CN103359773A - Preparation method of zinc oxide nanorod - Google Patents
Preparation method of zinc oxide nanorod Download PDFInfo
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- CN103359773A CN103359773A CN2013102645035A CN201310264503A CN103359773A CN 103359773 A CN103359773 A CN 103359773A CN 2013102645035 A CN2013102645035 A CN 2013102645035A CN 201310264503 A CN201310264503 A CN 201310264503A CN 103359773 A CN103359773 A CN 103359773A
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Abstract
The invention discloses a preparation method of a zinc oxide nanorod. The preparation method comprises the following steps of: preparing a water solution of sodium hydroxide or potassium hydroxide; weighting cetyltrimethylammonium bromide according to the mole ratio of the cetyltrimethylammonium bromide to the sodium hydroxide of (0.001:1)-(1:1), and adding the cetyltrimethylammonium bromide into the water solution of the sodium hydroxide; weighting carbamide according to the mole ratio of the carbamide to the sodium hydroxide of 0.05:1 to 1:1, adding the carbamide into the prepared solution, and stirring the solution; weighting a zinc precursor according to the mole ratio of the zinc precursor to the sodium hydroxide of (0.03-3):1, and preparing a zinc precursor solution with the concentration of 0.3-1M; heating and stirring the solution; and centrifuging the solution to obtain white powder, and drying to obtain the zinc oxide nanorod. The method is simple in operation; the prepared ZnO rod is adjustable in size; the prepared ZnO rod is small in size so as to be large in special surface area and suitable for application in a photocatalyst and a 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 that under alkaline condition, prepares zinc oxide nano rod.
Background technology
Utilize metal oxide 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 in the photodegradation field that utilizes sunlight water decomposition and organic pollutant, therefore becomes one of most active research field.In all kinds of photocatalyst materials, ZnO makes its optics with a lot of excellences, electrology characteristic owing to having wider energy gap and large exciton bind energy, in addition because low price, the chemistry and photochemistry good stability, material is pollution-free to become one of material of greatest concern.Zinc oxide has a lot of different structures, such as ZnO nano-wire, nanotube, nanometer rod, microballoon, wherein, ZnO nanorod has boundless application prospect owing to having adjustable particle diameter ratio, higher surface charge transmission rate and higher specific surface area in fields such as photochemical catalysis, chemical sensitization, solar cell and gas sensors.
The method for preparing at present zinc oxide nano rod is numerous, such as thermal evaporation, physical vaporous deposition Metalorganic Chemical Vapor Deposition, template, hydrothermal method etc.Hydrothermal method is because temperature of reaction is low, and have simple, cost is low, the productive rate advantages of higher, becomes most potential synthetic method.The technique of tradition hydrothermal method synthesizing zinc oxide nanometer rod is generally carried out in water heating kettle, and the reaction times is long, is generally tens hours to several days and does not wait, and energy consumption is larger, and the general small volume of reactor, is difficult to realize batch production.Therefore be necessary very much further to study the synthesis technique of zinc oxide nano rod, continue to reduce cost, improve productive rate, for the application that realizes 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 kind of preparation method of zinc oxide nano rod is characterized in that, comprises the steps:
(1) join the sodium hydroxide that concentration is 1～4 mmol/ml, or potassium hydroxide aqueous solution;
(2) mol ratio by cetyl trimethylammonium bromide and sodium hydroxide is that 0.001:1～1:1 takes by weighing cetyl trimethylammonium bromide, adds in the sodium hydroxide solution;
(3) take by weighing carbonyl diamine adding step (2) by carbonyl diamine and sodium hydroxide mol ratio by 0.05:1～1:1 and joined solution, stirred 20 minutes to one hour;
(4) be that 0.03～3:1 takes by weighing the zinc precursor body by zinc precursor body and sodium hydroxide mol ratio, joining concentration is the zinc precursor liquid solution of 0.3～1M;
(5) step (3) gained solution is heated to 60～90 ℃, step (4) gained solution is injected, stir half an hour;
(6) the centrifugal white powder that obtains 50～80 ℃ of lower dryings, obtains zinc oxide nano rod.
The described zinc precursor body of step (4) is a kind of or its combination in zinc nitrate, zinc acetate, the zinc sulfate.
The described reaction conditions of step (5) is air atmosphere.
The described drying means of step (6) is constant pressure and dry or vacuum-drying, and be 6～24 hours described time of drying.
The invention provides a kind of preparation method of zinc oxide nano rod of simple possible, solved the synthetic middle small scale of hydrothermal method, the problems such as long reaction time, synthesizing zinc oxide nanometer rod under alkaline condition, overcome the difficulty of nano structure of zinc oxide poor stability, made nano zinc oxide material have more wide application prospect in fields such as photochemical catalysis, chemical sensitization, solar cell and gas sensors.
Method of the present invention is to utilize solution method preparation synthesizing zinc oxide nanometer rod under alkaline condition, the parameters such as ratio of the pH value by adjustment and control system, concentration, system temperature of reaction, tensio-active agent and the presoma of presoma realize the regulation and control of zinc-oxide nano bar structure and size, the reactivity of the method zinc precursor body is more than 90%, and consuming time short, plant and instrument is required low, can greatly 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, is easy to control diameter and the length of nanometer rod, and the synthesizing zinc oxide nanometer rod has good stability under alkaline condition; The productive rate of synthesizing zinc oxide nanometer rod is high, and the zinc oxide nano rod of this invention preparation can be used for the fields such as photochemical catalysis, gas sensor and solar cell.
Description of drawings
Fig. 1 is the SEM figure of the zinc oxide nano rod of the embodiment of the invention 1.
Fig. 2 is the XRD figure of the zinc oxide nano rod of the embodiment of the invention 1.
Fig. 3 is the SEM figure of the zinc oxide nano rod of the embodiment of the invention 4.
Embodiment
Embodiment 1: take by weighing the sodium hydroxide of 3 g, add the water of 20 ml, add the cetyl trimethylammonium bromide of 0.1 g and the carbonyl diamine of 1.5 g after dissolution of sodium hydroxide, stir half an hour, be made into solution No. 1; Take by weighing the zinc nitrate of 2.5g, be dissolved in the water of 30 ml, be made into solution No. 2.No. 1 solution is heated to 70 ℃, with in No. 1 solution of No. 2 solution addings, reacted 20 minutes after 20 minutes; With white suspension centrifugation, with alcohol and water washing, 50 ℃ of dryings are 10 hours in the loft drier, obtain the zinc oxide nano rod powder.
Fig. 1 has provided the SEM figure of zinc oxide nano rod, and as seen from the figure, the nanometer rod diameter is about 100 nm, and length is about 350 nm.Fig. 2 is the XRD figure of zinc oxide nano rod, the demonstration of XRD data results, and the gained nanometer rod is standard hex wurtzite ZnO, diffraction peak is corresponding with the standard card JCPDS card number 36-1451 of ZnO.
Embodiment 2: take by weighing the sodium hydroxide of 2 g, add the water of 20 ml, add the cetyl trimethylammonium bromide of 0.15 g and the carbonyl diamine of 1.5 g after dissolution of sodium hydroxide, stir half an hour, be made into solution No. 1; Take by weighing the zinc acetate of 1.5 g, dissolve in the water of 20 ml, be made into solution No. 2.No. 1 solution is heated to 80 ℃, with in No. 1 solution of No. 2 solution addings, reacted 20 minutes after 20 minutes; With white suspension centrifugation, with alcohol and water washing, 60 ℃ of dryings are 9 hours in the loft drier, obtain the zinc oxide nano rod powder.The PH of change system is to the concentration that increases simultaneously cetyl trimethylammonium bromide, and the length of the zinc oxide nano rod of preparation and diameter proportion are 4:1.
Embodiment 3: take by weighing the potassium hydroxide of 3.5 g, add the water of 20 ml, add the cetyl trimethylammonium bromide of 0.1 g and the carbonyl diamine of 1.5 g after the potassium hydroxide dissolving, stir half an hour, be made into solution No. 1; Take by weighing the zinc acetate of 1.5 g, dissolve in the water of 20 ml, be made into solution No. 2.No. 1 solution is heated to 80 ℃, with in No. 1 solution of No. 2 solution addings, reacted 20 minutes after 20 minutes; With white suspension centrifugation, with alcohol and water washing, 60 ℃ of dryings are 9 hours in the loft drier, obtain the zinc oxide nano rod powder.With potassium hydroxide and sodium hydroxide highly basic, little on the net result impact, gained zinc oxide nano rod diameter is about 110 nm, and length is about 380 nm.
Embodiment 4: take by weighing the potassium hydroxide of 3.5 g, add the water of 20 ml, add the cetyl trimethylammonium bromide of 1.0 g and the carbonyl diamine of 2 g after the potassium hydroxide dissolving, stir half an hour, be made into solution No. 1; Take by weighing the zinc sulfate of 2 g, dissolve in the water of 30 ml, be made into solution No. 2.No. 1 solution is heated to 80 ℃, with in No. 1 solution of No. 2 solution addings, reacted 20 minutes after 20 minutes; With white suspension centrifugation, with alcohol and water washing, 60 ℃ of dryings are 9 hours in the loft drier, obtain the zinc oxide nano rod powder.Accompanying drawing 3 is the SEM figure of the zinc oxide nano rod of the present embodiment, increases as seen from the figure the content of carbonyl diamine, and the gained zinc oxide nano rod is self-assembled into flower-like structure.
Claims (4)
1. the preparation method of a zinc oxide nano rod is characterized in that, comprises the steps:
(1) join the sodium hydroxide that concentration is 1～4 mmol/ml, or potassium hydroxide aqueous solution;
(2) mol ratio by cetyl trimethylammonium bromide and sodium hydroxide is that 0.001:1～1:1 takes by weighing cetyl trimethylammonium bromide, adds in the sodium hydroxide solution;
(3) take by weighing carbonyl diamine adding step (2) by carbonyl diamine and sodium hydroxide mol ratio by 0.05:1～1:1 and joined solution, stirred 20 minutes to one hour;
(4) be that 0.03～3:1 takes by weighing the zinc precursor body by zinc precursor body and sodium hydroxide mol ratio, joining concentration is the zinc precursor liquid solution of 0.3～1M;
(5) step (3) gained solution is heated to 60～90 ℃, step (4) gained solution is injected, stir half an hour;
(6) the centrifugal white powder that obtains 50～80 ℃ of lower dryings, obtains zinc oxide nano rod.
2. the preparation method of described a kind of zinc oxide nano rod according to claim 1 is characterized in that, the described zinc precursor body of step (4) is a kind of or its combination in zinc nitrate, zinc acetate, the zinc sulfate.
3. the preparation method of described a kind of zinc oxide nano rod according to claim 1 is characterized in that, the described reaction conditions of step (5) is air atmosphere.
4. the preparation method of described a kind of zinc oxide nano rod according to claim 1 is characterized in that, the described drying means of step (6) is constant pressure and dry or vacuum-drying, and be 6～24 hours described time of drying.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675026A (en) * | 2013-11-27 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of classification self-assembly zinc oxide micro-nano structure for gas sensor |
| CN103771493A (en) * | 2014-02-14 | 2014-05-07 | 常州大学 | Method for preparing one-dimensional nano zinc oxide |
| CN104310458A (en) * | 2014-10-10 | 2015-01-28 | 九江学院 | Method for preparing zinc oxide nanorod |
| 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 |
| WO2016114625A1 (en) * | 2015-01-16 | 2016-07-21 | 고려대학교 산학협력단 | Nanoporous polymer membrane and method for preparing same |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (4)
| Title |
|---|
| HIROYUKI USUI: "The effect of surfactants on the morphology and optical properties of precipitated wurtzite ZnO", 《MATERIALS LETTERS》 * |
| Y.D. WANG ET AL.: "Synthesis and room temperature photoluminescence of ZnO/CTAB ordered layered nanocomposite with flake-like architecture", 《JOURNAL OF LUMINESCENCE》 * |
| 刘琳等: "纳米氧化锌的均匀沉淀法制备工艺研究", 《粉末冶金工业》 * |
| 孙继锋等: "棒状纳米氧化锌的制备及其光催化性能分析", 《安徽农业科学》 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103675026A (en) * | 2013-11-27 | 2014-03-26 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of classification self-assembly zinc oxide micro-nano structure for gas sensor |
| 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 |
| CN103771493A (en) * | 2014-02-14 | 2014-05-07 | 常州大学 | Method for preparing one-dimensional nano zinc oxide |
| CN103771493B (en) * | 2014-02-14 | 2016-01-27 | 常州大学 | A kind of method preparing one-D nano zinc oxide |
| CN104310458A (en) * | 2014-10-10 | 2015-01-28 | 九江学院 | Method for preparing zinc oxide nanorod |
| CN104310458B (en) * | 2014-10-10 | 2015-10-14 | 九江学院 | A kind of method preparing zinc oxide nano rod |
| WO2016114625A1 (en) * | 2015-01-16 | 2016-07-21 | 고려대학교 산학협력단 | Nanoporous polymer membrane and method for preparing same |
| 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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