Preparation method of ytterbium-doped lutecium lithium fluoride crystal
A technology of lithium lutetium fluoride and crystals, which is applied in the field of laser crystal material preparation, can solve the problems of increased crystal growth costs, large and complex crystal growth process equipment, etc., and achieves the effects of low growth costs, simple equipment, and simple processes
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[0026] The preparation method of ytterbium-doped lutetium fluoride lithium crystal of the present invention includes the following steps:
[0027] ①Select LiF and LuF with purity greater than 99.99% 3 And YbF 3 , After selecting the value of x, do the batching according to the following formula,
[0028] LiF+xYbF 3 +(1-x)LuF 3 = Yb x :LiLu (1-x) F 4
[0029] Where x=0.1~35mol.%, the raw material of ytterbium-doped lutetium fluoride lithium crystal is formed after mixing;
[0030] ②After dehydrating the raw material at 200-300°C for 4-6 hours, add 0.05-0.1g of deoxidizer and mix it evenly, put it into a bottomed crucible with a wall thickness of 0.15-0.3mm, and seal it tightly;
[0031] ③ Put the crucible in the lowering furnace in the high temperature zone of 900~960℃ to melt the material for 4~6 hours, then the crucible will drop at a rate of 0.5~1.2mm / h, at this time the crystal solid-liquid interface is within ±0.5cm The temperature gradient inside is 25-40°C / cm, and after the growt...
Embodiment 1
[0033] Example 1: LiYb 0.001 Lu 0.999 F 4 Crystal growth
[0034] YbF 3 , LiF and LuF 3 According to the structural formula LiYb of the crystal of this embodiment 0.001 Lu 0.999 F 4 After the ingredients are mixed, they are dehydrated and dried at 200°C for 6 hours. Add 0.05g of carbon powder as a deoxidizer and mix evenly. Add them to a platinum crucible with a φ30×150 sharp bottom and seal the crucible. Put the crucible in the lowering furnace and place the crucible in the high temperature zone with a temperature of 900℃ for 5 hours, then the crucible is lowered at a rate of 1.2mm / h, and the crystal solid-liquid interface is within ±0.5cm The temperature gradient inside is 25°C / cm, and after the growth is completed, it is cooled to room temperature at a rate of 20°C / h.
Embodiment 2
[0035] Example 2: LiYb 0.05 Lu 0.95 F 4 Crystal growth
[0036] YbF 3 , LiF and LuF 3 According to the structural formula LiYb of the crystal of this embodiment 0.05 Lu 0.95 F 4 After the ingredients are mixed, they are dehydrated and dried at 250°C for 5 hours, and 0.05g of rubber is added as a deoxidizer to mix evenly, and put into a platinum crucible with a size of φ40×40×180 with a flat bottom with a wall thickness of 0.2mm. Put in pure LiLuF 4 The crystal is used as a seed crystal to seal the crucible. Put the crucible in the lowering furnace and place the crucible in the high temperature zone of 920℃ for 6 hours, then the crucible will drop at a rate of 0.8mm / h, and the crystal solid-liquid interface is within ±0.5cm The temperature gradient inside is 30°C / cm, and after the growth is completed, it is cooled to room temperature at a rate of 30°C / h. After the crystal is taken out, it is processed into 10×10×1mm along the a direction 3 Spectral test of samples, absorption spe...
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