CN111099650A - CeO2Molten salt method for synthesizing nano spherical particles - Google Patents
CeO2Molten salt method for synthesizing nano spherical particles Download PDFInfo
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- CN111099650A CN111099650A CN202010070140.1A CN202010070140A CN111099650A CN 111099650 A CN111099650 A CN 111099650A CN 202010070140 A CN202010070140 A CN 202010070140A CN 111099650 A CN111099650 A CN 111099650A
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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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- 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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
The invention discloses CeO2A molten salt method for synthesizing nano-class spherical particles includes such steps as mixing trivalent cerium salt, KCl and LiCl, high-temp calcining, immersing in distilled water to remove salt, suction filtering, washing and drying2The nano particles are spherical, the particle size of the particles is 100-800 nm, the size is uniform, and the dispersibility is good; the method disclosed by the invention has the characteristics of low cost, simple process, environmental friendliness, short time consumption, low energy consumption and strong controllability, and the prepared product has good chemical stability and uniform appearance, thereby widening the range of CeO2The application of the nano-particles in the fields of electricity and catalysis has wide market application prospect.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to CeO2A fused salt method for synthesizing nano spherical particles.
Background
CeO2Belongs to a cubic system with a face-centered cubic structure, and has a space group of Fm3m and CeO2Has unique fluorite crystal structure characteristics. In CeO2In which each Ce atom is coordinated to 8 oxygen atoms, each oxygen atom is coordinated to 4 Ce atoms, the Ce atoms being located at the oxygen atomWithin the cubic hexahedron of subunits, this particular structure makes it possess oxygen ion transport properties. Ce3+/Ce4+The oxidation-reduction capability of mutual conversion between the Ce and the Ce, or the change of the valence state of the doped ion4+Equilibrium of valence states, resulting in CeO2Has strong oxygen storage capacity and oxygen release capacity. Thus, CeO2Has received great attention in photocatalysis. In addition, cerium ions have large radius and strong oxygen transmission capability compared with other metal ions, and can promote the rapid transmission of electrons, so that CeO2The material becomes a main energy storage material.
Nanomaterials generally refer to materials that have at least one dimension in the three-dimensional range that is on the order of nanometers and that have high-density interfacial phase components. The nano material shows quantum size effect, surface effect, small size effect, macroscopic quantum effect and other characteristics, so that the nano particles show many unusual physical and chemical properties and many basic characteristics different from the conventional size material. Adding CeO2The material nanocrystallization can improve CeO2The electrochemical activity of the catalyst is improved, the thoroughness of the reaction degree is improved, and the cycle stability of the material is improved.
To CeO2The nanoparticles are further performance-improved, mainly around improving electrolyte contact and ion diffusion, or improving the capacitance by improving electron transport in the active material. And CeO2The electrochemical activity of the nanoparticles can be influenced by their size and morphology, but the prior art CeO2The synthesis method of the nano-particles generally has the problems of high process cost, poor product performance, poor size controllability, non-uniform morphology, poor dispersibility and the like.
Therefore, CeO which is environment-friendly, good in size controllability, uniform in appearance, good in dispersity and easy to synthesize in large quantity is developed2Nanoparticles beneficial to increase of CeO2The electrochemical performance of the nano-particles enables the nano-particles to be widely applied in the field of lithium ion electrode materials.
Disclosure of Invention
The invention aims to solveOvercomes the defects in the prior art and provides CeO2The molten salt synthesis method of the nano spherical particles has simple preparation process and is easy for large-scale preparation, and simultaneously can solve the problems of poor size controllability, low morphology uniformity, poor dispersibility and the like of products prepared by the existing method.
The technical scheme of the invention is as follows: CeO (CeO)2The molten salt synthesis method of the nano spherical particles comprises the following steps:
(1) uniformly mixing cerium salt, KCl and LiCl;
(2) collecting the obtained mixture in an alumina crucible, putting the alumina crucible in a muffle furnace, heating, roasting and naturally cooling;
(3) soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a yellow solid;
(4) taking out the obtained yellow solid to a centrifuge tube, centrifugally washing the yellow solid for a plurality of times by deionized water, and drying the yellow solid in vacuum to obtain a product which is CeO2And (3) nanoparticles.
Further, in step 1, the amount ratio of the cerium salt, KCl and LiCl is 2: 50 x: 30x, wherein 0.2< x < 2.2.
Further, the trivalent cerium salt used in step 1 includes one or more of cerium nitrate, cerium acetate, cerium oxalate and cerium carbonate.
Further, the uniform mixing process in step 1 is accomplished by grinding using an agate mortar.
Further, in the step 2, the temperature is raised to 520-800 ℃ at the speed of 5 ℃/min for 1-8 h; if the reaction temperature is less than 520 ℃ or the reaction time is less than 1 hour, the solid mixture may not be completely reacted and may not be completely converted into cubic phase CeO2A nanoparticle; if the reaction temperature is higher than 800 deg.C, the solid mixture may be converted into CeO having large and non-uniform particles2Submicron particles.
Further, in the step 4, the temperature for vacuum drying is 60-80 ℃.
Cubic phase CeO prepared by the method2The diameter of the nano spherical particles is 100-800 nm, uniform size and good dispersibility.
The invention has the beneficial effects that:
the invention discloses CeO2A process for synthesizing the nano-class spherical particles by molten salt method includes such steps as proportionally mixing cerium salt, KCl and LiCl, high-temp calcining, immersing in distilled water to remove salt, suction filtering, washing and drying2A nanoparticle product; the synthesis method provided by the invention has the advantages of low use cost, simple process, environmental friendliness, short time consumption, low energy consumption and strong controllability, and the prepared CeO with good chemical stability, uniform appearance and good dispersibility2Nano material, widen CeO2The application of the nano-particles in the fields of electricity and catalysis has wide market application prospect.
Drawings
FIG. 1 shows CeO prepared in example 12An X-ray diffraction pattern of the nanoparticles;
FIG. 2 shows CeO prepared in example 12Scanning electron microscopy of the nanoparticles;
FIG. 3 shows CeO prepared in example 22Scanning electron microscopy of the nanoparticles;
FIG. 4 shows CeO prepared in example 32Scanning electron microscopy of nanoparticles.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit of the invention.
Example 1
Adding Ce (NO)3)3KCl and LiCl are mixed according to the mass ratio of 2: 50: 30, and are ground by using an agate mortar to obtain a solid mixture which is uniformly mixed; collecting the obtained mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating to 540 ℃ at the speed of 5 ℃/min, roasting for 4 h, and naturally cooling; soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a yellow solid; the resulting yellow solid was taken outAdding into a centrifuge tube, centrifugally washing with deionized water for several times, and vacuum drying at 60 deg.C to obtain yellow CeO2And (3) nanoparticles.
XRD test result shows that the product is pure phase CeO2The compound (FIG. 1), the scanning electron microscope examination result shows (FIG. 2), the synthesized CeO2The nano particle sample is uniform in appearance, good in dispersity and 60-100 nm in diameter.
Example 2
Adding Ce2(CO3)3KCl and LiCl are mixed according to the mass ratio of 2: 50: 30, and are ground by using an agate mortar to obtain a solid mixture which is uniformly mixed; collecting the obtained mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating to 660 ℃ at the speed of 5 ℃/min, roasting for 4 h, and naturally cooling; soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a yellow solid; taking out the obtained yellow solid to a centrifuge tube, centrifugally washing the yellow solid for a plurality of times by deionized water, and drying the yellow solid in vacuum at the temperature of 60 ℃ to obtain yellow CeO2And (3) nanoparticles.
FIG. 3 shows CeO prepared in this example2Scanning electron micrographs of the samples, it can be seen that the synthesized product CeO2Is spherical nano-particles with the diameter of 100-400 nm.
Example 3
Adding Ce2(CO3)3KCl and LiCl are mixed according to the mass ratio of 2: 50: 30, and are ground by using an agate mortar to obtain a solid mixture which is uniformly mixed; collecting the obtained mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating to 780 ℃ at the speed of 5 ℃/min, roasting for 3 h, and naturally cooling; soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a yellow solid; taking out the obtained yellow solid to a centrifuge tube, centrifugally washing the yellow solid for a plurality of times by deionized water, and drying the yellow solid in vacuum at the temperature of 60 ℃ to obtain yellow CeO2And (3) nanoparticles. FIG. 4 shows CeO prepared in this example2Scanning electron micrographs of the samples, it can be seen that the synthesized product CeO2Is spherical nano-particles with the diameter of 600-1000 nm.
Example 4
Adding Ce2(C2O4)3KCl and LiCl are mixed according to the mass ratio of 1: 15: 9, and are ground by using an agate mortar to obtain a solid mixture which is uniformly mixed; collecting the obtained mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating to 600 ℃ at the speed of 5 ℃/min, roasting for 3 h, and naturally cooling; soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a yellow solid; taking out the obtained yellow solid to a centrifuge tube, centrifugally washing the yellow solid for a plurality of times by deionized water, and drying the yellow solid in vacuum at the temperature of 60 ℃ to obtain yellow CeO2And (3) nanoparticles.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. However, the above description is only an example of the present invention, the technical features of the present invention are not limited thereto, and any other embodiments that can be obtained by those skilled in the art without departing from the technical solution of the present invention should be covered by the claims of the present invention.
Claims (7)
1. CeO (CeO)2The molten salt synthesis method of the nano spherical particles is characterized by comprising the following steps:
(1) uniformly mixing cerium salt, KCl and LiCl;
(2) collecting the obtained mixture in an alumina crucible, putting the alumina crucible into a muffle furnace, heating, roasting and naturally cooling;
(3) soaking the product after reaction in deionized water to remove salt, and performing suction filtration to obtain a yellow solid;
(4) taking out the obtained yellow solid to a centrifuge tube, centrifugally washing the yellow solid for a plurality of times by deionized water, and drying the yellow solid in vacuum to obtain a product CeO2And (3) nanoparticles.
2. The CeO of claim 12The molten salt synthesis method of the nano spherical particles is characterized in that in the step 1, the ratio of the cerium salt, KCl and LiCl is 2: 50: 30x, wherein 0.2<x<2.2。
3. The CeO of claim 12The molten salt method for synthesizing the nano spherical particles is characterized in that cerium salt used in the step 1 comprises one or more of cerium nitrate, cerium acetate, cerium oxalate and cerium carbonate.
4. The CeO of claim 12The molten salt synthesis method of the nano spherical particles is characterized in that the uniform mixing process in the step 1 is completed by grinding with an agate mortar.
5. The CeO of claim 12The molten salt synthesis method of the nano spherical particles is characterized in that in the step 2, the temperature is raised to 520-800 ℃ at the speed of 5 ℃/min, and then the roasting process is carried out, wherein the roasting time is 1-8 h.
6. The CeO of claim 12The molten salt synthesis method of the nano spherical particles is characterized in that in the step 4, the temperature for vacuum drying is 60-80 ℃.
7. The CeO of any one of claims 1 to 62Cubic phase CeO prepared by molten salt synthesis method of nano spherical particles2Spherical nanoparticles, characterized in that CeO2The diameter of the nano spherical particles is 100-800 nm, the size is uniform, and the dispersibility is good.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028105A (en) * | 2020-08-06 | 2020-12-04 | 常州市卓群纳米新材料有限公司 | Method for preparing nanometer praseodymium oxide by fused salt coprecipitation method |
| CN113044873A (en) * | 2021-04-16 | 2021-06-29 | 陕西科技大学 | CeO for chemical mechanical polishing2Nanoparticles and method for preparing same |
| CN113292929A (en) * | 2021-06-17 | 2021-08-24 | 陕西科技大学 | Nearly spherical La3+Doping with Ce1-xLaxO2Nano polishing powder and preparation method thereof |
| CN113860350A (en) * | 2021-11-03 | 2021-12-31 | 中国科学院上海应用物理研究所 | Method for preparing thorium dioxide nano material based on molten salt method and thorium dioxide nano material obtained by method |
| CN114735743A (en) * | 2022-05-19 | 2022-07-12 | 陕西科技大学 | CeO with polyhedral morphology2Granules and process for their preparation |
| CN115140756A (en) * | 2022-08-05 | 2022-10-04 | 湖南省产商品质量检验研究院 | Preparation method of sphere-like nano cerium oxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724380A (en) * | 2005-07-15 | 2006-01-25 | 清华大学 | Process for synthesizing nano cerium oxide crystal material |
-
2020
- 2020-01-21 CN CN202010070140.1A patent/CN111099650A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1724380A (en) * | 2005-07-15 | 2006-01-25 | 清华大学 | Process for synthesizing nano cerium oxide crystal material |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028105A (en) * | 2020-08-06 | 2020-12-04 | 常州市卓群纳米新材料有限公司 | Method for preparing nanometer praseodymium oxide by fused salt coprecipitation method |
| CN112028105B (en) * | 2020-08-06 | 2023-09-05 | 常州市卓群纳米新材料有限公司 | Method for preparing nano praseodymium oxide by fused salt coprecipitation method |
| CN113044873A (en) * | 2021-04-16 | 2021-06-29 | 陕西科技大学 | CeO for chemical mechanical polishing2Nanoparticles and method for preparing same |
| CN113292929A (en) * | 2021-06-17 | 2021-08-24 | 陕西科技大学 | Nearly spherical La3+Doping with Ce1-xLaxO2Nano polishing powder and preparation method thereof |
| CN113292929B (en) * | 2021-06-17 | 2022-08-05 | 陕西科技大学 | Nearly spherical La 3+ Doping with Ce 1-x La x O 2 Nano polishing powder and preparation method thereof |
| CN113860350A (en) * | 2021-11-03 | 2021-12-31 | 中国科学院上海应用物理研究所 | Method for preparing thorium dioxide nano material based on molten salt method and thorium dioxide nano material obtained by method |
| CN114735743A (en) * | 2022-05-19 | 2022-07-12 | 陕西科技大学 | CeO with polyhedral morphology2Granules and process for their preparation |
| CN115140756A (en) * | 2022-08-05 | 2022-10-04 | 湖南省产商品质量检验研究院 | Preparation method of sphere-like nano cerium oxide |
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