Method for directly preparing zirconium deuteride by using high temperature direct method

A technology of zirconium deuteride and direct method, which is applied in the interdisciplinary field of material science and nuclear science, can solve the problems of unfavorable industrial scale production of zirconium deuteride, and achieve simple and easy-to-purchase preparation equipment, good product stability, and harmless to human body and environment Effect

Inactive Publication Date: 2014-12-03
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that the preparation of existing zirconium deuteride is not conducive to industrial scale production, and to provide a method for preparing zirconium deuteride by direct method at high temperature

Method used

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  • Method for directly preparing zirconium deuteride by using high temperature direct method

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Experimental program
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Effect test

Embodiment 1

[0023] Metal zirconium with a purity of 99.4% was cut into small pieces with a particle size of 2 mm, weighed 503 g, and packed into a quartz glass tube. Under the protection of argon, place the quartz tube in the high-temperature heating furnace cabin, and close the furnace cabin, such as figure 1 shown. Introduce argon gas to replace the gas in the furnace chamber, and pump the pressure in the chamber to a negative pressure of 0.025MPa, then pass in deuterium gas with a purity of 99.999% to replace the argon in the chamber, and pump it again to a negative pressure of 0.018MPa, Repeat the operation 3 times; quickly raise the temperature to 567°C at a heating rate of 30°C / min, pass in deuterium gas, control the flow rate at 903ml / min, and heat at a rate of 10°C / min for 43 minutes to 890°C to stop heating , constant temperature and deuterium gas flow rate, and continue to react for 122min. At this time, the deuterium pressure gauge and the pressure in the heating reaction furn...

Embodiment 2

[0025] Metal zirconium with a purity of 99.99% is cut into small pieces with a particle size of 8mm, weighed 1400g of the zirconium piece, put it into a quartz glass tube, put the quartz tube in a high-temperature heating furnace cabin, and close the furnace cabin. Control the ventilation valve, and after argon gas is introduced into the furnace cabin, the pressure in the cabin is pumped to a negative pressure of 0.019MPa, and then high-purity deuterium gas is introduced. After repeated operations 4 times, all valves are closed. Rapidly raise the temperature to 586°C at a heating rate of 20°C / min, open the deuterium gas valve, and introduce deuterium gas with a purity of 99.999%, control the flow rate at 1994ml / min, and raise the temperature at a rate of 15°C / min for 36 minutes Stop heating at 867°C, keep the temperature and deuterium flow rate constant, and continue to react for 164 minutes. At this time, the deuterium pressure gauge and the pressure in the heating reaction fu...

Embodiment 3

[0027] Metal zirconium pieces with a purity of 99.99% and a particle size of 15mm were stirred in aqua regia at 5°C for 10 minutes under the protection of argon, washed 4 times with deionized water, and dried in vacuum; under the protection of argon, weigh the above-mentioned Put 2802g of zirconium block into the quartz glass tube, and plug the nozzle with a rubber stopper; under the protection of argon, place the quartz tube in the high-temperature heating furnace cabin, quickly pull out the rubber stopper and quickly close the furnace cabin; After replacing the gas in the furnace chamber with gas, the pressure in the chamber is pumped to a negative pressure of 0.022MPa, and then 99.999% deuterium gas is introduced, and the operation is repeated 3 times; Deuterium gas, control the flow rate at 4499ml / min, and at the same time raise the temperature at a rate of 10°C / min for 52min to 862°C to stop heating, keep the temperature and deuterium flow rate constant, and continue to re...

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Abstract

The invention relates to a method for directly preparing zirconium deuteride by using a high temperature direct method, belonging to the field of material science and nuclear science. According to the method, metal zirconium is reacted with deuterium gas, and thus zirconium deuteride is generated. By adopting the method, the problems of industrial-scale zirconium deuteride preparation techniques and preparation purity are solved, no complex production device is needed, the necessary preparation devices are simple and easy to purchase, and safety construction of a zirconium deuteride production line can be achieved under the existing factory conditions; the preparation process is simple and easy to operate, no high temperature pressurizing / depressurizing device is used in the preparation process, and due to protective inert gases, the production is safe and reliable; the zirconium deuteride product is relatively good in yield and purity, good in stability and can be stored for a long time; the production process is free of three wastes, is harmless for human bodies and the environment, is environment-friendly, and is significant for safe industrial scale preparation and large-scale application of high-purity zirconium deuteride.

Description

technical field [0001] The invention relates to a method for preparing zirconium deuteride by a high-temperature direct method, which belongs to the interdisciplinary field of material science and nuclear science. Background technique [0002] Materials are the material basis for the survival and development of human beings. People regard information, materials and energy as the pillars of social civilization, and regard new materials, information technology and biotechnology as an important symbol of the new technological revolution. In modern society, materials have become an important part of national economic construction, national defense construction and people's lives. Continuously developing new materials and using new materials in new fields has become the embodiment of a country's scientific research strength and comprehensive creativity. [0003] Zirconium (Zr) and titanium are in the fourth subgroup, and they have similarities in element properties, so they are ...

Claims

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Application Information

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IPC IPC(8): C01G25/00
Inventor 刘吉平刘晓波
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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