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Polycrystalline synthesis method and single-crystal growth method of gallium selenide

A synthesis method and a growth method technology are applied in the fields of polycrystalline synthesis and single crystal growth of gallium selenide, which can solve the problems of non-stoichiometric ratio and low yield, ineffective crystal nucleus and uncertain growth direction of single crystal, etc. Yield-enhancing effect

Inactive Publication Date: 2016-11-23
HARBIN INST OF TECH
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  • Application Information

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Problems solved by technology

[0005] The present invention aims to solve the technical problems of the non-stoichiometric ratio and low yield of the existing GaSe polycrystal synthesis and the easy formation of invalid crystal nuclei and uncertain single crystal growth direction in the spontaneous nucleation stage of GaSe, and provide GaSe polycrystal synthesis method and single crystal growth method

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  • Polycrystalline synthesis method and single-crystal growth method of gallium selenide
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  • Polycrystalline synthesis method and single-crystal growth method of gallium selenide

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specific Embodiment approach 1

[0022] Specific embodiment one: the polycrystalline synthesis method of GaSe of the present embodiment is carried out according to the following steps:

[0023] 1. Soak the quartz tube and the quartz boat or boron nitride boat used for holding the material with aqua regia, then wash with ultrapure water and dry; weigh the elemental raw material Ga according to the molar ratio Ga:Se=1:(1+n) and Se, where n=PV / RT, P are 1 atmospheric pressure, V is the cylinder void volume in the quartz tube, T is (600+273) K, and R is the gas constant;

[0024] 2. Place Ga in a small boat, place the small boat containing Ga at the closed end of the quartz tube, and place Se directly at the other end of the quartz tube; vacuumize the quartz tube, and then seal the quartz tube with a hydrogen-oxygen flame. Then put it into a horizontal dual temperature zone tubular resistance furnace, the boat filled with Ga is located in the high temperature zone, Se is located in the low temperature zone, and t...

specific Embodiment approach 2

[0026] Specific embodiment two: the difference between this embodiment and specific embodiment one is that the quartz tube and the quartz boat or boron nitride (PBN) boat used in step one are soaked in aqua regia for 6-8 hours. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0027] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that in step two, the quartz tube is evacuated to 10 -4 Pa~10 -6 Pa. Others are the same as in the first or second embodiment.

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Abstract

The invention provides a polycrystalline synthesis method and a single-crystal growth method of gallium selenide and relates to polycrystalline synthesis and single-crystal growth methods of mid-infrared and far-infrared non-linear materials, aiming at solving the technical problems of existing GaSe polycrystalline synthesis that the stoichiometric deviation is great and the yield is low, an invalid crystal nucleus is prone to form in a spontaneous nucleation phase and a single-crystal growth direction is uncertain. Polycrystalline synthesis comprises the following steps: putting monomer Ga into a small boat and putting the small boat at one end of a quartz tube; putting Se at the other end of the quartz tube; after vacuumizing, carrying out heat sealing; putting the quartz tube into a horizontal double-temperature-region pipe type resistance furnace and synthesizing to obtain a GaSe poly-crystal, wherein the stoichiometric ratio is 1 to (1 to 1.05) and the yield is more than 97 percent. Single-crystal growth comprises the following steps: adding the GaSe poly-crystal into a PBN (Pyrolytic Boron Nitride) crucible; then vertically putting the PBN crucible into the quartz tube; after vacuumizing, carrying out heat sealing; putting the quartz tube into a vertical double-temperature-region pipe type resistance furnace; after the single-crystal growth is finished, obtaining a GaSe single-crystal. The gallium selenide can be used as the mid-infrared and far-infrared laser materials for realizing output of 8Mum to 10Mum laser.

Description

technical field [0001] The invention relates to a method for polycrystal synthesis and single crystal growth of middle and far infrared nonlinear materials. Background technique [0002] Mid-to-far infrared lasers (especially 3-5μm and 8-10μm infrared bands) have very important applications in both military and civilian fields. Gallium selenide (GaSe) crystals have a large nonlinear coefficient (d 22 =54pm / V), wide light transmission band (0.65-18μm), large birefringence (Δn=0.36) and other excellent nonlinear optical properties, it is the best dielectric material for mid-to-far infrared laser frequency conversion, and can realize 8-10μm laser output. [0003] At present, the methods for synthesizing GaSe polycrystalline raw materials include single temperature zone method and double temperature zone method. The single temperature zone method only needs to set a constant temperature zone, the process is simple, and the operation is convenient. Due to the high-temperature ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B11/00C30B28/14C30B29/46
CPCC30B29/46C30B11/00C30B11/002C30B28/14
Inventor 杨春晖马天慧朱崇强雷作涛
Owner HARBIN INST OF TECH
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