CN102557105A - Monodisperse cerium oxide nanoparticle and preparation method thereof - Google Patents

Monodisperse cerium oxide nanoparticle and preparation method thereof Download PDF

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Publication number
CN102557105A
CN102557105A CN2011104599564A CN201110459956A CN102557105A CN 102557105 A CN102557105 A CN 102557105A CN 2011104599564 A CN2011104599564 A CN 2011104599564A CN 201110459956 A CN201110459956 A CN 201110459956A CN 102557105 A CN102557105 A CN 102557105A
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cerium oxide
cerium
oxide nanoparticles
disperses
salt
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CN102557105B (en
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王丹
胡柱东
毛丹
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Foshan Gaoming (cas) Center For New Materials
Institute of Process Engineering of CAS
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Foshan Gaoming (cas) Center For New Materials
Institute of Process Engineering of CAS
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Abstract

The invention provides a monodisperse cerium oxide nanoparticle and a preparation method thereof. Monodisperse cerium oxide nano-powder with high crystallinity can be prepared by controlling the reaction speed in a way of taking a soluble cerium salt, nitrate and a dispersant as reaction raw materials, taking water as a solvent and taking nitrate as a mineralizing agent and by controlling the concentration of a cerium salt solution, the proportions of reaction raw materials, hydrothermal time and hydrothermal temperature under a hydrothermal condition, and effective regulation and control over the particle diameter of cerium oxide is realized. The cerium oxide nano-powder prepared with the method has the advantages of uniform size distribution, high dispersity, simple preparation process, no need of complex raw material equipment, easiness for operating, low cost and high repeatability.

Description

Single cerium oxide nanoparticles and preparation method thereof of disperseing
Technical field
The invention belongs to the rare earth oxide field of materials, relate to a kind of single cerium oxide nanoparticles and preparation method thereof of disperseing.
Background technology
Cerium is a kind of important lanthanon, has good redox property.Cerium oxide is the highest active a kind of catalyzer in the rare earth oxide series, has comparatively unique crystalline structure, the higher oxygen storage capacity and the ability of release oxygen, stronger oxidation-reduction performance (Ce 3+/ Ce 4+), thereby received people's very big concern, be widely used in Industrial Catalysis, field such as precise polished.Nano-cerium oxide is adsorbed on has the redox property that can improve material on the active solid support material greatly.In high precision polishing, the homogeneity of the granularity of powder, pattern and distribution of sizes thereof has material impact, and particle is thin more, and it is even more to distribute, and then polishing effect is good more.
Chinese invention patent CN101792171A joins solubility cerium salt in water and the organic solvent mixing solutions, has prepared cerium oxide nanoballs through hydro-thermal reaction and combination calcining.Chinese invention patent CN101825551A as raw material, through twice hydro-thermal reaction, prepares the cerium oxide microballoon of 90~450nm with cerous salt.Chinese invention patent CN1699282A is a raw material with cerium salt and urea, adopts sluggish precipitation to synthesize the cerium oxide of submicron order.Chinese invention patent CN101306830A is the cerium source with the methyl ethyl diketone cerium, adopt the recirculation water solution, and the water-soluble spherical cerium oxide that between 225~240 ℃, has prepared median size and be 5~10nm is nanocrystalline.Chinese invention patent CN101541912A adopts the precursor solution of cerium to mix with precipitant solution and reacts, and simultaneously solution is carried out oxide treatment, and the ceria oxide powder particle diameter of preparation can be regulated between 50nm~3 μ m.
Foregoing invention prepares the process more complicated; Or need twice hydro-thermal reaction, or need follow-up calcination processing, maybe need use precipitation agent and organic solvent; And prepared product size distribution broad also has difficulties to effective control of morphology microstructure and size distribution.The present invention is intended to adopt simple raw material through a kind of easy technology, prepares the cerium oxide nano-powder of narrow size distribution.
Summary of the invention
The invention provides a kind of very easy hydro-thermal technology, adopt simple raw material can prepare the good dispersed nano cerium oxide nano-powder of crystallinity easily, distribution of sizes is narrower.Concrete technological process is: cerium salt, nitrate salt and dispersion agent are mixed according to a certain percentage and be dissolved in the water, and stirring obtains settled solution; The solution for preparing is put into reaction kettle, in baking oven, carry out hydro-thermal reaction; It is dry that the product of reaction after finishing put into baking oven through washing, washing with alcohol, after centrifugal, obtains cerium oxide nano-powder.
In the method for the invention, solubility cerium salt is ceric ammonium nitrate ((NH 4) 2Ce (NO 3) 6), the concentration of cerium solution is less than 1mol/L.Nitrate salt is one or several in lithium nitrate, SODIUMNITRATE, the saltpetre, and the mol ratio of cerium salt, nitrate salt is 1: 1.5~5.Dispersion agent is a kind of in polyoxyethylene glycol (PEG), Vinylpyrrolidone polymer (PVP), the polyoxyethylene (PEO), and the mass ratio of cerium salt and dispersion agent is 27.4~411: 1.
In the method for the invention, hydrothermal temperature is 120~220 ℃, and the hydro-thermal reaction time is 1~100h, 60~120 ℃ of oven dry in baking oven.
The present invention only needs under hydrothermal condition; Introduce nitrate salt as mineralizer, play the effect of controls reaction speed, make stable nucleation, deposition, the crystallization process of reaction experience; Need not follow-up high-temperature heat treatment, can prepare the good dispersed nano cerium oxide powder of crystallinity.Concentration, the ratio of reaction raw materials, hydro-thermal time, hydrothermal temperature through the control cerium solution can be realized the cerium oxide particle diameter controlled between 160~300nm.
The method of the invention has following beneficial effect:
1) production technique is simple, flow process is short, easy to operate, and good reproducibility;
2) raw material is simple, is solvent with water, need not with an organic solvent, has both practiced thrift cost, has reduced environmental pollution again;
3) a step hydro-thermal reaction can obtain the good nano cerium oxide powder of crystallization degree, need not additional high-temperature heat treatment, has reduced the technology cost;
4) good product dispersibility, narrow size distribution can be regulated and control particle diameter through temperature of reaction, reactant concn;
5) the prepared single cerium oxide nanoparticles of disperseing of the present invention can be used for aspects such as ultravioletlight screening, automotive exhaust catalysis, mechanical polishing.
Description of drawings
Fig. 1 is that embodiment 1 prepared list disperses the stereoscan photograph of cerium oxide nanoparticles, has the spherical morphology of corner angle, and size is homogeneous very, and particle diameter is 240 ± 2nm.
Fig. 2 is the XRD spectra of the prepared cerium oxide nanoparticles of embodiment 1, and is consistent with the result of JCPDS (34-0394) card, is the CeO of pure phase 2, and have good crystallinity.
Embodiment
Below in conjunction with specific embodiment the present invention is described in more detail and explains, but those skilled in the art will recognize that these embodiment only are used to illustrate the present invention, it does not constitute any restriction to scope of the present invention.
Embodiment 1
Take by weighing 2.74g ceric ammonium nitrate, 1.0g SODIUMNITRATE and 0.1g PEG 2000, be dissolved in the 15ml water,, obtain settled solution through the magnetic agitation thorough mixing.This solution is transferred in the reaction kettle, put into baking oven, 200 ℃ of hydro-thermal reactions 10 hours.After washing, washing with alcohol and spinning, throw out is placed 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 240 ± 2nm.
Embodiment 2
Take by weighing 4.11g ceric ammonium nitrate, 1.5g SODIUMNITRATE and 0.01g PEO, be dissolved in the 15ml water,, obtain clear solution through the magnetic agitation thorough mixing.This solution is transferred in the reaction kettle, put into baking oven, 220 ℃ of hydro-thermal reactions 1 hour.After washing, washing with alcohol and spinning, throw out is placed 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 270 ± 3nm.
Embodiment 3
Take by weighing 2.74g ceric ammonium nitrate, 2.0g lithium nitrate and 0.1g PVP, be dissolved in the 15ml water,, obtain settled solution through the magnetic agitation thorough mixing.This solution is transferred in the reaction kettle, put into baking oven, 120 ℃ of hydro-thermal reactions 100 hours.After washing, washing with alcohol and spinning, throw out is placed 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 180 ± 3nm.
Embodiment 4
Take by weighing 5.48g ceric ammonium nitrate, 2.0g SODIUMNITRATE and 0.8g PVP, be dissolved in the 15ml water,, obtain settled solution through the magnetic agitation thorough mixing.This solution is transferred in the reaction kettle, put into baking oven, 150 ℃ of hydro-thermal reactions 60 hours.After washing, washing with alcohol and spinning, throw out is placed 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 195 ± 3nm.
Embodiment 5
Take by weighing 2.74g ceric ammonium nitrate, 1.0g saltpetre and 0.18g PVP, be dissolved in the 15ml water,, obtain settled solution through the magnetic agitation thorough mixing.This solution is transferred in the reaction kettle, put into baking oven, 180 ℃ of hydro-thermal reactions 10 hours.After washing, washing with alcohol and spinning, throw out is placed 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 220 ± 3nm.

Claims (9)

1. single preparation method who disperses cerium oxide nanoparticles may further comprise the steps: cerium salt, nitrate salt and dispersion agent are mixed according to a certain percentage and be dissolved in the water, and stirring obtains settled solution; The solution for preparing is put into reaction kettle, in baking oven, carry out hydro-thermal reaction; It is dry that the product of reaction after finishing put into baking oven through washing, washing with alcohol, after centrifugal, obtains cerium oxide powder.
2. single preparation method who disperses cerium oxide nanoparticles according to claim 1 is characterized in that said solubility cerium salt is ceric ammonium nitrate.
3. single preparation method who disperses cerium oxide nanoparticles according to claim 1 is characterized in that the concentration of cerium solution is less than 1mol/L.
4. single preparation method who disperses cerium oxide nanoparticles according to claim 1 is characterized in that said nitrate salt is one or several in lithium nitrate, SODIUMNITRATE, the saltpetre.
5. single preparation method who disperses cerium oxide nanoparticles according to claim 1 is characterized in that, said dispersion agent is a kind of in polyoxyethylene glycol, Vinylpyrrolidone polymer, the polyoxyethylene.
6. single preparation method who disperses cerium oxide nanoparticles according to claim 1 is characterized in that hydrothermal temperature is 120~220 ℃, and the hydro-thermal reaction time is 1~100h.
7. single preparation method who disperses cerium oxide nanoparticles according to claim 1 is characterized in that the mol ratio of cerium salt, nitrate salt is 1: 1.5~5.
8. single preparation method who disperses cerium oxide nanoparticles according to claim 1 is characterized in that the mass ratio of cerium salt and dispersion agent is 27.4~411: 1.
9. single cerium oxide nanoparticles of disperseing is prepared by any described method among the claim 1-8, and size homogeneous, particle diameter are controlled between 160~300nm.
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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102877131A (en) * 2012-10-19 2013-01-16 浙江大学 Preparation method of octahedral structural perovskite lead titanate single crystal nano particles
CN105170130A (en) * 2015-09-02 2015-12-23 中国科学院新疆理化技术研究所 Preparation method and application of high-dispersion CeO2 modified TiO2 meso-porous photocatalyst
CN105417591A (en) * 2015-11-24 2016-03-23 青岛能迅新能源科技有限公司 Method for preparing nickel cobaltite nano material through solvothermal method
CN106145177A (en) * 2016-07-10 2016-11-23 九江学院 A kind of preparation method of small particle ceria nano-crystalline
CN108238627A (en) * 2018-04-20 2018-07-03 内江师范学院 The preparation method of the micro-nano ceria of high-specific surface area
CN108249471A (en) * 2018-04-20 2018-07-06 内江师范学院 A kind of method for preparing the micro-nano ceria of high-specific surface area
CN108929489A (en) * 2018-08-31 2018-12-04 芜湖盈奇塑业有限公司 A kind of ageing resistance polypropylene water horse enclosing and preparation method thereof
CN109135062A (en) * 2018-08-31 2019-01-04 芜湖盈奇塑业有限公司 A kind of preparation method of high waterproof performance water horse enclosing
CN111434380A (en) * 2019-01-11 2020-07-21 北京化工大学 Preparation method and application of oil-soluble monodisperse metal oxide nano catalyst
CN111579515A (en) * 2020-05-26 2020-08-25 山东理工大学 Method for oxidizing TMB by using nano-cerium dioxide as simulated oxidase
WO2021072641A1 (en) * 2019-10-15 2021-04-22 诸暨易联众创企业管理服务有限公司 Method for preparing ceric dioxide-based nanomaterial
CN115353639A (en) * 2022-07-12 2022-11-18 昆明理工大学 Method for preparing potassium humate by using corn straws and application
CN115974127A (en) * 2022-11-25 2023-04-18 深圳市聚芯半导体材料有限公司 Quasi-spherical nano cerium dioxide, suspension thereof, preparation method and application
JP2023545573A (en) * 2020-11-24 2023-10-30 ライナス レア アース リミテッド Materials, methods and techniques for producing doped cerium oxide

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1546382A (en) * 2003-12-10 2004-11-17 山东师范大学 Method for synthesizing cadmium hydroxide single-crystal nanowire

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1546382A (en) * 2003-12-10 2004-11-17 山东师范大学 Method for synthesizing cadmium hydroxide single-crystal nanowire

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
FU ZHOU ET AL.: "CeO2 Spherical Crystallites: Synthesis, Formation Mechanism, Size Control, and Electrochemical Property Study", 《J. PHYS. CHEM. C》 *
MASANORI HIRANO ET AL.: "Preparation and spherical agglomeration of crystalline cerium(Ⅳ)oxide nanoparticles by thermal hydrolysis", 《J. AM. CERAM. SOC》 *
YULAN LIU ET AL: "Wet Chemical Preparation of Well-dispersed Colloidal Cerium Oxide Nanocrystals", 《CHEMISTRY LETTERS》 *
谢丽英等: "纳米氧化铈粉体的制备技术研究进展", 《稀土》 *
陈建君等: "纳米二氧化铈的低温水热一步法合成", 《材料导报》 *

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102877131A (en) * 2012-10-19 2013-01-16 浙江大学 Preparation method of octahedral structural perovskite lead titanate single crystal nano particles
CN102877131B (en) * 2012-10-19 2015-04-29 浙江大学 Preparation method of octahedral structural perovskite lead titanate single crystal nano particles
CN105170130A (en) * 2015-09-02 2015-12-23 中国科学院新疆理化技术研究所 Preparation method and application of high-dispersion CeO2 modified TiO2 meso-porous photocatalyst
CN105170130B (en) * 2015-09-02 2017-09-22 中国科学院新疆理化技术研究所 High dispersive CeO2Modify TiO2Mesoporous photocatalytic agent preparation method and application
CN105417591A (en) * 2015-11-24 2016-03-23 青岛能迅新能源科技有限公司 Method for preparing nickel cobaltite nano material through solvothermal method
CN106145177A (en) * 2016-07-10 2016-11-23 九江学院 A kind of preparation method of small particle ceria nano-crystalline
CN108238627A (en) * 2018-04-20 2018-07-03 内江师范学院 The preparation method of the micro-nano ceria of high-specific surface area
CN108249471A (en) * 2018-04-20 2018-07-06 内江师范学院 A kind of method for preparing the micro-nano ceria of high-specific surface area
CN108929489A (en) * 2018-08-31 2018-12-04 芜湖盈奇塑业有限公司 A kind of ageing resistance polypropylene water horse enclosing and preparation method thereof
CN109135062A (en) * 2018-08-31 2019-01-04 芜湖盈奇塑业有限公司 A kind of preparation method of high waterproof performance water horse enclosing
CN111434380A (en) * 2019-01-11 2020-07-21 北京化工大学 Preparation method and application of oil-soluble monodisperse metal oxide nano catalyst
CN111434380B (en) * 2019-01-11 2021-12-21 北京化工大学 Preparation method and application of oil-soluble monodisperse metal oxide nano catalyst
WO2021072641A1 (en) * 2019-10-15 2021-04-22 诸暨易联众创企业管理服务有限公司 Method for preparing ceric dioxide-based nanomaterial
CN111579515A (en) * 2020-05-26 2020-08-25 山东理工大学 Method for oxidizing TMB by using nano-cerium dioxide as simulated oxidase
JP2023545573A (en) * 2020-11-24 2023-10-30 ライナス レア アース リミテッド Materials, methods and techniques for producing doped cerium oxide
JP7505124B2 (en) 2020-11-24 2024-06-24 ライナス レア アース リミテッド Materials, methods and techniques for producing doped cerium oxide
US12049407B2 (en) 2020-11-24 2024-07-30 Lynas Rare Earths Limited Materials, methods and techniques for generating doped cerium oxide
CN115353639A (en) * 2022-07-12 2022-11-18 昆明理工大学 Method for preparing potassium humate by using corn straws and application
CN115353639B (en) * 2022-07-12 2023-08-08 昆明理工大学 Method for preparing potassium humate by using corn straw and application
CN115974127A (en) * 2022-11-25 2023-04-18 深圳市聚芯半导体材料有限公司 Quasi-spherical nano cerium dioxide, suspension thereof, preparation method and application

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