Methanol thermosynthesis method for preparing stable spherical tetragonal phase rare-earth yttrium zirconium oxide

A technology of yttrium-stabilized zirconia and tetragonal phase, applied in zirconia and other directions, can solve the problems of high energy consumption, complex preparation and production process, product morphology, particle size control, etc., to achieve narrow particle size distribution, good dispersion, suitable for The effect of mass production

Inactive Publication Date: 2012-09-26
NANCHANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above methods are difficult to control the shape and particle size of the product.
A

Method used

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  • Methanol thermosynthesis method for preparing stable spherical tetragonal phase rare-earth yttrium zirconium oxide
  • Methanol thermosynthesis method for preparing stable spherical tetragonal phase rare-earth yttrium zirconium oxide
  • Methanol thermosynthesis method for preparing stable spherical tetragonal phase rare-earth yttrium zirconium oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Using ZrOCl 2 ·8H 2 O and YCl 3 ·6H 2 O is the raw material, accurately weigh the corresponding raw materials according to the molar ratio of 97:3, dissolve them in methanol, and transfer to the attached figure 2 Sealed in the PTFE liner shown. Each 10ml volume of the liner is weighed according to 1 gram of the total reactants; the sealed polytetrafluoroethylene liner is placed in a stainless steel jacket, tightened and placed in an oven, heated to 180°C, and kept for 12 hours. Naturally cool to room temperature, take out the inner container, suction filter the reactants, wash with methanol three times, collect the product, and dry it at 60°C for 2 hours. The scanning electron microscopy, XRD, and thermogravimetric images of the obtained product are shown respectively Attached image 3 , 4 , 5, 6. At the same time, part of the product is calcined to 1100°C and kept for 2 hours. The XRD pattern of the obtained product and its comparison with the standard patte...

Embodiment 2

[0034] Example 2: Using ZrOCl 2 ·8H 2 O and YCl 3 ·6H 2 O is the raw material, accurately weigh the corresponding raw materials according to the molar ratio of 97:3, dissolve them in a mixed solvent of methanol and water (the volume ratio of methanol to water is 5:5), dissolve quickly and transfer to the PTFE Seal in the gallbladder. Each 10ml volume of the liner is weighed according to 1 gram of the total reactants; the sealed polytetrafluoroethylene liner is placed in a stainless steel jacket, tightened and placed in an oven, heated to 180°C, and kept for 12 hours. Take out the inner tank, filter the reactants with suction, wash with methanol three times, collect the product, and dry it at 60°C for 2 hours. The scanning electron micrograph and XRD pattern of the obtained product are shown in the attachment. Figure 8 , 10 . It shows that the desired spherical tetragonal phase product cannot be obtained in a reaction system with a large water content. At the same time, part o...

Embodiment 3

[0035] Example 3: Using ZrOCl 2 . 8H 2 O and YCl 3 . 6H 2 O is the raw material, and the corresponding raw materials are accurately weighed according to the molar ratio of 97:3, trying to co-dissolve in ethanol, but it is found that ZrOCl is 2 . 8H 2 O cannot dissolve. Because ZrOCl 2 . 8H 2 O can only dissolve methanol in alcohols. Therefore, other alcohols are not suitable as reaction solvents.

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PUM

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Abstract

The invention discloses a methanol thermosynthesis method for preparing stable spherical tetragonal phase rare-earth yttrium zirconium oxide, comprising the following steps of: accurately weighing ZrOC12.8H2O and YC13.6H2O serving as raw materials according to a molar ratio of 98: (2-87): 13; drying the raw materials under the low temperature of less than 100 DEG C and dissolving the raw materials with absolute methanol; uniformly stirring a mixture and then transferring the mixture to a dry pressure-resistant container; sealing the dry pressure-resistant container and raising the temperature to 160 and 220 DEG C for reacting for 12-48 hours in a heat preservation mode; cooling to room temperature and opening the airtight container; filtering out precipitates; cleaning the mixture for three times with absolute methanol and drying the mixture in a baking oven under the temperature of between 50 and 150 DEG C to prepare zirconium oxide hydrate with stable tetragonal phase rare-earth yttrium having uniform granularity and regular sphere; and forging the zirconium oxide hydrate under high temperature to prepare zirconium oxide powder with stable tetragonal phase rare-earth yttrium. The method has the advantages of being simple in process, easy for operation, low in energy consumption and the like, and can be applied to preparation of high-quality yttrium zirconium ceramic powder in a large scale.

Description

Technical field [0001] The present invention is a technology field of oxidation -oxidation ceramic materials, which involves a new methanol thermal synthesis method to prepare tetraonic spheres to stabilize oxidative pink powder. Background technique [0002] The dioxide dioxide has good thermal stability, chemical stability, excellent high temperature conductivity, high high temperature intensity and toughness, and good corrosion resistance, which has become a very important high -temperature structure ceramics, functional electronic ceramics and biological ceramics.Pure dioxide 能 generally cannot be used directly to make finished products, because it will change the structure when temperature changes. figure 1 Essence [0003] During the phase change, it is accompanied by 5 % to 8 %.Because of the three structures of existence, its thermal expansion is different.And other metal ions that are similar to calcium ion radius, commonly such as rare earth ions, calcium ions, etc., re...

Claims

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Application Information

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IPC IPC(8): C01G25/02C04B35/48C04B35/626
Inventor 唐群周雪珍李永绣刘志军陈萍华
Owner NANCHANG UNIV
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