Fluxing agent for crystal growth and crystal growth method

A technology of crystal growth and flux, applied in the direction of crystal growth, single crystal growth, single crystal growth, etc., can solve the problems that crystals are easy to crack and difficult to meet physical property tests

Inactive Publication Date: 2020-07-07
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to Pb 17 o 8 Cl 18 The crystal is a molten compound with the same composition. The previous report used the method of spontaneous nucleation for crystal growth, but the grown crystals are all partially transparent, and there are a large number of macroscopic inclusions in the crystal. The grown crystal is easy to crack, which is difficult to meet Physical property test

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh PbO and PbCl according to stoichiometric ratio 2 , fully ground and mixed, and then transferred to an alumina ceramic crucible. In a muffle furnace, first sinter at 420°C for 24 hours. After cooling to room temperature, the obtained product was ground again and transferred to an alumina ceramic crucible, and then sintered in a muffle furnace at 480°C for 24 hours. Take it out after naturally cooling to room temperature to get Pb 17 o 8 Cl 18 polycrystalline material. will Pb 17 o 8 Cl 18 Polycrystalline raw material and flux PbCl 2 、LiF 2 Mix evenly according to the molar ratio of 65:35, grind and mix the weighed raw materials evenly, and melt them directly in a platinum crucible of Φ100mm×75mm, put the crucible containing the molten material into the molten salt furnace, and use the heat preservation material Seal the opening at the top of the furnace, leave a small hole at the position corresponding to the top of the furnace and the center of the cruci...

Embodiment 2

[0026] With stoichiometric ratio of PbO and PbCl 2 Mix the powder evenly, put it into an alumina ceramic crucible, cover it and place it in a muffle furnace, keep it warm at 470°C for 48 hours, take it out after natural cooling to room temperature, and get Pb 17 o 8 Cl 18 polycrystalline material. will Pb 17 o 8 Cl 18 Polycrystalline material and PbF 2 , PbCl 2 Mix evenly according to the molar ratio of 55:45. After grinding and mixing the weighed raw materials evenly, put the ground POC polycrystalline material into a Φ100mm×75mm platinum crucible, and place the charged crucible in a molten salt furnace. The upper opening of the crucible is covered with a crucible lid, the furnace temperature is controlled to be 575° C., the raw materials are completely melted, and the temperature is kept constant for 18 hours to make the high-temperature solution completely uniform. The saturation temperature of crystal growth was found to be 512°C by the crystal washing test method,...

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PUM

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Abstract

The invention discloses a fluxing agent for crystal growth and a crystal growth method. The crystal is Pb17O8Cl18, and a system of the fluxing agent comprises at least one of PbO, metal halide M'X, metal halide M''X2 and Bi2O3; wherein M' is Li, Na or K, M'' is Mg, Ca, Ba, Sr or Pb, and X is F or Cl. The crystal growth method comprises the following steps: mixing and melting a polycrystalline rawmaterial and the fluxing agent; starting seeding above a melt temperature saturation point, stabilizing the melt temperature at the saturation point, and starting crystal growth; and growing the crystal to a required size, lifting the seed rod crystal to be separated from the liquid level, and carrying out annealing treatment in a weak oxidizing atmosphere. According to the method, the crystal growth orientation is fully considered, the crystal growth stability is effectively improved, the solution volatilization and system viscosity in the growth process are reduced, the problems of needle-like growth of the crystal, easy cracking and color change of the grown crystal and the like are solved, and the grown crystal is large in size and high in optical quality.

Description

technical field [0001] The invention relates to a single crystal growth method, in particular to a mid-infrared nonlinear optical Pb 17 o 8 Cl 18 A flux for crystal growth and a crystal growth method. Background technique [0002] Pb 17 o 8 Cl 18 The crystal is a new type of mid-infrared nonlinear optical crystal with high laser damage threshold discovered in 2015. It has the advantages of large nonlinear optical coefficient, high laser damage threshold, wide light transmission range, and stable physical and chemical properties. Compared with other mid-infrared nonlinear optical crystals, Pb 17 o 8 Cl 18 The growth habit of the crystal is good, and it can grow in an open system, which greatly reduces the difficulty of growing traditional infrared frequency-doubling crystals in a closed system. Pb 17 o 8 Cl 18 The crystal can realize mid-to-far infrared laser output for visible light or near-infrared laser through laser frequency conversion. Since the crystal has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B15/00C30B29/12C30B33/02
CPCC30B15/00C30B29/12C30B33/02
Inventor 张彦王占勇徐家跃
Owner SHANGHAI INST OF TECH
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