CN106186036B - A kind of preparation method of hexagon cerium dioxide nano sheet material - Google Patents

A kind of preparation method of hexagon cerium dioxide nano sheet material Download PDF

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Publication number
CN106186036B
CN106186036B CN201610536097.7A CN201610536097A CN106186036B CN 106186036 B CN106186036 B CN 106186036B CN 201610536097 A CN201610536097 A CN 201610536097A CN 106186036 B CN106186036 B CN 106186036B
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China
Prior art keywords
hexagon
dioxide nano
cerium
cerium dioxide
sheet material
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CN201610536097.7A
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Chinese (zh)
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CN106186036A (en
Inventor
王殿元
王庆凯
王侃民
王芳
郭艳艳
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Jiujiang University
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Jiujiang University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/22—Particle morphology extending in two dimensions, e.g. plate-like with a polygonal circumferential shape

Abstract

The invention discloses a kind of preparation method of hexagon cerium dioxide nano sheet material, first using six water cerous nitrates and sodium fluoborate as raw material, water is solvent, and polyvinyl alcohol is surfactant, is heated to 80 DEG C of reactions, through centrifugation, washing, obtains nanometer cerium fluoride；Then gained nanometer cerium fluoride is mixed with sodium hydrate aqueous solution, heated sealed is moved in reactor to 180 DEG C, react 24 ~ 48h, cool down, centrifuge, wash, dry, then desciccate is annealed 1h in 600 DEG C of Muffle furnaces, obtain hexagon cerium dioxide nano piece, the 10nm of thickness 8, the 60nm of the length of side 50.This hexagon sheet cerium dioxide nano material good dispersion, with larger specific surface area, there is good application prospect in terms of catalyst, polishing material and fuel-cell electrolyte.

Description

A kind of preparation method of hexagon cerium dioxide nano sheet material
Technical field
The present invention relates to a kind of preparation method of hexagon cerium dioxide nano sheet material, nano material technology is particularly belonged to Field.
Background technology
Ceria is a kind of rare earth oxide material of high activity, with Ce4+And Ce3+Two kinds of variable valences, it stores Oxygen performance and catalytic capability are high, are widely used in auto-exhaust catalyst, polishing material, fuel-cell electrolyte, UV absorption The fields such as agent, vehicle exhaust absorbent, electronic ceramics.Nano-flake material is one of study hotspot of current nano material.By There is strong crystallization tendency in ceria, obtain single dispersing, flake nano ceria difficulty it is very big.But in recent years Come, the preparation method of cerium dioxide nano piece is more and more, has achieved many progress.Such as patent of invention CN201410193490.1 is with CeCl3·7H2O and urea are raw material, and ethylenediamine is template, and hydro-thermal method obtains hexagon nanometer Platy cerium oxide；Wang Dianyuan etc.（Angew. Chem. Int. Ed.2005,44:3256-3260）With oleic acid, oleyl amine and 1- ten Eight alkene are solvent, hydrate cerium acetate are thermally decomposed at 300-360 DEG C, sodium pyrophosphate or enuatrol are mineralizer, are prepared for single point Scattered square and strip cerium dioxide nano piece；Patent of invention CN201310194946.1 is using cerous nitrate or cerium chloride as original Material, reaction in excessive ammonia, reactor is added dropwise at -10 ~ 20 DEG C and obtains platy cerium oxide, thickness 10-30nm.It is existing from current research From the point of view of shape, otherwise flake nano ceria preparation technology employs the oil-based solvent of costliness, otherwise the ceria prepared is received Rice piece it is thicker, specific surface area is not big enough, thus develop it is a kind of it is inexpensive, simple to operate without template new method production ultra-thin two Cerium oxide nano-plate tool is of great significance.
The content of the invention
It is an object of the invention to provide a kind of preparation method of hexagon cerium dioxide nano sheet material, especially by with Lower technical scheme is realized.
The present invention discloses a kind of preparation method of hexagon cerium dioxide nano sheet material, comprises the following steps：
（1）Six water cerous nitrate 0.868g are dissolved in 30ml pure water, 0.4 gram of polyvinyl alcohol and 1.32 grams of fluoboric acid are added Sodium, magnetic agitation is simultaneously heated to 80 DEG C, insulation 60min；After reaction product cooling, be centrifuged, pure water 2 times, obtain Nanometer cerium fluoride；The mol ratio of six water cerous nitrates and sodium fluoborate is 1:6-8, polyvinyl alcohol water solution concentration 1-2%（Quality point Number）.
（2）In step（1）In the nanometer cerium fluoride of gained, 1M NaOH aqueous solution 30ml are added, in polytetrafluoroethyl-ne alkene reaction Heated sealed is to 180 DEG C in kettle, reacts 24 ~ 48h, and the centrifugation of reacted mixed liquor is obtained into sediment, with pure water 2 times, 60 DEG C of dry 24h, and 600 DEG C of annealing 1h in Muffle furnace, obtain hexagon cerium dioxide nano sheet material.
Beneficial effects of the present invention:It is, with cerous nitrate and sodium fluoborate reaction, to prepare in the preparation method of the present invention Cerium fluoride, then using hydro-thermal method, is transformed into after cerium hydroxide, annealing and obtains hexagon two by nanometer cerium fluoride with NaOH alkali lye Cerium oxide nano sheet material, the thickness 8-10nm of nanometer sheet, length of side 50-60nm.This cerium dioxide nano sheet material dispersiveness It is good, with larger specific surface area, have in terms of catalyst, polishing material and fuel-cell electrolyte before good application Scape.
Brief description of the drawings
Fig. 1 is the SEM photograph of hexagon cerium dioxide nano sheet material of the present invention.
Embodiment
Embodiment 1
A kind of preparation method of hexagon cerium dioxide nano sheet material, comprises the following steps：
（1）Six water cerous nitrate 0.868g are dissolved in 30ml pure water, 0.4 gram of polyvinyl alcohol and 1.32 grams of fluoboric acid are added Sodium, magnetic agitation is simultaneously heated to 80 DEG C, insulation 60min；After reaction product cooling, be centrifuged, pure water 2 times, obtain Nanometer cerium fluoride；
（2）In step（1）In the nanometer cerium fluoride of gained, 1M NaOH aqueous solution 30ml are added, in polytetrafluoroethyl-ne alkene reaction Heated sealed is to 180 DEG C in kettle, reacts 24 ~ 48h, and the centrifugation of reacted mixed liquor is obtained into sediment, with pure water 2 times, 60 DEG C of dry 24h, and 600 DEG C of annealing 1h in Muffle furnace, obtain hexagon cerium dioxide nano sheet material.

Claims (1)

1. a kind of preparation method of hexagon cerium dioxide nano sheet material, it is characterised in that：Described preparation method include with Lower step：
(1) six water cerous nitrate 0.868g are dissolved in 30ml pure water, add 0.4 gram of polyvinyl alcohol and 1.32 grams of sodium fluoborates, magnetic Power is stirred and heated to 80 DEG C, is incubated 60min；After reaction product cooling, be centrifuged, pure water 2 times, obtain nanometer fluorine Change cerium；The mol ratio of six water cerous nitrates and sodium fluoborate is 1:6-8, polyvinyl alcohol water solution concentration 1-2% mass fractions；
(2) in the nanometer cerium fluoride obtained by step (1), 1M NaOH aqueous solution 30ml are added, in ptfe autoclave Heated sealed reacts 24~48h to 180 DEG C, the centrifugation of reacted mixed liquor is obtained into sediment, with pure water 2 times, 60 DEG C 24h, and 600 DEG C of annealing 1h in Muffle furnace are dried, hexagon cerium dioxide nano sheet material is obtained.
CN201610536097.7A 2016-07-10 2016-07-10 A kind of preparation method of hexagon cerium dioxide nano sheet material Expired - Fee Related CN106186036B (en)

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CN106186036B true CN106186036B (en) 2017-10-24

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106673045B (en) * 2016-12-19 2017-11-14 九江学院 A kind of preparation method of ultra-small grain size cerium dioxide nano sheet material
CN107473256B (en) * 2017-08-23 2019-04-05 电子科技大学 A kind of Ce1-xZrxO2Nanometer sheet material and preparation method thereof
CN109809482B (en) * 2019-04-08 2021-03-30 西安工业大学 Preparation method of monodisperse multi-morphology zirconia powder

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CN101172638A (en) * 2007-11-16 2008-05-07 浙江大学 Method for microwave synthesis of cerium fluoride nano disk
CN101282910A (en) * 2005-10-08 2008-10-08 首尔国立大学工业基金会 Process for producing cerium oxide nanocrystals
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CN1522228A (en) * 2002-04-15 2004-08-18 LG��ѧ��ʽ���� Preparation of single crystalline cerium oxide powder
CN1635169A (en) * 2003-12-30 2005-07-06 北京方正稀土科技研究所有限公司 Process for preparing cerous hydroxide
CN101282910A (en) * 2005-10-08 2008-10-08 首尔国立大学工业基金会 Process for producing cerium oxide nanocrystals
CN101172638A (en) * 2007-11-16 2008-05-07 浙江大学 Method for microwave synthesis of cerium fluoride nano disk
CN104310455A (en) * 2014-10-10 2015-01-28 九江学院 Preparation method of cerium oxide nanosheet

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CeF3: Tb的水热合成及发光性能研究;贾佩云等;《中国稀土学报》;20150430;第33卷(第2期);第253-256页 *
CeF3向CeO2的转变对掺杂Tb3+离子发光性能的影响;张丹等;《光谱实验室》;20120930;第29卷(第5期);第2647-2651页 *
Morphological Control and Luminescent Properties of CeF3 Nanocrystals;Ling Zhu et al.;《J. Phys. Chem. C》;20070403;第111卷;第5898-5903页 *
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