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Method for preparing MgAlON transparent ceramic in pressureless sintering way

A technology of transparent ceramics and absolute ethanol, which is applied in the field of preparation of MgAlON transparent ceramics, can solve the problems of limiting the shape and size of sintered products, having no optical properties of materials, and difficult control of components, so as to achieve lower sintering temperature, uniform particle size, The effect of rapid reaction process

Active Publication Date: 2010-09-01
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2005, Zhang Houxing et al. ("Research on ultra-fast synthesis of MgAlON spinel by spark plasma sintering", Journal of Ceramics, 26(1), 2005, 13-16) also reported that under pressure sintering conditions at 1600 ° C for 5 min A single-phase dense MgAlON ceramic bulk can be obtained, but there are no reports on the optical properties of the prepared materials
The patent pointed out that the two-step method is easy to obtain a single phase, improves the density of ceramics, and overcomes the disadvantages of simultaneous densification of the reaction, complicated process, and difficult control of components in the one-step method.
However, two-step sintering often relies on hot pressing or hot isostatic pressing, which greatly limits the shape and size of sintered products, and is not suitable for producing large-sized and complex-shaped products. Therefore, after obtaining high-purity transparent ceramic powder, use The pressureless sintering method to prepare transparent ceramics shows incomparable advantages
At present, there is no report on the preparation of MgAlON transparent ceramics by two-step method.

Method used

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  • Method for preparing MgAlON transparent ceramic in pressureless sintering way
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  • Method for preparing MgAlON transparent ceramic in pressureless sintering way

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Effect test

Embodiment 1

[0045] The pressureless sintering preparation method of MgAlON transparent ceramics, it comprises the steps:

[0046] 1) Preparation of MgAlON transparent ceramic powder:

[0047] ①Weigh 88.21g of α-alumina powder, 3.79g of aluminum nitride powder and 8g of magnesium oxide powder, put them into a mixing bottle and mix to obtain mixed powder A; 1 Add alumina balls, add 200mL of absolute ethanol, and roller mill for 24 hours to obtain slurry A;

[0048] ②Dry the slurry A (dry in vacuum at 50°C) to obtain the mixture A;

[0049] ③ Pass the dried mixture A through a 100-mesh sieve, take 3g and put it into a graphite crucible coated with boron nitride on the inner wall. The crucible is placed in a graphite reactor, and the graphite reactor is placed in a high-current reaction synthesis device. 0.05Mpa nitrogen was introduced into the synthesis device as a protective gas; a large current was directly applied to the graphite reactor, heated to 1700°C at a heating rate of 100°C, kep...

Embodiment 2

[0063] The pressureless sintering preparation method of MgAlON transparent ceramics, it comprises the steps:

[0064] 1) Preparation of MgAlON transparent ceramic powder:

[0065] ① Weigh 88.77g of α-alumina powder, 7.23g of aluminum nitride powder and 4g of magnesium oxide powder, put them into a mixing bottle and mix to obtain mixed powder A; 1 Add alumina balls, add 200mL of absolute ethanol, and roller mill for 24 hours to obtain slurry A;

[0066] ②Dry the slurry A (dry in vacuum at 50°C) to obtain the mixture A;

[0067] ③Put the dried mixture A through a 100-mesh sieve, take 3g and put it into a graphite crucible coated with boron nitride on the inner wall. The crucible is placed in a graphite reactor, and the graphite reactor is placed in a high-current reaction synthesis device. 0.03Mpa nitrogen was introduced into the synthesis device as a protective gas; a large current was directly applied to the graphite reactor, heated to 1700°C at a heating rate of 200°C, kept...

Embodiment 3

[0081] The pressureless sintering preparation method of MgAlON transparent ceramics, it comprises the steps:

[0082] 1) Preparation of MgAlON transparent ceramic powder:

[0083] ① Measure 84.36g of α-alumina powder, 7.64g of aluminum nitride powder and 8g of magnesium oxide powder, put them into a mixing bottle and mix to obtain mixed powder A; 1 Add alumina balls, add 250mL of absolute ethanol, and roller mill for 24 hours to obtain slurry A;

[0084] ②Dry the slurry A (dry in vacuum at 50°C) to obtain the mixture A;

[0085] ③ Pass the dried mixture A through a 100-mesh sieve, take 3g and put it into a graphite crucible coated with boron nitride on the inner wall. The crucible is placed in a graphite reactor, and the graphite reactor is placed in a high-current reaction synthesis device. 0.05Mpa nitrogen was introduced into the synthesis device as a protective gas; a large current was directly applied to the graphite reactor, heated to 1650°C at a heating rate of 300°C, ...

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Abstract

The invention relates to a method for preparing MgAlON transparent ceramic, in particular to a method for preparing MgAlON transparent ceramic in a pressureless sintering way. The method is characterized by comprising the following steps of: (1) preparing MgAlON transparent ceramic powder; (2) mixing 95 to 99 percent by weight of MgAlON transparent ceramic powder and 0.1 to 5 percent by weight of fluoride, dispersing in absolute ethanol, and ball-milling to obtain slurry B; (3) drying the slurry B to obtain a mixture B; (4) carrying out pressing molding on the mixture B under the normal temperature by adopting axial mould pressing and then carrying out cold isostatic pressing to obtain a ceramic bisque; and (5) sintering to obtain the MgAlON transparent ceramic. The MgAlON transparent ceramic can obtain high-density (more than 99.5 percent) and excellent optical property without the processes of hot isostatic sintering, and the like; the optimal linear transmissivity of a flat material with the thickness of 2 mm within the wavelength range of 0.25 to 6mu m is more than 70 percent; and the material can be widely applied to various windows, shades, transparent safeguards, lamp tubes, optical devices, and the like.

Description

technical field [0001] The invention relates to a preparation method of MgAlON transparent ceramics, belonging to the field of preparation of transparent ceramic materials. Background technique [0002] In 1976, Jack K.H. first reported the crystal phase diagram of MgAlON, and then Weiss S, Sun Weiying, Willems HX, and Granon A studied the synthesis and phase relationship of MgAlON ceramics. MgAlON and MgAl 2 o 4 It has the same crystal structure and similar lattice constant as AlON, and has more stable thermodynamic properties than AlON. Because of its excellent mechanical properties, dielectric properties, physical and chemical stability, it shows good application prospects in the fields of high-temperature structural ceramics and refractory materials. In addition, high-purity, high-density MgAlON ceramics have excellent isotropic optical transmission properties from ultraviolet to mid-infrared light waves, making them widely used in high-temperature windows, fairings, ...

Claims

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Application Information

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IPC IPC(8): C04B35/58C04B35/622
Inventor 王皓商青琳王为民傅正义王玉成张清杰
Owner WUHAN UNIV OF TECH
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