A rare earth samarium zirconate nanomaterial and its hydrothermal preparation method

A technology of samarium zirconate and rare earth, which is applied in the chemical industry, can solve the problems of serious agglomeration, difficulty in filtering and washing, etc., and achieve the effects of easy control of the reaction process, simple and easy preparation method, and easy popularization and use

Inactive Publication Date: 2014-10-29
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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  • A rare earth samarium zirconate nanomaterial and its hydrothermal preparation method
  • A rare earth samarium zirconate nanomaterial and its hydrothermal preparation method
  • A rare earth samarium zirconate nanomaterial and its hydrothermal preparation method

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Experimental program
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Effect test

Embodiment 1

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

[0063] 2) Under the action of magnetic stirring, add 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, centrifuge the gel-like emulsion to obtain a solid precipitate, add water to make a slurry (The purpose is to disperse the precipitate 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 the temperature to 120°C at a rate of 5°C / min and react at a constant temperature for 24 hours, cool to room temperature, wash the product 7 times in a centrifuge with a rotating speed of 4000r / min, and then use Centrifuge and was...

Embodiment 2

[0066] 1) zirconium oxychloride that 30g particle size is 5 μm, pH value is 2.0 is dissolved in 200ml water and obtains aqueous solution, and 10g particle size is that samarium oxide of 3 μm is dissolved in the concentrated nitric acid that 30ml concentration is 8mol / L and makes samarium nitrate solution, will The zirconium oxychloride solution and the samarium nitrate solution are mixed evenly.

[0067] 2) Under the action of magnetic stirring, add ammonia water with a concentration of 10mol / L dropwise to the mixed solution to adjust the pH to 4.0, and then continue to stir for 10 minutes to obtain a gel-like emulsion, which is centrifuged to separate the gel-like emulsion Obtain a solid precipitate, add water to make a slurry (the purpose is to disperse the precipitate with water first), 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 the temperature to 120°C at a ...

Embodiment 3

[0074] 1) 45g of zirconyl sulfate was dissolved in 200ml water to obtain an aqueous solution, 13g of samarium chloride was dissolved in 40ml of water to obtain an aqueous solution, and the zirconyl sulfate solution and the samarium chloride solution were mixed evenly.

[0075] 2) Under the action of magnetic stirring, add 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, centrifuge the gel-like emulsion to obtain a solid precipitate, add water to make a slurry (The purpose is to disperse the precipitate 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 the temperature to 160°C at a rate of 5°C / min and react at a constant temperature for 24 hours, cool to room temperature, and wash the product 7 times in a centrifuge with a speed of 4000r / min, and then use Centrifuge and wash twice with water and e...

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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 chemical industry field, and the invention relates to a thermal barrier coating material, a photocatalytic material and preparation thereof, 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 catalytic, ion conductivity, dielectric properties and other physical and chemical properties. Due to its good high temperature stability, high chemical stability, high melting point, and high ionic conductivity, it is widely used in thermal barrier coatings, catalysts, hydrogen-oxygen fuel cells, organic hydrodehydrogenation, high-temperature pigments, and luminescent substrates. Materials and other aspects have broad application prospects. [0003] There are many methods for preparing rare earth samarium zirconate, the most common of which are solid state reaction method, ...

Claims

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Application Information

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Patent Type & Authority Patents(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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