Spherical lanthanum zirconate nano material preparation method

A nanomaterial, lanthanum zirconate technology, applied in chemical instruments and methods, zirconium compounds, inorganic chemistry, etc., can solve the problems of increased defects in use performance, easy deviation of components, unfavorable application and promotion, etc., and achieves high production efficiency and preparation. The effect of low cost and simple process route

Inactive Publication Date: 2017-01-25
BOHAI UNIV
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Problems solved by technology

The solid-phase sintering reaction method is one of the most commonly used methods for preparing powders, but the composition of the product is prone to deviation, and the single-phase calcination temperature is above 1450 °C
Although the sol-gel method is an ideal, simple and easy method for preparing ultrafine powder with high activity, it generally uses expensive alkoxides, which is not conducive to application and promotion.
The self-propagating combustion method has simple steps and does not require complicated equipment. It can prepare ultrafine lanthanum zirconate powder with a single phase composition at a relatively low temperature. However, during the combustion process, the material undergoes a large temperature change, and the Heating and cooling rates increase the number of defects in the product and affect its performance

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Embodiment 1

[0030] The molar ratio of lanthanum acetylacetonate and zirconium acetylacetonate is 1:1, accurately weighed and put into methanol (12C, 99.95%) to stir and dissolve. The molar concentration of lanthanum acetylacetonate is 0.01 mol / L. The resulting mixed solution was subjected to solvothermal reaction, the solvothermal reaction temperature was 200 ° C, and the solvothermal reaction time was 24 hours. After the solvothermal reaction was completed, it was naturally cooled to room temperature, and the product obtained by the reaction was filtered and washed and placed in an oven at a programmed temperature increase rate of 5°C / min, and dried at 120°C for 5 hours. Then place it in a muffle furnace for calcination, the calcination time is 8 hours, the calcination temperature is 600 °C, and the heating rate is 10 °C / min. Spherical lanthanum zirconate nanomaterials were obtained after natural cooling, the size of the spheres was 160 nm, and the yield of the product was 99.9%. The pu...

Embodiment 2

[0032] The molar ratio of lanthanum acetylacetonate and zirconium acetylacetonate is 1:1, accurately weighed and put into methanol (12C, 99.95%) to stir and dissolve. The molar concentration of lanthanum acetylacetonate is 0.05 mol / L. The resulting mixed solution was subjected to solvothermal reaction, the solvothermal reaction temperature was 220 ° C, and the solvothermal reaction time was 12 hours. After the solvothermal reaction was completed, it was naturally cooled to room temperature, and the product obtained by the reaction was filtered and washed and placed in an oven at a programmed temperature increase rate of 5°C / min, and dried at 120°C for 5 hours. Then place it in a muffle furnace for calcination, the calcination time is 2 hours, the calcination temperature is 800 °C, and the heating rate is 20 °C / min. Spherical lanthanum zirconate nanomaterials were obtained after natural cooling, the size of the spheres was 150 nm, and the yield of the product was 99.0%. The pu...

Embodiment 3

[0034] The molar ratio of lanthanum acetylacetonate and zirconium acetylacetonate is 1:1, accurately weighed and put into methanol (12C, 99.95%) to stir and dissolve. The molar concentration of lanthanum acetylacetonate is 0.1 mol / L. The resulting mixed solution was subjected to solvothermal reaction, the solvothermal reaction temperature was 200 ° C, and the solvothermal reaction time was 48 hours. After the solvothermal reaction was completed, it was naturally cooled to room temperature, and the product obtained by the reaction was filtered and washed and placed in an oven at a programmed temperature increase rate of 5°C / min, and dried at 120°C for 5 hours. Then place it in a muffle furnace for calcination, the calcination time is 8 hours, the calcination temperature is 800 °C, and the heating rate is 10 °C / min. Spherical lanthanum zirconate nanomaterials were obtained after natural cooling, the size of the spheres was 200 nm, and the yield of the product was 99.7%. The pur...

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Abstract

The invention belongs to the field of preparation of inorganic nonmetallic materials and particularly relates to a spherical lanthanum zirconate nano material preparation method. The method includes: completely dissolving lanthanum acetylacetonate and zirconium acetylacetonate into methanol solution, performing solvothermal reaction, filtering, washing, drying, calcining and cooling to obtain a spherical lanthanum zirconate nano material. The spherical lanthanum zirconate nano material preparation method is simple, convenient and feasible in process, high product purity and low preparation cost are realized, product size is 150-200nm, high uniformity and dispersity of products are achieved, and technical simplicity in production, low sintering temperature and easiness in application to practical large-scale production are realized. The spherical lanthanum zirconate nano material prepared according to the method has a promising application prospect in the field of high-temperature thermal insulation.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic non-metallic materials, and in particular relates to a preparation method of a spherical lanthanum zirconate nanometer material. Background technique [0002] Lanthanum zirconate (La 2 Zr 2 o 7 ) for A 2 B 2 o 7 Type binary metal oxide material, the crystal structure is the same as that of pyrochlore, which belongs to the cubic crystal system, and can also be regarded as derived from the fluorite structure. Due to its excellent crystal structure, lanthanum zirconate has many special properties, especially in the field of high-temperature heat-shielding coatings, which are widely used. The gas turbines used in the aerospace field are developing toward high inlet temperature and high thrust-to-weight ratio. The gas temperature and pressure in the combustion chamber are very high. It is required that the materials used in the manufacture of gas turbines must have high melting p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00
CPCC01G25/00C01P2002/72C01P2004/03C01P2004/32C01P2004/62C01P2006/80
Inventor 许家胜候春雨张杰
Owner BOHAI UNIV
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