Trifluoroamine oxide manufacturing apparatus and manufacturing method

Abstract

The trifluoroamine oxide manufacturing apparatus of the present invention is a process for producing FNO and F in the gas phase. 2 the ultraviolet ray irradiating means for irradiating the reactor with ultraviolet ray having a peak wavelength in a wavelength band of 300 nm to 400 nm; and a separation and collection means for separating and collecting the trifluoroamine oxide produced from the reaction products, the ultraviolet ray having an intensity in a wavelength band of less than 300 nm being less than 5% of the intensity of the light in a wavelength band of 300 nm to 400 nm.

Description

[Technical field]

[0001] The present invention relates to a method for producing trifluoroamine oxide (F3NO). [Background technology]

[0002] Chemical vapor deposition (CVD) process technology is widely known as a thin film manufacturing process for manufacturing semiconductor devices or display devices. When forming a thin film for a semiconductor device or display device in a CVD chamber, it is preferable that the thin film is formed only on the target in the CVD chamber, but the thin film forming material is also deposited on other exposed surfaces in the CVD chamber. For example, the thin film forming material is deposited on the wall surface of the CVD chamber. In addition, during the CVD process, the material deposited on the target may peel off and contaminate the surface of the thin film deposited on the target or the surface of the target on which the thin film is formed. Such contamination causes defects in the semiconductor device or display device and reduces the yield. Therefore, a cleaning process is performed at appropriate intervals to remove unnecessary deposits deposited in the CVD chamber. The cleaning process in the CVD chamber is performed manually or using a cleaning gas.

[0003] Conventional perfluorinated gases such as CF4, C2F6, SF6, and NF3 have been used as chamber cleaning gases or etching gases for deposited thin films in the manufacturing process of semiconductors or electronic devices.

[0004] However, such perfluorinated substances are stable substances and remain in the atmosphere for a very long time. In addition, waste gas after use contains a high concentration of undecomposed perfluorinated substances, so it is very costly to treat such waste gas to below the permissible standard value and release it into the atmosphere. Furthermore, such common perfluorinated substances are known to have very high Global Warming Potential (GWP) values ​​(ITH100 years, CO2 standard CF46,630, SF623,500, NF316,100), which imposes a considerable burden on the environment. Therefore, there is a high demand for alternative gases with low GWP values ​​that can be used in cleaning or etching processes.

[0005] In particular, nitrogen trifluoride (NF3) gas is not only used in large quantities worldwide, but also has a very high global warming potential. Therefore, in order to reduce the burden on the environment and ensure the sustainable development of the semiconductor industry, there is a need to reduce the use of NF3 gas and develop alternative materials. Among these candidate alternative gases, trifluoroamine oxide (F3NO) has an extremely low predicted GWP and is a substance that can replace NF3, which is currently used as a cleaning gas, in terms of performance. F3NO has a very high "F" content, which determines etching and cleaning performance, and unlike the persistent PFCs, HFCs, NF3, and SF6, it is predicted to have a low global warming potential, require less energy and have less environmental impact when treating unreacted remaining F3NO, and is non-irritating even if it leaks.

[0006] Methods for producing trifluoroamine oxide (F3NO), a candidate alternative gas, are extremely limited.

[0007] Patent Document 1 (US Patent Publication 2003 / 0143846A1) relates to a technology related to a gas composition for cleaning the inside of a reactor and etching a film of a silicon-containing compound, and discloses a gas composition containing F3NO. As for a method for synthesizing F3NO, it discloses a method of reacting NF3 and N2O at a temperature of 150°C under the presence of SbF5 catalyst to obtain NF2OSb2F 11They have disclosed a method in which the salt is synthesized and then thermally decomposed at high temperatures (>200°C) to obtain F3NO. However, the yield based on the raw materials NF3 and N2O is low at around 20%, and the purity of the final product is low.

[0008] The applicant of the present application has proposed a new method for producing trifluoroamine oxide in high yield and purity in Patent Document 2 (Korean Patent Registration No. 10-2010460B1) and Patent Document 3 (Korean Patent Registration No. 10-2010466B1), respectively, using the same SbF5 / NF3 / N2O reaction system as Patent Document 1. For example, according to the method disclosed in Patent Document 2, NF3 and N2O are reacted in the presence of SbF5 to obtain an intermediate product, NF2OSbF6, which is then contacted with NaF and subjected to a thermal decomposition reaction in a vacuum atmosphere to synthesize trifluoroamine oxide (F3NO) through a two-step reaction. According to the method disclosed in Patent Document 3, NF3 and N2O are reacted in the presence of SbF5 to obtain an intermediate product NF2OSbF6, and the reaction gas containing nitrogen (N2) produced in this reaction is removed, and nitrogen trifluoride and nitrous oxide are added to produce the intermediate product, which is then reacted with NaF to synthesize trifluoroamine oxide (F3NO) through a two-step reaction. [Prior art documents] [Patent documents]

[0009] [Patent Document 1] US Patent Publication 2003 / 0143846 A1 [Patent Document 2] Korean Patent 10-2010460 B1 [Patent Document 3] Korean Patent 10-2010466 B1 Summary of the Invention [Problem to be solved by the invention]

[0010] However, according to the synthesis methods of trifluoroamine oxide disclosed in the above-mentioned Patent Documents 2 and 3, the intermediate product must be heated to a temperature of about 150°C to 200°C under a vacuum atmosphere for the second step of reacting with NaF. As a result, not only must an expensive reactor capable of a vacuum process be used, but also a heating process is required for thermal decomposition, which increases the production cost of trifluoroamine oxide. In addition, the thermal decomposition reaction proceeds slowly, takes a considerable amount of time, and is a solid-phase reaction and not a continuous reaction, so the productivity is not high. In addition, there is a problem of stability of the production equipment due to clogging of pipes.

[0011] Therefore, one problem to be solved by the present invention is to provide a method for producing trifluoroamine oxide, which can suppress an increase in production cost, has high productivity, can reduce the impact on production equipment, and can improve the yield. [Means for solving the problem]

[0012] In order to solve such problems, an apparatus for producing trifluoroamine oxide according to one embodiment of the present invention includes a reactor in which a photochemical reaction is carried out to produce trifluoroamine oxide using gaseous FNO and F2 as starting materials, an ultraviolet ray irradiation means for irradiating the reactor with ultraviolet rays having a peak wavelength in a wavelength band of 300 nm to 400 nm, and a separation and collection means connected to the reactor in a gaseous phase for separating and collecting trifluoroamine oxide produced from the reaction products produced in the reactor, the ultraviolet ray being characterized in that the light intensity in a wavelength band of less than 300 nm is less than 5% of the light intensity in a wavelength band of 300 nm to 400 nm.

[0013] A method for producing trifluoroamine oxide according to another embodiment of the present invention includes the steps of: supplying gaseous FNO and F2 into a reactor; irradiating the reactor with ultraviolet light having a peak wavelength in a wavelength band of 300 nm to 400 nm; discharging a product from the reactor; and separating and collecting F3NO from the discharged product, wherein the ultraviolet light has a light intensity in a wavelength band of less than 300 nm that is less than 5% of the light intensity in a wavelength band of 300 nm to 400 nm. Effect of the Invention

[0014] According to the present invention, it is possible to suppress an increase in the production cost of trifluoroamine oxide, to increase the productivity, and to reduce the influence of pipe clogging and the like on the production equipment. In particular, according to the production method of the present invention, it is possible to improve the yield of trifluoroamine oxide. [Brief description of the drawings]

[0015] [Figure 1] FIG. 1 is a schematic diagram showing an apparatus for producing trifluoroamine oxide according to an embodiment of the present invention. [Diagram 2] 4 is a graph showing the emission spectrum of an ultraviolet light source of a manufacturing apparatus according to an embodiment of the present invention and the spectrum of irradiated ultraviolet light filtered by a bandpass filter. [Diagram 3] 13 is an emission spectrum of an ultraviolet LED as an ultraviolet irradiation means of a manufacturing apparatus according to another embodiment of the present invention. [Figure 4] 1 is a flowchart showing a method for producing trifluoroamine oxide according to an embodiment of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0016] Hereinafter, preferred embodiments and examples of the present invention will be described with reference to the drawings. However, the following embodiments and examples merely exemplify preferred configurations of the present invention, and the scope of the present invention is not limited to these configurations. In the following description, the hardware and software configurations of the device, the process flow, manufacturing conditions, size, material, shape, etc. are not intended to limit the scope of the present invention unless otherwise specified.

[0017] According to the method for producing trifluoroamine oxide of the present invention, gaseous FNO and F2 are used as starting materials, and a mixture of these starting materials is irradiated with ultraviolet light having a peak wavelength in the wavelength range of 300-400 nm and substantially no wavelength component below 300 nm to produce trifluoroamine oxide by photochemical fluorination. That is, the method for producing trifluoroamine oxide of the present invention is carried out according to the following reaction formula.

[0018] [ka]

[0019] This method does not require a vacuum reactor or additional heating for the reaction, which reduces production costs. In addition, the reaction rate is fast, which improves productivity. Since it is a gas-phase reaction, it is possible to reduce the deterioration of the stability of the production equipment, such as pipe clogging.

[0020] In particular, in the method for producing trifluoroamine oxide of the present invention, the ultraviolet light irradiated to the mixture of starting materials does not substantially contain wavelength components less than 300 nm, so that side reactions other than the product F3NO can be suppressed and the yield of F3NO can be improved.

[0021] The trifluoroamine oxide production apparatus and the production method using the same of the present invention will be specifically described with reference to the following drawings.

[0022] FIG. 1 is a schematic diagram showing an apparatus for producing trifluoroamine oxide according to one embodiment of the present invention. An apparatus 1 for producing trifluoroamine oxide according to one embodiment of the present invention includes a reactor 10, an ultraviolet ray irradiation means 20, and a means 30 for separating and collecting trifluoroamine oxide.

[0023] As shown in FIG. 1, the reactor 10 has an elongated tubular shape with both ends closed, and includes, for example, a cylindrical body portion and end plates 11, 12 provided at both ends of the body portion.

[0024] Reactor 10 is preferably constructed of materials that are resistant to corrosion by starting materials such as FNO and F2, and products such as F3NO. For example, reactor 10 is preferably constructed of Monel, nickel, stainless steel, or Teflon.

[0025] The reactor 10 is provided with one or more windows transparent to ultraviolet light. For example, at least one of the end plates 11, 12 provided at both ends of the longitudinal direction of the body of the reactor 10 is made of a material transparent to ultraviolet light so as to allow ultraviolet light of a predetermined wavelength band irradiated from the ultraviolet light irradiation means 20 to enter the reaction space in the reactor 10. Specifically, of the end plates 11, 12 at both ends of the reactor 10, the end plate 11 close to the inlet for the starting material is made of a material transparent to ultraviolet light, such as barium fluoride or calcium fluoride.

[0026] However, the present invention is not limited to such a configuration, and both end plates 11, 12 may be made of a material transparent to ultraviolet light, and one or more transparent windows may be further provided on the longitudinal cylindrical surface of the reactor 10.

[0027] An inlet and inlet valve 13 for introducing starting materials such as FNO and F2 or a purge gas (He) is provided on the longitudinal cylindrical surface of the reactor 10 at a position adjacent to the ultraviolet irradiation means 20, and an outlet and outlet valve 14 for discharging the product is provided at the opposite end.

[0028] The ultraviolet ray irradiation means 20 irradiates the inside of the reactor 10 with ultraviolet rays of a predetermined wavelength band so that the starting materials FNO and F2 react with each other to produce F3NO.

[0029] The ultraviolet light irradiated by the ultraviolet light irradiation means 20 does not substantially have components in a wavelength band less than 300 nm, and has a peak wavelength in a wavelength band of 300 nm to 400 nm. For example, the ultraviolet light irradiated by the ultraviolet light irradiation means 20 has a light intensity in a wavelength band less than 300 nm that is less than 5% of the light intensity in the wavelength band of 300 nm to 400 nm.

[0030] In this way, the ultraviolet light irradiated by the ultraviolet light irradiation means 20 does not contain high-energy components (deep ultraviolet light) in the wavelength band less than 300 nm, so that side reactions can be suppressed by the high-energy components in these wavelength bands, and a decrease in the yield of F3NO can be suppressed.

[0031] For this purpose, the ultraviolet irradiation means 20 of the trifluoroamine oxide manufacturing apparatus 1 according to one embodiment of the present invention includes an ultraviolet light source (not shown) and a filter (not shown) that blocks at least deep ultraviolet components of less than 300 nm from the ultraviolet light emitted from the ultraviolet light source, or a bandpass filter (not shown) that passes only components in the 300 nm to 400 nm wavelength band.

[0032] Examples of ultraviolet light sources include metal halide lamps (Fe, Tl, Sn, Zn, Hg, etc. are metals that have luminous properties in the ultraviolet wavelength range) with a peak wavelength in the ultraviolet wavelength range, xenon lamps, mercury xenon lamps, halogen lamps, etc. As shown in (a) of FIG. 2, such ultraviolet light sources have a peak wavelength in the wavelength range of 300 nm to 400 nm, but also have components in the deep ultraviolet wavelength range below 300 nm and visible light / infrared light components over 400 nm.

[0033] Here, as described above, components in the deep ultraviolet wavelength band less than 300 nm cause side reactions when F3NO is produced in the reactor 10, reducing the yield of F3NO, and visible light / infrared light components over 400 nm increase the temperature of the ultraviolet irradiation means 20, reducing the function of the bandpass filter.

[0034] Therefore, in one embodiment of the present invention, the bandpass filter includes a deep ultraviolet blocking filter (first filter) for blocking deep ultraviolet components less than 300 nm, and a visible light / infrared light blocking filter (second filter) for blocking visible light / infrared light over 400 nm. For example, the deep ultraviolet blocking filter can be composed of an oxide optical filter that can scatter or reflect components in the deep ultraviolet wavelength range, such as TiO2, and the visible light / infrared light blocking filter can be composed of an optical filter that can reflect or absorb wavelength components over 400 nm, such as SiO2 and ZrO2 or CeO2. However, the present invention is not limited to this, and optical filters made of other materials may be used as long as they can block deep ultraviolet and visible light / infrared light. For example, an optical filter including a thin film of silver (Ag) may be used.

[0035] Here, the deep ultraviolet blocking filter has a TiO2 film thickness that makes the transmittance of ultraviolet light in the wavelength range of less than 300 nm less than 5% of the transmittance of ultraviolet light in the wavelength range of 300 nm to 400 nm.

[0036] Such ultraviolet light that has passed through the bandpass filter according to one embodiment of the present invention substantially contains ultraviolet light components in the wavelength band of 300 nm to 400 nm, as shown in FIG. 2(b).

[0037] More preferably, the ultraviolet light irradiated by the ultraviolet light irradiation means 20 has a peak wavelength in the wavelength band of 350 nm to 370 nm, and the light intensity in the wavelength band less than 300 nm is less than 1% of the light intensity in the wavelength band of 300 nm to 400 nm. For this reason, the bandpass filter of the ultraviolet light irradiation means 20 has a configuration in which the transmittance of ultraviolet light in the wavelength band less than 300 nm is less than 1% of the transmittance of ultraviolet light in the wavelength range of 300 nm to 400 nm.

[0038] Most preferably, the ultraviolet light irradiated by the ultraviolet light irradiation means 20 is a single wavelength of 365 nm (so-called i-line). For this purpose, the ultraviolet light irradiation means 20 according to one embodiment of the present invention includes an ultraviolet light source (not shown) and a single wavelength pass filter (not shown). Here, the single wavelength pass filter is a narrow band pass filter including Ta2O3 and SiO2, and substantially passes only the 365 nm ultraviolet light component (i-line).

[0039] In this embodiment, the ultraviolet irradiation means 20 is described as using an ultraviolet light source such as a metal halide lamp, but the present invention is not limited to this, and a UV-LED having a peak wavelength in the wavelength band of 300 nm to 400 nm, more preferably in the wavelength band of 350 to 370 nm, may be used.

[0040] For example, the ultraviolet ray irradiation means 20 of the manufacturing apparatus 1 according to another embodiment of the present invention can use a UV-LED having an emission spectrum as shown in FIG.

[0041] Since UV-LEDs with such emission characteristics have a peak wavelength in the wavelength band of 350-370 nm, they can effectively suppress side reactions in the reaction results and further improve the yield of F3NO, compared to when they have a peak wavelength in a shorter wavelength band (e.g., 300-350 nm). In addition, LEDs have the advantage of being energy-saving and long-lasting, since the time it takes for the light output to stabilize after current is passed through the board circuit that controls the light emission is short and there is no need to emit light constantly like ultraviolet lamps. In addition, since the emission spectrum is concentrated in a narrow wavelength band compared to ultraviolet lamps, the structure of the bandpass filter can be simplified or the bandpass filter can be omitted, and the decrease in the illuminance of the ultraviolet light that passes through the bandpass filter can be suppressed, thereby reducing the ultraviolet light irradiation time and improving productivity.

[0042] An excimer laser may be used as another example of the ultraviolet irradiating means 20. For example, an XeCl excimer laser (wavelength 308 nm), an XeF excimer laser (wavelength 351 nm), or the like may be used as a laser that emits a single-wavelength laser in the wavelength band of 300 nm to 400 nm.

[0043] In FIG. 1, the ultraviolet ray irradiation means 20 is shown to be disposed near the end plate 11 installed at one end in the longitudinal direction of the reactor 10, but the present invention is not limited to this.

[0044] For example, in another embodiment of the trifluoroamine oxide manufacturing apparatus 1 of the present invention, an end plate (11, first end plate) installed at one end of the longitudinal direction of the reactor 10 and an end plate (12, second end plate) arranged at the other end are all formed of a material that is transparent to ultraviolet rays, and the ultraviolet irradiation means 20 may include a first ultraviolet irradiation means that irradiates ultraviolet rays through the end plate 11 and a second ultraviolet irradiation means that irradiates ultraviolet rays through the end plate 12.

[0045] With this configuration, ultraviolet light can be sufficiently irradiated into the reaction space through both end plates 11 and 12 of the reactor 10, and the product yield can be further improved.

[0046] The trifluoroamine oxide manufacturing apparatus 1 according to one embodiment of the present invention includes a cold trap as a trifluoroamine oxide separation and collection means 30 for separating and collecting trifluoroamine oxide from the product discharged in a gaseous state to the outside of the reactor 10.

[0047] The gaseous product discharged from the reactor 10 may contain unreacted FNO, F2, etc. in addition to trifluoroamine oxide. The boiling point of trifluoroamine oxide is -89°C, which is between the boiling point of FNO (-56°C) and the boiling point of F2 (-188°C), so it is preferable that the cold trap as the trifluoroamine oxide separation and collection means 30 is composed of at least two stages. That is, the first cold trap can first condense and separate FNO from the gaseous product discharged through the discharge valve 14 of the reactor 10, and the second cold trap can condense and separate trifluoroamine oxide from the gaseous stream discharged from the first cold trap. F2 contained in the gaseous stream discharged from the second cold trap can be removed by a scrubber. However, the present invention is not limited to this, and other means capable of separating and collecting trifluoroamine oxide discharged in a gaseous state may be used.

[0048] Although not shown in Fig. 1, the trifluoroamine oxide manufacturing apparatus 1 according to an embodiment of the present invention may further include an ultraviolet ray irradiation means 20 and a temperature control means (not shown) for controlling the temperature of the reactor 10 at an appropriate temperature. For example, a blower or a chiller may be used as the temperature control means. When controlling the temperature of the reactor 10 by a chiller coolant, it is preferable to provide a chiller coolant pipe on the cylindrical surface of the reactor 10 in the longitudinal direction.

[0049] Hereinafter, each step of the method for preparing trifluoroamine oxide according to an embodiment of the present invention will be described in detail with reference to Fig. 4. The method for preparing trifluoroamine oxide according to an embodiment of the present invention will be described on the assumption that it is a batch type, but the present invention is not limited thereto, and it may be performed in a continuous type or a combination of the two.

[0050] First, an inert gas (e.g., helium) is supplied into the reactor 10 to purge the reaction space in the reactor 10 (S10). This allows the gas-phase products remaining in the reactor 10 from the previous batch process to be completely removed from the reactor 10.

[0051] Next, gaseous F2 and FNO are supplied as starting materials into the reactor 10 (S20). At this time, not only the inlet valve 13 but also the outlet valve 14 are opened so that the reaction region in the reactor 10 is flushed with the mixture of starting materials, and when the flushing is completed, the inlet valve 13 and the outlet valve 14 are closed so that the reaction region in the reactor 10 is filled with the mixture of starting materials.

[0052] In the starting material supply step, F2 and FNO as starting materials are supplied in a ratio of 0.5 to 2.5 moles of F2 per mole of FNO, more preferably in a molar ratio of 0.5 to 1.2:1 between F2 and FNO, and even more preferably in a molar ratio of 1:1 between F2 and FNO.

[0053] In this embodiment, it has been described that the starting materials F2 and FNO (or a mixture thereof) are simultaneously supplied through the inlet valve 13 and flushed, but the present invention is not limited thereto, and any one of the starting materials may be supplied first to flush the reaction zone in the reactor 10, and then the other starting material may be supplied to fill the reaction zone in the reactor 10 with the two starting materials. For example, F2 may be supplied first into the reactor 10 to flush the reaction zone, and then FNO may be supplied into the reactor 10.

[0054] When the supply of the starting materials is completed, ultraviolet light of a predetermined wavelength band is irradiated by the ultraviolet light irradiation means 20 through a transparent window installed on the end plate 11 of the reactor 10 (S30). The ultraviolet light irradiated in the ultraviolet light irradiation step (S30) has a peak wavelength in the wavelength band of 300 nm to 400 nm, as described above, and does not substantially contain ultraviolet light components in a wavelength band less than 300 nm. For example, as shown in FIG. 2(b) or FIG. 3, the ultraviolet light irradiated in the ultraviolet light irradiation step (S30) has a peak wavelength at 365 nm, and the intensity of the ultraviolet light in the wavelength band less than 300 nm is 5% or less of the intensity of the ultraviolet light in the wavelength band of 300 nm to 400 nm, more preferably 1% or less of the intensity of the ultraviolet light in the wavelength band of 300 nm to 400 nm. Most preferably, the ultraviolet light is a single wavelength having a wavelength of 365 nm and does not contain ultraviolet light components in a wavelength band less than 300 nm.

[0055] The ultraviolet irradiation step (S30) is preferably performed for 2 to 6 hours so that the starting materials in the reactor 10 can react sufficiently to generate F3NO. If it is less than 2 hours, a sufficient amount of F3NO may not be generated in the mass-production reactor 10, and if it is longer than 6 hours, it may become uneconomical because the rate of F3NO generation decreases as the ultraviolet irradiation time increases. In this embodiment, the starting materials filled in the reactor 10 at a molar ratio of 1:1 were irradiated with 365 nm single wavelength ultraviolet light for 3 hours, and a yield of 80% based on the reaction pressure was achieved.

[0056] More preferably, in an initial batch process, data on the production amount (or yield) according to the ultraviolet irradiation time is obtained, and the optimal ultraviolet irradiation time is determined taking into consideration the balance between the F3NO production amount (or yield) and productivity, and in subsequent batch processes, ultraviolet irradiation can be carried out for the determined ultraviolet irradiation time.

[0057] However, since the illuminance of the ultraviolet light emitted by the ultraviolet light irradiation means 20 may decrease over time, and the transmittance of the transparent window of the reactor 10 may decrease due to continuous exposure to ultraviolet light, it is preferable to adjust the ultraviolet light irradiation time according to the accumulated usage time of the ultraviolet light irradiation means 20. For example, it is preferable to obtain data on the relationship between the ultraviolet light irradiation time and the amount of F3NO produced (yield) every predetermined number of batch processes, and adjust the ultraviolet light irradiation time of the subsequent batch processes.

[0058] In order to more accurately control the UV irradiation time or the degree of reaction progress in the reactor 10, the amount of F3NO generated in the reactor 10 can be measured in real time by infrared spectroscopy during the UV irradiation step (S30), and the UV irradiation time can be feedback-controlled in real time based on this.

[0059] During the ultraviolet irradiation step (S30), the temperature inside the reactor 10 is maintained at 15° C. to 75° C., more preferably 25° C. to 50° C. The temperature inside the reactor 10 may fluctuate due to the reaction heat of the synthesis reaction and heat transfer from the ultraviolet irradiation means 20 by ultraviolet irradiation, so it is preferable to maintain the temperature within the above-mentioned predetermined temperature range by a temperature control means such as a blower or chiller.

[0060] When the ultraviolet irradiation is completed, the discharge valve 14 is opened to discharge the reaction product mixture in the reactor 10 to the outside of the reactor 10 (S40). At this time, the reaction products in the reactor 10 may be discharged by a pressure difference, or the inlet valve 13 may be opened to blow in an inert gas (e.g., helium) to promote the discharge of the reaction products.

[0061] When a sufficient amount of the reaction product containing F3NO has been discharged, F3NO is separated and collected from the reaction product stream by a cold trap serving as trifluoroamine oxide separation and collection means 30 (S50). As described above, the reaction product stream may contain unreacted FNO and F2 in addition to F3NO, so FNO, which has a higher boiling point than F3NO, is first separated from the reaction product stream by a first cold trap, and then F3NO is separated and collected by a second cold trap. The separated and collected F3NO may be purified by fractional distillation as necessary.

[0062] Thus, when one batch process is completed, the process proceeds again to the purge step (S10) to carry out the next batch process.

[0063] As mentioned above, the above description is merely an embodiment and should not be construed as being limited thereto. The technical idea of ​​the present invention should be defined only by the invention described in the claims below, and all technical ideas within the scope equivalent thereto should be construed as being included in the scope of the present invention. Therefore, it is obvious to those skilled in the art that the above embodiment can be embodied in various forms. [Explanation of symbols]

[0064] 10. Reactor 20...Ultraviolet irradiation means 30...Separation and collection means

Claims

1. An apparatus for producing trifluoroamine oxide, comprising: Gas phase FNO and F ２ a reactor in which a photochemical reaction is carried out to produce trifluoroamine oxide using the above as a starting material; an ultraviolet ray irradiation means for irradiating the inside of the reactor with ultraviolet rays having a peak wavelength in a wavelength band of 300 nm to 400 nm; a separation and collection means connected to the reactor in a gas phase for separating and collecting trifluoroamine oxide produced from the reaction products produced in the reactor, The ultraviolet light has an intensity in a wavelength band of less than 300 nm that is less than 5% of an intensity of light in a wavelength band of 300 nm to 400 nm.

2. The ultraviolet light has a peak wavelength in a wavelength band of 350 nm to 370 nm, 2. The apparatus for producing trifluoroamine oxide according to claim 1, wherein the ultraviolet light has an intensity in a wavelength band of less than 300 nm that is less than 1% of the intensity of the ultraviolet light in a wavelength band of 300 nm to 400 nm.

3. 3. The apparatus for producing trifluoroamine oxide according to claim 2, wherein the ultraviolet light has a single wavelength of 365 nm.

4. The apparatus for producing trifluoroamine oxide according to claim 1, characterized in that the ultraviolet irradiation means includes an ultraviolet light source having an emission spectrum with a peak wavelength in the wavelength band of 300 nm to 400 nm, and a band-pass filter that passes the components of the light emitted from the ultraviolet light source in the wavelength band of 300 nm to 400 nm.

5. The apparatus for producing trifluoroamine oxide according to claim 4, characterized in that the bandpass filter includes a first filter that blocks a wavelength band less than 300 nm and a second filter that blocks a wavelength band greater than 400 nm.

6. 5. The apparatus for producing trifluoroamine oxide according to claim 4, wherein the bandpass filter is a single-wavelength filter that passes substantially only ultraviolet light of a single wavelength of 365 nm.

7. 5. The apparatus for producing trifluoroamine oxide according to claim 4, wherein the ultraviolet light source is a metal halide lamp, a mercury xenon lamp, a xenon lamp or a halogen lamp.

8. 2. The apparatus for producing trifluoroamine oxide according to claim 1, wherein the ultraviolet ray irradiation means is an ultraviolet ray (UV) LED.

9. 2. The apparatus for producing trifluoroamine oxide according to claim 1, wherein the ultraviolet ray irradiating means is an excimer laser which emits ultraviolet rays of a single wavelength.

10. 2. The apparatus for producing trifluoroamine oxide according to claim 1, wherein the separation and collection means is a cold trap.

11. 11. The apparatus for producing trifluoroamine oxide according to claim 10, wherein the cold trap comprises a first cold trap for collecting unreacted starting materials from the reaction product, and a second cold trap for collecting trifluoroamine oxide.

12. The reactor includes a cylindrical body and end plates disposed at both ends of the body in a longitudinal direction, At least one of the end plates is formed of a material transparent to ultraviolet light; 2. The apparatus for producing trifluoroamine oxide according to claim 1, wherein the ultraviolet ray irradiation means is arranged to irradiate ultraviolet rays through the at least one transparent end plate.

13. The end plates include a first end plate installed at one end of the body in the longitudinal direction and a second end plate arranged at the other end, The first end plate and the second end plate are both formed of a material transparent to ultraviolet light, The apparatus for producing trifluoroamine oxide according to claim 12, characterized in that the ultraviolet irradiation means includes a first ultraviolet irradiation means for irradiating ultraviolet light through the first end plate and a second ultraviolet irradiation means for irradiating ultraviolet light through the second end plate.

14. The reactor includes a cylindrical body and end plates disposed at both ends of the body in a longitudinal direction, 2. The apparatus for producing trifluoroamine oxide according to claim 1, wherein the body portion has a window made of a material transparent to ultraviolet light.

15. A method for producing trifluoroamine oxide, comprising the steps of: Gas phase FNO and F ２ into a reactor; Irradiating the reactor with ultraviolet light having a peak wavelength in a wavelength band of 300 nm to 400 nm; Discharging the product from the reactor; F from the discharged product ３ and separating and collecting the NOx. The ultraviolet light has an intensity of light in a wavelength band of less than 300 nm that is less than 5% of an intensity of light in a wavelength band of 300 nm to 400 nm.

16. The ultraviolet light has a peak wavelength in a wavelength band of 350 nm to 370 nm, The method for producing trifluoroamine oxide according to claim 15, wherein the ultraviolet light has an intensity of light in a wavelength band of less than 300 nm that is less than 1% of an intensity of light in a wavelength band of 300 nm to 400 nm.

17. The method for producing trifluoroamine oxide according to claim 16, characterized in that the ultraviolet light has a single wavelength of 365 nm.

18. 16. The method for producing trifluoroamine oxide according to claim 15, further comprising the step of purging the reactor with an inert gas before the supplying step.

19. In the step of supplying, the reaction zone in the reactor is filled with F ２ The method for producing trifluoroamine oxide according to claim 15, characterized in that flushing is performed with at least one of FNO and FNO.

20. In the step of irradiating ultraviolet light, the ultraviolet light irradiation time is set to F in the reactor. ３ The method for producing trifluoroamine oxide according to claim 15, characterized in that real-time feedback control is performed based on the amount of NO produced.

21. F in the reactor ３ The method for producing trifluoroamine oxide according to claim 20, characterized in that the amount of NO produced is measured by infrared spectroscopy.

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