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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 problems such as limiting the application of zirconia, and achieve the effect of cheap raw materials and wide sources

Active Publication Date: 2014-08-06
瑞金市工业投资发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 into the round bottom flask, and add 1ml of ethylene glycol (the substance of ethylene glycol and metal ions) The ratio of the amount is 0.86), the zirconium nitrate is completely dissolved into a transparent solution under magnetic stirring. Place the round bottom flask in an oil bath, connect the reflux tube, heat to 130°C, reflux for 8 hours, and form a sol. The obtained sol was transferred to an oven and dried at 110° C. for 12 hours to obtain a solid gel. Then it was placed in a muffle furnace and calcined at 800°C for 3 hours. 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, respectively, 3ml, 5ml and 10ml, and the corresponding ratio of the amount of ethylene glycol to the metal ion is 2.58, 4.30 and 8.61. M...

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 into the round bottom flask, and add 1ml of ethylene glycol (the substance of ethylene glycol and metal ions) The ratio of the amount is 0.86), NaCl solid is added, the ratio of its mass to the mass of NaCl and the total mass of nitrate is 0.5%, and the zirconium nitrate is completely dissolved into a transparent solution under magnetic stirring. Place the round bottom flask in an oil bath, connect the reflux tube, heat to 130°C, reflux for 8 hours, and form a sol. The obtained sol was transferred to an oven and dried at 110° C. for 12 hours to obtain a solid gel. The obtained solid gel was first washed with water and ethanol to remove sodium chloride, and then placed in a muffle furnace and calcined at 800°C for 3 hours. A partially stabilized zirconia (PSZ) powder was obtained.

[0023] According to the same method as above,...

Embodiment 3

[0025] According to the basic method of Example 2, the addition amount of sodium chloride was changed to 0.2%, 0.3%, 1.5%, 4.5%, 7.5%, 12%, and the obtained solid gel was not washed with water and ethanol. The sodium chloride is calcined directly in the muffle furnace. Measure the XRD patterns of the obtained powders respectively. The relationship between the content of the tetragonal phase and the amount of sodium chloride is shown in image 3 Compared with the sample that was calcined after washing off the sodium chloride in Example 2, the content of the tetragonal phase was significantly reduced. The SEM image of the synthesized sample is shown in Figure 6, which shows that the addition of sodium chloride can significantly improve the dispersion 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 more 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 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 oxide 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. . However, the huge stress and volume change caused by the mutual conversion of cubic-tetragonal-monoclinic phases during the cooling process of pure zirconia from high temperature to normal temperature limits the application of zirconia. The doping of some divalent and trivalent metal ions can make zirconia have a metastable tetragonal or cubic phase at room temperature, and produce a phase change toughening effect, which improves their application performance. [0003] Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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