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Method and apparatus for growth of large size nonlinear optical crystal by copple and inoculating crystal

A nonlinear optics, large-scale technology, applied in the direction of crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of inability to remove impurities, inability to change the seed crystal and the crucible synchronously, and the crystal and the crucible rotating in the same direction, etc. problems, to achieve the effect of inhibiting crystal drift

Active Publication Date: 2009-08-12
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The traditional methods of growing nonlinear optical crystals are mostly: in the process of growing nonlinear optical crystals, either using a separate rotating seed crystal to grow nonlinear optical crystals (ACRT technology); or using a separate rotating crucible to grow For nonlinear optical crystals, the disadvantages of the two methods are: in the early stage of growth, impurities cannot be well removed at the solid-liquid interface, and it is easy to form wrapping defects and cause defects to extend inside the crystal.
Since each crystal has a fixed shape and is not completely symmetrical to the seed crystal, a large torque will be formed at the seed crystal when the crystal rotates. If the crystal weight is too large, the seed crystal will be twisted and the crystal will fall off. Large size crystals are disadvantageous
The reason why the traditional dissolved salt method and ACRT technology cannot be used simultaneously in practical applications is that the movement of the seed crystal and the crucible cannot be changed synchronously, that is, the crystal and the crucible will rotate in the same direction due to the accumulation of time errors.

Method used

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  • Method and apparatus for growth of large size nonlinear optical crystal by copple and inoculating crystal
  • Method and apparatus for growth of large size nonlinear optical crystal by copple and inoculating crystal
  • Method and apparatus for growth of large size nonlinear optical crystal by copple and inoculating crystal

Examples

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Embodiment 1

[0030] Example 1: Using the device and method for growing large-size nonlinear optical crystals in conjunction with the crucible and seed crystals of the present invention to grow borate system LBO crystals:

[0031] LBO crystals belong to orthorhombic crystal system (orthorhombic system), negative biaxial crystal, space group , the point group is C 2v -mm2, unit cell parameter: a=8.4473 , b=7.3788 , c=5.1395 , Z=4. It is composed of a continuous network of B307 molecular groups, and lithium ions are filled in the molecular gaps.

[0032] This example uses a self-service solvent to grow LBO crystals, which overcomes the difficulty in growing the crystals and cracking easily due to the high viscosity of the system and insufficient solute transport in the previous growth process;

[0033] Press Li 2 CO 3 :H 3 BO 3 =1:8 molar ratio to prepare raw materials, fully stir in φ90 crucible, growth temperature is about 750°C, cooling rate is 0.2°C / day-1.0°C / day; during the ...

Embodiment 2

[0036] Embodiment 2: Using the device and method for growing large-size nonlinear optical crystals in conjunction with the crucible and seed crystals of the present invention to grow molybdate system LBO crystals:

[0037] Choose a crucible of φ150×130mm, with Li 2 CO 3 :H 3 BO 3 :MoO 3 =2.5:8:5 (molar ratio) Raw materials are prepared, melted in a muffle furnace at high temperature and then placed in a single crystal furnace for full stirring, and a 4×4mm C-direction seed crystal is selected.

[0038]The rotation cycle of this embodiment is: in the first direction (clockwise direction), accelerate (accelerate to 30 revolutions within 15 seconds) rotation, rotate at a constant speed (30 revolutions per second) for 150 seconds, decelerate and rotate (from 30 revolutions within 15 seconds) in the first direction (clockwise) / sec decelerates to 0 revolutions) and stops rotating for 100 seconds; after that, accelerates (accelerates to 30 revolutions within 15 seconds) and rota...

Embodiment 3

[0039] Embodiment 3: BBO crystals are grown using the device and method for growing large-size nonlinear optical crystals in conjunction with the crucible and seed crystals of the present invention:

[0040] with BaCO 3 :H 3 BO 3 :NaF:BaF 2 =11:22:5:1 ratio (molar ratio) to prepare raw materials, grind and mix, sinter in a muffle furnace at 950°C for 24 hours, then grind, and finally melt at high temperature, fully stir in a φ90 crucible, and grow at a temperature of about 930°C , The cooling rate is 0.2℃ / day-0.8℃ / day. After putting the shoulders to a certain size, start lifting, and the lifting rate is controlled at 0.2-0.5mm / day.

[0041] The rotation period of this embodiment is: in the first direction (clockwise direction), accelerate (accelerate to 10 revolutions within 30 seconds) rotation, rotate at a constant speed (10 revolutions per second) for 50 seconds, decelerate and rotate (from 10 revolutions within 30 seconds) in the first direction (clockwise) / sec decel...

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Abstract

The invention relates to a method for growing a large size non-linear optic crystal through the linkage of a crucible and a seed crystal. In the growth process of growing the non-linear optic crystal through a molten salt method, the seed crystal is placed in a fused mass or on the surface of the fused mass; and the seed crystal and the crucible rotate synchronously and oppositely according to a certain rotation period. A device comprises a crystal growth device and a controller capable of driving the seed crystal and the crucible to rotate synchronously and oppositely according to the certain rotation period. The synchronous and contrarotational rotation period comprises the following steps: rotating acceleratively, rotating at a uniform speed, rotating deceleratively and stopping rotation in turn in a first direction; and then rotating acceleratively, rotating at a uniform speed, rotating deceleratively and stopping rotation in turn in a second direction opposite to the first direction. The synchronous and contrarotational rotation of the seed crystal and the crucible with an adjustable rotating speed facilitates the impurity removal in an early growth period of the seed crystal, grows a single crystal with a regular shape, and reduces or even eliminates the risk of the breaking of the seed crystal caused by an oversize moment resulting from the overweight of the seed crystal.

Description

technical field [0001] The invention relates to the technical field of crystal growth, in particular to a method and device for growing a large-size nonlinear optical crystal in conjunction with a crucible and a seed crystal. Background technique [0002] Crystal growth includes a series of processes, such as the formation process of crystal growth units, the transport process of crystal growth, and the dynamic process of crystal growth interface, among which the transport process is an important link. The crystal growth process is actually a transport process of heat, mass and momentum. Crystal growth is a process of spatial discontinuity and non-uniformity, and crystallization is only at the growth interface. [0003] The effect of stirring on the growth rate and quality of crystals must be fully realized. When growing a crystal in a melt or solution, a forced convection will be generated by the rotation of the crystal or the rotation of the crucible. At this time, the tr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B11/00C30B35/00
Inventor 胡章贵赵营
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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