US-12617683-B2 - Method for producing trifluoroamine oxide

US12617683B2US 12617683 B2US12617683 B2US 12617683B2US-12617683-B2

Abstract

There is provided a method for producing trifluoroamine oxide. The method includes a step of preparing an intermediate product by simultaneously providing and reacting nitrogen trifluoride and nitrous oxide under the presence of a SbF 5 reaction activator; and a step of producing trifluoroamine oxide by reacting the intermediate product with potassium fluoride. The step of reacting the intermediate product with potassium fluoride is performed under atmospheric pressure and room temperature.

Inventors

Junghun KWAK
Jihoon BAIK
Juhyeon KIM
Myoungsook LEE
Wonwook SO
Byunghyang Kwon
Yongjun Cho
Injoon PARK
Shinhong YUK
Bongjun CHANG
Hongsuk KANG
Eunho SOHN
Sanggoo LEE

Assignees

SK SPECIALTY CO., LTD
KOREA RESEARCH INSTITUTE OF CHEMICAL TECHNOLOGY

Dates

Publication Date: 20260505
Application Date: 20210923
Priority Date: 20201014

Claims (1)

1 . A method for producing trifluoroamine oxide comprising steps of: preparing an intermediate product by simultaneously feeding and reacting nitrogen trifluoride and nitrous oxide under the presence of a reaction activator of SbF 5 ; and producing trifluoroamine oxide by reacting the intermediate product with potassium fluoride, wherein the step of reacting the intermediate product with potassium fluoride is performed under atmospheric pressure and room temperature conditions.

Description

CROSS-REFERENCE TO PRIOR APPLICATIONS This application is a National Stage Patent Application of PCT International Patent Application No. PCT/KR2021/012937 (filed on Sep. 23, 2021) under 35 U.S.C. § 371, which claims priority to Korean Patent Application No. 10-2020-0132911 (filed on Oct. 14, 2020), which are all hereby incorporated by reference in their entirety. BACKGROUND The present invention relates to a method for producing trifluoroamine oxide (F3NO). Chemical vapor deposition (CVD) process technology is widely known as a thin film forming process for manufacturing a semiconductor device. When the thin film of the semiconductor device is formed in the CVD chamber, it is preferable that the thin film is formed only on the target portion in the CVD chamber, but the thin film forming material is undesirably deposited on other exposed surfaces in the CVD chamber. For example, the thin film forming material may also be deposited on a wall surface, a product fixing jig, a pipe, or the like in the chamber. In addition, material deposited in addition to the target portion during the CVD process can be peeled off to contaminate the surface of the thin film deposited on the target portion or the surface of the target portion on which the thin film is to be deposited. Such contamination causes defects in the semiconductor device, resulting in a reduction in yield. Therefore, a cleaning process is periodically performed to remove unnecessary deposits deposited in the chamber. The cleaning process in the CVD chamber may be performed manually or by using a cleaning gas. Several basic physical properties are required for the cleaning gas of the CVD chamber. First, the cleaning gas must be able to clean the inside of the CVD chamber within a short time, and should not generate harmful substances. In addition, the cleaning gas should be eco-friendly. A perfluorinated compound, such as CF4, C2F6, SF6, and NF3, has been used as a chamber cleaning gas or as an etching gas for a deposited thin film in a semiconductor or electronic device manufacturing process. Particularly, the nitrogen trifluoride (NF3) gas is widely used as the cleaning gas in the world. However, these perfluorinated materials reside in the atmosphere for a very long period of time due to their stability. In addition, since a waste gas after using contains perfluorinated materials which are not decomposed, in a very high concentration, the waste gas should be treated before being released into the atmosphere so that the perfluorinated materials are less than or equal to an acceptable level, and thus a lot of costs are required. Furthermore, these conventional perfluorinated materials are known to have very high global warming potential (GWP) values (100 years with reference to CO2, CF4 9,200, SF6 23,900, NF3 17,200). Thus, these gases give a significant load to the environment. Therefore, demands for an etching or cleaning gas having a low GWP value are very high. In addition, even if the cleaning or etching gas itself is eco-friendly, decomposition into harmful CF4, NF3 and the like may occur during the cleaning or etching process, and thus, when they are discharged, they may remain in the atmosphere for a long period of time. In particular, the nitrogen trifluoride (NF3) gas is not only globally used in a large amount, but also has a very high global warming potential. Therefore, it is required to reduce the use of the NF3 gas and to develop a replaceable substance to reduce the load on the environment and to make a sustainable development of the semiconductor industry. Among the alternative candidate gases, trifluoroamine oxide (F3NO) is promising because it is easily decomposed in an aqueous solution to have an extremely low expected GWP and it can replace, in terms of performance. NF3 which is currently used as the cleaning gas. F3NO is very high in F content that decides the etching and cleaning performance, and is easily decomposed in an acid and an alkali aqueous solution and thus is estimated to have the expected global warming potential close to zero unlike indecomposable PFC. HFC, NF3, and SF6, and it is anticipated that the energy and environmental load in a decomposition treatment of the unreacted residual F3NO would be small. It is also non-toxic when it is leaked, and exhibits physical properties similar to NF3 at room temperature, and thus is highly promising as an alternative gas. Little is known for a method for producing trifluoroamine oxide (F3NO), which is an alternative gas material. Patent Literature 1 (US Patent Application Publication No. 2003/0143846 A1) discloses a gas composition containing F3NO for etching a film of a silicon-containing compound and for cleaning the inside of a reactor, and discloses a method for synthesizing F3NO wherein a NF2OSb2F11 salt is synthesized by reacting NF3 and N2O at a temperature of 150° C. under a SbF5 activator and then the salt is pyrolyzed at a high temperature (>200° C.) to obtain F3NO.