Method for preparing aluminum oxynitride transparent ceramic through gel casting

A technology of gel injection molding and aluminum oxynitride, which is applied in the field of preparation of transparent ceramics, can solve the problems of oxygen inhibition, toxic monomers, limited application of gel injection molding, etc., and achieves low cost, simple operation, and molding. Excellent effect

Active Publication Date: 2014-02-05
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are many problems in the previous gel system, such as oxygen inhibition, toxic monomers, and the need to add a variety of organic additives, etc., which limit the application of gel injection molding

Method used

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  • Method for preparing aluminum oxynitride transparent ceramic through gel casting
  • Method for preparing aluminum oxynitride transparent ceramic through gel casting
  • Method for preparing aluminum oxynitride transparent ceramic through gel casting

Examples

Experimental program
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preparation example Construction

[0029] (1) Preparation of aluminum oxynitride powder

[0030] Aluminum oxynitride powder can be prepared by solid phase reaction method, aluminothermic reduction method, carbothermal reduction method and / or combined method by ball milling and sieving or by spray granulation to obtain aluminum oxynitride powder with high uniform particles. Taking the carbothermal reduction method as an example, refer to the method disclosed by the inventor in Chinese patent CN101928150A.

[0031] (2) Anti-hydration treatment of aluminum oxynitride powder

[0032] Before the anti-hydration treatment, the synthesized AlON powder, sintering aid, and absolute ethanol can be mixed for ball milling, grinding, and sieving (for example, through a 200-mesh sieve). For example, a planetary ball mill can be used, with alumina balls as the ball milling medium, the ball milling speed is 100-300 rpm, and the ball milling time is more than 12 hours, preferably 20-30 hours. Sintering aid can use Y 2 o 3 an...

Embodiment 1

[0043] 1) Synthesis of AlON powder: high-purity alumina and carbon black are uniformly mixed at a mass ratio of 95:5, and then kept at 1550°C for one hour in a nitrogen atmosphere, and then kept at 1750°C for 2 hours, and finally single-phase AlON is obtained Powder;

[0044] 2) Mix 20g of AlON powder synthesized with 30ml of absolute ethanol and 150g of high-purity alumina balls and ball mill for 20h at a ball milling speed of 250rpm, dry the milled AlON powder at 60°C for 24h, and then pass through a 200-mesh sieve;

[0045] 3) Take 100g of AlON powder sieved in step 2), add 0.1g of dispersant polyacrylic acid and 50ml of absolute ethanol, mix ball mill for 1 hour, add 2g of isocyanate, and filter out the slurry after ball milling for 10 minutes, add Siya to the slurry Ethylpentamine 1.3g and stirred for 2h, then dried at 50°C for 20h and passed through a 200-mesh sieve;

[0046] 4) Mix 50g of AlON powder after anti-hydration treatment in step 3, 100g of water, and 0.5g of ...

Embodiment 2

[0050] 1) Same as step 1 in Example 1);

[0051] 2) Same as step 2 in Example 1);

[0052] 3) Same as step 3 in Example 1);

[0053] 4) Mix 60g of AlON powder after anti-hydration treatment in step 3, 100g of water, and 0.5g of water-soluble isobutylene polymer by ball milling for 2 hours. The obtained water-based slurry is first degassed under vacuum for 20 minutes, and then Pour into the mold. Cured at 40°C for 2 hours. After demoulding, the ceramic green body is first dried at a temperature of 40-50°C for 48 hours; then pre-fired in a muffle furnace to remove organic matter: the heating rate is 5°C / min, and the pre-fired temperature is 500°C , holding time is 8h;

[0054] 5) Sinter the pre-fired ceramic green body in step 4) in a nitrogen atmosphere furnace at a sintering temperature of 1900°C for 20 hours;

[0055] 6) The ceramic sample sintered in step 5) is processed and polished to 2 mm with a surface grinder and diamond grinding paste, and the sample transmittance...

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Abstract

The invention relates to a method for preparing an aluminum oxynitride transparent ceramic through gel casting. The method comprises the following steps: (1) ball-milling and mixing aluminum oxynitride powder, a dispersing agent and absolute ethyl alcohol, adding a hydration-resisting agent, performing hydration-resisting treatment, drying and sieving to obtain aluminum oxynitride powder processed by the hydration-resisting treatment, wherein the mass ratio of the aluminum oxynitride powder, the dispersing agent and the hydration-resisting agent is 100:(0.1-5):(0.1-5); (2) mixing the aluminum oxynitride powder processed by the hydration-resisting treatment, a water-soluble isobutene polymer and water to obtain a water-base slurry, wherein the mass ratio of the aluminum oxynitride powder processed by the hydration-resisting treatment, the water-soluble isobutene polymer and the water is (10-80):(0.1-5):100; (3) performing vacuum degassing on the base-base slurry, injecting the degassed base-base slurry into a mold, performing self-gel curing to obtain a biscuit, and drying the biscuit; (4) presintering the dried biscuit, and performing pressure-less sintering to obtain the aluminum oxynitride transparent ceramic.

Description

technical field [0001] The invention relates to a new method for preparing aluminum oxynitride (AlON) transparent ceramics by gel injection molding, and belongs to the technical field of transparent ceramics preparation. Background technique [0002] In 1959, Yamaguchi and Yanagida reported for the first time that cubic spinel aluminum oxynitride (AlON) is Al 2 o 3 - An important single phase that may exist in the AlN system, and its existence was confirmed by many studies in the following decades. It is a transparent polycrystalline ceramic, its strength and hardness are as high as 380MPa and 17.7GPa, second only to sapphire single crystal, and it has a good optical transmittance from near ultraviolet (0.2μm) to mid-infrared (5.0μm). One of the most important transparent armor materials at present. In addition, it also has good high temperature resistance, thermal shock resistance and corrosion resistance, so it is increasingly widely used in the fields of missile window...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/58C04B35/622
Inventor 王军张芳陈凤张海龙田润张昭章健王士维
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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