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Method for preparing micron and submicron-scale V1-XWXO2 powder

A V1-XWXO2, sub-micron-level technology, applied in the field of material preparation, can solve the problems of reduced variation range of optical and electrical characteristics, difficult to control the production process, expensive raw materials and equipment, etc., to achieve low price, easy process control, production The effect of simple operation of the equipment

Inactive Publication Date: 2013-12-04
XIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Traditional VO 2 The preparation method is in CO 2 atmosphere, heated with a platinum crucible V 2 o 5 To 1227 ℃, keep for three days, this method consumes a lot of energy, the efficiency is low, and the prepared VO 2 Coarse powder particles
Preparation of VO 2 Powder methods also include pyrolysis (NH 4 ) 2 V 6 o 16 and (NH 4 ) 6 [(VO) 6 (CO 3 ) 4 (OH) 9 ]·10H 2 O. Vacuum reduction method, spray decomposition of VOSO 4 etc., but these methods all have the disadvantages of expensive raw materials and equipment, difficult control of the production process, which leads to the mixed valence state of vanadium dioxide, so it is difficult to realize industrial production
On the other hand, as the doping amount increases, the substitution of vanadium dioxide ions by dopant ions also leads to changes in the lattice structure of vanadium dioxide, resulting in a decrease in the range of optical and electrical properties of vanadium dioxide before and after the phase transition.

Method used

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  • Method for preparing micron and submicron-scale V1-XWXO2 powder
  • Method for preparing micron and submicron-scale V1-XWXO2 powder
  • Method for preparing micron and submicron-scale V1-XWXO2 powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] V with a mass fraction of 93.99% 2 o 5 Powder, 3.29% of 5(NH 4 )·12WO 3 ·5H 2 O powder and C powder with a mass fraction of 2.78% are added to the ball mill tank, and a process control agent of 2% of the total mass of the mixed powder and hard alloy balls of 10 times the total mass are added, the ball mill tank is sealed, the circulating cooling system is opened, and mechanical ball milling is performed. 24 hours. Take out the mixed powder, place it in the heating tube of the atmosphere protection tube furnace, turn on the protection gas, heat to 600°C and keep it for 2.5 hours, then raise the temperature to 900°C and keep it for 5 hours, then cool down with the furnace. Take out the powder obtained by reduction, put the powder into a ball mill jar, and add a process control agent with a total mass of 2%, seal the ball mill jar, turn on the circulating cooling system and high-energy ball mill at a speed of 200r / min for 24 hours. After the high-energy ball milling, ...

Embodiment 2

[0030] V with a mass fraction of 88.66% 2 o 5 Powder, 7.87% of 5(NH 4 )·12WO 3 ·5H 2 O powder and C powder with a mass fraction of 3.47% are added to the ball mill tank, and a process control agent of 3% of the total mass of the mixed powder and cemented carbide balls 30 times the total mass are added, the ball mill tank is sealed, the circulating cooling system is opened, and mechanical ball milling is performed. 48 hours. Take out the mixed powder, put it into the heating tube of the atmosphere protection tube furnace, turn on the protection gas, heat to 600°C and keep it for 3 hours, then raise the temperature to 700°C and keep it for 3 hours, then cool down with the furnace. Take out the powder obtained by reduction, put the powder into a ball mill jar, and add a process control agent with a total mass of 3%, seal the ball mill jar, turn on the circulating cooling system and perform high-energy ball milling at a speed of 400r / min for 48 hours. After the high-energy ba...

Embodiment 3

[0032] V with a mass fraction of 83.72% 2 o 5 Powder, 12.65% of 5(NH 4 )·12WO 3 ·5H 2 O powder and C powder with a mass fraction of 3.63% are added to the ball mill tank, and a process control agent of 2.5% of the total mass of the mixed powder and hard alloy balls with a total mass of 40 times are added, the ball mill tank is sealed, the circulating cooling water is turned on, and mechanical ball milling is performed. 64 hours. Take out the mixed powder, place it in the heating tube of the atmosphere protection tube furnace, turn on the protection gas, heat to 600°C and keep it for 2 hours, then raise the temperature to 900°C and keep it for 4 hours, then cool down with the furnace. Take out the powder obtained by reduction, put the powder into a ball mill jar, and add a process control agent with a total mass of 2.5%, seal the ball mill jar, turn on the circulating cooling system and perform high-energy ball milling at a speed of 600r / min for 64 hours. After the high-en...

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Abstract

The invention discloses a method for preparing micron and submicron-scale V1-XWXO2 powder, which comprises the steps of: taking V2O5 powder, 5(NH4). 12WO3. 5H2O power and C powder as raw materials; evenly stirring the mixed powder by mechanical ball milling; carrying out high-temperature solid solution sintering under the protection of N2 to obtain the V1-XWXO2 powder; and carrying out high energy ball milling on the V1-XWXO2 powder under the different ratios of grinding media to material within different periods of time to obtain the micron and submicron-scale V1-XWXO2 powder with different particle sizes. The prepared V1-XWXO2 powder has the advantages of being fine in grains, even in composition and fuller in doped element solid solution; and the method is simple in manufacturing technology, easy in control of process, low in price of raw materials, simple in operation of production equipment, less in investment, low in energy consumption and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of material preparation and relates to a V 1-x W x o 2 Powder material preparation method, especially relates to a kind of high-energy ball milling to prepare particle size of micron and submicron V 1-x W x o 2 powder method. technical background [0002] High-energy ball milling technology (that is, a kind of mechanical alloying method) is a process in which the powder particles are repeatedly extruded, deformed, broken, and welded through the action of mechanical force, that is, repeated collisions between ball materials, ball mill jars, and powder. This process helps powder refinement, and forms a large number of defects to promote interdiffusion between powder atoms, and undergoes solid-state reaction to form dispersed ultrafine particle alloy powder, so as to obtain materials with excellent performance. [0003] Traditional VO 2 The preparation method is in CO 2 atmosphere, heated with a platinu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F9/04C04B35/495C04B35/626
Inventor 邹军涛王献辉梁淑华
Owner XIAN UNIV OF TECH
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