Compound Pb0.78Ba8.22B18O36, Pb0.78Ba8.22B18O36 nonlinear optical crystal, preparation methods and application
A technology of nonlinear optics, lead-barium-boron-oxygen, applied in the direction of nonlinear optics, chemical instruments and methods, boron compounds, etc., can solve the problems of serious layered growth habit, long growth cycle, deliquescence of crystals, etc., and achieve inclusions The effect of less, short growth cycle and high mechanical hardness
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[0046] A preparation method of compound lead, barium, boron and oxygen, adopting solid phase reaction method, mixing uniformly according to molar ratio Ba:Pb:B:O=8.22:0.78:18:36, grinding, putting into muffle furnace, heating up to 400 ℃, keep the temperature for 24 hours, cool to room temperature, and get the sample; grind the sample, then raise the temperature to 730-850°C, and keep the temperature for 48 hours; during the constant temperature period, grind the sample many times, and finally get a fully sintered lead-barium-boron-oxygen compound single-phase polycrystalline powder, and the polycrystalline powder was subjected to X-ray analysis.
[0047] A compound lead barium boron oxygen nonlinear optical crystal, the crystal chemical formula is Pb 0.78 Ba 8.22 B 18 o 36 , molecular weight 2060.84, belongs to hexagonal crystal system, space group R 32. The unit cell parameter is a =7.2225(2)?, c =19.2716(10)?, Z=1, V=870.61(6)? 3 .
[0048] A method for preparing a ...
Embodiment 1
[0062] According to the reaction formula: Synthetic Pb 0.78 Ba 8.22 B 18 o 36 compound;
[0063] BaO, PbO, H 3 BO 3 Put it into a mortar with a molar ratio of 8.22:0.78:18, 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 for 24 hours, and cool to room temperature , fully ground, and then heated to 850 ° C, kept at constant temperature for 48 hours, fully ground, and then a fully sintered lead-barium-boron-oxygen compound single-phase polycrystalline powder was obtained, and then X-ray analysis was performed on the polycrystalline powder, and the obtained X-ray spectrum was consistent with that of lead barium boron oxide Pb 0.78 Ba 8.22 B 18 o 36 The X-ray spectra obtained by the single crystal structure are consistent;
[0064] The barium oxide in the reaction formula can be replaced by barium carbonate or barium nitrate or barium oxala...
Embodiment 2
[0070] According to the reaction formula: Synthetic compound Pb 0.78 Ba 8.22 B 18 o 36 ;
[0071] BaCO 3 , PbO, H 3 BO 3 Weigh the raw materials directly according to the molar ratio of 8.22:0.78:18, and combine the weighed raw materials with flux H 3 BO 3 Mix according to a molar ratio of 1:3, put it into an open platinum crucible of Φ80mm×80mm, heat it to 900°C at a heating rate of 30°C / h, keep the temperature for 15 hours to obtain a mixed solution, and 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 750°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 lead-barium-boron-oxygen seed crystals are obtained;
[0072] The barium carbonate in the reaction formula can be replaced by barium oxide or barium nitrate or barium oxala...
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