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

A technology of alkaline earth metal salts and microwave radiation method, applied in nanotechnology, chemical instruments and methods, chemical/physical/physicochemical processes of energy application, etc., can solve the problem of restricting the vigorous development of alkaline earth metal vanadate materials and the growth of dominant directions Difficulty, fast material nucleation speed and other problems, to achieve the effect of adjustable product micro-morphology, fast and gentle reaction, and simple process

Inactive Publication Date: 2011-10-26
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 a calcium nitrate aqueous solution with a molar concentration of 0.0025mol / 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 the 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 SEM test of the product ( figure 2 ) shows that the main morphology is a mixed structure of nanoparticles and angular nanosheets; amo...

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

The invention relates to a synthesis method of an alkaline earth metal vanadate micro / nano material by utilizing microwave radiation. According to the method, with an alkaline earth metal salt and ammonium metavanadate as the raw materials and distilled water as a solvent, the alkaline earth metal vanadate micro / nano material is prepared in a microwave radiation heating mode in the presence of a structure directing agent. The synthesis method is characterized in that: the microwave heating efficiency is high, and the phase and morphology of the product are effectively controlled through the adjustment and control of the raw material properties or the structure directing agent, ultimately the high-efficiency functional nano material is acquired; and the synthesis method has the significant advantages of no temperature and concentration hysteresis, high operability, mild reaction conditions, simple process, and the like and the microstructure of the product is controllable. The invention also provides valuable experience for the application of the metal vanadate micro / nano material in the fields of energy storage and conversion, sewage treatment, photocatalysis, biomedicine, etc.

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 Applications(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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