tm for solar spectral modulation 3+ /yb 3+ Double doped α‑nayf 4 Single crystal and preparation method thereof
A solar spectrum and double-doping technology, which is applied in the field of Tm3+/Yb3+ double-doped α-NaYF4 single crystal and its preparation, can solve the problems of poor stability and performance of glass materials, and achieve good thermal, low matrix phonon energy, and luminescence high efficiency effect
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Embodiment 1
[0024] Weigh NaF, KF, YF with a purity greater than 99.99% 3 , TmF 3 , YbF 3 Raw materials, by molar ratio NaF: KF: (YF 3 +TmF 3 +YbF 3 )=1.6:1:2.8, and TmF 3 : YbF 3 =1:12, YF 3 :(TmF 3 +YbF 3 )=1:0.0695, put the raw materials in the grinder, grind and mix for 5.5 hours to obtain a mixture of uniform powder; put the mixture in a boat-shaped platinum crucible, and then install the boat-shaped platinum crucible on the tubular resistor in the platinum tube of the furnace, and then use high-purity N 2 Gas removes the air in the platinum pipe, and conducts leak detection on the platinum pipe; then gradually raises the temperature of the furnace body of the tubular resistance furnace to 790°C, passes HF gas, and reacts for 2 hours to remove possible H 2 O and oxyfluoride, during the reaction process, use NaOH solution to absorb HF gas in the tail gas. After the reaction, stop passing HF gas, close the tube resistance furnace, and finally use high-purity N 2 The gas remov...
Embodiment 2
[0029] Substantially the same as Example 1, the difference is only in molar ratio NaF: KF: (YF 3 +TmF 3 +YbF 3 )=1.6:1:2.8, and TmF 3 : YbF 3 =1:4, YF 3 :(TmF 3 +YbF 3 )=1:0.0256, the raw materials are placed in a mill, and milled and mixed for 5 hours to obtain a mixture of uniform powder; after the raw materials are mixed, they are placed in a mill, and then the temperature of the furnace body of the tubular resistance furnace is gradually increased To 800°C, pass HF gas, the reaction time is 2 hours, the furnace temperature is 970°C, the inoculation temperature is 840°C, the temperature gradient of the solid-liquid interface is 80°C / cm, the crystal growth rate is 0.2mm / h, and the furnace temperature drops to At 80°C / h, transparent crystals were obtained. Analysis and Detection of Tm in Crystal by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP) 3+ , Yb 3+ The actual molar content of rare earth ions, x = 0.0048, y = 0.0196, and the crystal chemical form...
Embodiment 3
[0031] Substantially the same as Example 1, the difference is only in molar ratio NaF: KF: (YF 3 +TmF 3 +YbF 3 )=1.6:1:2.8, and TmF 3 : YbF 3 =1:8, YF 3 :(TmF 3 +YbF 3 )=1:0.0989, the raw materials are placed in a mill, and milled and mixed for 5 hours to obtain a mixture of uniform powder; after the raw materials are mixed, they are placed in a mill, and then the temperature of the furnace body of the tubular resistance furnace is gradually increased To 770°C, pass HF gas, the reaction time is 5 hours, the furnace temperature is 950°C, the inoculation temperature is 820°C, the temperature gradient of the solid-liquid interface is 60°C / cm, the crystal growth rate is 0.6mm / h, and the furnace temperature drop temperature is 20°C / h, transparent crystals were obtained. Analysis and Detection of Tm in Crystal by Inductively Coupled Plasma Atomic Emission Spectrometry (ICP) 3+ , Yb 3+ The actual molar content of rare earth ions, x=0.0049, y=0.0398, and the crystal chemical ...
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