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Method for preparing ultra-pure cadmium

An ultra-high-purity technology, applied in the field of preparation of ultra-high-purity cadmium, can solve problems such as low efficiency, loss, and carbon film shedding of quartz boats

Inactive Publication Date: 2021-03-09
清远先导材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, this method has some defects. First, in the process of manufacturing by this method, due to the high content of impurities in the cadmium raw material, and the distribution of impurities is often not very uniform, when it is directly placed on a quartz boat for heating, the distribution is uneven. Uniform impurities are difficult to completely remove, and the impurities contained in them will also cause the carbon film on the quartz boat to fall off, affecting the purification effect of the product
[0005] Secondly, this kind of zone melting heating tube that uses electricity to generate heat basically adopts the structure of resistance wire, but on the one hand, the heat on the external resistance wire will be dissipated during the process of transferring the heat on the external resistance wire to the cadmium raw material in the zone melting tube through heat transfer and heat radiation. A lot of heat is lost, the heat transfer efficiency is low and the ambient temperature is too high; on the other hand, the temperature of the resistance wire is difficult to control accurately, and it is difficult to meet the requirements in the preparation of ultra-high-purity cadmium with very strict precision requirements, and the pass rate is difficult to improve
Furthermore, since the raw materials in the quartz boat need to be heated repeatedly to achieve the target purity, the production cycle of this type of equipment is only a single set of quartz boats and quartz boats, and the efficiency is relatively low.

Method used

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  • Method for preparing ultra-pure cadmium

Examples

Experimental program
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Effect test

Embodiment 1

[0051] Put the 5N raw material cadmium into the graphite crucible of the distillation furnace, install it in sequence: lower graphite cover, graphite guide plate, graphite condenser, upper graphite cover, close the furnace cover, and evacuate to 10 -2 Next, turn on the heating, raise the temperature to 390°C, and keep it warm for 10 hours; after cooling down, take out the product on the graphite condenser, cut off the tail of the taken out cadmium ingot by 10cm, and the product is 6N cadmium ingot.

[0052] Melt the 6N cadmium ingot in a high-purity graphite crucible, then pour it into a graphite boat to re-cool it and form it into a cadmium ingot; use nitric acid aqueous solution to corrode it for 2 hours, take it out, and then use nitric acid ethanol solution to clean the cadmium ingot until the surface of the cadmium ingot is bright , showing the true color of cadmium metal, the volume ratio of nitric acid and water in the nitric acid aqueous solution is 10%, and the volume ...

Embodiment 2

[0057] Put the 5N raw material cadmium into the graphite crucible of the distillation furnace, install it in sequence: lower graphite cover, graphite guide plate, graphite condenser, upper graphite cover, close the furnace cover, and evacuate to 10 -2 Next, turn on the heating, raise the temperature to 400°C, and keep it warm for 9 hours; after cooling down, take out the product on the graphite condenser, cut off 9cm of the tail of the taken out cadmium ingot, and the product is 6N cadmium ingot.

[0058] Melt the 6N cadmium ingot in a high-purity graphite crucible, then pour it into a graphite boat to re-cool it and form it into a cadmium ingot; use nitric acid aqueous solution to corrode it for 2 hours, take it out, and then use nitric acid ethanol solution to clean the cadmium ingot until the surface of the cadmium ingot is bright , showing the true color of cadmium metal, the volume ratio of nitric acid and water in the nitric acid aqueous solution is 10%, and the volume ra...

Embodiment 3

[0063] Put the 5N raw material cadmium into the graphite crucible of the distillation furnace, install it in sequence: lower graphite cover, graphite guide plate, graphite condenser, upper graphite cover, close the furnace cover, and evacuate to 10 -2 Next, turn on the heating, raise the temperature to 410°C, and keep it warm for 8 hours; after cooling down, take out the product on the graphite condenser, cut off the tail of the taken out cadmium ingot by 10cm, and the product is 6N cadmium ingot.

[0064] Melt the 6N cadmium ingot in a high-purity graphite crucible, then pour it into a graphite boat to re-cool it and form it into a cadmium ingot; use nitric acid aqueous solution to corrode it for 2 hours, take it out, and then use nitric acid ethanol solution to clean the cadmium ingot until the surface of the cadmium ingot is bright , showing the true color of cadmium metal, the volume ratio of nitric acid and water in the nitric acid aqueous solution is 10%, and the volume r...

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Abstract

The invention discloses a method for preparing ultrahigh-purity cadmium. The method for preparing the ultrahigh-purity cadmium comprises the following steps of: remelting and shaping: melting a cadmium ingot in a high-purity graphite crucible, pouring the melted cadmium ingot into a graphite boat, and cooling and shaping the melted cadmium ingot again to form the cadmium ingot; acid pickling: after corroding the cadmium ingot obtained in the remelting and shaping step by using a nitric acid aqueous solution for 1.5-2.5 hours, taking out the cadmium ingot, and then cleaning the cadmium ingot byusing a nitric acid ethanol solution until the surface of the cadmium ingot is bright and the cadmium ingot shows the natural color of cadmium metal; and cleaning the surface of the cadmium ingot byusing water until the surface of the cadmium ingot is neutral, and drying the surface moisture in vacuum; and zone melting: carrying out zone melting on the cadmium ingot subjected to the acid pickling step to obtain a finished cadmium product. According to the method for preparing the ultra-pure cadmium, the pre-treatment of the cadmium raw material is added before the zone-melting step, so thatthe purity of a cadmium finished product can be further improved.

Description

technical field [0001] The invention relates to the technical field of cadmium preparation equipment, in particular to a method for preparing ultra-high-purity cadmium. Background technique [0002] Cadmium is a silvery-white shiny metal with high tensile strength. It can be used in electroplating and manufacturing plastic stabilizers and pesticides, etc., and has a wide range of applications. Among them, the cadmium zinc telluride (CZT) nuclear radiation detector and the mercury cadmium telluride (MCT) infrared detector substrate material made of ultra-high-purity cadmium with a purity of 99.99999% (7N) are used in national defense, security, positioning, and guided infrared detection. The field has wide application. Impurities in cadmium directly affect the performance of CZT and MCT crystal materials, and then affect the detection range and detection accuracy of these two detectors. Therefore, it is of great significance to study and prepare an ultra-high-purity cadmium ...

Claims

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Application Information

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IPC IPC(8): C22B17/06
CPCC22B17/06
Inventor 黄杰杰朱刘何志达李清宇
Owner 清远先导材料有限公司