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Method for synthesizing sphere-like nano yttrium and cerium doped zirconia according to ethylene glycol sol-gel method

A glycol-like spherical technology, applied in the field of materials, can solve the problems of limiting the application of zirconia, and achieve the effect of cheap raw materials and wide sources

Active Publication Date: 2013-04-03
瑞金市工业投资发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the huge stress and volume change caused by the interconversion between cubic-tetragonal-monoclinic phases during the cooling process of pure zirconia from high temperature to room temperature limits the application of zirconia.

Method used

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  • Method for synthesizing sphere-like nano yttrium and cerium doped zirconia according to ethylene glycol sol-gel method
  • Method for synthesizing sphere-like nano yttrium and cerium doped zirconia according to ethylene glycol sol-gel method
  • Method for synthesizing sphere-like nano yttrium and cerium doped zirconia according to ethylene glycol sol-gel method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 0.625ml of 1mol / L yttrium nitrate solution, 0.521ml of 0.4mol / L cerous nitrate solution, 6.7848g of zirconium nitrate, 24ml of deionized water, and 1ml of ethylene glycol (the mixture of ethylene glycol and metal ions) into a round bottom flask. The ratio of the amount of substances is 0.86), and the zirconium nitrate is completely dissolved into a transparent solution under magnetic stirring. Place the round-bottomed flask in an oil bath, connect the reflux tube, heat to 130°C, and reflux for 8 hours to form a sol. The obtained sol was transferred to an oven and dried at 110° C. for 12 h to obtain a solid gel. Then placed in a muffle furnace and calcined at 800°C for 3h. A partially stabilized zirconia (PSZ) powder was obtained.

[0020] According to the same method as above, only the amount of ethylene glycol added is different, which are 3ml, 5ml and 10ml respectively, and the corresponding ratios of the amount of ethylene glycol to metal ions are 2.58, 4.30 an...

Embodiment 2

[0022] Add 0.625ml of 1mol / L yttrium nitrate solution, 0.521ml of 0.4mol / L cerous nitrate solution, 6.7848g of zirconium nitrate, 24ml of deionized water, and 1ml of ethylene glycol (the mixture of ethylene glycol and metal ions) into a round bottom flask. The ratio of the amount of substances is 0.86), adding NaCl solid, the ratio of its mass to the mass of NaCl and the total mass of nitrate is 0.5%, and all the zirconium nitrate is dissolved into a transparent solution under magnetic stirring. Place the round-bottomed flask in an oil bath, connect the reflux tube, heat to 130°C, and reflux for 8 hours to form a sol. The obtained sol was transferred to an oven and dried at 110° C. for 12 h to obtain a solid gel. The obtained solid gel was firstly washed with water and ethanol to remove the sodium chloride therein, and then placed in a muffle furnace for calcination at 800° C. for 3 h. A partially stabilized zirconia (PSZ) powder was obtained.

[0023] According to the same ...

Embodiment 3

[0025] According to the basic method of Example 2, the added amount of sodium chloride was changed, respectively 0.2%, 0.3%, 1.5%, 4.5%, 7.5%, 12%, and the obtained solid gel was not washed out with water and ethanol. Sodium chloride is directly put into the muffle furnace for calcination. Measure the XRD patterns of the obtained powders respectively, and the relationship diagram between the tetragonal phase content and the amount of sodium chloride added is shown in image 3 , compared with the sample that was calcined after washing off sodium chloride in Example 2, the tetragonal phase content decreased significantly. The SEM image of the synthesized sample is shown in Figure 6, which shows that the addition of sodium chloride can significantly improve the dispersibility and particle sphericity of the synthesized product, but the addition amount should not be too much. When it exceeds 7.5%, the particle agglomeration is serious.

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Abstract

A method for synthesizing sphere-like nano yttrium and cerium doped zirconia according to an ethylene glycol sol-gel method takes zirconium nitrate, yttrium nitrate, cerium nitrate and sodium chloride as raw materials, is a specific method used for preparing zirconia nano-crystalline with stable yttrium and cerium parts according to the ethylene glycol sol-gel method, and comprises the following steps: preparing aqueous solution containing zirconium nitrate, yttrium nitrate, cerium nitrate and sodium chloride according to the stoichiometric ratio of 96 : 3 : 1; adding ethylene glycol solution in such a manner that the ratio between the weight of ethylene glycol and the total weight of metal ions is 0.8 to 8.6; heating the mixed solution, reflowing and reacting for 1 to 12 h till sol is formed; reacting metal ions with ethylene glycol to form coordination polymer with a cross-linked structure; drying under 110 to 130 DEG C for 6 to 50 h till solid gel is obtained; washing off sodium chloride in gel with little water and alcohol; and calcining in a muffle furnace under 400 to 800 DEG C for 3 h, so as to obtain required sphere-like nano yttrium and cerium doped zirconia of which the principal crystalline phase is square phase and the particle size is about 60 nanometer.

Description

technical field [0001] The invention relates to a specific method for synthesizing a spherical nano rare earth-doped zirconia powder with a tetragonal phase structure as the main crystal phase, and belongs to the field of materials. technical background [0002] Zirconia and its composite oxides have a wide range of applications, such as: toughened ceramics, pH sensors, solid oxide fuel cell anodes, catalytic flue gas, NOx, chlorinated VOC and other combustion catalysts and adsorbents in purification technologies, etc. . However, the huge stress and volume change caused by the interconversion between cubic-tetragonal-monoclinic phases during the cooling process of pure zirconia from high temperature to normal temperature limit the application of zirconia. The doping of some divalent and trivalent metal ions can make zirconia exist in a metastable tetragonal or cubic phase at room temperature, and produce a phase change toughening effect, which improves their application pe...

Claims

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Application Information

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IPC IPC(8): C01G25/02B82Y30/00
Inventor 李永绣陈萍华周雪珍唐群陈伟凡李静刘艳珠
Owner 瑞金市工业投资发展有限公司
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