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Autoclave synthesis method of sulfur group compound

A multi-metal and synthesis method technology, applied in the field of chalcogenide synthesis, can solve problems such as difficulty in ensuring stoichiometric ratio, difficult process parameters, and quartz ampoule bursting, so as to avoid the problem of quartz tube explosion, the process is simple, and the success is improved. rate effect

Inactive Publication Date: 2008-02-13
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the above methods can obtain chalcogenide polycrystalline raw materials, they all have long synthesis cycles, difficult control of process parameters, and easy to cause problems such as the explosion of quartz ampoules. For indirect synthesis, impurities will be introduced in the middle process, and during grinding When dealing with intermediate products - sulfides, it is difficult to ensure the original stoichiometric ratio

Method used

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  • Autoclave synthesis method of sulfur group compound

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] First, put the raw materials and graphite crucible into the oven to dry and remove water; in the glove box, accurately weigh the high-purity elemental raw materials Li(3N), In(4N) and S(4N) respectively according to the molar ratio of 1:1:2. ), taking into account the loss of S and Li, respectively, in excess of 10at% and 2at%. According to steps ③~⑥ in the process, the highest reaction temperature is controlled at 950°C, and LiInS can be obtained at constant temperature for 10 hours. 2 polycrystalline material. After grinding a small piece of polycrystalline material, do X-ray powder diffraction analysis, as shown in the attached figure, it proves that the obtained polycrystalline material is high-purity, single-phase LiInS 2 polycrystalline material.

Embodiment 2

[0019] First, put the raw materials and graphite crucible into an oven to dry and remove water; in the glove box, accurately weigh the high-purity elemental raw materials Li(3N), In(4N) and Se(4N) respectively according to the molar ratio of 1:1:2. ), taking into account the loss of Se and Li, respectively, in excess of 8at% and 4at%. According to steps ③~⑥ in the process, the maximum reaction temperature is controlled at 1000, and the temperature is kept at 20 hours to obtain LiInSe 2 polycrystalline material. After grinding a small piece of polycrystalline material, X-ray powder diffraction analysis proves that the obtained polycrystalline material is high-purity, single-phase LiInSe 2 polycrystalline material.

Embodiment 3

[0021] First, put the raw materials and graphite crucible into the oven to dry and remove water; in the glove box, accurately weigh the high-purity elemental raw materials Cu(4N), In(4N) and S(4N) respectively according to the molar ratio of 1:1:2. ), taking into account the volatilization loss of S, an excess of 2at%. According to steps ③~⑥ in the process, the highest reaction temperature is controlled at 1100 °C, and the temperature is kept at 25 hours to obtain CuInS 2 polycrystalline material. After grinding a small piece of polycrystalline material, X-ray powder diffraction analysis proves that the obtained polycrystalline material is high-purity, single-phase CuInS 2 polycrystalline material.

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Abstract

The invention discloses a high-pressure autoclave synthesizing method of chalcogenide, which comprises the following steps: 1. placing raw material and graphite copple in the baker to dry; 2. weighing each group of raw material accurately in the glove box; loading in the prepared graphite copple; sealing; 3. placing the copple in the high-temperature high-pressure autoclave; sealing; 4. extracting into 2*10-3Pa through dispersing pump; closing valve of high-pressure autoclave; 5. placing high-pressure autoclave in the pipe-typed resistance furnace; controlling temperature through FP23 temperature control program; heating to 950-1200 deg.c at 10deg.c / min; insulating for 10-30h; cooling slowly to indoor temperature; 6. starting high-pressure autoclave; cutting graphite copple to obtain the high-purity single-phase dense multicrystal raw material.

Description

technical field [0001] The invention relates to a method for synthesizing chalcogenides, in particular to a method for rapidly and simply synthesizing multi-metal inorganic chalcogenides by using an autoclave. Background technique [0002] We know that in the field of laser technology, scientists are always pursuing the goal of obtaining a laser light source that can be continuously adjusted from the infrared region to the ultraviolet region. This is because although the current laser host materials have been able to produce tunable coherent light source output within a certain range, because their tunable wavelength range is determined by the gain bandwidth of the activated ions in the laser medium, their tunable range and Efficiency is considerably limited. Mid-infrared coherent light sources have very important applications. It is widely used in the military field, such as: laser guidance, laser directional infrared interference, laser communication, infrared remote sen...

Claims

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Application Information

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IPC IPC(8): C30B1/12C30B29/46C01B17/20
Inventor 陶绪堂王善朋董春明蒋民华
Owner SHANDONG UNIV
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