A kind of europium ion doped sodium gadolinium fluoride optical crystal and preparation method thereof
A technology of sodium gadolinium fluoride and optical crystals, which is applied in the field of europium ion-doped sodium gadolinium fluoride optical crystals and its preparation, and can solve problems affecting crystal utilization and quality, lack of original formula components, and uneven distribution of ions , to overcome the extremely uneven concentration distribution, improve optical performance and utilization, and reduce crystal stress
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Embodiment 1
[0024] Weigh raw materials NaF and 99.99% GdF with a purity greater than 99.99% 3 Raw material with 99.99% EuF 3 The raw materials are mixed according to the molar percentage of 56.0:43.59:0.41, placed in a grinder, milled and mixed for 5 hours to obtain a mixture of uniform powder; the mixture is fluffy placed in a boat-shaped platinum crucible, and then the boat-shaped platinum crucible is installed in the tube In the platinum pipe of the type resistance furnace, and then use high-purity N 2 Gas removes the air in the platinum pipeline, and conducts leak detection on the platinum pipeline; then gradually raises the furnace temperature of the tube resistance furnace to 750°C, passes HF gas, and reacts for 3 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 2The gas removes the residual HF gas...
Embodiment 2
[0026] It is basically the same as Example 1, except that NaF raw material is 56.0mol%, GdF 3 Raw material 41.2mol%, EuF 3 The raw material is 2.8mol%, the reaction time in the platinum tube is 5 hours, the temperature gradient of the solid-liquid interface is 65°C / cm, the crystal growth rate is 0.2mm / h, and the furnace temperature drop temperature is 80°C / h to obtain Eu 3+ doped NaGdF 4 crystals. Cutting and sampling, the X-ray diffraction pattern of the sample is similar to that of Example 1. The rare earth Eu in the single crystal 3+ The concentration is 2.78 mol%, α=0.0278. The obtained sample was polished into the same 2 mm thick sheet as in Example 1, and the same optical test conditions as in Example 1 were maintained, and the obtained fluorescence intensity was comparable to that of the sample in Example 1. Under the excitation of LD at 396nm, the fluorescence spectrum test was carried out, which produced four main bands of red fluorescence emission at ~591, 621, ...
Embodiment 3
[0028] It is basically the same as Example 1, except that NaF raw material is 56.0mol%, GdF 3 Raw material 39.2mol%, EuF 3 The raw material is 4.8mol%, the reaction time in the platinum tube is 4.5 hours, the temperature gradient of the solid-liquid interface is 70°C / cm, the crystal growth rate is 1.2mm / h, and the furnace temperature drop temperature is 65°C / h, and Eu 3+ doped NaGdF 4 crystals. Cutting and sampling, the X-ray diffraction pattern of the sample is similar to that of Example 1. The rare earth Eu in the single crystal 3+ The concentration is 4.76 mol%, α=0.0476. The obtained sample was polished into the same 2 mm thick sheet as in Example 1, and the same optical test conditions as in Example 1 were maintained, and the obtained fluorescence intensity was comparable to that of the sample in Example 1. Under the excitation of LD at 396nm, the fluorescence spectrum test was carried out, and red fluorescence emission in four main bands of ~591, 621, 650, and 705nm...
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