CN103880017A - Preparation method of SiO2-TiO2 double-size colloidal crystals - Google Patents
Preparation method of SiO2-TiO2 double-size colloidal crystals Download PDFInfo
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- CN103880017A CN103880017A CN201410056612.2A CN201410056612A CN103880017A CN 103880017 A CN103880017 A CN 103880017A CN 201410056612 A CN201410056612 A CN 201410056612A CN 103880017 A CN103880017 A CN 103880017A
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Abstract
The invention discloses a preparation method of SiO2-TiO2 double-size colloidal crystals. The preparation method disclosed by the invention comprises the following steps of: obtaining SiO2-TiO2 double-size colloidal crystals arranged periodically in an ordered manner, preparing monodispersed silicon dioxide spherical nanoparticles by taking LiCl as the surface modifier and ethyl orthosilicate as the raw material, preparing silicon dioxide colloidal crystal templates having different arrangement structures by taking ITO as the electrode and the substrate, filling gel prepared by taking titanous sulphate as the raw material, after drying and burning double substrates, restrictedly growing titanium oxide in a silicon dioxide template, and then, obtaining the SiO2-TiO2 double-size colloidal crystals.
Description
Technical field
The present invention relates to a kind of SiO
2-TiO
2the preparation method of two size colloidal crystals.
Background technology
Photonic crystal is the novel optical fine structure material changing in a kind of refractive index spatial cycle.Wherein, the ordered 3 D structure that single dispersoid ball is arranged in periodic arrangement with certain spaced interval each other in certain medium is called colloidal crystal, the preparation method of colloidal crystal mainly comprises microfabrication method and self-assembly method, microfabrication method can be processed various types of materials, form various structures, but its complex process equipment, cost are high; Although and self-assembly method processing unit is simple, cost is low, it limits to some extent to material, cannot obtain complete band gap material, and introduce the titania meterial with high-k, can effectively 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 size colloidal crystals, can obtain New Si O
2-TiO
2two size colloidal crystal structures.
To achieve these goals, the technical solution used in the present invention is:
A kind of SiO
2-TiO
2the preparation method of two size colloidal crystals, comprises the steps:
(1) the LiCl aqueous solution that preparation mass concentration is 0.1%～0.15%, configure respectively the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor, wherein solution A equates 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 stop stir under solution A is added in solution B, after reaction 20～22h, precipitation separation, dry in 50～60 ℃ after centrifuge washing, obtain the SiO of surface modification
2nanometer spherical particles,
(2) weigh SiO
2nano particle, by its ultrasonic being scattered in organic solution, ultrasonic time is 2～3h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2%～2.5%;
(3) two ITO slides are parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.4～0.5cm, and logical 12～14V voltage on two ITO slides, lifts anodal ITO slide with the speed of 0.5～0.6cm/min after energising 40～50s, finally dries ITO slide in 60 ℃ and 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 successively again titanium sulfate, dehydrated alcohol and water, after stirring and dissolving, obtain precursor sol with ammoniacal liquor adjust pH to 7～10, 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, under 80～90 ℃ of water-baths, evaporate after 1～2h, by SiO
2colloidal crystal template immerses 5～10min in precursor sol at a certain angle, slowly lift out after rete and remove the excessive precursor solution in surface with adsorption paper, the slide that presses a cleaning, drying at film surface forms double-basis sheet, will be after its horizontal positioned at 70～80 ℃, dry, obtain SiO after finally double-basis sheet being calcined to 3～4h at 500～600 ℃
2-TiO
2two size colloidal crystals.
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 for being 45～60 degree with horizontal direction.
Compared with prior art, SiO provided by the invention
2-TiO
2in the preparation method of two size colloidal crystals, prepare the silica nanosphere body particle of surface charge take LiCl as surface-modifying agent, again take ITO as electrode and substrate prepare silica colloidal crystal, the parameters such as, voltage charged by control surface, pull rate, interelectrode distance can obtain the silica colloidal crystal template of different arrangement architectures and gap length, the non-close pile structure particularly with larger gap, this is conducive to the filling of gel; Utilize the effect of gel citric acid can make titanium ion 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 limiting growth effect in template, make TiO
2evenly growth in template, thus orderly SiO formed
2-TiO
2two size colloidal crystal structures.
Embodiment
Describe embodiments of the present invention in detail below in conjunction with embodiment.
Embodiment 1
A kind of SiO
2-TiO
2the preparation method of two size colloidal crystals, comprises the steps:
(1) the LiCl aqueous solution that preparation mass concentration is 0.1%, configure respectively the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor, wherein solution A equates 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 stop stir under solution A is added in solution B, after reaction 20h, precipitation separation, dry in 50 ℃ after centrifuge washing, obtain the SiO of surface modification
2nanometer spherical particles,
(2) weigh SiO
2nano particle, by its ultrasonic being scattered in ethanol, ultrasonic time is 2h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2%;
(3) two ITO slides are parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.4cm, and logical 12V voltage on two ITO slides, lifts anodal ITO slide with the speed of 0.5cm/min after energising 40s, finally dries ITO slide in 60 ℃ and 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 successively again titanium sulfate, dehydrated alcohol and water, after stirring and dissolving, obtain precursor sol with ammoniacal liquor adjust pH to 7, wherein, the mole number of citric acid equates 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 equates with dehydrated alcohol volume, evaporates after 1h, by SiO under 80 ℃ of water-baths
2colloidal crystal template immerses 5min in precursor sol at a certain angle, slowly lift out after rete and remove the excessive precursor solution in surface with adsorption paper, the slide that presses a cleaning, drying at film surface forms double-basis sheet, will be after its horizontal positioned at 70 ℃, dry, obtain SiO after finally double-basis sheet being calcined to 3h at 500 ℃
2-TiO
2two size colloidal crystals.
Embodiment 2
A kind of SiO
2-TiO
2the preparation method of two size colloidal crystals, comprises the steps:
(1) the LiCl aqueous solution that preparation mass concentration is 0.15%, configure respectively the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor, wherein solution A equates 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 stop stir under solution A is added in solution B, after reaction 22h, precipitation separation, dry in 60 ℃ after centrifuge washing, obtain the SiO of surface modification
2nanometer spherical particles,
(2) weigh SiO
2nano particle, by its ultrasonic being scattered in methyl alcohol, ultrasonic time is 3h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2.5%;
(3) two ITO slides are parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.5cm, and logical 14V voltage on two ITO slides, lifts anodal ITO slide with the speed of 0.6cm/min after energising 50s, finally dries ITO slide in 60 ℃ and 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 successively again titanium sulfate, dehydrated alcohol and water, after stirring and dissolving, obtain precursor sol with ammoniacal liquor adjust pH to 7～10, 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, evaporates after 2h, by SiO under 90 ℃ of water-baths
2colloidal crystal template immerses 10min in precursor sol at a certain angle, slowly lift out after rete and remove the excessive precursor solution in surface with adsorption paper, the slide that presses a cleaning, drying at film surface forms double-basis sheet, will be after its horizontal positioned at 80 ℃, dry, obtain SiO after finally double-basis sheet being calcined to 4h at 600 ℃
2-TiO
2two size colloidal crystals.
Embodiment 3
A kind of SiO
2-TiO
2the preparation method of two size colloidal crystals, comprises the steps:
(1) the LiCl aqueous solution that preparation mass concentration is 0.125%, configure respectively the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor, wherein solution A equates 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 stop stir under solution A is added in solution B, after reaction 21h, precipitation separation, dry in 55 ℃ after centrifuge washing, obtain the SiO of surface modification
2nanometer spherical particles,
(2) weigh SiO
2nano particle, by its ultrasonic being scattered in ethanol, ultrasonic time is 2h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2.25%;
(3) two ITO slides are parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.45cm, and logical 13V voltage on two ITO slides, lifts anodal ITO slide with the speed of 0.55cm/min after energising 45s, finally dries ITO slide in 60 ℃ and 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 successively again titanium sulfate, dehydrated alcohol and water, after stirring and dissolving, obtain precursor sol with ammoniacal liquor adjust pH to 8, 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, evaporates after 1.5h, by SiO under 85 ℃ of water-baths
2colloidal crystal template immerses 8min in precursor sol at a certain angle, slowly lift out after rete and remove the excessive precursor solution in surface with adsorption paper, the slide that presses a cleaning, drying at film surface forms double-basis sheet, will be after its horizontal positioned at 75 ℃, dry, obtain SiO after finally double-basis sheet being calcined to 3.5h at 550 ℃
2-TiO
2two size colloidal crystals.
In the present invention, when the immersion angle of silica colloidal crystal is for being 45～60 while spending with horizontal direction, effect is better.
Claims (3)
1. a SiO
2-TiO
2the preparation method of two size colloidal crystals, is characterized in that, comprises the steps:
(1) the LiCl aqueous solution that preparation mass concentration is 0.1%～0.15%, configure respectively the ethanolic soln A of tetraethoxy and the ethanolic soln B of ammoniacal liquor, wherein solution A equates 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 stop stir under solution A is added in solution B, after reaction 20～22h, precipitation separation, dry in 50～60 ℃ after centrifuge washing, obtain the SiO of surface modification
2nanometer spherical particles,
(2) weigh SiO
2nano particle, by its ultrasonic being scattered in organic solution, ultrasonic time is 2～3h, obtains SiO
2particle suspension liquid, the massfraction of its particle is 2%～2.5%;
(3) two ITO slides are parallel to each other and vertically immerse SiO
2in particle suspension liquid, wherein, the spacing of two ITO slides is 0.4～0.5cm, and logical 12～14V voltage on two ITO slides, lifts anodal ITO slide with the speed of 0.5～0.6cm/min after energising 40～50s, finally dries ITO slide in 60 ℃ and 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 successively again titanium sulfate, dehydrated alcohol and water, after stirring and dissolving, obtain precursor sol with ammoniacal liquor adjust pH to 7～10, 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, under 80～90 ℃ of water-baths, evaporate after 1～2h, by SiO
2colloidal crystal template immerses 5～10min in precursor sol at a certain angle, slowly lift out after rete and remove the excessive precursor solution in surface with adsorption paper, the slide that presses a cleaning, drying at film surface forms double-basis sheet, will be after its horizontal positioned at 70～80 ℃, dry, obtain SiO after finally double-basis sheet being calcined to 3～4h at 500～600 ℃
2-TiO
2two size colloidal crystals.
2. SiO according to claim 1
2-TiO
2the preparation method of two size colloidal crystals, is characterized in that, the organic solution in described step (2) is ethanol or methyl alcohol.
3. SiO according to claim 1
2-TiO
2the preparation method of two size colloidal crystals, is characterized in that, SiO in described step (4)
2the immersion angle of colloidal crystal is for being 45～60 degree with horizontal direction.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106622107A (en) * | 2016-12-01 | 2017-05-10 | 湖北硅金凝节能减排科技有限公司 | Preparation method of TiO2/SiO2 composite aerogel |
| CN106669588A (en) * | 2016-12-01 | 2017-05-17 | 湖北硅金凝节能减排科技有限公司 | Preparation method of TiO2/SiO2 composite aerogel |
| CN107285323A (en) * | 2017-07-21 | 2017-10-24 | 南京航空航天大学 | A kind of silicon dioxide microsphere preparation method of high dispersive and size tunable |
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| JPS60246225A (en) * | 1984-05-21 | 1985-12-05 | Hisanori Bando | Ferric oxide particle powder and its production |
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|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106622107A (en) * | 2016-12-01 | 2017-05-10 | 湖北硅金凝节能减排科技有限公司 | Preparation method of TiO2/SiO2 composite aerogel |
| CN106669588A (en) * | 2016-12-01 | 2017-05-17 | 湖北硅金凝节能减排科技有限公司 | Preparation method of TiO2/SiO2 composite aerogel |
| CN107285323A (en) * | 2017-07-21 | 2017-10-24 | 南京航空航天大学 | A kind of silicon dioxide microsphere preparation method of high dispersive and size tunable |
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