CN102050479B - Ceric oxide nanorod and preparation method thereof - Google Patents
Ceric oxide nanorod and preparation method thereof Download PDFInfo
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- CN102050479B CN102050479B CN2011100287756A CN201110028775A CN102050479B CN 102050479 B CN102050479 B CN 102050479B CN 2011100287756 A CN2011100287756 A CN 2011100287756A CN 201110028775 A CN201110028775 A CN 201110028775A CN 102050479 B CN102050479 B CN 102050479B
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Abstract
The invention discloses a preparation method of a ceric oxide nanorod. The prepared ceric oxide nanorod is a ceric oxide one-dimension nanorod of which the diameter is 30-60nm and the length is 300-600nnm. The method disclosed by the invention is simple and quick, and can be used for preparing the ceric oxide nanorods with controllable diameters and lengths according to demands for functions. The prepared nanorod has the advantages of uniform dimension and favorable dispersity, has abundant active crystal faces, and can be widely used in the fields of catalysts, photoelectric nano devices and the like.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, be specifically related to a kind of preparation method of cerium dioxide nano rod.
Background technology
Nano Ce O
2Be the extremely wide rare earth material of a kind of purposes, can be widely used in catalyzer, electronic ceramics, uv-absorbing agent etc.
In recent years, people are for the nano Ce O of special appearance
2Research quite a few, pattern also differs from one another.For example; Chinese patent 200910062703.6 is with a kind of ceria nano-crystalline microsphere of graded structure of low temperature method preparation; This cerium dioxide nano microballoon is to be presoma with the cerium compound, is that solvent and tensio-active agent react under the abundant heating condition of oil and make with the phenylcarbinol.Patent CN101168447A is a basic raw material with cerium salt, and alcohol is as organic solvent, and solvent thermal reaction obtains presoma after for some time, and high-temperature calcination obtains the three-dimensional structure cerium dioxide that six square rods are formed.Patent CN101205078A is a precursor with solubility cerium salt, and adding excessive sodium hydroxide is precipitation agent, Hydrothermal Preparation cerium dioxide nano-tube, thickness of pipe 5～7nm, bore are 10～20nm.
CeO behind the nanometer
2Have special nature and application, high-tech development is to nano Ce O
2Pattern, particle diameter etc. require also increasingly high.Therefore, nano Ce O
2Preparation, functional performance and applied research become a problem that presses for solution.
Summary of the invention
To the deficiency of prior art, the problem that the present invention will solve provides a kind of preparation method of cerium dioxide nano rod.The cerium dioxide nano rod diameter Distribution of utilizing the present invention to prepare is narrow, length controlled, and reaction time is short, the CeO of good reproducibility
2Nanometer rod.
The preparation method of cerium dioxide nano rod according to the invention, step is:
(1) with Ce (NO
3)
36H
2O at room temperature is dissolved in the deionized water, and being mixed with concentration is 0.1～0.2molL
-1Cerium nitrate solution, again with 80r/min～150r/min stir speed (S.S.), stir 15min～30min, make the solution homogeneous transparent;
(2) by the mol ratio of cerous nitrate and sodium hydroxide be 1: 3～1: 4 amount; Dropwise to splash into concentration be 5～10mol/L sodium hydroxide solution to magnetic agitation limit, limit in the solution that step (1) makes; After engendering white depositions in the solution, continued magnetic agitation 20～50 minutes;
(3) deposition that obtains in the step (2) and solution are transferred in the reaction kettle, the kettle cover of screwing places under 150～170 ℃ of temperature and reacted 48～72 hours;
(4) centrifugal to step (3) reactant routine, separated products is used deionized water and absolute ethanol washing respectively 3～4 times, then in 60 ℃ of oven dry 24～30 hours;
(5) product that step (4) is made calcining 3～4 hours under 450～500 ℃, air atmosphere, promptly preparing diameter is that 30～60nm, length are the CeO of 300～600nnm
2Monodimension nano stick.
Among the preparation method of above-mentioned cerium dioxide nano rod: said Ce (NO
3)
36H
2O is an analytical pure.
Among the preparation method of above-mentioned cerium dioxide nano rod: said concentration of sodium hydroxide solution is preferably 6～8mol/L.
Among the preparation method of above-mentioned cerium dioxide nano rod: said reaction kettle is the stainless steel cauldron of polytetrafluoroethylsubstrate substrate preferably.
Among the preparation method of above-mentioned cerium dioxide nano rod: preferably 160 ℃ of the temperature of said reaction kettle heating, preferably 60 hours reaction times.
Among the preparation method of above-mentioned cerium dioxide nano rod: the product that said step (4) makes was preferably calcined 3 hours down at 480 ℃, air atmosphere.
Cerium dioxide nano rod according to the invention, it is characterized in that: described cerium dioxide nano rod is that diameter is that 30～60nm, length are the cerium dioxide monodimension nano stick of 300～600nnm, preferred above method makes.
Further preferred mode is: said cerium dioxide nano rod is that diameter is that 40～50nm, length are the cerium dioxide monodimension nano stick of 400～500nnm.
The invention has the beneficial effects as follows: the reactant that is dissolved in aqueous phase reaction under hydrothermal condition, in the nano level space generates deposition, thereby obtains the cerium dioxide nano rod.Overcome synthesis of nano CeO among the patent CN 101538061A
2Diameter and the defective of length distribution broad.Preparation is simple for this, and preparation cycle is short, and the cerium dioxide nano rod homogeneity that makes is good.
CeO of the present invention
2Nanometer rod has a large amount of surfactivity crystal faces, therefore good application is arranged aspect catalytic material, for the Application and Development of studying carefully of functional materials is had laid a good foundation.
Embodiment
Below in conjunction with embodiment the present invention is described further, but is not limited thereto.
Embodiment 1
Concrete steps are following:
(1) at room temperature with Ce (NO
3)
36H
2O is mixed with 0.1molL
-1Solution;
(2) be that the magnetic agitation limit, sodium hydroxide (NaOH) solution limit of 5mol/L dropwise splashes in the solution that step (1) obtains with concentration, separate out the tiny deposition of white gradually, continued magnetic agitation 30 minutes;
(3) with in deposition that obtains in the step (2) and the solution transferase 45 0ml water heating kettle, the kettle cover of screwing places baking oven 150 ℃ of reactions 48 hours, after the product spinning, uses deionized water and absolute ethanol washing 3～4 times respectively;
(4) with the sample of step (3) gained 60 ℃ of dryings 24 hours;
(5) with the calcining 3 hours under 450 ℃, air atmosphere of the sample of step (4) gained, can prepare CeO
2Monodimension nano stick, the diameter of nanometer rod are 30～40nm, and length is 300～400nm.
Embodiment 2
(1) at room temperature with Ce (NO
3)
36H
2O is mixed with 0.15molL
-1Solution;
(2) be that the magnetic agitation limit, sodium hydroxide (NaOH) solution limit of 8mol/L dropwise splashes in the solution that step (1) obtains with concentration, separate out the tiny deposition of white gradually, continued magnetic agitation 30 minutes;
(3) with in deposition that obtains in the step (2) and the solution transferase 45 0ml water heating kettle, the kettle cover of screwing places baking oven 160 ℃ of reactions 60 hours, after the product spinning, uses deionized water and absolute ethanol washing 3～4 times respectively;
(4) with the sample of step (3) gained 60 ℃ of dryings 24 hours;
(5) with the calcining 3 hours under 480 ℃, air atmosphere of the sample of step (4) gained, can prepare CeO
2Monodimension nano stick, the diameter of nanometer rod are 40～50nm, and length is 400～500nm.
Embodiment 3
(1) at room temperature with Ce (NO
3)
36H
2O is mixed with 0.2molL
-1Solution;
(2) be that the magnetic agitation limit, sodium hydroxide (NaOH) solution limit of 10mol/L dropwise splashes in the solution that step (1) obtains with concentration, separate out the tiny deposition of white gradually, continued magnetic agitation 30 minutes;
(3) with in deposition that obtains in the step (2) and the solution transferase 45 0ml water heating kettle, the kettle cover of screwing places baking oven 170 ℃ of reactions 72 hours, after the product spinning, uses deionized water and absolute ethanol washing 3～4 times respectively;
(4) with the sample of step (3) gained 60 ℃ of dryings 24 hours;
(5) with the calcining 3 hours under 500 ℃, air atmosphere of the sample of step (4) gained, can prepare CeO
2Monodimension nano stick, the diameter of nanometer rod are 50～60nm, and length is 500～600nm.
Claims (2)
1. the preparation method of cerium dioxide nano rod, step is:
(1) with Ce (NO
3)
36H
2O at room temperature is dissolved in the deionized water, and being mixed with concentration is 0.1～0.2molL
-1Cerium nitrate solution, again with 80r/min～150r/min stir speed (S.S.), stir 15min～30min, make the solution homogeneous transparent;
(2) by the mol ratio of cerous nitrate and sodium hydroxide be 1: 3～1: 4 amount, magnetic agitation limit in limit dropwise splashes into sodium hydroxide solution in the solution that step 1) makes, and after engendering white depositions in the solution, continues magnetic agitation 20～50 minutes;
(3) deposition that obtains in the step (2) and solution are transferred in the reaction kettle, the kettle cover of screwing places under 150～170 ℃ of temperature and reacted 48～72 hours;
(4) centrifugal to step (3) reactant routine, separated products is used deionized water and absolute ethanol washing respectively 3～4 times, then in 60 ℃ of oven dry 24～30 hours;
(5) product that step (4) is made calcining 3～4 hours under 450～500 ℃, air atmosphere, promptly preparing diameter is that 30～60nm, length are the CeO of 300～600nm
2Monodimension nano stick;
It is characterized in that: the concentration of said sodium hydroxide solution is 5～10mol/L.
2. the preparation method of cerium dioxide nano rod according to claim 1, it is characterized in that: said concentration of sodium hydroxide solution is 6～8mol/L.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011100287756A CN102050479B (en) | 2011-01-27 | 2011-01-27 | Ceric oxide nanorod and preparation method thereof |
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| CN2011100287756A CN102050479B (en) | 2011-01-27 | 2011-01-27 | Ceric oxide nanorod and preparation method thereof |
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| CN102050479B true CN102050479B (en) | 2012-05-23 |
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Families Citing this family (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102849774A (en) * | 2012-01-10 | 2013-01-02 | 浙江理工大学 | Method for preparing nanometer cerium oxide by hydrothermal method |
| CN102583495B (en) * | 2012-02-23 | 2014-08-06 | 清华大学 | Preparation method of rare earth metal ion doping cerium oxide nanometer material |
| CN102674431A (en) * | 2012-05-08 | 2012-09-19 | 南京大学 | Method for controllably synthesizing CeO2 nanobelt, CeO2 nanorod and CeO2 nanowire through promotion of formaldehyde |
| CN103143353B (en) * | 2013-04-02 | 2014-12-03 | 厦门大学 | Preparation method of reduced palladium catalyst |
| CN104150437B (en) * | 2014-08-01 | 2015-10-07 | 宁波大学 | A kind of large pore material of Supporting cerium oxide nanometer rods |
| CN105502468B (en) * | 2015-12-22 | 2017-06-16 | 天津大学 | A kind of ceric oxide nanorod and its preparation method and application |
| CN107243339A (en) * | 2017-06-22 | 2017-10-13 | 南昌航空大学 | A kind of preparation method of ceric oxide nanorod photochemical catalyst |
| CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
| CN107746069B (en) * | 2017-10-18 | 2019-10-18 | 西北师范大学 | The method that hydro-thermal method prepares different-shape ceria |
| CN111454126B (en) * | 2020-05-20 | 2023-06-02 | 浙江师范大学 | Nano rod-like CeO 2 Application of nanocrystalline catalyst in gas-solid phase crotonaldehyde selective hydrogenation catalytic reaction |
| CN111592029A (en) * | 2020-05-29 | 2020-08-28 | 淮阴师范学院 | Preparation method of rod-shaped silver-plated cerium dioxide |
| CN112516997B (en) * | 2020-11-30 | 2023-04-18 | 南京邮电大学 | CeO 2 /MnO 2 Method for preparing nano-rod |
| CN113772710B (en) * | 2021-10-11 | 2023-01-03 | 陕西科技大学 | Preparation method and application of cerium dioxide nanowire |
| CN115124064B (en) * | 2022-06-15 | 2023-08-29 | 厦门稀土材料研究所 | Cerium dioxide nano material and preparation method and application thereof |
| CN115555010B (en) * | 2022-08-17 | 2024-02-02 | 广州大学 | Mesoporous nanorod photocatalyst rich in oxygen vacancies, preparation method and application |
| CN115571904A (en) * | 2022-09-26 | 2023-01-06 | 武汉工程大学 | Growing CeO on SiC powder 2 Method for preparing nano-rod and SiC loaded CeO prepared by method 2 Nano-rod composite structure |
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|---|---|---|---|---|
| WO2006096936A1 (en) * | 2005-03-18 | 2006-09-21 | Advanced Nanotechnology Limited | Rare earth nanorods |
| CN1840480A (en) * | 2005-03-29 | 2006-10-04 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN101407330A (en) * | 2008-10-30 | 2009-04-15 | 上海大学 | Method of preparing cerium oxide nano-rod |
| CN101717108A (en) * | 2009-11-12 | 2010-06-02 | 济南大学 | Industrial preparation method of rare earth hydrate and oxide nano-rod |
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2011
- 2011-01-27 CN CN2011100287756A patent/CN102050479B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006096936A1 (en) * | 2005-03-18 | 2006-09-21 | Advanced Nanotechnology Limited | Rare earth nanorods |
| CN1840480A (en) * | 2005-03-29 | 2006-10-04 | 中国科学院大连化学物理研究所 | Cerium oxide nano materials and its preparation and use |
| CN101407330A (en) * | 2008-10-30 | 2009-04-15 | 上海大学 | Method of preparing cerium oxide nano-rod |
| CN101717108A (en) * | 2009-11-12 | 2010-06-02 | 济南大学 | Industrial preparation method of rare earth hydrate and oxide nano-rod |
Non-Patent Citations (1)
| Title |
|---|
| 尹小斌.几种稀土纳米材料的合成及性能研究.《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》.2011,(第01期),37-38. * |
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