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Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics

A technology of yttrium aluminum garnet and transparent ceramics, which is applied in the preparation of tetravalent chromium-doped yttrium aluminum garnet transparent ceramics, and in the field of Cr4+:YAG transparent ceramics, which can solve the problem of inability to use laser output or Q-switching, and the conversion rate of tetravalent chromium Low, low transmittance and other problems, to achieve the effect of reasonable grain distribution, high density and high transmittance

Active Publication Date: 2015-04-29
河南和光光电有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Cr reported in the above literature 4+ : YAG transparent ceramics generally have problems such as low conversion rate of tetravalent chromium or low transmittance, which is far from reaching Cr 4+ : The optical quality of YAG single crystal cannot be used to achieve laser output or Q-switching. The main reason is that no suitable sintering aid system is selected.

Method used

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  • Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics
  • Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics
  • Preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics

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Embodiment 1

[0030] Composition as in Table 1 1 # Shown, specific preparation method comprises the following steps:

[0031] ① Weigh the raw materials according to the composition in Table 1. First, put the oxide raw material powder into a high-purity alumina ball mill tank, add sintering aids, charge balance agents, and absolute ethanol to prepare the slurry; ball mill on a planetary ball mill Mix for 10 hours, and the rotating speed is 160r / min to obtain the prepared Cr 4+ : Slurry used for YAG transparent ceramics;

[0032] ② The slurry obtained in step ① was dried in an oven at 55°C and sieved, and then the obtained powder was pressed into discs by dry pressing at 60 MPa with a mold, and then subjected to cold isostatic pressing at 200 MPa to obtain a biscuit.

[0033] ③Put the biscuit obtained in step ② in the air at 920°C for 8 hours, then vacuum sinter at 1780°C for 8 hours, and finally anneal in air at 1500°C for 15 hours to obtain dense Cr 4+ : YAG transparent ceramics, after g...

Embodiment 2

[0035] Composition as in Table 1 2 # Shown, specific preparation method comprises the following steps:

[0036] ①Weigh the raw materials according to the composition in Table 1. First, put the oxide raw material powder into a high-purity alumina ball mill tank, and add sintering aids, charge balance agents, and absolute ethanol to prepare the slurry; Ball milling was mixed for 18 hours, and the rotating speed was 120r / min to obtain the prepared Cr 4+ : Slurry used for YAG transparent ceramics;

[0037] ②The slurry obtained in step ① was dried, sieved, and dry pressed according to the process parameters of step ② in Example 1, and then cold isostatic pressed at 150Mpa to obtain a green body.

[0038] ④Put the biscuit obtained in step ② in the air at 800°C for 10h, then vacuum sinter at 1730°C for 30h, and finally anneal in air at 1300°C for 25h to obtain dense Cr 4+ : YAG transparent ceramics, after grinding and polishing, the polished surface and cross-section SEM images of...

Embodiment 3

[0040] Composition as in Table 1 3 # Shown, specific preparation method comprises the following steps:

[0041] ① Weigh the raw materials according to the composition in Table 1. First, put the oxide raw material powder into a high-purity alumina ball mill tank, add sintering aids, charge balance agents, and absolute ethanol to prepare the slurry; ball mill on a planetary ball mill Mix for 8 hours, and the rotating speed is 300r / min to obtain the prepared Cr 4+ : Slurry used for YAG transparent ceramics;

[0042] ② The slurry obtained in step ① is dried, sieved, and dry pressed according to the process parameters of step ② in Example 1, and then cold isostatic pressed at 250Mpa to obtain a green body.

[0043] ④Put the biscuit obtained in step ② in the air at 1000°C for 5 hours, then place it in vacuum sintering at 1850°C for 4 hours, and finally anneal in the air at 1550°C for 10 hours to obtain dense Cr 4+ : YAG transparent ceramics, after grinding and polishing, the poli...

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Abstract

The invention relates to a preparation method of transparent tetravalent chromium-doped yttrium aluminum garnet ceramics. The preparation method comprises the following steps: weighing raw material powder according to a stoichiometric ratio of a to-be-prepared ceramic component structural formula (Al1-xCrx)5CayY3-yO12 (x is not smaller than 0.001 and not larger than 0.01, and y is not smaller than 10x and not larger than 40x); adding a sintering aid and a charge compensating agent; mixing by ball-milling to obtain a slurry material; drying and sieving the slurry material and then molding to obtain a biscuit; calcining to remove volatile impurities; sintering the biscuit in vacuum at the temperature of 1730 to 1850 DEG C for 4 to 30 hours; subsequently annealing in air at the temperature of 1300 to 1550 DEG C for 10 to 25 hours to obtain compact Cr<4+>:YAG transparent ceramics. The Cr<4+>:YAG transparent ceramics prepared by the method disclosed by the invention are high in compactness, good in uniformity, free of segregation, reasonable in grain graduation distribution, free of abnormal grain growth, free of grain interior and intergranular pores and high in penetration rate, and have the conditions for being a laser gain medium.

Description

technical field [0001] The present invention relates to a kind of preparation method of tetravalent chromium doped yttrium aluminum garnet transparent ceramics, relate to a kind of orthoethyl silicate (TEOS), B 2 o 3 and CaCO 3 Preparation of Cr with excellent optical quality and high conversion of tetravalent chromium as additive 4+ : YAG transparent ceramics, belonging to the field of advanced ceramic preparation. Background technique [0002] In 1964, Shkadarevich et al. prepared tetravalent chromium-doped YAG single crystal for the first time by pulling method, and it was widely used as a gain medium for tunable lasers. Compared with conventional gain media (Cr 4+ :Mg 2 o 4 , Ti 3+ :Al 2 o 3 etc.) compared to Cr 4+ :YAG single crystal has the advantages of high quantum efficiency, good stability and long fluorescence lifetime. Not only that, because tetravalent chromium ions have saturable absorption characteristics at 1000nm to 1200nm, they can not only be us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/44C04B35/505C04B35/622
Inventor 张乐周天元王骋
Owner 河南和光光电有限公司
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