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Method for preparing barium-cobalt-iron-niobium oxide material by low-heat solid-phase coordination method

A low-heat solid phase, niobium oxide technology, applied in the direction of calcium/strontium/barium oxide/hydroxide, niobium compounds, chemical instruments and methods, etc., can solve the temperature gap between the synthesis of pure cubic phase materials and the melting temperature of materials Small size, high energy consumption, long time, etc., to achieve the effects of burning, reducing synthesis temperature, and saving energy

Inactive Publication Date: 2009-10-28
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of adopting low-heat solid phase coordination method to prepare Ba 1.0 co 0.7 Fe 0.2 Nb 0.1 o 3-δ A materials approach to address the high-temperature solid-phase synthesis of Ba 1.0 co 0.7 Fe 0.2 Nb 0.1 o 3-δ The temperature in the material process is high, the time is long, the energy consumption is high, the temperature of the synthetic pure cubic phase material and the melting temperature of the material are relatively small, etc.

Method used

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  • Method for preparing barium-cobalt-iron-niobium oxide material by low-heat solid-phase coordination method
  • Method for preparing barium-cobalt-iron-niobium oxide material by low-heat solid-phase coordination method
  • Method for preparing barium-cobalt-iron-niobium oxide material by low-heat solid-phase coordination method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1) Mole ratio BaCO 3 : 2CoCO 3 3Co(OH) 2 ·H 2 O:Fe 2 (C 2 o 4 ) 3 ·5H 2 O: Nb 2 o 5 =1:0.14:0.1:0.05 ratio, weigh BaCO 3 9.867 g, 2CoCO 3 3Co(OH) 2 ·H 2 O 4.512 g, Fe 2 (C 2 o 4 ) 3 ·5H 2 O 2.452 g, Nb 2 o 5 0.665 g, high-speed mechanical stirring and mixing for 20 minutes;

[0021] 2) Take by weighing citric acid (C 6 h 8 o 7 ·5H 2 O) 21.014 grams of the powder mixed in the first step are put into a high-speed mechanical mixer together, stirred at high speed for 20 minutes, and mixed into a yellow wet powder.

[0022] 3) The obtained product is put into an oven and dried at 80°C for 24 hours to obtain a precursor powder;

[0023] 4) Put the precursor into a crucible furnace, raise the temperature at 5°C / min to 1000°C for 10 hours, cool down to room temperature at 5°C / min, and pass through a 320-mesh sieve after grinding. The XRD spectrum of the synthesized product is shown in figure 1 , no impurity phase was seen.

Embodiment 2

[0025] 1) 1) of synchronous embodiment 1;

[0026] 2) Weigh oxalic acid (H 2 C 2 o 4 2H 2 O) 12.606 g of the powder mixed in the first step is put into a high-speed mechanical mixer, stirred at high speed for 20 minutes, and mixed into a yellow wet powder.

[0027] 3) 3) of synchronous embodiment 1;

[0028] 4) 4) of synchronous embodiment 1), the XRD collection of illustrative plates of synthetic product sees figure 2 , no impurity phase was seen. .

Embodiment 3

[0030] 1) 1) of synchronous embodiment 1;

[0031] 2) Weigh the powder mixed in the first step and analytically pure potassium hydroxide (KOH) according to a certain stoichiometric ratio, and put them into a high-speed mixer with a rotation speed of 24,000 rpm. The molar ratio is: 1:10.4 . Mix with high-speed mechanical stirring for 20 minutes to allow sufficient reaction between potassium hydroxide (KOH) and raw materials. The resulting product is washed with water and filtered to wash off the by-product K 2 CO 3 , with BaCl 2 detected until no CO 3 2- . The resulting product was dried at 80°C to obtain a precursor powder;

[0032] 3) 3) of synchronous embodiment 1;

[0033] 4) Calcining the prepared precursor at 900°C for 10 hours to obtain the final product Ba in the perovskite phase 1.0 co 0.7 Fe 0.2 Nb 0.1 o 3-δ . The XRD spectrum of the synthesized product is shown in image 3 , no impurity phase was seen.

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Abstract

The invention belongs to the field of functional materials, and relates to a method for preparing a Ba1.0Co0.7Fe0.2Nb0.1O3-δ material by using a low-heat solid-phase coordination method, which is applied to the field of preparing ceramic oxygen-permeable membrane materials. It is characterized in that the precursor is prepared in two steps. First, the molar ratio of BaCO3: 2CoCO3·3Co(OH)2·H2O: Fe2(C2O4)3·5H2O: Nb2O5=1:0.14:0.1:0.05 is loaded into the high-speed machine Blend in a blender for 20 minutes. Then press (Ba+Co+Fe+Nb): citric acid or oxalic acid or acetic acid=1: 1 molar ratio and take acid, and put into the high-speed mechanical mixer together with the material that mixes and stir for 20 minutes, the obtained product after mixing After drying for 24 hours, the precursor powder is obtained; the prepared precursor is calcined at 900-1100° C. for 2-10 hours to obtain the Ba1.0Co0.7Fe0.2Nb0.1O3-δ of the perovskite phase as the final product. The invention reduces the synthesis temperature and energy consumption; increases the interval between the synthetic pure cubic phase material and the melting temperature of the material, and is beneficial to the firing of the tubular oxygen-permeable device.

Description

technical field [0001] The invention belongs to the field of functional materials, and relates to a method for preparing Ba 1.0 co 0.7 Fe 0.2 Nb 0.1 o 3-δ The material method is applied to the field of preparing ceramic oxygen-permeable membrane materials. Background technique: [0002] The mixed conductor ceramic oxygen permeable membrane material has the ability of oxygen ion conduction and electron conduction at the same time, and it has a very high oxygen permeability at high temperature. The oxygen permeation flux of some optimized materials can even be comparable to that of microporous membranes. . Economic accounting shows that the use of mixed conductor oxygen permeable membrane for oxygen production may save nearly 50% of the cost compared with the traditional air separation method. The research and development of ceramic oxygen-permeable membrane materials is the core and hot spot of oxygen-permeable membrane research. In 2006, Japanese scholar Makofo et al....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G51/04C01G49/02C01G33/00C01F11/02C04B35/01
Inventor 仇卫华李春宏丁伟中李敬康晓丽李福燊
Owner UNIV OF SCI & TECH BEIJING