Compound lead barium bromoborate and lead barium bromoborate optical crystal, preparation method and use
An optical crystal, bromoboric acid technology, applied in chemical instruments and methods, boron compounds, boron oxide compounds, etc., can solve the problems of low transmittance, low birefringence, and unsuitability for Glan prisms.
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Embodiment 1
[0033] According to the chemical equation: 6PbO+2BaCO 3 +5H 3 BO 3 +NH 4 Br→Pb 6 Ba 2 (BO 3 ) 5 Br+8H 2 O↑+2CO 2 ↑+NH 3 ↑Synthesis of lead barium bromoborate:
[0034] a. PbO, BaCO 3 、H 3 BO 3 and NH 4 Put Br into a mortar at a molar ratio of 6:2:5:1, mix and grind thoroughly, then put it into a corundum crucible, press it tightly, put it into a muffle furnace, slowly raise the temperature to 300°C, and keep the temperature constant for 15 hours , take out the crucible after cooling to room temperature, take out the sample and grind it evenly, then place it in the crucible, raise the temperature to 400°C, keep the temperature constant for 15 hours, take it out after cooling down to room temperature, grind it evenly again and put it in the crucible, put the muffle The temperature of the furnace was raised to 530°C, and after 72 hours of constant temperature, the sample was taken out and ground to obtain a single-phase polycrystalline powder of lead barium bromobor...
Embodiment 2
[0041] Embodiment 2, by reaction formula PbBr 2 +11PbO+4BaCO 3 +10H 3 BO 3 →2Pb 6 Ba 2 (BO 3 ) 5 Br+15H 2 O↑+4CO 2 ↑Synthetic compound Pb 6 Ba 2 (BO 3 ) 5 Br, the specific operation steps are the same as in Example 1 step a;
[0042] b. Put the compound lead barium bromoborate single-phase polycrystalline powder into a Φ50mm×50mm platinum crucible, heat to a temperature of 700°C, and keep the temperature for 5h to obtain lead barium bromoborate Pb 6 Ba 2 (BO 3 ) 5 Br melt;
[0043] c. Slowly cool the lead barium bromoborate melt obtained in step b to room temperature at a rate of 2°C / h to obtain seed crystals;
[0044] d. Cool the melt in step b to 592°C, fix the seed crystal obtained in step c on the seed rod, put it into contact with the surface of the melt from the top of the crystal growth furnace, and keep it warm for 20 minutes;
[0045] e. Cool the melt in step d to 589°C, rotate the seed rod at a speed of 10r / min, and grow crystals under the condition...
Embodiment 3
[0048] According to the reaction formula 12PbO+4BaCO 3 +5B 2 o 3 +2NH 4 Br→2Pb 6 Ba 2 (BO 3 ) 5 Br+H 2 O↑+4CO 2 ↑+2NH 3 ↑Synthetic compound Pb 6 Ba 2 (BO 3 ) 5 Br, the specific operation steps are the same as in Example 1 step a;
[0049] b. Put the compound lead barium bromoborate single-phase polycrystalline powder into a Φ30mm×30mm platinum crucible, heat to a temperature of 740°C, and keep the temperature for 10h to obtain a lead barium bromoborate melt;
[0050] c. Lower the lead barium bromoborate melt obtained in step b to room temperature at a rate of 0.5°C / h, and crystallize to obtain seed crystals;
[0051] d. Lower the temperature of the melt in step b to 600°C, fix the seed crystal obtained in step c on the seed rod, extend it into the melt from the top of the crystal growth furnace, and keep it warm for 30 minutes;
[0052] e. Cool the melt in step d to 593°C, rotate the seed rod at a speed of 30r / min, and then grow crystals under the condition of s...
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