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Pure-oxygen-atmosphere annealing device and method

An annealing device, technology of oxygen atmosphere

Active Publication Date: 2013-04-03
SUZHOU SIHAI CHANGJING PHOTOELECTRIC MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two serious shortcomings in this annealing method. First, due to the diffusion or back diffusion of dust in the atmosphere or other impurity ions in the annealing furnace, the crystal is prone to secondary pollution; second, the annealing efficiency is not high. Medium annealing requires higher annealing temperature, high energy consumption, and the crystal brightness and transmittance after annealing are not ideal

Method used

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  • Pure-oxygen-atmosphere annealing device and method

Examples

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Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1: adopt the device annealing Nd of the present invention: YAG crystal

[0046] Gently pull out the round stainless steel side cover lined with thermal insulation material from the annealing furnace, put the Nd:YAG crystal, wafer or ingot into the quartz tube, then seal the furnace tube with the side cover, and turn on the oxygen in sequence Bottle switch and oxygen decompression valve switch, the flow of pure oxygen is controlled through the oxygen decompression valve and valve, so that the pressure in the quartz tube is less than 1.2atm. The temperature controller is set at a heating rate of 60°C / h, the temperature is raised to 1300°C, the temperature is kept constant for 1200min, the cooling rate is 60°C / h, and the temperature controller is operated. After the program cools down to less than 200°C, close the program, the temperature drops below 50°C, open the furnace tube, take out the crystal, wafer or ingot, close the furnace tube, and the annealing is o...

Embodiment 2

[0047] Embodiment 2: using the device of the present invention to anneal Cr4+: YAG crystal

[0048] Gently pull out the round stainless steel side cover lined with thermal insulation material from the annealing furnace, put Cr4+:YAG crystals, wafers or ingots into the quartz tube, then seal the furnace tube with the side cover, and turn on the oxygen in sequence Bottle switch and oxygen decompression valve switch, the flow of pure oxygen is controlled through the oxygen decompression valve and valve, so that the pressure in the quartz tube is less than 1.2atm. The temperature controller is set at a heating rate of 50°C / h, the temperature is raised to 1300°C, the temperature is kept constant for 3000 minutes, the cooling rate is 50°C / h, and the temperature controller is operated. After the program cools down to less than 200°C, close the program, the temperature drops below 50°C, open the furnace tube, take out the crystal, wafer or ingot, close the furnace tube, and the anneal...

Embodiment 3

[0049] Embodiment 3: using the device of the present invention to anneal Yb:YAG crystal

[0050] Gently pull out the round stainless steel side cover lined with thermal insulation material from the annealing furnace, put the Yb:YAG crystal, wafer or ingot into the quartz tube, then seal the furnace tube with the side cover, and turn on the oxygen in sequence. Bottle switch and oxygen decompression valve switch, the flow of pure oxygen is controlled through the oxygen decompression valve and valve, so that the pressure in the quartz tube is less than 1.2atm. The temperature controller is set at a heating rate of 60°C / h, the temperature is raised to 1300°C, the temperature is kept constant for 1200min, the cooling rate is 60°C / h, and the temperature controller is operated. After the program cools down to less than 200°C, close the program, the temperature drops below 50°C, open the furnace tube, take out the crystal, wafer or ingot, close the furnace tube, and the annealing is o...

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Abstract

The invention discloses a pure-oxygen-atmosphere annealing device and method. According to the method, a material required for being annealed is loaded into quartz tubes, the quartz tubes are placed in an aluminum-oxide ceramic sleeve which is uniformly wound by nickel-chromium wires, oxygen of stable flow is introduced into the quartz tubes, the internal furnace temperature is uniformly and slowly increased, heat of a heater is transferred to crystals to be annealed in a radiation manner, and a temperature control instrument controls a heating-up rate, the degree of a constant temperature, the time for constant temperature and a cooling rate, so that the fully-automatic unattended annealing is realized, and the annealing temperature can reach 1,300 DEG C. The pure-oxygen-atmosphere annealing device and method disclosed by the invention are applicable to the pure-oxygen-atmosphere annealing of materials, such as laser crystals, scintillation crystals and the like, the annealing efficiency is high, and the light emitting efficiency of the laser and scintillation crystals can be increased by 20-40%; after annealing, the brightness, transparency, crystalline perfection and optical uniformity of the crystals can be greatly improved; and the pure-oxygen-atmosphere annealing device has the advantages of stable temperature field, simplicity and reliability, good universality and low energy consumption, so that the annealing cost is reduced.

Description

technical field [0001] The invention relates to the field of annealing treatment, in particular to a pure oxygen atmosphere annealing device and annealing method suitable for post-annealing treatment of laser crystals and scintillation crystals and the like. Background technique [0002] Today, the pulling method (Chuklarski method) is the most commonly used method for growing crystals. This method is used to grow high-quality high-temperature oxide crystals (gem, yttrium aluminum garnet, lutetium silicate, yttrium vanadate, gadolinium gallium Garnet, spinel, etc.) usually need to be carried out in an iridium crucible to reduce the pollution of the growth environment to the melt and crystal. [0003] Since the temperature gradient of the solid-liquid interface is large when the crystal is grown by the pulling method, the thermal stress of the grown crystal is relatively large, and annealing treatment is generally required before crystal processing; on the other hand, since t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B33/02
Inventor 陈建玉
Owner SUZHOU SIHAI CHANGJING PHOTOELECTRIC MATERIAL
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