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Method for preparing topographic controlled bismuth oxide poxder

A technology of bismuth oxide and morphology, applied in the direction of oxide/hydroxide preparation, chemical instruments and methods, bismuth compounds, etc., to achieve the effects of broadening applications, improving electrical properties, and reducing synthesis temperature

Inactive Publication Date: 2006-09-13
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It can be seen that if bismuth oxide with anisotropic grain morphology is used as the template seed crystal, textured Bi-containing functional ceramics can be prepared by using grain oriented growth technology, and the preparation of bismuth oxide with anisotropic grain morphology not yet reported

Method used

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  • Method for preparing topographic controlled bismuth oxide poxder
  • Method for preparing topographic controlled bismuth oxide poxder
  • Method for preparing topographic controlled bismuth oxide poxder

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specific Embodiment approach

[0006] The object of the present invention can be achieved through the following technical solutions: Bismuth nitrate (Bi(NO 3 ) 3 ·5H 2 O) or bismuth hydroxide (Bi(OH) 3 ) as raw material, with alkali (such as ammonia, potassium hydroxide or sodium hydroxide, etc.) or glacial acetic acid (C 2 h 4 o 2 ) as a mineralizer. A certain amount of raw materials and mineralizer (or no mineralizer) are put into a reaction kettle lined with polytetrafluoroethylene, and then deionized water is added to make the reaction vessel have a certain degree of filling. The bismuth oxide precursor is hydrothermally reacted at a certain reaction temperature and holding time. After the reaction is completed, the solid-liquid separation is carried out, the reaction product is cleaned, and then dispersed with absolute ethanol, and then carried out at a temperature of 60-80°C. After drying treatment, anisotropic bismuth oxide powder can be obtained. The specific implementation is as follows:

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Embodiment 1

[0026] ① Raw material preparation: Bi(NO 3 ) 3 ·5H 2 O and deionized water were of analytical grade. Will 10.188gBi (NO 3 ) 3 ·5H 2 O was added to 35.0ml deionized water, stirring constantly to make Bi(NO 3 ) 3 ·5H 2 O uniform dispersion; ②Charging: put the mixed raw materials into a PTFE-lined, 42ml stainless steel reaction kettle, tighten and seal; ③Hydrothermal reaction: put the reaction kettle into a program-controlled oven, Hydrothermal reaction at 220°C for 10hrs, heating rate at 3°C / min., cooling with furnace; ④ product treatment: ultrasonic dispersion for 15min., washing with deionized water 10 times, drying at 60°C for 24hrs. The crystal grains of the obtained bismuth oxide were football-shaped.

Embodiment 2

[0028] ① Raw material preparation: Bi(OH) 3 、C 2 h 4 o 2 (glacial acetic acid) and deionized water were of analytical grade. 2.730gBi(OH) 3 and 0.158g C 2 h 4 o 2 Mix evenly, and add deionized water at the same time to make the volume 35.0ml; ②Charging: Put the uniformly mixed raw materials into a PTFE-lined, stainless steel reaction kettle with a volume of 42ml, and tighten the seal; ③Hydrothermal reaction : Put the reaction kettle into a program-controlled oven, conduct a hydrothermal reaction at 220°C for 10hrs, heat up at a rate of 3°C / min., and cool with the furnace; ④Product treatment: Ultrasonic dispersion for 30min., cleaning with deionized water for 10 times, and drying at 60°C Dry 24hrs.. Bismuth oxide nanofibers with a diameter of about 100nm were synthesized by hydrothermal method.

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Abstract

The invention uses bismuth hydroxide (Bi(OH)3) or bismuth nitrate (Bi(NO3)3.5H2O) as raw material, adds in or does not add in mineralizer, and by adjusting the hydrothermal technical parameters, using low-temperature hydrothermal method to synthesize the bismuth oxide powder whose crystal particle is a football, a 2D sheet, a 1D needle and so on, in shape. The raw material's concentration is 0.05-2.0M, and the mineralizer includes glacial acetic acid (C2H4O2) or alkali, where the concentrations of the acid (C2H4O2) and alkali are 0.025-0.075M, respectively, the reaction temperature is 160-220deg.C, the insulating time is 0.5-80hrs, and the filling percent is 70-85%. The sheet and needle bismuth oxides can act as template crystal, and use orientating technique to induce the oriented growth of crystal particle, thus able to make textured bismuthic functional ceramic.

Description

technical field [0001] The invention relates to a new method for preparing bismuth oxide powder with controllable morphology and belongs to the field of oxide powder preparation. Background technique [0002] Bismuth oxide has α-Bi 2 o 3 , β-Bi 2 o 3 , γ-Bi 2 o 3 and δ-Bi 2 o 3 The four crystal forms belong to monoclinic structure, tetragonal structure, body-centered cubic structure and face-centered cubic structure respectively. Because the crystal structure contains a large number of oxygen vacancies, the conductivity of oxygen ions is good, and it can be used to make electrolytes for solid oxide fuel cells , oxygen sensor and high-purity oxygen generator, etc. As Tomchenko et al. in WO 3 Add 3~5wt% Bi to the thick film 2 o 3 Can inhibit WO 3 The growth of grains promotes the formation of porous structure, thereby improving the sensitivity of the film to NO gas; and doping modified ZrO 2 system electrolyte material compared to Bi 2 o 3 The base electrolyte m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G29/00C01B13/14
Inventor 杨群保李永祥殷庆瑞王佩玲
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI