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Preparation method of horizontal directional solidification of large-scale re:yap series laser crystals

A laser crystal, horizontally oriented technology, applied in the direction of self-solidification, crystal growth, chemical instruments and methods, etc., can solve the problems of difference in thermal expansion coefficient and difficulty in growing large-sized and high-quality crystals, and achieve large size, obvious economic benefits and Social benefit and cost saving effect

Inactive Publication Date: 2015-08-05
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 anisotropy of Re:YAP crystals, the thermal expansion coefficients of different crystal axes are quite different, so the growth of large-sized high-quality crystals is very difficult.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Put 3Kg of pre-crystallized material high-purity massive Nd:YAP powder into the boat-shaped molybdenum crucible washed with alcohol, and charge the furnace, and the furnace chamber is evacuated until the vacuum degree reaches 5×10 -3 At Pa, resistance heating is performed to raise the temperature. 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. When the raw material is completely melted, keep it for 3h. Slowly move the seed crystal into the high temperature zone, the seed crystal is oriented in the (010) direction, and the position of the seed crystal is located at the geometric center of the crucible. The melt contacted the seed crystal for 3 mm, kept the molten crystal for 5 minutes, and began to pull the crucible in the horizo...

Embodiment 2

[0034] Put the prepared pre-crystallization material high-purity massive Tm:YAP powder 6Kg into the boat-shaped molybdenum crucible washed with alcohol, install the furnace, and the furnace chamber is evacuated until the vacuum degree reaches 5×10 -3At Pa, resistance heating is performed to raise the temperature. 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. After fully chemicalizing the material, keep it for 1h. The crystal orientation of the seed crystal adopts the (010) direction, and the position of the seed crystal is located at the geometric center of the crucible. Slowly move the seed crystal into the high temperature zone, make the melt contact with the...

Embodiment 3

[0036] Put 4.5Kg of the prepared pre-crystallization material high-purity massive Er:YAP powder into the boat-shaped molybdenum crucible washed with alcohol, put into the furnace, and the furnace is evacuated until the vacuum degree reaches 5×10 -3 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. When the raw material is completely melted, keep it for 5h. Slowly move the seed crystal into the high temperature zone, and the direction of the seed crystal is (010). Make the melt contact with the seed crystal 4mm, keep the molten crystal for 8min, start to pull the crucible to seed the crystal along the horizontal direction, the seeding rate is 0.5mm / h, enter the shoulder growth process after 15 hours of seeding, the shoulder angle is 90°, the crucible The moving speed...

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Abstract

The invention relates to a horizontal directional solidification preparation method of a large-size Re:YAP series laser crystal, which is technologically characterized in that the Re:YAP laser crystal is grown by horizontal directional solidification crystallization under a vacuum condition. The specific growth process comprises six major steps of material melting, seeding, shouldering, equal-width growth, cooling and annealing. The method provided by the invention combines the advantages of a directional crystallization process and a vertical zone-melting process in growing crystals; and the prepared Re:YAP laser crystal has the advantages of higher quality, larger size, higher utilization rate, low defect density, better laser performance, non-doped ion core, low cost, low energy consumption and the like.

Description

technical field [0001] The invention relates to a method for growing single crystals of refractory oxides, in particular to a method for preparing large-scale plate-like Re:YAP series single crystals by horizontal directional solidification. Background technique [0002] Yttrium aluminate crystal is a high-quality laser crystal developed in the late 1960s and early 1970s. It is a potential substitute crystal for yttrium aluminum garnet crystal. It has excellent optical, chemical, thermal and mechanical properties. Its chemical formula is YAlO 3 (YAP). YAP crystal belongs to the orthorhombic crystal system, the space group is D 2h 16 -P bnm . This weaker spatial symmetry gives this crystal two main advantages: (1) when pumped at higher powers, the natural birefringence of the YAP crystal dominates over the thermal birefringence; (2) Anisotropy of stimulated emission. The solid-state laser based on YAP has the property of outputting linearly polarized light. Selecting an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/24C30B11/00
Inventor 张明福聂颖郭怀新韩杰才赵盼盼闫润泽
Owner HARBIN INST OF TECH
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