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Preparation method of metal hafnium raw material for iodization

A technology of iodination and raw materials, which is applied in the field of raw material preparation, can solve the problems of affecting the deposition rate of iodination reaction, unfavorable iodination furnace loading and discharge, and reducing production efficiency, so as to facilitate iodination operation, improve iodination efficiency, and prevent poisoning effect

Active Publication Date: 2014-06-11
有研资源环境技术研究院(北京)有限公司
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  • Summary
  • Abstract
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  • Claims
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Problems solved by technology

However, due to the small particle size of hafnium powder, which is sub-micron, the specific surface energy is large, and it is flammable in the process of friction and collision, which is not conducive to the iodine loading and discharge; at the same time, the particle size of hafnium powder is too small to affect the deposition of iodination reaction. The speed reduces the production efficiency, so the hafnium powder produced by direct reduction cannot be directly used in the iodination method, and must be treated accordingly

Method used

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preparation example Construction

[0027] The present invention is used for the preparation method of the raw material of metal hafnium iodide, comprises the steps:

[0028] a. Press the hafnium powder under a certain pressure into a hafnium block of a certain shape; the purity of the hafnium powder is greater than 90wt%, and the particle size is less than 1mm; the pressure during pressing is 1~5Mpa; the shape of the compact is cuboid or cylinder, cuboid The size is (length>5mm)×(width>5)×(height>5mm), and the typical size is (10~200mm)×(10~80mm)×(10~80mm).

[0029] b. Dry the compact at a certain temperature for several hours; the drying temperature is 40-200° C., and the drying time is 1-50 hours. The compact must be completely dehydrated.

[0030] c. Then put the compact into a crucible and put it into a vacuum tungsten wire furnace for vacuum sintering; the temperature of vacuum sintering is not lower than 500°C, and the optimum temperature is 500~1800°C; the vacuum degree of vacuum sintering must be not lo...

Embodiment 1

[0034] The hafnium powder with a purity of 90wt% and a particle size of less than 1mm was pressed into a compact of 10mm×10m×10mm under a pressure of 1Mpa. The compact was baked at a temperature of 40° C. for 1 hour to remove moisture in the compact. Put the dried compact into a molybdenum crucible and place it in a vacuum tungsten wire furnace for vacuum sintering with a vacuum degree of 5.0×10 -1 Pa; Heating is carried out by means of segmented heat preservation, at 200°C for 0.5h, and the final sintering temperature is 500°C, with heat preservation for 1h. The purity of the finally obtained hafnium block is above 95wt%, the hydrogen content is less than 1000ppm, and the pores are evenly distributed.

Embodiment 2

[0036] The hafnium powder with a purity of 90% and a particle size of less than 1mm was pressed into a compact of 50mm×30mm×30mm under a pressure of 2Mpa. The compact was baked at a temperature of 100° C. for 5 hours to remove moisture in the compact. Put the dried compact into a tantalum crucible and place it in a vacuum tungsten wire furnace for vacuum sintering with a vacuum degree of 4.0×10 -2 Pa; Heating is carried out by means of segmented heat preservation, at 200°C for 1h, and the final sintering temperature is 900°C, and hold for 3h. The resulting hafnium block has a purity of 96.5%, a hydrogen content of less than 1000ppm, and a uniform pore size distribution.

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Abstract

The invention relates to a preparation method of a metal hafnium raw material for iodization. The preparation method of the metal hafnium raw material for iodization comprises the following steps: firstly, pressing hafnium powder into a green compact; drying the obtained green compact; loading the green compact into a crucible, and carrying out vacuum sintering in a vacuum tungsten wire furnace; obtaining loose and porous hafnium raw material with even pores, wherein the purity of hafnium is above 95wt%, the total content of gas and metal impurities is less than 5wt%, the hydrogen content is less than 1000ppm, and the hafnium raw material is used for iodization. The preparation method of the metal hafnium raw material for iodization, which is disclosed by the invention, is safe and controllable and is favorable for the iodization operation, and the iodization efficiency is improved.

Description

technical field [0001] The invention relates to a method for preparing raw materials for iodination of metal hafnium. The raw materials can be iodized to obtain high-purity metal hafnium, titanium and zirconium used in fields such as atomic energy industry, information industry, petrochemical industry and aerospace. Background technique [0002] Hafnium has good thermal neutron absorption cross section and good corrosion resistance, and is the control rod material of nuclear reactors; hafnium has good oxidation resistance and corrosion resistance, and is the best choice for use in corrosive environments. In addition, hafnium plays a very important role in metallurgy, chemical industry, aerospace and other fields. For example, adding a small amount of hafnium to metals in the metallurgical industry can improve its mechanical properties and oxidation resistance at high temperatures; adding a small amount of hafnium to stainless steel can increase the strength of steel. In the...

Claims

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Application Information

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IPC IPC(8): B22F3/16C22B34/14
Inventor 王芳黄永章王力军江洪林罗远辉陈松张力
Owner 有研资源环境技术研究院(北京)有限公司
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