CN103880017B - A kind of SiO 2-TiO 2the preparation method of two sized colloidal crystal - Google Patents
A kind of SiO 2-TiO 2the preparation method of two sized colloidal crystal Download PDFInfo
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- CN103880017B CN103880017B CN201410056612.2A CN201410056612A CN103880017B CN 103880017 B CN103880017 B CN 103880017B CN 201410056612 A CN201410056612 A CN 201410056612A CN 103880017 B CN103880017 B CN 103880017B
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- ammoniacal liquor
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Abstract
The invention discloses a kind of SiO
2-TiO
2the preparation method of two sized colloidal crystal, can obtain the SiO of periodically ordered arrangement
2-TiO
2two sized colloidal crystal, take LiCl as surface-modifying agent, tetraethoxy is that monodisperse silica nanosphere body particle prepared by raw material, take ITO as the silica colloidal crystal template that different arrangement architecture is prepared in electrode and substrate, filling with titanium sulfate is the gel that raw material is prepared, after drying through double-basis sheet and calcining, namely the restricted growth of titanium oxide in silica template obtain SiO
2-TiO
2two sized colloidal crystal.
Description
Technical field
The present invention relates to a kind of SiO
2-TiO
2the preparation method of two sized colloidal crystal.
Background technology
Photonic crystal is a kind of novel optical fine structure material of refractive index spatial mechanical periodicity.Wherein, the ordered 3 D structure that monodisperse colloid ball is each other arranged in periodic arrangement with certain spaced interval in certain medium is called colloidal crystal, the preparation method of colloidal crystal mainly comprises micro-machining process and self-assembly method, micro-machining process can process various types of materials, form various structure, but its complex process equipment, cost are high; And although self-assembly method processing unit is simple, cost is low, it limits to some extent to material, cannot obtain complete band gap material, and introduces the titania meterial with high-k, effectively can widen its optical band gap scope.Utilize the feature of Rapid self assembly and the introducing of dissimilar materials, not only there is the simple advantage of processing unit, also can effectively improve its performance.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, the object of the present invention is to provide a kind of SiO
2-TiO
2the preparation method of two sized colloidal crystal, can obtain New Si O
2-TiO
2two sized colloidal crystalline structure.
To achieve these goals, the technical solution used in the present invention is:
A kind of SiO
2-TiO
2the preparation method of two sized colloidal crystal, comprises the steps:
(1) the LiCl aqueous solution that mass concentration is 0.1% ~ 0.15% is prepared, configure the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor respectively, wherein solution A is equal with dehydrated alcohol amount in solution B, the volume ratio of dehydrated alcohol total amount and ammoniacal liquor is (5.6 ~ 12.5): 1, the consumption of ammoniacal liquor and the volume ratio of tetraethoxy are (1.5 ~ 3): 1, again the LiCl aqueous solution of 3 ~ 4mL is joined in solution B, the volume ratio of the LiCl aqueous solution and ammoniacal liquor is 1:(1 ~ 3), then do not stopping under stirring, solution A to be added in solution B, after reaction 20 ~ 22h, precipitation separation, in 50 ~ 60 DEG C of dryings after centrifuge washing, obtain the SiO of surface modification
2nanosphere body particle,
(2) SiO is weighed
2nano particle, by its ultrasonic disperse in organic solution, ultrasonic time is 2 ~ 3h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2% ~ 2.5%;
(3) two panels ITO slide be parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.4 ~ 0.5cm, logical 12 ~ 14V voltage on two ITO slides, with the speed of 0.5 ~ 0.6cm/min lift positive pole ITO slide after energising 40 ~ 50s, finally dries ITO slide in 60 DEG C and namely obtains SiO
2colloidal crystal template;
(4) taking a certain amount of citric acid is dissolved in massfraction 25 ~ 28% ammoniacal liquor, ammoniacal liquor is as the criterion can dissolve citric acid, add titanium sulfate, dehydrated alcohol and water successively again, namely precursor sol is obtained with ammoniacal liquor adjust pH to 7 ~ 10 after stirring and dissolving, wherein, the mole number of citric acid is 1 ~ 1.5 times of titanium sulfate mole number, the volume of the total consumption of ammoniacal liquor is 1.5 ~ 2 times of dehydrated alcohol volume, the volume of water is 1 ~ 1.2 times of dehydrated alcohol volume, evaporate 1 ~ 2h under 80 ~ 90 DEG C of water-baths after, by SiO
2colloidal crystal template immerses 5 ~ 10min in precursor sol at a certain angle, slowly lift out precursor solution excessive with adsorption paper removing surface after rete, the slide pressing a cleaning, drying at film surface forms double-basis sheet, dry after its horizontal positioned at 70 ~ 80 DEG C, after finally double-basis sheet being calcined 3 ~ 4h at 500 ~ 600 DEG C, namely obtain SiO
2-TiO
2two sized colloidal crystal.
Preferably, the organic solution in described step (2) is ethanol or methyl alcohol.SiO in described step (4)
2the immersion angle of colloidal crystal is be 45 ~ 60 degree with horizontal direction.
Compared with prior art, SiO provided by the invention
2-TiO
2in the preparation method of two sized colloidal crystal, take LiCl as the silica nanosphere body particle that surface-modifying agent prepares surface charge, be that silica colloidal crystal is prepared in electrode and substrate again with ITO,, the parameter such as voltage, pull rate, interelectrode distance charged by control surface can obtain the silica colloidal crystal template of different arrangement architecture and gap length, particularly have the non-close pile structure compared with wide arc gap, this is conducive to the filling of gel; Utilize the effect of gel citric acid that titanium ion can be made to be distributed in gel equably, and be filled in equably in the space of silica colloidal crystal template, utilize the volumetric shrinkage of gel in calcination process, and the limiting growth effect in template, make TiO
2homoepitaxial in a template, thus define orderly SiO
2-TiO
2two sized colloidal crystalline structure.
Embodiment
Embodiments of the present invention are described in detail below in conjunction with embodiment.
Embodiment 1
A kind of SiO
2-TiO
2the preparation method of two sized colloidal crystal, comprises the steps:
(1) the LiCl aqueous solution that mass concentration is 0.1% is prepared, configure the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor respectively, wherein solution A is equal with dehydrated alcohol amount in solution B, the volume ratio of dehydrated alcohol total amount and ammoniacal liquor is 5.6:1, the consumption of ammoniacal liquor and the volume ratio of tetraethoxy are 1.5:1, again the LiCl aqueous solution of 3mL is joined in solution B, the volume ratio of the LiCl aqueous solution and ammoniacal liquor is 1:1, then do not stopping under stirring, solution A to be added in solution B, after reaction 20h, precipitation separation, in 50 DEG C of dryings after centrifuge washing, obtain the SiO of surface modification
2nanosphere body particle,
(2) SiO is weighed
2nano particle, by its ultrasonic disperse in ethanol, ultrasonic time is 2h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2%;
(3) two panels ITO slide be parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.4cm, logical 12V voltage on two ITO slides, with the speed of 0.5cm/min lift positive pole ITO slide after energising 40s, finally dries ITO slide in 60 DEG C and namely obtains SiO
2colloidal crystal template;
(4) taking a certain amount of citric acid is dissolved in massfraction 25% ammoniacal liquor, ammoniacal liquor is as the criterion can dissolve citric acid, add titanium sulfate, dehydrated alcohol and water successively again, namely obtain precursor sol with ammoniacal liquor adjust pH to 7 after stirring and dissolving, wherein, the mole number of citric acid is equal with the mole number of titanium sulfate, the volume of the total consumption of ammoniacal liquor is 1.5 times of dehydrated alcohol volume, the volume of water is equal with dehydrated alcohol volume, evaporate 1h under 80 DEG C of water-baths after, by SiO
2colloidal crystal template immerses 5min in precursor sol at a certain angle, slowly lift out precursor solution excessive with adsorption paper removing surface after rete, the slide pressing a cleaning, drying at film surface forms double-basis sheet, dry after its horizontal positioned at 70 DEG C, after finally double-basis sheet being calcined 3h at 500 DEG C, namely obtain SiO
2-TiO
2two sized colloidal crystal.
Embodiment 2
A kind of SiO
2-TiO
2the preparation method of two sized colloidal crystal, comprises the steps:
(1) the LiCl aqueous solution that mass concentration is 0.15% is prepared, configure the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor respectively, wherein solution A is equal with dehydrated alcohol amount in solution B, the volume ratio of dehydrated alcohol total amount and ammoniacal liquor is 12.5:1, the consumption of ammoniacal liquor and the volume ratio of tetraethoxy are 3:1, again the LiCl aqueous solution of 4mL is joined in solution B, the volume ratio of the LiCl aqueous solution and ammoniacal liquor is 1:3, then do not stopping under stirring, solution A to be added in solution B, after reaction 22h, precipitation separation, in 60 DEG C of dryings after centrifuge washing, obtain the SiO of surface modification
2nanosphere body particle,
(2) SiO is weighed
2nano particle, by its ultrasonic disperse in methyl alcohol, ultrasonic time is 3h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2.5%;
(3) two panels ITO slide be parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.5cm, logical 14V voltage on two ITO slides, with the speed of 0.6cm/min lift positive pole ITO slide after energising 50s, finally dries ITO slide in 60 DEG C and namely obtains SiO
2colloidal crystal template;
(4) taking a certain amount of citric acid is dissolved in massfraction 28% ammoniacal liquor, ammoniacal liquor is as the criterion can dissolve citric acid, add titanium sulfate, dehydrated alcohol and water successively again, namely obtain precursor sol with ammoniacal liquor adjust pH to 7 ~ 10 after stirring and dissolving, wherein, the mole number of citric acid is 1.5 times of titanium sulfate mole number, the volume of the total consumption of ammoniacal liquor is 2 times of dehydrated alcohol volume, the volume of water is 1.2 times of dehydrated alcohol volume, evaporate 2h under 90 DEG C of water-baths after, by SiO
2colloidal crystal template immerses 10min in precursor sol at a certain angle, slowly lift out precursor solution excessive with adsorption paper removing surface after rete, the slide pressing a cleaning, drying at film surface forms double-basis sheet, dry after its horizontal positioned at 80 DEG C, after finally double-basis sheet being calcined 4h at 600 DEG C, namely obtain SiO
2-TiO
2two sized colloidal crystal.
Embodiment 3
A kind of SiO
2-TiO
2the preparation method of two sized colloidal crystal, comprises the steps:
(1) the LiCl aqueous solution that mass concentration is 0.125% is prepared, configure the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor respectively, wherein solution A is equal with dehydrated alcohol amount in solution B, the volume ratio of dehydrated alcohol total amount and ammoniacal liquor is 8.75:1, the consumption of ammoniacal liquor and the volume ratio of tetraethoxy are 2.25:1, again the LiCl aqueous solution of 3 ~ 4mL is joined in solution B, the volume ratio of the LiCl aqueous solution and ammoniacal liquor is 1:2.25, then do not stopping under stirring, solution A to be added in solution B, after reaction 21h, precipitation separation, in 55 DEG C of dryings after centrifuge washing, obtain the SiO of surface modification
2nanosphere body particle,
(2) SiO is weighed
2nano particle, by its ultrasonic disperse in ethanol, ultrasonic time is 2h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2.25%;
(3) two panels ITO slide be parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.45cm, logical 13V voltage on two ITO slides, with the speed of 0.55cm/min lift positive pole ITO slide after energising 45s, finally dries ITO slide in 60 DEG C and namely obtains SiO
2colloidal crystal template;
(4) taking a certain amount of citric acid is dissolved in massfraction 26.5% ammoniacal liquor, ammoniacal liquor is as the criterion can dissolve citric acid, add titanium sulfate, dehydrated alcohol and water successively again, namely obtain precursor sol with ammoniacal liquor adjust pH to 8 after stirring and dissolving, wherein, the mole number of citric acid is 1.25 times of titanium sulfate mole number, the volume of the total consumption of ammoniacal liquor is 1.72 times of dehydrated alcohol volume, the volume of water is 1.1 times of dehydrated alcohol volume, evaporate 1.5h under 85 DEG C of water-baths after, by SiO
2colloidal crystal template immerses 8min in precursor sol at a certain angle, slowly lift out precursor solution excessive with adsorption paper removing surface after rete, the slide pressing a cleaning, drying at film surface forms double-basis sheet, dry after its horizontal positioned at 75 DEG C, after finally double-basis sheet being calcined 3.5h at 550 DEG C, namely obtain SiO
2-TiO
2two sized colloidal crystal.
In the present invention, when the immersion angle of silica colloidal crystal is for being 45 ~ 60 degree with horizontal direction, effect is better.
Claims (1)
1. a SiO
2-TiO
2the preparation method of two sized colloidal crystal, is characterized in that, comprise the steps:
(1) the LiCl aqueous solution that mass concentration is 0.1% ~ 0.15% is prepared, configure the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor respectively, wherein solution A is equal with dehydrated alcohol amount in solution B, the volume ratio of dehydrated alcohol total amount and ammoniacal liquor is (5.6 ~ 12.5): 1, the consumption of ammoniacal liquor and the volume ratio of tetraethoxy are (1.5 ~ 3): 1, again the LiCl aqueous solution of 3 ~ 4mL is joined in solution B, the volume ratio of the LiCl aqueous solution and ammoniacal liquor is 1:(1 ~ 3), then do not stopping under stirring, solution A to be added in solution B, after reaction 20 ~ 22h, precipitation separation, in 50 ~ 60 DEG C of dryings after centrifuge washing, obtain the SiO of surface modification
2nanosphere body particle,
(2) SiO is weighed
2nano particle, by its ultrasonic disperse in organic solution, ultrasonic time is 2 ~ 3h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2% ~ 2.5%;
(3) two panels ITO slide be parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.4 ~ 0.5cm, logical 12 ~ 14V voltage on two ITO slides, with the speed of 0.5 ~ 0.6cm/min lift positive pole ITO slide after energising 40 ~ 50s, finally dries ITO slide in 60 DEG C and namely obtains SiO
2colloidal crystal template;
(4) taking a certain amount of citric acid is dissolved in massfraction 25 ~ 28% ammoniacal liquor, ammoniacal liquor is as the criterion can dissolve citric acid, add titanium sulfate, dehydrated alcohol and water successively again, namely precursor sol is obtained with ammoniacal liquor adjust pH to 7 ~ 10 after stirring and dissolving, wherein, the mole number of citric acid is 1 ~ 1.5 times of titanium sulfate mole number, the volume of the total consumption of ammoniacal liquor is 1.5 ~ 2 times of dehydrated alcohol volume, the volume of water is 1 ~ 1.2 times of dehydrated alcohol volume, evaporate 1 ~ 2h under 80 ~ 90 DEG C of water-baths after, by SiO
2colloidal crystal template immerses 5 ~ 10min in precursor sol at a certain angle, slowly lift out precursor solution excessive with adsorption paper removing surface after rete, the slide pressing a cleaning, drying at film surface forms double-basis sheet, dry after its horizontal positioned at 70 ~ 80 DEG C, after finally double-basis sheet being calcined 3 ~ 4h at 500 ~ 600 DEG C, namely obtain SiO
2-TiO
2two sized colloidal crystal;
Organic solution in described step (2) is ethanol or methyl alcohol;
SiO in described step (4)
2the immersion angle of colloidal crystal is be 45 ~ 60 degree with horizontal direction.
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CN101891207A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing SiO2/TiO2 composite powder |
CN101891206A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Preparation method of SiO2/TiO2 composite microspheres |
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CN101891207A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Method for preparing SiO2/TiO2 composite powder |
CN101891206A (en) * | 2010-07-21 | 2010-11-24 | 陕西科技大学 | Preparation method of SiO2/TiO2 composite microspheres |
Non-Patent Citations (3)
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Photonic crystal heterostructures fabricated by TiO2 and ZnO inverse opals using colloidal crystal template with single kind of microspheres;Yongna Zhang et al.;《Optical Materials》;20120517;第34卷(第11期);第1758-1761页 * |
PS/TiO2复合材料的蛋白石结构光子晶体制备及表征;汤荣年;《电子元件与材料》;20030930;第22卷(第9期);第45页左栏第2段到右栏第2段 * |
双尺寸超材料结构的设计及自组装;伍媛婷;《中国博士学位论文全文数据库 工程科技Ⅰ辑》;20130515(第5期);第31-33,50,71,98页 * |
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