Method for preparing doped perovskite structural material

A perovskite structure and composite oxide technology, which is applied in the field of preparation of doped perovskite structure materials, can solve the problem of poor surface density and crystal morphology of powders, poor crystallinity and surface compactness, and non-unique crystal forms etc. to achieve the effect of high selectivity, dense surface and high crystallinity

Active Publication Date: 2010-06-09
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0008] Patent CN1342730A discloses a preparation method of titanium-based composite oxide powder. The mixed solution is prepared by complexing organic acid and non-titanium component water-soluble metal salt solution contained in the composite oxide. At the same time, the titanium source is added to stabilize the powder. The titanium stable solution was prepared by mixing the sol and then sintered to obtain a composite oxide powder. A single-phase composite oxide powder was obtained. However, due to the addition of water in the solution, the surface density and crystal morphology of the prepared powder were poor.
[0009] Literature "citric acid sol-gel synthesis YBa 2 Cu 3 o 7-δ "Journal of Northeastern University (Natural Science Edition) 2003, 24(11), 1061-1063 reported that under the condition of not adding ethylene glycol, a uniform YBa 2 Cu 3 o 7-δ Superconducting fine powder, the powder has high activity, but poor crystallinity and surface compactness
[0010] The present invention is designed to solve the above-mentioned problems of poor crystallinity and non-unique crystal form in the preparation of perovskite compounds. Preparation method of titanium ore compound

Method used

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  • Method for preparing doped perovskite structural material
  • Method for preparing doped perovskite structural material

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Embodiment 1

[0026] Accurately weigh 5.29g of strontium nitrate, 1.81g of copper nitrate, 6.06g of iron nitrate, measure TiO(NO 3 ) 2 Add 0.83ml of the solution into a three-necked flask, mix and stir evenly, add 9g of urea and 12ml of ethylene glycol, and keep stirring. At this time, the color of the sol is green, add about 5ml of ammonia water, adjust the pH value to 6.54, and put it in a water bath at 25°C And keep stirring, the color changes from green to dark brown, the viscosity keeps increasing, the temperature is raised to 65°C, and the stirring is continued for 3 hours, the gel is put into the muffle furnace for sintering, the sintering program is controlled from room temperature to 200°C, and the heating rate is 0.1°C / min, keep warm for 30min, and the heating rate is 0.5°C / min at 200-400°C. Keep it warm for 30min, then raise the temperature to 850°C at a heating rate of 1°C and min, and keep it warm for 4 hours to obtain a material with a single crystal form and a high crystalli...

Embodiment 2

[0028] Accurately weigh 6g of zirconium nitrate, 4.2g of copper nitrate, 6.06g of manganese nitrate, measure TiO(NO 3 ) 2 Add 0.8ml of the solution into a three-necked flask, mix and stir evenly, add 20g of citric acid and 30ml of glycerol, and keep stirring. At this time, the color of the sol is green. Add about 10ml of ammonia water, adjust the pH value to 7.0, and set the temperature at 25°C Water bath and constant stirring, the color changes from green to yellow, the viscosity continues to increase, the temperature is raised to 90°C, and the stirring is continued for 6 hours, the gel is put into the muffle furnace for sintering, the sintering program is controlled from room temperature to 200°C, and the heating rate 0.5°C / min, heat preservation 30min, 200-400°C heating rate 1°C / min. Keep it warm for 30 minutes, then raise the temperature to 1000° C. at a heating rate of 5° C. / min, and hold it for 6 hours to obtain a perovskite structure material with a single crystal form...

Embodiment 3

[0030] Accurately weigh 5.29g of strontium nitrate, 4.2g of copper nitrate, 6.06g of manganese nitrate, measure TiO(NO 3 ) 2 Add 0.8ml of the solution into a three-necked flask, mix and stir evenly, add 20g of citric acid and 30ml of methanol, and keep stirring. At this time, the color of the sol is light green. Add about 15ml of ammonia water, adjust the pH value to 8.5, and stir at room temperature. The color changed from light green to orange yellow, and the viscosity continued to increase. The temperature was raised to 80°C and continued to stir for 8 hours. The gel was sintered in a muffle furnace. The sintering program was controlled from room temperature to 200°C, and the heating rate was 0.1°C / min, keep warm for 30min, and the heating rate is 0.8℃ / min at 200-400℃. Keep it warm for 30 minutes, then raise the temperature to 1100° C. at a heating rate of 3° C. / min, and hold it for 10 hours to obtain a material with a single crystal form and a high crystallinity perovski...

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Abstract

The invention provides a method for preparing a doped perovskite structural composite oxide, which comprises two steps, namely preparation and sintering of sol-gel. The preparation of the sol-gel comprises the following steps of selecting an element containing Sr or Zr as a group A element and selecting an element containing three elements selected from Ti, Fe, Cu, Pd and Mn as a group B element to prepare perovskite structural composite oxide gel of which the general formula is AB1-x-yB'xB''yO3-epsilon, wherein x and y are more than 0 and less than 0.5; and epsilon is more than -0.5 and less than 0.5 and is an oxygen lattice defect number. The obtained gel is sintered in a muffle furnace of which the temperature can be controlled by a program to obtain a perovskite oxide material which has a high crystallization degree, a single crystal form and a compact surface. The perovskite oxide material can be applied to a piezoelectric material or an electronic apparatus and can also be made into a compact ion conducting oxygen-permeable membrane for oxygen separation.

Description

technical field [0001] The invention relates to a method for preparing a doped perovskite structure material, more specifically, a method for preparing a perovskite compound according to a certain doping ratio. technical background [0002] Generally speaking, perovskite compounds refer to compounds with the same crystal structure as calcium titanate (perovskite). Through grinding, molding, and sintering, oxygen-permeable membranes with mixed ion conductors can be obtained. Current literature reports There are mainly sheet and tubular forms. In recent years, these materials are not only used in communication equipment or computers as piezoelectric elements and thermistors, but also used to separate oxygen from oxygen-containing gases, especially air, so that they can be used in petrochemical industries. It has great application prospects in oxidation and reduction reactions. [0003] The preparation of perovskite powder materials currently reported mainly includes the follo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/462C04B35/622
Inventor 武洁花张明森柯丽冯静张飞
Owner CHINA PETROLEUM & CHEM CORP
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