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Internal gelation method for preparation of ceramic microspheres with glue solution stable at room temperature

A technology for ceramic microspheres and glue solution, which is applied in the field of internal gelation for preparing ceramic microspheres, can solve the problems that the inner gelation process needs to be deepened, the glue solution is unstable, and the large-scale application of the inner gelation process is restricted, and the realization of Mass production, uniform size, good sphericity effect

Active Publication Date: 2017-02-22
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the past few decades, the internal gelation process has made great progress, but the problem that the gel solution in the internal gelation process is unstable at room temperature or even low temperature has not been well solved, and this problem has always been One of the factors restricting the large-scale application of the internal gelation process
[0004] Therefore, the research on the inner gel process still needs to be deepened.

Method used

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  • Internal gelation method for preparation of ceramic microspheres with glue solution stable at room temperature
  • Internal gelation method for preparation of ceramic microspheres with glue solution stable at room temperature
  • Internal gelation method for preparation of ceramic microspheres with glue solution stable at room temperature

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070]ZrO 2 Preparation of ceramic microspheres:

[0071] (1) Prepare a mixed solution containing 3mol / L hexamethylenetetramine (HMTA) and 0.7mol / L urea (Urea) at room temperature;

[0072] (2) Configuration containing 1.6mol / L of ZrO(NO 3 ) 2 and 0.14mol / L of Y(NO 3 ) 3 The mixed solution, and concentrated nitric acid is added to the mixed solution to make the final hydrogen ion concentration be 1.35mol / L;

[0073] (3) The above two solutions were left to stand at room temperature for 1h, then the solution containing HMTA and Urea was added to the solution containing Zr and Y, and fully mixed; the prepared glue solution was stored at room temperature for 1h before use Dispersed in gelling. The concentration of metal ions in the final glue is about 0.8-1.1mol / L, the molar ratio of HMTA to metal ions is 1.1-1.3, the molar ratio of urea to metal ions is 0.3-0.65, and the pH value is between 1-2. between;

[0074] (4) Disperse the glue solution into the silicone oil at 85...

Embodiment 2

[0081] ZrC-ZrO 2 Preparation of composite ceramic microspheres

[0082] (1) Prepare a mixed solution containing 3mol / L hexamethylenetetramine (HMTA) and 0.7mol / L urea (Urea) at room temperature,

[0083] (2) Configuration containing 1.6mol / L of ZrO(NO 3 ) 2 and 0.14mol / L of Y(NO 3 ) 3 The mixed solution, and concentrated nitric acid is added to the mixed solution to make the final hydrogen ion concentration be 1.35mol / L;

[0084] (3) The above two solutions were left to stand at room temperature for 0.5-1 h, then the solution containing HMTA and Urea was added to the solution containing Zr and Y, and mixed well. Add carbon powder to the above mixture and add Triton X-100 to make the dispersion of carbon powder in the mixture uniform and stable. The prepared glue solution was stored at room temperature for 0.5-1 hour, and then ultrasonically dispersed for 5 minutes for gelation and dispersion. The concentration of metal ions in the final glue solution is about 0.8-1.1mol...

Embodiment 3

[0092] al 2 o 3 Preparation of Ceramic Microspheres

[0093] (1) Prepare a mixed solution containing 3.2mol / L hexamethylenetetramine (HMTA) and 1mol / L urea (Urea) at room temperature;

[0094] (2) Configuration containing 1.6mol / L Al(NO 3 ) 3 solution, and add an appropriate amount of concentrated ammonia water to the mixed solution to make the pH of the mixed solution 1.5 to 2.5;

[0095] (3) Put the above two solutions at room temperature for 1h, then add the solution containing HMTA and Urea to the solution containing Al, and mix well; the prepared glue solution is stored at room temperature for 1h and then used for glue Coagulation dispersed. The concentration of metal ions in the final glue solution is about 0.8-1.1mol / L, the molar ratio of HMTA to metal ions is 1.5-2, the molar ratio of urea to metal ions is 0.3-0.65, and the pH value is between 4-5. between;

[0096] (4) Disperse the glue solution into the silicone oil at 85-90°C using the bench of the internal g...

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Abstract

The invention provides an internal gelation method for ceramic microspheres capable of keeping a gel solution steady at normal temperature. The method comprises the following steps: (1) at room temperature, mixing metal salt, hexamethylene tetramine and urea together to obtain a gel solution; (2) dispersing the gel solution into hot silicone oil to obtain gel beads; (3) ageing the gel beads in the silicone oil to obtain aged gel beads; (4) washing the aged gel beads to obtain washed gel beads; (5) drying the washed gel beads to obtain dry gel beads; and (6) sintering the dry gel beads to obtain the ceramic microspheres. With the method provided by the invention, preparation and storage of the gel solution at normal temperature during the internal gelation process can be implemented.

Description

technical field [0001] The invention belongs to the field of ceramic forming technology, and in particular relates to a method for preparing ceramic microspheres by an internal gelling process, and more specifically, relates to an internal gelation method for preparing ceramic microspheres with a glue solution stable at room temperature. Background technique [0002] The internal gelation process is an advanced technology for preparing ceramic microspheres, which originated from the KEMA laboratory in the Netherlands. The internal gelation process is widely used in high-temperature gas-cooled reactor fuel cores such as UO 2 , PuO 2 and the preparation of the inert matrix (IMF). The basic principle of preparing ceramic microspheres in the internal gelation process is to drop the glue solution containing metal salts of hexamethylenetetramine and urea (such as zirconium, uranium, titanium, aluminum and other metals) into a hot organic medium. In hot organic medium, hexamethy...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C04B35/624
Inventor 马景陶高勇赵兴宇郝少昌邓长生刘兵
Owner TSINGHUA UNIV
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