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Device and method for synthesizing zinc germanium phosphide polycrystal

A germanium phosphide and zinc synthesis device technology, applied in the direction of phosphide, can solve the problems of vacuum sealed tubes that cannot be recycled, low synthesis rate, low output rate, etc., to save experiment and production costs, high synthesis rate, The effect of high productivity

Inactive Publication Date: 2012-11-14
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to propose a phosphorous zinc phosphide polycrystalline synthesis method in order to solve the problems of low synthesis rate, easy to explode, low yield, impure product, and non-recyclable vacuum sealed tube existing in the current polycrystalline synthesis method of germanium phosphide. Device and method for synthesizing germanium-zinc polycrystal

Method used

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  • Device and method for synthesizing zinc germanium phosphide polycrystal
  • Device and method for synthesizing zinc germanium phosphide polycrystal
  • Device and method for synthesizing zinc germanium phosphide polycrystal

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Experimental program
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Effect test

Embodiment 1

[0034] Put zinc and germanium in a stoichiometric 1:1 weight ratio of 50g in total, mix them uniformly and fully grind them under the protection of inert gas, and put them into the synthesis crucible 14, and put the synthesis crucible 14 containing the mixed raw materials of zinc and germanium into the internal reaction Room 13, press figure 1 After connecting the inner reaction chamber 13 and the argon protection chamber 12, place it in the furnace chamber (horizontal synthesis furnace) 11, vacuumize the inner reaction chamber 13 and the argon protection chamber 12, and then fill it with high-purity argon. Excess phosphorus is weighed and added into the evaporator 20 under an argon atmosphere. According to the stoichiometric amount of zinc and germanium used, the amount of phosphorus is 1.3-1.5 times of the stoichiometric amount of zinc or germanium. according to figure 1 After connecting the pipes, vacuumize the reaction tube as a whole, and repeatedly clean the entire gas ...

Embodiment 2

[0037] Put zinc and germanium in a stoichiometric ratio of 1:1.1 in a weight ratio of 150g, mix them evenly under the protection of an inert gas and grind them thoroughly, then put them into a synthetic crucible 14, and put the synthetic crucible 14 containing zinc-germanium mixed raw materials into the internal reaction Room 13, press figure 1 After connecting the inner reaction chamber 13 and the argon protection chamber 12, place it in the furnace cavity 11, vacuumize the inner reaction chamber 13 and the argon protection chamber 12, and then fill it with high-purity argon. Excess phosphorus is weighed and added into the evaporator 20 under an argon atmosphere. According to the stoichiometric amount of zinc and germanium used, the amount of phosphorus is 1.3-1.5 times of the stoichiometric amount of zinc or germanium. according to figure 1 After connecting the pipes, clean the entire gas path and reaction chamber repeatedly with high-purity argon for 3 to 5 times.

[0038...

Embodiment 3

[0040] Put zinc and germanium in a stoichiometric ratio of 1:1.05 in a weight ratio of 300g, mix them evenly under the protection of an inert gas and grind them fully, then put them into a synthetic crucible 14, and put the synthetic crucible 14 containing zinc-germanium mixed raw materials into the internal reaction Room 13, press figure 1 After connecting the inner reaction chamber 13 and the argon protection chamber 12, place it in the furnace cavity 11, vacuumize the inner reaction chamber 13 and the argon protection chamber 12, and then fill it with high-purity argon. Excess phosphorus is weighed and added into the evaporator 20 under an argon atmosphere. According to the stoichiometric amount of zinc and germanium used, the amount of phosphorus is 1.3-1.5 times of the stoichiometric amount of zinc or germanium. according to figure 1 After connecting the pipes, clean the entire gas path and reaction chamber repeatedly with high-purity argon for 3 to 5 times.

[0041] Af...

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Abstract

The invention discloses a device and method for synthesizing a zinc germanium phosphide polycrystal. The method comprises the steps of: fully mixing and uniformly grinding zinc and germanium according to the weight proportion of (1:1)-(1:11) in the terms of stoichiometry, placing into a synthesis crucible, placing the synthesis crucible at one end of a reaction tube, then placing the reaction tube in a horizontal synthesis furnace, repeatedly cleaning 3-5 times with high-purity argon, adding excessive phosphorus in an evaporator and closing under an argon environment; continuously and slowly introducing high-purity argon, raising the temperature of a furnace cavity to a certain constant temperature in the interval of 400-900 DEG C, slowly heating the evaporator to ensure that the phosphorus is slowly sublimated; and when the remained phosphorus in the phosphorus evaporator is less than the phosphorus deposited in a condenser, removing a heating element of the phosphorus evaporator to ensure that the temperature of the phosphorus evaporator is reduced to below 10 DEG C, then heating the phosphorus in a condensing bottle to ensure that the phosphorus in the condensing bottle slowly sublimates, introducing the argon into the condensing bottle, repeating the operation until the reaction is completed. The device and method disclosed by invention have the advantages of high synthesis rate, high product purity, complete reaction, high yield, safety, explosion prevention and the like.

Description

technical field [0001] The invention relates to the technical field of preparation of a ternary compound polycrystalline material, in particular to a synthesis device and method of germanium zinc phosphide polycrystalline. Background technique [0002] Chalcopyrite semiconductor crystal materials have the outstanding advantages of high nonlinear optical coefficient and high transmittance in the far infrared region. Zinc germanium phosphide (ZnGeP2, ZGP) crystal has the best comprehensive performance among chalcopyrite semiconductor crystals, and its advantages are very prominent. It is one of the highest nonlinear coefficients among all known infrared nonlinear optical crystals. It is currently the best nonlinear material for realizing high-power mid- and far-infrared tunable laser output, and has important application value in civil and national defense fields. The synthesis of high-quality zinc germanium phosphide polycrystals is a prerequisite for the preparation of zinc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/08
Inventor 吴东王彪申亮徐洪远王云华
Owner SUN YAT SEN UNIV
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