CN105480999A - Preparation method of multilevel-structure nano cerium oxide octahedron - Google Patents
Preparation method of multilevel-structure nano cerium oxide octahedron Download PDFInfo
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- CN105480999A CN105480999A CN201510966082.XA CN201510966082A CN105480999A CN 105480999 A CN105480999 A CN 105480999A CN 201510966082 A CN201510966082 A CN 201510966082A CN 105480999 A CN105480999 A CN 105480999A
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- Prior art keywords
- cerium oxide
- multilevel
- polyvinylpyrrolidone
- nano
- multilevel hierarchy
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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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/01—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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/41—Particle morphology extending in three dimensions octahedron-like
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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
Abstract
A preparation method of a multilevel-structure nano cerium oxide octahedron comprises the following specific steps: dissolving a certain amount of Ce(NO3)36H2O and a certain amount of polyvinylpyrrolidone into water, thus form a uniform mixed solution, wherein the molar concentration of Ce<3+> is 0.05-0.5mol/L, and the mass ratio of the Ce(NO3)36H2O to the polyvinylpyrrolidone is 1:(0.25 to 1); under a stirring condition, adjusting the pH value of the solution to 4.5-6.5 by using alkali; transferring the solution into a reaction still, performing a hydrothermal reaction under a temperature of 160-220 DEG C for 6-24h, after the reaction is ended, performing centrifugal separation, washing and drying to obtain the multilevel-structure nano cerium oxide octahedron. The multilevel-structure nano cerium oxide octahedron can be further used for preparing materials with special appearances and particle sizes, including a catalytic material, an optical material and the like.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, relate to the octahedral preparation method of a kind of multilevel hierarchy nano-cerium oxide.
Background technology
CeO
2it is a kind of important rare earth oxide functional materials, belong to typical cubic fluorite structure, stability is strong, there is good physical strength, excellent oxygen ion transport performance, in numerous areas extensive application such as luminescent material, fuel cell, middle temperature oxidation of solid fuels thing battery, polishing material, catalytic materials.CeO under nanoscale
2relative to body phase material, electronic structure changes, and specific surface area increases, and often shows some new physical propertiess (as lattice diffusion, the transition of lattice boundary stone, ultraviolet absorption peak blue shift) and higher chemically reactive.In recent years, develop and multiplely prepare nano Ce O
2method, comprise the precipitator method, sol-gel method, microemulsion method, water (solvent) hot method, microwave method.A series of different-shape, mono-dispersed nano CeO
2be successfully synthesized, such as nano cubic, octahedron, nanometer rod, nano wire, nanotube, nanometer sheet etc.But from the demand for development in future, the CeO of particle and morphology controllable
2nano material green synthesis method remains the focus of current research, because construct novel CeO
2nanostructure will effectively promote its using value.
The performance of nano material is except depending on the chemical constitution of material, crystallographic structure, also relevant to the size of nanocrystal, shape, surface tissue and the direction of growth, state of aggregation etc.Novel optical, electrical, magnetic property and high surface is often shown because complex structure, pattern are special by the multi-level nano-structure of basic nano unit self-assembly, multi-level nano-structure material not only can adopt as heir the characteristic of basic nano unit, also may have coupling effect, synergistic effect etc. that the combination of basic nano unit produces, therefore, the growth of multi-level nano-structure is one of popular domain of current research.
Comprise about multilevel hierarchy cerium oxide is octahedra reported: Chinese invention patent CN104445340A is raw material with cerous nitrate, cetyl trimethylammonium bromide is structure directing agent, water and ethanol are mixed solvent, and 150 DEG C of hydro-thermal reaction 22 ~ 24h have prepared by the octahedra cerium oxide of the micron order of nanometer blocks self-assembly; Han etc. are with six water cerous nitrates for raw material, and polyvinylpyrrolidone (PVP) is structure directing agent, and water and ethanol are mixed solvent, 200 DEG C of hydro-thermal reaction 12h obtain by the octahedra cerium oxide (Cryst.Eng.Comm. of nanometer sheet self-assembly, 2012,14,1939-1941).But above-mentioned preparation method with an organic solvent, and the multilevel hierarchy cerium oxide octahedron of synthesis is of a size of micron order and submicron order, and granular size is unadjustable.
Summary of the invention
The present invention is directed to prior art deficiency and provide the octahedral preparation method of a kind of multilevel hierarchy nano-cerium oxide.
Preparation method's step of the present invention is as follows:
1). by Ce (NO
3)
36H
2o and the water-soluble formation homogeneous mixture solotion of polyvinylpyrrolidone (PVP), wherein Ce
3+volumetric molar concentration is 0.05 ~ 0.5mol/L, Ce (NO
3)
36H
2o and polyvinylpyrrolidone (PVP) mass ratio are 1:0.25 ~ 1;
2). regulate above-mentioned mixing solutions pH value to 4.5 ~ 6.5 with alkali under agitation condition;
3). solution is transferred in reactor, at 160 ~ 220 DEG C of temperature, reacts 6 ~ 24h;
4). react complete and carry out centrifugation to solid product, washing is dry, obtains multilevel hierarchy nano-cerium oxide octahedra.
Wherein, step 1). described in polyvinylpyrrolidone (PVP) molecular-weight average be 10000 ~ 1300000, step 2). described in alkali be any one in sodium hydroxide, potassium hydroxide.
Beneficial effect of the present invention: compared with existing method, method provided by the present invention can complete in aqueous, and method is simple, and raw materials cost is low.And the size of assembly can be regulated and controled by the control of building-up reactions pH value of solution.Determine the synthesis condition of the octahedra cerium oxide of different size multilevel hierarchy.By octahedra for the multilevel hierarchy nano-cerium oxide of preparation at 300 ~ 600 DEG C of calcination 1 ~ 5h, as CO catalyst for oxidation reaction, air speed 36000mLg
-1h
-1, gas mixture forms: 1%CO, 21%O
2, 78%N
2, catalytic effect is good.
Accompanying drawing explanation
The octahedral SEM photo of multilevel hierarchy nano-cerium oxide that Fig. 1 embodiment 1 is synthesized;
The octahedral TEM photo of multilevel hierarchy nano-cerium oxide that Fig. 2 embodiment 1 is synthesized;
The octahedral X-ray diffraction spectrogram of multilevel hierarchy nano-cerium oxide that Fig. 3 embodiment 1 is synthesized;
The octahedral SEM photo of multilevel hierarchy nano-cerium oxide of the 2-in-1 one-tenth of Fig. 4 embodiment;
The octahedral SEM photo of multilevel hierarchy nano-cerium oxide that Fig. 5 embodiment 4 is synthesized;
The octahedral CO catalytic oxidation performance of multilevel hierarchy nano-cerium oxide that Fig. 6 embodiment 1 is synthesized.
Embodiment
Embodiment 1
Take 2.17gCe (NO
3)
3˙ 6H
2o and 1.11g polyvinylpyrrolidone (molecular-weight average 30000) is dissolved in 30ml water, dropwise adds 0.1mol/L sodium hydroxide solution to system pH=5.0 under stirring in above-mentioned solution, is then transferred in 50ml reactor by this solution, at 180 DEG C of reaction 24h.React complete, carry out centrifugation to solid product, washing is dry, obtains multilevel hierarchy nano-cerium oxide octahedra, and it is ~ 80nm that SEM characterizes display particle size.By product at 450 DEG C of calcination 4h, as CO catalyst for oxidation reaction, light-off temperature is 240 DEG C, and complete invert point is 400 DEG C.
Embodiment 2
Take 3.25gCe (NO
3)
3˙ 6H
2o and 2.95g polyvinylpyrrolidone (molecular-weight average 10000) is dissolved in 30ml water, dropwise adds 0.1mol/L potassium hydroxide solution to system pH=4.5 under stirring in above-mentioned solution, is then transferred in 50ml reactor by this solution, at 220 DEG C of reaction 12h.React complete, carry out centrifugation to solid product, washing is dry, obtains multilevel hierarchy nano-cerium oxide octahedra, and it is ~ 150nm that SEM characterizes display particle size.By product at 300 DEG C of calcination 5h, as CO catalyst for oxidation reaction, light-off temperature is 260 DEG C, and complete invert point is 440 DEG C.
Embodiment 3
Take 5.35gCe (NO
3)
3˙ 6H
2o and 2.67g polyvinylpyrrolidone (molecular-weight average 40000) is dissolved in 30ml water, dropwise adds 0.1mol/L sodium hydroxide solution to system pH=6.0 under stirring in above-mentioned solution, is then transferred in 50ml reactor by this solution, at 180 DEG C of reaction 12h.React complete, carry out centrifugation to solid product, washing is dry, obtains multilevel hierarchy nano-cerium oxide octahedra, and it is ~ 60nm that SEM characterizes display particle size.By product at 400 DEG C of calcination 3h, as CO catalyst for oxidation reaction, light-off temperature is 220 DEG C, and complete invert point is 380 DEG C.
Embodiment 4
Take 1.77gCe (NO
3)
3˙ 6H
2o and 0.71g polyvinylpyrrolidone (molecular-weight average 58000) is dissolved in 30ml water, in above-mentioned solution, 0.1mol/L sodium hydroxide solution is dropwise added to system pH=6.5 under stirring, then this solution is transferred in 50ml reactor, at 160 DEG C of reaction 10h.React complete, carry out centrifugation to solid product, washing is dry, obtains multilevel hierarchy nano-cerium oxide octahedra, and it is ~ 50nm that SEM characterizes display particle size.By product at 600 DEG C of calcination 4h, as CO catalyst for oxidation reaction, light-off temperature is 220 DEG C, and complete invert point is 400 DEG C.
Embodiment 5
Take 0.75gCe (NO
3)
3˙ 6H
2o and 0.56g polyvinylpyrrolidone (molecular-weight average 360000) is dissolved in 30ml water, in above-mentioned solution, 0.1mol/L potassium hydroxide solution is dropwise added to system pH=4.7 under stirring, then this solution is transferred in 50ml reactor, at 200 DEG C of reaction 8h.React complete, carry out centrifugation to solid product, washing is dry, obtains polycrystalline Nano cerium oxide octahedra, and it is ~ 120nm that SEM characterizes display particle size.By product at 400 DEG C of calcination 2h, as CO catalyst for oxidation reaction, light-off temperature is 240 DEG C, and complete invert point is 420 DEG C.
Claims (3)
1. the octahedral preparation method of multilevel hierarchy nano-cerium oxide, is characterized in that:
1) by Ce (NO
3)
36H
2o and polyvinylpyrrolidone and the water-soluble formation homogeneous mixture solotion of PVP, wherein Ce
3+volumetric molar concentration is 0.05 ~ 0.5mol/L, Ce (NO
3)
36H
2o and polyvinylpyrrolidone and PVP mass ratio are 1:0.25 ~ 1;
2) above-mentioned mixing solutions pH value to 4.5 ~ 6.5 are regulated with alkali under agitation condition;
3) solution is transferred in reactor, at 160 ~ 220 DEG C of temperature, reacts 6 ~ 24h;
4) react complete and carry out centrifugation to solid product, washing is dry, obtains multilevel hierarchy nano-cerium oxide octahedra.
2. the octahedral preparation method of a kind of multilevel hierarchy nano-cerium oxide according to claim 1, is characterized in that: the polyvinylpyrrolidone described in step 1) and PVP molecular-weight average are 10000 ~ 1300000.
3. the octahedral preparation method of a kind of multilevel hierarchy nano-cerium oxide according to claim 1, is characterized in that: step 2) described in alkali be any one in sodium hydroxide, potassium hydroxide.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
| CN107754779A (en) * | 2017-10-24 | 2018-03-06 | 山东师范大学 | Transient metal doped cerium-based composite oxides multiaspect body catalyst and preparation method |
| CN108226227A (en) * | 2017-12-31 | 2018-06-29 | 苏州南尔材料科技有限公司 | A kind of preparation method of nano-cellulose cerium oxide sensor material |
| CN115160935A (en) * | 2022-08-26 | 2022-10-11 | 江南大学 | Octahedral cerium oxide abrasive particle polishing solution and preparation method and application thereof |
| CN115368826A (en) * | 2022-08-26 | 2022-11-22 | 江南大学 | Polishing solution based on sphere-like cerium oxide abrasive particles and preparation method and application thereof |
Citations (2)
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| CN101825552A (en) * | 2009-07-23 | 2010-09-08 | 中国科学院过程工程研究所 | Method for preparing cerium dioxide microsphere used as dimension standard material |
| CN103708528A (en) * | 2014-01-03 | 2014-04-09 | 东华大学 | Preparation method of nano cerium dioxide with controllable size |
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2015
- 2015-12-22 CN CN201510966082.XA patent/CN105480999A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101825552A (en) * | 2009-07-23 | 2010-09-08 | 中国科学院过程工程研究所 | Method for preparing cerium dioxide microsphere used as dimension standard material |
| CN103708528A (en) * | 2014-01-03 | 2014-04-09 | 东华大学 | Preparation method of nano cerium dioxide with controllable size |
Non-Patent Citations (3)
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|---|
| FU ZHOU ET AL.: "Size-controlled synthesis and electrochemical characterization of spherical CeO2 crystallites", 《JOURNAL OF COLLOID AND INTERFACE SCIENCE》 * |
| MING LIN ET AL.: "Hydrothermal Synthesis of CeO2 Nanocrystals: Ostwald Ripening or Oriented Attachment", 《CRYSTAL GROWTH & DESIGN》 * |
| SUMALIN PHOKHA ET AL.: "Synthesis,characterization,and magnetic properties of monodisperse CeO2 nanospheres prepared by PVP-assisted hydrothermal method", 《NANOSCALE RESEARCH LETTERS》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107651703A (en) * | 2017-09-19 | 2018-02-02 | 天津大学 | The preparation method of particular crystal plane nano ceric oxide |
| CN107754779A (en) * | 2017-10-24 | 2018-03-06 | 山东师范大学 | Transient metal doped cerium-based composite oxides multiaspect body catalyst and preparation method |
| CN108226227A (en) * | 2017-12-31 | 2018-06-29 | 苏州南尔材料科技有限公司 | A kind of preparation method of nano-cellulose cerium oxide sensor material |
| CN115160935A (en) * | 2022-08-26 | 2022-10-11 | 江南大学 | Octahedral cerium oxide abrasive particle polishing solution and preparation method and application thereof |
| CN115368826A (en) * | 2022-08-26 | 2022-11-22 | 江南大学 | Polishing solution based on sphere-like cerium oxide abrasive particles and preparation method and application thereof |
| CN115160935B (en) * | 2022-08-26 | 2023-08-25 | 江南大学 | Octahedral cerium oxide abrasive particle polishing solution and preparation method and application thereof |
| CN115368826B (en) * | 2022-08-26 | 2023-08-25 | 江南大学 | Polishing solution based on spheroidal cerium oxide abrasive particles, and preparation method and application thereof |
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