Large size nonlinear optical crystal lead bromoborate, and preparation and use thereof
A technology of nonlinear optics and lead borate, applied in nonlinear optics, chemical instruments and methods, optics, etc., can solve problems such as crystals that cannot be purchased in the market
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Embodiment 1
[0033] Take reaction formula (1) as an example, but not limited to reaction formula (1);
[0034] According to the equation PbO+H 3 BO 3 +HBr→Pb 2 B 5 o 9 Br+H 2 O ↑ synthesis of Pb 2 B 5 o 9 Br compound, concrete operation steps are as follows:
[0035] PbO, H 3 BO 3 , HBr acid was put into a mortar with a stoichiometric ratio of 2:5:1, mixed and carefully ground, then put into a Φ200mm×200mm open corundum crucible, pressed it tightly, put it into a muffle furnace, and slowly heated up to 400°C, constant temperature for 5 hours, exhaust the gas as much as possible, take out the crucible after cooling, grind the sample evenly, then put it in the crucible, keep the temperature in the muffle furnace at 520°C for another 5 hours, wait for the temperature to drop to room temperature and then take it out , grind carefully, keep the temperature at 520°C for 24 hours again, put it into a mortar after cooling, and grind it lightly to get completely sintered Pb 2 B 5 o 9 ...
Embodiment 2
[0039] Take reaction formula (2) as an example, but not limited to reaction formula (2).
[0040] According to the equation PbO+B 2 o 3 +HBr→Pb 2 B 5 o 9 Br+H 2 O ↑ synthesis of Pb 2 B 5 o 9 Br compound, specific operation steps are carried out according to embodiment 1;
[0041] The synthesized Pb 2 B 5 o 9 Br compound and flux NaF and PbO molar ratio Pb 2 B 5 o 9 Mix Br:NaF:PbO=1:1:4, put it into a Φ60mm×40mm open platinum crucible, raise the temperature to 750°C, keep the temperature for 80 hours and then cool down to 620°C, and cut the Pb along the b-axis 2 B 5 o 9 The Br seed crystal is fixed on the lower end of the seed rod with a platinum wire, and the seed crystal is introduced into the crucible from the small hole on the top of the furnace to make it contact with the liquid surface. The seed crystal rotates at a rate of 50 rpm, and the direction of rotation is reversible. Time 3 Minutes, the time interval is 0.4 minutes, keep the temperature for 1 hou...
Embodiment 3
[0044] Take reaction formula (3) as an example: but not limited to (3).
[0045] According to the equation Pb(NO 3 ) 2 +H 3 BO 3 +HBr→Pb 2 B 5 o 9 Br+H 2 O↑+NO 2 ↑ Synthesis of Pb 2 B 5 o 9 Br compound, specific operation steps are carried out according to embodiment 1;
[0046] The synthesized Pb 2 B 5 o 9 Br compound and flux NaF and PbO molar ratio Pb 2 B 5 o 9 Mix Br:NaF:PbO=1:4:2, put it into an open platinum crucible of Φ50mm×40mm, raise the temperature to 750°C, keep the temperature for 50 hours and then cool down to 580°C, the Pb cut along the a-axis 2 B 5 o 9 The Br seed crystal is fixed on the lower end of the seed rod with a platinum wire, and the seed crystal is introduced into the crucible from the small hole on the top of the furnace to make it contact with the liquid surface. The seed crystal rotates at a rate of 30 rpm, and the rotation direction is unidirectional. 6 minutes, the time interval is 0.8 minutes, keep the temperature for 1 hour,...
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