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Device for preparing ultra-pure indium and method for preparing ultra-pure indium by adopting device

A heating device, initial position technology, applied in the direction of improving process efficiency, can solve the problems of high time cost, difficult to control the width of the melting zone, low yield, etc., to achieve uniform and stable temperature field, shorten production cycle, efficient and stable production Effect

Active Publication Date: 2020-11-10
云南锡业集团(控股)有限责任公司研发中心 +1
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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 invention titled "a method for purifying indium" discloses a preparation device and method for ultra-pure indium, and describes the use of 6N-7N grade high-purity indium as a seed crystal, using a suspension zone Ultra-pure indium with a purity of 6N can be obtained by melting method, but due to the small surface tension of indium melt, the output is very small each time, and large-scale 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 to obtain 6N-7N grade ultra-pure indium, but the solid-liquid interface of indium metal in the horizontal zone fused quartz boat is inclined, so the yield is generally lower than 60%; Moreover, it is difficult to apply a cooling system in the horizontal zone melting method, and it is difficult to control the width of the melting zone, resulting in low purification efficiency
The application number is CN201910606312.X, and the invention titled "A device for preparing ultra-pure indium and its preparation method" discloses a device and preparation method integrating vacuum distillation and vertical zone melting, heating and cooling by resistance wire The combination of devices realizes the precise control of the temperature zone, but in the zone melting process, it is necessary to carry out multi-pass repeated pulling process. After the sample is taken out, the impurity-enriched areas at both ends are removed, and then the multi-pass zone is repeated for many times. Only by melting can the indium be purified to 7N level, relatively speaking, the time and cost required are relatively high

Method used

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  • Device for preparing ultra-pure indium and method for preparing ultra-pure indium by adopting device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Put the quartz tube with 4N-grade indium raw material into the zone furnace, and evacuate to 1×10 -5 After Pa, backfill high-purity argon to 0.03MPa, and purify according to the following process flow.

[0049] 1. Vertical zone melting purification: move the quartz tube to the initial position, and perform 5 vertical zone melting purifications in sequence according to the following process parameters.

[0050] Zone melting parameters of the first pass: heating temperature is 400°C, cold trap temperature is 25°C, moving speed is 50μm / s;

[0051] Zone melting parameters of the second pass: heating temperature is 310°C, cold trap temperature is 25°C, moving speed is 25μm / s;

[0052] Zone melting parameters of the third pass: heating temperature is 310°C, cold trap temperature is 25°C, moving speed is 25μm / s;

[0053] The zone melting parameters of the 4th pass: the heating temperature is 310°C, the cold trap temperature is 25°C, and the moving speed is 25μm / s;

[0054] ...

Embodiment 2

[0061] Load the quartz tube with 4N-grade raw materials into the zone furnace and evacuate to 1×10 -5 After Pa, backfill high-purity argon to 0.03MPa, and purify according to the following process flow.

[0062] 1. Vertical zone melting purification: move the quartz tube to the initial position, and perform 7 vertical zone melting purifications in sequence according to the following process parameters.

[0063] Zone melting parameters of the first pass: heating temperature is 600°C, cold trap temperature is 25°C, moving speed is 50μm / s;

[0064] Zone melting parameters of the second pass: heating temperature is 310°C, cold trap temperature is 25°C, moving speed is 25μm / s;

[0065] Zone melting parameters of the third pass: heating temperature is 310°C, cold trap temperature is 25°C, moving speed is 25μm / s;

[0066] The zone melting parameters of the 4th pass: the heating temperature is 310°C, the cold trap temperature is 25°C, and the moving speed is 25μm / s;

[0067] Zone m...

Embodiment 3

[0076] Put the quartz tube containing the 5N grade indium raw material into the zone furnace and evacuate to 1×10 -5 After Pa, backfill high-purity argon to 0.03MPa, and purify according to the following process flow.

[0077] 1. Vertical zone melting purification: move the quartz tube to the initial position, and perform 7 vertical zone melting purifications in sequence according to the following process parameters.

[0078] Zone melting parameters of the first pass: heating temperature is 400°C, cold trap temperature is 25°C, moving speed is 50μm / s;

[0079] Zone melting parameters of the second pass: heating temperature is 310°C, cold trap temperature is 25°C, moving speed is 25μm / s;

[0080] Zone melting parameters of the third pass: heating temperature is 310°C, cold trap temperature is 25°C, moving speed is 25μm / s;

[0081] The zone melting parameters of the 4th pass: the heating temperature is 310°C, the cold trap temperature is 25°C, and the moving speed is 25μm / s; ...

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Abstract

The invention discloses a top end self-suction type vertical zone melting purification device and method for preparing ultra-pure indium. The device comprises a vacuum cavity, a vertical zone meltingsystem arranged in the vacuum cavity and a self-suction system arranged at the upper end of the vacuum cavity. The method is characterized in that a quartz tube filled with 4N / 5N-grade indium raw materials is installed into the vertical zone melting system, a heating temperature and a cold trap temperature are set, the quartz tube is driven to move up and down through a guide rod, multi-pass vertical zone melting is carried out, and after n (n ranges from 5 to 10) passes of vertical zone melting purification in each cycle is carried out, indium metal, with the volume fraction of 10 %-20 % of asample, at the top end in the quartz tube is molten, and sucking out is carried out through the self-suction system; indium raw materials with the same mass is supplemented; and after three cycles, total 3n times of vertical zone melting purification processes, are completed, taking out is carried out, the parts, both with the volume fraction of 5 %-15 % of the sample, at each of the two ends ofthe quartz tube are cut out, and the remaining part, in the middle area, of the sample is subjected to remelting sample preparation. By means of the top end self-suction type vertical zone melting device and method, the efficient and stable production of ultra-pure indium products of different grade purities of 6N or above can be achieved.

Description

technical field [0001] The invention belongs to the field of preparation of ultrapure indium, and in particular relates to a device for preparing ultrapure indium and a preparation method using the device. 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. For example, indium phosphide semiconductor materials made of ultra-pure indium are widely used in cutting-edge fields such as 5G communications, infrared detection, and image transmission. The purification methods of indium metal mainly include chemical electrol...

Claims

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Application Information

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IPC IPC(8): C22B9/16C22B58/00
CPCC22B9/16C22B58/00Y02P10/20
Inventor 郑红星彭巨擘李明旭伍美珍钱权张启旺张云虎卢兴伟陈丽诗雷云周京明
Owner 云南锡业集团(控股)有限责任公司研发中心
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