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a baga 4 the se 7 Polycrystalline synthesis device and synthesis method

A synthesis device and synthesis method technology, applied in polycrystalline material growth, chemical instruments and methods, single crystal growth, etc., can solve the problems of component deviation, yield drop, low reactivity of liquid metal Ga, etc., to achieve production rate-enhancing effect

Active Publication Date: 2020-07-17
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Because at this temperature, the vapor pressure of selenium is very high, and the active metal barium has a corrosive effect on the quartz tube, the reactivity of the liquid metal Ga is low, and the quartz tube often cracks and explodes. The amount of single synthesis is controlled at 50g Within , the repeatability of the reaction is poor, and the composition shift is prone to occur to form BaGa 2 Se 4 Impurity phase, and more deposition on the inner wall of the reaction quartz tube, resulting in a decrease in yield, and multiple batching, packaging, transfer and other processes will also bring additional pollution
All these restrict large-scale high-purity single-phase BaGa 4 Se 7 The acquisition of polycrystalline raw materials cannot satisfy BaGa 4 Se 7 Single Crystal Growth and Device Fabrication Requirements

Method used

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  • a baga <sub>4</sub> the se <sub>7</sub> Polycrystalline synthesis device and synthesis method
  • a baga <sub>4</sub> the se <sub>7</sub> Polycrystalline synthesis device and synthesis method
  • a baga <sub>4</sub> the se <sub>7</sub> Polycrystalline synthesis device and synthesis method

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Embodiment 1

[0033] Such as figure 1 As shown, a BaGa 4 Se 7 A polycrystalline synthesis device, the polycrystalline synthesis device comprises a gas phase transport quartz tube 1, a boron nitride boat 2 and a small quartz tube 3;

[0034] The gas-phase transmission quartz tube 1 is a quartz tube with one end closed, and an annular groove 4 is formed in the tube wall in the middle of the quartz tube, which divides the gas-phase transmission quartz tube into two parts. The end is the transition zone and the high temperature zone in turn, and the ring groove to the open end is the low temperature zone;

[0035] The boron nitride boat is used to contain high-purity barium element and gallium element, and placed in the high temperature zone of the gas phase transmission quartz tube 1;

[0036] The small quartz tube is used to contain simple selenium and is placed in the low temperature area of ​​the gas phase transmission quartz tube (1). One end of the small quartz tube is closed, and a sm...

Embodiment 2

[0040] In the present embodiment, the synthesis device described in Example 1 is adopted, and the raw materials barium (Ba), gallium (Ga), and selenium (Se) used are all 6N grades. During batching, the molar ratio of each raw material is barium: gallium: Selenium = 1:4:7, and according to the above ratio, appropriate selenium-enriched (1%-3% excess) ingredients: 35.082 grams of barium, 71.252 grams of gallium, and 142.617 grams of selenium. The synthesis process steps are as follows:

[0041] 1. Reaction vessel cleaning and drying

[0042] Rinse the gas-phase transmission quartz tube, boron nitride boat, and the inner wall of the small quartz tube with tap water, soak in aqua regia for 24 hours, then rinse with tap water until neutral, place in an ultrasonic cleaning tank for oscillating cleaning for 30 minutes, and use Rinse with deionized water repeatedly, then clean with high-purity alcohol, and dry in an oven at 100°C for later use.

[0043] 2. Loading

[0044] First pu...

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Abstract

The invention discloses a synthesis device and a synthesis method for BaGa4Se7 polycrystal, the synthesis device comprises a vapor phase transmission quartz tube (1), a boron nitride boat (2) and a quartz small tube (3); the vapor phase transmission quartz tube (1) is a quartz tube closed at one end, the middle tube wall of the quartz tube is concaved toward the inside of the tube to form an annular groove (4), and the annular groove divides the vapor phase transmission quartz tube into two parts, a transition zone and a high temperature zone are in turn arranged in the part from the annular groove is to the closed end, and a low temperature zone is arranged in the part from the annular groove to the open end; the boron nitride boat is used for holding high purity elemental barium and gallium, and is placed in the high temperature zone of the vapor phase transmission quartz tube (1), the quartz small tube is used for holding elemental selenium and is placed in the low temperature zoneof the vapor phase transmission quartz tube (1), the quartz tube is closed at one end, and the closed end is provided with a small hole (5). The BaGa4Se7 polycrystal is synthesized by gas phase transmission reaction of selenium vapor, the yield is more than 99%, and 200g of a high-purity polycrystalline raw material can be synthesized in a single time.

Description

technical field [0001] The invention belongs to the field of preparation of ternary compound semiconductor materials, in particular to a BaGa 4 Se 7 Polycrystalline synthesis device and synthesis method. Background technique [0002] Mid-to-far infrared lasers have important applications in environmental monitoring, medical surgery, lidar, space communication and other fields. The nonlinear frequency conversion method is a main method to generate mid-to-far infrared laser. The all-solid-state laser system with infrared nonlinear optical crystal as the key core component has the advantages of high power, wide tuning range, small size, light weight, and convenient maintenance. BaGa 4 Se 7 It is a new type of infrared nonlinear optical crystal discovered in recent years, and its nonlinear optical effect is large (d 11 =24pm / V), high laser damage threshold (557MW / cm 2 ), high transmittance in the range of 1-14μm, and large birefringence (Δn>0.06), it is currently the o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/46C30B28/14
Inventor 姚吉勇郭扬武李壮罗晓宇
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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