JPS63151608A - Purification of nitrogen trifluoride gas - Google Patents
Purification of nitrogen trifluoride gasInfo
- Publication number
- JPS63151608A JPS63151608A JP29764586A JP29764586A JPS63151608A JP S63151608 A JPS63151608 A JP S63151608A JP 29764586 A JP29764586 A JP 29764586A JP 29764586 A JP29764586 A JP 29764586A JP S63151608 A JPS63151608 A JP S63151608A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- solid oxide
- nitrogen trifluoride
- zeolite
- present
- 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.)
- Pending
Links
- 239000007789 gas Substances 0.000 title claims description 47
- 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 28
- 238000000746 purification Methods 0.000 title description 4
- 239000007787 solid Substances 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 25
- 238000005273 aeration Methods 0.000 claims description 10
- DUQAODNTUBJRGF-ONEGZZNKSA-N dinitrogen difluoride Chemical compound F\N=N\F DUQAODNTUBJRGF-ONEGZZNKSA-N 0.000 claims description 3
- 229910021536 Zeolite Inorganic materials 0.000 abstract description 11
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 abstract description 11
- 239000010457 zeolite Substances 0.000 abstract description 11
- 239000003795 chemical substances by application Substances 0.000 abstract description 3
- 238000001312 dry etching Methods 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003463 adsorbent Substances 0.000 description 6
- 238000009423 ventilation Methods 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 238000004817 gas chromatography Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- -1 metals are used Chemical class 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- XIQPNCZCDTUCTM-UHFFFAOYSA-N fluorane Chemical compound F.F.F.F XIQPNCZCDTUCTM-UHFFFAOYSA-N 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance 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)
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は三弗化窒素ガスの精製方法に関する。[Detailed description of the invention] (Industrial application field) The present invention relates to a method for purifying nitrogen trifluoride gas.
更に詳しくは、三弗化窒素ガス中の特に二弗化二窒素の
除去方法に関する。More specifically, the present invention relates to a method for removing dinitrogen difluoride from nitrogen trifluoride gas.
（従来技術及びその問題点）
三弗化窒素（ＮＦ２）ガスは、半導体のドライエツチン
グ剤やＣＶＤ装置のクリーニングガスとして近年注目さ
れているが、これらの用途に使用される三弗化窒素ガス
は、可及的高純度のものが要求されている。(Prior art and its problems) Nitrogen trifluoride (NF2) gas has recently attracted attention as a dry etching agent for semiconductors and as a cleaning gas for CVD equipment. , the highest possible purity is required.
三弗化窒素（ＮＦ３）ガスは、種々の方法で製造される
が何れの方法で得られたガスも殆どの場合、亜酸化窒素
（ＮＪ） 、二酸化炭素（Ｃ（ｈ） 、二弗化二窒素（
ＮＪｚ）などの不純物を比較的多量に含んでいるので、
高純度のＮＦ２ガスを得る為には精製が必要である。Nitrogen trifluoride (NF3) gas is produced by various methods, but in most cases the gas obtained by any of the methods is nitrous oxide (NJ), carbon dioxide (C(h), difluoride difluoride). nitrogen(
Since it contains relatively large amounts of impurities such as NJz),
Purification is necessary to obtain high purity NF2 gas.
ＮＦＳガス中のこれらの不純物を除去する精製方法とし
ては、ゼオライトなどの吸着剤を用いて不純物を吸着除
去する方法が、最も効率がよく簡便な方法の一つとして
よく知られている〔ケミカル・エンジニアング（Ｃｈｅ
ｗ、 Ｅｎｇ、） ８４．１１６． （１９７７）等〕
、シかしながら、この吸着による精製方法では、ＮＦ３
ガス中にＮ、Ｆ、が存在すると次のような弊害が生じる
。すなわち、
１）Ｎｚｈが存在すると、他の不純物であるＣＯ２やＮ
ｘＯなどの吸着能力が極端に小さくなる。As a purification method for removing these impurities from NFS gas, the method of adsorbing and removing impurities using an adsorbent such as zeolite is well known as one of the most efficient and simple methods [Chemical Engineering (Che
w, Eng,) 84.116. (1977) etc.]
However, in this adsorption purification method, NF3
The presence of N and F in the gas causes the following problems. That is, 1) When Nzh exists, other impurities such as CO2 and N
The ability to adsorb xO etc. becomes extremely small.
２）Ｎ□Ｆ、が存在すると、ＮＦ、も吸着剤に吸着され
易くなり、従ってＮＦ２ガスの損失を招く。2) When N□F exists, NF is also likely to be adsorbed by the adsorbent, thus causing loss of NF2 gas.
３）吸着剤に吸着し濃縮されたＮｚＦｚは、分解して熱
を発し易く、著しい場合には爆発を引き起こす。3) NzFz that has been adsorbed and concentrated on the adsorbent is likely to decompose and generate heat, causing an explosion in severe cases.
従って、ゼオライト等の吸着剤を使用してＮＦ２ガス中
の不純物を吸着除去する方法を採用する場合には、それ
に先立って予めＮＪｔを除去しておく必要がある。Therefore, when adopting a method of adsorbing and removing impurities in NF2 gas using an adsorbent such as zeolite, it is necessary to remove NJt in advance.
ＮＦ３ガス中のＮｚＦｚの除去方法としては、Ｋｌ、■
！、 Ｎａ１Ｓ、 Ｎａ＊５ｔＯ４、Ｎａ、ＳＯ２等
の水溶液とＮｔＦｔとを反応槽において反応させて除去
する方法が従来知られている（Ｊ、Ｍａｓｓｏｎｎｅ、
ケミ−・インジェニュール・テヒニーク（Ｃｈｅｗ、
Ｉｎｇ、 Ｔｅｃｈｎ、） ４１． （１２）、 ６９
５． （１９６９） ） ｌ、かじながら、この方法で
は、ＮＪｘを完全に除去する為には比較的長時間を要す
るので、従って反応槽がかなり大きくなるだけではなく
大量の薬剤も必要とする。As a method for removing NzFz in NF3 gas, Kl, ■
! , Na1S, Na*5tO4, Na, SO2, etc., and a method of removing NtFt by reacting them in a reaction tank is conventionally known (J. Massonne, et al.
Chemie Ingéneur Technique (Chew,
Ing, Techn, ) 41. (12), 69
5. (1969)) However, this method requires a relatively long time to completely remove NJx, and therefore requires not only a fairly large reaction vessel but also a large amount of chemicals.
また、ＮＪｔを除去する別の方法として、Ｎｚｐｚを含
有するＮＦ３ガスを加熱した金属と接触させる方法も知
られてる（特公昭５９−１５０８１） 、 Ｌかしなが
ら、この方法は、ニッケル等の高価な金属を使用するの
で、これら金属の損失も含めコストアップを招くという
問題がある。Furthermore, as another method for removing NJt, a method is known in which NF3 gas containing Nzpz is brought into contact with heated metal (Japanese Patent Publication No. 59-15081). Since metals such as metals are used, there is a problem in that costs including losses of these metals increase.
（問題を解決する為の手段）
本発明者等はＮＦｆｆガス中に含まれるＮＪｔの除去方
法について鋭意検討を重ねた結果、固体酸化物層に特定
な条件でＮ２Ｆオを含むＮＦｓガスを通気させれば、極
めて効率よ（安全にしかも経済的にこれを除去出来るこ
とを見出し、本発明を完成するに至ったものである。(Means for Solving the Problem) As a result of intensive study on a method for removing NJt contained in NFff gas, the inventors of the present invention ventilated NFs gas containing N2F into the solid oxide layer under specific conditions. We have discovered that this can be removed extremely efficiently (safely and economically) and have completed the present invention.
即ち本発明は少なくとも不純物として二弗化二窒素を含
有する三弗化窒素ガスを、固体酸化物層に温度１５０〜
４００″Ｃの範囲において通気させることを特徴とする
三弗化窒素ガスの精製法である。That is, the present invention applies nitrogen trifluoride gas containing at least dinitrogen difluoride as an impurity to a solid oxide layer at a temperature of 150 to
This is a method for purifying nitrogen trifluoride gas, which is characterized by aeration in a temperature range of 400''C.
（発明の詳細な開示） 以下本発明の詳細な説明する。(Detailed disclosure of the invention) The present invention will be explained in detail below.
本発明において使用可能な固体酸化物としては、ＮｔＦ
ｔと反応してフッ化物を生成するすべての固体酸化物が
使用出来る。このような固体酸化物を例示すると例えば
、５ｉＯ１、Ａｌｔｏｚ ％ ＺｎＯ、Ｆｅｔｃｈ、ｐ
ｅ３０４ 、Ｂｘ（ｈ、ＮｉＯｓ ＭｇＯ５ＣａＯ、Ｔ
４０ｔＳＣｕＯ１ＭｎＯ□等が有効であり、またゼオラ
イト等のような上記酸化物の複合酸化物も有効である。Solid oxides that can be used in the present invention include NtF
Any solid oxide that reacts with fluoride to form fluoride can be used. Examples of such solid oxides include 5iO1, Altoz% ZnO, Fetch, p
e304, Bx(h, NiOs MgO5CaO, T
40tSCuO1MnO□ etc. are effective, and composite oxides of the above oxides such as zeolite etc. are also effective.
尚、ゼオライトについては、特公昭５９−１５０８１号
公報の比較例に、約１００℃の温度でＮｈを分解する為
有効でない旨の記述があるが、本発明者等の検討によ糺
ば、この程度の温度ではＮＦ、は分解されず、従って本
発明においても有効である。Regarding zeolite, there is a description in the comparative example of Japanese Patent Publication No. 15081/1981 that it is not effective because it decomposes Nh at a temperature of about 100°C. NF is not decomposed at a certain temperature, and is therefore effective in the present invention.
本発明に使用する固体酸化物の形状は、ＮＦ、ガスをこ
れに接触させるという点から粒状で高比表面積のものが
好ましい、従って通常市販のシリカゲル、活性アルミナ
、ゼオライト等がその粒状でありそのまま使用出来る点
で特に好ましい。The shape of the solid oxide used in the present invention is preferably granular and has a high specific surface area from the viewpoint of bringing NF and gas into contact with it. Therefore, commercially available silica gel, activated alumina, zeolite, etc. are preferably granular and as they are. It is particularly preferable in that it can be used.
本発明においては、上記のごとき固体酸化物により充填
層を形成し、これにＮ、Ｆ、を含むＮＦ３ガスを通気す
る。ガスの固体酸化物層への通気温度は、１５０〜４０
０℃で実施される０通気温度がｔｓｏ ’ｃ未満ではｈ
Ｆｘを殆ど分解除去出来ない、逆に４００℃を超える温
度ではＮ、Ｆ、はほぼ完全に除去出来るものの、ＮＦ３
をも分解するのでＮＦ、の損失を招く為不都合である。In the present invention, a packed bed is formed using the solid oxide as described above, and NF3 gas containing N and F is passed through the packed bed. The temperature at which gas is introduced into the solid oxide layer is 150-40°C.
If the 0 aeration temperature carried out at 0 °C is less than tso 'c h
Fx can hardly be decomposed and removed; conversely, N and F can be almost completely removed at temperatures above 400°C, but NF3
This is inconvenient because it also decomposes NF, resulting in loss of NF.
また熱エネルギーの損失にもつながる。なお、この温度
範囲において、ＮｔＦｔと固体酸化物との反応は非常に
速いので、通気させるＮＦ２ガスの固体酸化物層内での
滞留時間は短くてかまわないが、通常１〜１０００秒程
度の範囲で実施される。It also leads to loss of thermal energy. In addition, in this temperature range, the reaction between NtFt and the solid oxide is very fast, so the residence time of the NF2 gas to be vented in the solid oxide layer may be short, but it is usually in the range of about 1 to 1000 seconds. It will be carried out in
本発明においては、固体酸化物層に通気するＮＦ３ガス
は、単独で供給してもかまわないが、Ｎ２、Ｈｅ等の不
活性ガスあるいは空気などで希釈したものでもかまわな
い、また、通気ガスの圧力については特に制限はないが
、通常、０〜５ｋｇ／ａｍ”−Ｈの圧力が操作し易いの
で好ましい。In the present invention, the NF3 gas to be vented to the solid oxide layer may be supplied alone, but it may also be diluted with an inert gas such as N2 or He, or air. There are no particular restrictions on the pressure, but a pressure of 0 to 5 kg/am''-H is usually preferred because it is easy to operate.
（発明の効果）
本発明は以上詳細に説明した如く、Ｎｈガス中のＮｔＦ
ｔを除去する方法において固体酸化物を用い、これに特
定の条件でＮＦ３ガスを通気させるという極めて簡単な
方法であり、しかも固体酸化物は安価であるので極めて
経済的な方法である。また後記する実施例が示す如く、
ＮｚＦｚの除去率が極めて優れているので、本発明の方
法で精製したＮＦ。(Effects of the Invention) As explained in detail above, the present invention provides NtF in Nh gas.
This is an extremely simple method of using a solid oxide to remove t and passing NF3 gas through it under specific conditions, and since solid oxide is inexpensive, it is an extremely economical method. In addition, as shown in the examples described later,
NF purified by the method of the present invention has an extremely excellent removal rate of NzFz.
ガスを従来公知の情調方法、例えば前記ゼオライトなど
の吸着剤を使用して再度精製すれば、参考例１が示す如
く、半導体ドライエツチング剤の原料等として好適な高
純度のＮＦ３ガスを容易に得ること出来ると云う、顕著
な作用効果を奏するのである。更に、本発明の方法はＮ
ｈの損失もなくかつ安全な方法である。If the gas is purified again using a conventionally known conditioning method, for example using an adsorbent such as the above-mentioned zeolite, it is easy to obtain highly purified NF3 gas suitable as a raw material for semiconductor dry etching agents, etc., as shown in Reference Example 1. It has remarkable effects. Furthermore, the method of the present invention
This is a safe method without any loss of h.
（実施例及び比較例）
以下、実施例及び比較例により本発明を更に具体的に説
明する。尚、実施例、比較例中の％及びｐｐｒｍは容量
基準を表す。(Examples and Comparative Examples) Hereinafter, the present invention will be explained in more detail with reference to Examples and Comparative Examples. Note that % and pprm in Examples and Comparative Examples represent capacity standards.
実施例１〜４
内径１５Ｉｌｌｌのガラス製カラムに、市販のシリカゲ
ル（２４〜４８メツシユの粒状品）を充填（充填高さ２
０ｃ１１）シた後、このシリカゲル層に第１表に示す条
件でＮＦ３ガスの通気を行なった０通気後のガスは更に
純水中にバブリングさせた。Examples 1 to 4 A glass column with an inner diameter of 15 Illl was filled with commercially available silica gel (granular product of 24 to 48 mesh) (filling height 2
After 0c11), NF3 gas was aerated through the silica gel layer under the conditions shown in Table 1.The gas after the aeration was further bubbled into pure water.
通気前後のＮＦｓガスの組成をガスクロ分析により測定
した。その結果は第１表に示す通りＮ１Ｆｔは極めて高
い除去率であった。The composition of the NFs gas before and after ventilation was measured by gas chromatography. As shown in Table 1, the results showed that N1Ft had an extremely high removal rate.
第１表
実施例５〜８
内径１５＋ａｍのアルミナ製カラムに活性アルミナ（２
４〜４８メツシユの粒状品）を充填（充填高さ２０ｃ＋
ｗ）した後、この活性アルミナ層に第２表に示す条件で
ＮＦ、ガスの通気を行なった０通気後のガスは実施例１
〜４と同様にして、更に純水中にバブリングさせた。Table 1 Examples 5 to 8 Activated alumina (2
Filling with 4 to 48 mesh granular products (filling height 20c+
After w), NF and gas were aerated into this activated alumina layer under the conditions shown in Table 2.The gas after aeration was as in Example 1.
In the same manner as in ~4, bubbles were further bubbled into pure water.
通気前後のＮＦｓガスの組成をガスクロ分析により測定
した。その結果は第２表に示す通り、ＮｔＦｔは極めて
高い除去率であった。尚、活性アルミナを分析したとこ
ろＡｌＦ３が生成していたが、この事実はＮ＊ｈが活性
アルミナと反応して除去されることを証明するものであ
る。The composition of the NFs gas before and after ventilation was measured by gas chromatography. As shown in Table 2, the results showed that NtFt had an extremely high removal rate. Incidentally, when activated alumina was analyzed, AlF3 was generated, which proves that N*h is removed by reacting with activated alumina.
第２表
実施例９．１０
実施例１〜４で使用したと同一のガラス製カラムに、市
販のゼオライト（細孔径５人）（２４〜４日メツシュの
粒状品）を充填（充填高さ２０ｃｍ） した後、このゼ
オライト層にＮＦ３ガスとＮ２ガスをそれぞれ２０８ｄ
／＋ｉｎ、の流量で同時に第３表に示す条件で通気を行
なった０通気後のガスは実施例１〜４と同様に、更に純
水中にバブリングさせた。Table 2 Example 9.10 A glass column identical to that used in Examples 1 to 4 was packed with commercially available zeolite (5 pore size) (24-4 day mesh granules) (packing height 20 cm). ) After that, 208 d of NF3 gas and N2 gas were added to this zeolite layer.
The gas after zero aeration, which was simultaneously aerated under the conditions shown in Table 3 at a flow rate of /+in, was further bubbled into pure water in the same manner as in Examples 1 to 4.
通気後のガスの組成をガスクロ分析により測定した。そ
の結果は第３表に示す通りＮｔＦ、は極めて高い除去率
であり、またＮＦ、の分解は全くなかっ第 ３ 表
比較例１〜３
実施例５〜８と同一の活性アルミナを充填したカラムを
使用し、ＮＦ３ガスとＮ８ガスをそれぞれ２０ Ｎｄ／
ｗｉｎ、で同時に第４表に示す条件で通気を行なった０
通気後のガスは実施例１〜４と同様に、更に純水中にバ
ブリングさせた６通気後のガスの組成をガスクロ分析に
より測定した。その結果は第４表に示す通りであり、通
気温度が１５０℃未満ではＮｚＦｚは殆ど除去出来ない
、また４００ ’Ｃを超える温度ではＮｚｐｚの除去率
は極めて高いものの、ＮＦｆｆ も分解しその収率が悪
くなることが分かる。The composition of the gas after ventilation was measured by gas chromatography. As shown in Table 3, the removal rate of NtF was extremely high, and there was no decomposition of NF. NF3 gas and N8 gas each at 20 Nd/
At the same time, ventilation was carried out under the conditions shown in Table 4.
The gas after aeration was further bubbled into pure water in the same manner as in Examples 1 to 4, and the composition of the gas after aeration was measured by gas chromatography. The results are shown in Table 4. When the ventilation temperature is below 150°C, almost no NzFz can be removed, and when the temperature exceeds 400°C, although the removal rate of Nzpz is extremely high, NFff is also decomposed and its yield decreases. It turns out that it gets worse.
第４表
参考例１
実施例１〜４で使用したと同一のガラス製カラムに、市
販のゼオライト（細孔径５人）（２４〜４８メツシユの
粒状品）を充填（充填高さ２０ｃ＋ｓ） ｔ、た後、こ
のゼオライト層に実施例４で得たＮｚＦｘを除去したＮ
Ｆ３ガスを通気した。通気条件としては温度は常温（２
０℃）、ＮＦ２ガス流量２ＯＮｍ／ｓｉｎ、 、通気圧
カフ６０Ｔｏｒｒであった０通気後のＮＦ３ガスの組成
をガスクロ分析により測定した。その結果はＮｚＦｚ２
０ｐｐｍ以下、ＮｔＯ２０ｐｐｍ以下、ＣＯｚ ２０ｐ
ｐｍ以下で、本発明の方法により、予めＮｚｈを除去し
たＮＦ、ガスを従来公知の吸着剤で精製すれば、ＮＺＯ
やＣｏｔ等Ｎｘｈ以外の不純物が極めて高い除去率で除
去された高純度のＮｈが得られることが理解されるので
ある。Table 4 Reference Example 1 The same glass column used in Examples 1 to 4 was filled with commercially available zeolite (pore size 5) (granular product of 24 to 48 mesh) (packing height 20c+s). After that, the NzFx obtained in Example 4 was removed from this zeolite layer.
F3 gas was bubbled through. The ventilation conditions are room temperature (2
The composition of the NF3 gas was measured by gas chromatography after aeration at 0 °C), an NF2 gas flow rate of 2ONm/sin, and an aeration pressure of 60 Torr. The result is NzFz2
0ppm or less, NtO 20ppm or less, COz 20p
pm or less, if the NF gas from which Nzh has been removed in advance by the method of the present invention is purified using a conventionally known adsorbent, NZO
It is understood that high-purity Nh from which impurities other than Nxh, such as Cot and Cot, are removed at an extremely high removal rate can be obtained.
Claims (1)
三弗化窒素ガスを、固体酸化物層に温度１５０〜４００
℃の範囲において通気させることを特徴とする三弗化窒
素ガスの精製法。(1) Nitrogen trifluoride gas containing at least dinitrogen difluoride as an impurity is added to the solid oxide layer at a temperature of 150 to 400.
A method for purifying nitrogen trifluoride gas, characterized by aeration in a temperature range of °C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29764586A JPS63151608A (en) | 1986-12-16 | 1986-12-16 | Purification of nitrogen trifluoride gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29764586A JPS63151608A (en) | 1986-12-16 | 1986-12-16 | Purification of nitrogen trifluoride gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63151608A true JPS63151608A (en) | 1988-06-24 |
Family
ID=17849266
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29764586A Pending JPS63151608A (en) | 1986-12-16 | 1986-12-16 | Purification of nitrogen trifluoride gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63151608A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0366078A2 (en) * | 1988-10-25 | 1990-05-02 | MITSUI TOATSU CHEMICALS, Inc. | Method for Purifying nitrogen trifluoride gas |
| US5069887A (en) * | 1990-01-10 | 1991-12-03 | Central Glass Company, Limited | Method of refining nitrogen trifluoride gas |
| US5094825A (en) * | 1990-02-05 | 1992-03-10 | Ebara Corporation | Process for treating waste gases containing clf3 |
| 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 |
| WO1999024358A1 (en) * | 1997-11-10 | 1999-05-20 | E.I. Du Pont De Nemours And Company | Process for purifying perfluorinated products |
-
1986
- 1986-12-16 JP JP29764586A patent/JPS63151608A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0366078A2 (en) * | 1988-10-25 | 1990-05-02 | MITSUI TOATSU CHEMICALS, Inc. | Method for Purifying nitrogen trifluoride gas |
| US4933158A (en) * | 1988-10-25 | 1990-06-12 | Mitsui Toatsu Chemicals, Incorporated | Method for purifying nitrogen trifluoride gas |
| US5069887A (en) * | 1990-01-10 | 1991-12-03 | Central Glass Company, Limited | Method of refining nitrogen trifluoride gas |
| US5094825A (en) * | 1990-02-05 | 1992-03-10 | Ebara Corporation | Process for treating waste gases containing clf3 |
| 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 |
| WO1999024358A1 (en) * | 1997-11-10 | 1999-05-20 | E.I. Du Pont De Nemours And Company | Process for purifying perfluorinated products |
| US6458249B2 (en) | 1997-11-10 | 2002-10-01 | E. I. Du Pont De Nemours And Company | Process for purifying perfluorinated products |
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