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Preparation method of high purity tellurium

A technology of high-purity tellurium and purification method, which is applied in the field of preparation of high-purity tellurium, can solve the problem of low purification effect of tellurium vacuum distillation, and achieve the effect of low preparation cost

Inactive Publication Date: 2011-08-17
JIAXING DAZE PHOTOELECTRIC TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the vacuum distillation of tellurium proved to be much less effective than expected

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 100g of industrial tellurium powder into 500ml of concentrated nitric acid solution with a mass fraction of 40%, stir for 2h, and react at 25°C for 40min. After filtering, the prepared tellurium dioxide was boiled in deionized water for 20 minutes, filtered, and rinsed with deionized water for 3 times.

[0017] Add 100 g of the prepared tellurium dioxide into 500 ml of 40% hydrochloric acid by mass fraction, stir, add 30% hydrogen peroxide during the reaction, the reaction temperature is 80° C., and filter after the tellurium dioxide is dissolved.

[0018] Heat the filtrate to 85°C, add sodium sulfite solution to the filtrate, fully reduce tellurium, filter, wash and dry to obtain tellurium powder with a purity of 99.97%.

[0019] Put the prepared tellurium powder into a single crystal furnace, pump it into a vacuum of 1 Pa, and pass in hydrogen as a protective atmosphere, melt the tellurium powder at 420 ° C, and stir the melt by rotating the crucible. until all t...

Embodiment 2

[0021] Add 50g of industrial tellurium powder into 500ml of concentrated nitric acid solution with a mass fraction of 50%, stir for 1h, and react at 60°C for 60min. After filtering, the prepared tellurium dioxide was put into deionized water and boiled for 20 minutes, filtered, and rinsed twice with deionized water.

[0022] Add 100 g of the prepared tellurium dioxide into 500 ml of 30% hydrochloric acid by mass fraction, stir, add 20% hydrogen peroxide during the reaction, the reaction temperature is 60°C, and filter after the tellurium dioxide is dissolved.

[0023] Heat the filtrate to 80°C, add sodium sulfite solution to the filtrate, fully reduce tellurium, filter, wash and dry to obtain tellurium powder with a purity of 99.99%.

[0024] Put the prepared tellurium powder into a single crystal furnace, pump it into a high vacuum, and pass in hydrogen as a protective atmosphere, melt the tellurium powder at 450°C, and stir the melt by rotating the crucible. until all the m...

Embodiment 3

[0026] Add 70g of industrial tellurium powder into 250ml of concentrated nitric acid solution with a mass fraction of 69%, stir for 3h, and react at 80°C for 30min. After filtering, the prepared tellurium dioxide was boiled in deionized water for 30 minutes, filtered, and then rinsed with deionized water for 4 times.

[0027] Add 100 g of the prepared tellurium dioxide into 200 ml of 40% hydrochloric acid by mass fraction, stir, add 10% hydrogen peroxide during the reaction, the reaction temperature is 40°C, and filter after the tellurium dioxide is dissolved.

[0028] Heat the filtrate to 75°C, add sodium sulfite solution to the filtrate, fully reduce tellurium, filter, wash and dry to obtain tellurium powder with a purity of 99.95%.

[0029] Put the prepared tellurium powder into a single crystal furnace, pump it into a high vacuum, and pass in hydrogen as a protective atmosphere, melt the tellurium powder at 500 ° C, and stir the melt by rotating the crucible. until all th...

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Abstract

The invention discloses a preparation method of high purity tellurium. In the method, industrial tellurium of which purity is 99% is used as a raw material and the chemical and physical methods are combined to prepare high purity tellurium. The method comprises the following steps: dissolving the raw material in nitric acid, stirring, heating, filtering, adding the obtained tellurium dioxide in hydrochloric acid, introducing hydrogen peroxide, filtering after dissolving; adding sodium sulfite solution in the filtrate to reduce and obtain 3N-4N of fine tellurium; and dissolving at 400-450 DEG C in hydrogen atmosphere, and adopting the Czochralski purification method to treat fine tellurium and obtain 5N-6N of high purity tellurium. The method has low preparation cost; and the high purity tellurium can be used in the semiconductor material fields such as solar cell, light-emitting diode (LED), thermoelectricity and infrared field.

Description

technical field [0001] The invention relates to a method for preparing tellurium, in particular to a method for preparing high-purity tellurium. Background technique [0002] High-purity tellurium is widely used in semiconductor materials, such as CdTe, HgCdTe, CdZnTe, PbTe, BiTe is the main material for the preparation of solar cells, infrared measurement materials, electro-optical modulators, ray detection materials and cooling materials. Since even very small amounts (10 -5 Grade) impurities will also lead to poor electrical properties of materials, and the purity of tellurium is an important factor that directly affects the properties of materials. [0003] At present, tellurium with a content of 99.99% is generally obtained by electrolysis, and high-purity tellurium is prepared by multiple vacuum distillation and zone melting to form a physical purification process. The effect of this process depends on the effect of vacuum distillation purification of tellurium, that...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/02
Inventor 席珍强徐敏
Owner JIAXING DAZE PHOTOELECTRIC TECH
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