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A multi-layer core-shell structure CEO 2 Template-free synthesis of hollow nanospheres

A technology of multi-layer core-shell structure and synthesis method, which is applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve problems such as the number of layers of the core-shell structure, thickness control, low synthesis efficiency, and high cost of ligands. Achieve the effect of simple and efficient synthesis method, uniform distribution, and not easy to agglomerate

Active Publication Date: 2017-03-01
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Materials of this structure, the hard template method and the soft template method used in the traditional synthesis of the multi-shell structure have the characteristics of cumbersome steps and low synthesis efficiency. Some progress has been made in this area in the past two years, but the template-free method Synthesizing core-shell structures remains a challenge
Literature [Nanoscale,2012,4(21):6835-6840] using cerium nitrate as metal ion, 1,3-adamantanedicarboxylic acid and 2-aminoterephthalic acid as ligands, using simple solvothermal synthesis smooth coordination polymer solid microspheres, followed by a simple one-step calcination to prepare CeO with a core-shell structure 2 ; However, it cannot control the number of layers, thickness, etc. of the core-shell structure, and the cost of the ligand used is relatively high

Method used

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  • A multi-layer core-shell structure CEO  <sub>2</sub> Template-free synthesis of hollow nanospheres
  • A multi-layer core-shell structure CEO  <sub>2</sub> Template-free synthesis of hollow nanospheres
  • A multi-layer core-shell structure CEO  <sub>2</sub> Template-free synthesis of hollow nanospheres

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1: Synthesis of multilayer core-shell structure CeO 2 Nano Hollow Ball:

[0038] A multilayer core-shell structure CeO 2 A highly efficient template-free synthesis method for hollow nanospheres, comprising the following steps:

[0039] (1) 0.4mol Ce(NO 3 ) 3 ·6H 2 O and 1.2mol of pyridine-2,5-dicarboxylic acid were dissolved in a mixed solvent of 16ml of absolute ethanol and 16ml of dimethylamide to prepare Ce(NO 3 ) 3 solution;

[0040] (2) Put the above mixed solution in a reaction kettle, react at 160°C for 12h, centrifuge after the reaction (centrifugal speed is 1000 rpm, time is 5min), wash, and dry at 80°C to obtain a coordination polymer of cerium Nano solid ball;

[0041] (3) Place the above-mentioned cerium coordination polymer nanosolid spheres in a muffle furnace, calcinate at 600°C for 4h, and cool to room temperature to obtain a multilayer core-shell structure CeO 2 nano hollow spheres.

[0042] The resulting multilayer core-shell CeO ...

Embodiment 2

[0043] Embodiment 2: Synthesis of multilayer core-shell structure CeO 2 Nano Hollow Ball:

[0044] A multilayer core-shell structure CeO 2 A highly efficient template-free synthesis method for hollow nanospheres, comprising the following steps:

[0045] (1) 0.4mol Ce(NO 3 ) 3 ·6H 2 O and 1.2mol of pyridine-2,5-dicarboxylic acid were dissolved in a mixed solvent of 16ml of absolute ethanol and 16ml of dimethylamide to prepare Ce(NO 3 ) 3 solution;

[0046] (2) Put the above mixed solution in a reaction kettle, react at 160°C for 6h, centrifuge after the reaction (centrifugation speed is 1000 rpm, time is 5min), and dry at 80°C to obtain the coordination polymer of cerium Nano solid ball;

[0047] (3) Place the above-mentioned cerium coordination polymer nanosolid spheres in a muffle furnace, calcinate at 800°C for 4 hours, and cool to room temperature to obtain multilayer core-shell structure CeO 2 nano hollow spheres.

[0048] The resulting multilayer core-shell CeO ...

Embodiment 3

[0049] Example 3: Detection of the multilayer core-shell structure CeO prepared in Examples 1-2 2 Purity of hollow nanospheres:

[0050] Using Rigaku / Max-3A X-ray diffractometer to measure the multilayer core-shell structure CeO prepared in Examples 1-2 2 Nano hollow spheres (CuKα radiation, ), the result is as figure 1 As shown, all the peaks of the hollow nanospheres correspond to the cubic phase of CeO 2 The standard card (JCPDS 34-0394) is completely consistent, indicating that the calcined coordination polymer is completely converted to CeO 2 .

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Abstract

The invention discloses a template-free synthesis method of CeO2 nano hollow spheres with a multilayer core-shell structure. First, cerium nitrate and pyridine-2,5-dicarboxylic acid are dissolved in a mixed solvent of absolute ethanol and DMF; then the mixed solution is Place in a reaction kettle, react at 100-160°C for 6-12 hours, centrifuge and wash after reaction, and dry at 80°C to obtain cerium coordination polymer nano-solid spheres; finally, place the obtained dried sample in a muffle furnace , Calcined at 400-800°C for 1-4h, and cooled to room temperature to obtain CeO2 hollow spheres with multilayer core-shell structure. The synthesis step of the method of the present invention is simple, and can accurately control the core-shell number and thickness of the product; the CeO2 hollow nanospheres with multilayer core-shell structure have an average particle diameter of 400nm and are uniformly distributed, and most of them are composed of three hollow The spherical shell and a hollow spherical core are composed, and the obtained material has a stable structure; this method provides a new way for the synthesis of ceria with a complex core-shell structure.

Description

technical field [0001] The invention relates to a multilayer core-shell structure CeO 2 Template-free synthesis of hollow nanospheres. Background technique [0002] Due to their unique physical and chemical properties, rare earth coordination polymers have shown good potential application value in the fields of light, electricity, magnetism, catalysis, and gas storage, so they have attracted much attention from researchers. At present, research centers in this field are mainly focused on synthesizing coordination polymers with unique structures by simple and novel methods. Its special coordination mode and crystal structure are very likely to make materials have special properties and expand the application space of materials. In the research of various rare earth materials, the preparation and application of rare earth oxides have always been the key research objects. It is also one of the focuses of current research to control the properties and applications of rare eart...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B82Y30/00
Inventor 钟声亮赵永霞王雷李苑马丹阳
Owner JIANGXI NORMAL UNIV
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