a bi 4 br 4 preparation method
A direct-top, temperature-controlled technology, applied in the field of preparation of infrared photoelectric detection material Bi4Br4, can solve the problems of unfavorable production and preparation, long growth cycle, easy decomposition, etc., and achieve the effect of easy promotion, less impurity content and safe preparation process
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Embodiment 1
[0024] Step 1. Elemental Bi and BiBr with a purity of 99.99% 3 Mix according to the mass ratio of 10:1, and put the mixed raw materials of the two into the bottom of the quartz tube with one end closed and one end open, and then put 5mm long quartz wool directly above the mixed raw materials; connect the open end of the quartz tube to On the molecular pump unit, use the molecular pump unit to pump the vacuum inside the quartz tube to 10 -3 After Pa, the open end of the quartz tube is closed by the method of oxygen welding and fused quartz tube;
[0025] Step 2. Place the sealed quartz tube vertically in the muffle furnace, and one end of the quartz tube containing the mixed raw materials (that is, the closed end of the quartz tube) is in contact with the bottom end of the muffle furnace; first raise the temperature to 310°C, and keep it warm for 6 hours , then lower the temperature to 271°C at a rate of 1°C / h, and keep it warm for 2h;
[0026] Step 3. After the heat preserva...
Embodiment 2
[0030] Step 1. Elemental Bi and BiBr with a purity of 99.999% 3 Mix according to the mass ratio of 20:1, and put the mixed raw material of the two into the bottom of the quartz tube with one end closed and one end open, and then put 10mm long quartz wool directly above the mixed raw material; connect the open end of the quartz tube to On the molecular pump unit, use the molecular pump unit to pump the vacuum inside the quartz tube to 10 - 5 After Pa, the open end of the quartz tube is closed by the method of oxygen welding and fused quartz tube;
[0031] Step 2. Place the sealed quartz tube vertically in the muffle furnace, and one end of the quartz tube with mixed raw materials (that is, the closed end of the quartz tube) is in contact with the bottom end of the muffle furnace; first raise the temperature to 500°C, and keep it warm for 10 hours , then lower the temperature to 294°C at a rate of 2°C / h, and keep it warm for 5h;
[0032] Step 3. After the heat preservation at...
Embodiment 3
[0036] Step 1. Elemental Bi and BiBr with a purity of 99.5% 3 Mix according to the mass ratio of 15:1, and put the mixed raw material of the two into the bottom of the quartz tube with one end closed and one end open, and then put 7mm long quartz wool directly above the mixed raw material; connect the open end of the quartz tube to On the molecular pump unit, use the molecular pump unit to pump the vacuum inside the quartz tube to 10 -4 After Pa, the open end of the quartz tube is closed by the method of oxygen welding and fused quartz tube;
[0037] Step 2. Place the sealed quartz tube vertically in the muffle furnace, and one end of the quartz tube with mixed raw materials (that is, the closed end of the quartz tube) is in contact with the bottom end of the muffle furnace; first raise the temperature to 420°C, and keep it warm for 8 hours , then lower the temperature to 280°C at a rate of 1.5°C / h, and keep it warm for 4h;
[0038] Step 3. After the heat preservation at 280...
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