Preparation method of stable nanometer yttrium oxide powder

A nano-yttrium oxide and powder technology is applied in the field of preparation of rare earth ultrafine powder, can solve the problems of complicated operation, reduced powder activity, unfavorable transparent ceramic preparation and application, etc., and achieves high purity, low cost, and easy industrialization. production effect

Inactive Publication Date: 2021-07-27
SOUTHWEST PETROLEUM UNIV
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Problems solved by technology

Using ammonium sulfate as a dispersant to prepare nano-yttrium oxide is currently the most commonly used method, but Zhigang Jiang et al. pointed out in the above-mentioned article that the decomposition temperature of sulfate ions is very high, greater than 1180 degrees Celsius, which means to obtain high For pure yttrium oxide powder, the calcination temperature must be increased, and if the calcination temperature is too high, the activity of the powder will be reduced, which is not conducive to the preparation and application of transparent ceramics in the later stage
In addition, it can be seen from the above that the technical solution needs to adjust the pH value of the reaction system to be constant, so the operation is complicated

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  • Preparation method of stable nanometer yttrium oxide powder
  • Preparation method of stable nanometer yttrium oxide powder
  • Preparation method of stable nanometer yttrium oxide powder

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preparation example Construction

[0023] The invention provides a kind of preparation method of stable nanometer yttrium oxide powder, comprises the following steps:

[0024] (1) Prepare an aqueous solution of yttrium salt with a concentration of 0.1-1mol / L, which is recorded as solution A;

[0025] (2) preparation contains the mixed precipitant solution of triethanolamine and ammonium bicarbonate, and is recorded as B solution;

[0026] (3) A solution and B solution are dripped into the other side by titration, and a precipitation reaction occurs. After the titration ends, the suspension of the precipitate containing yttrium is obtained, which is designated as C solution;

[0027] (4) Continue to stir the obtained C solution for a period of time, then age, separate by suction filtration to obtain the precipitate, then wash and dry the precipitate to obtain the yttrium oxide precursor;

[0028] (5) Put the above precursor into a high-temperature resistance furnace for firing to obtain nanometer yttrium oxide ...

Embodiment 1

[0037] Prepare 500ml of yttrium nitrate aqueous solution of 0.2mol / L; Prepare the composite precipitant solution 500ml of triethanolamine and ammonium bicarbonate, wherein the concentration of ammonium bicarbonate is 0.2mol / L, the total number of moles of triethanolamine and ammonium bicarbonate and nitric acid The molar ratio of yttrium is 4:1; Add the composite precipitant solution dropwise in the yttrium nitrate aqueous solution at a speed of 10ml / min, stir while adding dropwise, the stirring speed is 65rpm, after the composite precipitant solution is added dropwise After continuing to stir at a speed of 65rpm for 30min, stop stirring, leave the resulting mixture at room temperature for 6h, then filter the mixture with suction to obtain a precipitate of yttrium; wash the precipitate of yttrium with deionized water 3 times, Then washed twice with absolute ethanol, dried in a drying oven at 90 °C for 6 h after washing to obtain the yttrium oxide precursor; finally, the precurs...

Embodiment 2

[0039] Prepare 500ml of yttrium nitrate aqueous solution of 0.2mol / L; Prepare the composite precipitation agent solution 500ml of triethanolamine and ammonium bicarbonate, wherein the concentration of ammonium bicarbonate is 0.3mol / L, the total number of moles of triethanolamine and ammonium bicarbonate and nitric acid The molar ratio of yttrium is 3:1; The compound precipitant solution is added dropwise in the yttrium nitrate aqueous solution with the speed of 8ml / min, stirs while adding dropwise, and stirring speed is 65rpm, after the compound precipitant solution is added dropwise After continuing to stir at a speed of 65rpm for 30min, stop stirring, leave the resulting mixture at room temperature for 8h, then filter the mixture with suction to obtain a precipitate of yttrium; wash the precipitate of yttrium with deionized water 3 times, Then washed twice with absolute ethanol, dried in a drying oven at 90 °C for 8 h after washing to obtain the yttrium oxide precursor; final...

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Abstract

The invention discloses a preparation method of stable nanometer yttrium oxide powder, belonging to the technical field of preparation of rare earth ultrafine powder. The method comprises the following steps: dropwise adding a mixed precipitant solution containing triethanolamine and ammonium bicarbonate as well as an inorganic salt solution containing yttrium into the mixed precipitant solution in a titration manner at normal pressure and normal temperature so as to obtain a milk white turbid liquid; after titration is finished, continuing stirring and aging; carrying out suction filtration, washing and drying on an aged precipitation solution to obtain an yttrium oxide precursor; and calcining the precursor at 900-1100 DEG C for 2-3 hours to obtain the nanometer yttrium oxide powder. According to the method for preparing yttrium oxide, a pH value does not need to be specially controlled, conditions such as heating and pressurizing are not needed, the method is not limited by special equipment, process is simple, process conditions are easy to control, the monodisperse nanometer yttrium oxide powder can be stably obtained, cost is low, and industrial production is easy.

Description

technical field [0001] The invention belongs to the technical field of preparation of rare earth ultrafine powder, in particular to a preparation method of nanometer yttrium oxide powder. Background technique [0002] Yttrium oxide (Y 2 o 3 ) belongs to the cubic crystal system, which has excellent physical, chemical and optical properties such as good high temperature stability, heat resistance, corrosion resistance, high dielectric constant, low phonon energy and wide transparent range. It is used in functional ceramic materials, luminescent materials, laser Ceramic materials and other fields have a wide range of applications. For example, yttrium oxide polycrystalline ceramics has become a very important high-temperature window material because of its good light transmission; adding Pr 3+ 、Eu 3+ 、Nd 3+ Y such as rare earth elements 2 o 3 It can be used as fluorescent material and working substance of solid-state laser. The key to preparing highly transparent ceram...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/218B82Y40/00C01F17/10
CPCB82Y40/00C01P2002/72C01P2004/03C01P2004/32C01P2004/64C01F17/10C01F17/218
Inventor 仝世红金泽昊杨浩松
Owner SOUTHWEST PETROLEUM UNIV
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