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Synthesis method of alkaline earth metal vanadate micro/nano material by utilizing microwave radiation

A microwave radiation method and nanomaterial technology, which is applied in the field of preparation of inorganic functional materials, can solve the problems of difficult growth in the dominant direction, fast material nucleation, and restrict the vigorous development of alkaline earth metal vanadate materials, and achieve the microscopic appearance of products. Adjustable, fast and gentle response, high maneuverability effect

Inactive Publication Date: 2014-07-02
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But, alkaline earth metal vanadate powder material only has a small number of literature reports (Y.Takita, K.Kikitani, C.Xia, H.Takami and K.Nagaoka.Appl.Catal., A, 2005,283,209-216 ; Y.Takita, S.Hikazudani, K.Soda and K.Nagaoka.J.Mol.Catal.A:Chem., 2008,280,164-172.), while for the controllable preparation of alkaline earth metal vanadate nanomaterials There are even fewer literatures, mainly due to the problems of fast material nucleation and difficult growth in the dominant direction under the conventional traditional synthesis system, which undoubtedly limits the vigorous development of this type of alkaline earth metal vanadate materials.

Method used

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  • Synthesis method of alkaline earth metal vanadate micro/nano material by utilizing microwave radiation
  • Synthesis method of alkaline earth metal vanadate micro/nano material by utilizing microwave radiation
  • Synthesis method of alkaline earth metal vanadate micro/nano material by utilizing microwave radiation

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Embodiment 1

[0029] Embodiment 1: Preparation of calcium vanadate nanoparticles

[0030] At room temperature, prepare an aqueous solution of calcium nitrate with a molar concentration of 0.00125 mol / L; weigh the ammonium metavanadate solid so that the molar number is twice that of calcium nitrate, add distilled water at 60-75°C, and stir until metavanadic acid The ammonium was completely dissolved, and the obtained homogeneous solution was slowly added dropwise to the calcium nitrate aqueous solution, kept at a constant temperature of 60°C, and continued to stir vigorously for 15 minutes; the above-mentioned reaction raw material mixture was poured into a round-bottomed flask, and placed in a microwave radiation reactor for 30 minutes Minutes, the prepared material after the reaction is calcium vanadate micro / nano material. The product was detected by scanning electron microscopy (SEM) and showed that ( figure 1 ), its main shape is nanoparticles with good dispersion, its microstructure i...

Embodiment 2

[0031] Embodiment 2: Preparation of calcium vanadate nanoparticles and nanosheet hybrid structure

[0032] At room temperature, prepare an aqueous solution of calcium nitrate with a molar concentration of 0.0025 mol / L; weigh the ammonium metavanadate solid so that its molar number is twice that of calcium nitrate, add distilled water at 60-75°C, and stir until metavanadic acid The ammonium is completely dissolved, and the obtained homogeneous solution is slowly added dropwise to the calcium nitrate aqueous solution, kept at a constant temperature of 60°C, and continued to stir vigorously for 15 minutes; the above-mentioned reaction raw material mixture is poured into a round-bottomed flask, and placed in a microwave radiation reactor for 30 minutes. Minutes, the prepared material after the reaction is calcium vanadate micro / nano material. The SEM test of the product ( figure 2 ) shows that the main morphology is a mixed structure of nanoparticles and angular nanosheets; amon...

Embodiment 3

[0033] Embodiment 3: the preparation of calcium vanadate ultrathin nanosheet

[0034] At room temperature, prepare an aqueous solution of calcium nitrate with a molar concentration of 0.0050 mol / L; weigh the ammonium metavanadate solid so that its molar number is twice that of calcium nitrate, add distilled water at 60-75°C, and stir until metavanadic acid The ammonium is completely dissolved, and the obtained homogeneous solution is slowly added dropwise to the calcium nitrate aqueous solution, kept at a constant temperature of 60°C, and continued to stir vigorously for 15 minutes; the above-mentioned reaction raw material mixture is poured into a round-bottomed flask, and placed in a microwave radiation reactor for 30 minutes. Minutes, the prepared material after the reaction is calcium vanadate micro-nano material. Product SEM test ( image 3) shows that: the sample is an ultra-thin nanosheet structure, the surface of the sheet product is smooth, and there is no other coex...

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Abstract

A method for synthesizing alkaline earth metal vanadate micro / nano materials by microwave radiation method, which uses alkaline earth metal salt and ammonium metavanadate as raw materials, uses distilled water as solvent and introduces a structure-directing agent, and uses the heating method of microwave radiation method To prepare alkaline earth metal vanadate micro / nanomaterials. The present invention is characterized by high microwave heating efficiency, and can effectively control the phase and microscopic appearance of the product through the regulation of the physical properties of the raw materials or the structure-directing agent, and finally obtain high-efficiency functional nanomaterials; the significant advantage of this method is that there is no temperature and concentration Hysteresis, high operability, mild reaction conditions, simple process, controllable microscopic morphology, etc. The invention also provides valuable practical experience for the application of metal vanadate micro-nano materials in energy storage and conversion, sewage treatment, photocatalysis, biomedicine and even broader fields.

Description

technical field [0001] The invention belongs to the preparation technology of inorganic functional materials, in particular to a method for synthesizing alkaline earth metal vanadate micro / nano materials by microwave radiation. technical background [0002] The vanadium element in metal vanadate is easy to form multivalent compounds, which makes the spatial coordination configuration changeable, and can coordinate with different metal ions to form a unique crystal structure, and then exhibit various chemical properties, so it is widely used in Energy storage and conversion, sewage treatment, photocatalysis, biomedicine and other fields, and will have bright market prospects in other fields in the future. [0003] In order to further exploit the small size effect of materials and improve utilization efficiency, the controllable preparation of metal vanadate micro / nanomaterials has become one of the research hotspots. Alkaline earth metal micro / nano materials, as an important...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G31/00B01J19/12B82Y40/00
Inventor 孙嬿李春生张志佳王莉娜宋明阳马雪刚
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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