JPH02153809A - Purification of nitrogen trifluoride gas - Google Patents
Purification of nitrogen trifluoride gasInfo
- Publication number
- JPH02153809A JPH02153809A JP30688088A JP30688088A JPH02153809A JP H02153809 A JPH02153809 A JP H02153809A JP 30688088 A JP30688088 A JP 30688088A JP 30688088 A JP30688088 A JP 30688088A JP H02153809 A JPH02153809 A JP H02153809A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- silica gel
- nitrogen trifluoride
- temperature
- 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 abstract description 66
- 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 abstract description 22
- 238000000746 purification Methods 0.000 title description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000000741 silica gel Substances 0.000 claims abstract description 34
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000005273 aeration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000001179 sorption measurement Methods 0.000 abstract description 4
- 238000009423 ventilation Methods 0.000 abstract description 4
- 238000001312 dry etching Methods 0.000 abstract description 3
- 239000004065 semiconductor Substances 0.000 abstract description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 208000005156 Dehydration Diseases 0.000 description 7
- 230000018044 dehydration Effects 0.000 description 7
- 238000006297 dehydration reaction Methods 0.000 description 7
- 239000003463 adsorbent Substances 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 238000004821 distillation Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 235000001674 Agaricus brunnescens Nutrition 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- DUQAODNTUBJRGF-ONEGZZNKSA-N dinitrogen difluoride Chemical compound F\N=N\F DUQAODNTUBJRGF-ONEGZZNKSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 239000001272 nitrous oxide Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Separation Of Gases By Adsorption (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.
さらに詳しくは、三弗化窒素ガス中に含まれる亜酸化窒
素（Ｎ富ｏ）、二酸化炭素（ＣＯｔ）及び二弗化二窒素
（ＮｇＦｔ）の除去方法に関する。More specifically, the present invention relates to a method for removing nitrous oxide (N-rich o), carbon dioxide (COt), and dinitrogen difluoride (NgFt) contained in nitrogen trifluoride gas.
〔従来の技術及び発明が解決しようとする課題〕三弗化
窒素（ＮＦ３）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ＮＦｓガスは、高純度
のものが要求されている。[Prior art and problems to be solved by the invention] Nitrogen trifluoride (NF3) gas has recently attracted attention as a dry etching agent for semiconductors and a cleaning gas for CVD equipment. High purity gas is required.
ＮＦ、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、Ｎ、ｏ 、ｃｏｔ 。NF and gas are produced by various methods, but in most cases the gas obtained by any method is N, o, cot.
Ｎ！Ｆよなどの不純物を比較的多量に含んでいるので、
上記用途としての高純度のＮＦ、ガスを得るためには精
製が必要である。N! Because it contains a relatively large amount of impurities such as F,
Purification is necessary to obtain high purity NF and gas for the above uses.
ＮＦ３ガス中のこれらの不純物を除去する精製方法とし
ては、モレキエラシープ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・エンジュアング（
Ｃｈｅｗ、 Ｅｎｇ、） ８４．１１６゜（１９７７）
等〕、シかしながら、この吸着による精製方法では、Ｎ
Ｆ、ガス中にＮｔｈが存在するとＮＦ。As a purification method for removing these impurities from NF3 gas, the method of adsorbing and removing impurities using an adsorbent such as Molecuyra Sheep is well known as one of the most efficient and simple methods [Chemical Enjuang (
Chew, Eng,) 84.116° (1977)
[etc.], but in this purification method by adsorption, N
F, NF when Nth exists in the gas.
も吸着剤に吸着され易くなり、従ってＮｈガスの損失を
招くという極めて不都合な問題があり、ＮＦ、ガスの精
製方法としては実質的でない。There is also the extremely inconvenient problem that Nh gas is easily adsorbed by the adsorbent, resulting in loss of Nh gas, and is therefore not practical as a method for purifying NF gas.
本発明者等はかかる状況に鑑み、Ｎｈガス中に含まれて
いるＮｅｏ 、ｃｏ、及びＮｘＰｘの除去方法について
種々の吸着剤を用いて鋭意検討を重ねた結果、予め特定
の温度に加熱して脱水処理したシリカゲル層へ特定の温
度でＮＦ、ガスを通気させれば、ＮＦ、がシリカゲルに
吸着されることなく、極めて効率よく経済的にＮＦ、ガ
ス中のＮ、０ 、 Ｃｏオ及びＮ。In view of this situation, the present inventors have conducted intensive studies on methods for removing Neo, co, and NxPx contained in Nh gas using various adsorbents. If NF and gas are passed through the dehydrated silica gel layer at a specific temperature, NF will not be adsorbed by the silica gel, and N, 0, Co and N in the NF and gas will be removed very efficiently and economically.
Ｆ、を除去できることを見出し、本発明を完成するに至
ったものである。It was discovered that F can be removed, and the present invention was completed.
即ち本発明の三弗化窒素ガスの精製方法は、予め１５０
〜３００″Ｃの範囲の温度に加熱して脱水処理したシリ
カゲル層へ、三弗化窒素ガスを０〜＝１２５℃の温度で
かつ実質的に水分の混入しない状態で通気させることを
特徴とするものである。That is, in the method for purifying nitrogen trifluoride gas of the present invention, 150
It is characterized by passing nitrogen trifluoride gas through the silica gel layer heated to a temperature in the range of ~300"C and subjected to dehydration treatment at a temperature of 0 to =125"C and in a state in which substantially no moisture is mixed. It is something.
（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.
本発明において吸着剤として使用するシリカゲルは、特
に限定はなく通常市販のものが何れも使用可能であるが
、粒状かつ高比表面積のものがより好ましい。The silica gel used as an adsorbent in the present invention is not particularly limited, and any commercially available silica gel can be used, but granular silica gel with a high specific surface area is more preferable.
シリカゲルの脱水処理は１５０〜３００℃、好ましくは
１５０〜２００℃の温度に加熱することで実施される。The dehydration treatment of silica gel is carried out by heating to a temperature of 150 to 300°C, preferably 150 to 200°C.
加熱温度が１５０℃未満ではシリカゲル中に水分が残存
するので、該シリカゲル層へＮＦ２ガスを通気した際に
ＮｘＯ、Ｃ（ｈ 、ＮｚＰｔの除去能力が低下する。逆
に、例えば３５０℃以上の高温に加熱すると、シリカゲ
ルの吸着能力が大きく低下するので不都合であり、また
エネルギーの損失でもある。If the heating temperature is lower than 150°C, water will remain in the silica gel, so when NF2 gas is passed through the silica gel layer, the ability to remove NxO, C(h2, and NzPt) will decrease. Heating to silica gel greatly reduces the adsorption ability of silica gel, which is disadvantageous and also results in a loss of energy.
シリカゲルの加熱による脱水処理は空気中で行なっても
良いが、該加熱はシリカゲル中に含有する水分を気化逸
散させるために行なうので、例えば窒素ガスのように水
分を含有しない不活性ガスの気流中で行なうのが良く、
またガスを吸引しながら減圧下で行なうことも好ましい
。Dehydration treatment by heating silica gel may be performed in the air, but since the heating is performed to vaporize and dissipate the moisture contained in the silica gel, for example, an air stream of an inert gas that does not contain moisture such as nitrogen gas is used. It is better to do it inside.
It is also preferable to conduct the reaction under reduced pressure while sucking gas.
加熱時間は上記の加熱温度及び雰囲気において３０分以
上であれば良いが、念のために通常１〜２時間行なわれ
る。The heating time may be 30 minutes or more at the above-mentioned heating temperature and atmosphere, but it is usually carried out for 1 to 2 hours just to be sure.
かくして加熱によって脱水処理されたシリカゲルは、放
冷または強制冷却によって常温以下に冷却されるが、こ
の際には水分の混入を回避しなければならない、従って
、その方法として上記のシリカゲルの加熱による脱水処
理を、例えばカラム等にシリカゲルを充填した状態で行
ない、脱水処理後これを冷却し、しかるのち引続きこの
シリカゲル層へＮＦ、ガスを通気する方法が好ましい。The silica gel that has been dehydrated by heating is then cooled down to room temperature or below by letting it cool or forced cooling, but at this time, it is necessary to avoid contamination with water. It is preferable to carry out the treatment, for example, in a column filled with silica gel, cool it after dehydration, and then pass NF or gas through the silica gel layer.
ＮＦ３ガスの精製は、上記の通りカラム等に充填された
シリカゲル層に通気する方法で実施されるが、この際の
通気温度は重要で、０℃以下の温度でなければならず、
低温はど好ましい、しかし、ＮＦＳの沸点は一１２９℃
であるので、この温度以下では操作が事実上困難である
。従ってＮＦ３ガスの通気温度は本発明では、０〜−１
２５℃の範囲で実施される。Purification of NF3 gas is carried out by aeration through a silica gel layer packed in a column etc. as described above, but the aeration temperature at this time is important and must be below 0°C.
Lower temperatures are preferable, but the boiling point of NFS is -129°C.
Therefore, operation is practically difficult below this temperature. Therefore, in the present invention, the ventilation temperature of NF3 gas is 0 to -1.
It is carried out in the range of 25°C.
通気時のＮＦ３ガスの圧力はこれまた特に限定はないが
、例えばＯ〜５ ｋｇ／ｃ＋ｊ−Ｇ程度の圧力が操作し
やすいので好ましい。The pressure of the NF3 gas during ventilation is also not particularly limited, but a pressure of, for example, about 0 to 5 kg/c+j-G is preferred because it is easy to operate.
尚、本発明の実施により精製されたＮＦ３ガスは、本発
明者等が先に提案した特願昭６２−１３８９７２号の方
法、即ち、ＮＦ３より低沸点でかつＮＦ、と相互溶解性
のない第三成分、例えばヘリウム（）ｌｅ）ガスの共存
下でＮＦ３を深冷蒸留することにより、含有するＮｚＯ
、Ｃｏｔ 、Ｎｘｈ以外のＮｔ、 ｏｘ等の不純物を除
去することができ、半導体のドライエツチング剤やＣＶ
Ｄ装置のクリーニングガスとして好適な高純度のＮＦ、
ガスを容易に得ることが可能となるのである。Note that the NF3 gas purified by carrying out the present invention can be obtained by the method of Japanese Patent Application No. 138972/1987, which was previously proposed by the present inventors. By cryogenic distillation of NF3 in the coexistence of three components, such as helium ()le) gas, the NzO contained in
, Cot, Nt other than Nxh, ox, and other impurities can be removed, and it can be used as a semiconductor dry etching agent or CV
High purity NF suitable as cleaning gas for D device,
This makes it possible to easily obtain gas.
以下、実施例により本発明を更に具体的に説明する。尚
、以下において％及びｐｐｍは特記しない限り容量基準
を表す。Hereinafter, the present invention will be explained in more detail with reference to Examples. Note that in the following, % and ppm represent capacity standards unless otherwise specified.
実施例１〜４
内径１５ｍｍのステンレス製カラムに粒度が２４〜４８
メツシユの粒状シリカゲルを充填（充填高さ３００−）
シた後、シリカゲルの加熱による脱水処理並びにＮＦｓ
ガスの通気を、第１表に示す条件で行なった。Examples 1-4 Particle size 24-48 in a stainless steel column with an inner diameter of 15 mm
Filled with mesh granular silica gel (filling height 300-)
After drying, dehydration treatment by heating the silica gel and NFs
Gas ventilation was performed under the conditions shown in Table 1.
ＮＦ２ガスのシリカゲル層への通気前後のＮＦＩガスを
ガスクロマトグラフィーにて分析した。The NFI gas before and after the NF2 gas was introduced into the silica gel layer was analyzed by gas chromatography.
その結果は第１表に示す通りであり、本発明の方法で精
製すればＮｈガス中のＮｔＯ、Ｃｏｔ 、ＮｘＦｚは極
めて良好に除去される。またＮＦＳの損失もないことが
分かる。The results are shown in Table 1, and when purified by the method of the present invention, NtO, Cot, and NxFz in Nh gas can be removed extremely well. It can also be seen that there is no NFS loss.
比較例１〜６
実施例と同一のシリカゲルを充填したカラムを使用して
、第２表に示す条件でシリカゲルの加熱による脱水処理
と、ＮＰ、ガスの通気を行なった。Comparative Examples 1 to 6 Using a column filled with the same silica gel as in the example, dehydration treatment by heating the silica gel and aeration of NP and gas were performed under the conditions shown in Table 2.
結果を第２表に示すが、本発明で特定する条件（加熱温
度）で脱水処理したシリカゲルを使用しなければ、たと
え長時間脱水処理したシリカゲルでもＮｔＯ、Ｃｏｔ
、 Ｎｘｈの除去効果は不十分であることが分かる。ま
たＮＦ、ガスのシリカゲル層への通気温度が本発明で特
定する温度よりも高いと、ＮｔＯ、Ｃｏｔ及びＮ！Ｆ！
の除去率が極端に悪くなることが分かる。The results are shown in Table 2, but if silica gel that has been dehydrated under the conditions (heating temperature) specified in the present invention is not used, even silica gel that has been dehydrated for a long time will not contain NtO, Cot, etc.
, it can be seen that the removal effect of Nxh is insufficient. Furthermore, if the temperature at which NF and gas are introduced into the silica gel layer is higher than the temperature specified in the present invention, NtO, Cot and N! F!
It can be seen that the removal rate becomes extremely poor.
比較例７〜９
実施例及び比較例１〜６に用いたシリカゲルに代え、第
３表に示す各吸着剤を充填したカラムを用いて、ＮＦｓ
ガスの精製を試みた。カラムの形状、原料ＮＦｓガスは
実施例と同じものを使用した。Comparative Examples 7 to 9 Instead of the silica gel used in Examples and Comparative Examples 1 to 6, NFs
An attempt was made to purify the gas. The shape of the column and the raw material NFs gas were the same as in the example.
その結果は第３表に示す通り、本発明の脱水処理したシ
リカゲルを使用しないと、Ｎｈガス中のＮｚｏ 、 Ｃ
Ｏ，、Ｎ□Ｐｇの除去は何れも不完全であることが分か
る。The results are shown in Table 3. If the dehydrated silica gel of the present invention is not used, Nzo, C in Nh gas
It can be seen that the removal of O, N□Pg is incomplete.
第３表
参考例１（特願昭６２−１３８９７２号の方法）実施例
１でＮ、Ｏ、Ｃｏ□、ＮＪｘを除去されたＮＦＳガスを
、第１図に示す装置を用いて深冷蒸留により更に精製し
た。Table 3 Reference Example 1 (Method of Japanese Patent Application No. 138972/1982) The NFS gas from which N, O, Co□, and NJx were removed in Example 1 was subjected to deep cold distillation using the apparatus shown in It was further purified.
即ち液体窒素６を満たした保冷容器５中に容器ｌ（内容
積ｌｌ）を浸漬して容器１を冷却した後、該容器ｌに実
施例１で得られたＮＦ３ガスと第三成分としてＨｅガス
を、ライン２及び３を通して各５０ｄ／ｗｉｎ、 、３
ｍ／−ｉｎ、の流量で１０時間フィードした。That is, after cooling the container 1 by immersing it in a cold storage container 5 filled with liquid nitrogen 6, the NF3 gas obtained in Example 1 and He gas as the third component are added to the container 1. , 50d/win each through lines 2 and 3, , 3
It was fed for 10 hours at a flow rate of m/-in.
ＮＦ３ガスは容器１内で液化し、共存させたＨｅガス及
び分留したＮ、ガス等の不純物は水シール槽７を通して
排気させた。The NF3 gas was liquefied in the container 1, and the coexisting He gas and impurities such as fractionated N and gas were exhausted through the water seal tank 7.
ＮＦｓガス及びＨｅガスのフィード停止後、フィード答
弁１２及び水シール槽７に至る弁１６を閉じ弁１７を開
いて、真空ポンプ８にて容器１内のガスを排気しながら
、この液化させたＮＦｓガス中にＨｅガスを１００ ｄ
／ｍ１１１．の流量で３０分間フィードしバブリングさ
せた。この時の容器ｌ内の圧力は１０■謡Ｉｔ。After the feed of NFs gas and He gas is stopped, the feed valve 12 and the valve 16 leading to the water seal tank 7 are closed, the valve 17 is opened, and the liquefied NFs is pumped while exhausting the gas in the container 1 with the vacuum pump 8. 100 d of He gas in the gas
/m111. It was fed and bubbled for 30 minutes at a flow rate of . At this time, the pressure inside the container is 10.
ａｂｓ、にした、排気完了後、弁１３及び弁１５を閉じ
た後、容器１を常温に戻して容器ｌ内の液化ＮＦ３をガ
ス化して、ガスクロマトグラフィーにて分析した。After completing the evacuation and closing the valves 13 and 15, the container 1 was returned to room temperature, and the liquefied NF3 in the container 1 was gasified and analyzed by gas chromatography.
その結果は、Ｎ８、ＮｓＯ、Ｃｏｔ 、 Ｎ！Ｆ茸の含
有量は何れも１０ｐｐ−以下と極めて微量で、得られた
ＮＦＳガスは橿めて高純度であった。The results are N8, NsO, Cot, N! The content of F mushrooms was extremely small, less than 10 pp-, and the resulting NFS gas was highly pure.
本発明は以上詳細に説明したように、ＮＦ、ガス中のＮ
意０ 、ＧＯ！及びＮ！Ｆ！を除去をする方法において
、吸着剤として安価なシリカゲルを予め特定の温度に加
熱して脱水処理し、このシリカゲル層へ特定の温度でか
つ実質的に水分の混入しない状態で、Ｎｈガスを通気す
るという極めて簡単な方法であり、本発明の実施により
ＮＦ、ガス中のＮｔＯ。As explained in detail above, the present invention is based on NF, N in gas,
0 intention, GO! and N! F! In this method, silica gel, which is inexpensive as an adsorbent, is heated to a specific temperature in advance to dehydrate it, and Nh gas is bubbled through the silica gel layer at a specific temperature and in a state where substantially no moisture is mixed. This is an extremely simple method, and by implementing the present invention, NF, NtO in gas.
Ｃ０８及びＮｔｐｔが、効率よくかつ経済的に除去でき
るのである。また、本発明の方法は吸着剤であるシリカ
ゲルへのＮＦｓの吸着もない。C08 and Ntpt can be removed efficiently and economically. Furthermore, the method of the present invention does not involve adsorption of NFs to silica gel, which is an adsorbent.
更に、本発明の方法で精製したＮＰｓガスを、本発明者
が先に提案した特願昭和６２−１３８９７２号の方法で
更に精製すれば、参考例１が示す如く極めて高純度のＮ
Ｆ３ガスを得ることができるのである。Furthermore, if the NPs gas purified by the method of the present invention is further purified by the method of Japanese Patent Application No. 138972/1989 proposed by the present inventor, extremely high purity N can be obtained as shown in Reference Example 1.
F3 gas can be obtained.
尚、シリカゲルの加熱による脱水処理の際の加熱温度は
特に重要であり、比較例５及び６が示す如く本発明で特
定する温度未満での加熱では、この加熱が長時間でｚっ
でもｃｏ、、ＮｘＯ、ＮｔＦよを十分除去することは不
可能である。The heating temperature during the dehydration treatment of silica gel by heating is particularly important, and as shown in Comparative Examples 5 and 6, heating below the temperature specified in the present invention may result in co- , NxO, and NtF cannot be sufficiently removed.
第１図は参考例１で使用した深冷蒸留装置を示すフロー
シートである。
図において、
ｌ・・−・・・・・容器、
２−・・・−Ｎ Ｆ 、ガスフィードライン、３−・−
・−−−−−・・Ｈｅガスフィードライン、４・−・・
・・・−排気ライン、
５−・・−・−保冷容器、
６・・・・−・−・・・・液体窒素、
７−−−−−・−・・−水シール槽、
Ｂ−・・−・・−・・−真空ポンプ、
９−・・−・−・・・・常圧排気ライン、１０−−−・
−・・−真空排気ライン、１１・・−・−・・・−挿入
管、
１２．１３．１４．１５、
を示す。FIG. 1 is a flow sheet showing the cryogenic distillation apparatus used in Reference Example 1. In the figure, 1... Container, 2-...-NF, Gas feed line, 3-...-
・-------・He gas feed line, 4・-・・
...-Exhaust line, 5--Cold container, 6--Liquid nitrogen, 7--Water seal tank, B--・−・・−・・−Vacuum pump, 9−・・−・−・・Normal pressure exhaust line, 10−−−・
-...-Evacuation line, 11...--Insertion tube, 12.13.14.15, are shown.
Claims (1)
水処理したシリカゲル層へ、三弗化窒素ガスを０〜−１
２５℃の温度でかつ実質的に水分の混入しない状態で通
気させることを特徴とする三弗化窒素ガスの精製方法。(1) Add nitrogen trifluoride gas from 0 to -1 to the silica gel layer that has been heated to a temperature in the range of 150 to 300°C and dehydrated in advance.
A method for purifying nitrogen trifluoride gas, comprising aeration at a temperature of 25° C. and in a state substantially free of moisture.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30688088A JPH02153809A (en) | 1988-12-06 | 1988-12-06 | Purification of nitrogen trifluoride gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30688088A JPH02153809A (en) | 1988-12-06 | 1988-12-06 | Purification of nitrogen trifluoride gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02153809A true JPH02153809A (en) | 1990-06-13 |
Family
ID=17962359
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30688088A Pending JPH02153809A (en) | 1988-12-06 | 1988-12-06 | Purification of nitrogen trifluoride gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02153809A (en) |
-
1988
- 1988-12-06 JP JP30688088A patent/JPH02153809A/en active Pending
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