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A method for preparing nanometer ba(fe0.5nb0.5)o3 powder by microwave hydrothermal method

A microwave hydrothermal method and nano-technology, which is applied in the field of wet chemical method to prepare nano-powder, can solve the problems of large particle size, limited ceramic performance, powder agglomeration, etc., and achieves improved dielectric properties and shortened reaction time , good shape effect

Active Publication Date: 2018-06-19
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently preparing Ba(Fe 0.5 Nb 0.5 )O 3 There are two main methods of powder, one is the traditional solid phase method, this method is simple and easy, but there are defects such as large particle size of the prepared powder, long ball milling cycle, high calcination temperature and low sinterability. Improved performance of ceramics
The other is the co-precipitation method, although the nanometer Ba(Fe 0.5 Nb 0.5 )O 3 powder, but the synthesized powder requires a higher calcination temperature, and the powder agglomeration phenomenon is serious

Method used

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  • A method for preparing nanometer ba(fe0.5nb0.5)o3 powder by microwave hydrothermal method
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Embodiment 1

[0031] A kind of microwave hydrothermal method of the present invention prepares nanometer Ba(Fe 0.5 Nb 0.5 )O 3 The method of powder, comprises the steps,

[0032] (1) Prepare a dilute hydrochloric acid solution with a concentration of 1 mol / L and a NaOH solution with a concentration of 5 mol / L in advance for future use. According to Ba(Fe 0.5 Nb 0.5 )O 3 The stoichiometric ratio of 2:1:1 accurately weighs Ba(NO 3 ) 2 , Fe(NO 3 ) 3 9H 2 O, NbCl 5 .

[0033] (2) Quickly weigh NbCl 5 , dissolve it in the dilute hydrochloric acid prepared in advance, seal it with plastic wrap, and place it in a magnetic stirrer to stir for 10h to make the NbCl 5 Dissolve completely in hydrochloric acid solution to give NbCl 5 hydrochloric acid solution, Nb 5+ The ion concentration is 0.06mol / L.

[0034] (3) Ba(NO 3 ) 2 Added in deionized water, stirred until completely dissolved to obtain Ba(NO 3 ) 2 Aqueous solution, Ba(NO3 ) 2 The concentration of the aqueous solution is 0...

Embodiment 2

[0040] A kind of microwave hydrothermal method of the present invention prepares nanometer Ba(Fe 0.5 Nb 0.5 )O 3 The method of powder, comprises the steps,

[0041] (1) Prepare a dilute hydrochloric acid solution with a concentration of 2 mol / L and a NaOH solution with a concentration of 8 mol / L in advance for future use. According to Ba(Fe 0.5 Nb 0.5 )O 3 The stoichiometric ratio of 2:1:1 accurately weighs Ba(NO 3 ) 2 , Fe(NO 3 ) 3 9H 2 O, NbCl 5 .

[0042] (2) Quickly weigh NbCl 5 , dissolve it in the dilute hydrochloric acid prepared in advance, seal it with plastic wrap, and place it in a magnetic stirrer to stir for 12 hours to make NbCl 5 Dissolve completely in hydrochloric acid solution to give NbCl 5 hydrochloric acid solution, Nb 5+ The ion concentration is 0.07mol / L.

[0043] (3) Ba(NO 3 ) 2 Add deionized water, stir until completely dissolved, and get Ba(NO 3 ) 2 Aqueous solution, Ba(NO 3 ) 2 The concentration of the aqueous solution is 0.07mol...

Embodiment 3

[0049] A kind of microwave hydrothermal method of the present invention prepares nanometer Ba(Fe 0.5 Nb 0.5 )O 3 The method of powder, comprises the steps,

[0050] (1) Prepare a dilute hydrochloric acid solution with a concentration of 3 mol / L and a NaOH solution with a concentration of 10 mol / L in advance for future use. According to Ba(Fe 0.5 Nb 0.5 )O 3 The stoichiometric ratio of 2:1:1 accurately weighs Ba(NO 3 ) 2 , Fe(NO 3 ) 3 9H 2 O, NbCl 5 .

[0051] (2) Quickly weigh NbCl 5 , dissolve it in the dilute hydrochloric acid prepared in advance, seal it with plastic wrap, and place it in a magnetic stirrer to stir for 15 hours to make the NbCl 5 Dissolve completely in hydrochloric acid solution to give NbCl 5 hydrochloric acid solution, Nb 5+ The ion concentration is 0.08mol / L.

[0052] (3) Ba(NO 3 ) 2 Add deionized water, stir until completely dissolved, and get Ba(NO 3 ) 2 Aqueous solution, Ba(NO 3 ) 2 The concentration of the aqueous solution is 0....

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Abstract

The invention relates to a method for preparing nanometer Ba(Fe0.5Nb0.5)O3 powder through a microwave hydrothermal method. The molar ratio of Ba(NO3)2 to Fe(NO3)3.9H2O to NbC15 is 2:1:1, according to the molar ratio, Fe(NO3)3.9H2O is added into a Ba(NO3)2 water solution, and then NbC15 hydrochloric acid solution is added and mixed uniformly; then the pH of the mixed solution is adjusted to be larger than 12, a coprecipitation precursor is formed, the coprecipitation precursor is transferred into a microwave hydrothermal reaction kettle and subjected to a reaction for 1-1.5 h at the temperature of 200-220 DEG C to obtain a material, and the obtained material is washed, dried and screened to obtain the nanometer Ba(Fe0.5Nb0.5)O3 powder. The method combines advantages of the microwave hydrothermal method and a traditional hydrothermal method, is fast and efficient, saves energy, and reduces the opportunity of impurity element doping; reaction time is short, the reaction temperature is low, the powder does not need to be subjected to the later-period high-temperature calcinations working procedure, and the prepared powder is high in purity, uniform in size distribution and good in dispersity.

Description

【Technical field】 [0001] The invention belongs to the field of preparing nano powder by wet chemical method, in particular to a microwave hydrothermal method for preparing nano Ba(Fe 0.5 Nb 0.5 )O 3 powder method. 【Background technique】 [0002] In recent years, high dielectric constant materials have played an increasingly important role in the field of microelectronics. where Ba(Fe 0.5 Nb 0.5 )O 3 (BFN) material is one of the typical Fe-based composite perovskite structure materials, which has attracted extensive attention due to its high dielectric constant and good temperature and frequency stability. [0003] It is well known that the macroscopic properties of materials are closely related to their microstructures (such as particle size, morphology, internal defects, etc.). Ceramic dielectric materials with fine grain size tend to exhibit superior dielectric properties, which requires the selected powder grain size to be as small as possible, so the preparation ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/495C04B35/626
CPCC04B35/495C04B35/626C04B2235/3215C04B2235/3272
Inventor 王卓王春房明瑞王添肖雨佳王永乐
Owner SHAANXI UNIV OF SCI & TECH
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