Lead barium borate compound and lead barium borate nonlinear optical crystal and preparation method and application
A technology of nonlinear optics and lead-barium borate, applied in nonlinear optics, chemical instruments and methods, optics, etc., can solve the problems of crystal deliquescence, high price, long growth cycle, etc.
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[0045] A preparation method of compound lead barium borate, adopting solid phase reaction method, mixing uniformly according to molar ratio Ba:Pb:B:O=8.19:0.81:18:36, grinding, putting into muffle furnace, heating up to 400°C , keep the temperature for 24 hours, cool to room temperature, and get the sample; grind the sample, then raise the temperature to 750-850°C, and keep the temperature for 48 hours; during the constant temperature period, grind the sample many times, and finally obtain a fully sintered lead-barium borate compound single-phase polycrystalline powder.
[0046] A compound lead barium borate nonlinear optical crystal, the crystal chemical formula is Pb 0.81 Ba 8.19 B 18 o 36 , molecular weight 2063.14, belongs to hexagonal crystal system, space group R 32. The unit cell parameter is a =7.2116(7)?, c =19.226(4)?, Z=1, V=865.9(2)? 3 .
[0047] A method for preparing a compound lead barium borate nonlinear optical crystal, using a solid-state reaction meth...
Embodiment 1
[0061] According to the reaction formula: 8.19BaO+0.81PbO+18H 3 BO 3 →Pb 0.81 Ba 8.19 B 18 o 36 +26H 2 O ↑ synthesis of Pb 0.81 Ba 8.19 B 18 o 36 compound;
[0062] BaO, PbO, H 3 BO 3 Put it into a mortar with a molar ratio of 8.19:0.81:18, mix and grind it carefully, then put it into a corundum crucible with an opening of Φ100mm×100mm, put it in a muffle furnace, raise the temperature to 400°C, keep the temperature constant for 24 hours, and cool to room temperature , fully ground, then heated up to 850°C, kept at a constant temperature for 48 hours, and fully ground to obtain a fully sintered lead-barium borate compound single-phase polycrystalline powder, and then X-ray analysis was performed on the polycrystalline powder. Lead Barium Pb 0.81 Ba 8.19 B 18 o 36 The X-ray spectra obtained by the single crystal structure are consistent;
[0063] The barium oxide in the reaction formula can be replaced by barium carbonate or barium nitrate or barium oxalate or ...
Embodiment 2
[0069] According to the reaction formula: 8.19BaCO 3 +0.81PbO+18H 3 BO 3 →Pb 0.81 Ba 8.19 B 18 o 36 +8.19CO 2 ↑+26H 2 O ↑ Synthetic compound Pb 0.81 Ba 8.19 B 18 o 36 ;
[0070] BaCO 3 , PbO, H 3 BO 3 Weigh the raw materials directly according to the molar ratio of 8.19:0.81:18, and combine the weighed raw materials with flux H 3 BO 3 Mix according to a molar ratio of 1:4, put it into an open platinum crucible of Φ80mm×80mm, heat it to 880°C at a heating rate of 30°C / h, and keep the temperature for 15 hours to obtain a mixed solution, then cool it down to 820°C, At this time, the seed rod is quickly extended under the liquid surface, and the temperature is slowly lowered to 720°C at a rate of 1°C / h, and the seed rod is lifted out of the liquid surface. Small crystals will gather on the seed rod, and the temperature is 35°C / h. The rate of h is reduced to room temperature, and the lead barium borate seed crystal is obtained;
[0071] The barium carbonate in the...
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