Large size non-linear optic crystal of boron phosphate, flux growth method and usage
A technology of nonlinear optics and growth method, which is applied in the field of molten salt growth of large-sized boron phosphate nonlinear optical crystals. question
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Embodiment 1
[0074] Example 1. Crystal Growth
[0075] (1) Mix the pre-synthesized boron phosphate and flux in proportion, put it into a platinum crucible with an opening of Φ60mm×60mm, put the crucible into a vertical heating furnace, and seal the opening at the top of the furnace with insulating material Above, leave a small hole at the position corresponding to the top of the furnace and the center of the crucible for the entry and exit of the seed crystal rod, rapidly heat up to 880°C for melting, keep the temperature for 24 hours and quickly cool down to 815°C (10°C above the saturation temperature), and obtain the Mixed melt of boron phosphate and flux;
[0076] The flux is Li-containing 4 P 2 o 7 and Li 2 Composite flux of O;
[0077] The boron phosphate and Li 4 P 2 o 7 and Li 2 The molar ratio of compound flux compounding of O is: BPO 4 : Li 4 P 2 o 7 : Li 2 O=1:0.35:0.24;
[0078] (2) At 815°C (10°C above the saturation temperature), the BPO cut along the c-axis 4...
Embodiment 2
[0079] Example 2. Crystal Growth
[0080] The pre-synthesized boron phosphate and Li-containing 4 P 2 o 7 and Li 2 The compound flux of O is mixed, and its molar ratio is: BPO 4 : Li 4 P 2 o 7 : Li 2 O=1:0.35:0.18;, put it into an open platinum crucible of Φ60mm×60mm, put the crucible into a vertical heating furnace, seal the opening at the top of the furnace with insulating material, and place it between the top of the furnace and the center of the crucible Leave a small hole in the corresponding place for the seed rod to enter and exit, quickly heat up to 890°C for melting, and then quickly cool down to 816°C (5°C above the saturation temperature) after constant temperature for 48 hours to obtain a mixed melt containing boron phosphate and flux . BPO that will be cut along the c-axis 4 The seed crystal is fixed on the lower end of the seed rod with a platinum wire. The seed crystal is introduced into the crucible from the small hole on the top of the furnace, immer...
Embodiment 3
[0081] Embodiment 3 crystal growth
[0082] Crystal growth was performed using the top seed method. Using one-time synthesis, directly select analytically pure H 3 BO 3 , NH 4 h 2 PO 4 and Li 2 CO 3 , according to the following molar ratio: H 3 BO 3 : NH 4 h 2 PO 4 : Li 2 CO 3 =1:1.7:0.82, (actual BPO 4 Compounds and Li 4 P 2 o 7 and Li 2 The molar ratio of O composite flux is: BPO 4 : Li 4 P 2 o 7 : Li 2 O=1:0.35:0.12), accurately weigh the above reagents according to the stoichiometric ratio, put them in an agate mortar and grind them evenly, put them into a corundum crucible, pre-fire in a muffle furnace at 400°C for 10 hours, and then put them into the mortar and then sintered at 650°C for 48 hours, put it into an open platinum crucible, place the open platinum crucible on a certain position of the heating furnace, and seal the opening of the furnace with a suitable insulating material, and then heat up to 900 ℃ melting, constant temperature for 72 ...
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