Freeze forming preparation 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: 2009-10-21
INST OF NUCLEAR PHYSICS & CHEM CHINA ACADEMY OF
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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 preparation process of ternary lithium ceramic microphere

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Dissolve 4g of polyvinyl alcohol completely in 96g of distilled water and let it stand for use; (2) Weigh 150g of the mixture of lithium carbonate and silicon dioxide according to the metering ratio, and add it to (1) the prepared polyvinyl alcohol solution , 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, and control the pressure at 40kPa, and the slurry from the nozzle Sprayed out and dropped into a container with liquid nitrogen at the bottom to form a precursor of ceramic microspheres; (4) Transfer the precursor of ceramic microspheres to an enamel tray, put it in a cold dryer and freeze-dry for 12 hours at a temperature of -30℃; (5) Put the dried microspheres obtained by the treatment in (4) into a high-temperature sintering furnace, and carry out program heating treatment, 120℃ for 24h, then 500℃ for 36h, and then heated to 1000℃ for 20h ...

Embodiment 2

[0034] (1) Dissolve 2g of polyvinyl alcohol in 98g of distilled water until it is transparent, and set it aside; (2) Weigh 150g of the mixture of lithium nitrate and silica according to the metering ratio, add it to (1), and grind on a planetary grinder. After hours, a stable suspension is obtained; (3) Pour the suspension into a container with a nozzle, turn on the pressure control system, and control the pressure at 40kPa. Small droplets are ejected from the nozzle and fall to the bottom with liquid nitrogen. In the container, the formed ceramic microsphere precursor; (4) Transfer the ceramic microsphere precursor to an enamel tray, and freeze-dry it in a freeze dryer for 8 hours at a temperature of -30°C; (5) Transfer the ceramic microsphere precursor to (4) The dried microspheres obtained by the treatment are put into a high-temperature sintering furnace, and the program is heated, 120°C for 24h, 400°C for 48h, then heated to 1050°C for 24h, and then heated to 1150°C for 4h. T...

Embodiment 3

[0036] (1) Dissolve 5g of polyvinyl alcohol in 95g of ethanol and let it stand for use; (2) Weigh 150g of a mixture of lithium carbonate and titanium dioxide according to the metering ratio, add it to (1), and grind on a planetary grinder for 2 hours, Obtain a stable suspension slurry; (3) Transfer the suspension slurry to a container with a nozzle, turn on the pressure control system, and control the pressure at 70kPa. The droplets are ejected from the nozzle mouth and become spherical due to surface tension. , Drip to the bottom of the ethylene glycol liquid nitrogen mixture to form a ceramic microsphere precursor; (4) Transfer the microsphere precursor to an enamel tray, put it in a freeze dryer and freeze-dry for 10 hours, the freezing temperature is- 20℃; (5) Put the dried microspheres obtained by the treatment of (4) into a high-temperature sintering furnace, and carry out program heating treatment, 150℃ for 24h, 700℃ for 18h, and then heated to 1100℃ for 12h, continue heati...

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Abstract

The invention provides a method for preparing ternary lithium ceramic microspheres by freeze molding, which is characterized in that: mixing the reactant raw materials of ternary lithium ceramic microspheres or ceramic powder with a polymer binder and a solvent, and mixing them in a ball mill Mix evenly to form a suspension slurry, and perform defoaming treatment. The slurry after defoaming treatment is transferred to the microsphere forming device, and the slurry is dropped into the low-temperature cooling medium through the microsphere forming device. During the movement of the droplets, microspheres are formed due to the surface tension, and the microspheres enter the low-temperature cooling medium. The spherical shape can be maintained by rapid cooling, and the ceramic microsphere precursor is formed by low-temperature vacuum drying in a freeze dryer. The microsphere green body undergoes multi-step program-controlled temperature-controlled heat treatment of calcination, calcination and sintering, and finally forms ternary lithium ceramic microspheres. Ceramic microspheres have good sphericity, controllable particle size, good particle size dispersion, high apparent density, high phase purity, and high breaking strength. The preparation method of the invention has the characteristics of simple process and low cost, and is easy to expand to large-scale production.

Description

Technical field [0001] The invention belongs to the technical field of preparation of porous ceramic microspheres, and specifically relates to a method for preparing ternary lithium ceramic microspheres by freezing and forming. Background technique [0002] In order to solve the world's energy shortage problem, various countries regard research as one of the effective ways to develop new energy and solve the energy crisis. The fuel tritium needed in thermonuclear fusion reactors is generally through 6 Li (n, α) T reaction to achieve. In order to realize the fuel cycle, the reactor must be “self-sustaining” of tritium. To this end, it is necessary to add a lithium-containing tritium breeder to the cladding, and use the neutrons produced by the core DT reaction to react with the lithium-containing materials in the breeder cladding. Tritium is produced to realize tritium proliferation. [0003] As a solid tritium ceramic material (tritium multiplier), lithium ceramic has the charact...

Claims

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Application Information

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Patent Type & Authority Patents(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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