CN103359773B - A kind of preparation method of zinc oxide nano rod - Google Patents
A kind of preparation method of zinc oxide nano rod Download PDFInfo
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- CN103359773B CN103359773B CN201310264503.5A CN201310264503A CN103359773B CN 103359773 B CN103359773 B CN 103359773B CN 201310264503 A CN201310264503 A CN 201310264503A CN 103359773 B CN103359773 B CN 103359773B
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Abstract
The invention discloses a kind of preparation method of zinc oxide nano rod, comprise the steps: to join sodium hydroxide, or potassium hydroxide aqueous solution; Be that 0.001:1 ~ 1:1 takes cetyl trimethylammonium bromide by the mol ratio of cetyl trimethylammonium bromide and sodium hydroxide, add in sodium hydroxide solution; Add by carbonyl diamine and sodium hydroxide mol ratio joined solution by 0.05:1 ~ 1:1 takes carbonyl diamine, stir; Be that 0.03 ~ 3:1 takes zinc precursor by zinc precursor and sodium hydroxide mol ratio, join the zinc precursor solution that concentration is 0.3 ~ 1M; Heating, stirs; Centrifugally obtain white powder, dry, obtain zinc oxide nano rod.The method is simple to operate, and the ZnO rod size adjustable prepared, because ZnO rod size is little, therefore has very large specific surface area, be adapted at applying in photocatalyst and gas sensor.
Description
Technical field
The present invention relates to the technology of preparing of metal oxide nanorods, specifically refer to a kind of method preparing zinc oxide nano rod in the basic conditions.
Background technology
Metal oxide is utilized to be widely used as a kind of new air and water purification technology as photocatalyst material, Photocatalitic Technique of Semiconductor has boundless application prospect utilizing the photodegradation field of sunlight water decomposition and organic pollutant, therefore becomes one of most active research field.In all kinds of photocatalyst material, ZnO, owing to having wider energy gap and large exciton bind energy, makes it have a lot of excellent optics, electrology characteristic, in addition due to low price, chemistry and photochemistry good stability, material is pollution-free becomes one of material of greatest concern.Zinc oxide has much different structures, as ZnO nano-wire, nanotube, nanometer rod, microballoon, wherein, ZnO nanorod, owing to having adjustable particle diameter ratio, higher surface charge transport rate and higher specific surface area, has boundless application prospect in fields such as photochemical catalysis, photosensitive, the solar cell of chemistry and gas sensors.
The method preparing zinc oxide nano rod is at present numerous, as thermal evaporation, physical vaporous deposition Metalorganic Chemical Vapor Deposition, template, hydrothermal method etc.Hydrothermal method due to temperature of reaction low, and have simple, cost is low, productive rate advantages of higher, becomes most potential synthetic method.The technique of conventional hydrothermal method synthesizing zinc oxide nanometer rod is generally carried out in water heating kettle, and the reaction times is long, is not generally tens hours to several days not etc., and observable index is comparatively large, and the general small volume of reactor, be difficult to realize batch production.Therefore be necessary very much the synthesis technique studying zinc oxide nano rod further, continue to reduce costs, improve productive rate, for the application realizing zinc oxide nano rod provides technique means.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of preparation method of zinc oxide nano rod.
A preparation method for zinc oxide nano rod, is characterized in that, comprises the steps:
(1) sodium hydroxide that concentration is 1 ~ 4 mmol/ml is joined, or potassium hydroxide aqueous solution;
(2) be that 0.001:1 ~ 1:1 takes cetyl trimethylammonium bromide by the mol ratio of cetyl trimethylammonium bromide and sodium hydroxide, add in sodium hydroxide solution;
(3) add step (2) by carbonyl diamine and sodium hydroxide mol ratio joined solution by 0.05:1 ~ 1:1 takes carbonyl diamine, stir 20 minutes to one hour;
(4) be that 0.03 ~ 3:1 takes zinc precursor by zinc precursor and sodium hydroxide mol ratio, join the zinc precursor solution that concentration is 0.3 ~ 1M;
(5) step (3) gained solution is heated to 60 ~ 90 DEG C, step (4) gained solution is injected, stir half an hour;
(6) centrifugally white powder is obtained, dry at 50 ~ 80 DEG C, obtain zinc oxide nano rod.
Zinc precursor described in step (4) is one in zinc nitrate, zinc acetate, zinc sulfate or its combination.
Reaction conditions described in step (5) is air atmosphere.
Drying means described in step (6) is constant pressure and dry or vacuum-drying, and described time of drying is 6 ~ 24 hours.
The invention provides a kind of preparation method of zinc oxide nano rod of simple possible, solve small scale in hydrothermal method synthesis, the problems such as long reaction time, synthesizing zinc oxide nanometer rod in the basic conditions, overcome the difficulty of nano structure of zinc oxide poor stability, make nano zinc oxide material have more wide application prospect in fields such as photochemical catalysis, photosensitive, the solar cell of chemistry and gas sensors.
Method of the present invention utilizes solution method to prepare synthesizing zinc oxide nanometer rod in the basic conditions, the regulation and control of zinc oxide nanorod structures and size are realized by parameters such as the ratios of the concentration of the pH value of adjustment and control system, presoma, system temperature of reaction, tensio-active agent and presoma, the reactivity of the method zinc precursor is more than 90%, and it is consuming time short, require low to plant and instrument, greatly can reduce the cost of synthesizing zinc oxide nanometer rod.
The invention has the advantages that: the preparation method of zinc oxide nano rod is simple, be easy to the diameter and the length that control nanometer rod, synthesizing zinc oxide nanometer rod has good stability in the basic conditions; The productive rate of synthesizing zinc oxide nanometer rod is high, and zinc oxide nano rod prepared by this invention can be used for the fields such as photochemical catalysis, gas sensor and solar cell.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the zinc oxide nano rod of the embodiment of the present invention 1.
Fig. 2 is the XRD figure of the zinc oxide nano rod of the embodiment of the present invention 1.
Fig. 3 is the SEM figure of the zinc oxide nano rod of the embodiment of the present invention 4.
Embodiment
Embodiment 1: the sodium hydroxide taking 3 g, adds the water of 20 ml, after sodium hydroxide dissolves, add the cetyl trimethylammonium bromide of 0.1 g and the carbonyl diamine of 1.5 g, stirs half an hour, is made into No. 1 solution; Take the zinc nitrate of 2.5g, be dissolved in the water of 30 ml, be made into No. 2 solution.No. 1 solution is heated to 70 DEG C, after 20 minutes, No. 2 solution is added in No. 1 solution, react 20 minutes; By white suspension centrifugation, with alcohol and water washing, in loft drier, 50 DEG C of dryings 10 hours, obtain zinc oxide nano rod powder.
Fig. 1 gives the SEM figure of zinc oxide nano rod, and as seen from the figure, nanorod diameter is at about 100 nm, and length is at about 350 nm.Fig. 2 is the XRD figure of zinc oxide nano rod, and XRD data results shows, and gained nanometer rod is standard hex wurtzite ZnO, and diffraction peak is corresponding with the standard card JCPDS card number 36-1451 of ZnO.
Embodiment 2: the sodium hydroxide taking 2 g, adds the water of 20 ml, after sodium hydroxide dissolves, add the cetyl trimethylammonium bromide of 0.15 g and the carbonyl diamine of 1.5 g, stirs half an hour, is made into No. 1 solution; Take the zinc acetate of 1.5 g, dissolve in the water of 20 ml, be made into No. 2 solution.No. 1 solution is heated to 80 DEG C, after 20 minutes, No. 2 solution is added in No. 1 solution, react 20 minutes; By white suspension centrifugation, with alcohol and water washing, in loft drier, 60 DEG C of dryings 9 hours, obtain zinc oxide nano rod powder.The PH of change system is to the concentration increasing cetyl trimethylammonium bromide simultaneously, and the length of the zinc oxide nano rod of preparation and diameter proportion are 4:1.
Embodiment 3: the potassium hydroxide taking 3.5 g, adds the water of 20 ml, after potassium hydroxide dissolves, add the cetyl trimethylammonium bromide of 0.1 g and the carbonyl diamine of 1.5 g, stirs half an hour, is made into No. 1 solution; Take the zinc acetate of 1.5 g, dissolve in the water of 20 ml, be made into No. 2 solution.No. 1 solution is heated to 80 DEG C, after 20 minutes, No. 2 solution is added in No. 1 solution, react 20 minutes; By white suspension centrifugation, with alcohol and water washing, in loft drier, 60 DEG C of dryings 9 hours, obtain zinc oxide nano rod powder.With potassium hydroxide and sodium hydroxide highly basic, little on net result impact, gained zinc oxide nano rod diameter is at about 110 nm, and length is at about 380 nm.
Embodiment 4: the potassium hydroxide taking 3.5 g, adds the water of 20 ml, after potassium hydroxide dissolves, add the cetyl trimethylammonium bromide of 1.0 g and the carbonyl diamine of 2 g, stirs half an hour, is made into No. 1 solution; Take the zinc sulfate of 2 g, dissolve in the water of 30 ml, be made into No. 2 solution.No. 1 solution is heated to 80 DEG C, after 20 minutes, No. 2 solution is added in No. 1 solution, react 20 minutes; By white suspension centrifugation, with alcohol and water washing, in loft drier, 60 DEG C of dryings 9 hours, obtain zinc oxide nano rod powder.Accompanying drawing 3 is the SEM figure of the zinc oxide nano rod of the present embodiment, and increase the content of carbonyl diamine as seen from the figure, gained zinc oxide nano rod is self-assembled into flower-like structure.
Claims (4)
1. a preparation method for zinc oxide nano rod, is characterized in that, comprises the steps:
(1) sodium hydroxide that concentration is 1 ~ 4 mmol/mL is joined, or potassium hydroxide aqueous solution;
(2) be that 0.001:1 ~ 1:1 takes cetyl trimethylammonium bromide by the mol ratio of cetyl trimethylammonium bromide and sodium hydroxide, add in sodium hydroxide solution;
(3) add step (2) by carbonyl diamine and sodium hydroxide mol ratio joined solution by 0.05:1 ~ 1:1 takes carbonyl diamine, stir 20 minutes to one hour;
(4) be that 0.03 ~ 3:1 takes zinc precursor by zinc precursor and sodium hydroxide mol ratio, join the zinc precursor solution that concentration is 0.3 ~ 1M;
(5) step (3) gained solution is heated to 60 ~ 90 DEG C, step (4) gained solution is injected, stir half an hour;
(6) centrifugally white powder is obtained, dry at 50 ~ 80 DEG C, obtain zinc oxide nano rod.
2. the preparation method of a kind of zinc oxide nano rod according to claim 1, is characterized in that, the zinc precursor described in step (4) is one in zinc nitrate, zinc acetate, zinc sulfate or its combination.
3. the preparation method of a kind of zinc oxide nano rod according to claim 1, it is characterized in that, the reaction conditions described in step (5) is air atmosphere.
4. the preparation method of a kind of zinc oxide nano rod according to claim 1, it is characterized in that, the drying means described in step (6) is constant pressure and dry or vacuum-drying, and described time of drying is 6 ~ 24 hours.
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| CN103675026B (en) * | 2013-11-27 | 2016-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | For the preparation method of the Hierarchical self-assembly zinc paste micro-nano structure of gas sensor |
| CN103771493B (en) * | 2014-02-14 | 2016-01-27 | 常州大学 | A kind of method preparing one-D nano zinc oxide |
| CN104310458B (en) * | 2014-10-10 | 2015-10-14 | 九江学院 | A kind of method preparing zinc oxide nano rod |
| KR101767236B1 (en) * | 2015-01-16 | 2017-08-10 | 고려대학교 산학협력단 | Nanoporous polymer membrane and preparation method thereof |
| CN105424759A (en) * | 2015-10-22 | 2016-03-23 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of zinc oxide nanotube array gas sensitive sensor |
| CN105460970A (en) * | 2015-12-21 | 2016-04-06 | 厦门理工学院 | Method for urea assisted hydrothermal synthesis of zinc oxide nanosheet |
| CN106025083A (en) * | 2016-07-20 | 2016-10-12 | 上海交通大学 | Perovskite solar cell electronic transmission layer and preparation method thereof |
| CN110564457A (en) * | 2019-07-26 | 2019-12-13 | 沈阳三聚凯特催化剂有限公司 | Deep purification fine desulfurizer and preparation method thereof |
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| CN1673094A (en) * | 2005-02-01 | 2005-09-28 | 山东师范大学 | Synthesis process of nano zinc oxide material |
| CN101475206A (en) * | 2009-01-13 | 2009-07-08 | 东华大学 | Method for preparing ZnO nanorod with controllable distribution by growing in microchannel |
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