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Erbium/yttrium-doped zirconium oxide transparent ceramic as well as preparation method and application thereof

A technology of yttrium-doped zirconia and transparent ceramics, applied in the field of erbium/yttrium-doped zirconia transparent ceramics and their preparation, can solve the problems of low transmittance, limitation, low visible light transmittance and the like

Active Publication Date: 2021-03-19
中国计量大学上虞高等研究院有限公司
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  • Abstract
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  • Claims
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Problems solved by technology

However, the existing YSZ transparent ceramics have low visible light transmittance, which limits the application of YSZ transparent ceramics in the fields of laser materials, lighting materials, and fluorescent sensing materials.
[0003] As early as the 1980s, Tsukuma et al. reported for the first time that by using TiO 2 As a sintering aid, YSZ transparent ceramics were prepared after sintering at 1630°C for 7 hours, hot isostatic pressing at 1500°C and 100 MPa for 0.5 hours, and finally annealed at 1200°C. The failure rate is not high (J.Mater.Sci.Lett.1986,5:1143-1144)
In 2012, Lei et al. prepared YSZ nanopowder by glycine-nitrate-high-energy ball milling method, and then sintered YSZ transparent ceramics at 1200-1350°C for 5 minutes by spark plasma sintering method, but it is transparent in the visible light range. Low failure rate (<30%) (Ceramics International 2012,38:23-28)
In 2019, Dash et al prepared YSZ transparent ceramics by hot isostatic pressing at 1100°C after spark plasma sintering at 1100°C, but its linear transmittance in the visible light wavelength range was lower than 50% (J.Eur.Ceram. Soc.2019,39:1428-1435)
However, the light transmittance of YSZ transparent ceramics prepared by this method is still difficult to meet the requirements for the light transmittance of transparent ceramics in the fields of laser materials, lighting materials, and fluorescent sensing materials.

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  • Erbium/yttrium-doped zirconium oxide transparent ceramic as well as preparation method and application thereof
  • Erbium/yttrium-doped zirconium oxide transparent ceramic as well as preparation method and application thereof
  • Erbium/yttrium-doped zirconium oxide transparent ceramic as well as preparation method and application thereof

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[0029] The invention provides a preparation method of erbium / yttrium doped zirconia transparent ceramics, comprising the following steps:

[0030] Change the chemical composition to (Zr 1-x-y Er x Y y )O 2 The nanorods are cold isostatically pressed to obtain a green body; wherein 0.005≤x≤0.01, 0.06≤y≤0.09;

[0031] The green body is sintered to obtain erbium / yttrium doped zirconia transparent ceramics, the sintering temperature is 500-600° C., and the pressure is 4-6 GPa.

[0032] In the present invention, the chemical composition is (Zr 1-x-y Er x Y y )O 2 The nanorods are formed by cold isostatic pressing to obtain a green body; wherein 0.005≤x≤0.01, 0.06≤y≤0.09. In the present invention, the x may be specifically 0.005 or 0.01; the y may be specifically 0.06 or 0.09.

[0033] In the present invention, the chemical composition is (Zr 1-x-y Er x Y y )O 2 The preparation method of the nanorod preferably comprises the following steps:

[0034] ZrOCl 2 ·8H 2 O, st...

Embodiment 1

[0075] 2.9168g ZrOCl 2 ·8H 2 O was dissolved in 90.51 mL of distilled water to obtain a zirconium oxychloride solution with a molar concentration of 0.1 mol / L;

[0076] Dissolve 20g of NaOH in 1000mL of distilled water to obtain a NaOH solution with a molar concentration of 0.5mol / L;

[0077] Drop 18.1mL of NaOH solution into 90.51mL of zirconium oxychloride solution at a rate of 60 drops / min, stir at a speed of 400r / min for 30min, then transfer it to a polytetrafluoroethylene-lined autoclave, and heat it at 160°C. Thermal reaction for 3 hours; naturally cool the hydrothermal reaction product to room temperature and then centrifuge to remove the supernatant; disperse the centrifuged precipitate in distilled water and centrifuge at a speed of 5000r / min for 8 min; remove the distilled water, and disperse the centrifuged precipitate in In ethanol, centrifuge at a rotating speed of 5000r / min for 8min; repeat the above-mentioned cleaning and centrifugal operation 5 times, remove ...

Embodiment 2

[0083] 2.9974g ZrOCl 2 ·8H 2 O was dissolved in 93.02 mL of distilled water to obtain a zirconium oxychloride solution with a molar concentration of 0.1 mol / L;

[0084] Dissolve 20g of NaOH in 1000mL of distilled water to obtain a NaOH solution with a molar concentration of 0.5mol / L;

[0085] Drop 23.25mL of NaOH solution into 93.02mL of zirconium oxychloride solution at a rate of 50 drops / min. After stirring for 30 minutes at a speed of 500r / min, transfer it to a polytetrafluoroethylene-lined autoclave. Thermal reaction for 5 hours; naturally cool the hydrothermal reaction product to room temperature and then centrifuge to remove the supernatant; disperse the centrifuged precipitate in distilled water and centrifuge at a speed of 6000r / min for 6 min; remove the distilled water, and disperse the centrifuged precipitate in In ethanol, centrifuge at a speed of 6000r / min for 6min; repeat the above-mentioned cleaning and centrifugation operations 5 times, remove the solvent, and...

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Abstract

The invention belongs to the technical field of transparent ceramics, and particularly relates to an erbium / yttrium-doped zirconium oxide transparent ceramic as well as a preparation method and application thereof. The invention provides a preparation method of erbium / yttrium-doped zirconium oxide transparent ceramic, which comprises the following steps: carrying out isostatic cool pressing on a nanorod with the chemical composition of (Zr1-x-yErxYy)O2 to obtain a biscuit, wherein x is greater than or equal to 0.005 and less than or equal to 0.01, and y is greater than or equal to 0.06 and less than or equal to 0.09; and sintering the biscuit to obtain the erbium / yttrium doped zirconium oxide transparent ceramic, wherein the sintering temperature ranges from 500 DEG C to 600 DEG C, and thepressure ranges from 4 GPa to 6 GPa. In the invention, the compactness of the erbium / yttrium-doped zirconium oxide transparent ceramic can be improved through sintering under the conditions of mediumtemperature and high pressure, and the erbium / yttrium-doped zirconium oxide transparent ceramic with high optical transmittance in a visible light wave band and a near-infrared light wave band is obtained.

Description

technical field [0001] The invention belongs to the technical field of transparent ceramics, and in particular relates to an erbium / yttrium doped zirconia transparent ceramic and a preparation method and application thereof. Background technique [0002] Yttrium oxide (Y 2 o 3 ) as a stabilizer for cubic ZrO 2 Transparent ceramics (YSZ) are widely used due to their unique optical properties. For example: due to the high refractive index of YSZ transparent ceramics, the use of optical lenses can effectively reduce the focal length of the lens and meet the development requirements of the miniaturization of modern optical devices; at the same time, YSZ transparent ceramics have a low absorption rate for the mid-infrared band , and has high hardness, which can be used for infrared window materials; in addition, YSZ transparent ceramics doped with rare earth elements have lower phonon energy (about 430-500cm -1 ) and not easy to absorb moisture, so adding rare earth ions (Er ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/488C04B35/622C04B35/626C09K11/67
CPCC04B35/488C04B35/622C04B35/626C04B35/62645C04B35/6268C09K11/7769C04B2235/3225C04B2235/3224C04B2235/5296C04B2235/5276C04B2235/5454C04B2235/5445C04B2235/656C04B2235/9653C04B2235/96
Inventor 雷若姗王焕平李明辉田颖徐时清杨清华华有杰黄飞飞
Owner 中国计量大学上虞高等研究院有限公司