CN103540926A - Light control SiO2/TiO2 composite micro-nano structure micro-channel valve and preparation method thereof - Google Patents
Light control SiO2/TiO2 composite micro-nano structure micro-channel valve and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a light control SiO2/TiO2 composite micro-nano structure micro-channel valve and a preparation method thereof. The preparation method comprises the following steps: firstly preparing a micro-channel sample for covering a SiO2 micro-structure, further treating and calcining a micro-channel at the temperature of 500 DEG C to prepare a dense SiO2/TiO2 composite micro-nano structure layer capillary; and finally soaking in a trimethylchlorosilane solution to perform surface modification on the micro-channel so as to obtain the light control SiO2/TiO2 composite micro-nano structure micro-channel valve target object. The method disclosed by the invention is simple and convenient, the time consumption is low, and special instruments are not required. The product disclosed by the invention has great capability of realizing ultraviolet light control over opening and closing of the micro-channel valve, and the valve is opened to allow water to pass after ultraviolet light irradiation; and compared with a single TiO2 nano structure light control micro-valve, the light control SiO2/TiO2 composite micro-nano structure micro-channel valve has the advantages that the water-repellent pressure is improved by 276.08% and the water-absorbent pressure is improved by 94.76%. The inner surface of the valve shows a lotus leaf-like surface structure wrapping micro-SiO2 microspheres with nano-TiO2 microspheres, so that the light control SiO2/TiO2 composite micro-nano structure micro-channel valve has a bright application prospects in the field of engineering.
Description
Technical field
The present invention relates to Chemical Process Equipment, especially microfluidic device field.
Background technology
Microfluidic device is due to its large mass transfer specific surface area and few reagent dosage, for rapid reaction and trace detection provide desirable means, at medicine food, chemical reaction and screening analysis field, has a wide range of applications.Micro-valve is in microfluidic device, to control one of mobile key component of fluid, by the ON/OFF response mode of valve, can be divided into active micro-valve and the micro-valve of passive-type.Wherein active micro-valve comprises the micro-valve of electromagnetism and the rotation valve etc. that declines; The micro-valve of passive-type comprises the micro-valve of electrochemistry, the micro-valve of thermal response and light-operated micro-valve etc.Light-operated micro-valve is as the Yi Ge branch of micro-valve research, to utilize illumination to change the volume size of micro-valve gel parts or the parent/hydrophobic property of microchannel internal surface, reach and control the mobile object of fluid, removed complicated external control system from, there is the advantage of untouchable control.But due to reasons such as technology of preparing and materials, the performance of the micro-valve of the light-operated parent that reported so far/hydrophobic conversion hysteria still can not meet the requirement of microfluidic control completely, trace it to its cause is light-operated micro-valve internal surface parent/hydrophobicity conversion insufficient strength, and the scope of reply flow rate of liquid is too narrow.Therefore, parent/hydrophobicity of strengthening light-operated micro-valve changes degree, improves and scolds water and water suction pressure, answers the scope of fluid flow rate for the micro-valve of lifting, the liquid residue of farthest avoiding valve part folding to cause, the performance and the practical application that improve light-operated valve are significant.
Based on above deficiency, if construct SiO in glass capillary base material
2/ TiO
2composite micro-nano rice structure microchannel valve, utilizes composite microstructure to strengthen the effect of light-operated parent/hydrophobic reversible transformation, certainly will greatly promote the switching effect of microfluid valve.With single TiO
2nanostructure is compared, composite S iO
2/ TiO
2the wetting property that micro nano structure can significantly be strengthened microchannel internal surface changes degree, promotes " ON/OFF " effect of the light-operated microchannel of UV valve.And the preparation method of this microchannel valve is simple, with low cost, raw material is easy to get, without complicated external control devices.But so far, yet there are no SiO
2/ TiO
2the relevant report of light-operated parent/hydrophobicity reversible transformation microchannel valve of composite micro-nano rice structure.
Summary of the invention
In view of the above deficiency of prior art, the present invention aims to provide a kind of SiO of light-operated parent/hydrophobicity reversible transformation
2/ TiO
2composite micro-nano rice structure microchannel valve and preparation method, make it to overcome the above shortcoming of prior art.
Object of the present invention realizes by following means.
1, a kind of light-operated SiO
2/ TiO
2composite micro-nano rice structure microchannel valve preparation method, is characterized in that, adopts following step:
(a) preparation of microchannel valve micrometer structure: 1) in reaction solution, each component volume ratio is ammoniacal liquor: ethanol: tetraethoxy=30:50:3, operation according to the following steps, mass ratio is that 25% ammoniacal liquor is added drop-wise in dehydrated alcohol, and 60 ℃ of constant temperature stir 30 minutes, more slowly drip tetraethoxy; Complete rear continuation keeps 60 ℃ of constant temperature to stir 90 minutes to obtain SiO
2microballoon dispersion liquid; 2) glass capillary is put into the sulfuric acid lotion of 90 ℃ and is soaked taking-up in 30 minutes, deionized water is cleaned, cold wind after drying up will, above-mentioned microballoon dispersion liquid is immersed in its one end, treats that dispersion liquid rises to exceed dispersion liquid liquid level 3cm place, block the kapillary the other end, keep the interior liquid level stabilizing of kapillary 30 seconds, take out and suck inside residual, be placed in 220 ℃ of retort furnaces and calcine 2 hours, repeat this step 2 time, obtain fine and close SiO
2micrometer structure;
(b) preparation of microchannel valve composite micro-nano rice structure: 1) in reaction solution, each component volume ratio is butyl (tetra) titanate: ethanol: water: Glacial acetic acid=9:36:12:40, operation according to the following steps, it is in 95% ethanolic soln that butyl (tetra) titanate reagent is joined to volume percent, stir after 5～10 minutes and be added drop-wise in the deionized water and Glacial acetic acid mixing solutions under whipped state, continue to stir, until mixed solution, by muddy bleach, then obtains TiO for standing 30 hours
2dispersion liquid; 2) get the fine and close SiO that has that (a) step obtains
2after the kapillary sulfuric acid lotion of micrometer structure cleans; Above-mentioned TiO is immersed in one end
2dispersion liquid, treats that dispersion liquid rises to and exceeds dispersion liquid liquid level 3cm place, blocks the kapillary the other end, keeps in kapillary liquid level stabilizing 30 seconds, takes out and suck inner residual, is placed in 500 ℃ of retort furnaces and calcines 30 minutes, repeats this step 2 time, makes fine and close SiO
2/ TiO
2composite micro-nano rice structural sheet kapillary;
(c) modification of microchannel valve composite micro-nano rice structure: get the fine and close SiO that has that (b) step obtains
2/ TiO
2composite micro-nano rice structural sheet kapillary, one end is immersed in trimethylchlorosilane solution, guarantees the complete submergence composite micro-nano of solution rice structure, and sealing was statically placed in dark place after 2 hours, removed and sealed and be placed in 50 ℃ of oven dry of baking oven; In dark place, place 15～20 minutes again, after sample is cooling, obtain the light-operated SiO of target compound
2/ TiO
2composite micro-nano rice structure microchannel valve.
Another object of the present invention is to adopt aforesaid method to obtain a kind of light-operated SiO
2/ TiO
2composite micro-nano rice structure microchannel valve.
Adopt the inventive method to obtain the SiO of light-operated parent/hydrophobicity reversible transformation
2/ TiO
2composite micro-nano rice structure microchannel valve invention product, there is the light-operated micro-valve of good ultraviolet " unlatching " and " closing " reversible transformation ability, faint ultraviolet luminous energy causes that micro-valve water suction pressure+509.1Pa(opens) with scold hydraulic pressure strong-95.9Pa(closes) conversion, and above-mentioned light-operated micro-valve switch ability is through repeatedly repeatedly still unattenuated after ultraviolet/dark cycle.Compare single TiO
2light-operated micro-valve of nanostructure, it scolds hydraulic pressure to improve by force 276.08%, and water suction pressure has improved 94.76%.The method of the micro-valve of light-operated parent/hydrophobic conversion hysteria of preparation was compared in the past, and the preparation method of this valve is easier, expended time in few, did not need specific apparatus, was also applicable to the preparation of other inorganic materials microchannel valve.Micro-valve internal surface presents nano-TiO
2microballoon parcel micron SiO
2the class lotus leaf surface structure of microballoon has a good application prospect in engineering field.This kind of light-operated composite micro-nano rice structure microchannel valve is mainly hydroxyl and the SiO that relies on microchannel surface
2, TiO
2by chemical bonded refractory, be combined, before this by electroless plating micron order SiO
2microballoon is to substrate surface, then TiO
2nano particle is wrapped in SiO again
2microsphere surface, so microchannel valve has composite micro-nano rice structure, (shown in accompanying drawing).After trimethylchlorosilane modification, the hydrophobic significant part of micro-valve is methyl group, and this group has stronger hydrophobic performance; That play valve switch transition function is TiO
2, UV-irradiation makes it produce both hole and electron, brings out near the H of coating
2o becomes hydroxyl; Moreover the constructed class lotus leaf composite micro-nano rice structure of microchannel valve make micro-valve parent/hydrophobic conversion " ON/OFF " ability further strengthen.
Accompanying drawing is described as follows:
Accompanying drawing 1 is the valve of product of the present invention " ON/OFF " design sketch; (a) the microchannel valve " pass " before UV illumination, (b) the composite micro-nano rice structure before UV illumination is hydrophobic state; (c) the microchannel valve after UV illumination " is opened ", and (d) the composite micro-nano rice structure after UV illumination is hydrophily.
Embodiment
Below in conjunction with accompanying drawing, enforcement of the present invention is further described.But should be emphasized that, embodiment is below exemplary, rather than in order to limit the scope of the invention and to apply.In processing step, related chemical feedstocks and reagent are conventional commercially available technical pure.
Embodiment 1
By 25%(W/W) ammoniacal liquor 30mL drops in 50mL dehydrated alcohol, and 400 revs/min of temperature constant magnetic stirrings are 30 minutes at 60 ℃; Slowly drip again 3mL tetraethoxy, continue constant temperature and stir 90 minutes, get final product to obtain SiO
2microballoon dispersion liquid.The internal diameter that Piranha solution-treated is crossed is that above-mentioned microballoon dispersion liquid is immersed in glass capillary one end of 500 μ m, treating that dispersion liquid rises to exceeds liquid level 3cm place, keep kapillary 30 seconds, take out and suck inner residual, being placed in 220 ℃ of retort furnaces calcines 2 hours, repeat this step 2 time, can obtain fine and close SiO
2micrometer structure.
To deposit SiO
2the kapillary of microballoon is put into 90 ℃ of Piranha solution constant temperature and is soaked 90 minutes, cleans, dries stand-by; 9mL butyl (tetra) titanate is added drop-wise in 95% ethanol of 36mL, continue stirs, be then added dropwise in the 12mL deionized water and 40mL Glacial acetic acid mixed solution under whipped state, be stirred to transparently, ageing 30 hours, obtains TiO
2microballoon dispersion liquid; What upper step was processed deposits SiO
2tiO is immersed in kapillary one end of microballoon
2in microballoon dispersion liquid, treat that dispersion liquid rises to and exceed liquid level 3cm place, keep kapillary 30s, take out and suck inner residual, be placed in 500 ℃ of retort furnaces and process 30 minutes, repeat this step 2 time, can obtain fine and close SiO
2/ TiO
2composite micro-nano rice structure.
Will be with SiO
2/ TiO
2kapillary one end immersion 13%(v/v of composite micro-nano rice structure) in trimethylchlorosilane-hexane solution, guarantee the complete submergence composite micro-nano of solution rice structure microchannel, seal standing 2 hours; Take out kapillary and be placed in 50 ℃ of oven dry of baking oven, obtain the SiO of trimethylchlorosilane modification
2/ TiO
2composite micro-nano rice structure microchannel valve.
As shown in accompanying drawing (a), the aqueous solution of the rhodamine B that constant flow pump pushes can pass through blank kapillary microchannel, and the SiO of trimethylchlorosilane modification
2/ TiO
2composite micro-nano rice structure microchannel valve is hydrophobicity, and valve is in " closing " state, and the liquid that constant flow pump pushes can not pass through microchannel valve; After modification microchannel valve is irradiated under the ultraviolet lamp of 12W, valve presents " unlatching " state, constant flow pump pushes liquid with identical speed and passes through device, as shown in accompanying drawing (b), the rhodamine B aqueous solution can not only pass through blank microchannel, also can flow out by the composite micro-nano rice structure microchannel valve of trimethylchlorosilane modification; Under dark condition, place after a few hours, due to TiO
2the loss of surface-OH, composite micro-nano rice structure microchannel valve reverts to again hydrophobic (closing) state gradually.Through 5 times, illumination/dark cycle experimental result is identical repeatedly.Visible, the composite micro-nano rice structure microchannel valve of this research preparation has UV light-operated reversible " ON/OFF " effect.
This coating has the light-operated close and distant water of good ultraviolet and close and distant oily reversible transformation ability, the micro-valve of faint ultraviolet luminous energy water suction pressure+509.1Pa(opens) with scold hydraulic pressure strong-95.9Pa(closes) conversion, and above-mentioned light-operated micro-valve switch ability is through repeatedly repeatedly still unattenuated after ultraviolet/dark cycle.Compare single TiO
2light-operated micro-valve of nanostructure, it scolds hydraulic pressure to improve by force 276.08%, and water suction pressure has improved 94.76%.By the electric Microscopic observation of transmitting on the scene, find, a lot of beads are wrapped in large ball proper alignment at micro-valve internal surface.Large ball is SiO
2, diameter is about 150～200nm, the regular bottom that is arranged in; Bead is TiO
2, diameter is about 10～20nm, is wrapped in SiO dispersedly
2the surface of ball.This coating has the composite micro-nano rice structure of similar lotus leaf surface.Exactly because there is the surface topography of this composite micro-nano rice structure, make this micro-valve there is well light-operated " ON/OFF " transfer capability.The SiO of bottom
2large ball makes micro-valve internal have larger specific surface area, can deposit more TiO
2nano particle.Valve closes before illumination, forms air cushion between adjacent two nanometer beads of composite micro-nano rice structure, steadily oil droplet or water droplet is held up, and has strengthened micro-valve hydrophobic performance; Valve opening after illumination, forms nanotube capillaries between adjacent two nanometer beads, has further strengthened the hydrophilicity of micro-valve.
The SiO of the present invention obtains light-operated close and distant/water reversible transformation
2/ TiO
2microchannel valve is significant in chemical process fluid machinery research field.This achievement in research has very wide application prospect in gene delivery, the conveying of free of losses liquid, contactless Long-distance Control, microfluid, biochip, medicament slow release, field of petrochemical industry.
Claims (2)
1. a light-operated SiO
2/ TiO
2composite micro-nano rice structure microchannel valve preparation method, is characterized in that, adopts following step:
(a) preparation of microchannel valve micrometer structure: 1) in reaction solution, each component volume ratio is ammoniacal liquor: ethanol: tetraethoxy=30:50:3, operation according to the following steps, mass ratio is that 25% ammoniacal liquor is added drop-wise in dehydrated alcohol, and 60 ℃ of constant temperature stir 30 minutes, more slowly drip tetraethoxy; Complete rear continuation keeps 60 ℃ of constant temperature to stir 90 minutes to obtain SiO
2microballoon dispersion liquid; 2) glass capillary is put into the sulfuric acid lotion of 90 ℃ and is soaked taking-up in 30 minutes, deionized water is cleaned, cold wind after drying up will, above-mentioned microballoon dispersion liquid is immersed in its one end, treats that dispersion liquid rises to exceed dispersion liquid liquid level 3cm place, block the kapillary the other end, keep the interior liquid level stabilizing of kapillary 30 seconds, take out and suck inside residual, be placed in 220 ℃ of retort furnaces and calcine 2 hours, repeat this step 2 time, obtain fine and close SiO
2micrometer structure;
(b) preparation of microchannel valve composite micro-nano rice structure: 1) in reaction solution, each component volume ratio is butyl (tetra) titanate: ethanol: water: Glacial acetic acid=9:36:12:40, operation according to the following steps, it is in 95% ethanolic soln that butyl (tetra) titanate reagent is joined to volume percent, stir after 5～10 minutes and be added drop-wise in the deionized water and Glacial acetic acid mixing solutions under whipped state, continue to stir, until mixed solution, by muddy bleach, then obtains TiO for standing 30 hours
2dispersion liquid; 2) get the fine and close SiO that has that (a) step obtains
2after the kapillary sulfuric acid lotion of micrometer structure cleans; Above-mentioned TiO is immersed in one end
2dispersion liquid, treats that dispersion liquid rises to and exceeds dispersion liquid liquid level 3cm place, blocks the kapillary the other end, keeps in kapillary liquid level stabilizing 30 seconds, takes out and suck inner residual, is placed in 500 ℃ of retort furnaces and calcines 30 minutes, repeats this step 2 time, makes fine and close SiO
2/ TiO
2composite micro-nano rice structural sheet kapillary;
(c) modification of microchannel valve composite micro-nano rice structure: get the fine and close SiO that has that (b) step obtains
2/ TiO
2composite micro-nano rice structural sheet kapillary, one end is immersed in trimethylchlorosilane solution, guarantees the complete submergence composite micro-nano of solution rice structure, and sealing was statically placed in dark place after 2 hours, removed and sealed and be placed in 50 ℃ of oven dry of baking oven; In dark place, place 15～20 minutes again, after sample is cooling, obtain the light-operated SiO of target compound
2/ TiO
2composite micro-nano rice structure microchannel valve.
2. a light-operated SiO
2/ TiO
2composite micro-nano rice structure microchannel valve, is characterized in that, adopts the light-operated SiO described in claim 1
2/ TiO
2the preparation method of composite micro-nano rice structure microchannel valve makes.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881422A (en) * | 2014-03-21 | 2014-06-25 | 西南交通大学 | Light-operated switch type TiO2 nano-particles surfactant and preparation method thereof |
| CN104841345A (en) * | 2015-04-21 | 2015-08-19 | 西南交通大学 | Photomagnetic dual-response Pickering emulsion coalescence reaction system and application thereof |
| CN104941553A (en) * | 2015-06-12 | 2015-09-30 | 衢州学院 | Preparation method for nano-TiO2 modified micro-channel reactor |
| CN113775818A (en) * | 2020-06-10 | 2021-12-10 | 南京工业大学 | Microfluid control valve based on controllable wetting gradient surface |
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| CN102503554A (en) * | 2011-11-02 | 2012-06-20 | 西南交通大学 | Method for preparing oil-water-soaked light-operated reversible SiO2/TiO2 composite coating on silicon substrate surface |
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| CN102503554A (en) * | 2011-11-02 | 2012-06-20 | 西南交通大学 | Method for preparing oil-water-soaked light-operated reversible SiO2/TiO2 composite coating on silicon substrate surface |
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| WEI LI，ET AL.: "Enhanced reversible wettability conversion of micro-nano hierarchical TiO2/SiO2 composite films under UV irradiation", 《APPLIED SURFACE SCIENCE》 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881422A (en) * | 2014-03-21 | 2014-06-25 | 西南交通大学 | Light-operated switch type TiO2 nano-particles surfactant and preparation method thereof |
| CN103881422B (en) * | 2014-03-21 | 2015-04-22 | 西南交通大学 | Light-operated switch type TiO2 nano-particles surfactant and preparation method thereof |
| CN104841345A (en) * | 2015-04-21 | 2015-08-19 | 西南交通大学 | Photomagnetic dual-response Pickering emulsion coalescence reaction system and application thereof |
| CN104941553A (en) * | 2015-06-12 | 2015-09-30 | 衢州学院 | Preparation method for nano-TiO2 modified micro-channel reactor |
| CN104941553B (en) * | 2015-06-12 | 2017-03-01 | 衢州学院 | The preparation method of the micro passage reaction that nano titanium oxide is modified |
| CN113775818A (en) * | 2020-06-10 | 2021-12-10 | 南京工业大学 | Microfluid control valve based on controllable wetting gradient surface |
| CN113775818B (en) * | 2020-06-10 | 2022-06-03 | 南京工业大学 | Microfluid control valve based on controllable wetting gradient surface |
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Application publication date: 20140129 |