JPH04114910A - Production of nitrogen trifluoride gas - Google Patents
Production of nitrogen trifluoride gasInfo
- Publication number
- JPH04114910A JPH04114910A JP22795390A JP22795390A JPH04114910A JP H04114910 A JPH04114910 A JP H04114910A JP 22795390 A JP22795390 A JP 22795390A JP 22795390 A JP22795390 A JP 22795390A JP H04114910 A JPH04114910 A JP H04114910A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- liquefied
- heat exchanger
- storage tank
- 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 77
- 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 56
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 238000003860 storage Methods 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 10
- 238000009835 boiling Methods 0.000 abstract description 17
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000006260 foam Substances 0.000 abstract description 5
- 238000009413 insulation Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 13
- 239000003507 refrigerant Substances 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- UJMWVICAENGCRF-UHFFFAOYSA-N oxygen difluoride Chemical compound FOF UJMWVICAENGCRF-UHFFFAOYSA-N 0.000 description 3
- 229910000127 oxygen difluoride Inorganic materials 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- KVBCYCWRDBDGBG-UHFFFAOYSA-N azane;dihydrofluoride Chemical compound [NH4+].F.[F-] KVBCYCWRDBDGBG-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000001312 dry etching Methods 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 235000003270 potassium fluoride Nutrition 0.000 description 2
- 239000011698 potassium fluoride Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- DUQAODNTUBJRGF-UHFFFAOYSA-N difluorodiazene Chemical compound FN=NF DUQAODNTUBJRGF-UHFFFAOYSA-N 0.000 description 1
- DUQAODNTUBJRGF-ONEGZZNKSA-N dinitrogen difluoride Chemical compound F\N=N\F DUQAODNTUBJRGF-ONEGZZNKSA-N 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001512 metal fluoride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229960001730 nitrous oxide Drugs 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Landscapes
- Separation By Low-Temperature Treatments (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（ＮＦ３）ガスの製造方法に関する
。更に詳しくは、Ｎ１１４Ｆ−１１Ｆ系溶融塩の電解法
によるＮｈガスの製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for producing nitrogen trifluoride (NF3) gas. More specifically, the present invention relates to a method for producing Nh gas by electrolyzing N114F-11F-based molten salt.
（従来の技術及び発明が解決しようとする課題）ＮＦ３
は沸点が−１２９’Ｃ１融点が一２０７°Ｃの物性を示
す無色の化学的に安定な気体である。(Problems to be solved by conventional technology and invention) NF3
is a colorless chemically stable gas with a boiling point of -129'C and a melting point of 1207°C.
ＮＦ３ガスは半導体製造工程におけるドライエツチング
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ＮＦ３ガスは、高
純度のものが要求されている。NF3 gas has recently attracted attention as a dry etching agent in semiconductor manufacturing processes and as a cleaning gas for CVD equipment, but NF3 gas used for these purposes is required to be of high purity.
Ｎｌｉ、ｌガスは、種々の方法で製造される。たとえば
、アンモニウム酸弗化物の溶融塩を電解する方法、アン
モニウム酸弗化物を溶融状態において気相状の弗素と反
応させる方法、固体状の金属弗化物のアンモニウム錯体
と元素状弗素を反応させる方法、弗化アンモニウムまた
は酸性弗化アンモニウムと弗化水素を原料とするＮ１１
４Ｆ・ＩＩＦや、さらにこれに弗化カリウムまたは酸性
弗化カリウムを、該原料に加えたＫＦ −Ｎ１１４Ｆ・
ＩＩ＋’系での溶融塩電解法などがある。Nli,l gas is produced in various ways. For example, a method of electrolyzing a molten salt of ammonium acid fluoride, a method of reacting ammonium acid fluoride with gaseous fluorine in a molten state, a method of reacting an ammonium complex of a solid metal fluoride with elemental fluorine, N11 made from ammonium fluoride or acidic ammonium fluoride and hydrogen fluoride
4F・IIF and KF-N114F・IIF, which is made by adding potassium fluoride or acidic potassium fluoride to the raw material.
There is a molten salt electrolysis method using II+' system.
しかしながら、何れの方法で得られたガスも殆どの場合
、窒素（Ｎ２）、酸素（０□）、ニフッ化酸素（ＯＦ２
） 、−酸化二窒素（Ｎ２０） 、二酸化炭素（ＣＯ２
）、ニフッ化二窒素（Ｎ２Ｐ２）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
ｆｆガスを得るためには精製が必要である。However, in most cases, the gases obtained by either method are nitrogen (N2), oxygen (0□), or oxygen difluoride (OF2).
), - dinitrogen oxide (N20), carbon dioxide (CO2
), contains relatively large amounts of impurities such as dinitrogen difluoride (N2P2), so it is difficult to use high-purity NF for the above applications.
Purification is necessary to obtain ff gas.
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、下記する方法が知られている。As a purification method for removing these impurities from NF3 gas, the following method is known.
即ち、１）Ｎ２Ｆ２はＫｌ、ＮａｚＳ、 Ｎａ２Ｓ２Ｏ
３等の水？＠液と接触させる方法［Ｊ、 Ｍａｓｓｏｎ
ｎｅ、ケミー°インジェニュール・テヒニール（Ｃｈｅ
ｍ、 Ｉｎｇ、 Ｔｅｃｈｒｌ、）４１（１２）、６９
５．（１９６９） ）や１．１８．９〜５３７．１１１
°Ｃの温度で金属と接触させる方法（特公昭５９−１５
０８１号）等で除去することができる。２）ＯＦ２は、
Ｎａ２５ｚ０３、Ｋｌ、Ｎａ２５Ｏ，、ＩＩＬ Ｎａｚ
Ｓ等の水溶液と接触させる方法で除去することができる
。３）Ｎ２０やＣＯ□等のような比較的高沸点の成分は
ゼオライト等の吸着剤と接触させることで効率よく除去
することができる（Ｃｈｅｍ、 Ｅｎｇ、、 ８４．１
１６． （１９７７）等〕。That is, 1) N2F2 is Kl, NazS, Na2S2O
Third class water? @Method of contacting with liquid [J, Masson
ne, Chemie
m, Ing, Techrl, ) 41(12), 69
5. (1969)) and 1.18.9-537.111
Method of contacting metal at a temperature of °C (Special Publication Publication No. 59-15
081) etc. 2) OF2 is
Na25z03, Kl, Na25O,, IIL Naz
It can be removed by contacting with an aqueous solution such as S. 3) Relatively high boiling point components such as N20 and CO□ can be efficiently removed by contacting with an adsorbent such as zeolite (Chem, Eng, 84.1)
16. (1977) etc.].
一方、Ｎ２．０□等の低沸点成分は、ＮＦ３ガスが組成
の主体であるために反応あるいは吸着を利用して除去す
る方法には限界があり、高純度のＮｈガスを得る方法と
しては好ましくない。また、Ｎ２は液化ＮＦ３ との親
和性が強いため、一般には−１５０〜−１９０’Ｃの温
度に冷却してＮＦ３ガスを液化状態とし、更に真空排気
を行なうことでＮ２．０□の除去を行なっていた。On the other hand, since NF3 gas is the main component of the composition of low-boiling components such as N2.0□, there are limits to how to remove them using reaction or adsorption, and this is the preferred method for obtaining high-purity Nh gas. do not have. In addition, since N2 has a strong affinity with liquefied NF3, it is generally cooled to a temperature of -150 to -190'C to liquefy the NF3 gas, and then vacuumed to remove N2.0□. I was doing it.
しかしながら、上記の方法においてもＮ２．０゜は高純
度ＮＦ：ｌガスの品質を満足できるほどには除去できな
かった。また、真空排気を伴うため、除去作業中にＮＦ
３ガスを供給し処理することば困難であり、必然的にパ
ンチ運転とならざるを得す、工程および作業が複雑にな
る等の問題を有している。However, even in the above method, N2.0° could not be removed to a level that would satisfy the quality of high-purity NF:l gas. In addition, since vacuum evacuation is involved, NF
It is difficult to supply and process three gases, and there are problems such as a punch operation is inevitably required, and the process and work become complicated.
（課題を解決するための手段）
本発明者等はかかる状況に鑑み、鋭意検討を重ねた結果
、逆流凝縮器にＮＦ３ガスを供給し、連続的にＮＦ３ガ
スの液化処理ができると共に、該逆流凝縮器に接続され
た液化ＮＦ、の貯槽に、該逆流凝縮器で液化させたＮＦ
、ｌを貯液し、更に該貯槽内の液化ＮＰ３を沸騰状態と
し、該逆流凝縮器でＮＦ、ａガスを還流させることによ
り、Ｎ２．０２等の低沸点成分を除去できることを見い
だし、本発明を完成するに至ったものである。(Means for Solving the Problems) In view of the above situation, the inventors of the present invention have made extensive studies and found that it is possible to continuously liquefy NF3 gas by supplying NF3 gas to a backflow condenser, and to The liquefied NF connected to the condenser is stored in the liquefied NF storage tank.
, 1, and further brought the liquefied NP3 in the storage tank to a boiling state, and refluxed the NF and a gases in the reverse flow condenser, it was found that low boiling point components such as N2.02 could be removed, and the present invention This is what we have come to complete.
即ち、本発明は三弗化窒素ガスの製造に於いて、三弗化
窒素ガス凝縮用熱交換器とこれに接続された液体三弗化
窒素の貯槽からなる装置を用いて三弗化窒素を捕集およ
び／または貯蔵することを特徴とする三弗化窒素の製造
方法である。That is, in the production of nitrogen trifluoride gas, the present invention uses a device consisting of a heat exchanger for condensing nitrogen trifluoride gas and a storage tank for liquid nitrogen trifluoride connected to the heat exchanger. This is a method for producing nitrogen trifluoride, which includes collection and/or storage.
（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.
上記した通り、ＮＦ３ガスは、種々の方法で製造される
ものであるが、本発明はその製造方法の種類を選ばない
ことはもとより、本発明の実施以前の態様がどの様なも
のであっても実施可能である。As mentioned above, NF3 gas can be produced by various methods, but the present invention is not limited to any type of production method, and is applicable to any embodiment prior to implementation of the present invention. is also possible.
次に本発明で用いるＮＦ、ガス凝縮用熱交換器１並びに
液化ＮＦ３貯槽２について説明する。Next, the NF, gas condensing heat exchanger 1 and liquefied NF3 storage tank 2 used in the present invention will be explained.
ＮＦ３ガス凝縮用熱交換器１のプロセス側の一端は、液
化ＮＦ３貯槽２に接続され、液化ＮＦ、ガス抜き出し口
３が設けられている。該ＮＦ３ガス凝縮用熱交換器１で
凝縮したＮＦ３が該液化ＮＦ３貯槽２に容易に流入でき
る配置および構造となっていることが好ましい。また該
ＮＦ３ガス凝縮用熱交換器１の他端からはＮＦ３ガス中
に含まれる低沸点成分が排出されるため、低沸点成分排
気口４が設けられ排出を妨げない構造となっている必要
がある。One end on the process side of the NF3 gas condensing heat exchanger 1 is connected to a liquefied NF3 storage tank 2, and is provided with a liquefied NF and gas extraction port 3. Preferably, the arrangement and structure are such that the NF3 condensed in the NF3 gas condensing heat exchanger 1 can easily flow into the liquefied NF3 storage tank 2. Furthermore, since the low boiling point components contained in the NF3 gas are discharged from the other end of the NF3 gas condensing heat exchanger 1, it is necessary to have a structure in which a low boiling point component exhaust port 4 is provided so that the discharge is not obstructed. be.
般的には大気放出することで問題はないが、空気が逆流
して該ＮＦ３ガス凝縮用熱交換器１側に流入することの
ない様、水銀等でガスシール５を施すことが好ましい。Generally speaking, there is no problem with releasing the gas into the atmosphere, but it is preferable to provide a gas seal 5 with mercury or the like to prevent air from flowing backward into the NF3 gas condensing heat exchanger 1 side.
ここで使用するＮＦ３ガス凝縮用熱交換器１は多管式熱
交換器が好ましい。The NF3 gas condensing heat exchanger 1 used here is preferably a shell-and-tube heat exchanger.
該液化ＮＦ３貯槽２の外部は、ウレタンフオーム６等の
保冷材で覆うが、ＮＦ３が沸騰状態となるよう若干の熱
流入が必要であるため、完全な保冷である必要はない。The outside of the liquefied NF3 storage tank 2 is covered with a cold insulating material such as urethane foam 6, but it does not need to be completely cold insulated since a slight amount of heat is required to bring the NF3 to a boiling state.
保冷の程度は、該Ｎｈガス凝縮用熱交換器１の能力によ
り適宜選択されるものである。これらにより、ＮＦ３ガ
スの還流が可能となる。尚、ＮＦ３ガスの還流を必要と
しない捕集および／または貯蔵においては、デユワ−瓶
の如く真空二重構造の貯槽とする等、強力な保冷を行う
ことは差し支えない。The degree of cold storage is appropriately selected depending on the capacity of the Nh gas condensing heat exchanger 1. These enable reflux of NF3 gas. In addition, for collection and/or storage that does not require reflux of NF3 gas, strong cold storage may be used, such as in a vacuum double-structured storage tank such as a dewar bottle.
外部からの該ＮＦ３ガス凝縮用熱交換器１へのＮＦ。NF from the outside to the heat exchanger 1 for condensing the NF3 gas.
ガスの供給は、ＮＦｆｌ貯槽に接続されたＮｌ’、ｌガ
ス供給ロアより行なう。これによりＮＦ３ガス中に含ま
れる低沸点成分の大部分は除去された後、該液化ＮＦ３
貯槽２に溜るのである。Gas is supplied from the Nl',l gas supply lower connected to the NFfl storage tank. As a result, most of the low boiling point components contained in the NF3 gas are removed, and then the liquefied NF3
It accumulates in storage tank 2.
該ＮＦ３ガス凝縮用熱交換器１の共役側には冷媒が供給
され、冷媒供給口８及び冷媒排出口９が設けられている
。冷媒としては液体空気（−１８６〜１９６°Ｃ）、液
体窒素（−１，９６°Ｃ）の他、液体窒素などで任意の
温度に冷却した石油エーテル等を用いることも可能であ
る。しかし、−ｇには取り扱い等が容易な液体窒素が冷
媒として使用される。A refrigerant is supplied to the conjugate side of the NF3 gas condensing heat exchanger 1, and a refrigerant supply port 8 and a refrigerant discharge port 9 are provided. As the refrigerant, in addition to liquid air (-186 to 196°C) and liquid nitrogen (-1.96°C), it is also possible to use petroleum ether cooled to an arbitrary temperature with liquid nitrogen or the like. However, liquid nitrogen, which is easy to handle, is used as a refrigerant for -g.
捕集されたＮＦ３ガスは液化ＮＦｉ貯槽２から抜き出さ
れる。具体的には、気相部より圧縮器を用いて抜き出す
か、あるいは液化ＮＰ、貯槽２下部より液化状態でＮＦ
、を抜き出される。その後、ボンベに充填されるか、あ
るいは引き続き何らかの工程に移される。The collected NF3 gas is extracted from the liquefied NFi storage tank 2. Specifically, the method is to extract liquefied NP from the gas phase using a compressor, or extract NF in a liquefied state from the lower part of the storage tank 2.
, is extracted. It is then filled into cylinders or transferred to some subsequent process.
尚、ボンベに充填されたものは、上記した通り、半導体
製造工程に於いて、ドライエツチングガスあるいはＣｖ
Ｄチャンバーのクリーニングガスとして使用される。As mentioned above, the cylinder is filled with dry etching gas or Cv during the semiconductor manufacturing process.
Used as a cleaning gas for the D chamber.
（実施例）
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％、ｐｐｍは特記しない限り容量基準を
表わす。(Example) 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
第１図に示す装置を使用して、低沸点成分を含有するＮ
Ｆ、ガスを捕集した。装置は伝熱面積２ｍ２を有するＮ
Ｆ、ガス凝縮用熱交換器１とその一端には厚さ約１０ｃ
ｍのウレタンフオームで覆われた容量約２０Ｅの液化Ｎ
Ｆ、貯槽２が接続されている。Example 1 Using the apparatus shown in FIG.
F. Gas was collected. The device has a heat transfer area of 2 m2
F. Heat exchanger 1 for gas condensation and one end thereof has a thickness of approximately 10 cm.
Liquefied N with a capacity of about 20E covered with m urethane foam
F. Storage tank 2 is connected.
まず、ＮＦ、ｌガス凝縮用熱交換器１の共役側には、温
度調節器で制御しながら圧力約５ ｋｇ／ｃｍ２の液体
窒素を供給し、該ＮＦｆｆガス凝縮用熱交換器の温度を
一１８０°Ｃに保持した。First, liquid nitrogen at a pressure of approximately 5 kg/cm2 is supplied to the conjugate side of the NFff gas condensing heat exchanger 1 while being controlled by a temperature controller, and the temperature of the NFff gas condensing heat exchanger 1 is kept constant. It was maintained at 180°C.
次に不純物としてＮ２ガスを約２０％、０□ガスを約１
％含有するＮＦ３ガスを５℃／ｍｉｎにて外部ＮＦ３ガ
ス供給ロアより６時間供給し、約５ｋｇのＮＦ３ガスを
液化捕集した。Next, as impurities, add about 20% N2 gas and about 1% 0□ gas.
% containing NF3 gas was supplied from an external NF3 gas supply lower at 5° C./min for 6 hours, and about 5 kg of NF3 gas was liquefied and collected.
この間、液化ＮＦ３貯槽２低部付近に設置された温度計
は、常時、ＮＦ３の沸点である一１２９°Ｃを指示した
。また、ＮＦ３ガス凝縮用熱交換器１から大気に放出さ
れるガスを採取し分析したところ、はぼ全量が窒素およ
び酸素であった。During this time, the thermometer installed near the bottom of the liquefied NF3 storage tank 2 constantly indicated -129°C, which is the boiling point of NF3. Further, when the gas released into the atmosphere from the NF3 gas condensing heat exchanger 1 was sampled and analyzed, it was found that almost the entire amount was nitrogen and oxygen.
次に液化ＮＦ、貯槽２のＮＦ３ガス抜き出し口１ｏよリ
ガスを抜き出し、ガスクロマトグラフィーにて分析を行
なったところ、Ｎ２ガスは約２０ ｐｐｍ、 ０２ガス
は５ ｐｐｍであった。Next, the liquefied NF and regas were extracted from the NF3 gas outlet 1o of the storage tank 2, and analyzed by gas chromatography, and the amount of N2 gas was about 20 ppm, and the amount of 02 gas was 5 ppm.
実施例２
実施例１において用いた不純物を含有するＮＦ３ガスを
連続して７時間供給し、供給開始から５時間後に液化Ｎ
Ｆ３貯槽２の低部より液化ＮＦ、をボンベに少量抜き出
し、気化後、ガスクロマトグラフィーにて分析を行なっ
た他は実施例１と同様な方法で行なった。Example 2 The impurity-containing NF3 gas used in Example 1 was continuously supplied for 7 hours, and liquefied N was added 5 hours after the start of supply.
A small amount of liquefied NF was drawn out into a cylinder from the lower part of the F3 storage tank 2, and the same method as in Example 1 was conducted except that after vaporization, analysis was performed by gas chromatography.
その結果Ｎ２ガスは約２５ ｐｐｍ、０□ガスは５ ｐ
ｐＩｎであった。As a result, N2 gas is about 25 ppm, 0□ gas is 5 p
It was pIn.
比較例１
実施例１における装置において液化ＮＰ３貯槽２のウレ
タンフオームを外し、該液化ＮＦ、３貯槽２を液体窒素
を満たしたデユワ−瓶に浸した他は実施例１と同様に行
なった。Comparative Example 1 The same procedure as in Example 1 was carried out, except that the urethane foam of the liquefied NP3 storage tank 2 was removed from the apparatus in Example 1, and the liquefied NF3 storage tank 2 was immersed in a dewar bottle filled with liquid nitrogen.
その結果、Ｎ２ガスは約２８０１＋ｐｍ 、０２ガスは
１２０ｐｐｍであった。As a result, the N2 gas was approximately 2801+pm, and the 02 gas was 120 ppm.
（発明の効果）
従来行なっていたＮＦ、ガスの液化と真空排気の組合せ
では、低沸点成分の除去は満足できるものではなかった
。さらに真空排気中はＮＦ３ガスの液化捕集ができない
ため、ガスの捕集はバッチ運転とならざるを得す、連続
でガス捕集を行なう場合は捕集設備を２系列以上設ける
必要があった。(Effects of the Invention) The conventional combination of liquefaction of NF and gas and vacuum evacuation has not been able to satisfactorily remove low boiling point components. Furthermore, since liquefied NF3 gas cannot be collected during vacuum evacuation, gas collection has to be done in batch operation, and if gas collection is to be performed continuously, it is necessary to install two or more collection equipment lines. .
しかし、本発明によっては液化ＮＦ、を沸騰状態とする
ことで低沸点成分が効率的に除去されるため、従来法と
比較して捕集後のＮＦ３に含まれる０□、Ｎ２の含有量
は著しく減少する。さらに連続でガスを捕集、精製でき
る利点も有している。However, according to the present invention, low boiling point components are efficiently removed by bringing the liquefied NF to a boiling state, so the content of 0□ and N2 contained in the collected NF3 is lower than that in the conventional method. significantly reduced. It also has the advantage of being able to continuously collect and purify gas.
第１図は実施例及び比較例で使用したＮＦ、凝縮用熱交
換器、液化ＮＦ３凝縮器を示す図である。
図において、
１−一−ＮＰ、ガス凝縮用熱交換器
２−−−液化ＮＦ３貯槽
３−−−液化ＮＦ３ガス抜き出しロ
４−−−低沸点成分排気口
ガスジール
ウレタンフオーム
ＮＦｓガス供給口
冷媒供給口
冷媒排出口
Ｏ
ＮＦ、ガス抜き出し口
を示す。FIG. 1 is a diagram showing NF, a condensing heat exchanger, and a liquefied NF3 condenser used in Examples and Comparative Examples. In the figure, 1-1-NP, heat exchanger for gas condensation 2 --- Liquefied NF3 storage tank 3 --- Liquefied NF3 gas extraction hole 4 --- Low boiling point component exhaust port Gas Zeal urethane foam NFs gas supply port Refrigerant supply Refrigerant outlet O NF indicates gas extraction port.
Claims (1)
縮用熱交換器と、該三弗化窒素ガス凝縮用熱交換器に接
続された、液体三弗化窒素の貯槽からなる装置を用いて
、三弗化窒素ガスを捕集および／または貯蔵することを
特徴とする三弗化窒素ガスの製造方法。1) In the production of nitrogen trifluoride gas, it consists of a heat exchanger for condensing nitrogen trifluoride gas and a storage tank for liquid nitrogen trifluoride connected to the heat exchanger for condensing nitrogen trifluoride gas. A method for producing nitrogen trifluoride gas, which comprises collecting and/or storing nitrogen trifluoride gas using an apparatus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22795390A JP2927914B2 (en) | 1990-08-31 | 1990-08-31 | Method for producing nitrogen trifluoride gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22795390A JP2927914B2 (en) | 1990-08-31 | 1990-08-31 | Method for producing nitrogen trifluoride gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04114910A true JPH04114910A (en) | 1992-04-15 |
| JP2927914B2 JP2927914B2 (en) | 1999-07-28 |
Family
ID=16868855
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22795390A Expired - Lifetime JP2927914B2 (en) | 1990-08-31 | 1990-08-31 | Method for producing nitrogen trifluoride gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2927914B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460745C (en) * | 2005-06-14 | 2009-02-11 | 株式会社厚成 | Method of storing nitrogen trifluoride |
-
1990
- 1990-08-31 JP JP22795390A patent/JP2927914B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100460745C (en) * | 2005-06-14 | 2009-02-11 | 株式会社厚成 | Method of storing nitrogen trifluoride |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2927914B2 (en) | 1999-07-28 |
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