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Preparation method of 5-inch calcium yttrium oxyborate nonlinear optical crystal

A calcium yttrium oxyborate, crystal technology, applied in nonlinear optics, chemical instruments and methods, optics, etc., can solve the problems of inclusions, small caliber, and difficulty in preparing large-sized YCOB crystals, and achieve high crystal performance and crystal stress. small effect

Active Publication Date: 2021-01-12
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the difficulty in preparing large-sized YCOB crystals, defects such as inclusions and cracks are prone to occur, and the usable aperture is very small, which cannot meet the needs of ultra-intense and ultra-short laser pulse applications.

Method used

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  • Preparation method of 5-inch calcium yttrium oxyborate nonlinear optical crystal
  • Preparation method of 5-inch calcium yttrium oxyborate nonlinear optical crystal
  • Preparation method of 5-inch calcium yttrium oxyborate nonlinear optical crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] (1) Adopting Y with a purity of 99.99% 2 o 3 , CaCO 3 、H 3 BO 3 As a raw material, according to Y:Ca:B=1:4:3 ingredients, and additionally add 1% H 3 BO 3 , after mixing, briquetting, and sintering into polycrystalline YCOB raw materials, then fill it into a Φ200mm iridium gold crucible (the roundness of the bottom of the crucible is R170), put the crucible into the furnace cavity of the crystal growth and pulling furnace, and adjust figure 1 The thickness of middle insulation materials 1 and 6 makes the radial temperature gradient 6°C / cm, adjust figure 1 The thickness of the middle insulation material 7 makes the axial temperature gradient 30°C / cm, and the protective atmosphere adopts N 2 +1%O 2 (Volume ratio);

[0061] (2) Heat up until the polycrystalline YCOB raw material melts, and then keep it at 80°C higher than the melting temperature for 8 hours to stabilize the melt, and then use the b-direction YCOB seed crystal to contact the melt at about 10°C highe...

Embodiment 2

[0069] (1) Adopting Y with a purity of 99.99% 2 o 3 , CaCO 3 、H 3 BO3 As a raw material, according to Y:Ca:B=1:4:3 ingredients, and additionally add 1% H 3 BO 3 , after mixing, briquetting, and sintering into polycrystalline YCOB raw materials, then fill it into a Φ220mm iridium crucible (the roundness of the bottom of the crucible is R200), put the crucible into the furnace cavity of the crystal growth and pulling furnace, and adjust figure 1 The thickness of middle insulation materials 1 and 6 makes the radial temperature gradient 4°C / cm, adjust figure 1 The thickness of the medium 7 insulation material makes the axial temperature gradient 35°C / cm, and the protective atmosphere adopts N 2 +1.5%O 2 (Volume ratio);

[0070] (2) Heat up until the polycrystalline YCOB raw material melts, and then keep it at 70°C higher than the melting temperature for 8 hours to stabilize the melt, and then use YCOB homogeneous seed crystals to contact the melt at about 12°C higher than t...

Embodiment 3

[0078] (1) Adopting Y with a purity of 99.99% 2 o 3 , CaCO 3 、H 3 BO 3 As a raw material, according to Y:Ca:B=1:4:3 ingredients, and additionally add 1% H 3 BO 3 , after mixing, briquetting, and sintering into polycrystalline YCOB raw materials, then fill it into a Φ240mm iridium gold crucible (the roundness of the bottom of the crucible is R240), put the crucible into the furnace cavity of the crystal growth and pulling furnace, and adjust figure 1 The thickness of middle insulation materials 1 and 6 makes the radial temperature gradient 7°C / cm, adjust figure 1 The thickness of the medium 7 insulation material makes the axial temperature gradient 30°C / cm, and the protective atmosphere adopts N 2 +1.5%O 2 (Volume ratio);

[0079] (2) Heat up until the polycrystalline YCOB raw material melts, and then keep the temperature at 100°C higher than the melting temperature for 6 hours to stabilize the melt, and then use YCOB homogeneous seed crystals to contact the melt at abo...

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Abstract

The invention relates to a preparation method of a 5-inch YCOB (YCa4OB3O9) non-linear optical crystal. The method comprises the steps as follows: seed crystals are contacted with a crystal growth material melt at the temperature of 5-20 DEG C higher than crystal growth material melting temperature; the seed crystals are pulled at the pulling speed of 2-4 mm / h and the rotating speed of 18-24 rpm and heated, so that the pulling height is 3-6 mm; the crystals are pulled at the pulling speed of 0.5-1.5 mm / h and the rotating speed of 14-24 rpm and cooled; the crystals are pulled at the pulling speed of 0.5-1.5 mm / h and the rotating speed of 14-24 rpm; the crystals are pulled at the pulling speed of 2-5 mm / h and the rotating speed of 20-24 rpm and heated; the crystals are pulled at the pulling speed of 40-80 mm / min and the rotating speed of 5-10 rpm to be separated from the melt, and then, the crystals are cooled to the room temperature.

Description

technical field [0001] The invention relates to a 5-inch yttrium oxycalcium borate (YCOB) nonlinear optical crystal with few defects and no cracking. More specifically, the invention relates to a YCOB crystal for high-power laser and its preparation method, belonging to crystal growth technology field. Background technique [0002] Nonlinear optical crystals are crystals that exhibit secondary or higher nonlinear optical effects for strong laser electric fields. They are functional materials and are widely used in laser wavelength conversion and optical switches. Due to their special importance, nonlinear optical crystals have become a new interdisciplinary subject developed on the basis of crystal materials and related to laser technology. Since the invention of the first laser in the 1860s, various harmonic generators, sum frequency and difference frequency generators, and optical parametric oscillators based on nonlinear optical crystals have been commercially applied, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G02F1/355
CPCC30B15/00C30B29/10C30B33/02
Inventor 涂小牛郑燕青王升熊开南孔海宽施尔畏
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI