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Preparation method of transparent yttria ceramics with high optical quality

A technology for optical quality, transparent ceramics, applied in the field of preparation of yttrium oxide transparent ceramics, can solve the problems of difficulty in preparing complex-shaped samples, affecting the optical quality of samples, easy introduction of calcium ions, etc., and achieves reduced grain size and low sintering temperature. , the effect of improving optical quality

Active Publication Date: 2011-04-20
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In summary, currently in Y 2 o 3 There are mainly problems in the following aspects in the field of transparent ceramic preparation: ① using different methods to synthesize Y 2 o 3 Powder, complex process, easy to introduce impurities; ② plaster mold is used in the molding process, easy to introduce calcium ions, affecting the optical quality of the sample; ③ needs to be sintered at a higher temperature or pressure, or add toxic or radioactive sintering aids In order to reduce the sintering temperature; ④ Vacuum hot pressing sintering is not easy to prepare samples with complex shapes; ⑤ Using hot isostatic pressing sintering, the equipment is expensive, the process is complicated, and the preparation cost is high

Method used

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  • Preparation method of transparent yttria ceramics with high optical quality

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Using commercial high-purity Y 2 o3 powder as raw material, Zr(NO 3 ) 4 ·3H 2 O is used as a sintering aid, and the addition amount is 0.1mol% (corresponding to ZrO 2 with Y 2 o 3 mole percent), two powders and ZrO 2 Put the balls and absolute ethanol together in a ball mill jar and mill for 3 hours, dry at 60°C for 24 hours, pass through a 200-mesh sieve, and calcinate at 1200°C for 3 hours to make Zr(NO 3 ) 4 ·3H 2 O is decomposed; then ammonium polyacrylate is used as a dispersant, and the addition amount is 0.05wt%, and the preparation of Y with a solid content of 30vol% 2 o 3 Water-based slurry; porous resin mold is used for grouting molding, and the green body is pre-fired at 600°C to remove organic additives; then sintered in a vacuum furnace at 1730°C, kept for 24h, and finally annealed at 1450°C for 10h in an air atmosphere. After polishing, the transmittance of the 1mm thick sample is 12.5% ​​at 1100nm, and the grain size is about 70μm. The specific...

Embodiment 2

[0019] Using commercial high-purity Y 2 o 3 Powder as raw material, ZrO 2 As a sintering aid, the amount added is 1.5mol% (corresponding to ZrO 2 with Y 2 o 3 mole percent), two powders and ZrO 2 Put the balls and absolute ethanol together in a ball mill tank and mix for 10 hours, dry at 60°C for 12 hours, pass through a 200-mesh sieve, and then calcinate at 600°C for 3 hours; then use ammonium polyacrylate as a dispersant, adding 0.5wt% , the preparation of Y with a solid content of 30vol% 2 o 3 Water-based slurry; porous resin mold is used for grouting molding, and the green body is pre-fired at 800°C to remove organic additives; then sintered in a vacuum furnace at 1860°C, kept for 3 hours, and finally annealed at 1520°C for 10 hours in an air atmosphere. After polishing, the transmittance of the 2mm thick sample is 81.3% at 1100nm, and the grain size is about 9μm. The specific process parameters and sample properties are listed in Table 1.

Embodiment 3

[0021] Using commercial high-purity Y 2 o 3 Powder as raw material, ZrOCl 2 ·8H 2 O is used as a sintering aid, and the addition amount is 15mol% (corresponding to ZrO 2 with Y 2 o 3 mole percent), two powders and ZrO 2 Put the balls and absolute ethanol together in a ball mill tank and mix for 12 hours, dry at 60°C for 24 hours, pass through a 200-mesh sieve, and then calcinate at 1100°C for 3 hours; then use ammonium polyacrylate as a dispersant, and add 1.5wt% , the preparation of Y with a solid content of 30vol% 2 o 3 Water-based slurry; porous alumina ceramic mold is used for grouting molding, and the green body is pre-fired at 600°C to remove organic additives; then sintered in a hydrogen furnace at 1960°C, kept for 8 hours, and finally annealed at 1520°C for 10 hours in an air atmosphere. After polishing, the transmittance of the 1mm thick sample is 81.2% at 1100nm, and the grain size is about 4μm. The specific process parameters and sample properties are liste...

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Abstract

The invention relates to a preparation method of transparent yttria ceramics with high optical quality, which belongs to the field of preparation of transparent ceramics. The preparation method comprises the following steps: adding anhydrous ethanol to the mixture of commercial high-purity Y2O3 powder serving as a raw material, ZrO2 serving as a sintering additive and zirconia balls serving as a grinding medium, and carrying out mixing and ball milling for 3-30 hours; adding a crylic acid salt dispersant in the powder to prepare water-based slurry of Y2O3, and adopting a porous resin mold or porous alumina ceramic mold to achieve slip casting; and finally, carrying out pressureless sintering in a vacuum or hydrogen atmosphere furnace to obtain the transparent yttria ceramics with high optical quality. The transmission rate of the Y2O3 transparent ceramics with thickness of 2mm is up to 81.3% at the wavelength of 1100nm. The invention has the advantages of simple process, low cost and no pollution, and is easy to control, and the transparent yttria ceramics with high optical quality can be prepared at lower sintering temperature in shorter holding time.

Description

technical field [0001] The invention relates to a method for preparing yttrium oxide transparent ceramics with high optical quality, belonging to the field of transparent ceramics preparation. Background technique [0002] In the preparation process of transparent ceramics, the performance of powder is an important factor to determine the sintering temperature and transparency of ceramics. Most researchers use different methods to synthesize Y 2 o 3 Powder to prepare Y 2 o 3 transparent ceramics, while the commercial Y 2 o 3 There are fewer reports on powder as raw material. For example, Akio Ikesue synthesized Y by thermal decomposition method 2 o 3 Powder, U.S. Patents 4,166,831 and 4,147,744 use liquid phase method to synthesize Y 2 o 3 For ultrafine powder, the process is more complicated, difficult to control, and it is easy to introduce impurities, which will finally affect the optical quality of transparent ceramics. [0003] Second, in terms of molding, Y ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/622C04B35/63C04B35/505
Inventor 靳玲玲周国红岛井骏藏章健王士维
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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