JP2000005561A - Fluoride treatment method - Google Patents
Fluoride treatment methodInfo
- Publication number
- JP2000005561A JP2000005561A JP10171922A JP17192298A JP2000005561A JP 2000005561 A JP2000005561 A JP 2000005561A JP 10171922 A JP10171922 A JP 10171922A JP 17192298 A JP17192298 A JP 17192298A JP 2000005561 A JP2000005561 A JP 2000005561A
- Authority
- JP
- Japan
- Prior art keywords
- fluoride
- gas
- membrane separation
- separation device
- chemically stable
- 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
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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/30—Capture or disposal of greenhouse gases of perfluorocarbons [PFC], hydrofluorocarbons [HFC] or sulfur hexafluoride [SF6]
Landscapes
- Treating Waste Gases (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、フッ化物の処理方
法に関し、詳しくは、半導体製造工程から排出される排
ガスの無害化とフッ化物の回収とを行うための処理方法
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for treating fluoride, and more particularly, to a method for detoxifying exhaust gas discharged from a semiconductor manufacturing process and recovering fluoride.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】半導体
製造工程では、エッチング工程やチャンバークリーニン
グ工程で、パーフルオロカーボン（ＰＦＣ）やハイドロ
フルオロカーボン（ＨＦＣ），三フッ化窒素（Ｎ
Ｆ３），六フッ化硫黄（ＳＦ６）等のフッ化物を使用し
ており、半導体製造工程から排出される排ガス中には、
これらのフッ化物が含まれている。このようなフッ化物
は、地球温暖化の原因となる物質であることから、排ガ
スを大気に放出する前にフッ化物を除去しておく必要が
ある。2. Description of the Related Art In a semiconductor manufacturing process, a perfluorocarbon (PFC), a hydrofluorocarbon (HFC), a nitrogen trifluoride (NFC) is used in an etching process and a chamber cleaning process.
Fluoride such as F 3 ) and sulfur hexafluoride (SF 6 ) is used, and in the exhaust gas discharged from the semiconductor manufacturing process,
These fluorides are included. Since such a fluoride is a substance causing global warming, it is necessary to remove the fluoride before discharging the exhaust gas to the atmosphere.
【０００３】しかし、上述のようなパーフルオロカーボ
ン等のフッ化物は、非常に安定で分解処理が困難な化合
物であり、１０００℃程度の高温下で分解処理を行わな
ければならず、処理コストが高いだけでなく、さらに、
固形廃棄物やフッ酸等の有害物質が大量に発生するとい
う問題もあり、その解決が求められている。[0003] However, the above-mentioned fluorides such as perfluorocarbons are compounds that are very stable and difficult to decompose, and must be decomposed at a high temperature of about 1000 ° C, resulting in high processing costs. Not only that,
There is also a problem that a large amount of harmful substances such as solid waste and hydrofluoric acid are generated, and a solution is required.
【０００４】そこで本発明は、排ガス中に含まれるフッ
化物の大部分を回収することができ、経済的にフッ化物
を含むガスを処理することができる方法を提供すること
を目的としている。Accordingly, an object of the present invention is to provide a method capable of recovering most of the fluoride contained in exhaust gas and economically treating a gas containing fluoride.
【０００５】[0005]
【課題を解決するための手段】上記目的を達成するた
め、本発明のフッ化物の処理方法は、半導体製造工程か
ら排出される排ガス中のフッ化物を処理する方法におい
て、前記排ガスを構成する主成分ガス中に含まれている
パーフルオロカーボン，ハイドロフルオロカーボン，三
フッ化窒素，六フッ化硫黄等の化学的に安定なフッ化物
以外の不純物成分をあらかじめ除去した後、前記化学的
に安定なフッ化物の濃縮処理を行い、濃縮された該フッ
化物を回収するとともに、濃縮処理を終えた主成分ガス
中に残留する微量のフッ化物を分解処理することを特徴
とし、特に、濃縮処理が、膜分離であることを特徴とし
ている。In order to achieve the above object, a method for treating fluoride according to the present invention is directed to a method for treating fluoride in exhaust gas discharged from a semiconductor manufacturing process. After removing impurity components other than chemically stable fluoride, such as perfluorocarbon, hydrofluorocarbon, nitrogen trifluoride, and sulfur hexafluoride, contained in the component gas in advance, the chemically stable fluoride is removed. And the concentrated fluoride is recovered, and a small amount of fluoride remaining in the main component gas after the concentration treatment is decomposed. In particular, the concentration treatment is performed by membrane separation. It is characterized by being.
【０００６】まず、半導体製造工程から排出される排ガ
スは、通常、窒素，酸素，水素等のキャリアガス（ベー
スガス）を主成分とし、これに前述のフッ化物や各種原
料ガス等が含まれた状態となっている。このような排ガ
ス中に含まれているパーフルオロカーボン，ハイドロフ
ルオロカーボン，三フッ化窒素，六フッ化硫黄等の化学
的に安定なフッ化物を回収するためには、フッ化物を回
収する工程に導入する前に排ガスを前処理設備に導入
し、該排ガス中に含まれているフッ化物の中でも、四フ
ッ化ケイ素（ＳｉＦ４），二フッ化カルボニル（ＣＯＦ
２），フッ化水素（ＨＦ）等の不安定で反応性の高いフ
ッ化物を含む各種ハロゲン化物や、冷却したときに固化
する水分や二酸化炭素等の不純物成分を除去しておく。
この前処理は、適当な吸着剤や除害剤を用いることによ
って周知の方法で行うことができ、このような前処理を
行うことにより、フッ化物回収工程には、化学的に安定
なフッ化物（以下、単にフッ化物という）を含むベース
ガスが導入されることになる。First, the exhaust gas discharged from the semiconductor manufacturing process usually contains a carrier gas (base gas) such as nitrogen, oxygen, hydrogen or the like as a main component, and contains the above-mentioned fluoride and various raw material gases. It is in a state. In order to recover chemically stable fluorides such as perfluorocarbon, hydrofluorocarbon, nitrogen trifluoride, sulfur hexafluoride and the like contained in such exhaust gas, a process for recovering the fluoride is introduced. Exhaust gas is introduced into a pretreatment facility beforehand, and among the fluorides contained in the exhaust gas, silicon tetrafluoride (SiF 4 ) and carbonyl difluoride (COF)
2 ) Various halides including fluorides such as hydrogen fluoride (HF), which are unstable and highly reactive, and impurities such as water and carbon dioxide which solidify when cooled are removed.
This pretreatment can be performed by a well-known method by using an appropriate adsorbent or a detoxifying agent. By performing such a pretreatment, a chemically stable fluoride can be used in the fluoride recovery step. A base gas containing (hereinafter simply referred to as fluoride) will be introduced.
【０００７】フッ化物回収工程は、高分子膜を利用した
膜分離法、活性炭やゼオライトを用いた吸着法、低温流
体で冷却して液化分離する深冷法等の周知の方法で行う
ことができ、ベースガスの種類やフッ化物の種類及び含
有量に応じて最適なものを採用することができる。中で
も、装置構成やランニングコストを考慮すると、膜分離
法が最適であるといえる。また、フッ化物回収工程は、
一段階で行うこともできるが、複数段階で行うことが好
ましい。The fluoride recovery step can be performed by a known method such as a membrane separation method using a polymer membrane, an adsorption method using activated carbon or zeolite, or a cryogenic method in which liquefaction is performed by cooling with a low-temperature fluid. The most suitable gas can be adopted according to the type of base gas and the type and content of fluoride. Above all, it can be said that the membrane separation method is optimal in consideration of the device configuration and the running cost. In addition, the fluoride recovery step
Although it can be carried out in one step, it is preferable to carry out in a plurality of steps.
【０００８】上述のフッ化物回収工程を行うことによ
り、大部分のフッ化物をベースガスから分離して回収す
ることができるが、フッ化物とベースガスとを完全に分
離することは困難であり、分離性能を高めようとする
と、装置が大型化したり、運転コストが非常に高くなっ
たりするというデメリットを生じる。[0008] By performing the above-described fluoride recovery step, most of the fluoride can be separated and recovered from the base gas, but it is difficult to completely separate the fluoride and the base gas. Attempts to increase the separation performance have the disadvantage of increasing the size of the device and increasing the operating costs.
【０００９】したがって、本発明では、フッ化物回収工
程で大部分のフッ化物を分離して回収するとともに、フ
ッ化物回収工程から導出されるベースガスをフッ化物分
解工程に導入し、ベースガス中に残留するフッ化物を分
解処理するようにしている。Therefore, in the present invention, most of the fluorides are separated and recovered in the fluoride recovery step, and the base gas derived from the fluoride recovery step is introduced into the fluoride decomposition step, so that the base gas is contained in the base gas. The remaining fluoride is decomposed.
【００１０】フッ化物分解工程は、可燃性ガス、例え
ば、ＬＰＧやＬＮＧ，水素等を燃焼させた熱により分解
する方法、ＣａＯやＣａ（ＯＨ）２等の塩基性化合物と
フッ化物とを高温化で反応させて分解する方法、金属ナ
トリウムを加熱蒸発させた蒸気とフッ化物とを反応させ
て分解する方法、ＴｉＯ２等の触媒とフッ化物とを高温
下で接触させて分解する方法等、従来から行われている
様々な方法を採用することができ、フッ化物の処理量等
に応じて最適な方法を採用することができる。[0010] The fluoride decomposition step is a method of decomposing a combustible gas, for example, LPG, LNG, hydrogen, or the like, by the heat of combustion, and increasing the temperature of a basic compound such as CaO or Ca (OH) 2 and the fluoride. Such as a method of decomposing by reacting with sodium, a method of decomposing by reacting a vapor obtained by heating and evaporating metal sodium with a fluoride, and a method of decomposing by contacting a catalyst such as TiO 2 with a fluoride at a high temperature. Can be adopted, and an optimal method can be adopted according to the throughput of the fluoride and the like.
【００１１】このように、排ガス中のフッ化物の大部分
を濃縮して回収するとともに、分離回収が困難な極微量
のフッ化物を分解処理することにより、濃縮回収方法の
利点であるランニングコストの安さを生かしながら、分
解処理方法の利点である高い処理効率を生かすことがで
きる。したがって、全体としてのランニングコストを低
く抑えながら、フッ化物の回収処理と分解処理とを効果
的に行うことができる。As described above, by concentrating and recovering most of the fluoride in the exhaust gas and decomposing the trace amount of fluoride which is difficult to separate and recover, the running cost, which is an advantage of the concentration and recovery method, is reduced. High processing efficiency, which is an advantage of the decomposition method, can be utilized while making use of inexpensiveness. Therefore, the fluoride recovery processing and the decomposition processing can be performed effectively while the running cost as a whole is kept low.
【００１２】[0012]
【発明の実施の形態】図１は本発明方法を実施する際の
好ましい装置構成例を示す系統図である。このフッ化物
処理装置は、前処理設備１の後段に、第一膜分離装置２
と第二膜分離装置３とを設置し、第一膜分離装置２でフ
ッ化物が濃縮したガス（非透過ガス）を経路４を通して
第二膜分離装置３に導入し、二段階でフッ化物を濃縮す
るように形成したものであって、第二膜分離装置３で非
透過ガス側に濃縮されたフッ化物は、容器５に回収され
て精製設備に送られ、両膜分離装置２，３で分離膜を透
過したガスを排出する経路６には、該ガス中に含まれる
フッ化物を分解するためのフッ化物分解筒７を設けてい
る。このようにフッ化物の濃縮を二段階で行うことによ
り、フッ化物を高濃度で回収でき、精製処理も容易に行
うことができる。DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. 1 is a system diagram showing an example of a preferred apparatus configuration for implementing the method of the present invention. This fluoride treatment device is provided with a first membrane separation device 2
And the second membrane separation device 3 are installed, and a gas (non-permeated gas) in which the fluoride is concentrated in the first membrane separation device 2 is introduced into the second membrane separation device 3 through the path 4 and the fluoride is separated in two stages. The fluoride formed so as to be concentrated and concentrated on the non-permeate gas side in the second membrane separation device 3 is collected in the container 5 and sent to the purification facility, where it is separated by the two membrane separation devices 2 and 3. In a path 6 for discharging gas permeated through the separation membrane, a fluoride decomposing cylinder 7 for decomposing fluoride contained in the gas is provided. By performing the concentration of the fluoride in two stages as described above, the fluoride can be recovered at a high concentration, and the purification treatment can be easily performed.
【００１３】なお、分離膜としては、各種高分子膜、例
えば、特開平９−１０３６３３号公報に記載されている
ガラス状ポリマー膜等を用いることができる。As the separation membrane, various polymer membranes, for example, a glassy polymer membrane described in JP-A-9-103633 can be used.
【００１４】[0014]
【実施例】試験ガスとして、化学的に安定な四フッ化炭
素（ＣＦ４）を１％含む窒素ガスを用意し、図１と略同
じ構成の試験装置により四フッ化炭素を回収する実験を
行った。分離膜には、窒素ガスは通過するが、四フッ化
炭素はほとんど通過できない高分子膜を使用し、フッ化
物分解筒内にはＣａＯを充填して１０００℃に加熱し
た。なお、試験ガス中には、前述のような不純物が含ま
れていないため、不純物除去のための前処理は省略し
た。EXAMPLE As a test gas, a nitrogen gas containing 1% of chemically stable carbon tetrafluoride (CF 4 ) was prepared, and an experiment of recovering carbon tetrafluoride by a test device having substantially the same configuration as in FIG. 1 was conducted. went. For the separation membrane, a polymer membrane that allows nitrogen gas to pass but hardly allows carbon tetrafluoride to pass was used, and the inside of the fluoride decomposition tube was filled with CaO and heated to 1000 ° C. Since the test gas does not contain the above-described impurities, the pretreatment for removing the impurities was omitted.
【００１５】前記試験ガスを第一膜分離装置に毎分１０
０リットルで導入した。その結果、毎分９８リットルの
ガスが分離膜を通過してきた。このガスには、約０．１
％の四フッ化炭素が含まれていた。The test gas is supplied to the first membrane separation device at a rate of 10 / min.
It was introduced at 0 liter. As a result, 98 liters of gas per minute passed through the separation membrane. This gas contains about 0.1
% Carbon tetrafluoride.
【００１６】この第一段目の膜分離により、濃度約４５
％に濃縮された四フッ化炭素を含むガスが毎分２リット
ルで得られたので、これを第二膜分離装置に導入して再
度濃縮操作を行った。その結果、四フッ化炭素濃度約９
５％のガスを毎分０．９リットルで回収することができ
た。By the first stage of membrane separation, a concentration of about 45
Since a gas containing carbon tetrafluoride concentrated to 2% was obtained at a rate of 2 liters per minute, the gas was introduced into the second membrane separation device, and the concentration operation was performed again. As a result, the carbon tetrafluoride concentration was about 9
5% gas could be recovered at 0.9 liters per minute.
【００１７】第二膜分離装置で分離膜を通過してきた毎
分１．１リットルの透過ガス中の四フッ化炭素の濃度
は、約４．１％であった。両膜分離装置で分離膜を通過
したガスは、まとめて前記フッ化物分解筒に導入し、四
フッ化炭素の分解処理を行った。フッ化物分解筒から導
出したガスをガスクロマトグラフに導入し、四フッ化炭
素の分析を行ったが、検出限界（１０ｐｐｍ）以下であ
った。The concentration of carbon tetrafluoride in the permeated gas at a rate of 1.1 liter per minute passed through the separation membrane in the second membrane separation device was about 4.1%. Gases that passed through the separation membranes in both membrane separation devices were collectively introduced into the above-mentioned fluoride decomposition column, where carbon tetrafluoride was decomposed. The gas derived from the fluoride decomposition column was introduced into a gas chromatograph, and the analysis of carbon tetrafluoride was performed. The result was below the detection limit (10 ppm).
【００１８】フッ化物分解筒で処理した四フッ化炭素の
量は、毎分０．１４３リットルであった。この量は、試
験ガスの全量をフッ化物分解筒に導入した場合に比べて
約１／７以下である。この実験結果から、ＣａＯのよう
な処理剤の交換期間を７倍以上にできるとともに、廃棄
物の発生量も１／７以下にできることがわかる。The amount of carbon tetrafluoride treated in the fluoride decomposition tube was 0.143 liter per minute. This amount is about 1/7 or less as compared with the case where the whole amount of the test gas is introduced into the fluoride decomposition tube. From this experimental result, it can be seen that the replacement period of the treatment agent such as CaO can be increased seven times or more and the amount of waste generated can be reduced to 1/7 or less.
【００１９】[0019]
【発明の効果】以上説明したように、本発明のフッ化物
の処理方法によれば、半導体製造工程から排出される排
ガス中に含まれる化学的に安定なフッ化物を効率よく回
収できるとともに、残留する微量のフッ化物の分解処理
も効果的に行うことができる。As described above, according to the method for treating fluoride of the present invention, it is possible to efficiently recover chemically stable fluoride contained in exhaust gas discharged from a semiconductor manufacturing process, A small amount of fluoride can be effectively decomposed.
【図１】 本発明方法を実施する際の好ましい装置構成
例を示す系統図である。FIG. 1 is a system diagram showing an example of a preferred apparatus configuration when implementing the method of the present invention.
１…前処理設備、２…第一膜分離装置、３…第二膜分離
装置、７…フッ化物分解筒DESCRIPTION OF SYMBOLS 1 ... Pre-processing equipment, 2 ... First membrane separation device, 3 ... Second membrane separation device, 7 ... Fluoride decomposition cylinder
フロントページの続き (72)発明者 新田 昭彦 東京都港区西新橋１−16−７ 日本酸素株 式会社内 (72)発明者 宮澤 和浩 東京都港区西新橋１−16−７ 日本酸素株 式会社内 Ｆターム(参考） 4D002 AA22 AC10 BA05 BA12 DA05 DA11 DA21 DA54 DA56 EA01 EA02 EA05 FA01 HA02 HA04 4D006 GA41 KB30 MC09 PA04 PB19 PB70 PC01 Continuing on the front page (72) Inventor Akihiko Nitta 1-16-7 Nishi-Shimbashi, Minato-ku, Tokyo Nippon Sanso Co., Ltd. (72) Inventor Kazuhiro Miyazawa 1-16-7 Nishi-Shimbashi, Minato-ku, Tokyo Nippon Sanso Corporation F-term in the formula company (reference) 4D002 AA22 AC10 BA05 BA12 DA05 DA11 DA21 DA54 DA56 EA01 EA02 EA05 FA01 HA02 HA04 4D006 GA41 KB30 MC09 PA04 PB19 PB70 PC01
Claims (3)
のフッ化物を処理する方法において、前記排ガスを構成
する主成分ガス中の化学的に安定なフッ化物以外の不純
物成分をあらかじめ除去した後、前記化学的に安定なフ
ッ化物の濃縮処理を行い、濃縮された該フッ化物を回収
するとともに、濃縮処理を終えた主成分ガス中に残留す
る微量のフッ化物を分解処理することを特徴とするフッ
化物の処理方法。In a method for treating a fluoride in an exhaust gas discharged from a semiconductor manufacturing process, after removing in advance a chemically stable impurity component other than a fluoride in a main component gas constituting the exhaust gas, Performing a concentration treatment of the chemically stable fluoride, recovering the concentrated fluoride, and decomposing a trace amount of fluoride remaining in the main component gas after the concentration treatment. How to treat fluoride.
徴とする請求項１記載のフッ化物の処理方法。2. The fluoride treatment method according to claim 1, wherein the concentration treatment is a membrane separation.
ルオロカーボン，ハイドロフルオロカーボン，三フッ化
窒素，六フッ化硫黄の少なくともいずれか一種であるこ
とを特徴とする請求項１記載のフッ化物の処理方法。3. The fluoride according to claim 1, wherein the chemically stable fluoride is at least one of perfluorocarbon, hydrofluorocarbon, nitrogen trifluoride, and sulfur hexafluoride. Processing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10171922A JP2000005561A (en) | 1998-06-18 | 1998-06-18 | Fluoride treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10171922A JP2000005561A (en) | 1998-06-18 | 1998-06-18 | Fluoride treatment method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2000005561A true JP2000005561A (en) | 2000-01-11 |
Family
ID=15932346
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10171922A Pending JP2000005561A (en) | 1998-06-18 | 1998-06-18 | Fluoride treatment method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2000005561A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002035527A (en) * | 2000-07-26 | 2002-02-05 | Japan Atom Energy Res Inst | Gas separation equipment |
| JP2004174391A (en) * | 2002-11-27 | 2004-06-24 | Central Res Inst Of Electric Power Ind | Method for selectively removing fluorine components from exhaust gas |
| JP2007319811A (en) * | 2006-06-02 | 2007-12-13 | Hitachi Ltd | PFC gas concentration method |
| KR100860835B1 (en) | 2007-01-10 | 2008-09-29 | 서윤석 | Treatment of sulfur hexafluoride |
| WO2013125792A1 (en) * | 2012-02-23 | 2013-08-29 | (주) 파인텍 | System for separating and reusing perfluorocarbon compound |
| WO2013125791A1 (en) * | 2012-02-23 | 2013-08-29 | (주) 파인텍 | System for separating and reusing perfluorocarbon compound |
-
1998
- 1998-06-18 JP JP10171922A patent/JP2000005561A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002035527A (en) * | 2000-07-26 | 2002-02-05 | Japan Atom Energy Res Inst | Gas separation equipment |
| JP2004174391A (en) * | 2002-11-27 | 2004-06-24 | Central Res Inst Of Electric Power Ind | Method for selectively removing fluorine components from exhaust gas |
| JP2007319811A (en) * | 2006-06-02 | 2007-12-13 | Hitachi Ltd | PFC gas concentration method |
| KR100860835B1 (en) | 2007-01-10 | 2008-09-29 | 서윤석 | Treatment of sulfur hexafluoride |
| WO2013125792A1 (en) * | 2012-02-23 | 2013-08-29 | (주) 파인텍 | System for separating and reusing perfluorocarbon compound |
| WO2013125791A1 (en) * | 2012-02-23 | 2013-08-29 | (주) 파인텍 | System for separating and reusing perfluorocarbon compound |
| KR101410914B1 (en) | 2012-02-23 | 2014-06-24 | (주)파인텍 | The separation and recycling system for a perfluoro compounds |
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