Melt growth process of sodium borophosphate crystal
A technology of melt growth and sodium borophosphate, applied in the directions of crystal growth, single crystal growth, single crystal growth, etc., can solve the problem that the melt growth of single crystal has not yet been reported, and achieves easy processing and storage, low viscosity , the effect of facilitating ion transport
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Embodiment 1
[0025] Preparation of powdered Na 5 [B 2 P 3 o 13 ] compound:
[0026] 132.5 g Na 2 CO 3 and 172.95 g NH 4 h 2 PO 4 and 61.83 g H 3 BO 3 After mixing evenly (the molar ratio of Na, B and P contained in the mixture is 5:2:3), place it in an open platinum crucible of Φ80×60mm, put the crucible in a muffle furnace (heating electric furnace), After slowly raising the temperature to 450°C, grind it; put it into a furnace and raise the temperature to 700°C, keep the temperature constant for 48 hours to sinter, and grind to obtain powder after cooling, do powder X-ray diffraction on it, and compare with Na in the ICSD database 5 [B2 P 3 o 13 ] powder X-ray diffraction line for comparison, the results show that the obtained powder is Na 5 [B 2 P 3 o 13 ] compound powder.
Embodiment 2
[0028] Preparation of Na by pulling method 5 [B 2 P 3 o 13 ] crystal:
[0029] Na obtained in embodiment 1 5 [B 2 P 3 o 13 ]Put the powder in a Φ60×40mm open platinum crucible, put the crucible into a crystal pulling furnace, heat up to 850°C (melting), keep the temperature for 20 hours, cool down to 10°C above the saturation point temperature, and place the seeds in the c direction The crystal is fixed on the lower end of the seed rod with a platinum wire, so that the seed crystal is in contact with the liquid surface of the melt; after 5 minutes, the temperature is lowered to the saturation temperature, the rotation speed of the seed rod is 15rpm, the pulling speed is 1.0mm / h, and the temperature gradient in the growth zone 30°C / cm; increase the pulling speed at the end of the growth, so that the crystal is separated from the melt surface, and anneal at a rate of 50°C / hr to room temperature to obtain the Na 5 [B 2 P 3 o 13 ] crystal. The preparation period of the...
Embodiment 3
[0031] Preparation of Na by pulling method 5 [B 2 P 3 o 13 ] crystal:
[0032] Na obtained in embodiment 1 5 [B 2 P 3 o 13 ]Put the powder in an open platinum crucible of Φ60×40mm, put the crucible into the crystal pulling furnace, heat up to melting, keep the temperature for 20 hours, cool down to 10°C above the saturation point temperature, and wrap the seed crystal in the b direction with a platinum wire Fix the seed crystal at the lower end of the rod, so that the seed crystal is in contact with the liquid surface of the melt; after 10 minutes, cool down to the saturation temperature, the rotation speed of the seed crystal rod is 9rpm, the pulling speed is 0.8mm / h, and the temperature gradient in the growth zone is 20℃ / cm; increase the pulling speed at the end of the growth, so that the crystal is separated from the melt surface, and anneal at a rate of 50°C / hr to room temperature to obtain the Na in this example 5 [B 2 P 3 o 13 ] crystal. The preparation peri...
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