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Preparation method of yttrium-aluminum garnet single crystal

A technology of yttrium aluminum garnet and garnet powder, which is applied in the field of preparation of yttrium aluminum garnet single crystal by static pressure combined process, can solve problems such as difficulty in obtaining uniform crystals with optical quality, damage, and poor optical quality of ceramics, and achieve shortening The effect of the preparation cycle

Active Publication Date: 2015-01-07
SINOMA SYNTHETIC CRYSTALS CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since YAG single crystal is currently mainly grown by medium-frequency induction pulling method, its growth cycle is long, and the precious metal iridium is required as a crucible, which has high cost. Due to the existence of "core" and stress stripes, the "core" and "core" must be avoided when cutting the crystal. Stress fringes, therefore, low utilization of crystals, making it difficult to obtain crystals of uniform optical quality with diameters greater than 50 mm
In addition, affected by the segregation coefficient, the doping concentration of Nd ions in the YAG crystal is difficult to exceed 1.5at%.
Chinese patent CN101338453A discloses "a large-scale coreless YAG series laser crystal growth device and its growth method", using this method to obtain YAG series crystals with a diameter of 35 to 50 mm, no core, no dislocation, and no scattering, but Nd ions The doping concentration can only be up to 2at%, which limits the utilization of materials
However, compared with single crystals, there are grain boundaries between grains in ceramics. In optical applications, grain boundaries act as scattering centers, which may lead to poor optical quality of ceramics.
Especially for laser ceramics, a large number of defects exist at the grain boundaries, and these defects will cause damage under the conditions of ultra-high power and ultra-long laser service

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh 50g of Nd(1at%):YAG powder, add 0.5wt% tetraethyl orthosilicate (TEOS), use 25g of absolute ethanol as the medium, mix by wet ball milling for 8h, place in an oven, and keep warm at 80°C Dry for 24 hours, calcined at 600°C, and remove organic matter after calcining for 5 hours, then install it in a vacuum hot-press furnace at a temperature of 1400°C, a pressure of 40MPa, and a vacuum of 10 -2 The Nd(5at%):YAG ceramics with a grain size of 2μm were obtained under Pa, heat preservation and pressure for 1h; the prepared Nd(1at%):YAG ceramics were polished on one side, and the Nd (1at%): After the YAG single crystal photoresist is treated, it is placed in a hot isostatic pressing furnace, under an Ar atmosphere, the temperature is 1550 ° C, the pressure is 100 MPa, and the temperature is kept at 100 MPa for 3 hours to obtain Nd(1at%): YAG single crystal. The abnormal grain growth rate was 3mm / h.

Embodiment 2

[0032] Weigh 50g of Nd(5at%):YAG powder, add 0.5wt% magnesium oxide (MgO), use 50g of absolute ethanol as the medium, mix for 10h, place in an oven, heat-preserve and dry at 90°C for 18h, and calcined The temperature is 700°C, and after calcination for 5 hours to remove organic matter, it is installed in a vacuum hot-press furnace at a temperature of 1450°C, a pressure of 30MPa, and a vacuum degree of 10 -3 Under Pa, heat preservation and pressure for 2h, Nd(5at%):YAG ceramics with a grain size of 3μm were obtained; after the prepared Nd(5at%):YAG ceramics were polished on one side, they were combined with YAG polished on one side in the direction After the single crystal is photoresist treated, it is placed in a hot isostatic pressing furnace under an Ar atmosphere at a temperature of 1600°C and a pressure of 150 MPa, and is kept at a pressure of 1.5 hours to obtain a Nd(5at%):YAG single crystal. The abnormal grain growth rate was 4 mm / h.

Embodiment 3

[0034] Weigh 50g of Nd(10at%):YAG powder, add 0.4wt% tetraethyl orthosilicate (TEOS), use 100g of absolute ethanol as the medium, mix by wet ball milling for 15h, place in an oven, and keep warm at 100°C Dry for 12 hours, calcined at 800°C, and remove organic matter after calcining for 3 hours, then install it in a vacuum hot-press furnace at a temperature of 1520°C, a pressure of 30MPa, and a vacuum of 10 -3 Under Pa, heat preservation and pressure for 2 hours, Nd(10at%):YAG ceramics with a grain size of 4 μm were obtained; after the prepared Nd(1at%):YAG ceramics were polished on one side, they were combined with YAG polished on one side in the direction After the single crystal is photoresist treated, it is placed in a hot isostatic pressing furnace under an Ar atmosphere at a temperature of 1650 °C and a pressure of 200 MPa. The Nd(10at%):YAG single crystal is obtained after holding the heat for 2 hours. The abnormal grain growth rate was 4.5 mm / h.

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Abstract

The invention relates to a preparation method of an yttrium-aluminum garnet single crystal. The preparation method comprises the following steps of: 1) adding ethyl silicate and / or magnesium oxide to yttrium-aluminum garnet powder, then adding absolute ethane, mixing, and sequentially carrying out drying, calcining and vacuum hot pressing treatment to obtain an yttrium-aluminum garnet ceramic; and 2) carrying out single-side polishing on the yttrium-aluminum garnet ceramic obtained in the step 1) to obtain a single-side polished yttrium-aluminum garnet ceramic, then carrying out photoresist treatment on the single-side polished yttrium-aluminum garnet ceramic and single-side polished yttrium-aluminum garnet single crystal, and then carrying out hot isostatic pressing treatment to obtain the yttrium-aluminum garnet single crystal. By utilizing the preparation method provided by the invention, a single crystal with Nd doping concentration up to 10at% can be prepared, and a YAG (yttrium-aluminum garnet) single crystal can be prepared at a lower temperature (1550-1750 DEG C).

Description

technical field [0001] The invention relates to a method for preparing yttrium aluminum garnet single crystal, in particular to a method for preparing yttrium aluminum garnet single crystal by using a combined process of vacuum hot pressing and hot isostatic pressing. Background technique [0002] Yttrium aluminum garnet (Y 3 al 5 o 12 , referred to as YAG) single crystal has excellent mechanical and optical properties, and is a very important infrared and laser window material. Rare earth ion-doped YAG single crystal is an excellent laser gain medium, such as Nd:YAG single crystal is currently the most widely used solid-state laser material. However, since YAG single crystal is currently mainly grown by medium-frequency induction pulling method, its growth cycle is long, and the precious metal iridium is required as a crucible, which has high cost. Due to the existence of "core" and stress stripes, the "core" and "core" must be avoided when cutting the crystal. Stress f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B1/12C30B29/28
Inventor 王海丽沈德忠黄存新陈建荣张书峰王震
Owner SINOMA SYNTHETIC CRYSTALS CO LTD
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