Large-size Yb,R:CaF2/SrF2 laser crystal and preparation method thereof

A technology of laser crystal and crystal growth, which is applied to lasers, crystal growth, laser components, etc. It can solve the problems of low fluorescence quantum efficiency and difficult crystal preparation, and achieve the effects of reducing temperature gradient, reducing thermal stress, and inhibiting cracking

Inactive Publication Date: 2018-02-27
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention is aimed at Yb in the prior art 3+ ions in CaF 2 or SrF 2 It is easy to form a cluster structure in the crystal, which leads to low fluorescence quantum efficiency, and the technical problem that it is difficult to prepare large-diameter (diameter ≥ 4 inches) crystals. The purpose is to provide a new Yb,R:CaF 2 / SrF 2 Crystal and its preparation method

Method used

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  • Large-size Yb,R:CaF2/SrF2 laser crystal and preparation method thereof
  • Large-size Yb,R:CaF2/SrF2 laser crystal and preparation method thereof
  • Large-size Yb,R:CaF2/SrF2 laser crystal and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0050] Growth Yb,Y:CaF 2 Laser crystal, the specific preparation method is as follows:

[0051] Select high-purity (99.99%) YbF 3 , YF 3 and CaF 2 As a raw material, 12kg is prepared in a molar ratio of 0.03:0.05:1, and 0.5wt% of PbF is added at the same time 2 Mix well after being used as an oxygen scavenger; choose CaF in the direction of Φ35mm×40mm[111] 2 The crystal is used as the seed crystal, and the 30mm thick graphite felt is used as the heat shield. Put the seed crystal and raw materials into the graphite crucible together, then place it on the crucible water-cooled support rod and fix it, then raise the crucible to the appropriate position in the gradient area (the upper end surface of the seed crystal is parallel to the upper surface of the heat shield), and the closed furnace chamber starts to pump Vacuum, when vacuum degree≤5×10 -3 After pa, start to heat up the chemical material at a rate of 50°C / h; when the temperature of the monitoring thermocouple at the...

Embodiment 2

[0053] Growth of Yb,La:CaF 2 Laser crystal, the specific preparation method is as follows:

[0054] Select high-purity YbF 3 、LaF 3 and CaF 2 As a raw material, 15kg is prepared in a molar ratio of 0.02:0.05:1, and 0.8wt% of PbF is added at the same time 2 After being used as an oxygen scavenger, mix well; choose CaF in the direction of Φ40mm×40mm[111] 2 The crystal is used as the seed crystal, and the 50mm thick medium-coarse graphite is used as the heat shield. Put the seed crystal and the raw material into the graphite crucible together, then place it on the crucible water-cooled support rod and fix it, then lift the crucible to the appropriate position in the gradient area (the upper end surface of the seed crystal is 10mm higher than the upper surface of the heat shield), and the closed furnace chamber starts Vacuuming, when the vacuum degree is ≤5×10 -3 Pa filled with high-purity Ar and CF 4 The mixed gas (ratio: 0.95:0.05) was used as a protective atmosphere, and...

Embodiment 3

[0056] Growth of Yb,Gd:CaF 2 Laser crystal, the specific preparation method is as follows:

[0057] Select high-purity YbF 3 , GdF 3 and CaF 2 As a raw material, 15kg is prepared in a molar ratio of 0.05:0.05:1, and 0.5wt% of PbF is added at the same time 2 Mix well after being used as an oxygen scavenger; choose CaF in the direction of Φ50mm×40mm[111] 2 The crystal is used as the seed crystal, and the 40mm thick medium-coarse graphite is used as the heat shield. Put the seed crystal and the raw material into the graphite crucible together, then place it on the crucible water-cooled support rod and fix it, then lift the crucible to the appropriate position in the gradient area (the upper end surface of the seed crystal is 10mm higher than the upper surface of the heat shield), and the closed furnace chamber starts Vacuuming, when the vacuum degree is ≤5×10 -3 Pa filled with high-purity Ar and CF 4 The mixed gas (ratio: 0.95:0.05) was used as a protective atmosphere, and...

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Abstract

The invention relates to large-size Yb,R:CaF2 / SrF2 laser crystal and a preparation method thereof. The preparation method comprises the steps: (1) charging a seed crystal and crystal growth raw material in the specific direction into a crucible of a crystal growth device, wherein the crystal growth device comprises an upper heating body, a lower heating body and a thermal insulation plate arrangedbetween the upper heating body and the lower heating body, a high temperature area is arranged above the thermal insulation plate, a low temperature area is arranged under the thermal insulation plate, a gradient area is arranged near the thermal insulation plate, and the crystal grow raw material is arranged in the high temperature area; (2) sealing a furnace chamber of the crystal growth device, warming to melt the material after vacuumizing, then inoculating at a constant temperature and descending the crucible to make the crystal growth raw material move from the high temperature area tothe low temperature area through the gradient area after the crystal growth raw material is fully molten to make the crystal grow; (3) stopping descending the crucible after the crystal growth finishes, reducing a temperature of the high temperature area to be equal to a temperature of the low temperature area and synchronously cooling the high temperature area and the low temperature area to roomtemperature in a stage mode.

Description

technical field [0001] The invention relates to a large diameter Yb,R:CaF 2 / SrF 2 Laser crystal and its growth device and method, specifically relates to the preparation of large-size (diameter ≥ 4 inches) Yb,R:CaF by using an improved high-vacuum Bridgman method growth device 2 / SrF 2 A laser crystal method belongs to the technical field of crystal growth. Background technique [0002] All-solid-state lasers are rapidly developing towards the practical direction of high power, multi-wavelength, wide tuning, long life, high stability, etc. Among them, ultrafast femtosecond laser gain media and amplified laser crystals suitable for diode laser (LD) pumping have become One of the mainstream directions of development. Femtosecond laser has four characteristics of ultra-short pulse, high repetition rate, high peak power and wide spectrum, which promotes the development of information science, physics, chemistry, biology and material science to a deeper level, and is widely ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/12C30B11/00H01S3/16
CPCC30B29/12C30B11/00H01S3/1603
Inventor 姜大朋苏良碧唐飞吴庆辉王静雅钱小波马凤凯
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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