Glass film containing rare-earth-ion-doped lithium iodide microcrystalline and preparation method thereof
A rare earth ion and glass thin film technology, which is applied in the field of rare earth ion doped lithium iodide microcrystal glass thin film and its sol-gel preparation field, can solve problems such as device development limitations, overcome incomplete uniformity, and prevent decomposition High effect with volatilization and high transmittance
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Embodiment 1
[0040] The preparation method of the glass film containing rare earth ion-doped lithium iodide microcrystals comprises the following specific steps:
[0041] (1) The preparation raw materials are in molar ratio: tetraethoxygermanium: niobium ethylate: lithium iodide: cerium iodide=79: 24: 8: 1, take by weighing each preparation raw material that total amount is the analytical purity of 20 grams, stand-by;
[0042] (2), the hydrolysis of tetraethoxygermanium: the tetraethoxygermanium weighed in the step (1) is dissolved in dehydrated alcohol, and the mol ratio of dehydrated alcohol and tetraethoxygermanium is 2.5: 1, fast Add acetylacetone, the volume ratio of tetraethoxygermanium to acetylacetone is 0.8:1, and carry out strong magnetic stirring, gradually drop distilled water, the molar ratio of distilled water to tetraethoxygermanium is 0.8:1, adjust with concentrated nitric acid The pH value reaches 4-5, and the hydrolysis reaction is carried out at room temperature for 1 h...
Embodiment 2
[0051] It is basically the same as Example 1, except that in the step (1), the raw materials are prepared according to the following molar ratios: tetraethoxygermanium: niobium ethylate: lithium iodide: europium iodide=76: 16: 12: 4, respectively Weigh each raw material for preparation; in step (7), the pulling speed of the glass substrate in the gel solution is controlled at 1 mm / s, and the pulling is repeated 5 times, and the interval between each pulling is 15 minutes; step (8) In the process, the temperature is raised to 100°C at a rate of 50°C per hour, and then the furnace is heated to 340°C at a rate of 50°C per hour; in step (9), the furnace is gradually heated to 380°C, and the reaction is carried out 1 hour, the molar composition of the obtained glass film is: 76GeO 2 -8Nb 2 o 5 -12LiI-4EuI 3 .
[0052] For prepared Eu-containing 3+ Ion-doped lithium iodide microcrystalline glass film was tested for performance, and the XRD pattern of the glass film after hydrog...
Embodiment 3
[0054] It is basically the same as Example 1, except that in the step (1), the raw materials are prepared according to the following molar ratios: tetraethoxygermanium: niobium ethylate: lithium iodide: terbium iodide=78: 20: 10: 2, respectively Weigh each raw material for preparation; in step (7), the pulling speed of the glass substrate in the gel solution is controlled at 0.6 mm / s, and the pulling is repeated 3 times, and the interval between each pulling is 15 minutes; step (8) In the process, the temperature is raised to 100°C at a rate of 40°C per hour, and then the furnace is heated to 340°C at a rate of 40°C per hour; in step (10), the furnace is gradually heated to 370°C, and the reaction is carried out After 2 hours, the molar composition of the obtained glass film is: 78GeO 2 -10Nb 2 o 5 -10LiI-2TbI 3 .
[0055] For prepared Tb-containing 3+ Ion-doped lithium iodide microcrystalline glass film was tested for performance, and the XRD pattern of the glass film af...
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