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Thermal control Bridgman method single crystal growth device and method for fluoride single crystals

A growth device and single crystal technology, which is applied in the direction of single crystal growth, single crystal growth, crystal growth, etc., can solve the problems of unstable solid-liquid interface and difficulty in releasing latent heat of crystallization, so as to avoid the phenomenon of easy polycrystalline growth and strengthen the seed crystal Heat conduction effect, effect of enhancing water cooling effect

Inactive Publication Date: 2016-11-23
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

[0008] Aiming at the problems in the prior art that it is difficult to release latent heat of crystallization during the growth of fluoride single crystals, and the solid-liquid interface is often concave and unstable, the present invention aims to provide a thermally controlled Bridgman method for single crystal growth of fluoride single crystals Devices and methods to solve the problem of difficult release of latent heat of crystallization during the growth of large-sized fluoride single crystals; combined with reasonable process parameters, to ensure that the solid-liquid interface is always slightly convex as the crystal grows, improving the crystallization quality of fluoride single crystals

Method used

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  • Thermal control Bridgman method single crystal growth device and method for fluoride single crystals

Examples

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Effect test

Embodiment 1

[0049] growCaF 2 Single crystal, the specific preparation method is as follows:

[0050] 8Kg CaF 2 Crystal feedstock and 80g PbF 2 The powder is evenly mixed and loaded with CaF at the bottom 2 In the crucible 13 made of graphite of the crystal seed crystal, the crucible 13 is then fixed on the zirconia bracket 15 on the crucible water-cooled support column 19 inside the furnace chamber 1, wherein the PbF 2 as an oxygen scavenger. Raise the crucible 13 to an appropriate position in the high temperature zone A (the upper surface of the seed crystal is slightly higher than the heat shield 14), close the furnace chamber 1 and start vacuuming, when the vacuum degree is ≤5*10 -3 After pa, start to raise the temperature of the chemical material at a rate of 50°C / h; when the temperature of the monitoring thermocouple at the seed crystal reaches 800°C, keep the temperature for 10 hours to fully remove the oxygen component inside the crucible 13 . Then continue to heat up at a rat...

Embodiment 2

[0052] Growth of Yb,Na:CaF 2 Single crystal, the specific preparation method is as follows:

[0053] 6 Kg Yb, Na co-doped CaF 2 Crystal feedstock and 60g PbF 2 The powder is evenly mixed and loaded with CaF at the bottom 2 In the crucible 13 made of graphite of the crystal seed crystal, the crucible 13 is then fixed on the zirconia bracket 15 on the crucible water-cooled support column 19 inside the furnace chamber 1, wherein the PbF 2 as an oxygen scavenger. Raise the crucible 13 to an appropriate position in the high temperature zone A (the upper surface of the seed crystal is slightly higher than the heat shield 14), close the furnace chamber 1 and start vacuuming, when the vacuum degree is ≤5*10 -3 After pa, start to raise the temperature of the chemical material at a rate of 50°C / h; when the temperature of the monitoring thermocouple at the seed crystal reaches 800°C, keep the temperature for 10 hours to fully remove the oxygen component inside the crucible 13 . Then...

Embodiment 3

[0055] growSrF 2 Single crystal, the specific preparation method is as follows:

[0056] 8Kg SrF 2 Crystal feedstock and 80g PbF 2 The powder is evenly mixed and loaded with SrF at the bottom 2 In the crucible 13 made of graphite of the crystal seed crystal, the crucible 13 is then fixed on the zirconia bracket 15 on the crucible water-cooled support column 19 inside the furnace chamber 1, wherein the PbF 2 as an oxygen scavenger. Raise the crucible 13 to an appropriate position in the high temperature zone A (the upper surface of the seed crystal is slightly higher than the heat shield 14), close the furnace chamber 1 and start vacuuming, when the vacuum degree is ≤5*10 -3 After pa, start to raise the temperature of the chemical material at a rate of 50°C / h; when the temperature of the monitoring thermocouple at the seed crystal reaches 800°C, keep the temperature for 10 hours to fully remove the oxygen component inside the crucible 13 . Then continue to heat up at a rat...

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Abstract

The invention relates to a thermal control Bridgman method single crystal growth device and method for fluoride single crystals. A furnace body system is provided with a furnace cavity, a furnace bottom plate with a hole in the center, and a vacuum pipeline communicated with the furnace cavity, the hole in the center of the furnace bottom plate is communicated with a cavity body of the furnace cavity, the furnace cavity and the furnace bottom plate are both of a double-layer structure, and cooling water channels are distributed in interlayers. A heating and heat preservation system is arranged in the furnace cavity and provided with a heat insulation plate, heaters located on the upper side and the lower side of the heat insulation plate respectively and heat preservation screens located on the upper side and the lower side of the heat insulation plate respectively, and three temperature zones including the upper high temperature zone, the middle gradient zone and the lower low temperature zone are formed through the heat insulation plate. A crucible descending system comprises a crucible water cooling supporting pillar and a crucible descending transmission device, the lower end of the crucible water cooling supporting pillar is connected with the crucible descending transmission device, the upper end of the crucible water cooling supporting pillar penetrates through the hole in the center of the furnace bottom plate and stretches into the furnace cavity to support a crucible bracket, cooling water circulates in the crucible water cooling supporting pillar, and the flow and temperature of the cooling water in the crucible water cooling supporting pillar can be independently regulated and controlled in real time.

Description

technical field [0001] The invention belongs to the technical field of crystal growth, and in particular relates to a thermally controlled Bridgman method single crystal growth device and method for fluoride single crystals. Background technique [0002] Fluoride crystals (such as CaF 2 , SrF 2 , MgF 2 、BaF 2 and LaF 2 etc.) are very important solid-state laser matrix materials. Compared with oxide matrix materials, fluoride has the following characteristics: fluoride crystal has a very wide transmission range, from far ultraviolet to mid-infrared; the refractive index of fluoride crystal is relatively low, which can minimize the surface of the spectrum used Reflectivity and limiting nonlinear effects under high-intensity laser pumping; low phonon energy can reduce the probability of non-radiative transitions between energy levels and improve radiation quantum efficiency. Therefore, the fluoride crystal doped with trivalent rare earth ions is an ideal system for people...

Claims

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Application Information

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IPC IPC(8): C30B29/12C30B11/00
Inventor 姜大朋苏良碧钱小波唐飞徐军王静雅吴锋
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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