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Method for synthesizing mercurous iodide

A technology of mercurous iodide and mercuric iodide, applied in directions such as mercuric halide, can solve the problems of difficulty in preparing raw materials of mercurous iodide, and achieve the effect of wide crystallization temperature range and easy control.

Inactive Publication Date: 2014-02-05
XIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Mercury is liquid at normal temperature, and iodine and mercuric iodide are solid, so it is not suitable to synthesize mercurous iodide through solid-liquid phase reaction; More mercurous iodide gas is generated, it is difficult to prepare high-purity mercurous iodide raw materials by gas phase synthesis

Method used

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  • Method for synthesizing mercurous iodide
  • Method for synthesizing mercurous iodide
  • Method for synthesizing mercurous iodide

Examples

Experimental program
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Effect test

Embodiment 1

[0033] The method for the synthesis of mercurous iodide in the present embodiment may further comprise the steps:

[0034] S1: Clean the ampoule and dry it for later use;

[0035] S2: Measure mercury and mercury iodide as the reaction raw materials, and put the measured mercury and mercury iodide into the ampoule prepared in S1, and vacuum the ampoule until the vacuum degree reaches 1×10 -2 Seal the ampoule at Pa;

[0036] S3: Fix the ampoule in S2 vertically in the reaction furnace, and raise the temperature of the reaction furnace to 300°C at a heating rate of 20°C / h;

[0037] S4: After all the mercury iodide is melted, let stand for 4 hours;

[0038] S5: Lower the reaction furnace at a cooling rate of 200°C / h to any temperature below the medromic reaction temperature of the iodine-mercury binary system and above the eutectic reaction temperature, keep warm for 2 hours and then cool to room temperature with the furnace;

[0039] S6: Take out the product obtained in the am...

Embodiment 2

[0045] The method for the synthesis of mercurous iodide in the present embodiment may further comprise the steps:

[0046] S1: Clean the ampoule and dry it for later use;

[0047] S2: Measure mercury and mercury iodide as the reaction raw materials, and put the measured mercury and mercury iodide into the ampoule prepared in S1, and vacuum the ampoule until the vacuum degree reaches 1×10 -3 Seal the ampoule at Pa;

[0048] S3: Fix the ampoule in S2 vertically in the reaction furnace, and raise the temperature of the reaction furnace to 370°C at a heating rate of 100°C / h;

[0049] S4: After all the mercury iodide is melted, let stand for 1 hour;

[0050] S5: Lower the reaction furnace at a cooling rate of 400°C / h to any temperature below the medromic reaction temperature of the iodine-mercury binary system and above the eutectic reaction temperature, keep it warm for 10 hours, and then cool to room temperature with the furnace;

[0051] S6: Take out the product obtained in t...

Embodiment 3

[0054] The main steps of the method for synthesizing mercurous iodide in this embodiment are the same as those in Examples 1 and 2, except that the reaction raw material mercuric iodide in this embodiment is formed from iodine and mercury in the synthetic process of mercurous iodide Synthetic, specifically, the synthetic mercurous iodide method in the present embodiment comprises the following steps:

[0055] S1: Clean the ampoule and dry it for later use;

[0056] S2: includes the following steps:

[0057] S21: Measure mercury and iodine as the raw materials for the reaction, put the measured mercury and iodine into the ampoule prepared in S1, and evacuate the ampoule until the vacuum degree reaches 1×10 -2 Seal the ampoule at Pa;

[0058] S22: Fix the ampoule in S21 in the tube furnace with two temperature zones and make the mercury and iodine contained in the ampoule located at the high temperature end of the tube furnace with two temperature zones; the structure of the t...

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Abstract

The invention discloses a method for synthesizing mercurous iodide. The method comprises the steps of: S1, cleaning and drying an ampoule for future use; S2, putting the measured mercury and mercury iodide into the ampoule prepared in the step S1, vacuumizing the ampoule and sealing the ampoule when the vacuum degree is reduced to the range from 10<-2> to 10<-3> Pa; S3, vertically fixing the ampoule in the step S2 in a reaction furnace, and increasing the temperature of the reaction furnace to the range from 300 to 370 DEG C at a temperature rise rate of 20-100 DEG C per hour; S4, after all the mercury iodide is melted, standing for 1-4 h; S5, reducing the temperature of the reaction furnace to any temperature under the syntectic reaction temperature of an iodine-mercury binary system and above the eutectic reaction temperature of the iodine-mercury binary system at a temperature reduction rate of 200-400 DEG C per hour, preserving heat for 2-10 h and then cooling to the room temperature; and S6, taking out the obtained product in the ampoule and removing mercury at the bottom and mercury iodide at the top. The method for synthesizing the mercurous iodide is capable of obtaining the mercurous iodide in which the ratio of mercury atoms to iodine atoms is 1: 1; and the crystallization temperature range is wide and the method is easy to control.

Description

technical field [0001] The invention belongs to the technical field of material engineering, and in particular relates to a method for synthesizing mercurous iodide. Background technique [0002] Mercury iodide is a metamorphic compound formed by the metamorphic reaction of mercury-rich melt and iodine-rich melt. Mercurous iodide single crystal is one of the materials for making tunable acousto-optic devices. Its light transmission range is 0.55-40 μm, and it has an irreplaceable role in making infrared acousto-optic devices. [0003] The synthesis of mercurous iodide raw material can lay the foundation for the growth of mercurous iodide single crystal. Mercury is liquid at normal temperature, and iodine and mercuric iodide are solid, so it is not suitable to synthesize mercurous iodide by solid-liquid phase reaction; More mercurous iodide gas is generated, and it is difficult to prepare high-purity mercurous iodide raw materials by gas-phase synthesis. Contents of the i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G13/04
Inventor 金应荣贺毅张洁陈宝军何知宇苏敏龚鹏
Owner XIHUA UNIV
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