A kind of preparation method of metallic arsenic single crystal

A metal arsenic and single crystal technology, applied in the fields of metallurgy technology and materials science and engineering, can solve the problems of complex surface structure and crystal structure, high oxidation risk, low economic value, etc., to improve oxidation resistance, storage capacity, Surface mirror light effect

Active Publication Date: 2021-03-23
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of preparing metal arsenic mainly adopts thermal reduction method, such as carbothermal reduction method and its improved method (Chinese patent ZL89101045.9, Chinese patent ZL 92110735.8, Shandong Hengbang published patent (application number: 201911003123.X, publication number: CN 110747355A), Central South University published patent (application number: 201710186489.X, publication number: CN107043862A), etc.), hydrogen reduction method and its improved method (US Patent US 3657379), and preparation of metal arsenic block by wet reduction-hot pressing sintering method (application number: 201510992870.6, publication number CN 105506311A); however, the prepared metallic arsenic is metallic gray arsenic, with complex surface and crystal structures, high oxidation risk in subsequent storage and use, and can only be used as crude arsenic. Low economic value; Chen Guozhong and Yang Weidong developed a method for preparing ultra-high-purity arsenic single wafers (application number: 201210312574.3, publication number CN 102899712A), which uses ultra-high-purity raw materials to perform sublimation crystallization at 36atm at 817°C to form twin wafers , the method uses high temperature and high pressure, and requires high equipment

Method used

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  • A kind of preparation method of metallic arsenic single crystal
  • A kind of preparation method of metallic arsenic single crystal
  • A kind of preparation method of metallic arsenic single crystal

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Experimental program
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Effect test

Embodiment 1

[0025] The mass of metal arsenic raw material is 1.9g, and the maximum reaction pressure is about 1.2MPa in a closed container. According to the molar ratio of As and I is 1:1, mix elemental arsenic and elemental iodine and place them in the Q1 area, and react at 650°C for 30min. At the same time, the arsenic vapor generated by the reaction condenses and crystallizes at 500 ° C in the Q2 area, and the axial temperature gradient between the Q1 area and the Q2 area is 8 ° C / cm, and the metallic arsenic single crystal is obtained;

[0026] After condensing and crystallizing the metal arsenic single crystal, the temperature in the Q2 area is lowered to 150°C, and the temperature in the Q1 area is lowered to 48°C to condense and recover elemental iodine and continue to use it for the reaction.

Embodiment 2

[0028] The mass of metal arsenic raw material is 2.2g, and the maximum reaction pressure is about 1.5MPa in a closed environment. According to the molar ratio of As and I is 40:1, the elemental arsenic and arsenic triiodide are mixed and placed in the Q1 area, and reacted at 700°C For 40 minutes, the arsenic vapor generated by the reaction was condensed and crystallized at 520 °C in the Q2 area, and the axial temperature gradient between the Q1 area and the Q2 area was 9 °C / cm, and the metallic arsenic single crystal was obtained;

[0029] After the metal arsenic single crystal is obtained by condensation and crystallization, the temperature in the Q2 area is lowered to 150°C, and the temperature in the Q1 area is lowered to 48°C to carry out condensation recovery of arsenic triiodide and continue to use it for the reaction.

Embodiment 3

[0031] The mass of metal arsenic raw material is 1.1g, and the maximum reaction pressure is about 0.7MPa in a closed environment. According to the molar ratio of As and I is 80:1, the elemental arsenic and elemental iodine are mixed and placed in the Q1 area, and reacted at 650°C for 60min. At the same time, the arsenic vapor generated by the reaction condenses and crystallizes at 500°C in the Q2 area, and the axial temperature gradient between the Q1 area and the Q2 area is 8°C / cm, and the metallic arsenic single crystal is obtained;

[0032] After condensing and crystallizing the metal arsenic single crystal, the temperature in the Q2 area is lowered to 150°C, and the temperature in the Q1 area is lowered to 48°C to condense and recover elemental iodine and continue to use it for the reaction.

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Abstract

The invention discloses a preparation method of a metal arsenic single crystal. The preparation method comprises the following steps: in a closed container with oxygen content of less than 1 ppm and water content of less than 1ppm, mixing elemental arsenic and an iodine-containing hardening and tempering agent, carrying out reacting in a high-temperature reaction area, and condensing and crystallizing arsenic vapor generated by the reaction in a condensing and crystallizing area to obtain a metal arsenic single crystal, wherein the iodine-containing hardening and tempering agent is elemental iodine and / or arsenic triiodide. According to the invention, the iodine-containing hardening and tempering agent is added, so the surface structure of metal arsenic is adjusted in the crystallization process, the preferred growth of the metal arsenic is controlled, and the exposed growth crystal face structure of metal arsenic is mainly based on a (0001) crystal face family; and since crystal facesin the crystal face family have lower surface energy, lower oxidation tendency and oxidation degree is obtained, the oxidation resistance of the metal arsenic can be remarkably improved, and the useand storage capacity of the metal arsenic is improved.

Description

technical field [0001] The invention belongs to the fields of metallurgical technology, material science and engineering, and relates to a method for preparing metal arsenic single crystal. Background technique [0002] Arsenic is an inevitable by-product of the non-ferrous smelting industry. Proper disposal and recycling of arsenic resources can avoid secondary harm to the environment, which is conducive to the green and sustainable development of the non-ferrous industry and the protection of the ecological environment. At present, the main forms of arsenic-containing products in the non-ferrous smelting industry are white arsenic and metallic arsenic, among which metallic arsenic is the main raw material form for the high-tech application of materialization of arsenic resources. The process of preparing metal arsenic mainly adopts thermal reduction method, such as carbothermal reduction method and its improved method (Chinese patent ZL89101045.9, Chinese patent ZL 9211073...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/02C30B23/00
CPCC30B23/00C30B29/02
Inventor 梁彦杰刘振兴柴立元邓方杰杨志辉闵小波刘恢周艺伟
Owner CENT SOUTH UNIV
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