JP2002363113A - Method and apparatus for separating and recovering perfluoro compound gas - Google Patents
Method and apparatus for separating and recovering perfluoro compound gasInfo
- Publication number
- JP2002363113A JP2002363113A JP2001165872A JP2001165872A JP2002363113A JP 2002363113 A JP2002363113 A JP 2002363113A JP 2001165872 A JP2001165872 A JP 2001165872A JP 2001165872 A JP2001165872 A JP 2001165872A JP 2002363113 A JP2002363113 A JP 2002363113A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- gas mixture
- separation
- perfluoro compound
- carbon membrane
- 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
- -1 perfluoro compound Chemical class 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000000926 separation method Methods 0.000 claims abstract description 105
- 239000000203 mixture Substances 0.000 claims abstract description 83
- 239000012528 membrane Substances 0.000 claims abstract description 78
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 238000011084 recovery Methods 0.000 claims description 33
- 229910052731 fluorine Inorganic materials 0.000 claims description 21
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 20
- 239000011737 fluorine Substances 0.000 claims description 20
- 238000001179 sorption measurement Methods 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 7
- 230000005494 condensation Effects 0.000 claims description 7
- 238000011144 upstream manufacturing Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 description 150
- 238000010521 absorption reaction Methods 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 229920000620 organic polymer Polymers 0.000 description 6
- 239000012466 permeate Substances 0.000 description 6
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 239000002250 absorbent Substances 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000006866 deterioration Effects 0.000 description 3
- 230000002542 deteriorative effect Effects 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 239000004642 Polyimide Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 238000010000 carbonizing Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000012510 hollow fiber Substances 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 229920002492 poly(sulfone) Polymers 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
- Y02P20/155—Perfluorocarbons [PFC]; Hydrofluorocarbons [HFC]; Hydrochlorofluorocarbons [HCFC]; Chlorofluorocarbons [CFC]
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Drying Of Gases (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、半導体製造などに
おいて用いられるＣＦ4、Ｃ2Ｆ6、Ｃ3Ｆ8、Ｃ4Ｆ 10、Ｓ
Ｆ6、ＮＦ3などのパーフルオロ化合物ガスを分離回収す
る方法および装置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention
CF used inFour, CTwoF6, CThreeF8, CFourF Ten, S
F6, NFThreeSeparation and recovery of perfluoro compound gas such as
Method and apparatus.
【０００２】[0002]
【従来の技術】半導体製造などにおいては、エッチン
グ、洗浄等の工程に、ＣＦ4、Ｃ2Ｆ6、Ｃ3Ｆ8、Ｃ
4Ｆ10、ＳＦ6、ＮＦ3などのパーフルオロ化合物ガスが
用いられている。またガス絶縁開閉装置などのガス絶縁
電気機器には、電気絶縁ガスとしてパーフルオロ化合物
ガスが用いられることがある。パーフルオロ化合物ガス
は、地球環境に対し有害なガス（例えば温室効果ガス）
となり得ることが指摘されている。このため、半導体製
造工程などから排出されるガス中に含まれるパーフルオ
ロ化合物ガスを分離回収し、再利用することが行われて
いる。特開平９−１０３６３３号公報、および特開平１
０−１２８０３４号公報には、排出ガス中のパーフルオ
ロ化合物ガスを、有機高分子（ポリスルホン等）膜を用
いた膜分離により分離回収する方法が記載されている。2. Description of the Related Art In semiconductor manufacturing and the like, CF 4 , C 2 F 6 , C 3 F 8 , C 3
4 F 10, perfluoro compound gas such as SF 6, NF 3 is used. In some gas-insulated electric devices such as gas-insulated switchgear, perfluoro compound gas is used as an electric insulating gas. Perfluoro compound gas is a gas harmful to the global environment (for example, greenhouse gas)
It has been pointed out that For this reason, a perfluoro compound gas contained in a gas discharged from a semiconductor manufacturing process or the like is separated and collected, and is reused. JP-A-9-103633 and JP-A-9-103633
Japanese Patent Application Publication No. 0-128034 describes a method for separating and recovering a perfluoro compound gas in an exhaust gas by membrane separation using an organic polymer (such as polysulfone) membrane.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、上記有
機高分子膜を用いた分離回収方法では、パーフルオロ化
合物ガスの回収率が不十分となることがあった。このた
め、パーフルオロ化合物ガスの分離性能に優れた炭素膜
を用いた分離回収方法が提案されている。例えば、特開
２０００−１８５２１２号公報には、有機高分子膜を熱
処理により炭素化して得られた炭素膜を用いて、ガス混
合物からパーフルオロ化合物ガスを分離回収する方法が
開示されている。しかしながら、炭素膜を用いる場合に
は、ガス透過量が変動しやすく、パーフルオロ化合物ガ
スの回収率が低下することがあった。本発明は、上記事
情に鑑みてなされたもので、パーフルオロ化合物ガスを
より効率よく分離回収することができる分離回収方法お
よび装置を提供することを目的とする。However, in the separation and recovery method using the organic polymer membrane, the recovery rate of the perfluoro compound gas may be insufficient. For this reason, a separation and recovery method using a carbon membrane excellent in perfluoro compound gas separation performance has been proposed. For example, JP-A-2000-185212 discloses a method of separating and recovering a perfluoro compound gas from a gas mixture using a carbon film obtained by carbonizing an organic polymer film by heat treatment. However, when a carbon membrane is used, the amount of gas permeation tends to fluctuate, and the recovery of the perfluoro compound gas may decrease. The present invention has been made in view of the above circumstances, and it is an object of the present invention to provide a method and an apparatus for separating and recovering a perfluoro compound gas more efficiently.
【０００４】[0004]
【課題を解決するための手段】本発明者は、炭素膜を用
いる場合に起きるガス透過量の変動が、ガス中の水分に
より炭素膜の透過特性が劣化することに起因することを
見出し、この知見に基づいて本発明を完成した。本発明
のパーフルオロ化合物ガスの分離回収方法は、パーフル
オロ化合物ガスを含むガス混合物を炭素膜分離手段に供
給するに先だって、ガス混合物中の水分を除去すること
を特徴とする。これによって、ガス混合物中の水分濃度
を低くし、水の付着により炭素膜のガス透過特性が劣化
するのを防ぎ、炭素膜分離手段におけるガス透過流量を
高く維持することができる。従って、ガス混合物中のパ
ーフルオロ化合物ガスを効率よく分離回収することがで
きる。ガス混合物中の水分を除去する方法としては、膜
分離、吸着分離、および凝縮分離のうち少なくとも１つ
を用いるのが好ましい。またガス混合物を炭素膜分離手
段に供給するに先だって、ガス混合物中の反応性フッ素
系ガスを除去するのが好ましい。Means for Solving the Problems The present inventor has found that a change in the amount of gas permeation that occurs when a carbon film is used is caused by deterioration of the permeation characteristics of the carbon film due to moisture in the gas. The present invention has been completed based on the findings. The method for separating and recovering a perfluoro compound gas of the present invention is characterized in that moisture in the gas mixture is removed before supplying the gas mixture containing the perfluoro compound gas to the carbon membrane separation means. This makes it possible to reduce the water concentration in the gas mixture, prevent the gas permeation characteristics of the carbon membrane from deteriorating due to the adhesion of water, and maintain a high gas permeation flow rate in the carbon membrane separation means. Therefore, the perfluoro compound gas in the gas mixture can be efficiently separated and recovered. As a method for removing moisture in the gas mixture, it is preferable to use at least one of membrane separation, adsorption separation, and condensation separation. It is preferable to remove the reactive fluorine-based gas in the gas mixture before supplying the gas mixture to the carbon membrane separation means.
【０００５】本発明のパーフルオロ化合物ガスの分離回
収装置は、パーフルオロ化合物ガスを含むガス混合物中
のパーフルオロ化合物ガスを、炭素膜を用いて分離回収
する炭素膜分離手段を備え、この炭素膜分離手段の上流
側に、ガス混合物中の水分を除去する水分除去手段が設
けられていることを特徴とする。水分除去手段は、膜分
離、吸着分離、および凝縮分離のうち少なくとも１つに
よりガス混合物中の水分を除去することができるもので
あることが好ましい。本発明では、炭素膜分離手段の上
流側に、ガス混合物中の反応性フッ素系ガスを除去する
反応性フッ素系ガス除去手段が設けるのが好ましい。The apparatus for separating and recovering a perfluoro compound gas of the present invention is provided with a carbon film separation means for separating and recovering a perfluoro compound gas in a gas mixture containing the perfluoro compound gas using a carbon film. A moisture removing means for removing moisture in the gas mixture is provided upstream of the separating means. It is preferable that the water removing means can remove water in the gas mixture by at least one of membrane separation, adsorption separation, and condensation separation. In the present invention, it is preferable that a reactive fluorine-based gas removing unit that removes a reactive fluorine-based gas in the gas mixture be provided upstream of the carbon membrane separation unit.
【０００６】[0006]
【発明の実施の形態】図１は、本発明のパーフルオロ化
合物ガスの分離回収装置の第１の実施形態を示すもので
ある。ここに示す分離回収装置１は、パーフルオロ化合
物ガスを含むガス混合物を圧縮する圧縮ユニット２と、
圧縮ユニット２を経たガス混合物中の水分を除去する水
分除去手段３と、水分除去手段３を経たガス混合物中の
パーフルオロ化合物ガスを回収する膜分離ユニット４と
を備えている。FIG. 1 shows a first embodiment of an apparatus for separating and recovering a perfluoro compound gas according to the present invention. The separation and recovery apparatus 1 shown here includes a compression unit 2 that compresses a gas mixture containing a perfluoro compound gas,
The apparatus includes a water removing unit 3 that removes moisture in the gas mixture that has passed through the compression unit 2, and a membrane separation unit 4 that recovers a perfluoro compound gas in the gas mixture that has passed through the moisture removing unit 3.
【０００７】圧縮ユニット２は、ガス混合物を貯留する
貯留タンク５と、貯留タンク５からのガス混合物を圧縮
する圧縮機６とを備えている。The compression unit 2 has a storage tank 5 for storing a gas mixture and a compressor 6 for compressing the gas mixture from the storage tank 5.
【０００８】本実施形態の分離回収装置１において、水
分除去手段３としては、膜分離によりガス混合物中の水
分を除去することができるものを用いることができる。
具体的には、水分を透過し、かつパーフルオロ化合物ガ
スを透過しない分離膜を用いたものが好適である。この
分離膜としては、ポリイミド、ポリスルホンなどからな
る有機高分子材料からなるものを例示できる。In the separation and recovery apparatus 1 of the present embodiment, as the water removing means 3, a means capable of removing the water in the gas mixture by membrane separation can be used.
Specifically, it is preferable to use a separation membrane that transmits moisture and does not transmit a perfluoro compound gas. Examples of the separation membrane include those made of an organic polymer material such as polyimide and polysulfone.
【０００９】水分除去手段３としては、吸着分離により
ガス混合物中の水分を除去することができるものを用い
ることもできる。具体的には、シリカ、アルミナゲル、
モレキュラーシーブなどの水分吸着剤からなる水分吸着
層を外筒内に備えたものを例示できる。As the water removing means 3, a means capable of removing the water in the gas mixture by adsorption separation may be used. Specifically, silica, alumina gel,
An example in which a water adsorption layer made of a water adsorbent such as molecular sieve is provided in an outer cylinder can be exemplified.
【００１０】水分除去手段３としては、凝縮分離により
ガス混合物中の水分を除去することができるものを用い
ることもできる。具体的には、ガス混合物を冷却する冷
却手段と、冷却により凝縮または凝固した水分をガス成
分から分離する水分分離手段とを備えたものが好適であ
る。As the water removing means 3, a means capable of removing the water in the gas mixture by condensation and separation can be used. Specifically, it is preferable to use a device provided with a cooling means for cooling a gas mixture and a water separating means for separating water condensed or solidified by cooling from gas components.
【００１１】水分除去手段３は、上記膜分離、吸着分
離、および凝縮分離のうち２つ以上によりガス混合物中
の水分を除去することができる構成とすることもでき
る。The water removing means 3 may be configured to be capable of removing water in the gas mixture by two or more of the above-mentioned membrane separation, adsorption separation, and condensation separation.
【００１２】膜分離ユニット４は、水分除去手段３を経
たガス混合物中のパーフルオロ化合物ガスを分離回収す
る第１および第２炭素膜分離部（炭素膜分離手段）７、
８を備えている。The membrane separation unit 4 includes first and second carbon membrane separation units (carbon membrane separation means) 7 for separating and recovering the perfluoro compound gas in the gas mixture that has passed through the water removing means 3.
8 is provided.
【００１３】第１および第２炭素膜分離部７、８として
は、有機高分子材料（ポリイミド、ポリピロロン、ポリ
アクリロニトリル等）からなる膜を、熱処理により炭素
化して得られた炭素膜を備えたものが好適である。この
炭素膜としては、上記有機高分子材料からなる膜を、不
活性ガス（窒素等）雰囲気下において５００〜９００℃
で熱処理し、少なくとも一部を炭素化したものを用いる
ことができる。炭素膜分離部７、８の炭素膜の形状は、
中空糸状、管状、スパイラル状などとすることができ
る。炭素膜分離部７、８では、中空糸状、管状などの炭
素膜の内側から外側へガスを透過させる内圧型構造を採
用してもよいし、炭素膜の外側から内側へガスを透過さ
せる外圧型構造を採用してもよい。Each of the first and second carbon film separating sections 7 and 8 is provided with a carbon film obtained by carbonizing a film made of an organic polymer material (polyimide, polypyrrololone, polyacrylonitrile, etc.) by heat treatment. Is preferred. As the carbon film, a film made of the above organic polymer material is formed at 500 to 900 ° C. in an inert gas (nitrogen or the like) atmosphere.
And at least a part thereof is carbonized. The shape of the carbon membrane of the carbon membrane separation units 7 and 8 is as follows:
It can be in the form of a hollow fiber, a tube, a spiral, or the like. The carbon membrane separation units 7 and 8 may employ an internal pressure type structure that allows gas to permeate from the inside to the outside of the carbon membrane, such as a hollow fiber or a tube, or an external pressure type structure that allows gas to permeate from the outside to the inside of the carbon membrane. A structure may be adopted.
【００１４】次に、図１に示す分離回収装置１を用いた
場合を例として、本発明の分離回収方法の第１の実施形
態を説明する。本実施形態の分離回収方法の対象となる
ガス混合物としては、半導体製造工程などからの排出さ
れ、パーフルオロ化合物ガスを含むガス混合物を例示で
きる。例えば、パーフルオロ化合物ガス（ＣＦ4、Ｃ2Ｆ
6、Ｃ3Ｆ8、Ｃ4Ｆ10、ＳＦ6、ＮＦ3など）と不活性ガス
（窒素ガス等）との混合ガスを例示できる。このガス混
合物を、管路１１を通して貯留タンク５に導入する。こ
の際、大気を管路１２を通して貯留タンク５に導入する
こともできる。Next, a first embodiment of the separation and recovery method of the present invention will be described by taking as an example the case where the separation and recovery apparatus 1 shown in FIG. 1 is used. Examples of the gas mixture to be subjected to the separation and recovery method of the present embodiment include a gas mixture discharged from a semiconductor manufacturing process or the like and containing a perfluoro compound gas. For example, a perfluoro compound gas (CF 4 , C 2 F
6 , C 3 F 8 , C 4 F 10 , SF 6 , NF 3, etc.) and an inert gas (nitrogen gas, etc.). This gas mixture is introduced into the storage tank 5 through the line 11. At this time, the atmosphere can be introduced into the storage tank 5 through the pipe 12.
【００１５】次いで、貯留タンク５内のガス混合物を、
管路１３を通して圧縮機６に導入し、圧縮機６において
圧縮した後、管路１４を通して水分除去手段３に導入す
る。水分除去手段３では、ガス混合物中の水分を、膜分
離、吸着分離、凝縮分離等により除去する。この水分除
去にあたっては、ガス混合物の露点が−４０℃以下（好
ましくは−６０℃以下）となるようにするのが好まし
い。この露点がこの範囲を越えると、炭素膜分離部７、
８において透過流量が変動しパーフルオロ化合物ガスの
回収率が低下しやすくなるため好ましくない。Next, the gas mixture in the storage tank 5 is
After being introduced into the compressor 6 through the pipe 13 and compressed in the compressor 6, it is introduced into the moisture removing means 3 through the pipe 14. In the moisture removing means 3, moisture in the gas mixture is removed by membrane separation, adsorption separation, condensation separation, or the like. In removing the moisture, it is preferable that the dew point of the gas mixture be -40C or less (preferably -60C or less). When the dew point exceeds this range, the carbon membrane separation unit 7,
In No. 8, the permeation flow rate fluctuates and the recovery rate of the perfluoro compound gas tends to decrease, which is not preferable.
【００１６】水分除去手段３によって水分を除去したガ
ス混合物を、管路１５を通して第１炭素膜分離部７に導
入する。第１炭素膜分離部７においては、ガス混合物中
の不活性ガス（窒素ガス等）の大部分が炭素膜を透過す
る。透過ガスの一部は、管路１６を通して貯留タンク５
に返送され、残りの他部は、管路１６から分岐した管路
１７を通して系外に排出される。一方、ガス混合物中の
パーフルオロ化合物ガスは、炭素膜を透過しにくいた
め、大部分が炭素膜を透過せず、濃縮ガスとして管路１
８を通して第２の炭素膜分離部８に送られる。The gas mixture from which the moisture has been removed by the moisture removing means 3 is introduced into the first carbon membrane separation section 7 through a pipe 15. In the first carbon membrane separation section 7, most of the inert gas (such as nitrogen gas) in the gas mixture permeates the carbon membrane. A part of the permeated gas passes through the pipe 16 to the storage tank 5.
The remaining part is discharged out of the system through a pipe 17 branched from the pipe 16. On the other hand, since the perfluoro compound gas in the gas mixture hardly permeates the carbon membrane, most of the gas does not permeate the carbon membrane, and as a concentrated gas,
8 and is sent to the second carbon membrane separation unit 8.
【００１７】第２の炭素膜分離部８においては、濃縮ガ
ス中に残留した不活性ガスなどが炭素膜を透過し、透過
ガスとして管路１９から貯留タンク５に返送される。濃
縮ガス中のパーフルオロ化合物ガスは、管路２０を通し
て回収される。このように、膜分離ユニット４では、ガ
ス混合物中のパーフルオロ化合物ガスが炭素膜分離部
７、８における膜分離によって分離されて回収される。In the second carbon membrane separation section 8, the inert gas and the like remaining in the concentrated gas permeate the carbon membrane and are returned to the storage tank 5 from the pipe 19 as a permeated gas. The perfluoro compound gas in the concentrated gas is recovered through the pipe 20. As described above, in the membrane separation unit 4, the perfluoro compound gas in the gas mixture is separated and collected by the membrane separation in the carbon membrane separation units 7, 8.
【００１８】本実施形態の分離回収方法では、ガス混合
物を炭素膜分離部７、８に供給するに先だって、水分除
去手段３によってガス混合物中の水分を除去するので、
炭素膜分離部７、８に供給されるガス混合物の水分濃度
を低くすることができる。このため、炭素膜分離部７、
８において、水の付着により炭素膜のガス透過特性が劣
化するのを防ぎ、ガス透過流量を高く維持することがで
きる。従って、ガス混合物中のパーフルオロ化合物ガス
を効率よく分離回収することができる。In the separation and recovery method of the present embodiment, the moisture in the gas mixture is removed by the moisture removing means 3 before the gas mixture is supplied to the carbon membrane separation units 7 and 8.
The water concentration of the gas mixture supplied to the carbon membrane separation units 7 and 8 can be reduced. For this reason, the carbon membrane separation unit 7,
In 8, the gas permeation characteristics of the carbon membrane are prevented from deteriorating due to the adhesion of water, and the gas permeation flow rate can be kept high. Therefore, the perfluoro compound gas in the gas mixture can be efficiently separated and recovered.
【００１９】半導体製造工程などから排出される排出ガ
スには、パーフルオロ化合物ガス、不活性ガスなどに加
え、反応性フッ素系ガス（ＨＦ、Ｆ2、ＷＦ6、Ｓｉ
Ｆ4、ＢＦ3など）を含むものがある。反応性フッ素系ガ
スは、反応性が高いため、炭素膜分離部７、８の炭素膜
の劣化の原因となり得る。このため、以下に示すように
して反応性フッ素系ガスを除去するのが好ましい。Exhaust gas discharged from a semiconductor manufacturing process or the like includes reactive fluorine-based gases (HF, F 2 , WF 6 , Si
F 4 , BF 3, etc.). Since the reactive fluorine-based gas has high reactivity, it can cause deterioration of the carbon films of the carbon film separation units 7 and 8. For this reason, it is preferable to remove the reactive fluorine-based gas as described below.
【００２０】図２は、本発明の分離回収装置の第２の実
施形態を示すもので、ここに示す分離回収装置２１は、
圧縮機６と水分除去手段３との間に、反応性フッ素系ガ
スを吸収除去する反応性フッ素系ガス吸収剤を備えた吸
収筒（反応性フッ素系ガス除去手段）２２が設けられて
いる。吸収筒２２に用いられる吸収剤としては、水酸化
カルシウム含有処理剤（例えばソーダライム）を用いる
ことができる。FIG. 2 shows a second embodiment of the separation and recovery apparatus according to the present invention. The separation and recovery apparatus 21 shown in FIG.
An absorption cylinder (reactive fluorine-based gas removing unit) 22 provided with a reactive fluorine-based gas absorbent for absorbing and removing the reactive fluorine-based gas is provided between the compressor 6 and the water removing unit 3. As the absorbent used for the absorption cylinder 22, a calcium hydroxide-containing treating agent (for example, soda lime) can be used.
【００２１】この分離回収装置２１を用いてガス混合物
中のパーフルオロ化合物ガスを分離回収するには、パー
フルオロ化合物ガスを含むガス混合物を、貯留タンク
５、圧縮機６を経て吸収筒２２に導入する。吸収筒２２
では、ガス混合物中の反応性フッ素系ガスが吸収剤によ
り吸収除去される。吸収筒２２を経たガス混合物は、水
分除去手段３に導入され、ここでガス混合物中の水分が
除去される。水分除去手段３を経たガス混合物は、膜分
離ユニット４に導入され、膜分離ユニット４では、ガス
混合物中のパーフルオロ化合物ガスが炭素膜分離部７、
８における膜分離によって濃縮されて回収される。In order to separate and recover the perfluoro compound gas in the gas mixture by using the separation and recovery device 21, the gas mixture containing the perfluoro compound gas is introduced into the absorption cylinder 22 through the storage tank 5 and the compressor 6. I do. Absorption cylinder 22
In the above, the reactive fluorine-based gas in the gas mixture is absorbed and removed by the absorbent. The gas mixture that has passed through the absorption tube 22 is introduced into the moisture removing means 3, where moisture in the gas mixture is removed. The gas mixture that has passed through the water removing means 3 is introduced into the membrane separation unit 4, where the perfluoro compound gas in the gas mixture is removed from the carbon membrane separation unit 7.
Concentrated and recovered by membrane separation in 8.
【００２２】この分離回収方法では、ガス混合物を炭素
膜分離部７、８に供給するに先だって、吸収筒２２によ
ってガス混合物中の反応性フッ素系ガスを除去するの
で、反応性フッ素系ガスによる炭素膜分離部７、８の劣
化を未然に防ぐことができる。従って、炭素膜分離部
７、８の透過性能を長期間にわたって維持することがで
きる。In this separation / recovery method, the reactive fluorine-based gas in the gas mixture is removed by the absorption cylinder 22 before the gas mixture is supplied to the carbon membrane separation units 7 and 8, so that the carbon Deterioration of the membrane separation parts 7 and 8 can be prevented beforehand. Therefore, the permeation performance of the carbon membrane separation units 7 and 8 can be maintained for a long period of time.
【００２３】また、ガス混合物を水分除去手段３に供給
するに先だって、吸収筒２２によってガス混合物中の反
応性フッ素系ガスを除去するので、反応性フッ素系ガス
によって水分除去手段３が劣化し水分除去性能が低下す
るのを未然に防ぐことができる。Prior to supplying the gas mixture to the water removing means 3, the reactive fluorine-based gas in the gas mixture is removed by the absorption tube 22. It is possible to prevent the removal performance from decreasing.
【００２４】図３は本発明の分離回収装置の第３の実施
形態を表すもので、ここに示す分離回収装置３１は、ガ
ス混合物中の水分を除去する水分除去手段３と、水分除
去手段３を経たガス混合物を圧縮する圧縮ユニット２
と、圧縮ユニット２を経たガス混合物中のパーフルオロ
化合物ガスを回収する膜分離ユニット４とを備え、水分
除去手段３の前段（上流側）に、反応性フッ素系ガスを
除去する吸収筒（反応性フッ素系ガス除去手段）３２が
設けられている。吸収筒３２としては、上記吸収筒２２
と同様の構成のものを用いることができる。FIG. 3 shows a third embodiment of the separation and recovery apparatus according to the present invention. The separation and recovery apparatus 31 shown here comprises a water removal means 3 for removing moisture in a gas mixture, and a water removal means 3. Unit 2 for compressing the gas mixture that has passed through
And a membrane separation unit 4 for recovering the perfluoro compound gas in the gas mixture that has passed through the compression unit 2. An absorption cylinder (reaction) for removing the reactive fluorine-based gas is provided upstream (upstream) of the water removing means 3. (A fluorine-based gas removing means) 32 is provided. As the absorption cylinder 32, the absorption cylinder 22 is used.
A configuration similar to that described above can be used.
【００２５】この分離回収装置３１を使用するには、ガ
ス混合物中の反応性フッ素系ガスを吸収筒３２で除去し
た後、水分除去手段３において水分を除去する。反応性
フッ素化合物と水分を除去したガス混合物を圧縮ユニッ
ト２にて圧縮した後、膜分離ユニット４に導入し、ガス
混合物中のパーフルオロ化合物ガスを膜分離により分離
回収する。In order to use the separation / recovery device 31, the reactive fluorine-based gas in the gas mixture is removed by the absorption cylinder 32, and then the moisture is removed by the moisture removing means 3. The gas mixture from which the reactive fluorine compound and water have been removed is compressed by the compression unit 2, and then introduced into the membrane separation unit 4, where the perfluoro compound gas in the gas mixture is separated and recovered by membrane separation.
【００２６】この方法によれば、吸収筒３２によってガ
ス混合物中の反応性フッ素系ガスを除去するので、水分
除去手段３、膜分離ユニット４の性能低下を防ぐことが
できる。According to this method, since the reactive fluorine-based gas in the gas mixture is removed by the absorption cylinder 32, the performance of the water removing means 3 and the membrane separation unit 4 can be prevented from being deteriorated.
【００２７】[0027]
【実施例】以下、具体例を示して本発明の分離回収方法
を説明する。 （実施例）図１に示す分離回収装置１を用いて以下の試
験を行った。水分除去手段３としては、モレキュラーシ
ーブからなる水分吸着剤層を外筒内に備えたものを使用
した。本実施形態では、ガス混合物として窒素とＣＦ4
の混合物を使用した。窒素とＣＦ4は以下に示す流量で
供給した。このガス混合物には露点が−２０℃となるよ
うに水分を加えた。 窒素：４５Ｌ／ｍｉｎ ＣＦ4：９０ｍＬ／ｍｉｎ このガス混合物を、貯留タンク５、圧縮機６を経て水分
除去手段３に導入し、ガス混合物中の水分を除去した。
これによってガス混合物の露点は−６３℃となった。水
分除去手段３を経たガス混合物を、第１炭素膜分離部７
に導入し、透過ガスの約７０％を貯留タンク５に返送
し、濃縮ガスを第２炭素膜分離部８に導入した。第２炭
素膜分離部８を経た濃縮ガスを管路２０から回収した。
試験開始時の炭素膜分離部７、８におけるガス混合物の
流入圧力は、それぞれ０．８ＭＰａ、０．７ＭＰａに設
定した。第１炭素膜分離部７における透過ガスの流量の
経時変化を図４に示す。Hereinafter, the separation and recovery method of the present invention will be described with reference to specific examples. (Example) The following tests were performed using the separation and recovery apparatus 1 shown in FIG. As the moisture removing means 3, one having a moisture adsorbent layer made of molecular sieve in the outer cylinder was used. In the present embodiment, nitrogen and CF 4 are used as a gas mixture.
Was used. Nitrogen and CF 4 were supplied at the following flow rates. Water was added to the gas mixture so that the dew point was -20 ° C. Nitrogen: 45 L / min CF 4 : 90 mL / min This gas mixture was introduced into the water removing means 3 via the storage tank 5 and the compressor 6 to remove water in the gas mixture.
This brought the dew point of the gas mixture to -63 ° C. The gas mixture that has passed through the water removing means 3 is separated into a first carbon membrane separation unit 7
And about 70% of the permeated gas was returned to the storage tank 5, and the concentrated gas was introduced into the second carbon membrane separation unit 8. The concentrated gas having passed through the second carbon membrane separation section 8 was recovered from the pipe 20.
The inflow pressure of the gas mixture in the carbon membrane separation units 7 and 8 at the start of the test was set to 0.8 MPa and 0.7 MPa, respectively. FIG. 4 shows a change with time of the flow rate of the permeated gas in the first carbon membrane separation section 7.
【００２８】（比較例）図５に示すように、水分除去手
段３を備えていないこと以外は実施例で用いたものと同
様の分離回収装置４１を用い、実施例１と同様の条件で
パーフルオロ化合物ガス回収試験を行った。第１炭素膜
分離部７における透過ガスの流量の経時変化を図４に併
せて示す。(Comparative Example) As shown in FIG. 5, a separation / recovery device 41 similar to that used in the example was used except that the water removing means 3 was not provided. A fluoro compound gas recovery test was performed. FIG. 4 also shows the change over time in the flow rate of the permeated gas in the first carbon membrane separation section 7.
【００２９】図４より、ガス混合物の水分除去を行わな
い比較例では、第１炭素膜分離部７における透過流量が
低下したのに対し、水分除去を行う実施例では透過流量
が維持され、長時間にわたり良好な運転が可能となった
ことがわかる。FIG. 4 shows that in the comparative example in which the water removal of the gas mixture was not performed, the permeation flow rate in the first carbon membrane separation unit 7 was reduced, whereas in the embodiment in which the water removal was performed, the permeation flow rate was maintained, and the permeation flow rate was maintained. It can be seen that good operation has become possible over time.
【００３０】[0030]
【発明の効果】以上説明したように、本発明の分離回収
方法では、ガス混合物を炭素膜分離手段に供給するに先
だって、ガス混合物中の水分を除去するので、炭素膜分
離手段に供給されるガス混合物の水分濃度を低くするこ
とができる。このため、炭素膜分離手段において、水の
付着により炭素膜のガス透過特性が劣化するのを防ぎ、
ガス透過流量を高く維持することができる。従って、ガ
ス混合物中のパーフルオロ化合物ガスを効率よく分離回
収することができる。As described above, according to the separation / recovery method of the present invention, the water in the gas mixture is removed before the gas mixture is supplied to the carbon membrane separation means, so that the gas mixture is supplied to the carbon membrane separation means. The water concentration of the gas mixture can be reduced. For this reason, in the carbon membrane separation means, the gas permeation characteristics of the carbon membrane are prevented from deteriorating due to the adhesion of water,
The gas permeation flow rate can be kept high. Therefore, the perfluoro compound gas in the gas mixture can be efficiently separated and recovered.
【図１】 本発明のパーフルオロ化合物ガスの分離回収
装置の第１の実施形態を示す構成図である。FIG. 1 is a configuration diagram showing a first embodiment of a perfluoro compound gas separation / recovery device of the present invention.
【図２】 本発明の分離回収装置の第２の実施形態を示
す構成図である。FIG. 2 is a configuration diagram showing a second embodiment of the separation and recovery device of the present invention.
【図３】 本発明の分離回収装置の第３の実施形態を示
す構成図である。FIG. 3 is a configuration diagram showing a third embodiment of the separation and recovery device of the present invention.
【図４】 試験結果を示すグラフである。FIG. 4 is a graph showing test results.
【図５】 分離回収装置の一例を示す構成図である。FIG. 5 is a configuration diagram illustrating an example of a separation and recovery device.
１、２１、３１、４１・・・分離回収装置、３・・・水分除去
手段、７、８・・・炭素膜分離部（炭素膜分離手段）、２
２、３２・・・吸収筒（反応性フッ素系ガス除去手段）1, 21, 31, 41: separation / recovery device, 3: moisture removal means, 7, 8: carbon membrane separation unit (carbon membrane separation means), 2
2, 32 ... absorption cylinder (reactive fluorine-based gas removing means)
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｂ０１Ｄ 61/58 Ｂ０１Ｄ 61/58 65/00 65/00 71/02 ５００ 71/02 ５００ Ｃ０７Ｃ 19/08 Ｃ０７Ｃ 19/08 (72)発明者 新田 昭彦 東京都港区西新橋１丁目５番13号 第８東 洋海事ビル８階 ＰＦＣ回収・再利用プロ ジェクト室内 (72)発明者 枝澤 克人 東京都港区西新橋１丁目５番13号 第８東 洋海事ビル８階 ＰＦＣ回収・再利用プロ ジェクト室内 (72)発明者 真鍋 岳史 東京都港区西新橋１丁目５番13号 第８東 洋海事ビル８階 ＰＦＣ回収・再利用プロ ジェクト室内 (72)発明者 大矢 浩三 東京都港区西新橋１丁目５番13号 第８東 洋海事ビル８階 ＰＦＣ回収・再利用プロ ジェクト室内 (72)発明者 永野 修次 東京都港区西新橋１丁目５番13号 第８東 洋海事ビル８階 ＰＦＣ回収・再利用プロ ジェクト室内 (72)発明者 八高 賢一 東京都港区西新橋１丁目５番13号 第８東 洋海事ビル８階 ＰＦＣ回収・再利用プロ ジェクト室内 (72)発明者 安藤 秀樹 東京都港区西新橋１丁目５番13号 第８東 洋海事ビル８階 ＰＦＣ回収・再利用プロ ジェクト室内 (72)発明者 後藤 正敏 東京都港区西新橋１丁目５番13号 第８東 洋海事ビル８階 ＰＦＣ回収・再利用プロ ジェクト室内 (72)発明者 記村 隆章 神奈川県横浜市戸塚区吉田町292 株式会 社半導体先端テクノロジーズＰＦＣグルー プ内 (72)発明者 上村 隆 神奈川県横浜市戸塚区吉田町292 株式会 社半導体先端テクノロジーズＰＦＣグルー プ内 (72)発明者 中坊 康司 神奈川県横浜市戸塚区吉田町292 株式会 社半導体先端テクノロジーズＰＦＣグルー プ内 (72)発明者 関屋 章 茨城県つくば市東１−１−１ 独立行政法 人産業技術総合研究所つくばセンター内 (72)発明者 原谷 賢治 茨城県つくば市東１−１−１ 独立行政法 人産業技術総合研究所つくばセンター内 Ｆターム(参考） 4D006 GA41 HA01 HA21 HA61 JA52A JA55A JA67A KA02 KA52 KA54 KA56 KA68 KB12 KB30 KD17 MA01 MA02 MA03 MC05X NA50 PA01 PB19 PB70 PC01 4D052 AA01 AA02 BA04 CE00 EA01 HA03 4H006 AA02 AB78 AD17 AD18 AD19 BD10 BD60 BD84 EA02 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) B01D 61/58 B01D 61/58 65/00 65/00 71/02 500 71/02 500 C07C 19/08 C07C 19/08 (72) Inventor Akihiko Nitta 1-8-13 Nishi-Shimbashi, Minato-ku, Tokyo 8th Toyo Maritime Building 8th Floor PFC Collection / Reuse Project Room (72) Inventor Katsato Ezawa 8th floor of the 8th Toyo Kaikai Building, 1-5-13 Nishi-Shimbashi, Minato-ku PFC collection / reuse project room (72) Inventor Takefumi Manabe 1-5-13 Nishi-Shimbashi, Minato-ku, Tokyo Building 8th floor PFC collection / reuse project room (72) Inventor Kozo Oya 1-5-13 Nishishinbashi, Minato-ku, Tokyo 8th Toyo Maritime Building 8th floor PFC collection / reuse project Indoors (72) Inventor Shuji Nagano 1-5-13 Nishi-Shimbashi, Minato-ku, Tokyo 8th Oriental Maritime Building 8th Floor PFC Collection / Reuse Project Room (72) Inventor Kenichi Yataka Nishi-ku, Tokyo 1-5-13 Shimbashi, 8th floor of the 8th East Maritime Building PFC collection and reuse project room (72) Inventor Hideki Ando 1st-5-13, Nishishinbashi, Minato-ku, Tokyo 8th floor of 8th East Maritime Building PFC Collection and Reuse Project Room (72) Inventor Masatoshi Goto 1-8-13 Nishi-Shimbashi, Minato-ku, Tokyo 8th Toyo Maritime Building 8F PFC Collection and Reuse Project Room (72) Inventor Kikimura Takaaki Uemura Takashi Uemura 292 Yoshida-cho, Totsuka-ku, Yokohama-shi, Kanagawa Pref. (72) Invention Person Koji Nakabo 292 Yoshida-cho, Totsuka-ku, Yokohama-shi, Kanagawa (72) Inventor: Akira Sekiya 1-1-1, Higashi, Tsukuba, Ibaraki Prefecture Independent Administrative Law Within Tsukuba Center, National Institute of Advanced Industrial Science and Technology (72) Inventor: Kenji Haratani, Higashi 1, Tsukuba, Ibaraki -1-1 F-term in Tsukuba Center, National Institute of Advanced Industrial Science and Technology (reference) CE00 EA01 HA03 4H006 AA02 AB78 AD17 AD18 AD19 BD10 BD60 BD84 EA02
Claims (6)
物を炭素膜分離手段に供給し、炭素膜を用いてガス混合
物中のパーフルオロ化合物ガスを分離回収する方法であ
って、 ガス混合物を炭素膜分離手段に供給するに先だって、ガ
ス混合物中の水分を除去することを特徴とするパーフル
オロ化合物ガスの分離回収方法。1. A method for supplying a gas mixture containing a perfluoro compound gas to a carbon membrane separation means and separating and recovering the perfluoro compound gas in the gas mixture using a carbon membrane, wherein the gas mixture is separated by a carbon membrane. A method for separating and recovering a perfluoro compound gas, comprising removing water in a gas mixture before supplying the gas to a means.
て、膜分離、吸着分離、および凝縮分離のうち少なくと
も１つを用いることを特徴とする請求項１記載のパーフ
ルオロ化合物ガスの分離回収方法。2. The method according to claim 1, wherein at least one of membrane separation, adsorption separation, and condensation separation is used as a method for removing water in the gas mixture. .
に先だって、ガス混合物中の反応性フッ素系ガスを除去
することを特徴とする請求項１または２記載のパーフル
オロ化合物ガスの分離回収方法。3. The method for separating and recovering a perfluoro compound gas according to claim 1, wherein a reactive fluorine-based gas in the gas mixture is removed before supplying the gas mixture to the carbon membrane separation means. .
物中のパーフルオロ化合物ガスを、炭素膜を用いて分離
回収する炭素膜分離手段を備えた分離回収装置であっ
て、 炭素膜分離手段の上流側に、ガス混合物中の水分を除去
する水分除去手段が設けられていることを特徴とするパ
ーフルオロ化合物ガスの分離回収装置。4. A separation and recovery apparatus provided with a carbon membrane separation means for separating and recovering a perfluoro compound gas in a gas mixture containing a perfluoro compound gas by using a carbon membrane, wherein the upstream side of the carbon membrane separation means is provided. A perfluoro compound gas separation and recovery device, further comprising a water removing means for removing water in the gas mixture.
よび凝縮分離のうち少なくとも１つによりガス混合物中
の水分を除去することができるものであることを特徴と
する請求項４記載のパーフルオロ化合物ガスの分離回収
装置。5. The par according to claim 4, wherein the water removing means is capable of removing water in the gas mixture by at least one of membrane separation, adsorption separation, and condensation separation. Separation and recovery equipment for fluoro compound gas.
中の反応性フッ素系ガスを除去する反応性フッ素系ガス
除去手段が設けられていることを特徴とする請求項４ま
たは５記載のパーフルオロ化合物ガスの分離回収装置。6. The reactive fluorine-based gas removing means for removing a reactive fluorine-based gas in a gas mixture is provided upstream of the carbon membrane separation means. Perfluoro compound gas separation and recovery device.
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| JP2001165872A JP3727551B2 (en) | 2001-05-31 | 2001-05-31 | Method and apparatus for separating and recovering perfluoro compound gas |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001165872A JP3727551B2 (en) | 2001-05-31 | 2001-05-31 | Method and apparatus for separating and recovering perfluoro compound gas |
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| JP3727551B2 JP3727551B2 (en) | 2005-12-14 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2311551A1 (en) * | 2008-07-08 | 2011-04-20 | Dalian University of Technology | A curlable carbon membrane and preparation method thereof |
| RU2467994C1 (en) * | 2011-06-08 | 2012-11-27 | Государственное образовательное учреждение высшего профессионального образования "Нижегородский государственный технический университет им. Р.Е. Алексеева" (НГТУ) | Method of purifying tetrafluoromethane and apparatus for realising said method |
| JP2015525134A (en) * | 2013-06-25 | 2015-09-03 | ファインテック．カンパニー，リミテッド | Perfluoro compound separation and recycling system |
| JP2017039074A (en) * | 2015-08-19 | 2017-02-23 | 株式会社ディスコ | Recovery method of plasma etching gas |
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| JP2000140576A (en) * | 1998-11-05 | 2000-05-23 | Kanto Denka Kogyo Co Ltd | System for making fluorogas-containing mixture harmless |
| JP2000185212A (en) * | 1998-12-22 | 2000-07-04 | Ube Ind Ltd | Method for separating and recovering perfluoro compound gas and device therefor |
| JP2000342944A (en) * | 1999-03-05 | 2000-12-12 | Ube Ind Ltd | Partially carbonized asymmetric hollow fiber separation membrane, production thereof and gas separation method |
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2001
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000140576A (en) * | 1998-11-05 | 2000-05-23 | Kanto Denka Kogyo Co Ltd | System for making fluorogas-containing mixture harmless |
| JP2000185212A (en) * | 1998-12-22 | 2000-07-04 | Ube Ind Ltd | Method for separating and recovering perfluoro compound gas and device therefor |
| JP2000342944A (en) * | 1999-03-05 | 2000-12-12 | Ube Ind Ltd | Partially carbonized asymmetric hollow fiber separation membrane, production thereof and gas separation method |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2311551A1 (en) * | 2008-07-08 | 2011-04-20 | Dalian University of Technology | A curlable carbon membrane and preparation method thereof |
| EP2311551A4 (en) * | 2008-07-08 | 2014-09-17 | Univ Dalian Tech | A curlable carbon membrane and preparation method thereof |
| RU2467994C1 (en) * | 2011-06-08 | 2012-11-27 | Государственное образовательное учреждение высшего профессионального образования "Нижегородский государственный технический университет им. Р.Е. Алексеева" (НГТУ) | Method of purifying tetrafluoromethane and apparatus for realising said method |
| JP2015525134A (en) * | 2013-06-25 | 2015-09-03 | ファインテック．カンパニー，リミテッド | Perfluoro compound separation and recycling system |
| JP2017039074A (en) * | 2015-08-19 | 2017-02-23 | 株式会社ディスコ | Recovery method of plasma etching gas |
| CN106466547A (en) * | 2015-08-19 | 2017-03-01 | 株式会社迪思科 | The recovery method of plasma etching gas |
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|---|---|
| JP3727551B2 (en) | 2005-12-14 |
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