Rare earth samarium zirconate nano material and hydrothermal preparation method thereof

A samarium zirconate and rare earth technology, applied in the chemical industry, can solve the problems of severe agglomeration, difficulty in filtering and washing, and large particle size of the product, so as to achieve easy control of the reaction process, simple and easy preparation method, and complete grain development Effect

Inactive Publication Date: 2012-09-19
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

They have their own advantages and disadvantages: the products prepared by the sol-gel method have good uniformity, small particle size, and large specific surface area. The disadvantages are that the organic solvent is toxic and requires high-temperature calcination; the high-temperature solid-phase method does not require solvents during the preparation process and has high yields. , The process is simple, the disadvantage is that the obtained product has a large particle size, and the agglomeration is severe, the specific surface area is small, and the crystallinity is poor
The ceramic powder prepared by the chemical co-precipitation method has a fine particle size and good sintering performance. The disadvantage is that the formed precipitate is in a colloidal state, which is difficult to filter and wash, and has serious agglomeration during the drying and dehydration process.
At present, the preparation of rare earth zirconates is mainly concentrated on high-temperature solid-phase synthesis, but the temperature required for the reaction is very high, and a long reaction time is required; at the same time, it is also reported that rare earth zirconates are synthesized by methods such as hydrazine hydrate. The problem is that the particle size is large and the particle agglomeration is serious

Method used

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  • Rare earth samarium zirconate nano material and hydrothermal preparation method thereof
  • Rare earth samarium zirconate nano material and hydrothermal preparation method thereof
  • Rare earth samarium zirconate nano material and hydrothermal preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1) Dissolve 30 g of zirconium oxychloride in 200 ml of water to obtain an aqueous solution. Dissolve 10 g of samarium oxide in 30 ml of concentrated nitric acid to prepare a samarium nitrate solution. Mix the zirconium oxychloride solution and the samarium nitrate solution uniformly.

[0063] 2) Under the action of magnetic stirring, add ammonia water dropwise to the mixed solution to adjust to pH=4.0, then stir continuously for 10 minutes to obtain a gel-like emulsion, centrifuge the gel-like emulsion to obtain a solid precipitate, add water to make a slurry (The purpose is to disperse the precipitation with water first) and then add KOH solution to PH=9 to obtain a white slurry.

[0064] 3) Put the above slurry into the reaction kettle, raise it to 120°C at a heating rate of 5°C / min and react at a constant temperature for 24h, then cool to room temperature. The product is washed with water 7 times in a centrifuge with a speed of 4000r / min, and then used without The product...

Embodiment 2

[0066] 1) Dissolve 30g of zirconium oxychloride with a particle size of 5μm and a pH of 2.0 in 200ml of water to obtain an aqueous solution. Dissolve 10g of samarium oxide with a particle size of 3μm in 30ml of concentrated nitric acid with a concentration of 8mol / L to obtain a samarium nitrate solution. The zirconium oxychloride solution and the samarium nitrate solution are mixed uniformly.

[0067] 2) Under the action of magnetic stirring, add 10 mol / L ammonia water dropwise to the mixed solution to adjust to PH=4.0, and then continue to stir for 10 minutes to obtain a gel-like emulsion, and centrifuge the gel-like emulsion Obtain a solid precipitate, add water to make a slurry (the purpose is to first disperse the precipitate with water) and then add a KOH solution with a concentration of 6 mol / L to PH=13 to obtain a white slurry.

[0068] 3) Put the above slurry into the reaction kettle, raise it to 120°C at a heating rate of 5°C / min and react at a constant temperature for 24h...

Embodiment 3

[0074] 1) Dissolve 45 g of zirconyl sulfate in 200 ml of water to obtain an aqueous solution, and dissolve 13 g of samarium chloride in 40 ml of water to obtain an aqueous solution, and mix the zirconyl sulfate solution and the samarium chloride solution uniformly.

[0075] 2) Under the action of magnetic stirring, add ammonia water dropwise to the mixed solution to adjust to pH=4.0, then stir continuously for 10 minutes to obtain a gel-like emulsion, centrifuge the gel-like emulsion to obtain a solid precipitate, add water to make a slurry (The purpose is to disperse the precipitation with water first) and then add KOH solution to PH=9 to obtain a white slurry.

[0076] 3) Put the above slurry into the reaction kettle, raise it to 160°C at a heating rate of 5°C / min and react at a constant temperature for 24h, then cool to room temperature. The product is washed 7 times in a centrifuge with a rotating speed of 4000r / min, and then used without The product powder can be obtained by c...

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Abstract

The invention discloses rare earth samarium zirconate nano material and a hydrothermal preparation method of the rare earth samarium zirconate nano material. The rare earth samarium zirconate nano material adopts nanoscale rare earth samarium zirconate powder formed by directly performing hydro-thermal synthesis on coprecipitated precursors. The rare earth samarium zirconate powder prepared through the method has a low thermal coefficient and a good thermal barrier effect, and belongs to potential photocatalytic semiconductor material. The method comprises the following steps: firstly, dissolving a zirconium source in deionized water, and then mixing the zirconium source with samarium source solution, secondly, adding prepared strong alkali solution in the mixed solution of the step one, sufficiently stirring to obtain precursor products, and performing centrifugalization to obtain solid precipitate, thirdly, dispersing the solid precipitate of the step two in deionized water, adjusting the PH value of solution, and adding slurry in a high-pressure reaction kettle to be reacted; and fourthly, taking out powder after the reaction, and washing the powder obtain pour phase samarium zirconate nano powder.

Description

Technical field [0001] The invention belongs to the field of chemical industry. The invention relates to a thermal barrier coating material and a photocatalytic material and preparation thereof, and in particular to a rare earth samarium zirconate nano material and a water preparation method thereof. Background technique [0002] Rare earth samarium zirconate is a new type of inorganic composite material with various physical and chemical properties such as catalytic, ionic conductivity, and dielectric properties. Due to its good high temperature stability, high chemical stability, high melting point, and high ionic conductivity, it is used in thermal barrier coatings, catalysts, hydrogen-oxygen fuel cells, organic hydrogenation, high-temperature pigments, and light-emitting substrates. Materials and other aspects have broad application prospects. [0003] There are many methods for preparing rare earth samarium zirconate, among which the most common are solid-phase reaction metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/00B82Y40/00C04B35/50B01J23/10
Inventor 王全胜陈立亮金海波豆艳坤
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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