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Multicomponent compound infrared crystal growth method

A crystal growth and compound technology, applied in crystal growth, single crystal growth, chemical instruments and methods, etc., can solve the problems of solid-liquid interface drift, small temperature gradient, large difference in melting point, etc., and achieve complete appearance and good crystallization performance. , the effect of maintaining stability

Inactive Publication Date: 2008-12-17
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The infrared crystals of the above-mentioned compounds are recognized as relatively difficult crystals to grow. Generally, the Bridgman method (Bridgman method) can be used for single crystal growth. The gradient area of ​​the temperature field of the traditional Bridgman method, that is, the temperature gradient at the solid-liquid interface is small. and cannot be adjusted according to different crystal growth habits
These compounds have many components, large difference in melting point, large difference in saturated vapor pressure, and easy to decompose at high temperature; especially in the crystallization process, due to the different segregation coefficients of the components of the compound, and the large difference in thermal conductivity between solid and melt , as the crystal growth process changes, the temperature field in the crystallization region will change, causing the solid-liquid interface to drift, and it is difficult to maintain the flat (or slightly convex) interface growth required for crystal growth. Therefore, the usual Bridgman method It is difficult to obtain compound semiconductor single crystals with good integrity, which restricts the application of infrared crystals

Method used

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  • Multicomponent compound infrared crystal growth method
  • Multicomponent compound infrared crystal growth method
  • Multicomponent compound infrared crystal growth method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1: Infrared Crystal LiInS 2 growth

[0023] Take LiInS 2 Polycrystalline powder is used as a raw material, and the polycrystalline powder raw material is loaded into a graphite crucible 3, and then sealed in a quartz tube 2, and the crystal growth is carried out according to the following process steps:

[0024] (1) Clean the quartz tube 2:

[0025] Soak in aqua regia solution for 24 hours to remove metal ions attached to the wall of the quartz tube, then soak in acetone for 24 hours to remove organic impurities attached to the wall of the quartz tube, then soak in dilute hydrochloric acid solution for 5 to 10 minutes, and finally use Rinse with deionized water and dry in an oven for later use. At the same time, the crucible is cleaned to remove impurities on the inner wall of the crucible.

[0026] (2) Charge and vacuumize, seal the quartz tube 2:

[0027] Weigh 10g~20g LiInS 2 The polycrystalline powder is loaded into a graphite crucible 3 with a tempera...

Embodiment 2

[0034] Example 2: Infrared Crystal ZnGeP 2 growth

[0035] Using ZnGeP2 polycrystalline powder as the raw material, the polycrystalline raw material is put into the graphite crucible 3 and then sealed into the quartz tube 2 . Crystal growth includes the following process steps in sequence:

[0036] (1) Clean the quartz tube 2 and the crucible 3 as described in Example 1.

[0037] (2) Charge and vacuumize, seal the quartz tube 2:

[0038] Weigh 10g~20g ZnGeP 2 The polycrystalline powder is loaded into a graphite crucible 3 with a temperature-measuring thermocouple 14 placed at the tip, and then the charged graphite crucible 3 is loaded into a cleaned quartz tube 2, and then heated to 200°C to 300°C on an electric furnace for pumping. Vacuum, when the vacuum degree in the crucible reaches 10 -3 ~10 -4 pa, seal the quartz tube with an oxyhydrogen flame.

[0039] (3)ZnGeP 2 crystal growth

[0040] a. Put the sealed quartz tube into figure 1 In the hearth of the growth fu...

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Abstract

The invention provides a growth method of an infrared crystal of polynary compounds, which takes crystal powder of polynary compounds as a raw material and a crucible pot as a growth container, and comprises following technical processes: (1) metallic ions and organic impurities that are adhesive to a wall of a quartz pipe are removed, and impurities on an inner wall of the crucible pot are removed; (2) the crystal powder of polynary compounds is filled into the crucible pot, the crucible pot is vacuumized, and the quartz pipe is sealed with oxyhydrogen flame; (3) the crucible pot is positioned inside a high-temperature region, temperature of the high-temperature region is raised over the melting point of the crystal of polynary compounds, temperature of a low-temperature region is raised under the melting point of the crystal of polynary compounds, and heat preservation is implemented after certain objective temperature is reached; lowering of a pointed part of the crucible pot is stopped at a position of a solid-liquid interface, the crucible pot is lowered after the heat preservation, and the crystal starts to grow; crystal growth finishes after all fusants in the crucible pot pass through the solid-liquid interface in a middle gradient region; (4) the crucible pot is lowered to the lower low-temperature region so as to implement annealing, and the crystal is taken out after room temperature is reached. The growth method can be used for preparing the infrared crystal of polynary compounds with complete appearance and well crystal property.

Description

technical field [0001] The invention relates to a method for growing multi-component infrared crystals, belonging to the technical field of inorganic crystal growth. Background technique [0002] Mid-to-far infrared coherent light sources have very important applications in the laser field. In the military field, such as: laser guidance, laser directional infrared interference, laser communication, infrared remote sensing, infrared thermal imager, infrared ranging, laser aiming, etc.; in the civilian field, Such as: trace gas detection in the environment, biology, medicine, etc. have a wide range of applications. The current laser host materials have been able to produce tunable coherent light source output within a certain range, but because their tunable wavelength range is determined by the gain bandwidth of the active ions in the laser medium, their tunable range and efficiency are greatly limited. limits. Multi-component infrared crystals such as: AgGaS 2 , AgGaSe 2...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B11/00
Inventor 王善朋陶绪堂蒋民华
Owner SHANDONG UNIV
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