Rubidium lithium titanium germanate compound, rubidium lithium titanium germanate non-linear optical crystal and preparation methods and application thereof
A technology of nonlinear optics and lithium compounds, applied in the direction of nonlinear optics, germanium compounds, chemical instruments and methods, etc., can solve the problems of low crystal damage threshold, poor optical uniformity, high half-wave voltage, etc., and achieve large nonlinear optical effects , no deliquescent raw material cost, good physical and chemical properties
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Embodiment 1
[0047] a Rb 4 Li 2 TiGe 4 o 13 Compound, preparation method comprises the steps:
[0048] Prepared by solid phase reaction method, the reaction equation is 2Rb 2 CO 3 +Li 2 CO 3 +TiO 2 +4GeO 2 =Rb 4 Li 2 TiGe 4 o 13 ; The proportioning ratio of the above three reagents: Rb 2 CO 3 (4.6189g, 0.02mol), Li 2 CO 3 (0.7389, 0.01mol), TiO 2 (0.7987g, 0.01mol), GeO 2 (4.1844g, 0.04mol); Its specific preparation steps are: take reagent by weighing respectively by above-mentioned dosage, put them in mortar, grind and mix, then pack in platinum crucible, put into muffle furnace, with 50 The rate of ℃ / h is raised to 500 ℃ for pre-calcination, and then cooled for 24 hours. After cooling to room temperature, the sample is taken out and re-ground and mixed, and then placed in a muffle furnace for sintering at 800 ℃ for 48 hours to obtain polycrystalline Rb 4 Li 2 TiGe 4 o 13 compound.
Embodiment 2
[0050] Preparation of Rb by flux method 4 Li 2 TiGe 4 o 13 A nonlinear optical crystal, comprising the steps of:
[0051] LiF was used as a flux, and the molar ratio of solute to solvent was 1:0.5. Weigh 461.89 g of Rb respectively 2 CO 3 (2mol), 73.89 g Li 2 CO 3 (1mol), 79.87 grams of TiO 2 (1mol), 418.44 g GeO 2 (4mol) and 12.97 grams of LiF (0.5mol), after grinding and mixing in the mortar, melting in batches into the crucible of Φ80mm * 80mm; the crucible after the chemical material is put into the vertical crystal growth furnace, Raise the temperature to 900°C, stir at constant temperature for 48 hours, then cool down to 5°C above the saturation point, introduce the seed crystal and cool down at a rate of 0.5°C / day, and start crystal growth at a rotation speed of 10r / min. After the crystal growth is completed, lift the seed crystal Rod, lift the crystal from the liquid surface, and then cool down to room temperature at a rate of 20°C / h to obtain transparent Rb...
Embodiment 3
[0053] Preparation of Rb by Flux Top-Seed Method 4 Li 2 TiGe 4 o 13 A nonlinear optical crystal, comprising the steps of:
[0054] Use LiF-RbF as a flux, and the molar ratio of solute to solvent is 1:1:0.5. Weigh 230.959 grams of Rb respectively 2 CO 3 (1mol), 36.95 g Li 2 CO 3 (0.5mol), 39.94 grams of TiO 2 (0.5mol), 209.22 grams of GeO 2 (2mol), 12.97 grams of LiF (0.5mol) and 26.12 grams of RbF (0.25mol), after grinding and mixing in a mortar, they were melted in batches and loaded into a Φ70mm×70mm crucible; the crucible after the material was put into In the vertical crystal growth furnace, heat up to 800°C, stir at constant temperature for 48 hours, then cool down to 10°C above the saturation point, introduce seed crystals, make the seed crystals just contact with the liquid surface, and then cool down at a rate of 0.5°C / day , the rotation speed is 25r / min to start crystal growth, after the crystal growth is completed, the crystal is lifted from the liquid surf...
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