JPS62237929A - Method and device for treating nitrogen trifluoride gas - Google Patents
Method and device for treating nitrogen trifluoride gasInfo
- Publication number
- JPS62237929A JPS62237929A JP61078863A JP7886386A JPS62237929A JP S62237929 A JPS62237929 A JP S62237929A JP 61078863 A JP61078863 A JP 61078863A JP 7886386 A JP7886386 A JP 7886386A JP S62237929 A JPS62237929 A JP S62237929A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- reaction
- temperature
- carbon
- nitrogen trifluoride
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000007789 gas Substances 0.000 title claims description 40
- QKCGXXHCELUCKW-UHFFFAOYSA-N n-[4-[4-(dinaphthalen-2-ylamino)phenyl]phenyl]-n-naphthalen-2-ylnaphthalen-2-amine Chemical compound C1=CC=CC2=CC(N(C=3C=CC(=CC=3)C=3C=CC(=CC=3)N(C=3C=C4C=CC=CC4=CC=3)C=3C=C4C=CC=CC4=CC=3)C3=CC4=CC=CC=C4C=C3)=CC=C21 QKCGXXHCELUCKW-UHFFFAOYSA-N 0.000 title claims description 11
- 238000000034 method Methods 0.000 title claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 25
- 239000011261 inert gas Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 3
- 231100000252 nontoxic Toxicity 0.000 claims description 3
- 230000003000 nontoxic effect Effects 0.000 claims description 3
- ZQXCQTAELHSNAT-UHFFFAOYSA-N 1-chloro-3-nitro-5-(trifluoromethyl)benzene Chemical compound [O-][N+](=O)C1=CC(Cl)=CC(C(F)(F)F)=C1 ZQXCQTAELHSNAT-UHFFFAOYSA-N 0.000 claims 1
- 229910001873 dinitrogen Inorganic materials 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- 238000001816 cooling Methods 0.000 abstract description 2
- 238000010926 purge Methods 0.000 abstract description 2
- 239000003610 charcoal Substances 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002341 toxic gas Substances 0.000 description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001312 dry etching Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012212 insulator Substances 0.000 description 2
- 238000003672 processing method Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 101000613598 Carica papaya Caricain Proteins 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- 229910000792 Monel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- GVGCUCJTUSOZKP-UHFFFAOYSA-N nitrogen trifluoride Chemical compound FN(F)F GVGCUCJTUSOZKP-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/30—Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]
Landscapes
- Treating Waste Gases (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は三フッ化窒素ガス（ＮＦ３）を含有する排ガス
等の処理方法および処理装置に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method and apparatus for treating exhaust gas and the like containing nitrogen trifluoride gas (NF3).
し従来の技術１
最近、ＬＳＩ素子は年々高集積化され、製造プロセスの
精密化と新技術の導入か進み、新しい半導体用ガスの利
用の重要性が強調されている。半導体用のドライエツチ
ングガス、おるいはクリーニングガスとして有望なひと
つの特別なガスはＮＦ３である。例えば、Ｎ「３放電中
でイオン化した反応性ガスがシリコンをエツチングする
と、反応生成物は揮発性物質となるので、従来のフロロ
カーボンプラズマ中でのエツチングに較べ、Ｃ或はＳに
よるウェハー表面の反応残渣汚染がない。Conventional Technology 1 Recently, LSI devices have become more highly integrated year by year, manufacturing processes have become more precise and new technologies have been introduced, and the importance of using new semiconductor gases has been emphasized. One particular gas that shows promise as a dry etching or cleaning gas for semiconductors is NF3. For example, when silicon is etched by an ionized reactive gas in a N3 discharge, the reaction product becomes a volatile substance, so the reaction of the wafer surface with C or S is more effective than etching in a conventional fluorocarbon plasma. No residue contamination.
又反応残渣かないためエツチング速度が速くなる。Furthermore, since there is no reaction residue, the etching speed becomes faster.
一般に上に挙げた利点が、ドライエツチングガスあるい
はクリーニングガスとして、ＮＦ３が有望視されている
理由である。Generally, the above-mentioned advantages are the reasons why NF3 is considered promising as a dry etching gas or cleaning gas.
［発明が解決しようとする問題点］
上記ＮＦ３は、常温では非常に安定で、不燃性のガスで
あるが、許容濃度１０ＰＰＩＩＩの毒性ガスであるため
、その毒性ガス対策が急がれていた。しかしながら、Ｎ
Ｆ３は水、アルカリ、酸水溶液と反応しないため、これ
らの水溶液では処理できす、大量の窒素、空気で稀釈排
出されているのが実情である。一方、稀釈排出されたＮ
Ｆ３は、自然界では分解されないことが証明されており
、生物に対する悪影響が懸念されている。[Problems to be Solved by the Invention] The above-mentioned NF3 is a very stable and nonflammable gas at room temperature, but it is a toxic gas with a permissible concentration of 10 PPIII, so countermeasures against the toxic gas have been urgently needed. However, N
Since F3 does not react with water, alkali, or acid aqueous solutions, it cannot be treated with these aqueous solutions, and the reality is that it is diluted with large amounts of nitrogen and air and then discharged. On the other hand, the diluted N
It has been proven that F3 does not decompose in nature, and there are concerns about its negative effects on living organisms.
本発明は、Ｎ「３排ガスの稀釈処理法の問題点を解決す
べくなされたもので、有ＲなＮＦ３を無害なＣＦ４とＮ
２ガスに変換して処理するものである。The present invention was made to solve the problems of the dilution treatment method for N3 exhaust gas, and the present invention was made to solve the problems of the dilution treatment method for N3 exhaust gas.
It is processed by converting it into two gases.
［問題点を解決するための手段］
上記問題点を解決するため本発明は次のような処理方法
と処理装置を提供する。[Means for Solving the Problems] In order to solve the above problems, the present invention provides the following processing method and processing apparatus.
すなわち、本発明にかかる三フッ化窒素ガス（ＮＦ３）
の処理方法は、三フッ化窒素ガスＮＦ３を含有する排ガ
スを活性炭、木炭等の炭素塊と反応温度３００〜６００
”Ｃで反応させ、毒性のないＣＦ４ガスとＮ２ガスに変
えることを特徴としている。That is, nitrogen trifluoride gas (NF3) according to the present invention
The treatment method is to react exhaust gas containing nitrogen trifluoride gas NF3 with carbon lumps such as activated carbon and charcoal at a temperature of 300 to 600 ml.
``It is characterized by reacting with C and converting it into non-toxic CF4 gas and N2 gas.
また、発明にかかる処理装置は、炭素塊が充填される反
応筒、該反応筒に三フッ化窒素ガスを導く流通用配管、
および前記反応筒に並列に設けられているバイパスをそ
なえ、前記反応筒の温度が設定値以上となったとき、ま
たは反応筒の圧力が設定値以上となったときは反応筒へ
供給される三フッ化窒素ガスをバイパスを通して放出す
るようにバルブを開閉操作する制御装置が設（プられて
いることを特徴としている。Further, the processing apparatus according to the invention includes a reaction tube filled with carbon lumps, a flow pipe for introducing nitrogen trifluoride gas into the reaction tube,
and a bypass provided in parallel with the reaction column, so that when the temperature of the reaction column exceeds a set value or the pressure of the reaction column exceeds a set value, three It is characterized by being equipped with a control device that opens and closes a valve so as to release nitrogen fluoride gas through a bypass.
［実施例１ 以下、実施例を挙げつつより詳細に説明する。[Example 1 Hereinafter, it will be explained in more detail by giving examples.
本発明においてＮＦ３を炭素塊と反応させると、次の反
応によりＮＦ３がＣＦ４とＮ２に変換される。In the present invention, when NF3 is reacted with a carbon mass, NF3 is converted into CF4 and N2 by the following reaction.
４ＮＦ３ ＋３Ｃ→ ３ＣＦ４＋２Ｎ２このときの反応
温度は３００〜６００°Ｃとするのが望ましい。この温
度が低すぎるとＮＦ３が炭素塊に吸着され、四フッ化炭
素ＣＦ４として脱着しなくなる。逆にこの温度が高すぎ
ると、対腐蝕性の反応筒を使用しても腐蝕が急激に進行
する。ざらに、高い温度での反応は急激に進行するため
、反応熱の制御が困難となる。4NF3 +3C→3CF4+2N2 The reaction temperature at this time is preferably 300 to 600°C. If this temperature is too low, NF3 will be adsorbed by the carbon mass and will not be desorbed as carbon tetrafluoride CF4. Conversely, if this temperature is too high, corrosion will rapidly proceed even if a corrosion-resistant reaction tube is used. Generally speaking, the reaction at high temperatures progresses rapidly, making it difficult to control the reaction heat.
ＮＦ３の濃度は、低濃度から１００％の濃度まで処理が
可能であるが、上記の反応は発熱反応であるので、高濃
度のＮＦ３を処理する場合は反応温度を制御するのが困
難となる。したがって、反応温度の制御の観点から、処
理すべきＮＦ３の濃度は１０〜３０％とするのが望まし
い。The concentration of NF3 can be treated from a low concentration to 100% concentration, but since the above reaction is an exothermic reaction, it is difficult to control the reaction temperature when treating a high concentration of NF3. Therefore, from the viewpoint of controlling the reaction temperature, it is desirable that the concentration of NF3 to be treated is 10 to 30%.
つぎに、反応筒への充填材である炭素塊について述べれ
ば、この炭素塊の粒度は４〜８メツシュとするのが好ま
しい。反応の面からは粒度が小さいほど表面積が大きく
なるので有利であるが、圧力損失が大きくなるのであま
り細いものは実用的ではない。また、粒度が４メツシュ
よりも人ぎくなると、表面積が小さくなり、所望の効果
が得られなくなる。Next, regarding the carbon mass which is a filler material for the reaction tube, it is preferable that the particle size of this carbon mass is 4 to 8 mesh. From the viewpoint of reaction, the smaller the particle size, the larger the surface area, which is advantageous, but the smaller the particle size, the greater the pressure loss, so it is not practical. Moreover, if the particle size becomes larger than 4 mesh, the surface area becomes small and the desired effect cannot be obtained.
炭素塊としては、例えば活性炭や木炭等が使用されるが
、この種の炭素塊には通常１５〜２０％の水分が含有さ
れており、このように水分を含有する炭素塊とＮＦ３と
を反応させると１−ＩＦが発生し、装置材料の腐蝕の原
因となる。したがって、反応筒に炭素塊を最初に充填し
たとぎは、予め炭素塊中の水分を加熱除去するのが好ま
しい。For example, activated carbon or charcoal is used as the carbon mass, but this type of carbon mass usually contains 15 to 20% moisture, and in this way, the carbon mass containing moisture is reacted with NF3. If this happens, 1-IF will occur, causing corrosion of the equipment material. Therefore, it is preferable to first heat and remove the moisture in the carbon mass before filling the reaction tube with the carbon mass.
水分除去のための加熱処理を例示すれば、例えば第１図
のような処理が実用的に好ましい。先ず反応筒内に不活
性ガス（Ｎ２、Ａｒ、またはト１ｅ）を２．１！／１ｌ
ｌｉｏの流量で流し、反応筒温度コントローラの温度を
２００°Ｃに設定する。２００°Ｃに昇温後約３０分間
この温度を保持するか、この間に大部分の水分が除去さ
れる。つきて反応筒の温度を４００°Ｃまで弄温し、約
６０分間この温度を保つ。As an example of heat treatment for removing moisture, the treatment shown in FIG. 1 is practically preferable. First, 2.1! /1l
The reaction tube temperature controller was set at 200°C. After raising the temperature to 200°C, this temperature is maintained for about 30 minutes, during which time most of the moisture is removed. Then, the temperature of the reaction tube was increased to 400°C and maintained at this temperature for about 60 minutes.
この保持により、炭素塊中の含有水分を完全に脱看させ
、ＮＦ３と炭素塊の反応時における１−ＩＦ生成を防ぐ
ことができる。一旦乾燥させた後は、Ｎ［３の処理を行
なわない時でも常時乾燥不活性ガス例えばＮ２ガス（通
常は露点−６９°Ｃ）を流しておくことにより乾燥状態
を保つことかできる。This retention makes it possible to completely remove the moisture contained in the carbon mass and prevent the generation of 1-IF during the reaction between NF3 and the carbon mass. Once dried, the dry state can be maintained by constantly flowing a dry inert gas such as N2 gas (usually with a dew point of -69°C) even when the N[3 treatment is not performed.
この場合、反応筒の温度は昇温したままでもよく、室温
で保持してもよい。なお、上記乾燥処理条件を例示すれ
ば、第１図の加熱時間中に流す乾燥用不活性ガス量は、
例えば炭素塊１．３Ｎｇにつき３６０、Ｑ以上とするの
が好ましく、当該不活性ガスの露点は一６８°Ｃ以下で
、０２濃度は’ ｐｐｍ以下とするのが好ましい。また
、乾燥圧力は大気圧で温度は４００°Ｃとするのが好ま
しい。In this case, the temperature of the reaction column may remain elevated or may be maintained at room temperature. In addition, to illustrate the above drying processing conditions, the amount of drying inert gas flowed during the heating time in Fig. 1 is as follows:
For example, it is preferable that the inert gas has a dew point of 360.Q or higher per 1.3 Ng of carbon mass, a dew point of the inert gas of 168° C. or lower, and a 02 concentration of 1 ppm or lower. Further, it is preferable that the drying pressure is atmospheric pressure and the temperature is 400°C.
つぎに、上記ＮＦ３ガス処理に用いられる処理装置につ
いて説明する。Next, a processing apparatus used for the above-mentioned NF3 gas processing will be explained.
第２図は本装置の構成をあられすもので、この処理装置
１は、装置本体２とコントロールボックス３をそなえて
いる。装置本体２は、切換使用される１対の反応筒４，
５をそなえ、各反応筒には１００Ｖの電熱ヒータ６．７
が設けられている。一方の反応筒４を使用する場合を例
にとって説明すると、処理されるべきＮＦ３は、入口１
０からバルブ１１、オイルセパレータ１２、三方切換弁
１３を経由して左側の反応筒４に供給され、該反応筒内
に充填されている炭素１鬼と反応してＣＦ４とＮ２とな
り、冷却コイル１４、バルブ１５．１６を通って排出さ
れる。一方、稀釈用Ｎ２ガスは、フローメータ１９から
供給され、Ｎ「３淵度か好ましい濃度すなわち１０〜３
０％になるようにＮＦ３を稀釈する。この定常運転時に
は、空気作動バイパス弁２０は閉じられている。FIG. 2 shows the configuration of this apparatus. This processing apparatus 1 includes an apparatus main body 2 and a control box 3. As shown in FIG. The apparatus main body 2 includes a pair of reaction tubes 4, which are used selectively.
5, and each reaction tube is equipped with a 100V electric heater 6.7
is provided. Taking as an example the case where one reaction tube 4 is used, the NF3 to be treated is at the inlet 1.
0 is supplied to the reaction cylinder 4 on the left side via the valve 11, oil separator 12, and three-way switching valve 13, and reacts with carbon 1 filled in the reaction cylinder to become CF4 and N2, which are then supplied to the cooling coil 14. , is discharged through valves 15.16. On the other hand, N2 gas for dilution is supplied from the flow meter 19, and N2 gas is supplied from the flow meter 19 at a preferable concentration of 10 to 3 degrees N2.
Dilute NF3 to 0%. During this steady operation, the air-operated bypass valve 20 is closed.
つぎに、温度が異常上昇した場合について説明する。処
理中に反応筒温度が設定値以上（こなると、反応筒人口
の空気作動弁２２が自動的に開となり、バイパス空気作
動弁２３が自動的に開となって、ＮＦ３含有ガスはバイ
パス回路２４を通って排出される。また、緊急用不活性
ガス供給バルブ２６か自動的に開き、反応筒４をパージ
しながら筒内温度を降温させる。Next, a case where the temperature rises abnormally will be explained. During processing, the temperature of the reaction cylinder exceeds the set value (when this happens, the air-operated valve 22 for the reaction cylinder is automatically opened, the bypass air-operated valve 23 is automatically opened, and the NF3-containing gas is transferred to the bypass circuit 24). In addition, the emergency inert gas supply valve 26 is automatically opened to purge the reaction tube 4 and lower the temperature inside the tube.
同様に、圧力異状上昇時の動作について説明すれば、装
置内の圧力が設定値以上になると、圧力スイッチ３０が
作動し、反応筒入口空気作動弁２２が自動的に閉となり
、メインバイパス空気作動弁２０が自動的に開となって
装置内の圧力を設定値１ス下に下げるようになっている
。Similarly, to explain the operation when the pressure abnormally increases, when the pressure inside the device exceeds the set value, the pressure switch 30 is activated, the reaction tube inlet air-operated valve 22 is automatically closed, and the main bypass air-operated valve is activated. Valve 20 is automatically opened to reduce the pressure within the device to 1 s below the set point.
つぎに、停電時の動作について説明すると、処理中に停
電したとぎは、反応筒入口の空気作動弁２２が自動的に
閉となると同時に、バイパス空気作動弁２０．２３が開
となり、停電による反応筒４の温度降下によるＮＦ３の
吸着を防ぐようになっている。ＮＦ３の吸着は、反応開
始時に大きな発熱を伴い温度制御が困難となるが、停電
時にその吸着が防止されるので、吸着によるこのような
事故が生じない。Next, to explain the operation during a power outage, if there is a power outage during processing, the air-operated valve 22 at the inlet of the reaction cylinder will automatically close, and at the same time the bypass air-operated valves 20 and 23 will open, and the reaction due to the power outage will be automatically closed. This is to prevent adsorption of NF3 due to temperature drop in the cylinder 4. Adsorption of NF3 generates a large amount of heat at the start of the reaction, making temperature control difficult; however, since adsorption is prevented during a power outage, such accidents due to adsorption do not occur.
なお、図中、３２は圧力計、３３はレギュレータ、３４
はストップ弁、３５はサンプルプラグ、３６はソレノイ
ドバルブ、３７はバルブヘッドおよびドレンプラグをあ
られす。In addition, in the figure, 32 is a pressure gauge, 33 is a regulator, and 34
35 is a stop valve, 35 is a sample plug, 36 is a solenoid valve, and 37 is a valve head and a drain plug.
なお運転に必要な反応筒、弁、計器、配管類は処理ボッ
クス内に機能的に納められている。この−〇 −
処理ボックスには排気ファンと空気吸込口および排気口
が設けられており、排気口は設置場所の排気ダクトに接
続されるようになっている。The reaction cylinders, valves, instruments, and piping necessary for operation are functionally housed inside the processing box. This -〇- processing box is equipped with an exhaust fan, an air suction port, and an exhaust port, and the exhaust port is connected to the exhaust duct at the installation location.
配管継手類等からＮＦ３ガスの漏洩が生じた場合は、排
気ファンによって処理ボックスの下部に設（プられてい
る空気吸込口から外部空気を吸込み、排気口から排出す
ることにより、処理ボックス外への漏洩が防止される。If NF3 gas leaks from piping joints, etc., it can be removed from the processing box by using an exhaust fan to suck in external air from the air intake port installed at the bottom of the processing box and exhaust it from the exhaust port. leakage is prevented.
また、この排気ファンの働きにより反応筒４，５の冷却
を効率的に行なわしめて、反応筒の温度制御を容易にし
ている。Furthermore, the exhaust fan works to efficiently cool the reaction tubes 4 and 5, making it easy to control the temperature of the reaction tubes.
反応筒はフッ素系ガスに対する耐蝕性の良好なモネル、
ニッケル等の材質で製作される。この反応筒は円筒形の
本体、ＮＦ３導入口、排出口、充填材（炭素塊）補給口
、充填材取出口、ヒーター、熱電対、保温剤、保温ケー
ス等をそなえ、充填材取出口と排出口には炭素微粉の漏
出を防止するフィルタとドレン扱ぎがそれぞれ８堪すら
れている。The reaction tube is made of Monel, which has good corrosion resistance against fluorine gases.
Manufactured from materials such as nickel. This reaction tube is equipped with a cylindrical main body, an NF3 inlet, an outlet, a filler (carbon lump) replenishment port, a filler outlet, a heater, a thermocouple, a heat insulator, a heat insulator case, etc., and a filler outlet and outlet. At the outlet, there are 8 filters and 8 drains each to prevent the leakage of carbon fines.
ＮＦ３排出口は冷五〇コイル１４に接続される。The NF3 outlet is connected to the cold 50 coil 14.
つぎに、本発明を実施してＮ「３ガス処理を行なった具
体例について説明する。Next, a specific example in which the present invention is implemented and N'3 gas treatment is performed will be described.
（具体的実施例１）
濃度１００％のＮＦ３を反応温度４００’ Ｃ１反応圧
力１気圧、流量５Ｖ１５〜１７０．Ｑ ／ｌｌｒで処理
した結果を第１表に示す。ここでＳＶ＝流量（、ｆｌ
／Ｄｒ）／充頃容積（、Ｑ）である。同表かられかる通
り、ＮＦ３は５ｐｐｍ以下（ガスクロマトグラフィー検
出限界）まで処理されている。(Specific Example 1) NF3 with a concentration of 100% was reacted at a reaction temperature of 400'C1, a reaction pressure of 1 atm, and a flow rate of 5V15-170. Table 1 shows the results of processing with Q/llr. Here, SV=flow rate (, fl
/Dr)/full volume (,Q). As can be seen from the table, NF3 was treated to 5 ppm or less (gas chromatography detection limit).
（具体的実施例２）
Ｎ［３をＮ２ガスで濃度３％まで稀釈して反応処理を行
なった結果を第２表に示す。本発明によればこのような
低濃度のものも完全に処理できることがわかる。(Specific Example 2) Table 2 shows the results of a reaction treatment performed by diluting N[3 with N2 gas to a concentration of 3%. It can be seen that according to the present invention, even such low concentrations can be completely treated.
（具体的実施例３）
ＮＦ３の濃度を４％とし、１％の塩素ガス（ＣＩ２＞と
１％の塩Ｍ （ＨＣＩ ）を加えたものを処理した結果
を第３表に示す。同表から、塩素系のガスが混入しても
反応が阻害されずに処理が行なわれることがわかる。(Specific Example 3) Table 3 shows the results of processing with 4% NF3 concentration and 1% chlorine gas (CI2) and 1% salt M (HCI). From the table It can be seen that even if chlorine-based gas is mixed in, the reaction is not inhibited and the treatment is carried out.
［発明の効果］
以上の説明から明らかなように、本発明によれば、常温
で非常に安定で毒性の高いＮ「３を毒性のないガスに変
換させることが可能となった。[Effects of the Invention] As is clear from the above explanation, according to the present invention, it has become possible to convert N'3, which is very stable and highly toxic at room temperature, into a non-toxic gas.
本発明の処理方法はＴ業的規模の処理に適したものであ
り、その装置は構造的に簡単で実用性の高いものである
。The processing method of the present invention is suitable for processing on a commercial scale, and the apparatus thereof is structurally simple and highly practical.
第１図は炭素塊の乾燥処理をあられすグラフ、第２図は
処理装置の１例をあられす構成説明図である。
１・・・処理装置 ２・・・装置本体３・・・コン
トロールボックス
４．５・・・反応筒FIG. 1 is a graph showing the drying process of carbon lumps, and FIG. 2 is a diagram illustrating the configuration of an example of the processing apparatus. 1... Processing device 2... Device body 3... Control box 4.5... Reaction tube
Claims (4)
性炭、木炭等の炭素塊と反応温度３００〜６００℃で反
応させ、毒性のないＣＦ＿４ガスとＮ＿２ガスに変える
ことを特徴とする三フッ化窒素ガスの処理方法。(1) Trifluoride, which is characterized by reacting exhaust gas containing nitrogen trifluoride gas NF_3 with carbon lumps such as activated carbon and charcoal at a reaction temperature of 300 to 600°C to convert it into non-toxic CF_4 gas and N_2 gas. How to treat nitrogen gas.
請求の範囲第１項記載の三フッ化窒素ガスの処理方法。(2) The method for treating nitrogen trifluoride gas according to claim 1, wherein the carbon mass is a granular material with a particle size of 4 to 8 mesh.
スを流通させることにより予め乾燥させられている特許
請求の範囲第１項または第２項記載の三フッ化窒素ガス
の処理方法。(3) The method for treating nitrogen trifluoride gas according to claim 1 or 2, wherein the carbon mass is dried in advance by flowing an inert gas such as N_2, Ar, or He gas.
窒素ガスを導く流通用配管、および前記反応筒に並列に
設けられているバイパスをそなえ、前記反応筒の温度が
設定値以上となつたとき、または反応筒の圧力が設定値
以上となつたときは反応筒へ供給される三フッ化窒素ガ
スをバイパスを通して放出するようにバルブを開閉操作
する制御装置が設けられていることを特徴とする三フッ
化窒素ガス処理装置。(4) A reaction tube filled with carbon lumps, a flow pipe for introducing nitrogen trifluoride gas into the reaction tube, and a bypass provided in parallel with the reaction tube, and the temperature of the reaction tube is set to a set value. A control device is provided that opens and closes a valve to release nitrogen trifluoride gas supplied to the reaction cylinder through a bypass when the pressure in the reaction cylinder exceeds a set value. A nitrogen trifluoride gas treatment device characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61078863A JPH0230731B2 (en) | 1986-04-05 | 1986-04-05 | SANFUTSUKACHITSUSOGASUNOSHORIHOHOOYOBISONOSOCHI |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61078863A JPH0230731B2 (en) | 1986-04-05 | 1986-04-05 | SANFUTSUKACHITSUSOGASUNOSHORIHOHOOYOBISONOSOCHI |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62237929A true JPS62237929A (en) | 1987-10-17 |
| JPH0230731B2 JPH0230731B2 (en) | 1990-07-09 |
Family
ID=13673663
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61078863A Expired - Lifetime JPH0230731B2 (en) | 1986-04-05 | 1986-04-05 | SANFUTSUKACHITSUSOGASUNOSHORIHOHOOYOBISONOSOCHI |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0230731B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5176889A (en) * | 1990-07-09 | 1993-01-05 | Daidousanso Co., Ltd. | Method and apparatus for treatment of NF3 gas |
| JPH05277341A (en) * | 1991-03-04 | 1993-10-26 | Iwatani Internatl Corp | Device for removing harmful gaseous nitrogen fluoride |
| US5401473A (en) * | 1990-07-09 | 1995-03-28 | Daidousanso Co., Ltd. | Method and apparatus for treatment of NF3 gas |
| US5728642A (en) * | 1994-02-03 | 1998-03-17 | Mitsui Toatsu Chemicals, Inc. | Exhaust gas treating agent and a method of treating exhaust gas using the agent |
| JP2022512245A (en) * | 2018-12-13 | 2022-02-02 | エドワーズ リミテッド | Harmment method and equipment |
-
1986
- 1986-04-05 JP JP61078863A patent/JPH0230731B2/en not_active Expired - Lifetime
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5176889A (en) * | 1990-07-09 | 1993-01-05 | Daidousanso Co., Ltd. | Method and apparatus for treatment of NF3 gas |
| US5401473A (en) * | 1990-07-09 | 1995-03-28 | Daidousanso Co., Ltd. | Method and apparatus for treatment of NF3 gas |
| JPH05277341A (en) * | 1991-03-04 | 1993-10-26 | Iwatani Internatl Corp | Device for removing harmful gaseous nitrogen fluoride |
| US5728642A (en) * | 1994-02-03 | 1998-03-17 | Mitsui Toatsu Chemicals, Inc. | Exhaust gas treating agent and a method of treating exhaust gas using the agent |
| JP2022512245A (en) * | 2018-12-13 | 2022-02-02 | エドワーズ リミテッド | Harmment method and equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0230731B2 (en) | 1990-07-09 |
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