Method for preparing uniform carbon-coated vanadium phosphate sodium material

A carbon-coated sodium vanadium phosphate, carbon-coated technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of uneven carbon layer coating, large particle size distribution range, etc., and achieve inhibition of agglomeration phenomenon, coating uniformity, and the effect of improving conductivity

Active Publication Date: 2015-06-24
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Na 3 V 2 (PO 4 ) 3 The traditional preparation methods of materials, such as high-temperature solid-phase method, sol-gel method, etc., are relatively large in size and have a large particle size distribution range, and the coating of the carbon layer is not uniform.

Method used

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  • Method for preparing uniform carbon-coated vanadium phosphate sodium material
  • Method for preparing uniform carbon-coated vanadium phosphate sodium material
  • Method for preparing uniform carbon-coated vanadium phosphate sodium material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 4mmolV 2 o 5 , 12 mmol NH 4 h 2 PO 4 , 6 mmol Na 2 CO 3 Dissolve in 70ml of distilled water, then add 6mmol of glucose and stir evenly, transfer the above solution to the reaction kettle, heat it in water at 180°C for 12h, cool it at room temperature, open the kettle, ultrasonicate the obtained suspension for 90min, and then heat it at 70°C The water was evaporated with magnetic stirring in a water bath to obtain a sol, and the sol was dried in an oven at 60° C. for 12 hours to obtain a gel. The above gel was fully ground and pre-calcined in argon at 350 °C for 4 h; the pre-fired sample was fully ground again and calcined in argon at 650 °C for 8 h to obtain the product. The prepared Na 3 V 2 (PO 4 ) 3 The scanning electron microscope photograph of the material is as figure 1 As shown, it shows that the prepared products have uniform size.

Embodiment 2

[0026] 4mmolV 2 o 5 , 12 mmol NH 4 h 2 PO 4 , 6 mmol Na 2 CO 3 Dissolve in 70ml of distilled water, then add 3mmol of glucose and stir evenly, transfer the above solution to a reaction kettle, heat it in water at 180°C for 40h, cool it at room temperature and open the kettle, ultrasonicate the obtained suspension for 90min, and then heat it at 95°C The water was evaporated by magnetic stirring in a water bath to obtain a sol, and the sol was dried in an oven at 80° C. for 6 hours to obtain a gel. Grind the above gel thoroughly and pre-calcine in argon at 350°C for 4 hours; grind the pre-fired sample fully again, and calcinate in argon at 800°C for 6 hours to obtain the product. The prepared Na 3 V 2 (PO 4 ) 3 The X-ray diffraction pattern of the material is as figure 2 As shown, the prepared product has a pure composition.

Embodiment 3

[0028] 4mmolV 2 o 5 , 12 mmol NH 4 h 2 PO 4 , 6 mmol Na 2 CO 3 Dissolve in 70ml of distilled water, then add 4.5mmol of glucose and stir evenly, transfer the above solution to a reaction kettle, heat it in water at 180°C for 24h, cool it at room temperature and open the kettle, ultrasonicate the obtained suspension for 90min, and then in 80 The water was evaporated by magnetic stirring in a water bath at °C to obtain a sol, and the sol was dried in an oven at 70 °C for 9 hours to obtain a gel. The above gel was thoroughly ground and pre-calcined in argon at 350 °C for 4 h; the pre-fired sample was fully ground again, and calcined in argon at 750 °C for 7 h to obtain the product. The prepared Na 3 V 2 (PO 4 ) 3 The transmission electron microscope pictures of the material are as image 3 As shown, it shows that the surface of the prepared product is coated with a uniform carbon layer.

[0029] It can also be clearly seen from the accompanying drawings of the above ex...

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Abstract

The invention provides a method for preparing a uniform carbon-coated vanadium phosphate sodium material. The method comprises the following steps: dissolving V2O5, NH4H2PO4 and Na2CO3 or NH4VO3, H3PO4 and Na2CO3 in distilled water; uniformly mixing Na3V2(PO4)2 and glucose at a molar ratio of 2: (3-4); transferring the mixed solution into a hydrothermal reaction kettle, and carrying out the glycosidation reaction; cooling the hydrothermal reaction kettle at the room temperature, opening the hydrothermal reaction kettle, ultrasonic uniformly dispersing the obtained turbid liquid, magnetically stirring the turbid liquid in a water bath, and evaporating the water to obtain sol, and drying the sol in a drying oven to obtain gel; adequately grinding gel, and pre-burning the ground gel in argon; adequately grinding the pre-burned gel again, and calcining in argon to obtain the uniform carbon-coated Na3V2(PO4)3 material. The carbon-source glucose is added in the hydrothermal process, the surface of the particle is coated with a carbon layer, the conductivity of the material is improved, the clustering phenomenon of the particle in the sintering process can be inhibited, and a product with uniform size can be obtained.

Description

technical field [0001] The invention belongs to the field of synthesis of inorganic nanometer materials. More specifically, it relates to a method for preparing a sodium vanadium phosphate material with a uniform shape and size and a uniform carbon layer by a hydrothermal assisted sol-gel method Background technique [0002] Sodium vanadium phosphate (Na 3 V 2 (PO 4 ) 3 ) is an electrode material used in sodium-ion batteries and belongs to the NASICON structure (sodium superionic conductor). NASICON structure compound Na 3 m 2 (PO 4 ) 3 (M=Ti, Fe, V) is a kind of phosphate cathode material, which has a three-dimensional open ion transport channel, and generally has a high ion diffusion rate and ion conductivity. where Na 3 V 2 (PO 4 ) 3 With high energy density (400Wh / kg), good thermal stability (450℃) and excellent electrochemical performance, it has received extensive attention. Na 3 V 2 (PO 4 ) 3 has a hexagonal lattice, belongs to the R-3c space group, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58C01B25/45
CPCY02E60/10
Inventor 孙晓红杨以娜张思敏郑春明
Owner TIANJIN UNIV
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