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A device for preparing ultra-high-purity indium and its preparation method

A technology of ultra-high and pure indium, which is applied in the preparation of ultra-high-purity indium and its preparation field, which can solve the problems of low surface tension of liquid metal indium, low preparation efficiency, and inability to realize industrial production.

Active Publication Date: 2021-07-06
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the application number is CN201711305879.0, and the title is "a method for purifying indium". The invention discloses a preparation device and method for ultra-high-purity indium. High-purity indium with a purity of 6N can be obtained by the method, but it cannot meet the production of ultra-high-purity indium above 7N, and because the surface tension of liquid metal indium is small, the output is very small each time, and industrial production cannot be realized
The application number is CN201711441250.9, and the invention titled "A Purification Device and Method for High-purity Indium" discloses a method for smelting in a horizontal area. Control the temperature of several resistance heaters to achieve multi-stage heating, and obtain ultra-high-purity indium of 6N to 7N based on the horizontal zone melting method, but the products prepared by the horizontal zone melting method have large quality fluctuations in different regions, and the single horizontal region low production efficiency

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  • A device for preparing ultra-high-purity indium and its preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Clean the quartz tube with 1% dilute nitric acid first, then rinse it repeatedly with high-purity deionized water, put it into the upper part of the second guide rod in the vertical zone melting system after drying and fix it;

[0030](2) Accurately weigh 250 grams of 4N refined indium with an electronic balance, put it into a high-purity graphite crucible heated by intermediate frequency induction, move the condensation plate downward to 10cm above the crucible, turn on the molecular pump, and evacuate to a vacuum degree of 5Pa ; Turn on the medium-frequency induction power supply to heat the graphite crucible, and keep it warm for 2 hours after the temperature reaches 900°C, and the volatilization rate of the raw materials is about 15.5266%;

[0031] (3) When the metal indium melt is cooled to about 200°C, move the condensing plate upwards, start the rotating device, slowly turn over the crucible, pour the indium melt in the crucible into the self-heating drainage ...

Embodiment 2

[0034] (1) Clean the quartz tube with 1% dilute nitric acid first, then rinse it repeatedly with high-purity deionized water, put it into the upper part of the second guide rod in the vertical zone melting system after drying and fix it;

[0035] (2) Accurately weigh 250 grams of 4N refined indium with an electronic balance, put it into a high-purity graphite crucible heated by intermediate frequency induction, move the condensation plate downward to 10 cm above the crucible, and turn on the molecular pump to evacuate to 1×10 -5 Pa; turn on the medium frequency induction power supply to heat the graphite crucible, after the temperature reaches 950°C, keep it warm for 2 hours, and the volatilization rate of raw materials is about 17.7921%;

[0036] (3) When the metal indium melt is cooled to about 200°C, move the condensing plate upwards, start the rotating device, slowly turn over the crucible, pour the indium melt in the crucible into the self-heating drainage tank, and then i...

Embodiment 3

[0039] (1) Clean the quartz tube with 1% dilute nitric acid first, then rinse it repeatedly with high-purity deionized water, put it into the upper part of the second guide rod in the vertical zone melting system after drying and fix it;

[0040] (2) Accurately weigh 250 grams of 4N refined indium with an electronic balance, put it into a high-purity graphite crucible heated by intermediate frequency induction, move the condensation plate downward to 10cm above the crucible, turn on the molecular pump to evacuate to 5Pa; turn on the intermediate frequency induction The graphite crucible is heated by the power supply. After the temperature reaches 550°C, 600°C, 750°C, and 950°C, it is kept for 120min, 60min, 90min, and 60min respectively, and the volatilization rate of the raw material is about 18.5516%;

[0041] (3) When the metal indium melt is cooled to about 200°C, move the condensing plate upwards, start the rotating device, slowly turn over the crucible, pour the indium me...

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Abstract

The invention discloses a device for preparing ultra-high-purity indium and a preparation method thereof, comprising a vacuum chamber, a distillation system arranged in the vacuum chamber and a vertical zone melting system located at the lower right of the distillation system; The raw material is placed in the graphite crucible, and the cooling plate is moved down through the first guide rod to carry out vacuum distillation. After the metal indium melt in the graphite crucible is cooled down, the cooling plate is moved up, and the rotating device tilts the crucible at a certain angle to dissipate the metal The indium melt is poured into the quartz tube, and the heating temperature and cooling temperature are respectively set by three independent heating devices and cooling devices, and the second guide rod drives the quartz tube to move up and down and spin to perform vertical zone melting to obtain ultra-high pure indium. The invention organically combines the vacuum distillation method and the vertical zone melting method, thereby realizing efficient and stable production of ultra-high-purity indium of 7N or more.

Description

technical field [0001] The invention belongs to the field of preparation of pure indium, and in particular relates to a device for preparing ultra-high-purity indium and a preparation method thereof. Background technique [0002] Indium metal has unique and excellent physical and chemical properties. It is widely used in high-tech fields such as energy, national defense, aerospace, nuclear industry and modern information industry. It plays an increasingly important role in the national economy. However, since the introduction of trace impurities will seriously affect the performance of the material itself, the purity of metal indium directly determines the performance of the subsequently synthesized material. The electronics industry and the semiconductor industry require the purity of indium to be above 6N. At present, the preparation methods of high-purity indium mainly include electrolysis, vacuum distillation, regional smelting, ion exchange, and low-halogen compound me...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B58/00C22B9/02C22B9/00
CPCC22B9/00C22B9/02C22B58/00Y02P10/20Y02P10/25
Inventor 李明旭郑红星张云虎翟启杰
Owner SHANGHAI UNIV