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Method for preparing aluminum oxynitride transparent ceramic

A technology of transparent ceramics and aluminum oxynitride, which is applied in the field of preparation of aluminum oxynitride transparent ceramics, and can solve problems such as low transmittance, high AlON phase synthesis temperature, and blackened sample color

Inactive Publication Date: 2017-11-14
SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Kaplan et al. tried to use SPS sintering to manufacture AlON transparent ceramics (Journal of the European Ceramic Society 35(2015) 3255–3262), but the color of the obtained samples was black and the transmittance was very low
The reason is that the synthesis temperature of the AlON phase is higher, and the carburization caused by the use of graphite molds in the SPS sintering process

Method used

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  • Method for preparing aluminum oxynitride transparent ceramic
  • Method for preparing aluminum oxynitride transparent ceramic
  • Method for preparing aluminum oxynitride transparent ceramic

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1) Powder mixing: high-purity alumina and aluminum nitride are weighed at a mass ratio of 70:30, and sintering aids MgO and Y 2 o 3 The added amounts of are respectively 0.04wt% and 0.08wt%. The mixed powder with a mass of 80g was mixed with 60ml of absolute ethanol and 300g of high-purity alumina balls and ball milled at a speed of 250 rpm. The milled powder was dried at 70°C for 8 hours, and then passed through a 200-mesh sieve;

[0033] 2) Pretreatment: put the mixed powder sieved in step 1) in a muffle furnace for pre-calcination treatment to remove organic matter: the pre-calcination temperature is 800°C, and the holding time is 3h;

[0034] 3) Abrasive tooling: Put 5g of decarbonized powder in a Φ20 graphite mold. Before loading, a layer of graphite paper should be placed between the indenter and the powder and the inner wall of the mold, and the inner wall of the mold needs to be coated with a layer of boron nitride, which is convenient for demoulding after sin...

Embodiment 2

[0040] 1) with step 1) in embodiment 1);

[0041] 2) with step 2) in embodiment 1;

[0042] 3) with step 3) in embodiment 1;

[0043] 4) Spark plasma sintering

[0044] Place the assembled mold in an SPS sintering furnace for rapid sintering under the following conditions: the pressure is 50MPa, the temperature is 1450°C, and the temperature is kept for 5 minutes to obtain a dense AlON ceramic phase.

[0045] 5) Pressureless sintering

[0046] Put the AlON ceramics obtained in step (4) into a pressureless sintering furnace for pressureless sintering, the condition is nitrogen atmosphere, the sintering temperature is 1700 ° C, and the temperature is kept for 3 hours to remove the carbon infiltrated in the SPS rapid sintering, and further improve the Density increases the transmittance of AlON ceramics.

[0047] 6) The ceramic sample sintered in step 5) is processed and polished to 2mm with a surface grinder and diamond grinding paste.

Embodiment 3

[0049] 1) Powder mixing: high-purity alumina and aluminum nitride are weighed at a mass ratio of 73:27, sintering aids MgO and Y 2 o 3 The addition amounts of are respectively 0.04wt% and 0.06wt%. The mixed powder with a mass of 80g was mixed with 60ml of absolute ethanol and 300g of high-purity alumina balls for ball milling, the milling speed was 250rpm, and the milled powder was dried at 70°C for 8 hours, and then passed through a 200-mesh sieve;

[0050] 2) with step 2) in embodiment 1;

[0051] 3) with step 3) in embodiment 1;

[0052] 4) Spark plasma sintering

[0053] Place the assembled mold in an SPS sintering furnace for rapid sintering under the following conditions: the pressure is 100MPa, the temperature is 1700°C, and the temperature is kept for 5 minutes to obtain a dense AlON ceramic phase.

[0054] 5) Pressureless sintering

[0055] Put the AlON ceramics obtained in step (4) into a pressureless sintering furnace for pressureless sintering, the conditions ...

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Abstract

The invention discloses a method for preparing aluminum oxynitride transparent ceramic. The method comprises the following steps: performing ball-milling mixing of aluminum oxide powder, aluminum nitride powder and a sintering aid, and then drying and sieving to obtain mixed powder; putting the mixed powder in a graphite mould; spark plasma sintering: putting the prepared mould in a SPS sintering furnace and sintering quickly; putting AlON ceramic in a graphite sintering furnace; preserving heat for 2-4 hours at sintering temperature of 1,650-1,800 DEG C in a nitrogen atmosphere; removing carbon permeating in SPS to further improve the transmittance of AlON. According to the method disclosed by the invention, AlON transparent ceramic with high transmittance is obtained when the sintering temperature is lower than that of a common pressureless sintering technology.

Description

technical field [0001] The invention relates to the technical field of preparation of aluminum oxynitride transparent ceramics, in particular to a method for preparing aluminum oxynitride transparent ceramics by combining spark plasma sintering technology with pressureless sintering technology. 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 was confirmed by later studies. It is a transparent polycrystalline ceramic with strength and hardness as high as 380MPa and 17.7GPa, second only to single crystal sapphire, and has good optical transmittance from near ultraviolet (0.2μm) to mid-infrared (6.0μm), so It has potential application value in fields such as high-temperature infrared windows, mobile computer screens, and transparent windows of POS machines. [0003] Usually, the preparation method of AlON transpa...

Claims

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Application Information

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IPC IPC(8): C04B35/581C04B35/64
CPCC04B35/581C04B35/64C04B2235/3206C04B2235/3217C04B2235/3225C04B2235/3865C04B2235/5436C04B2235/658C04B2235/661C04B2235/666C04B2235/9653
Inventor 张龙齐申毛小建许杨阳胡旭谢俊喜
Owner SHANGHAI INST OF OPTICS & FINE MECHANICS CHINESE ACAD OF SCI
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