CN101786652A - Method for preparing zinc oxide nano rod with concave end - Google Patents
Method for preparing zinc oxide nano rod with concave end Download PDFInfo
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- CN101786652A CN101786652A CN 201010114372 CN201010114372A CN101786652A CN 101786652 A CN101786652 A CN 101786652A CN 201010114372 CN201010114372 CN 201010114372 CN 201010114372 A CN201010114372 A CN 201010114372A CN 101786652 A CN101786652 A CN 101786652A
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Abstract
The invention discloses a method for preparing a zinc oxide nano rod with a concave end, which is characterized by comprising the following steps: fully mixing zinc nitrate solution and hexamethylenetetramine which have the equivalent molar concentration in a bottle in an isovolumetric manner, sealing the bottle by a plastics film, placing the bottle in a constant temperature drying oven under the conditions that the constant temperature reaction temperature is 70 DEG C and the constant temperature reaction time is 1-3h, taking the bottle out, removing the plastic film for sealing, absorbing and removing supernate by using a suction pipe, placing the bottle and residual precipitate therein in the constant temperature drying oven once again in an open manner, and drying at constant temperature to obtain the zinc oxide nano rod with a concave end. The method in the invention has simple reaction, requires no adjustment of the pH value and no addition of other additives, has low cost and low energy consumption, and protects environment without pollution; and the rod zinc oxide nano structure with the concave end can be obtained by reacting for 1-3h under the low temperature of 60-70 DEG C.
Description
Technical field
The present invention relates to a kind of preparation method of zinc oxide nano rod of concave end, belong to the nano material preparation technical field.
Background technology
Zinc oxide is a kind of semiconductor material with significant application value, is that a few is easy to one of oxide semiconductor material of realizing quantum size effect.Nano structure of zinc oxide has good electrical conductivity, thermal conductivity, chemical stability, biological friendly, fluorescence, piezoelectricity and the ultraviolet ability of absorption, is the focus of researchs such as present shortwave semiconductor laser device material, solar-energy photo-voltaic cell material, stealth material in the world.The preparation method of nano structure of zinc oxide, oriented growth mechanism, property and application are domestic in recent years newer research focuses.
Nano structure of zinc oxide has diversified form, as nano wire, nano belt, nano-rings, nanometer spiral, quadrangular pyramid shape, plum blossom shape, sheet, pattern such as bar-shaped, spherical; Because unidimensional nano wire or nanometer rod, electronics and photoproduction exciton are along axially effectively transmission, therefore can be used as the elementary cell of integrated nanometer array device, or as the lead that is connected in nano-device and the super large-scale integration, photoconductive fiber and nanometer cantilever, nano-probe, nanometer sky equality, so the applied research for zinc oxide nanowire or this one dimension Nano structure of nanometer rod is more extensive, in addition, because zinc oxide is also nontoxic because of it, low cost and other advantages, become the novel environment friendly material that is widely studied at present, be used in the various organic pollutants of photocatalytic degradation field.
The preparation method of zinc oxide monodimension nano structure is rich and varied, and commonly used have gas phase synthesis method and a liquid phase synthesizing method.Gas phase synthesis method comprises chemical Vapor deposition process, magnetron sputtering method, spray pyrolysis, pulsed laser deposition and molecular beam epitaxy etc., but the temperature of reaction height, equipment complexity, cost height and efficient is low.Liquid phase synthesizing method comprises sol-gel method, hydrolysis method, hydrothermal method, the precipitator method etc., and reaction process is simple, easy handling, and cost is low, and efficient is higher.
World Intellectual Property Organization WIPO office has announced a kind of method (application number: WO05044722) for preparing nanometic zinc oxide rod array, in substrate, form a kind of alloy or molten drop that includes catalyst elements earlier, after treating the alloy liquid droplet supersaturation, nanometer rod begins growth, form one dimension Nano structure, the nanostructure particle diameter that this method is produced is even, but the process complexity, the energy consumption height, and introduced alloy or metallic impurity.
Patent Office of the People's Republic of China has announced a kind of single nano-ZnO preparation (publication number: CN1562762) that disperses not have reunion and strong uv-absorbing, at first be dissolved in zinc salt zinc nitrate hexahydrate and ammonia source hexamethylene tetraammonia in the methanol solution by a certain percentage, add certain polyvinylpyrrolidone again, pour into after stirring in the tetrafluoroethylene reactor, airtight be warming up to 95-100 ℃ the reaction 3-4h, finish back naturally cooling and centrifugation, this method in a large number with an organic solvent and tensio-active agent, easily produce and pollute, raw materials cost is high and higher to equipment requirements; Also have molecular beam epitaxy etc. in addition, the nanostructure quality of generation is good, but preparation condition requires height, and the cost height is not suitable for large-scale production.
Summary of the invention
The invention discloses a kind of preparation method of concave end zinc oxide nano rod, its purpose is to overcome prior art and adopts gas phase synthesis method temperature of reaction height, the equipment complexity, cost height and efficient is low adopts the high and easy drawback such as contaminate environment of liquid phase synthesizing method production cost.The inventive method not only can be prepared the bar-shaped nano structure of zinc oxide with concave end feature quickly and easily, and the preparation process temperature is low, and cost is low, energy consumption is low.The inventive method operating process is simple, and is environment friendly and pollution-free.
A kind of preparation method of zinc oxide nano rod of concave end, it is characterized in that: zinc nitrate solution and hexamethylene tetraammonia solution equal-volume thorough mixing in container bottle that will wait volumetric molar concentration, with putting into thermostatic drying chamber behind the plastics film encloses container bottle, the isothermal reaction temperature is 70 ℃, the isothermal reaction time is 1-3h, after taking out container bottle, remove sealing and draw the removing upper strata stillness of night with plastics film and with suction pipe, with container bottle and the uncovered thermostatic drying chamber of putting into once more of interior residue throw out thereof, promptly obtain the zinc oxide nano rod of concave end behind the freeze-day with constant temperature.
The volumetric molar concentration scope of described zinc nitrate solution and hexamethylene tetraammonia solution is 0.03-0.05mol/L.
Described freeze-day with constant temperature temperature is 60 ℃, and the freeze-day with constant temperature time is 2h.
Adopt the zinc oxide nano rod of the inventive method preparation to have the concave end feature, as Fig. 1, Fig. 2, shown in Figure 3.
Advantage of the present invention is that at first the bar-shaped nano structure of zinc oxide of concave end is a kind of one dimension Nano structure of novelty, the structure of this concave end has increased the specific surface area of zinc oxide bar-shaped nanostructure, changed the configuration of surface of zinc oxide bar-shaped nanostructure, for zinc oxide provides more wide application prospect, simultaneously, preparation method of the present invention is simple, need not to regulate pH value, need not other additives, under 60-70 ℃ cold condition, can obtain the bar-shaped nano structure of zinc oxide of concave end by the reaction of 1-3h, cost is low, energy consumption is low, and environment friendly and pollution-free.
Description of drawings
Fig. 1 is the SEM image of bar-shaped nano structure of zinc oxide of the concave end of specific embodiment 1 preparation gained.
Fig. 2 is the SEM image of bar-shaped nano structure of zinc oxide of the concave end of specific embodiment 2 preparation gained.
Fig. 3 is the SEM image of bar-shaped nano structure of zinc oxide of the concave end of specific embodiment 3 preparation gained.
Embodiment
Below in conjunction with embodiment and SEM image preparation method of the present invention is described in further detail, but present embodiment is not limited to the present invention, every employing similarity method of the present invention and similar variation thereof all should be listed protection scope of the present invention in.
Embodiment 1
A. dispose the zinc nitrate solution and the hexamethylene tetraammonia solution of same molar ratio, concentration is 0.03mol/L;
B. get isopyknic zinc nitrate solution and each 100ml of hexamethylene tetraammonia solution, thorough mixing in volumetric flask need not to regulate pH value;
C. get the cover glass that specification is 20mm * 20mm, ultrasonic cleaning 10min in ethanol solution;
D. take out cover glass, the capacity of lying in is the beaker bottom of 50ml, adds the mixing solutions 40ml of B step in beaker;
E. setting the thermostatic drying chamber temperature is 70 ℃, behind the temperature-stable beaker is put into thermostatic drying chamber with the plastics film sealing;
F. behind the isothermal reaction 3h beaker is taken out, draw the upper strata stillness of night of removing in the beaker, need not to clean the white zinc oxide film with suction pipe;
G. setting the thermostatic drying chamber temperature is 60 ℃, behind the temperature-stable that beaker is uncovered, and wherein remains throw out and puts into thermostatic drying chamber once more;
H. take out behind the freeze-day with constant temperature 2h.
The zinc-oxide nano bar structure that is concave end that obtains, as shown in Figure 1: magnification is 50000 times, and the club shaped structure cross section is a hexagon, and the configuration of surface of significant depressions appears in the top, and diameter is 300-400nm, length is 2-4 μ m.
The zinc-oxide nano bar structure of concave end is gone up the white film that forms one deck even compact in simple glass substrate (cover glass), and tackyness is good, and no external force is scraped, can not come off when carving, and helps the application and the recovery of nanostructure.
Embodiment 2
A. dispose the zinc nitrate solution and the hexamethylene tetraammonia solution of same molar ratio, concentration is 0.05mol/L;
B. get isopyknic zinc nitrate solution and each 100ml of hexamethylene tetraammonia solution, thorough mixing in volumetric flask need not to regulate pH value;
C. get the cover glass that specification is 20mm * 20mm, ultrasonic cleaning 10min in ethanol solution;
D. take out cover glass, the capacity of lying in is the beaker bottom of 50ml, adds the mixing solutions 40ml of B step in beaker;
E. setting the thermostatic drying chamber temperature is 70 ℃, behind the temperature-stable beaker is put into thermostatic drying chamber with the plastics film sealing;
F. behind the isothermal reaction 1h beaker is taken out, draw the upper strata stillness of night of removing in the beaker, need not to clean the white zinc oxide film with suction pipe;
G. setting the thermostatic drying chamber temperature is 60 ℃, behind the temperature-stable that beaker is uncovered, and wherein remains throw out and puts into thermostatic drying chamber once more;
H. take out behind the freeze-day with constant temperature 2h.
The zinc-oxide nano bar structure that is concave end that obtains, as shown in Figure 2: magnification is 20000 times, and the club shaped structure cross section is a hexagon, and the configuration of surface of significant depressions appears in the top, and diameter is 300-600nm, length is 3-5 μ m.
The zinc-oxide nano bar structure of concave end is gone up the white film that forms one deck even compact in simple glass substrate (cover glass), and tackyness is good, and no external force is scraped, can not come off when carving.
Embodiment 3
A. dispose the zinc nitrate solution and the hexamethylene tetraammonia solution of same molar ratio, concentration is 0.05mol/L;
B. get isopyknic zinc nitrate solution and each 100ml of hexamethylene tetraammonia solution, thorough mixing in volumetric flask need not to regulate pH value;
C. get the cover glass that specification is 20mm * 20mm, ultrasonic cleaning 10min in ethanol solution;
D. take out cover glass, the capacity of lying in is the beaker bottom of 50ml, adds the mixing solutions 40ml of B step in beaker;
E. setting the thermostatic drying chamber temperature is 70 ℃, behind the temperature-stable beaker is put into thermostatic drying chamber with the plastics film sealing;
F. behind the isothermal reaction 2h beaker is taken out, draw the upper strata stillness of night of removing in the beaker, need not to clean the white zinc oxide film with suction pipe;
G. setting the thermostatic drying chamber temperature is 60 ℃, behind the temperature-stable that beaker is uncovered, and wherein remains throw out and puts into thermostatic drying chamber once more;
H. take out behind the freeze-day with constant temperature 2h.
The zinc-oxide nano bar structure that is concave end that obtains, as shown in Figure 3: magnification is 20000 times, and the club shaped structure cross section is a hexagon, and the configuration of surface of significant depressions appears in the top, and diameter is 300-600nm, length is 1-4 μ m.
The zinc-oxide nano bar structure of concave end is gone up the white film that forms one deck even compact in simple glass substrate (cover glass), and tackyness is good, and no external force is scraped, can not come off when carving.
Claims (3)
1. the preparation method of the zinc oxide nano rod of a concave end, it is characterized in that: a kind of preparation method of zinc oxide nano rod of concave end, it is characterized in that: zinc nitrate solution and hexamethylene tetraammonia solution equal-volume thorough mixing in container bottle that will wait volumetric molar concentration, with putting into thermostatic drying chamber behind the plastics film encloses container bottle, the isothermal reaction temperature is 70 ℃, the isothermal reaction time is 1-3h, after taking out container bottle, remove sealing and draw the removing upper strata stillness of night with plastics film and with suction pipe, with container bottle and the uncovered thermostatic drying chamber of putting into once more of interior residue throw out thereof, promptly obtain the zinc oxide nano rod of concave end behind the freeze-day with constant temperature.
2. the preparation method of the zinc oxide nano rod of a kind of concave end according to claim 1, it is characterized in that: the volumetric molar concentration scope of described zinc nitrate solution and hexamethylene tetraammonia solution is 0.03-0.05mol/L.
3. the preparation method of the zinc oxide nano rod of a kind of concave end according to claim 1, it is characterized in that: described freeze-day with constant temperature temperature is 60 ℃, the freeze-day with constant temperature time is 2h.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870558A (en) * | 2010-06-12 | 2010-10-27 | 上海理工大学 | Method for preparing zinc oxide nano-rod on common glass sheet substrate |
| CN102701267A (en) * | 2012-06-04 | 2012-10-03 | 兰州大学 | Preparation method for ZnO nanosphere with yolk-eggshell structure |
| CN106783186A (en) * | 2016-12-22 | 2017-05-31 | 广东昭信光电科技有限公司 | A kind of ZnO nanorod light anode and preparation method thereof, solar cell |
| CN108949085A (en) * | 2018-07-02 | 2018-12-07 | 合肥萃励新材料科技有限公司 | A kind of preparation method of electrostatic dissipation pressure sensitive adhesive |
| CN109054660A (en) * | 2018-07-02 | 2018-12-21 | 合肥萃励新材料科技有限公司 | A kind of preparation method of PESD function adhesive |
| CN110790301A (en) * | 2019-12-11 | 2020-02-14 | 大连理工大学 | Device and method for preparing high-quality-density uniform vertical zinc oxide nanorod array |
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| CN1296041A (en) * | 2000-11-30 | 2001-05-23 | 上海博纳科技发展有限公司 | Process for preparing nanometer zinc oxide |
| CN1562762A (en) * | 2004-04-22 | 2005-01-12 | 上海交通大学 | Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption |
| WO2005062785A2 (en) * | 2003-12-17 | 2005-07-14 | The University Of North Carolina At Chapel Hill | Solution-phase synthesis of metal oxide nanostructures |
| DE102008037177A1 (en) * | 2008-08-09 | 2010-02-11 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Preparing nanostructured metal oxide or -chalcogenide using chemical bath deposition on a substrate, comprises adding a soluble metal precursor and basic solution in a vessel, in which the substrate is added and stirring the solution |
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2010
- 2010-02-26 CN CN 201010114372 patent/CN101786652A/en active Pending
Patent Citations (4)
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| CN1296041A (en) * | 2000-11-30 | 2001-05-23 | 上海博纳科技发展有限公司 | Process for preparing nanometer zinc oxide |
| WO2005062785A2 (en) * | 2003-12-17 | 2005-07-14 | The University Of North Carolina At Chapel Hill | Solution-phase synthesis of metal oxide nanostructures |
| CN1562762A (en) * | 2004-04-22 | 2005-01-12 | 上海交通大学 | Method for preparing nano zinc oxide in monodisperse, with no agglomeration and strong ultraviolet absorption |
| DE102008037177A1 (en) * | 2008-08-09 | 2010-02-11 | Helmholtz-Zentrum Berlin Für Materialien Und Energie Gmbh | Preparing nanostructured metal oxide or -chalcogenide using chemical bath deposition on a substrate, comprises adding a soluble metal precursor and basic solution in a vessel, in which the substrate is added and stirring the solution |
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| 《Chemistry Letters》 20041113 Yongnan Zhao et al. Templateless Hydrothermal Synthesis of Aligned ZnO Nanorods 第1578-1579页 1-3 第33卷, 第12期 2 * |
| 《中国优秀硕士学位论文全文数据库 工程科技Iota辑》 20090315 李江勇 不同形貌Zn0纳米结构的制备及其发光性能研究 正文第36-42页 1-3 , 第3期 2 * |
| 《中国博士学位论文全文数据库 工程科技Iota辑》 20081115 于清江 低维Zn0纳米结构的制备及其性能研究 正文第45－49页 1－3 , 第11期 2 * |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870558A (en) * | 2010-06-12 | 2010-10-27 | 上海理工大学 | Method for preparing zinc oxide nano-rod on common glass sheet substrate |
| CN102701267A (en) * | 2012-06-04 | 2012-10-03 | 兰州大学 | Preparation method for ZnO nanosphere with yolk-eggshell structure |
| CN106783186A (en) * | 2016-12-22 | 2017-05-31 | 广东昭信光电科技有限公司 | A kind of ZnO nanorod light anode and preparation method thereof, solar cell |
| CN108949085A (en) * | 2018-07-02 | 2018-12-07 | 合肥萃励新材料科技有限公司 | A kind of preparation method of electrostatic dissipation pressure sensitive adhesive |
| CN109054660A (en) * | 2018-07-02 | 2018-12-21 | 合肥萃励新材料科技有限公司 | A kind of preparation method of PESD function adhesive |
| CN110790301A (en) * | 2019-12-11 | 2020-02-14 | 大连理工大学 | Device and method for preparing high-quality-density uniform vertical zinc oxide nanorod array |
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Open date: 20100728 |