Single crystal growth method of monopotassium phosphate with large caliber and high quality

A technology of potassium dihydrogen phosphate and growth method, which is applied in the field of cooling growth of large-caliber high-quality potassium dihydrogen phosphate single crystal, which can solve the problems of prolonging the production cycle of KDP crystal, destroying the growth of the crystal cone, and affecting the quality of the finished product, and shortening the production time. Crystal growth cycle, increase the success rate of crystal growth, and improve the effect of crystal quality

Inactive Publication Date: 2010-07-14
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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Problems solved by technology

Under such control conditions, the seed crystal is cone-shaped and the cooling rate is maintained at 0.2°C/day. If the cooling rate is too large, the accumulation of supersaturation will easily increase, and the phenomenon of "pulling cone" will easily occur, such as figure 2 As shown, it takes a long time for the seed crystal to form a cone, which prolongs the production cycle of the KDP crystal, and white streaks are prone to appear on each crystal face of the crystal, which affects...

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  • Single crystal growth method of monopotassium phosphate with large caliber and high quality
  • Single crystal growth method of monopotassium phosphate with large caliber and high quality
  • Single crystal growth method of monopotassium phosphate with large caliber and high quality

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Embodiment Construction

[0013] In the crystal growth cylinder (2) with a size of φ1200×1600mm, add 750Kg of AR-grade KDP powder produced by Shanghai Reagent No. The rate reached 18.2MΩ·cm, and after preparing a saturated KDP growth solution with a saturation point of 61.0°C, the temperature was raised to 75°C, and the temperature was overheated and kept at constant temperature for 24 hours. Put a plate-shaped KDP seed crystal with a size of 360×360×20mm upside down on the crystal carrier, bake it at 75°C for 24 hours, introduce it into KDP saturated solution to lower the temperature to 60.5°C, and set the cooling rate to 0.05°C / day, growing in cones. The crystal rotation mode follows the cycle sequence of "acceleration-forward rotation-deceleration-stop rotation-acceleration-reverse rotation-deceleration-stop rotation", and the time interval is "20 seconds-60 seconds-20 seconds-20 seconds-20 seconds-60 seconds- Rotate the seed crystal in the mode of 20 seconds to 20 seconds, and keep the forward an...

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Abstract

The invention relates to a single crystal growth method of monopotassium phosphate with large caliber and high quality, comprising the following steps: when seed crystal forms a cone, initial growth temperature lowers to the temperature of 0.5 DEG C below solution saturating point, and cone forming begins; cooling rate is controlled at 0.05 DEG/ day; the mode of cooling by stage is adopted after the seed crystal is in phragmocone; the crystal is in phragmocone until 50 DEG C; cooling rate is kept to 0.05 DEG C/ day; at the temperature of 50-35 DEG C, cooling rate is kept to 0.1 DEG C/ day; at the temperature of 35 DEG C to room temperature, cooling rate is kept to 0.15 DEG C/ day; a crystal rotation mode adopts the following circulation sequence: quickening, positive rotating, slowing down, stalling, quickening, reverse rotating, slowing down and stalling; seed crystal rotates at time interval as follows: 20 seconds, 60 seconds, 20 seconds, 20 seconds, 20 seconds, 60 seconds, 20 seconds and 20 seconds; and the positive rotating rate and the reversal rate are kept to 40-60 turns/ minute.

Description

technical field [0001] The present invention relates to crystal growth, in particular to large diameter (> 350mm) high quality potassium dihydrogen phosphate (KH 2 PO 4 , referred to as KDP) single crystal cooling growth. Background technique [0002] KDP crystal is an excellent nonlinear optical material, which is mainly used in the second, third, and fourth times of laser frequency doubling, especially the high-quality large-size KDP crystal, which has been listed as the only practical material for laser nuclear fusion frequency conversion internationally. , is also a hot topic in international crystal growth research. So far, the traditional cooling method is still used in China to grow large-aperture single crystals. [0003] Large-diameter KDP crystal growth is carried out in a φ1200×1600mm cylindrical stainless steel crystal growth cylinder with a volume of 1.5 tons. growing equipment such as figure 1 As shown, 1 is the crystal growth cylinder, 2 is the cylinde...

Claims

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Application Information

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IPC IPC(8): C30B29/14C30B7/08
Inventor 李国辉李征东苏根博贺友平林秀钦庄欣欣
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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