CN106673045B - A kind of preparation method of ultra-small grain size cerium dioxide nano sheet material - Google Patents
A kind of preparation method of ultra-small grain size cerium dioxide nano sheet material Download PDFInfo
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- CN106673045B CN106673045B CN201611173680.2A CN201611173680A CN106673045B CN 106673045 B CN106673045 B CN 106673045B CN 201611173680 A CN201611173680 A CN 201611173680A CN 106673045 B CN106673045 B CN 106673045B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The invention discloses a kind of preparation method of ultra-small grain size cerium dioxide nano sheet material, sodium fluoborate is dissolved in water first, magnetic agitation, sequentially adds citric acid and cerous acetate hydrate, react 4 ~ 5d at room temperature, through centrifuging, washing, obtain nanometer cerium fluoride；Then gained nanometer cerium fluoride is mixed with sodium hydrate aqueous solution, magnetic agitation is heated to 80 ~ 90 DEG C of 20 ~ 24h of reaction, cooling, centrifugation, wash, dry, then desciccate is annealed 1h in 600 DEG C of Muffle furnaces, obtain ultra-small grain size cerium dioxide nano sheet material, its thickness about 1.4nm, the 10nm of diameter 7.The inventive method technique is simple, equipment need not be special procured, it is low to prepare cost, obtained cerium dioxide nano piece particle diameter is extra small, size is homogeneous, good dispersion, specific surface area are big, there is good application prospect in catalyst, polishing material and fuel-cell electrolyte etc..
Description
Technical field
The present invention relates to a kind of preparation method of ultra-small grain size cerium dioxide nano sheet material, nano material skill is particularly belonged to
Art field.
Background technology
Ceria is a kind of very important rare earth oxide, and ceria surface can be with vacuum or reducing atmosphere
Low price cerium and oxygen defect are produced, there is excellent redox catalysis performance and gas-sensing function, is particularly had and binding molecule
Exchange charge, exchange species function, auto-exhaust catalyst, polishing material, fuel-cell electrolyte, ultraviolet absorber,
The fields such as electronic ceramics are with a wide range of applications.Nanometer titanium dioxide cerium material in structure and aspect of performance ratio body shape material all
Improve a lot, there is some new physics and chemical property, therefore the study on the synthesis of nanometer titanium dioxide cerium material is turned into and worked as
One of study hotspot of modern nano material.
At present, preparing the method for cerium dioxide nano material has the precipitation method, sol-gal process, hydro-thermal method, solvent-thermal method, combustion
Burning method, oil phase thermal decomposition method etc..Using these methods, people have been obtained for the nano ceric oxide of different morphologies.But by
It is face-centred cubic structure in ceria, crystallization trend is difficult to control in preparation process, obtains single dispersing, flake nano dioxy
The difficulty for changing cerium is very big.In recent years, the preparation method of cerium dioxide nano piece is more and more, has achieved many progress.Example
If patent of invention CN201310194946.1 is using cerous nitrate or cerium chloride as raw material, excessive ammonias, reaction are added dropwise at -10 ~ 20 DEG C
Reaction obtains platy cerium oxide, thickness 10-30nm in kettle；Patent of invention CN201410193490.1 is with CeCl3×7H2O and urea
For raw material, ethylenediamine is template, and hydro-thermal method obtains hexagonal nanosheet shape cerium oxide；Wang Dianyuan etc.（Angew. Chem.
Int. Ed.2005,44:3256-3260）Using oleic acid, oleyl amine and 1- octadecylenes as solvent, hydration is thermally decomposed at 300-360 DEG C
Cerous acetate, sodium pyrophosphate or enuatrol are mineralizer, are prepared for monodispersed square and strip cerium dioxide nano piece.From
Apparently, or cerium dioxide nano piece prepared by flake nano ceria is thicker, specific surface area is inadequate for current research present situation
Greatly, or preparation technology employs the oil-based solvent of costliness, therefore a kind of inexpensive, simple to operate no template new method is developed
Ultra-thin cerium dioxide nano sheet material tool is produced to be of great significance.
The content of the invention
It is an object of the invention to provide a kind of preparation method of ultra-small grain size cerium dioxide nano sheet material, especially by
Following technical scheme is realized.
The present invention discloses a kind of preparation method of ultra-small grain size cerium dioxide nano sheet material, comprises the following steps：
（1）0.30g sodium fluoborates are dissolved in 40mL deionized waters, magnetic agitation, add Citric Acid Mono at room temperature, are treated
After citric acid is completely dissolved, add cerous acetate hydrate, at room temperature magnetic agitation react 4 ~ 5d, reaction product respectively through go from
Sub- water and absolute ethyl alcohol respectively after washing, are centrifuged, obtain a nanometer cerium fluoride filter cake；Cerous acetate hydrate and sodium fluoborate
Mol ratio be 1:2 ~ 6, the mol ratio of cerous acetate and citric acid is 1:2~10；
（2）By step（1）The nanometer cerium fluoride filter cake of gained is added in 30mL deionized waters, magnetic agitation, is then added
1M NaOH aqueous solution 10mL, it is heated to 80 ~ 90 DEG C of 20 ~ 24h of reaction；Reaction product is cooled to after room temperature through centrifuging, gained
Filter cake uses deionized water and absolute ethyl alcohol carrying out washing treatment respectively, then 24h is dried at a temperature of 70 DEG C, and desciccate is in Muffle thereafter
600 DEG C of annealing 1h, obtain ultra-small grain size cerium dioxide nano sheet material in stove.
Beneficial effects of the present invention：
It is using sodium fluoborate, citric acid and cerous acetate as raw material in the preparation method of the present invention, room temperature liquid-phase precipitation method obtains
To nanometer cerium fluoride, cerium fluoride is then transformed into cerium hydroxide with NaOH alkali lye, ultra-small grain size ceria is obtained after annealing
Nanometer sheet material, the thickness 1.4nm of nanometer sheet, diameter 7-10nm.The inventive method technique is simple, without special procuring equipment, prepares
Cost is low, and obtained cerium dioxide nano piece particle diameter is extra small, size is homogeneous, good dispersion, specific surface area are big, in catalyst, throws
Luminescent material and fuel-cell electrolyte etc. have good application prospect.
Brief description of the drawings
Fig. 1 is the TEM photos of cerium dioxide nano sheet material made from the embodiment of the present invention 1；
Fig. 2 is the TEM photos of cerium dioxide nano sheet material made from the embodiment of the present invention 2.
Embodiment
Embodiment 1
（1）0.30g sodium fluoborates are dissolved in 40mL deionized waters, magnetic agitation, add 0.42g citric acids at room temperature,
After citric acid is completely dissolved, 0.20g cerous acetate hydrates are added, at room temperature magnetic agitation reaction 4d, reaction product is through going
Ionized water and absolute ethyl alcohol are respectively washed, centrifuged, and obtain a nanometer cerium fluoride filter cake；
（2）By step（1）The nanometer cerium fluoride filter cake of gained is added in 30mL deionized waters, magnetic agitation, is then added
1M NaOH aqueous solution 10mL, 90 DEG C of reaction 24h are heated to, after cooling, mixed liquor is centrifuged to obtain sediment, uses deionized water
With absolute ethyl alcohol washing, 70 DEG C of drys 24h, by desciccate in Muffle furnace 600 DEG C anneal 1h, obtain ultra-small grain size titanium dioxide
Cerium nanometer sheet material.
Embodiment 2
（1）0.30g sodium fluoborates are dissolved in 40mL deionized waters, magnetic agitation, add 0.84g citric acids at room temperature,
After citric acid is completely dissolved, 0.20g cerous acetate hydrates are added, at room temperature magnetic agitation reaction 5d, reaction product is through going
Ionized water and absolute ethyl alcohol are respectively washed, centrifuged, and obtain a nanometer cerium fluoride filter cake；
（2）By step（1）The nanometer cerium fluoride filter cake of gained is added in 30mL deionized waters, magnetic agitation, is then added
1M NaOH aqueous solution 10mL, 90 DEG C of reaction 24h are heated to, after cooling, mixed liquor is centrifuged to obtain sediment, uses deionized water
With absolute ethyl alcohol washing, 70 DEG C of drys 24h, by desciccate in Muffle furnace 600 DEG C anneal 1h, obtain ultra-small grain size titanium dioxide
Cerium nanometer sheet material.
Claims (1)
- A kind of 1. preparation method of ultra-small grain size cerium dioxide nano sheet material, it is characterised in that：Described preparation method includes Following steps：（1）0.30g sodium fluoborates are dissolved in 40mL deionized waters, magnetic agitation, add Citric Acid Mono at room temperature, treat lemon After acid is completely dissolved, cerous acetate hydrate is added, magnetic agitation reacts 4 ~ 5d at room temperature, and reaction product is respectively through deionized water After respectively being washed with absolute ethyl alcohol, it is centrifuged, obtains a nanometer cerium fluoride filter cake；Cerous acetate hydrate and sodium fluoborate rub You are than being 1:2 ~ 6, the mol ratio of cerous acetate and citric acid is 1:2~10；（2）By step（1）The nanometer cerium fluoride filter cake of gained is added in 30mL deionized waters, magnetic agitation, then adds 1M NaOH aqueous solution 10mL, it is heated to 80 ~ 90 DEG C of 20 ~ 24h of reaction；Reaction product is cooled to after room temperature through centrifuging, gained filter Cake uses deionized water and absolute ethyl alcohol carrying out washing treatment respectively, then 24h is dried at a temperature of 70 DEG C, and desciccate is in Muffle furnace thereafter In 600 DEG C annealing 1h, obtain ultra-small grain size cerium dioxide nano sheet material.
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