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Process for Purifying Nitrogen Trifluoride Gas

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Process for Purifying Nitrogen Trifluoride Gas Europaisches Patentamt 19 European Patent Office Office europeen des brevets © Publication number: 0 344 612 B1 12 EUROPEAN PATENT SPECIFICATION @ Date of publication of patent specification <&) Int. CI.5: C01B 21/083 17.03.93 Bulletin 93/11 (21) Application number: 89109439.3 (22) Date of filing : 24.05.89 (S) Process for purifying nitrogen trifluoride gas. (So) Priority: 01.06.88 JP 135061/88 @ Proprietor : MITSUI TOATSU CHEMICALS, Inc. 2-5 Kasumigaseki 3-chome Chiyoda-Ku Tokyo 100 (JP) (43) Date of publication of application 06.12.89 Bulletin 89/49 (72) Inventor : Koto, Nobuhiko 5-7-2, Hikoshima Sakomachi, (45) Publication of the grant of the patent : Shimonoseki-shi, Yamaguchi-ken, (JP) 17.03.93 Bulletin 93/11 Inventor : Nishitsuji, Toshihiko 5-9-6, Hikoshima Sakomachi, Shimonoseki-shi, Yamaguchi-ken, (JP) @ Designated Contracting States : Inventor : Iwanaga, Naruyuki BE CH DE FR GB IT LI NL SE 5-7-1, Hikoshima Sakomachi, Shimonoseki-shi, Yamaguchi-ken, (JP) Inventor : Harada, Isao @ References cited : 5-7-2, Hikoshima Sakomachi, EP-A- 0 004 767 Shimonoseki-shi, Yamaguchi-ken, (JP) EP-A- 0 007 175 PATENT ABSTRACTS OF JAPAN vol. 11, no. 96 (C-412)(2543), 26 March 1987; & JP-A-61 247 (74) Representative : Schiiler, Horst, Dr. 609 (SHOWA DENKO K.K.) 04-11-1986 Patentanwalt, Kaiserstrasse 69 CHEMIE INGENIEUR TECHNIK vol. 41, no. 12, W-6000 Frankfurt/Main 1 (DE) 1969, pages 695-700; J. MASSONE: "Herstellung und Reinigung und Stickstofftrif- luorid in einer Versuchsanlage " PATENT ABSTRACTS OF JAPAN vol. 9, no. 205 (C-299)(1928), 22 August 1985; & JP - A - 60 71503 (CENTRAL GLASS K.K.) 23-04-1985 CO CM S CO Note : Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been LU filed until the opposition fee has been paid (Art. 99(1) European patent convention). Jouve, 18, rue Saint-Denis, 75001 PARIS EP 0 344 612 B1 Description The present invention relates to a process for purifying a nitrogen trif luoride gas. More specifically, it relates to a process for particularly removing oxygen difluoride from a nitrogen trifluoride gas. 5 In recent years, a nitrogen trifluoride (NF3) gas is noticed as a dry etching agent for semiconductors and as a cleaning gas for CVD apparatus, but the nitrogen trifluoride gas for use in these use purposes is required to be pure as highly as possible. The NF3gascan be prepared by a variety of methods such as the so-called molten salt electrolysis method in which NH4F xHF which is prepared by acidic ammonium fluoride alone or ammonium fluoride and hydrogen 10 fluoride as the starting materials is electrolyzed, or the method in which ammonia and fluorine are reacted. The present inventors have confirmed that NF3 gases obtained by any of the methods contain oxygen difluor- ide (OF2) in most of the cases with a relatively large amount. Particularly, in NF3 gas obtained by the molten salt electrolysis method, at most several hundred ppm or so (wherein "ppm" represents a volume standard, hereinafter the same) thereof are contained. 15 It has been known that in the NF3 gases prepared by the above methods, various compounds such as nitrogen (N2), dinitrogen difluoride (N2F2), nitrous oxide (N20), carbon dioxide (C02) and unreacted hydrogen fluoride (HF) are contained as impurities. Accordingly, in order to obtain a high purity NF3 gas, it is required to remove these impurities, and various methods for purification have been proposed. Regarding OF2, in "Deutsche Luft und Raumfahrt", Forschungs- 20 bericht, Oktober 1966, Herstellung von Stickstoff-fluoriden durch Elektrolyse, p. 21, lines 19 to 20, there is de- scribed that OF2 in a NF3 gas can be reduced by using sodium sulfite and potassium iodide aqueous solutions. Also, in "Fluorine Chemistry and Industry, Advance and Application", edited by Nobuatsu Watanabe (Published by Kagaku Kogyosha), p. 208 (1973), there is described the method that a NF3gas is washed with an aqueous sodium thiosulfate solution to remove N20 in the NF3 gas. However, there is not described that OF2 in the NF3 25 gas can be removed. Also, in J. Massonne, Chem. Ing. Techn. vol. 41(12), p. 695 (1969), there is described, as a method of removing N2F2 in a NF3 gas, the method in which an aqueous solution such as of Kl, HI, Na2S, Na2S204 or Na2S03 is used to remove N2F2 therefrom. However, according to the method, for removing N2F2 completely, a relatively long time is required so that the reaction bath becomes considerably large as well as a large amount 30 of chemicals is required. In this literature, no removal of OF2 is described. The present inventors have established the under-mentioned quantitative method of OF2 which uses a low temperature gas chromatography and confirmed that the content of OF2 in a NF3 gas sometimes reaches even to several hundred ppm. Since the OF2 is an oxygen-containing compound, it can be estimated that it is extremely dangerous in 35 the step of purifying a NF3 gas. Accordingly, in the case of purifying a NF3 gas, it is necessary to possibly re- move OF2 at a relatively initial stage. Also, if OF2 remains in a NF3 gas, it is inconvenient for further treating the NF3 gas to obtain a high purity NF3 gas, Moreover, if such an oxygen-containing compound is contained, it involves the problem that it exerts bad effect when the NF3 gas is used as a dry etching agent for semiconductors or as a cleaning gas for CVD 40 apparatus. An object of the present invention is to provide a process for purifying nitrogen trifluoride gas in which oxy- gen difluoride in the nitrogen trifluoride gas can be removed with extremely good efficiency and economically. That is, the present invention is a process for purifying a nitrogen trifluoride gas which comprises removing hydrogen fluoride from a nitrogen trif luoride gas containing hydrogen fluoride in an amount more than 100 ppm 45 and oxygen difluoride until the content of hydrogen fluoride becomes 100 ppm or less, or using a nitrogen tri- fluoride gas containing 100 ppm or less of hydrogen fluoride and oxygen difluoride, and then contacting the nitrogen trifluoride gas containing 1 00 ppm or less of hydrogen fluoride with at least one aqueous solution con- taining one selected from the group consisting of sodium thiosulfate, hydrogen iodide and sodium sulfide to reduce the content of oxygen difluoride to 10 ppm or less. 50 For removing hydrogen fluoride, it is preferred to control the concentration of hydrogen fluoride to 1 00 ppm or lower by contacting a nitrogen trifluoride gas with water or an aqueous NaOH solution. For removing oxygen difluoride, it is preferred that the NF3 gas is contacted with the aforesaid at least one aqueous solution containing one selected from the group consisting of sodium thiosulfate, hydrogen iodide and sodium sulfide at a temperature of 0 to 20°C. 55 For the operation of the gas-liquid contact, it is preferred to use a gas scrubber. In the following, the present invention will be described in more detail. NF3 gases can be prepared by various methods such as the so-called molten salt electrolysis method in which NH4F xHF prepared by acidic ammonium fluoride alone or ammonium fluoride and hydrogen fluoride 2 EP 0 344 612 B1 as the starting materials is electrolyzed, or the method in which ammonia and fluorine are reacted. In the present invention, HF in a NF3 gas should firstly be removed. The method of removing the HF is not particularly limited, but, for example, there may be employed the method in which, as shown in Fig. 1, by using a gas scrubber, water or an alkaline aqueous solution such as of sodium hydroxide, etc. is circulated in 5 the gas scrubber and the NF3 gas is contacted with the water or the alkaline aqueous solution so that HF is absorbed by the water or the above aqueous solution to remove it (in this case, the procedure is usually carried out with a concentration of the aqueous solution of generally 0.1 to 1% by weight) orthe method in which by using a compound such as sodium fluoride (NaF) as an adsorbent, and the adsorbent and NF3 gas are con- tacted at a temperature of 100°C or so to adsorb and remove HF, and the like. In the step of removing HF, it 10 is preferred that HF in a NF3 gas is removed as much as possible. It is required to remove it at least by 100 ppm or less. It is needless to say that if a NF3gas containing 100 ppm or less of HF is used from the beginning, no HF removing process is required. As the temperature of contacting the NF3 gas with water or an aqueous alkaline solution, as in the removing process of OF2 as mentioned below, it is preferred as low as possible in such a range that no hindrance is 15 caused to the operation. But considering the facts that to use water is more economical and the OF2 removing process is present thereafter, it is preferred in the range of, for example, 15 to 30°C or so. The NF3 gas freed of HF mentioned above is then contacted with at least one aqueous solution containing one selected from the group consisting of sodium thiosulfate (Na2S203), hydrogen iodide (HI) and sodium sul- fide (Na2S) to remove OF2 contained therein.
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