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Freeze forming prepn process of ternary lithium ceramic microphere

A technology of ceramic microspheres and freeze molding, which is applied in ceramic products, applications, household appliances, etc., can solve the problems of insufficient internal pore structure, difficulty in high density of lithium ceramic microspheres, and poor sphericity of ceramic microspheres. Controllable particle size of microspheres, good internal pore structure, and low cost

Inactive Publication Date: 2007-11-07
INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the melt-spray method can produce high-density lithium ceramic microspheres, but the defect of this method is that it uses an expensive platinum-rhodium alloy furnace
When using the traditional wet method to prepare lithium ceramic microspheres, since the gel solid content of the microsphere precursor is difficult to exceed 50%, the density of the final formed lithium ceramic microspheres is difficult to be higher than 90% T.D. (theoretical density)
[0005] Most of the existing ceramic microsphere preparation methods need to pre-prepare the ceramic powder of the ternary lithium compound, and then generate ceramic microspheres. The sphericity of the ceramic microspheres is not good, the internal pore structure is not rich enough, and the particle size of the microspheres is difficult to control. Poor particle size dispersion

Method used

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  • Freeze forming prepn process of ternary lithium ceramic microphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Dissolve 4g of polyvinyl alcohol in 96g of distilled water completely, and let it stand for use; (2) Weigh 150g of lithium carbonate and silicon dioxide mixture according to the metering ratio, and add it into the prepared polyvinyl alcohol solution of (1) , Grind on a planetary grinder for 3 hours to form a stable suspension slurry; (3) transfer the suspension slurry to a container with a nozzle, open the pressure control system, the pressure is controlled at 40kPa, and the slurry flows from the nozzle Squirt out and drop into a container with liquid nitrogen at the bottom to form a ceramic microsphere precursor; (4) transfer the ceramic microsphere precursor to an enamel plate, put it into a freeze dryer and freeze-dry it for 12 hours at a temperature of -30°C; (5) Put the dried microspheres obtained from (4) into a high-temperature sintering furnace, and perform programmed heating treatment, 120°C for 24 hours, then 500°C for 36 hours, and then heat up to 1000°C f...

Embodiment 2

[0034] (1) Dissolve 2g of polyvinyl alcohol in 98g of distilled water until transparent and ready to use; (2) Weigh 150g of lithium nitrate and silicon dioxide mixture according to the metering ratio, add it to (1), and grind it on a planetary grinder for 4 (3) the suspension is poured into a container with a nozzle, the pressure control system is opened, the pressure is controlled at 40kPa, the droplets are ejected from the nozzle, and drop to the bottom of the container equipped with liquid nitrogen. In the container, the formed ceramic microsphere precursor; (4) transfer the ceramic microsphere precursor to an enamel plate, put it into a freeze dryer and freeze-dry it for 8 hours at a temperature of -30°C; The dried microspheres obtained from the treatment were placed in a high-temperature sintering furnace, and subjected to programmed heating treatment, treated at 120°C for 24 hours, then at 400°C for 48 hours, then raised to 1050°C for 24 hours, and continued to heat up to...

Embodiment 3

[0036] (1) Dissolving 5g polyvinyl alcohol in 95g ethanol, leave standstill for use; (2) Weigh 150g lithium carbonate and titanium dioxide mixture according to the metering ratio, join in (1), grind 2 hours on planetary grinder, Obtain a stable suspension slurry; (3) transfer the suspension slurry to a container with a nozzle, open the pressure control system, the pressure is controlled at 70kPa, the droplets are ejected from the nozzle mouth, and become spherical due to surface tension , dripped into the ethylene glycol liquid nitrogen mixture at the bottom to form a ceramic microsphere precursor; (4) transfer the microsphere precursor to an enamel plate, put it into a freeze dryer and freeze-dry it for 10 hours, and the freezing temperature is - 20°C; (5) Put the dried microspheres obtained through (4) into a high-temperature sintering furnace, and perform programmed heating treatment, 150°C for 24 hours, 700°C for 18 hours, and then heat up to 1100°C for 12 hours, and contin...

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Abstract

The freeze forming preparation process of ternary lithium ceramic microsphere includes the following steps: mixing the material for ternary lithium ceramic microsphere, high molecular adhesive and solvent, mixing in a ball mill to form suspension slurry and defoaming; dropping the slurry into cooling medium to form microsphere in a microsphere forming unit, and low temperature vacuum drying in a freezing drier to form ceramic microsphere precursor; roasting, calcining and sintering; and programmed heat treatment to obtain ternary lithium ceramic microsphere. The ternary lithium ceramic microsphere has high sphericity, controllable size, high size dispersivity, high apparent density, high phase purity, high strength and other features.

Description

technical field [0001] The invention belongs to the technical field of preparation of porous ceramic microspheres, and in particular relates to a method for preparing ternary lithium ceramic microspheres by freeze molding. Background technique [0002] In order to solve the world's energy shortage problem, countries regard research as one of the effective ways to develop new energy and solve the energy crisis. The fuel tritium needed in the thermonuclear fusion reactor is generally passed through 6 Li(n,α)T reaction to achieve. In order to realize the fuel cycle, the reactor must achieve the "self-sustainability" of tritium. For this reason, it is necessary to add a lithium-containing tritium breeder to the cladding, and use the neutrons produced by the D-T reaction in the core to react with the lithium-containing material in the breeding cladding. Tritium multiplication is achieved by generating tritium. [0003] As a solid tritium-producing ceramic material (tritium mul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B38/00C04B35/634C04B35/64C04B35/622C04B35/10C04B35/14C04B35/16C04B35/462C04B35/48C04B35/01
Inventor 陈晓军王和义高小铃黄玮罗阳明肖成建古梅
Owner INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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