CN101475206A - Method for preparing ZnO nanorod with controllable distribution by growing in microchannel - Google Patents
Method for preparing ZnO nanorod with controllable distribution by growing in microchannel Download PDFInfo
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Abstract
The invention relates to a preparation method for growing ZnO nano-rods with controllable distribution in a micro-channel, which comprises the steps of: taking a glass capillary as the micro-channel, soluble zinc salt and alkali as initial raw materials, and deionized water as a solvent, adding CTAB, normal butanol and an organic solvent to configure an inverse microemulsion, utilizing a microinjection pump to convey the microemulsion to the micro-channel arranged in a baking oven, and growing ZnO seed crystals with good dispersivity on a substrate; and then taking the soluble zinc salt and amine as raw materials and the deionized water as the solvent to configure a reaction liquid, conveying the reaction liquid into the pre-fabricated glass capillary with the seed crystals, and obtaining the ZnO nano-rods with controllable distribution after the fluid transportation. The preparation method combines the preparation of one-dimension nano-materials and the modification of micro-fluidic channels, can obtain a ZnO nano-rod array with controllable distribution without any patterned technology or template, and provides an approach with convenience, universality, simple process and small consumption for the modification of geometric structures of inner surfaces of the micro-fluidic channels.
Description
Technical field
The invention belongs to the preparation field of ZnO nanometer rod, particularly relate to the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel.
Background technology
In more than ten years in the past, micro-fluidic device has demonstrated great application prospect in the synthetic fields such as (as making up synthetic and high flux screening) of life science (as medicinal design, conveying, detection and medical diagnosis on disease) and industry.And along with the increase for particular demands such as the structurizing of microfluidic system, functionalization, inevitable requirement is carried out modification to the internal surface of microchannel.Various micro-/ nano manufacturing technologies such as micromachined, photoetching technique etc. have been used to make micro to reach the purpose of modification on the microchannel.But these methods all can not be implemented under the nanoscale modification to the microchannel, and are difficult to be applied in microchannel sealing, that have only narrow and small gangway, in kapillary.In addition, these methods are applied in the open microchannel, all need sealing technology just can become a complete microchannel at last, so also will certainly cause destruction established micro.Thereby seek under nanoscale, be applicable to that the Micro Channel Architecture method of modifying that has only narrow and small gangway is necessary very much simultaneously.
The 21 century the reach of science is integrated as a big research focus with the nano material assembling of one dimension ordered arrangement, and specific one dimension micro is integrated in the microchannel, can give the new function of micro-/ nano device that these monodimension nanometer materials are formed.Zinc oxide is because the different habits of the anisotropy of its crystalline structure, each crystal face and higher energy gap (3.37eV) and bigger exciton bind energy (60meV) make it have excellent semiconducting behavior such as piezoelectricity, light transfer characteristic.The one dimension Nano structure of zinc oxide such as nanometer rod, nanotube etc. are to the device application development, as WangZ.L in 2007 etc. in the Science above-reported ZnO nano generator (Science, 2007.316 (5821): p.102-105.).
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel, this preparation method combines the preparation of monodimension nanometer material and modification, the modification of microfluidic channel, without any need for patterning techniques or the template ZnO nanometer stick array that promptly obtained controlled distribution; Be the geometry modification of microfluidic channel internal surface, provide a convenience, general, process simple, expend little approach.
The preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel of the present invention comprises:
(1) cleaning of microchannel
As the microchannel, prepare washing lotion I (V with glass capillary
The vitriol oil: V
Hydrogen peroxide: V
Distilled water=4:1:20) and washing lotion II (V
Ammoniacal liquor: V
Two Oxygen water: V
Distilled water=1:4:20), the microchannel is soaked among the washing lotion I at 110～130 ℃ of 10～30min down, behind the deionized water rinsing, again the microchannel is soaked among the washing lotion II and soaks 10～30min down at 60～80 ℃, behind the last deionized water rinsing, oven dry;
(2) disperse the preparation of controlled crystal seed in the microchannel
The Zinc diacetate dihydrate solution of preparation 0.001～0.01M, 0.004 the sodium hydroxide solution of～0.04M, dispose two portions of mixed solutions of forming by 2g CTAB, 12.8mL octane, 5mL propyl carbinol (is 26.67%:13.33%:60% according to CTAB, propyl carbinol, octane mass ratio), the Zinc diacetate dihydrate solution that in mixed solution wherein, adds 0.4～1.0mL, the sodium hydroxide solution that adds 0.4～1.0mL in another mixed solution obtains two kinds of transparent reverse micro emulsions under the ultrasonication.Two reverse micro emulsions suck the syringe of two 10mL respectively, it is 5～50 μ L/min that the setting micro syringe pump pushes away speed, it is transported to the microchannel that the step (1) that places 30～80 ℃ of baking ovens was in advance cleaned simultaneously, fluid stops to carry after carrying 10～60min, oven temperature is increased to 150～200 ℃, time 1～2h realizes that high temperature goes emulsifying effect.Successively utilize volume ratio to be the ethanol of 1:1 and acetone mixed solution, washed with de-ionized water microchannel, and, on the internal surface of microchannel, obtain the ZnO crystal seed at 150 ℃ of oven dry 1～2h down;
(3) distribute in the microchannel growth of controlled ZnO nanometer rod
The zinc nitrate hexahydrate solution of preparation 0.025～2M, the vulkacit H solution of 0.025～2M.Two solution are inhaled into the syringe of two 10mL respectively, it is 5～50 μ L/min that the setting micro syringe pump pushes away speed, two solution are transported to step (2) simultaneously to be shaped in the microchannel of ZnO crystal seed, after reacting 10～60min under 85～120 ℃ in the baking oven, stop delivered solution, dry 1～2h down with the washed with de-ionized water microchannel and at 150～200 ℃, obtain the ZnO nanometer stick array.
Reaction process is as follows:
(CH
2)
6N
4+6H
2O→6HCHO+4NH
3 (1)
NH
3+H
2O→NH
4 ++OH
- (2)
2OH
-+Zn
2+→Zn(OH)
2 (3)
Zn(OH)
2→ZnO+H
2O (4)
The preparation method's of ZnO nanorod with controllable distribution by growing route is in a kind of microchannel of the present invention: configuration washing lotion I, II, clean the glass capillary microchannel under the certain temperature and with its oven dry, under the room temperature, configuration zinc salt and aqueous sodium hydroxide solution, get a certain amount of mixed solution of forming by cetyl trimethylammonium bromide, octane and the propyl carbinol of same ratio that adds respectively, under the ultra-sonic dispersion effect, form two kinds of reverse micro emulsions; The microchannel of cleaning is placed baking oven, under the certain temperature, utilize micro syringe pump to wherein carrying two kinds of microemulsions simultaneously, behind the certain hour, stop to carry, after the emulsification certain hour is removed in intensification, utilize acetone and alcohol mixeding liquid to clean the microchannel, the oven dry back obtains the crystal seed of good dispersity on the internal surface of microchannel; Be transported to zinc nitrate and vulkacit H solution in the microchannel simultaneously subsequently, under the certain temperature, after fluid is carried for some time, stop delivered solution, behind the intensification oven dry microchannel, utilize the deionized water wash microchannel, oven dry again, good ZnO nanometer rod obtains distributing on the internal surface of microchannel.
Beneficial effect
(1) preparation of monodimension nanometer material and modification, the modification of microfluidic channel are combined, without any need for patterning techniques or the template ZnO nanometer stick array that promptly obtained controlled distribution;
(2) be the geometry modification of microfluidic channel internal surface, provide a convenience, general, process simple, expend little approach.
Description of drawings
The low power of the ZnO nanometer stick array on the internal surface of Fig. 1 microchannel a) and high power b) stereoscan photograph;
The field emission scanning electron microscope photo of the ZnO crystal seed on the internal surface of Fig. 2 microchannel;
The size of the molar ratio of Fig. 3 water and tensio-active agent (w) is to the figure that influences of drop size in the microemulsion;
The size of the molar ratio of Fig. 4 water and tensio-active agent (w) is to the figure that influences of flower-shaped bunch of distribution density of ZnO nanometer rod.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Configuration washing lotion I (V
The vitriol oil: V
Hydrogen peroxide: V
Distilled water=4:1:20) and washing lotion II (V
Ammoniacal liquor: V
Hydrogen peroxide: V
Distilled water=1:4:20).The microchannel is soaked among the washing lotion I at 110 ℃ of following 10min, behind the deionized water rinsing, again the microchannel is soaked among the washing lotion II and soaks 10min down at 70 ℃, behind the last deionized water rinsing, dry for standby.The Zinc diacetate dihydrate solution of configuration 0.01M, 0.04M sodium hydroxide solution, 0.05M zinc nitrate hexahydrate solution, 0.05M vulkacit H solution, dispose two portions of mixed solutions of forming by 2gCTAB, 12.8mL octane, 5mL propyl carbinol (according to CTAB, propyl carbinol, octane mass ratio are 26.67%:13.33%:60%).The Zinc diacetate dihydrate solution that in an above mixed solution, adds the 0.01M of 0.8mL, add the sodium hydroxide solution of the 0.04M of 0.8mL in another mixed solution, obtain two kinds of transparent reverse micro emulsions (the wherein molar ratio w=8 of water and tensio-active agent) under the ultrasonication.Two reverse micro emulsions suck the syringe of two 10mL respectively, it is 25 μ L/min that the setting micro syringe pump pushes away speed, it is transported to the microchannel that places 60 ℃ of baking ovens in advance simultaneously, fluid stops to carry after carrying 30min, oven temperature is increased to 150 ℃, time 1.5h realizes that high temperature goes emulsifying effect.Successively utilizing volume ratio is 1: 1 ethanol and acetone mixed solution, washed with de-ionized water microchannel, and 150 ℃ of oven dry down, obtains the ZnO crystal seed on the internal surface of microchannel.Utilize micro syringe pump that zinc nitrate hexahydrate solution and vulkacit H solution are transported in the microchannel of existing ZnO crystal seed simultaneously subsequently, after reacting 2h under 90 ℃ in the baking oven, stop delivered solution, be warming up to 150 ℃, 1h is dried in the microchannel, after the cleaning, 150 ℃ of oven dry down, obtain the ZnO nanometer stick array again.The field emission scanning electron microscope photo of the ZnO crystal seed on the internal surface of microchannel that Fig. 2 obtains for present embodiment, as can be seen: crystal seed dispersed fine.The stereoscan photograph of the ZnO nanometer stick array on the microchannel internal surface that Fig. 1 obtains for this example, the ZnO nanometer rod is flower-shaped as can be seen, and is evenly distributed on the internal surface of whole microchannel.Fig. 3 is the size of the w value that obtains by means of the result of the dynamic light scattering figure that influences to drop size in the micro emulsion, and the drop size in the time of can finding this example w=8 from figure is about 7.2nm.Fig. 4 is the influence figure of the size of the w value that obtains of the result according to dynamic light scattering to ZnO nanometer stick array distribution density, and the distance in the time of can seeing this example w=8 between flower-shaped bunch of center of nanometer rod is approximately 0.6 μ m.
Embodiment 2
Configuration washing lotion I (V
The vitriol oil: V
Hydrogen peroxide: V
Distilled water=4:1:20) and washing lotion II (V
Ammoniacal liquor: V
Hydrogen peroxide: V
Distilled water=1:4:20).The microchannel is soaked among the washing lotion I at 110 ℃ of following 30min, behind the deionized water rinsing, again the microchannel is soaked among the washing lotion II and soaks 30min down at 60 ℃, behind the last deionized water rinsing, dry for standby.The Zinc diacetate dihydrate solution of configuration 0.01M, 0.04M sodium hydroxide solution, 0.025M zinc nitrate hexahydrate solution, 0.025M vulkacit H solution, dispose two portions of mixed solutions of forming by 2g CTAB, 12.8mL octane, 5mL propyl carbinol (according to CTAB, propyl carbinol, octane mass ratio are 26.67%:13.33%:60%).The Zinc diacetate dihydrate solution that in an above mixed solution, adds the 0.01M of 0.4mL, add the sodium hydroxide solution of the 0.04M of 0.4mL in another mixed solution, obtain two kinds of transparent reverse micro emulsions (the wherein molar ratio w=4 of water and tensio-active agent) under the ultrasonication.Two reverse micro emulsions suck the syringe of two 10mL respectively, it is 50 μ L/min that the setting micro syringe pump pushes away speed, it is transported to the microchannel that places 80 ℃ of baking ovens in advance simultaneously, fluid stops to carry after carrying 10min, oven temperature is increased to 180 ℃, time 1h realizes that high temperature goes emulsifying effect.Successively utilize volume ratio to be the ethanol of 1:1 and acetone mixed solution, washed with de-ionized water microchannel, and, on the internal surface of microchannel, obtain the ZnO crystal seed 150 ℃ of oven dry down.Utilize micro syringe pump that zinc nitrate hexahydrate solution and vulkacit H solution are transported in the microchannel of existing ZnO crystal seed simultaneously subsequently, after reacting 1h under 85 ℃ in the baking oven, stop delivered solution, be warming up to 150 ℃, 1.5h is dried in the microchannel, after the cleaning, 150 ℃ of oven dry down, obtain the ZnO nanometer stick array again.Can find ZnO crystal seed dispersed fine on the internal surface of microchannel by the field emission scanning electron microscope photo.Fig. 3 is the size of the w value that obtains by means of the result of the dynamic light scattering figure that influences to drop size in the micro emulsion, and the drop size in the time of can finding this example w=4 from figure is about 3.5nm.Fig. 4 is the influence figure of the size of the w value that obtains of the result according to dynamic light scattering to ZnO nanometer stick array distribution density, and the distance in the time of can seeing this example w=4 between flower-shaped bunch of center of nanometer rod is approximately 1.3 μ m.
Configuration washing lotion I (V
The vitriol oil: V
Hydrogen peroxide: V
Distilled water=4:1:20) and washing lotion II (V
Ammoniacal liquor: V
Hydrogen peroxide: V
Distilled water=1:4:20).The microchannel is soaked among the washing lotion I at 130 ℃ of following 10min, behind the deionized water rinsing, again the microchannel is soaked among the washing lotion II and soaks 10min down at 80 ℃, behind the last deionized water rinsing, dry for standby.The Zinc diacetate dihydrate solution of configuration 0.001M, 0.004M sodium hydroxide solution, the zinc nitrate hexahydrate solution of 1M, the vulkacit H solution of 1M, dispose two portions of mixed solutions of forming by 2gCTAB, 12.8mL octane, 5mL propyl carbinol (according to CTAB, propyl carbinol, octane mass ratio are 26.67%:13.33%:60%).The Zinc diacetate dihydrate solution that in an above mixed solution, adds the 0.001M of 0.6mL, add the sodium hydroxide solution of the 0.004M of 0.6mL in another mixed solution, obtain two kinds of transparent reverse micro emulsions (the wherein molar ratio w=6 of water and tensio-active agent) under the ultrasonication.Two reverse micro emulsions suck the syringe of two 10mL respectively, it is 10 μ L/min that the setting micro syringe pump pushes away speed, it is transported to the microchannel that places 60 ℃ of baking ovens in advance simultaneously, fluid stops to carry after carrying 40min, oven temperature is increased to 150 ℃, and time 2h realizes that high temperature goes emulsifying effect.Successively utilize volume ratio to be the ethanol of 1:1 and acetone mixed solution, washed with de-ionized water microchannel, and, on the internal surface of microchannel, obtain the ZnO crystal seed 150 ℃ of oven dry down.Utilize micro syringe pump that zinc nitrate hexahydrate solution and vulkacit H solution are transported in the microchannel of existing ZnO crystal seed simultaneously subsequently, after reacting 4h under 120 ℃ in the baking oven, stop delivered solution, be warming up to 150 ℃, 2h is dried in the microchannel, after the cleaning, 150 ℃ of oven dry down, obtain the ZnO nanometer stick array again.Can find ZnO crystal seed dispersed fine on the internal surface of microchannel by the field emission scanning electron microscope photo.Fig. 3 is the size of the w value that obtains by means of the result of the dynamic light scattering figure that influences to drop size in the micro emulsion, and the drop size in the time of can finding this example w=6 from figure is about 5.3nm.Fig. 4 is the influence figure of the size of the w value that obtains of the result according to dynamic light scattering to ZnO nanometer stick array distribution density, and the distance in the time of can seeing this example w=6 between flower-shaped bunch of center of nanometer rod is approximately 0.92 μ m.
Configuration washing lotion I (V
The vitriol oil: V
Hydrogen peroxide: V
Distilled water=4:1:20) and washing lotion II (V
Ammoniacal liquor: V
Hydrogen peroxide: V
Distilled water=1:4:20).The microchannel is soaked among the washing lotion I at 130 ℃ of following 30min, behind the deionized water rinsing, again the microchannel is soaked among the washing lotion II and soaks 30min down at 80 ℃, behind the last deionized water rinsing, dry for standby.The Zinc diacetate dihydrate solution of configuration 0.005M, 0.02M sodium hydroxide solution, the zinc nitrate hexahydrate solution of 2M, the vulkacit H solution of 2M, dispose two portions of mixed solutions of forming by 2gCTAB, 12.8mL octane, 5mL propyl carbinol (according to CTAB, propyl carbinol, octane mass ratio are 26.67%:13.33%:60%).The Zinc diacetate dihydrate solution that in an above mixed solution, adds the 0.01M of 1.0mL, add the sodium hydroxide solution of the 0.04M of 1.0mL in another mixed solution, obtain two kinds of transparent reverse micro emulsions (the wherein molar ratio w=10 of water and tensio-active agent) under the ultrasonication.Two reverse micro emulsions suck the syringe of two 10mL respectively, it is 5 μ L/min that the setting micro syringe pump pushes away speed, it is transported to the microchannel that places 30 ℃ of baking ovens in advance simultaneously, fluid stops to carry after carrying 60min, oven temperature is increased to 200 ℃, time 1h realizes that high temperature goes emulsifying effect.Successively utilize volume ratio to be the ethanol of 1:1 and acetone mixed solution, washed with de-ionized water microchannel, and, on the internal surface of microchannel, obtain the ZnO crystal seed 150 ℃ of oven dry down.Utilize micro syringe pump that zinc nitrate hexahydrate solution and vulkacit H solution are transported in the microchannel of existing ZnO crystal seed simultaneously subsequently, after reacting 10h under 90 ℃ in the baking oven, stop delivered solution, be warming up to 150 ℃, 1h is dried in the microchannel, after the cleaning, 150 ℃ of oven dry down, obtain the ZnO nanometer stick array again.Can find ZnO crystal seed dispersed fine on the internal surface of microchannel by the field emission scanning electron microscope photo.Fig. 3 is the size of the w value that obtains by means of the result of the dynamic light scattering figure that influences to drop size in the micro emulsion, and the drop size in the time of can finding this example w=10 from figure is about 9.1nm.Fig. 4 is the influence figure of the size of the w value that obtains of the result according to dynamic light scattering to ZnO nanometer stick array distribution density, and the distance in the time of can seeing this example w=10 between flower-shaped bunch of center of nanometer rod is approximately 0.10 μ m.
Claims (8)
1. the preparation method of ZnO nanorod with controllable distribution by growing in the microchannel comprises:
(1) cleaning of microchannel
As the microchannel, prepare washing lotion I, V with glass capillary
The vitriol oil: V
Hydrogen peroxide: V
Distilled water=4:1:20 and washing lotion II, V
Ammoniacal liquor: V
Hydrogen peroxide: V
Distilled water=1:4:20 is soaked among the washing lotion I microchannel at 110～130 ℃ of 10～30min down, and behind the deionized water rinsing, again the microchannel is soaked among the washing lotion II and soaks 10～30min down at 60～80 ℃, behind the last deionized water rinsing, oven dry;
(2) preparation of the controlled crystal seed of dispersion in the microchannel
Prepare the soluble Zn salts solution respectively, 0.004 the alkaline solution of～0.04M, dispose two portions of mixed solutions of forming by 2g cetyl trimethylammonium bromide (CTAB), 12.8mL octane, 5mL propyl carbinol, the zinc solution that in a mixed solution wherein, adds 0.4～1.0mL, the alkaline solution that adds 0.4～1.0mL in another mixed solution obtains two kinds of transparent reverse micro emulsions under the ultrasonication; Two reverse micro emulsions suck the syringe of two 10mL respectively, it is 5～50 μ L/min that the setting micro syringe pump pushes away speed, it is transported to the microchannel that the step (1) that places 30～80 ℃ of baking ovens was in advance cleaned simultaneously, fluid stops to carry after carrying 10～60min, oven temperature is increased to 150～200 ℃, time 1～2h, realize that high temperature goes emulsifying effect, successively utilize volume ratio to be the ethanol of 1:1 and acetone mixed solution, washed with de-ionized water microchannel, and under 150 ℃, dry 1～2h, on the internal surface of microchannel, obtain the ZnO crystal seed;
(3) distribute in the microchannel growth of controlled ZnO nanometer rod
Prepare the soluble Zn salts solution respectively, 0.025 the amine aqueous solution of～2M, two solution are inhaled into the syringe of two 10mL respectively, two solution are transported to step (2) simultaneously to be shaped in the microchannel of ZnO crystal seed, after reacting 10～60min under 85～120 ℃ in the baking oven, stop delivered solution, dry 1～2h down, obtain the ZnO nanometer stick array with the washed with de-ionized water microchannel and at 150～200 ℃.
2. the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel according to claim 1 is characterized in that: the zinc salt that relates in described step (2) or (3) is zinc acetate, zinc sulfate, zinc chloride or zinc nitrate.
3. the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel according to claim 1 and 2 is characterized in that: described step (2) acetic acid zinc concentration is 0.001～0.01M.
4. the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel according to claim 1 is characterized in that: described step (2) CTAB, octane, propyl carbinol mass ratio are 26.67%:60%:13.33%.
5. the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel according to claim 1 and 2 is characterized in that: described step (3) nitric acid zinc concentration is 0.025～2M.
6. the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel according to claim 1 is characterized in that: described step (2) alkali is sodium hydroxide, ammoniacal liquor, urea or hydrazine hydrate.
7, the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel according to claim 1, it is characterized in that: the amine of described step (3) is vulkacit H or diethylenetriamine.
8, the preparation method of ZnO nanorod with controllable distribution by growing in a kind of microchannel according to claim 1, it is characterized in that: by the mol ratio of water and tensio-active agent in the regulation and control microemulsion system, on the internal surface of microchannel, obtain controlled dispersive ZnO crystal seed, and then on the internal surface of microchannel, obtained the controlled ZnO nanometer rod of distribution density.
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