Method for preparing Cr<3+>, Nd<3+>:YVO4 crystal and Cr<4+>, Nd<3+>:YVO4 crystal

Abstract

The invention relates to the field of laser materials, in particular to a method for preparing a Cr3+, Nd3+:YVO4 crystal and a Cr4+, Nd3+:YVO4 crystal. The method mainly comprises two steps of synthesis of polycrystal materials and growth of the crystal. The synthesis of the polycrystal materials adopts a solid phase method or a liquid phase method. The growth of the crystal comprises the following steps of: D, melting of the crystal, namely melting sintered polycrystalline ingots at a certain temperature, cleaning seed crystal and keeping melts at the temperature for a period of time; E, drawing growth of the crystal, namely reducing certain temperature, and starting the growth of the crystal at a certain drawing speed and rotary speed; and F, annealing of the crystal, namely drawing the crystal out of the liquid level, and cooling the crystal to the room temperature at a certain cooling rate in stages. By the drawing method, the crystal with large size and high quality can be easily grown, and has high growing speed and good optical characteristics.

Description

technical field

[0001] The invention relates to the field of laser materials, in particular to Cr 3+ 、Nd 3+ :YVO 4 Crystal and Cr 4+ 、Nd 3+ :YVO 4 Crystal preparation method. Background technique

[0002] Yttrium vanadate (YVO 4 ) crystal has the characteristics of good chemical stability, excellent mechanical properties and high laser damage threshold, and is an excellent laser crystal matrix material. doped active ion Nd 3+ Formed Nd:YVO 4 Laser crystals are the preferred materials for making miniaturized, high-efficiency, and low-threshold LD pump lasers, and have been widely used in LD pump lasers.

[0003] Cr 3+ Ion is an important center-luminescent ion, and solid-state lasers such as Cr 3+ :Al 2 o 3 , (Ruby), Cr 3+ :BeAl 2 o 4 (Alexandrite), etc., which can tunably output lasers of different wavelengths in the visible and near-infrared bands, have been widely used in medicine and distance measurement. Due to Cr 3+ The fluorescent emission of the ions...

Examples

Embodiment 1

[0056] Raw material Y with a purity of 99.99% 2 o 3 、Nd 2 o 3 , CaO and Cr 2 o 3 Dried at 800°C to remove water, the raw material V with a purity of 99.9% 2 o5 Dry at 150°C to remove water. Weigh the raw material after drying and removing water: 445.97g of Y 2 o 3 , 20.16g of Nd 2 o 3 , 3.04g of Cr 2 o 3 , 3.36g CaO and 360.36g of V 2 o 5 , Put the raw materials into an agate mortar and grind them thoroughly, mix them evenly, press them into billets with 2000kg of hydrostatic pressure, put the billets into a Φ100mm clean corundum cup, heat them in a silicon carbide rod furnace to 1200°C, Insulated for 24 hours to carry out solid phase reaction to form (Ca, Cr, Nd): YVO 4 polycrystalline blocks. Use DJL-400 single crystal furnace to grow crystals, use intermediate frequency induction heating, use Φ70mm iridium gold crucible to hold the obtained polycrystalline block, the growth atmosphere is high-purity nitrogen (pressure 0.04MPa), and use pure YVO 4 For the see...

Embodiment 2

[0058] Raw material Y with a purity of 99.99% 2 o 3 、Nd 2 o 3 Dry at 800°C to remove water, CaCO 3 Dried at 200°C to remove water, the raw material Cr(NO 3 ) 3 and NH 4 VO 3 Dry and set aside. Weigh the raw material after drying and removing water: 426.39g of Y 2 o 3 , 33.6g of Nd 2 o 3 , 19.04g of Cr(NO 3 ) 3 , 8g of CaCO3 and 229.32g of NH 4 VO 3 , the Cr(NO 3 ) 3 and NH 4 VO 3 Dissolve in distilled water at 80-90°C to obtain a solution; Y 2 o 3 、Nd 2 o 3 , CaCO 3 Dissolve in dilute nitric acid at 80-90°C to obtain nitric acid; mix and react the above two solutions at 60-70°C to obtain a precipitate, and control the pH value of the solution to 7.0-7.5. The resulting precipitate was left to stand, centrifuged, dried, and then pressed into tablets. Put the billet into a Φ100mm clean corundum cup, heat it in a silicon carbide rod furnace to 1000°C, and keep it warm for 24 hours to form (Ca, Cr, Nd):YVO 4 polycrystalline blocks. Use DJL-400 single crys...

technical field

[0001] The invention relates to the field of laser materials, in particular to Cr 3+ 、Nd 3+ :YVO 4 Crystal and Cr 4+ 、Nd 3+ :YVO 4 Crystal preparation method. Background technique

[0002] Yttrium vanadate (YVO 4 ) crystal has the characteristics of good chemical stability, excellent mechanical properties and high laser damage threshold, and is an excellent laser crystal matrix material. doped active ion Nd 3+ Formed Nd:YVO 4 Laser crystals are the preferred materials for making miniaturized, high-efficiency, and low-threshold LD pump lasers, and have been widely used in LD pump lasers.

[0003] Cr 3+ Ion is an important center-luminescent ion, and solid-state lasers such as Cr 3+ :Al 2 o 3 , (Ruby), Cr 3+ :BeAl 2 o 4 (Alexandrite), etc., which can tunably output lasers of different wavelengths in the visible and near-infrared bands, have been widely used in medicine and distance measurement. Due to Cr 3+ The fluorescent emission of the ions...

Examples

Embodiment 1

[0056] Raw material Y with a purity of 99.99% 2 o 3 、Nd 2 o 3 , CaO and Cr 2 o 3 Dried at 800°C to remove water, the raw material V with a purity of 99.9% 2 o5 Dry at 150°C to remove water. Weigh the raw material after drying and removing water: 445.97g of Y 2 o 3 , 20.16g of Nd 2 o 3 , 3.04g of Cr 2 o 3 , 3.36g CaO and 360.36g of V 2 o 5 , Put the raw materials into an agate mortar and grind them thoroughly, mix them evenly, press them into billets with 2000kg of hydrostatic pressure, put the billets into a Φ100mm clean corundum cup, heat them in a silicon carbide rod furnace to 1200°C, Insulated for 24 hours to carry out solid phase reaction to form (Ca, Cr, Nd): YVO 4 polycrystalline blocks. Use DJL-400 single crystal furnace to grow crystals, use intermediate frequency induction heating, use Φ70mm iridium gold crucible to hold the obtained polycrystalline block, the growth atmosphere is high-purity nitrogen (pressure 0.04MPa), and use pure YVO 4 For the see...

Embodiment 2

[0058] Raw material Y with a purity of 99.99% 2 o 3 、Nd 2 o 3 Dry at 800°C to remove water, CaCO 3 Dried at 200°C to remove water, the raw material Cr(NO 3 ) 3 and NH 4 VO 3 Dry and set aside. Weigh the raw material after drying and removing water: 426.39g of Y 2 o 3 , 33.6g of Nd 2 o 3 , 19.04g of Cr(NO 3 ) 3 , 8g of CaCO3 and 229.32g of NH 4 VO 3 , the Cr(NO 3 ) 3 and NH 4 VO 3 Dissolve in distilled water at 80-90°C to obtain a solution; Y 2 o 3 、Nd 2 o 3 , CaCO 3 Dissolve in dilute nitric acid at 80-90°C to obtain nitric acid; mix and react the above two solutions at 60-70°C to obtain a precipitate, and control the pH value of the solution to 7.0-7.5. The resulting precipitate was left to stand, centrifuged, dried, and then pressed into tablets. Put the billet into a Φ100mm clean corundum cup, heat it in a silicon carbide rod furnace to 1000°C, and keep it warm for 24 hours to form (Ca, Cr, Nd):YVO 4 polycrystalline blocks. Use DJL-400 single crys...