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Horizontally directional zone-melting crystallization preparation method for large-size Re:YAG series of laser crystals

A laser crystal, horizontal orientation technology, applied in self-regional melting method, crystal growth, single crystal growth, etc., can solve high residual stress and dislocation density of crystal, large temperature gradient of temperature gradient method growth, and heat exchange method growth cycle Long and other issues, to achieve the effect of reducing macro defects, avoiding heat radiation, obvious economic and social benefits

Inactive Publication Date: 2013-08-14
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the inherent nature of the RE:YAG crystal itself, each growth method has its own advantages and disadvantages, and it is difficult to be perfect. For example, in the above-mentioned growth method, the pulling method is due to the forced convection formed by mechanical movement in the melt during the growth process. effect, the temperature gradient near the solid / liquid interface is large, so that there are high residual stress and dislocation density in the crystal; the growth temperature gradient of the temperature gradient method is large, which leads to high stress and defects in the grown crystal, and the crystal The blank needs to be annealed in high temperature oxidation and reducing atmosphere respectively, and the subsequent treatment process of the blank is relatively complicated; the growth cycle of the heat exchange method is long, and the grown crystal is easy to crack, which is difficult to be marketed

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Put 4.5Kg of pre-crystallized high-purity massive Nd:YAG powder into the treated boat-shaped molybdenum crucible, load the furnace, and vacuumize and open the cooling circulation system. The outlet water temperature of the circulation cooling system is controlled at 30 ± 8 ℃ range, when the vacuum reaches 1.0×10 -4 At Pa, resistance heating is performed to raise the temperature. As the temperature increases, the vacuum degree decreases, but the vacuum degree is always controlled at 1.0×10 during the temperature rise process. -3Pa. When the temperature is raised until the melt flow line is observed, when the power is increased to 27kW, the melt flow is observed, and the power change (250W / h) is properly fine-tuned, so that the solid-liquid conversion phenomenon of orderly convection just appears on the liquid surface. Under this condition, it was stable for 4 hours, and the material was fully compounded. Slowly move the seed crystal into the high temperature zone, the...

Embodiment 2

[0033] Put 5.0Kg of the prepared pre-crystallized material high-purity massive Yb:YAG powder into the processed boat-shaped molybdenum crucible, install the furnace, open the cooling circulation system and vacuumize, when the vacuum degree reaches 3.0×10 -4 At Pa, resistance heating is performed to raise the temperature. During the heating process, the vacuum degree is always controlled at 5.0×10 -3 Pa. The power was increased to 28kW, and the liquid flow of the melt was observed. It was found that the fog on the liquid surface increased, and it was judged that the temperature in the crucible was too high. Therefore, the power change was fine-tuned at 500W / h, so that the solid-liquid conversion phenomenon of orderly convection just appeared on the liquid surface. Under this condition, it was stable for 4 hours, and the material was fully compounded. The crystal orientation of the seed crystal adopts the [111] direction, the position of the seed crystal is located at the geom...

Embodiment 3

[0035] Put 4.8Kg of the prepared pre-crystallization material high-purity bulk Er:YAG powder into the processed boat-shaped molybdenum crucible, install the furnace, open the cooling circulation system and vacuumize, when the vacuum degree reaches 1.0×10 -4 At Pa, resistance heating is performed to raise the temperature. Increase the power to 28kW, observe the melt flow, and fine-tune the power change at 500W / h, so that the solid-liquid conversion phenomenon of orderly convection just appears on the liquid surface. And stable for 4 hours, fully compounded. The crystal orientation of the seed crystal adopts the [111] direction, the position of the seed crystal is located at the geometric center of the crucible, and the deviation is not greater than 10.0mm. Slowly move the seed crystal into the high temperature zone, make the melt contact with the seed crystal 4mm, keep the molten crystal for 8min, start seeding, the seeding rate is 0.8mm / h, and adjust the power drop at a speed...

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Abstract

The invention relates to a horizontally directional zone-melting crystallization preparation method for large-size Re:YAG series of laser crystals. The horizontally directional zone-melting crystallization preparation method is technically characterized in that the Re:YAG laser crystals are grown by means of horizontally directional zone-melting crystallization in a vacuum condition; and the specific growth process comprises the six processes of material melting, seeding, shouldering, equal-width growing, cooling and annealing. According to the horizontally directional zone-melting crystallization preparation method disclosed by the invention, the advantages of a directional crystallization method and a vertical zone-melting method for crystal growth are combined, so that the prepared Re:YAG laser crystals have the advantages of being higher in quality, larger in size, higher in utilization rate, low in defect density, better in laser performance, without doped ion central cores or lateral cores, and the like.

Description

technical field [0001] The invention relates to a growth method for preparing a single crystal, in particular to a method for preparing a large-size plate-shaped Re:YAG single crystal by horizontally oriented zone melting crystallization. Background technique [0002] Yttrium aluminum garnet has excellent optical, chemical, thermal and mechanical properties, and its chemical formula is Y 3 al 5 o 12 (YAG) belongs to the cubic crystal system with space group Ia3d. Its lattice constant is Each unit cell contains 8 Y 3 al 5 o 12 Numerator, a total of 24 Y 3+ ion, 40 Al 3+ ion, 96 O 2- ion. al 3+ Occupy two kinds of lattice positions respectively, a part of Al 3+ Four-coordinated [AlO 4 ] tetrahedron, a part of Al 3+ In six coordinated [AlO 6 ] octahedron, each [AlO 4 The four vertices of the tetrahedron are all aligned with the [AlO 6 ] The vertices of the octahedron are connected to form a three-dimensional skeleton, and Y 3+ Occupy the interstitial position...

Claims

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Application Information

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IPC IPC(8): C30B13/10C30B29/28
Inventor 张明福郭怀新聂颖韩杰才赵盼盼
Owner HARBIN INST OF TECH
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