CN102050479A - Ceric oxide nanorod and preparation method thereof - Google Patents

Ceric oxide nanorod and preparation method thereof Download PDF

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Publication number
CN102050479A
CN102050479A CN 201110028775 CN201110028775A CN102050479A CN 102050479 A CN102050479 A CN 102050479A CN 201110028775 CN201110028775 CN 201110028775 CN 201110028775 A CN201110028775 A CN 201110028775A CN 102050479 A CN102050479 A CN 102050479A
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cerium dioxide
dioxide nano
nano rod
preparation
solution
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CN102050479B (en
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庞来学
唐新德
史红
张金升
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Shandong Jiaotong University
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Shandong Jiaotong University
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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

A kind of cerium dioxide nano rod and preparation method thereof
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 more and more higher.Therefore, nano Ce O 2Preparation, functional performance and applied research become a problem that presses for solution.
Summary of the invention
At the deficiencies in the prior art, the problem to be solved in the present invention 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 of the present 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) precipitation and the solution that obtains in the step (2) is transferred in the reactor, screws kettle cover, place 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 was calcined 3～4 hours under 450～500 ℃, air atmosphere, and 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: described Ce (NO 3) 36H 2O is an analytical pure.
Among the preparation method of above-mentioned cerium dioxide nano rod: described concentration of sodium hydroxide solution is preferably 6～8mol/L.
Among the preparation method of above-mentioned cerium dioxide nano rod: described reactor 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 described reactor heating, preferably 60 hours reaction times.
Among the preparation method of above-mentioned cerium dioxide nano rod: preferably calcining 3 hours under 480 ℃, air atmosphere of the product that described step (4) makes.
Cerium dioxide nano rod of the present invention 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, and preferred above method makes.
Further preferred mode is: described 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 precipitation, 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
The invention will be further described below in conjunction with embodiment, but be not limited thereto.
Embodiment 1
Concrete steps are as follows:
(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 precipitation of white gradually, continued magnetic agitation 30 minutes;
(3) with in the precipitation and solution transferase 45 0ml water heating kettle that obtain in the step (2), screw kettle cover, place baking oven, after the product centrifugation, use deionized water and absolute ethanol washing 3～4 times respectively 150 ℃ of reactions 48 hours;
(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 precipitation of white gradually, continued magnetic agitation 30 minutes;
(3) with in the precipitation and solution transferase 45 0ml water heating kettle that obtain in the step (2), screw kettle cover, place baking oven, after the product centrifugation, use deionized water and absolute ethanol washing 3～4 times respectively 160 ℃ of reactions 60 hours;
(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 precipitation of white gradually, continued magnetic agitation 30 minutes;
(3) with in the precipitation and solution transferase 45 0ml water heating kettle that obtain in the step (2), screw kettle cover, place baking oven, after the product centrifugation, use deionized water and absolute ethanol washing 3～4 times respectively 170 ℃ of reactions 72 hours;
(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 (8)

1. the preparation method of a 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, 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) precipitation and the solution that obtains in the step (2) is transferred in the reactor, screws kettle cover, place 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 was calcined 3～4 hours under 450～500 ℃, air atmosphere, and promptly preparing diameter is that 30～60nm, length are the CeO of 300～600nnm 2Monodimension nano stick.
2. the preparation method of cerium dioxide nano rod according to claim 1 is characterized in that: described Ce (NO 3) 36H 2O is an analytical pure.
3. the preparation method of cerium dioxide nano rod according to claim 1, it is characterized in that: described concentration of sodium hydroxide solution is 6～8mol/L.
4. the preparation method of cerium dioxide nano rod according to claim 1, it is characterized in that: described reactor is the stainless steel cauldron of polytetrafluoroethylsubstrate substrate.
5. the preparation method of cerium dioxide nano rod according to claim 1, it is characterized in that: the temperature of described reactor heating is 160 ℃, and the reaction times is 60 hours.
6. the preparation method of cerium dioxide nano rod according to claim 1 is characterized in that: the product that described step (4) makes calcining 3 hours under 480 ℃, air atmosphere.
7. cerium dioxide nano rod, it is characterized in that: described cerium dioxide nano rod is made by the described method of claim 1; Wherein said cerium dioxide nano rod is that diameter is that 30～60nm, length are the cerium dioxide monodimension nano stick of 300～600nnm.
8. cerium dioxide nano rod as claimed in claim 7 is characterized in that: described cerium dioxide nano rod is that diameter is that 40～50nm, length are the cerium dioxide monodimension nano stick of 400～500nnm.
CN2011100287756A 2011-01-27 2011-01-27 Ceric oxide nanorod and preparation method thereof Expired - Fee Related CN102050479B (en)

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Cited By (16)

* Cited by examiner, † Cited by third party
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CN102583495A (en) * 2012-02-23 2012-07-18 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
CN102849774A (en) * 2012-01-10 2013-01-02 浙江理工大学 Method for preparing nanometer cerium oxide by hydrothermal method
CN103143353A (en) * 2013-04-02 2013-06-12 厦门大学 Preparation method of reduced palladium catalyst
CN104150437A (en) * 2014-08-01 2014-11-19 宁波大学 Macroporous material carried with cerium oxide nano-rods
CN105502468A (en) * 2015-12-22 2016-04-20 天津大学 Ceric oxide nanorod and preparation method and application thereof
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
CN107746069A (en) * 2017-10-18 2018-03-02 西北师范大学 The method that hydro-thermal method prepares different-shape ceria
CN111454126A (en) * 2020-05-20 2020-07-28 浙江师范大学 Nano rod-like CeO2Application 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
CN112516997A (en) * 2020-11-30 2021-03-19 南京邮电大学 CeO2/MnO2Method for preparing nano-rod
CN113772710A (en) * 2021-10-11 2021-12-10 陕西科技大学 Preparation method and application of cerium dioxide nanowire
CN115124064A (en) * 2022-06-15 2022-09-30 厦门稀土材料研究所 Cerium dioxide nano material and preparation method and application thereof
CN115555010A (en) * 2022-08-17 2023-01-03 广州大学 Oxygen vacancy-rich mesoporous nanorod photocatalyst, 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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CN101407330A (en) * 2008-10-30 2009-04-15 上海大学 Method of preparing cerium oxide nano-rod
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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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Cited By (21)

* Cited by examiner, † Cited by third party
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
CN102583495A (en) * 2012-02-23 2012-07-18 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
CN103143353A (en) * 2013-04-02 2013-06-12 厦门大学 Preparation method of reduced palladium catalyst
CN103143353B (en) * 2013-04-02 2014-12-03 厦门大学 Preparation method of reduced palladium catalyst
CN104150437A (en) * 2014-08-01 2014-11-19 宁波大学 Macroporous material carried with cerium oxide nano-rods
CN105502468A (en) * 2015-12-22 2016-04-20 天津大学 Ceric oxide nanorod and preparation method and application thereof
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
CN107746069A (en) * 2017-10-18 2018-03-02 西北师范大学 The method that hydro-thermal method prepares different-shape ceria
CN111454126A (en) * 2020-05-20 2020-07-28 浙江师范大学 Nano rod-like CeO2Application of nanocrystalline catalyst in gas-solid phase crotonaldehyde selective hydrogenation catalytic reaction
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
CN112516997A (en) * 2020-11-30 2021-03-19 南京邮电大学 CeO2/MnO2Method for preparing nano-rod
CN113772710A (en) * 2021-10-11 2021-12-10 陕西科技大学 Preparation method and application of cerium dioxide nanowire
CN115124064A (en) * 2022-06-15 2022-09-30 厦门稀土材料研究所 Cerium dioxide nano material and preparation method and application thereof
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
CN115555010A (en) * 2022-08-17 2023-01-03 广州大学 Oxygen vacancy-rich mesoporous nanorod photocatalyst, preparation method and application
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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