Glass film containing rare-earth-ion-doped calcium iodide microcrystalline and preparation method thereof
A technology of rare earth ions and glass thin films, which is applied in the field of rare earth ion doped calcium iodide microcrystal glass thin films and its sol-gel preparation, can solve problems such as device development limitations, overcome incomplete uniformity, and promote the formation of , prevent the effect of decomposition and volatilization
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Embodiment 1
[0039] The preparation method of the glass film containing rare earth ion-doped calcium iodide microcrystals comprises the following specific steps:
[0040] (1) Prepare raw materials in molar ratio: tetraethoxygermanium: tri-n-butyl borate: calcium iodide: europium iodide = 70: 20: 16: 4, take by weighing a total amount of 20 grams of analytically pure Each preparation raw material, stand-by;
[0041] (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 1:1, and carry out strong magnetic stirring, gradually drop in 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 hour to prep...
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 ratio: tetraethoxygermanium: tri-n-butyl borate: calcium iodide: cerium iodide=74: 30: 10: 1, each preparation raw material is weighed respectively; In the 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; In (8), heat up to 100°C at a rate of 50°C per hour, then heat up the furnace to 340°C at a rate of 50°C per hour; in step (9), gradually heat up the furnace to 600°C, and at this temperature The next reaction treatment was 2 hours. The molar composition of the film composition is: 74GeO 2 -15B 2 o 3 -10CaI 2 -1CeI 3 .
[0052] For the prepared Ce-containing 3+ Ion-doped calcium iodide crystallite glass film was tested for performance, and the XRD pattern of the glass film after hydrogen iodide tre...
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 ratio: tetraethoxygermanium: tri-n-butyl borate: calcium iodide: terbium iodide=72: 28: 12: 2. Weigh each preparation raw material respectively; 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; In (8), heat up to 100°C at a rate of 40°C per hour, then heat up the furnace to 340°C at a rate of 40°C per hour; in step (10), gradually heat up the furnace to 590°C, and at this temperature The next reaction treatment was 3 hours. The molar composition of the film composition is: 72GeO 2 -14B 2 o 3 -12CaI 2 -2TbI 3 .
[0055] For prepared Tb-containing 3+ Ion-doped calcium iodide crystallite glass film was tested for performance, and the XRD pattern of the glass film after hydrogen iodide treatment wa...
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