Large size vanadium sodium borate nonlinear optical crystal, and preparation and use thereof
A kind of nonlinear optics, sodium borate technology, applied in nonlinear optics, chemical instruments and methods, optics, etc., can solve the detailed report of the single crystal structure of the compound that has not been seen or seen, and the crystal cannot be purchased in the market. And other issues
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Embodiment 1
[0042] Take reaction formula (1) as an example: but not limited to reaction formula (1)
[0043] Na 2 O+H 3 BO 3 +V 2 O 5 →Na 3 B 6 VO 13 +H 2 O↑ Synthetic Na 3 B 6 VO 13 Compound, the specific steps are as follows:
[0044] Will Na 2 O, H 3 BO 3 , V 2 O 5 Put it into a mortar at the stoichiometric ratio, mix and grind it carefully, then put it into an open corundum crucible of Φ200mm×200mm, press it tightly, put it in a muffle furnace, slowly heat up to 450℃, keep the temperature for 5 hours, try to Drive out the gas, take out the crucible after cooling, grind the sample evenly, place it in the crucible, and keep the temperature at 600°C for 5 hours in the muffle furnace. After the temperature drops to room temperature, take it out, grind carefully, and keep it at 630°C again. After cooling for 24 hours, put it in a mortar and grind slightly to obtain sintered sodium borate vanadium Na 3 B 6 VO 13 Compound, and then X-ray analysis of the product, the obtained X-ray spectrum is co...
Embodiment 2
[0053] Take reaction formula (2) as an example: but not limited to reaction formula (2)
[0054] Na 2 CO 3 +B 2 O 3 +V 2 O 5 →Na 3 B 6 VO 13 +CO 2 ↑Synthetic Na 3 B 6 VO 13 Compound, the specific operation steps were carried out according to Example 1;
[0055] Na will be synthesized 3 B 6 VO 13 Compound and flux Na 2 CO 3 : V 2 O 5 =1:1.5:1.5 for mixing, put it into an open platinum crucible of Φ100mm×100mm, raise the temperature to 1000°C, and then cool it down to 655°C after 100 hours at a constant temperature. The Na cut along the b axis 3 B 6 VO 13 The seed crystal is fixed on the lower end of the seed crystal rod with 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 revolutions per minute. The temperature is kept constant for 1 hour, and the temperature is quickly cooled to 645°C. Then, the temperature is lowered at a rate of 2...
Embodiment 3
[0063] Take reaction formula (4) as an example: but not limited to (4)
[0064] NaNO 3 +V 2 O 5 +H 3 BO3 →Na 3 B 6 VO 13 +NO 2 ↑+O 2 ↑Synthetic Na 3 B 6 VO 13 Compound, the specific operation steps were carried out according to Example 1;
[0065] Na will be synthesized 3 B 6 VO 13 Compound and flux NaNO 3 : V 2 O 5 Mix according to the molar ratio of 1:3:2, put it into an open platinum crucible of Φ110mm×110mm, raise the temperature to 920°C, and cool down to 650°C after 50 hours of constant temperature. The Na cut along the a-axis 3 B 6 VO 13 The seed crystal is fixed on the lower end of the seed rod with 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 revolutions per minute. The temperature is kept constant for 1 hour, and the temperature is quickly reduced to 645°C. Then, the temperature is lowered at a rate of 1°C / day. After th...
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