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Rapid synthesis method of AgGaGenSe2(n+1) series compounds

A synthesis method and compound technology, which can be applied to selenium/tellurium compounds, elemental compounds other than selenium/tellurium, chemical instruments and methods, etc. Long cycle and other problems, to achieve the effect of large single synthesis amount, easy control of components, and fast synthesis rate

Inactive Publication Date: 2017-09-15
HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Adopting such a method, affected by the factor of high vapor pressure of elemental selenium at high temperature, the synthesis period is long (≧72h), the amount of single synthesis is small (≦200g), and improper operation can easily lead to the occurrence of explosion; in addition After the synthesis, a certain amount of selenium and other compounds often adhere to the walls of the synthesis crucible, and the synthetic polycrystalline raw materials deviate from the stoichiometric ratio more seriously.

Method used

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  • Rapid synthesis method of AgGaGenSe2(n+1) series compounds
  • Rapid synthesis method of AgGaGenSe2(n+1) series compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Example 1: AgGaGe 5 Se 12 Rapid Synthesis of Compounds

[0029] ①Clean and dry the synthetic crucible made of quartz with deionized water, and coat the surface of the crucible with a carbon film;

[0030] ② Use 99.995% pure AgGaSe 2 and GeSe 2 As the initial raw material, according to the amount ratio of 1:5 substance, the total is 400g, the reaction raw material is put into the quartz crucible, and the vacuum is evacuated to 10 -2 Pa sealed;

[0031] ③Put the sealed quartz crucible into a horizontal resistance synthesis furnace, and plug the furnace mouth with high-temperature refractory cotton. 200°C / h to raise the temperature of the resistance synthesis furnace to 900°C. After 4 hours of constant temperature, use manual oscillation to shake the resistance synthesis furnace at a constant speed of 10° / min. The shaking amplitude maintains an angle of 10° with the horizontal ground for 5 minutes;

[0032] ④ After shaking, lower the furnace temperature to 750°C at a...

Embodiment 2

[0033] Example 2: AgGaGe 3 Se 8 Rapid Synthesis of Compounds

[0034] ①Clean and dry the synthetic crucible made of quartz with deionized water, and coat the surface of the crucible with a carbon film;

[0035] ② Use 99.995% purity Ag 2 Se, Ga 2 Se 3 and GeSe 2 As the initial raw material, according to the amount ratio of 1:1:6 substances, the total is 300g, the reaction raw material is put into the quartz crucible, and the vacuum is evacuated to 10 -3 Pa sealed;

[0036] ③ Put the sealed quartz crucible into the vertical resistance synthesis furnace, and plug the furnace mouth with high-temperature refractory cotton. 100°C / h to raise the temperature of the resistance synthesis furnace to 950°C, and after constant temperature for 3 hours, use mechanical oscillation to shake the resistance synthesis furnace at a constant speed of 8° / min. The shaking amplitude maintains an angle of 30° with the horizontal ground for 10 minutes;

[0037] ④ After shaking, lower the furnace...

Embodiment 3

[0038] Example 3: AgGaGe 2 Se 6 Rapid Synthesis of Compounds

[0039] ①Clean and dry the synthetic crucible made of quartz with deionized water, and coat the surface of the crucible with a carbon film;

[0040] ② Use 99.995% pure AgGaSe 2 and GeSe 2 As the initial raw material, according to the ratio of 1:2 substance, the total is 350g, the reaction raw material is put into the quartz crucible, and the vacuum is evacuated to 10 -2 Pa sealed;

[0041] ③Put the sealed quartz crucible into a horizontal resistance synthesis furnace, and plug the furnace mouth with high-temperature refractory cotton. 50°C / h to raise the temperature of the resistance synthesis furnace to 920°C. After constant temperature for 2 hours, use manual oscillation to shake the resistance synthesis furnace at a constant speed of 5° / min. The shaking amplitude maintains an angle of 20° with the horizontal ground for 8 minutes;

[0042] ④ After shaking, lower the furnace temperature to 780°C at a rate of ...

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Abstract

The invention relates to a rapid synthesis method of AgGaGenSe2(n+1) series compounds and aims at solving the problems that an existing conventional AgGaGenSe2(n+1) (n=2,3,4,5) series compound element high temperature synthesis method is low in synthesis speed and the proportion of ingredients is difficult to control. The synthesis method comprises the following steps: taking high-purity Ag2Se, Ga2Se3 or AgGaSe2 and GeSe2 as initial raw materials, adjusting the molar ratio of GeSe2, and rapidly synthesizing the AgGaGenSe2(n+1) series compounds, namely AgGaGe2Se6, AgGaGe3Se8, AgGaGe4Se10 and AgGaGe5Se12. Specific operation steps are as follows: (1) pretreatment on a synthesis crucible; (2) determination of a raw material ratio; (3) heating oscillation; and (4) cooling. The characteristics of convenient operation, high synthesis speed and easy-to-control components are realized by adopting the method provided by the invention for synthesizing the AgGaGenSe2(n+1) series compounds.

Description

technical field [0001] The present invention relates to a kind of AgGaGe n Se 2(n+1) A rapid synthesis method for (n=2,3,4,5) series compounds. Specifically, a single temperature zone synthesis method is used to quickly synthesize high-quality AgGaGe with good uniformity and near stoichiometric ratio. n Se 2(n+1) (n=2,3,4,5) series polycrystalline, for subsequent growth of high-quality AgGaGe n Se 2(n+1) (n=2,3,4,5) series single crystal provides raw material guarantee. Background technique [0002] Selenium germanium gallium silver series compound, chemical formula AgGaGe n Se 2(n+1) (n=2,3,4,5), it can be simply regarded as the AgGaSe in the chalcopyrite structure 2 Based on the filled GeSe 2 Microscopic nonlinear optical effect group (Ge 4+ replace Ga 3+ , Ag + vacancy compensation, to maintain the overall charge balance), derived a class of excellent performance in the long-range infrared nonlinear crystal materials, they have a wide band of light transmissio...

Claims

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Application Information

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IPC IPC(8): C01B19/00C30B35/00
CPCC01B19/002C01P2002/72C01P2002/89C30B35/007
Inventor 倪友保吴海信毛明生王振友黄昌保
Owner HEFEI INSTITUTES OF PHYSICAL SCIENCE - CHINESE ACAD OF SCI
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