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Preparation method of cubic lanthanum zirconate nanometer monocrystal

A nano single crystal, lanthanum zirconate technology, applied in the direction of nanotechnology, nanotechnology, chemical instruments and methods, etc., can solve the problem of high calcination temperature, achieve the effects of lower calcination temperature, easy control of process parameters, and simple equipment

Inactive Publication Date: 2015-08-19
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current methods for synthesizing lanthanum zirconate include traditional high-temperature solid-phase method and liquid-phase method. These methods have their own characteristics, but they all have shortcomings. For example, the calcination temperature required for the phase formation of lanthanum zirconate is as high as 1200 ° C

Method used

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  • Preparation method of cubic lanthanum zirconate nanometer monocrystal

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Embodiment 1

[0029] A method for preparing cubic lanthanum zirconate nano single crystals, comprising the steps of:

[0030] 1) Preparation of hydroxide colloid (preparation of hydroxide precursor):

[0031] The zirconium oxychloride solution is mixed with the lanthanum nitrate solution to obtain a mixed solution in which the molar ratio of zirconium ions to lanthanum ions is 1:1, the concentration of zirconium ions is 0.2mol / L, and the concentration of lanthanum ions is 0.2mol / L;

[0032] The mixed solution is added to ammonia water with a volume concentration of 30% to 80% and stirred to make the pH of the system reach 8-11; stand and age for 2 hours to obtain a hydroxide colloid;

[0033] 2) Solid-liquid separation and washing: Pour off the aged supernatant, and remove impurities from the hydroxide colloid by centrifugal separation (or filter press washing), until the separated water cannot detect chloride ions with silver nitrate ( No precipitation was detected), and a semi-so...

Embodiment 2

[0041] A method for preparing cubic lanthanum zirconate nano single crystals, comprising the steps of:

[0042] 1) Preparation of hydroxide colloid (preparation of hydroxide precursor):

[0043] The zirconium oxychloride solution is mixed with the lanthanum nitrate solution to obtain a mixed solution in which the molar ratio of zirconium ions to lanthanum ions is 1:1, the concentration of zirconium ions is 1.0mol / L, and the concentration of lanthanum ions is 0.5mol / L;

[0044] The mixed solution is added to ammonia water with a volume concentration of 30% to 80% and stirred to make the pH of the system reach 8-11; stand and age for 2 hours to obtain a hydroxide colloid;

[0045] 2) Solid-liquid separation and washing: Pour off the aged supernatant, and remove impurities from the hydroxide colloid by centrifugal separation (or filter press washing), until the separated water cannot detect chloride ions with silver nitrate ( No precipitation was detected), and a semi-so...

Embodiment 3

[0052] A method for preparing cubic lanthanum zirconate nano single crystals, comprising the steps of:

[0053] 1) Preparation of hydroxide colloid (preparation of hydroxide precursor):

[0054] The zirconium oxychloride solution is mixed with the lanthanum nitrate solution to obtain a mixed solution in which the molar ratio of zirconium ions to lanthanum ions is 1:1, the concentration of zirconium ions is 0.5mol / L, and the concentration of lanthanum ions is 0.5mol / L;

[0055] Add it into ammonia water with a volume concentration of 30% to 80% and stir to make the pH of the system reach 8-11; leave it to stand for 2 hours to obtain a hydroxide colloid;

[0056] 2) Solid-liquid separation and washing: Pour off the aged supernatant, and remove impurities from the hydroxide colloid by centrifugal separation (or filter press washing), until the separated water cannot detect chloride ions with silver nitrate ( test without precipitation), and obtain a semi-solid high-viscosity...

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Abstract

The invention relates to a preparation method of a cubic lanthanum zirconate nanometer monocrystal. The method comprises the following steps: 1, preparing a hydroxide colloid: mixing an aqueous solution of a water-soluble zirconium salt with an aqueous solution of a water-soluble lanthanum salt, adding the obtained mixed solution into ammonia water, and stirring to obtain the hydroxide colloid; 2, carrying out solid-liquid separation, and washing; 3, drying; 4, carrying out salt melting: mixing the above obtained dried powder with a salt melting agent according to a mass ratio of 1:9, grinding, and carrying out salt melting at 450-700DEG C for 0.5-96h in order to obtain a salt melted product; and 5, carrying out centrifugal drying to obtain the cubic lanthanum zirconate nanometer monocrystal. The large-scale process production of the cubic nanometer monocrystal with the lanthanum zirconate of a pyrrhite structure and the crystal grain size of 10-40nm is easy; and the salt melting agent is added to effectively reduce the calcining temperature of lanthanum zirconate, and the calcining temperature is 500-750DEG C and is lower than that of traditional high temperature solid phase methods and coprecipitation methods, so the required energy is greatly reduced.

Description

technical field [0001] The invention relates to a preparation method of cubic lanthanum zirconate nano single crystal, which belongs to the field of preparation and application of inorganic non-metallic materials. Background technique [0002] Lanthanum zirconate is widely used in solidified dielectrics, solid fuel cells, gas-sensitive materials, fluorescent materials etc. At the same time, because of its chemical stability, low thermal conductivity and other advantages, this material is one of the most extensively researched and most promising candidate materials for new thermal barrier coatings. A major breakthrough has been made in the field of multilayer ceramic materials. [0003] With the development of aviation gas turbines in the direction of high flow ratio, high thrust-to-weight ratio, and high inlet temperature, the gas temperature and pressure in the combustion chamber continue to increase. The classic YSZ thermal barrier coating material is prone to phase c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00B82Y30/00
Inventor 靳洪允刘敏侯书恩侯盼徐春辉
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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