High-temperature and high-pressure preparation method for cubic phase barium-iron-antimony oxide

A technology of antimony oxide, high temperature and high pressure, applied in the direction of iron oxide/iron hydroxide, etc., to achieve the effect of fast industrialization, simple operation and high purity

Inactive Publication Date: 2013-01-30
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no report on the preparation of high temperature and high pressure

Method used

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  • High-temperature and high-pressure preparation method for cubic phase barium-iron-antimony oxide
  • High-temperature and high-pressure preparation method for cubic phase barium-iron-antimony oxide
  • High-temperature and high-pressure preparation method for cubic phase barium-iron-antimony oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Embodiment 1: prepare Ba with sol-gel method 2 FeSbO 6 :

[0023] Weigh 3 grams C 4 h 6 o 6 (tartaric acid), completely dissolved in 150ml of distilled water as a solvent. Then add 0.0015mol of Sb 2 o 3 (0.4373 g), heated and stirred. Wait for Sb 2 o 3 When completely dissolved in tartaric acid solution, weigh 0.003mol of Fe(NO 3 ) 3 , 0.006mol of Ba(NO 3 ) 2 Dissolve in tartaric acid solution, adjust the temperature to 90°C, continue heating and stirring until the solution becomes viscous and forms a sol. Put the obtained sol-like product into an oven and bake it at 100°C for about 12 hours to obtain a dry and bulky colloid, then put the colloid in a muffle furnace for sintering for 12 hours (800°C) to obtain a sol-gel Precursor. The precursor is ground into a fine powder, put into a muffle furnace and sintered again to obtain the final sample (precursor). The hexagonal structure Ba prepared under this condition 2 FeSbO 6 X-ray results see figure 1 ....

Embodiment 2

[0025] Embodiment 2: prepare Ba with the method for high temperature and high pressure 2 FeSbO 6

[0026] Using the precursor prepared in Example 1, press the precursor powder and wrap it with a layer of BN (you can put the pressure-induced precursor into the BN tube), and put the sample into the pyrophyllite synthesis chamber body. Graphite is used as the heating tube in the synthesis chamber, and pyrophyllite is used as the insulating tube. The synthesis pressure is 5GPa, the temperature is 1373K, and the pressure holding time is 1 hour. After the heating is stopped, the sample is naturally cooled to room temperature and then the pressure is released. The cubic structure Ba prepared under this condition 2 FeSbO 6 The degree of crystallization is the best, the purity is the highest, and the X-ray results can be seen figure 2 .

Embodiment 3

[0027] Embodiment 3: prepare Ba with the method for high temperature and high pressure 2 FeSbO 6

[0028] Using the same assembly and raw materials as in Example 2, the synthesis pressure is 5GPa, the temperature is 1473K, and the pressure holding time is 1 hour. After the heating is stopped, the sample is naturally cooled to room temperature and then the pressure is released. The cubic structure Ba prepared under this condition 2 FeSbO 6 Contains oxide impurities. For specific X-ray results, see image 3 .

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PUM

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Abstract

The invention discloses a high-temperature and high-pressure preparation method for a cubic phase barium-iron-antimony oxide, and belongs to the technical field of preparation of low field magneto-resistance materials. Barium nitrate, ferric nitrate and antimony trioxide are used as raw materials; the method comprises the process of preparation of a precursor and high-temperature and high-pressure synthesis; the precursor is prepared by mixing raw materials through a sol-gel method; and according to the high-temperature and high-pressure synthesis, heat and pressure are preserved for 1 to 2 hours under the pressure of 5GPa and at the temperature of between 1,100 and 1,300 DEG C, and cooling and pressure relief are carried out to obtain a Ba2FeSbO6 material with a cubic structure. According to the method, the precursor is prepared by using the sol-gel method, so that the reactants are mixed uniformly, and the purity of the final product is high; by adopting the conventional high-temperature and high-pressure equipment, the method is easy to operate and can quickly implement industrialization; and the obtained high-quality barium-iron-antimony oxide is a cubic phase material.

Description

technical field [0001] The invention belongs to the technical field of low-field magnetoresistance material preparation. Specifically related to the cubic phase of barium iron antimony oxide, and barium nitrate (Ba(NO 3 ) 2 ), ferric nitrate (Fe(NO 3 ) 3 ), antimony trioxide (Sb 2 o 3 ) as raw materials, using the sol-gel method and high temperature and high pressure sintering technology to synthesize the cubic phase of barium iron antimony oxide. Background technique [0002] With the continuous development and progress of society, people have a deeper understanding of materials, and perovskite-type iron-based oxides have already become a class of materials that occupy an important position in wide applications. Perovskite AFeO 3 with double perovskite A 2 FeBO 6 The compound has a stable crystal structure, unique electromagnetic properties and high redox, hydrogenolysis, isomerization, electrocatalysis and other activities, and has great development potential in t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G49/02
Inventor 王欣李娜娜朱品文陶强
Owner JILIN UNIV
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