Method of electrolytically synthesizing nitrogen trifluoride

A technology of nitrogen trifluoride and electrolytic synthesis, which is applied in the direction of electrolytic components, electrolytic process, electrodes, etc., and can solve the problems of not including

Active Publication Date: 2010-01-13
DE NORA PERMELEC LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the literature does not include information on the electrolytic synthesis of NF from highly oxidized metal fluorides by molten salt electrolysis. 3 The content of the application in the method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Graphite plates were used as conductive substrates, and conductive diamond electrodes were prepared using a hot wire CVD apparatus under the following conditions.

[0068] The surface of the substrate was polished with abrasives composed of diamond particles with a particle size of 1 μm. The average surface roughness (Ra) of the substrate surface was 0.2 μm, and the ten-point surface roughness (Rz) was 6 μm. Subsequently, diamond particles having a particle diameter of 4 nm were fixed on the surface of the substrate as nuclei, and the substrate was connected to a hot-filament CVD apparatus. A gaseous mixture obtained by mixing hydrogen gas with 1 volume % of methane gas and 0.5 ppm of trimethylboron gas was fed into the apparatus. While passing the gaseous mixture at a rate of 5 L / min through the device and maintaining the internal pressure of the device at 75 Torr, electric power was supplied to the filament to heat the filament to a temperature of 2,400°C. Under the...

Embodiment 2

[0075] Electrolysis was carried out in the same manner as in Example 1, except that the current density was changed to 0.4A / cm 2 . It was found that the NF 3 The current efficiency of the preparation was 50%.

Embodiment 3

[0079] Both lithium and nickel ions dissolve into NH 4 In F-2HF molten salt until saturated concentration, and at 120°C temperature and 0.1A / cm 2 Under the current density condition, use the equipment used in embodiment 1 to carry out constant current electrolysis. Analysis of the gas generated at the anode 100 hours after the start of electrolysis indicated that the relevant NF 3 The current efficiency of the preparation was 65%.

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Abstract

The present invention provides an electrolytic synthesis method of nitrogen trifluoride, comprising electrolytically synthesizing nitrogen trifluoride gas from ammonium fluoride in an ammonium fluoride-containing molten salt mixture using a carbonaceous electrode as an anode, wherein the method comprises: a step of dissolving, in the molten salt mixture, metal ions capable of electrolytically yielding a highly oxidized metal fluoride through reaction with fluorine radicals (F.) that are generated upon the discharge of fluoride ions which are a component of the ammonium fluoride, thereby reacting the metal ions with the fluorine radicals (F.) to yield the highly oxidized metal fluoride, and reacting the highly oxidized metal fluoride with ammonium ions on a surface of the electrode and in a solution to synthesize nitrogen trifluoride gas.

Description

technical field [0001] The invention relates to a method for electrolytically synthesizing nitrogen trifluoride gas from a molten salt mixture containing ammonium fluoride. More specifically, the present invention relates to an electrolytic synthesis method in which the occurrence of an anode effect is suppressed and generation of sludge due to electrode wear is avoided even when the battery is operated at a high current density, which enables efficient continuous Synthesis of nitrogen trifluoride gas. Background technique [0002] Nitrogen trifluoride (NF 3 ) is a fluoride of nitrogen that was first synthesized by Ruff et al. in 1928 by molten salt electrolysis. In the planetary exploration rocketry planned and implemented by NASA in the United States, trifluoride is consumed as a fuel oxidizer in large quantities, and has received a lot of attention. At present, nitrogen trifluoride is widely used as a dry etching gas in the production steps of semiconductor devices and...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B1/24C25B11/12
CPCC25B1/245C01B21/083C25B1/24
Inventor 田坂明政
Owner DE NORA PERMELEC LTD
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