Hydrolysis-hydrothermal method for preparing scandium-cerium-ytterbium-doped zirconium oxide ultrafine powder

Abstract

The invention belongs to the technical field of nano material preparation, and discloses a hydrolysis-hydrothermal method for preparing scandium-cerium-ytterbium doped zirconium oxide ultrafine powder. The method comprises the following steps: firstly, preparing a reaction mother solution containing zirconium, cerium, scandium and ytterbium elements, and then heating the reaction mother solution to 100-104 DEG C for hydrolysis reaction to obtain milk white hydrolysis slurry; cooling to 50-70 DEG C, adding ammonia water to adjust the pH value to 3.6-4, then adding a mineralizer, heating to 90-100 DEG C, carrying out a hydrothermal reaction, and washing and drying a product to obtain coarse powder; and successively carrying out two-step calcination on the obtained coarse powder at 600-800 DEG C and 900-1100 DEG C, crushing and granulating to obtain the scandium-cerium-ytterbium doped zirconium oxide ultrafine powder. The powder obtained by adopting the preparation method disclosed by the invention is uniform in particle size, uniform in element distribution and stable in physicochemical property. And the process flow is simple, the hydrothermal hydrolysis process is easy to directly observe, the process is controllable, and the method is suitable for large-scale industrial production.

Description

technical field

[0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a hydrolysis-hydrothermal method for preparing scandium, cerium and ytterbium-doped zirconia ultrafine powder. Background technique

[0002] Zirconium dioxide ceramic material has excellent physical and chemical properties such as high melting point and high boiling point, excellent electrical conductivity, good thermal conductivity, high high temperature strength and toughness, good corrosion resistance and wear resistance, etc. It is common in recent years. applications in solid oxide fuel cells (SOFC).

[0003] A solid oxide fuel cell is a clean and efficient energy conversion device, the core of which is a solid electrolyte. At present, the common SOFC on the market is 6-10% yttria-stabilized zirconia (YSZ) powder, which has a high oxygen ion conductivity at a high temperature of 1000 ° C. In addition, it also has high mechanical strength and hig...

Examples

Embodiment 1

[0047] Step 1. Dissolution: Weigh zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide, and ytterbium oxide, and put them in a flask, add water and mix well, then heat in an electric heating mantle to make scandium oxide and ytterbium oxide Dissolve to obtain the reaction mother liquor. The concentration of zirconium oxychloride octahydrate in the reaction mother liquor is 2.5mol / L. The ratio of zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide and ytterbium oxide is ZrO according to the powder composition 2 84wt.%, Sc 2 o 3 11wt.%, Yb 2 o 3 3wt.%, CeO 2 2wt.%.

[0048] Step 2, hydrolysis: transfer the reaction mother liquid to the reaction kettle, and add water to dilute the Zr concentration in the solution to 50g / L to obtain the reaction stock solution; then turn on the heating hydrolysis, use a steam heat exchanger to heat, and raise the temperature of the reaction stock solution to 100 ~104°C, keep warm at ...

Embodiment 2

[0053] Step 1. Dissolution: Weigh zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide, and ytterbium oxide, and put them in a flask, add water and mix well, then heat in an electric heating mantle to make scandium oxide and ytterbium oxide Dissolving to obtain a reaction mother liquor; the concentration of zirconium oxychloride octahydrate in the reaction mother liquor is 2.2mol / L. The ratio of zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide and ytterbium oxide is ZrO according to the powder composition 2 82wt.%, Sc 2 o 3 12wt.%, Yb 2 o 3 4wt.%, CeO 2 2wt.%.

[0054] Step 2, hydrolysis: transfer the reaction mother liquid to the reaction kettle, and add water to dilute the Zr concentration in the solution to 50g / L to obtain the reaction stock solution; then turn on the heating hydrolysis, use a steam heat exchanger to heat, and raise the temperature of the reaction stock solution to 100 ~104°C, keep warm at ...

Embodiment 3

[0059] Step 1. Dissolution: Weigh zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide, and ytterbium oxide, and put them in a flask, add water and mix well, then heat in an electric heating mantle to make scandium oxide and ytterbium oxide Dissolving to obtain a reaction mother liquor; the concentration of zirconium oxychloride octahydrate in the reaction mother liquor is 2.8mol / L. The ratio of zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide and ytterbium oxide is ZrO according to the powder composition 2 86wt.%, Sc 2 o 3 10wt.%, Yb 2 o 3 3wt.%, CeO 2 1 wt.%.

[0060] Step 2, hydrolysis: transfer the reaction mother liquid to the reaction kettle, and add water to dilute the Zr concentration in the solution to 50g / L to obtain the reaction stock solution; then turn on the heating hydrolysis, use a steam heat exchanger to heat, and raise the temperature of the reaction stock solution to 100 ~104°C, keep warm at...

technical field

[0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a hydrolysis-hydrothermal method for preparing scandium, cerium and ytterbium-doped zirconia ultrafine powder. Background technique

[0002] Zirconium dioxide ceramic material has excellent physical and chemical properties such as high melting point and high boiling point, excellent electrical conductivity, good thermal conductivity, high high temperature strength and toughness, good corrosion resistance and wear resistance, etc. It is common in recent years. applications in solid oxide fuel cells (SOFC).

[0003] A solid oxide fuel cell is a clean and efficient energy conversion device, the core of which is a solid electrolyte. At present, the common SOFC on the market is 6-10% yttria-stabilized zirconia (YSZ) powder, which has a high oxygen ion conductivity at a high temperature of 1000 ° C. In addition, it also has high mechanical strength and hig...

Examples

Embodiment 1

[0047] Step 1. Dissolution: Weigh zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide, and ytterbium oxide, and put them in a flask, add water and mix well, then heat in an electric heating mantle to make scandium oxide and ytterbium oxide Dissolve to obtain the reaction mother liquor. The concentration of zirconium oxychloride octahydrate in the reaction mother liquor is 2.5mol / L. The ratio of zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide and ytterbium oxide is ZrO according to the powder composition 2 84wt.%, Sc 2 o 3 11wt.%, Yb 2 o 3 3wt.%, CeO 2 2wt.%.

[0048] Step 2, hydrolysis: transfer the reaction mother liquid to the reaction kettle, and add water to dilute the Zr concentration in the solution to 50g / L to obtain the reaction stock solution; then turn on the heating hydrolysis, use a steam heat exchanger to heat, and raise the temperature of the reaction stock solution to 100 ~104°C, keep warm at ...

Embodiment 2

[0053] Step 1. Dissolution: Weigh zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide, and ytterbium oxide, and put them in a flask, add water and mix well, then heat in an electric heating mantle to make scandium oxide and ytterbium oxide Dissolving to obtain a reaction mother liquor; the concentration of zirconium oxychloride octahydrate in the reaction mother liquor is 2.2mol / L. The ratio of zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide and ytterbium oxide is ZrO according to the powder composition 2 82wt.%, Sc 2 o 3 12wt.%, Yb 2 o 3 4wt.%, CeO 2 2wt.%.

[0054] Step 2, hydrolysis: transfer the reaction mother liquid to the reaction kettle, and add water to dilute the Zr concentration in the solution to 50g / L to obtain the reaction stock solution; then turn on the heating hydrolysis, use a steam heat exchanger to heat, and raise the temperature of the reaction stock solution to 100 ~104°C, keep warm at ...

Embodiment 3

[0059] Step 1. Dissolution: Weigh zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide, and ytterbium oxide, and put them in a flask, add water and mix well, then heat in an electric heating mantle to make scandium oxide and ytterbium oxide Dissolving to obtain a reaction mother liquor; the concentration of zirconium oxychloride octahydrate in the reaction mother liquor is 2.8mol / L. The ratio of zirconium oxychloride octahydrate, cerium chloride heptahydrate, scandium oxide and ytterbium oxide is ZrO according to the powder composition 2 86wt.%, Sc 2 o 3 10wt.%, Yb 2 o 3 3wt.%, CeO 2 1 wt.%.

[0060] Step 2, hydrolysis: transfer the reaction mother liquid to the reaction kettle, and add water to dilute the Zr concentration in the solution to 50g / L to obtain the reaction stock solution; then turn on the heating hydrolysis, use a steam heat exchanger to heat, and raise the temperature of the reaction stock solution to 100 ~104°C, keep warm at...

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