG C.Other is identical with embodiment one.
Embodiment six: present embodiment is different from embodiment one: in step 5, the mass concentration of PMMA/MMA solution is 25%～35%.Other is identical with embodiment one.
Embodiment seven: present embodiment is different from one of embodiment one to six: in step 5, the mass concentration of PMMA/MMA solution is 30%.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from embodiment one: controlling temperature in step 5 is 65 DEG C～75 DEG C, keeps 14h～22h.Other is identical with embodiment one.
Embodiment nine: present embodiment is different from embodiment one: in step 6, the temperature of film stretching instrument is 78 DEG C～82 DEG C.Other is identical with embodiment one.
Embodiment ten: present embodiment is different from one of embodiment one to nine: in step 6, the temperature of film stretching instrument is 80 DEG C.Other is identical with one of embodiment one to nine.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment mono-:
The preparation method of a kind of colorful film of the present embodiment, specifically prepares according to following steps:
One, L-arginine and deionized water are mixed, then put into water-bath, by even to L-arginine and deionized water and stirring, then add hexanaphthene, obtain mixing solutions; Regulating bath temperature is 60 DEG C, and control stirring velocity is 300rpm, and mixing solutions is stirred, and then constant water bath temperature is 60 DEG C, and adds tetraethoxy, then stirs 20h, obtains SiO
2seed, wherein, the quality of L-arginine 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, the ammoniacal liquor that is 30% by dehydrated alcohol and mass concentration mixes, and then putting into temperature is the water-bath of 25 DEG C, then the SiO that adds step 1 to obtain
2seed, control stirring velocity is 200rpm, keeps 15min, then adds mixed liquor A and mixed liquid B, 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, ammoniacal liquor and dehydrated alcohol that mixed liquid B is 30% by deionized water, mass concentration form, and wherein the volume of deionized water is that the volume of 5.48mL, the mass concentration ammoniacal liquor that is 30% is that the volume of 8.22mL, dehydrated alcohol is 19.18mL;
Three, SiO step 2 being obtained
2colloid micro ball deionized water centrifuge washing 4 times, then use absolute ethanol washing, then centrifuge washing 5 times, drier, obtain dry SiO
2colloid micro ball;
Four, dry SiO step 3 being obtained
2colloid micro ball is dissolved in dehydrated alcohol, is mixed with mass concentration and is 35% SiO
2colloid emulsion, then vertically inserts SiO by substrate
2in colloid emulsion, controlling temperature is 30 DEG C, SiO
2after absolute ethanol volatilizes in colloid emulsion, take out substrate, obtain SiO
2colloidal crystal template, wherein substrate is glass substrate;
Five, PMMA/MMA solution is evenly cast in to the SiO that step 4 obtains
2on colloidal crystal template, controlling temperature is 80 DEG C, keeps 24h, obtains PMMA composite membrane;
Six, it is 2% HF that PMMA composite membrane step 5 being obtained is put into mass concentration, keeps 10h, takes out PMMA composite membrane, then to be immersed in new mass concentration be, in 2% HF, to keep 8h; Dry up with ultrapure water washing and with nitrogen, then PMMA composite membrane is loaded on film stretching instrument, the temperature that film stretching instrument is set is 80 DEG C, prepares colorful film.
As shown in Figure 1, wherein a represents redness to the digital photograph of colorful film prepared by the present embodiment, and 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 ray, and this film has unique optical property.
As shown in Figure 2, wherein a represents redness to the reflected light spectrogram of colorful film prepared by the present embodiment, and 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, then corrodes 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 in one direction certain orientation degree simultaneously, has retained its characteristic in three-dimensional structure field; Secondly the optical property of the caused uniqueness of this colorful film counter opal structure, it presents iris under visible ray, not only has broad application prospects in photonic crystal field, but also has had the characteristic of polymkeric substance.
Claims (10)
1. a preparation method for 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, then put into water-bath, by even to L-arginine and deionized water and stirring, then add hexanaphthene, obtain mixing solutions; Regulating bath temperature is 55 DEG C～65 DEG C, and control stirring velocity is 280rpm～320rpm, and mixing solutions is stirred, and then constant water bath temperature is 58 DEG C～62 DEG C, and adds tetraethoxy, then stirs 18h～24h, obtains SiO
2seed, wherein, the quality of L-arginine and the volume ratio of deionized water are (12～14) mg: (9～11) mL, the volume of hexanaphthene is 16mL～20mL, the volume of tetraethoxy is 20mL～24mL;
Two, the ammoniacal liquor that is 25%～30% by dehydrated alcohol and mass concentration mixes, and then puts into temperature and be the water-bath of 20 DEG C～30 DEG C, then the SiO that adds step 1 to obtain
2seed, control stirring velocity is 180rpm～220rpm, keeps 12min～18min, then adds mixed liquor A and mixed liquid B, 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 tetraethyl orthosilicate and dehydrated alcohol is (1～3): (3～5), ammoniacal liquor and dehydrated alcohol that mixed liquid B is 25%～30% by deionized water, mass concentration form, and wherein deionized water, ammoniacal liquor that mass concentration is 25%～30% and the volume ratio of dehydrated alcohol are (1～3): (2～4): (6～8);
Three, SiO step 2 being obtained
2colloid micro ball deionized water centrifuge washing 3～5 times, then use absolute ethanol washing, then centrifuge washing 4～6 times, drier, obtain dry SiO
2colloid micro ball;
Four, dry SiO step 3 being obtained
2colloid micro ball is dissolved in dehydrated alcohol, is mixed with mass concentration and is 30%～40% SiO
2colloid emulsion, then vertically inserts SiO by substrate
2in colloid emulsion, controlling temperature is 28 DEG C～32 DEG C, SiO
2after absolute ethanol volatilizes in colloid emulsion, take out substrate, obtain SiO
2colloidal crystal template, wherein substrate is glass substrate;
Five, PMMA/MMA solution is evenly cast in to the SiO that step 4 obtains
2on colloidal crystal template, controlling temperature is 60 DEG C～80 DEG C, keeps 12h～24h, obtains PMMA composite membrane;
Six, it is 1%～3% HF that PMMA composite membrane step 5 being obtained is put into mass concentration, keeps 10h～12h, takes out PMMA composite membrane, then to be immersed in new mass concentration be, in 1%～3% HF, to keep 8h～10h; Dry up with ultrapure water washing and with nitrogen, then PMMA composite membrane is loaded on film stretching instrument, the temperature that film stretching instrument is set is 75 DEG C～85 DEG C, prepares colorful film.
2. the preparation method of a kind of colorful film according to claim 1, is characterized in that in step 1, controlling stirring velocity is 300rpm.
3. the preparation method of a kind of colorful film according to claim 1, is characterized in that in step 1 that the quality of L-arginine and the volume ratio of deionized water are 13mg: 10mL.
4. the preparation method of a kind of colorful film according to claim 1, is characterized in that SiO in 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 in step 4, controlling temperature is 30 DEG C.
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 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 step 5 is 30%.
8. the preparation method of a kind of colorful film according to claim 1, is characterized in that in step 5, controlling temperature is 65 DEG C～75 DEG C, 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 step 6 is 78 DEG C～82 DEG C.
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 step 6 is 80 DEG C.
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| 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 |
| 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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| US20050270633A1 (en) * | 2004-05-14 | 2005-12-08 | Peter Herman | Photonic crystal mirrors for high-resolving power fabry perots |
| CN101655610B (en) * | 2009-09-11 | 2011-08-10 | 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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