CN102557105B - Monodisperse cerium oxide nanoparticle and preparation method thereof - Google Patents
Monodisperse cerium oxide nanoparticle and preparation method thereof Download PDFInfo
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- CN102557105B CN102557105B CN201110459956.4A CN201110459956A CN102557105B CN 102557105 B CN102557105 B CN 102557105B CN 201110459956 A CN201110459956 A CN 201110459956A CN 102557105 B CN102557105 B CN 102557105B
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- cerium oxide
- nitrate
- cerium
- solution
- ceric ammonium
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- 229910000420 cerium oxide Inorganic materials 0.000 title claims abstract description 32
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910002651 NO3 Inorganic materials 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- XMPZTFVPEKAKFH-UHFFFAOYSA-P ceric ammonium nitrate Chemical compound [NH4+].[NH4+].[Ce+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O XMPZTFVPEKAKFH-UHFFFAOYSA-P 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 13
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 6
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 235000010344 sodium nitrate Nutrition 0.000 claims description 5
- 239000004317 sodium nitrate Substances 0.000 claims description 5
- 229940001516 sodium nitrate Drugs 0.000 claims description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 4
- -1 polyoxyethylene Polymers 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 3
- 239000004323 potassium nitrate Substances 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 12
- 238000000034 method Methods 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 9
- 150000000703 Cerium Chemical class 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 7
- 239000011858 nanopowder Substances 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000002270 dispersing agent Substances 0.000 abstract 1
- 230000001089 mineralizing effect Effects 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 6
- 229910052684 Cerium Inorganic materials 0.000 description 5
- 238000013019 agitation Methods 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 5
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 230000002468 redox effect Effects 0.000 description 2
- 229910000667 (NH4)2Ce(NO3)6 Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- AUQXCHZNUWQQDB-UHFFFAOYSA-N [Ce].C(C)C(=O)C(=O)C Chemical compound [Ce].C(C)C(=O)C(=O)C AUQXCHZNUWQQDB-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011807 nanoball Substances 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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
Technical field
The invention belongs to rare earth oxide Material Field, 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 rare earth oxide series, has comparatively unique crystalline structure, the ability of higher oxygen storage capacity and release oxygen, stronger oxidation-reduction performance (Ce
3+/ Ce
4+), thereby receive people's very big concern, be widely used in Industrial Catalysis, the field such as precise polished.Nano-cerium oxide is adsorbed on the redox property that can greatly improve material on the activated solid support material of tool.In high precision polishing, the homogeneity of the granularity of powder, pattern and distribution of sizes thereof has material impact, and particle is thinner, distributes more even, and polishing effect is better.
Chinese invention patent CN101792171A joins solubility cerium salt in water and organic solvent mixing solutions, has prepared cerium oxide nanoballs by hydro-thermal reaction and in conjunction with calcining.Chinese invention patent CN101825551A, using cerous salt as raw material, by twice hydro-thermal reaction, prepares the cerium oxide microballoon of 90~450nm.Chinese invention patent CN1699282A, take cerium salt and urea as raw material, adopts sluggish precipitation to synthesize the cerium oxide of submicron order.Chinese invention patent CN101306830A is take methyl ethyl diketone cerium as cerium source, adopt recirculation water solution, the Water soluble spherical cerium oxide nanocrystal that to have prepared median size between 225~240 ℃ be 5~10nm.Chinese invention patent CN101541912A adopts the precursor solution of cerium mix with precipitant solution and react, and solution is carried out to oxide treatment simultaneously, and the ceria oxide powder particle diameter of preparation can regulate between the μ m of 50nm~3.
Foregoing invention preparation process more complicated, or need twice hydro-thermal reaction, or need follow-up calcination processing, maybe need to use precipitation agent and organic solvent, and prepared particle size were wider distribution, also has difficulties to effective control of morphology microstructure and size distribution.The present invention is intended to, by a kind of easy technique, adopt simple raw material, prepares the cerium oxide nano-powder of narrow size distribution.
Summary of the invention
The invention provides a kind of very easy hydro-thermal technique, adopt simple raw material can prepare easily the good dispersed nano cerium oxide nano-powder of crystallinity, distribution of sizes is narrower.Specific embodiment is: cerium salt, nitrate and dispersion agent are mixed according to a certain percentage and be dissolved in the water, stir and obtain settled solution; The solution preparing is put into reactor, in baking oven, carry out hydro-thermal reaction; It is dry that product is after completion of the reaction 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 is one or several in lithium nitrate, SODIUMNITRATE, saltpetre, and the mol ratio of cerium salt, nitrate is 1: 1.5~5.Dispersion agent is the one in polyoxyethylene glycol (PEG), polyvinylpyrrolidone (PVP), 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 need be under hydrothermal condition, introduce nitrate as mineralizer, play the effect of controlling speed of response, make stable nucleation, precipitation, the crystallization process of reaction experience, without follow-up high-temperature heat treatment, can prepare the good dispersed nano cerium oxide powder of crystallinity.Can realize cerium oxide particle diameter controlled between 160~300nm by concentration, the ratio of reaction raw materials, hydro-thermal time, the hydrothermal temperature of controlling cerium solution.
The method of the invention has following beneficial effect:
1) production technique is simple, flow process is short, easy to operate, and reproducible;
2) raw material is simple, take water as solvent, without with an organic solvent, has both saved cost, has reduced again environmental pollution;
3) a step hydro-thermal reaction can obtain the nano cerium oxide powder that crystallization degree is good, without additional high-temperature heat treatment, has reduced process costs;
4) good product dispersibility, narrow size distribution, can regulate and control particle diameter by temperature of reaction, reactant concn;
5) the prepared single cerium oxide nanoparticles of disperseing of the present invention can be for aspects such as ultravioletlight screening, automotive exhaust catalysis, mechanical polishinges.
Accompanying drawing explanation
Fig. 1 is the prepared single stereoscan photograph that disperses cerium oxide nanoparticles of embodiment 1, 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, consistent with the result of JCPDS (34-0394) card, is the CeO of pure phase
2, and there is good crystallinity.
Embodiment
Below in conjunction with specific embodiment, the present invention is described and illustrated in more detail, but those skilled in the art will recognize that these embodiment are only for illustrating the present invention, it does not form any restriction to scope of the present invention.
Embodiment 1
Take 2.74g ceric ammonium nitrate, 1.0g SODIUMNITRATE and 0.1g PEG 2000, be dissolved in 15ml water, fully mix by magnetic agitation, obtain settled solution.This solution is transferred in reactor, put into baking oven, 200 ℃ of hydro-thermal reactions 10 hours.After washing, washing with alcohol centrifugation, throw out is placed in to 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 240 ± 2nm.
Embodiment 2
Take 4.11g ceric ammonium nitrate, 1.5g SODIUMNITRATE and 0.01g PEO, be dissolved in 15ml water, fully mix by magnetic agitation, obtain clear solution.This solution is transferred in reactor, put into baking oven, 220 ℃ of hydro-thermal reactions 1 hour.After washing, washing with alcohol centrifugation, throw out is placed in to 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 270 ± 3nm.
Embodiment 3
Take 2.74g ceric ammonium nitrate, 2.0g lithium nitrate and 0.1g PVP, be dissolved in 15ml water, fully mix by magnetic agitation, obtain settled solution.This solution is transferred in reactor, put into baking oven, 120 ℃ of hydro-thermal reactions 100 hours.After washing, washing with alcohol centrifugation, throw out is placed in to 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 180 ± 3nm.
Embodiment 4
Take 5.48g ceric ammonium nitrate, 2.0g SODIUMNITRATE and 0.8g PVP, be dissolved in 15ml water, fully mix by magnetic agitation, obtain settled solution.This solution is transferred in reactor, put into baking oven, 150 ℃ of hydro-thermal reactions 60 hours.After washing, washing with alcohol centrifugation, throw out is placed in to 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 195 ± 3nm.
Embodiment 5
Take 2.74g ceric ammonium nitrate, 1.0g saltpetre and 0.18g PVP, be dissolved in 15ml water, fully mix by magnetic agitation, obtain settled solution.This solution is transferred in reactor, put into baking oven, 180 ℃ of hydro-thermal reactions 10 hours.After washing, washing with alcohol centrifugation, throw out is placed in to 80 ℃ of oven dry of baking oven, obtaining particle diameter is single cerium oxide that disperses of 220 ± 3nm.
Claims (4)
1. a single preparation method who disperses cerium oxide nanoparticles, comprise the following steps: ceric ammonium nitrate, nitrate and dispersion agent are mixed according to a certain percentage and be dissolved in the water, stir and obtain settled solution, wherein the concentration of ceric ammonium nitrate solution is less than 1mol/L, the mol ratio of ceric ammonium nitrate, nitrate is 1:1.5~5, and the mass ratio of ceric ammonium nitrate and dispersion agent is 27.4~411:1; The solution preparing is put into reactor, in baking oven, carry out hydro-thermal reaction; It is dry that product is after completion of the reaction 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, described nitrate is one or several in lithium nitrate, SODIUMNITRATE, saltpetre.
3. single preparation method who disperses cerium oxide nanoparticles according to claim 1, is characterized in that, described dispersion agent is the one in polyoxyethylene glycol, polyvinylpyrrolidone, polyoxyethylene.
4. 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.
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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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