JPH0242766B2 - - Google Patents
Info
- Publication number
- JPH0242766B2 JPH0242766B2 JP8879985A JP8879985A JPH0242766B2 JP H0242766 B2 JPH0242766 B2 JP H0242766B2 JP 8879985 A JP8879985 A JP 8879985A JP 8879985 A JP8879985 A JP 8879985A JP H0242766 B2 JPH0242766 B2 JP H0242766B2
- Authority
- JP
- Japan
- Prior art keywords
- activated carbon
- nitrogen trifluoride
- gas
- dinitrogen difluoride
- nitrogen
- 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.)
- Expired
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 45
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 30
- 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 claims description 25
- DUQAODNTUBJRGF-ONEGZZNKSA-N dinitrogen difluoride Chemical compound F\N=N\F DUQAODNTUBJRGF-ONEGZZNKSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 19
- 239000001272 nitrous oxide Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 4
- 238000000746 purification Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 description 19
- 239000007789 gas Substances 0.000 description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 239000012535 impurity Substances 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 235000013162 Cocos nucifera Nutrition 0.000 description 4
- 244000060011 Cocos nucifera Species 0.000 description 4
- 239000003463 adsorbent Substances 0.000 description 4
- 238000001312 dry etching Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- GVGCUCJTUSOZKP-UHFFFAOYSA-N nitrogen trifluoride Chemical compound FN(F)F GVGCUCJTUSOZKP-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 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 description 1
- 208000005156 Dehydration Diseases 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- ULFHSQLFQYTZLS-UHFFFAOYSA-N difluoroamine Chemical compound FNF ULFHSQLFQYTZLS-UHFFFAOYSA-N 0.000 description 1
- DUQAODNTUBJRGF-UHFFFAOYSA-N difluorodiazene Chemical compound FN=NF DUQAODNTUBJRGF-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying 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
- 238000010438 heat treatment Methods 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910017051 nitrogen difluoride Inorganic materials 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011301 petroleum pitch Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/083—Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms
- C01B21/0832—Binary compounds of nitrogen with halogens
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Description
【発明の詳細な説明】
産業上の利用分野
本発明は、超LSI用ドライエツチングガス等の
用途に適する高純度三弗化窒素の製造方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a method for producing high purity nitrogen trifluoride suitable for uses such as dry etching gas for VLSI.
さらに詳しくは、二弗化二窒素（N2F2）或は
二弗化二窒素と亜酸化窒素（N2O）を含む三弗
化二窒素（NF3）を、活性炭と接触させることに
より、二弗化二窒素或は二弗化二窒素と亜酸化窒
素を一工程で除去し、三弗化窒素を精製する方法
に関する。 More specifically, by contacting dinitrogen difluoride (N 2 F 2 ) or dinitrogen trifluoride (NF 3 ) containing dinitrogen difluoride and nitrous oxide (N 2 O) with activated carbon. , relates to a method for purifying nitrogen trifluoride by removing dinitrogen difluoride or dinitrogen difluoride and nitrous oxide in one step.
従来の技術と問題点
三弗化窒素は、化学レーザーのフツ素源とし
て、或はCVD装置のクリーニングガスとして用
いられ、中でも近年、超LSI用ドライエツチング
ガスとして、フロロカーボン系エツチング剤に比
べシリコン基板上の堆積物を抑え、しかもエツチ
ング速度、選択性が優れている等の理由で注目さ
れている有用なガスである。ドライエツチングガ
スとして使用される場合、特に高純度の三弗化窒
素が必要とされる。Conventional technology and problems Nitrogen trifluoride is used as a fluorine source for chemical lasers or as a cleaning gas for CVD equipment.In recent years, nitrogen trifluoride has been used as a dry etching gas for VLSI, and has been used as a dry etching gas for silicon substrates compared to fluorocarbon-based etching agents. It is a useful gas that is attracting attention because it suppresses deposits on the surface and has excellent etching speed and selectivity. Particularly high purity nitrogen trifluoride is required when used as a dry etching gas.
三弗化窒素の製造方法により、含有される不純
物の種類および組成は幾分異なるが、主として二
弗化二窒素及び亜酸化窒素が含まれるのが一般で
ある。 The types and composition of impurities contained in nitrogen trifluoride vary depending on the manufacturing method, but generally dinitrogen difluoride and nitrous oxide are mainly contained.
従来、三弗化窒素の精製方法として、
(1) 液体窒素温度で粗三弗化窒素ガスを液化した
後分留する方法
（NF3B.P.−129℃、N2F2B.P.−106〜111
℃、N2OB.P.−89℃）
(2) ゼオライト系吸着剤による吸着法
がとられていた。 Conventionally, methods for purifying nitrogen trifluoride include (1) a method in which crude nitrogen trifluoride gas is liquefied at liquid nitrogen temperature and then fractionated (NF 3 BP−129°C, N 2 F 2 BP−106 to 111
℃, N 2 OB.P.−89℃) (2) An adsorption method using a zeolite adsorbent was used.
ところで、(1)の方法では、比較的複雑な装置と
なり、煩雑な低温操作を要すること、
また、(2)の方法では、ゼオライト系吸着剤の性
能が不充分であり、吸着剤の寿命を伸ばすため、
前工程であらかじめ二弗化二窒素を非常に低濃度
にまで下げる必要がある（特開昭54−161588）等
の欠点を有していた。 By the way, method (1) requires a relatively complicated device and complicated low-temperature operation, and method (2) has insufficient performance of the zeolite adsorbent, which may shorten the life of the adsorbent. In order to stretch
This method had drawbacks such as the need to reduce the concentration of dinitrogen difluoride to a very low level in advance (Japanese Patent Application Laid-Open No. 161588/1983).
発明が解決しようとする問題点
本発明は、上記の事情を考慮し、二弗化二窒素
或は二弗化二窒素と亜酸化窒素を含む三弗化窒素
から、煩雑な操作を必要とせず、長時間連続的に
二弗化二窒素或は二弗化二窒素と亜酸化窒素を一
工程で除去するという特徴を有する三弗化窒素の
精製方法の提供を目的としている。Problems to be Solved by the Invention In consideration of the above circumstances, the present invention has been developed to produce nitrogen difluoride or nitrogen trifluoride containing dinitrogen difluoride and nitrous oxide without the need for complicated operations. The object of the present invention is to provide a method for purifying nitrogen trifluoride, which is characterized by continuously removing dinitrogen difluoride or dinitrogen difluoride and nitrous oxide in one step.
問題点を解決するための手段
上記目的を達成するため、検討を重ねた結果、
本発明者らは、三弗化窒素中に主な不純物として
含まれる二弗化二窒素或は二弗化二窒素と亜酸化
窒素の除去に、活性炭が特異的に優れていること
を見出した。Means to solve the problem In order to achieve the above purpose, as a result of repeated consideration,
The present inventors have discovered that activated carbon is uniquely superior in removing dinitrogen difluoride or dinitrogen difluoride and nitrous oxide contained as main impurities in nitrogen trifluoride. .
すなわち、本発明の要旨は、二弗化二窒素或は
二弗化二窒素と亜酸化窒素を含む三弗化窒素を活
性炭と接触させ、二弗化二窒素或は二弗化二窒素
と亜酸化窒素を一工程で除去することを特徴とす
る三弗化窒素の精製方法にある。 That is, the gist of the present invention is to contact dinitrogen difluoride or dinitrogen difluoride and nitrogen trifluoride containing nitrous oxide with activated carbon, and to A method for purifying nitrogen trifluoride characterized by removing nitrogen oxide in one step.
本発明に用いる活性炭は、ヤシ殻炭、石油系活
性炭、石炭系活性炭等種類の如何を問わず、また
形状についても操作性のよい形状であれば破砕
状、粒状等いずれも使用できる。吸着温度は常温
でよい。 The activated carbon used in the present invention may be of any type, such as coconut shell carbon, petroleum-based activated carbon, or coal-based activated carbon, and may be in any shape, such as crushed or granular, as long as it is easy to handle. The adsorption temperature may be room temperature.
ところで、活性炭中には、通常、関係湿度50％
にて、乾量基準で1.5〜10％の平衡量の水が吸着
している。通常は、このまま使用するか、もしく
は乾燥のため100〜120℃の温度で加熱、脱水後使
用される。 By the way, activated carbon usually has a relative humidity of 50%
, an equilibrium amount of water of 1.5 to 10% on a dry basis is adsorbed. Usually, it is used as is or after being heated and dehydrated at a temperature of 100 to 120°C for drying.
本発明者らは、吸着性能の向上について検討を
重ねた結果、上記の如き通常の脱水処理では、活
性炭中になお1.5％程度の吸着水が残存しており、
この残存する吸着水量を１％以下にすることによ
り、活性炭の特異的吸着能力が飛躍的に増加する
ことを見出した。 As a result of repeated studies on improving adsorption performance, the present inventors found that with the above-mentioned normal dehydration treatment, about 1.5% of adsorbed water still remains in activated carbon.
It has been found that by reducing the amount of residual adsorbed water to 1% or less, the specific adsorption capacity of activated carbon can be dramatically increased.
残存する吸着水量を１％以下とするような活性
炭の活性化方法として、例えば、乾燥窒素ガス等
の不活性ガス雰囲気下、或は減圧下、120〜550℃
好ましくは150〜400℃の温度で加熱、脱水処理す
ると活性炭中の水分は各々１重量％以下、0.6重
量％以下となる。 As a method for activating activated carbon to reduce the amount of residual adsorbed water to 1% or less, for example, under an inert gas atmosphere such as dry nitrogen gas, or under reduced pressure, at 120 to 550°C.
When heated and dehydrated preferably at a temperature of 150 to 400°C, the moisture content in activated carbon becomes 1% by weight or less and 0.6% by weight or less, respectively.
加熱処理条件は、活性炭量、処理温度等を勘案
し、適宜選択することが出来すが、550℃を越え
ると加熱してもその効果は平衡に達しその必要性
がなくなる。 The heat treatment conditions can be selected as appropriate, taking into consideration the amount of activated carbon, the treatment temperature, etc., but when the temperature exceeds 550°C, the effect reaches equilibrium even if heated, and there is no need for it.
なお、活性炭の残存吸着水量は、乾燥窒素中で
550℃に試料を加熱し、日本工業規格に規定され
る強熱減量をもつて測定値とした。 In addition, the amount of residual adsorbed water on activated carbon is measured in dry nitrogen.
The sample was heated to 550°C, and the loss on ignition specified in Japanese Industrial Standards was taken as the measured value.
本発明の方法で処理できる三弗化窒素は、含有
される不純物の種類及び組成にかなり広い差異が
あつてもよい。すなわち、三弗化窒素中に二弗化
二窒素、亜酸化窒素以外の不純物、例えば四弗化
炭素、四弗化珪素等が存在しても、その性能には
全く影響がない。また特に、二弗化二窒素４容積
％以下、或は亜酸化窒素３容積％以下の組成であ
れば、吸着剤の寿命も長く好ましい。 The nitrogen trifluoride that can be treated by the method of the invention can vary considerably in the type and composition of impurities it contains. That is, even if impurities other than dinitrogen difluoride and nitrous oxide, such as carbon tetrafluoride and silicon tetrafluoride, are present in nitrogen trifluoride, its performance is not affected at all. In particular, a composition containing 4% by volume or less of dinitrogen difluoride or 3% by volume or less of nitrous oxide is preferable because the life of the adsorbent is long.
本発明の方法によれば、公知の方法により製造
される粗三弗化窒素、或は、汎用品として市場に
提供されている比較的低純度の三弗化窒素等、い
づれも処理可能であり、高純度化が達成できる。
また、CVD装置のクリーニングガスとして、三
弗化窒素が用いられた場合など、その廃ガスを本
方により処理することにより、不純物で汚染され
た三弗化窒素を精製、再利用することも可能であ
り、高価な三弗化窒素を有効に利用することがで
きる。 According to the method of the present invention, it is possible to process both crude nitrogen trifluoride produced by known methods and relatively low-purity nitrogen trifluoride provided on the market as a general-purpose product. , high purity can be achieved.
In addition, when nitrogen trifluoride is used as a cleaning gas for CVD equipment, it is also possible to purify and reuse nitrogen trifluoride contaminated with impurities by processing the waste gas ourselves. Therefore, expensive nitrogen trifluoride can be used effectively.
実施例
以下に実施例を示し、本発明を具体的に説明す
る。Examples Examples will be shown below to specifically explain the present invention.
実施例 １
内径20mmφの吸着塔に破砕状ヤシガラ活性炭
を、32ｇ充填し、系内を真空ポンプで1torr以下
に保ちながら、250℃で６時間加熱処理した。処
理後の活性炭中の水分量は、乾量基準で0.07％で
あつた。Example 1 An adsorption tower with an inner diameter of 20 mmφ was filled with 32 g of crushed coconut shell activated carbon, and heated at 250° C. for 6 hours while maintaining the inside of the system at 1 torr or less using a vacuum pump. The moisture content in the activated carbon after treatment was 0.07% on a dry basis.
このように処理した吸着塔へ、N2F21.5vol％、
N2O0.4vol％を不純物として含むNF3ガスを、20
ml／minの流量にて、常温にて導入した。吸着塔
出口ガスの分析（ガスクロマト）を経時的に行な
つた結果、これら不純物成分が検出されるまでの
時間（破過時間）は、N2F2：93時間、N2O：12
時間であつた。 To the adsorption tower treated in this way, 1.5 vol% of N 2 F 2 ,
NF3 gas containing 0.4vol% of N2O as an impurity was
It was introduced at room temperature at a flow rate of ml/min. As a result of analyzing the adsorption tower outlet gas over time (gas chromatography), the time (breakthrough time) until these impurity components were detected was 93 hours for N 2 F 2 and 12 hours for N 2 O.
It was time.
実施例 ２
ペレツト状の石油ピツチ系活性炭を、実施例１
と同様の吸着塔に、40ｇ充填し、乾燥窒素気流
下、200℃にて10時間加熱処理した。Example 2 Pellet-like petroleum pitch activated carbon was prepared in Example 1.
40g of the product was packed into an adsorption tower similar to the above, and heat-treated at 200°C for 10 hours under a stream of dry nitrogen.
処理後の活性炭中の水分量は、乾量基準で0.15
％であつた。上記処理を施した吸着塔へ、実施例
１と同じく、N2F21.5vol％、N2O0.4vol％を不純
物として含むNF3ガスを20ml／minの流量にて常
温で導入した。 The moisture content in activated carbon after treatment is 0.15 on a dry basis.
It was %. As in Example 1, NF 3 gas containing 1.5 vol % of N 2 F 2 and 0.4 vol % of N 2 O as impurities was introduced into the adsorption tower subjected to the above treatment at a flow rate of 20 ml/min at room temperature.
吸着塔出口ガスの分析を経時的に行なつた結果
破過時間は、N2F2：77時間、N2O：11時間であ
つた。 As a result of analyzing the gas at the outlet of the adsorption tower over time, the breakthrough time was 77 hours for N 2 F 2 and 11 hours for N 2 O.
実施例 ３
市販の粒状のヤシガラ炭を実施例１と同様の吸
着塔に、32ｇを充填した。Example 3 The same adsorption tower as in Example 1 was filled with 32 g of commercially available granular coconut husk charcoal.
活性炭中の水分量は、乾量基準で1.50％であつ
た。上記吸着塔へ、実施例１と同じく、
N2F21.5vol％、N2O0.4vol％を不純物として含む
NF3ガスを20ml／minの流量にて常温で導入し
た。 The moisture content in the activated carbon was 1.50% on a dry basis. To the above adsorption tower, as in Example 1,
Contains 1.5vol% of N 2 F 2 and 0.4vol% of N 2 O as impurities.
NF 3 gas was introduced at room temperature at a flow rate of 20 ml/min.
吸着塔出口ガスの分析を経時的に行なつた結
果、破過時間は、N2F2：48時間、N2O：10時間
であつた。 As a result of analyzing the gas at the outlet of the adsorption tower over time, the breakthrough time was 48 hours for N 2 F 2 and 10 hours for N 2 O.
実施例 ４
破砕状のヤシガラ炭を実施例１と同様の吸着塔
に、24ｇ充填し、乾燥窒素気流下、290℃にて８
時間加熱処理した。Example 4 24g of crushed coconut shell charcoal was packed into the same adsorption tower as in Example 1, and heated at 290°C under a stream of dry nitrogen for 8 hours.
Heat treated for hours.
処理後の活性炭中の水分量は、乾量基準で0.08
％であつた。上記処理を施した吸着塔へ、
N2F21.0vol％を不純物として含むNF3ガスを20
ml／minの流量にて常温で導入した。 The moisture content in activated carbon after treatment is 0.08 on a dry basis.
It was %. To the adsorption tower subjected to the above treatment,
20% of NF3 gas containing 1.0vol % of N2F2 as an impurity
It was introduced at room temperature at a flow rate of ml/min.
吸着塔出口ガスの分析を経時的に行なつた結
果、破過時間は、N2F2について113時間であつ
た。 As a result of analyzing the gas at the outlet of the adsorption tower over time, the breakthrough time for N 2 F 2 was 113 hours.
比較例 １
実施例１と同様の吸着塔に、ペレツト状のモレ
キユラーシーブ5Aを、65ｇで充填し、乾燥窒素
気流下200℃にて10時間加熱処理した。Comparative Example 1 The same adsorption tower as in Example 1 was filled with 65 g of pelleted molecular sieve 5A, and heat-treated at 200° C. for 10 hours under a stream of dry nitrogen.
上記処理を施した吸着塔へN2F21.5vol％、
N2O0.4vol％を不純物として含むNF3ガスを20
ml／minの流量にて常温で導入した。 1.5vol% of N 2 F 2 to the adsorption tower subjected to the above treatment,
NF3 gas containing 0.4vol% N2O as an impurity was added to the
It was introduced at room temperature at a flow rate of ml/min.
吸着塔出口ガスの分析を経時的に行なつた結
果、破過時間はN2F2：９時間、N2O：11時間で
あつた。 As a result of analyzing the gas at the outlet of the adsorption tower over time, the breakthrough time was 9 hours for N 2 F 2 and 11 hours for N 2 O.
発明の効果
以上述べたように、本発明に係る三弗化窒素の
精製方法は、極めて単純な方法により、常温にて
極めて長時間、しかも三弗化窒素中に不純物とし
て含まれる二弗化二窒素或は二弗化二窒素と亜酸
化窒素を一工程で除去する方法を提供するもので
ある。Effects of the Invention As described above, the method for purifying nitrogen trifluoride according to the present invention is a very simple method, can be carried out at room temperature for a very long time, and is capable of purifying nitrogen trifluoride containing difluoride contained as an impurity in nitrogen trifluoride. The present invention provides a method for removing nitrogen or dinitrogen difluoride and nitrous oxide in one step.
Claims (1)
を含む三弗化窒素を活性炭と接触させることによ
り、前記二弗化二窒素又は二弗化二窒素と亜酸化
窒素を除去することを特徴とする三弗化窒素の精
製方法。 ２ 前記活性炭が、120℃〜550℃で処理し、該活
性炭中の水分量を１重量％以下とした活性炭であ
る特許請求の範囲第１項記載の精製方法。[Scope of Claims] 1. By contacting dinitrogen difluoride or dinitrogen difluoride and nitrogen trifluoride containing nitrous oxide with activated carbon, the dinitrogen difluoride or dinitrogen difluoride and nitrous oxide A method for purifying nitrogen trifluoride, characterized by removing nitrogen oxide. 2. The purification method according to claim 1, wherein the activated carbon is treated at 120°C to 550°C to reduce the water content in the activated carbon to 1% by weight or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8879985A JPS61247609A (en) | 1985-04-26 | 1985-04-26 | Purifying method for nitrogen trifluoride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8879985A JPS61247609A (en) | 1985-04-26 | 1985-04-26 | Purifying method for nitrogen trifluoride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61247609A JPS61247609A (en) | 1986-11-04 |
| JPH0242766B2 true JPH0242766B2 (en) | 1990-09-26 |
Family
ID=13952908
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8879985A Granted JPS61247609A (en) | 1985-04-26 | 1985-04-26 | Purifying method for nitrogen trifluoride |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61247609A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0755807B2 (en) * | 1987-11-04 | 1995-06-14 | 三井東圧化学株式会社 | Method for producing nitrogen trifluoride |
| JPH0280310A (en) * | 1988-06-01 | 1990-03-20 | Mitsui Toatsu Chem Inc | Purifying method for gaseous nf3 |
| US4933158A (en) * | 1988-10-25 | 1990-06-12 | Mitsui Toatsu Chemicals, Incorporated | Method for purifying nitrogen trifluoride gas |
-
1985
- 1985-04-26 JP JP8879985A patent/JPS61247609A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61247609A (en) | 1986-11-04 |
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