US20050115674A1 - Method for treating exhaust gas - Google Patents

Method for treating exhaust gas Download PDF

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Publication number
US20050115674A1
US20050115674A1 US10/474,765 US47476503A US2005115674A1 US 20050115674 A1 US20050115674 A1 US 20050115674A1 US 47476503 A US47476503 A US 47476503A US 2005115674 A1 US2005115674 A1 US 2005115674A1
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US
United States
Prior art keywords
fluoride
gas
combustion
nickel
exhaust gas
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Abandoned
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US10/474,765
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English (en)
Inventor
Hiroyasu Taguchi
Yasuyuki Hoshino
Byoung-sup Park
Bingzhe Jin
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Koike Sanso Kogyo Co Ltd
Resonac Holdings Corp
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Individual
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Assigned to KOIKE SANSO KOGYO CO., LTD., SHOWA DENKO K.K. reassignment KOIKE SANSO KOGYO CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: HOSHINO, YASUYUKI, JIN, BINGZHE, PARK, BYOUNG-SUP, TAGUCHI, HIROYASU
Publication of US20050115674A1 publication Critical patent/US20050115674A1/en
Assigned to SHOWA DENKO K.K., KOIKE SANSO KOGYO CO., LTD. reassignment SHOWA DENKO K.K. RE-RECORD TO CORRECT THE ADDRESS OF THE FIRST ASSIGNEE, PREVIOUSLY RECORDED ON REEL 015053 FRAME 0767. Assignors: HOSHINO, YASUYUKI, JIN, BINGZHE, PARK, BYOUNG-SUP, TAGUCHI, HIROYASU
Abandoned legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F23G7/061—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases with supplementary heating
    • F23G7/065—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases with supplementary heating using gaseous or liquid fuel
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23J—REMOVAL OR TREATMENT OF COMBUSTION PRODUCTS OR COMBUSTION RESIDUES; FLUES 
    • F23J2215/00—Preventing emissions
    • F23J2215/30—Halogen; Compounds thereof

Definitions

  • the present invention relates to an exhaust gas treatment process and treatment apparatus. More particularly, the invention relates to a process and apparatus for treatment of an exhaust gas, containing fluorine gas or halogen fluoride gas, which is emitted from the etching or the cleaning steps of semiconductor fabrication processes, and to a semiconductor device fabrication process which employs the process and apparatus.
  • the exhaust gas emitted from various steps in the fabrication of semiconductors contains gases such as semiconductor material gas, etching gas or cleaning gas, and these gases are often harmful. They sometimes include environmentally unfriendly gases and, therefore, exhaust gas containing such components cannot be directly emitted into the atmosphere.
  • Methods for exhaust gas treatment are widely known, and include:
  • thermal treatment-type abatement methods such as combustion-type or thermal decomposition-type methods
  • combustion-type or thermal decomposition-type methods have been investigated as abatement methods whereby flammable fuel gases or the like are burned at high temperature to convert toxic components in the exhaust gas or the environmentally-unfriendly exhaust gas components to harmless substances, or to convert them to substances that can be easily treated.
  • the exhaust gas emitted from the semiconductor fabrication process is subjected to combustion treatment at high temperature together with fuel gases such as utility gas, LPG, methane or the like and with supporting gases such as air and oxygen, and this results in the generation of NO x gases, as by-products, from the elemental nitrogen in the exhaust gas or the nitrogen gas in the air.
  • fuel gases such as utility gas, LPG, methane or the like
  • supporting gases such as air and oxygen
  • NO x gases are often generated, in burned exhaust gas, at very high concentrations of 1-30%, depending on the apparatus and combustion conditions employed, and several methods have been investigated to limit the concentration to the TLV (25 ppm NO, 3 ppm NO 2 ).
  • Japanese Unexamined Patent Publication No. 2001-193918 describes studies of combustion chamber shapes and nozzle shapes to reduce generation of NO x .
  • the generation of NO x is particularly high, creating a situation in need of improvement.
  • fluorine gas or halogen fluoride gases are highly active, strong oxidizers with high chemical reactivity and therefore often react with oxidizing substances at ordinary temperature resulting in ignition, while they are also highly corrosive to apparatus materials.
  • the apparatus materials must therefore be strictly selected from among specific highly corrosion-resistant metals, and be free from oils and water; moreover, tetrafluoroethylene resins which are widely used as highly corrosion-resistant resins for semiconductor fabrication apparatuses are often unsuitable for the given conditions of use.
  • abatement systems for fluorine gas or halogen fluoride gases such as chlorine trifluoride there are used wet absorption systems which accomplish neutralizing absorption with scrubbers employing alkali aqueous solutions such as caustic soda or caustic potash, or dry abatement systems which accomplish adsorption removal with a solid adsorbent such as active alumina or soda lime. All such methods, however, have a drawback in that they do not allow treatment of exhaust gas containing high concentrations of fluorine gas or halogen fluoride gases.
  • the invention provides an exhaust gas treatment process which comprises burning exhaust gas containing fluorine gas or halogen fluoride gases emitted from etching or cleaning steps, in a combustion chamber having a fluoride passivation film formed on its surface.
  • the fluoride passivation film is preferably composed of nickel fluoride.
  • the concentration of fluorine gas or halogen fluoride gases is preferably no greater than 5 vol %.
  • the content of nitrogen oxides in the exhaust gas after combustion is preferably less than 5 volppm.
  • the invention further provides an exhaust gas treatment system equipped with an exhaust gas introduction port, a fuel introduction port, a precombustion chamber, a combustion chamber, an air introduction port and an exhaust duct, and having a fluoride passivation film formed on at least the surface of the combustion chamber.
  • the combustion chamber is formed of at least one type of material selected from the group consisting of nickel, nickel-rich alloys and Monel metal, and a fluoride passivation film is formed on the surface of the material.
  • the combustion chamber is formed of at least one type of material selected from the group consisting of stainless steel and steel materials, with the surface of the material having a thin-film composed of nickel, nickel alloy electroplating, electrocast plating or nickel alloy electroless plating or a ceramic thin-film composed of alumina or aluminum nitride, and a fluoride passivation film formed over the surface of the thin-film.
  • the invention still further provides a semiconductor device fabrication process comprising an etching or cleaning step employing fluorine gas or halogen fluoride gas as the etching gas or cleaning gas and an abatement step wherein the gas containing fluorine gas or halogen fluoride gas emitted from the previous step is burned, the abatement step being carried out in a combustion chamber having a fluoride passivation film formed on its surface.
  • the fluoride passivation film is preferably composed of nickel fluoride.
  • FIG. 1 is a schematic view showing an embodiment of a treatment system for carrying out the exhaust gas treatment process of the invention.
  • 1 is process exhaust gas
  • 2 is diluting gas
  • 3 is supporting gas
  • 4 is flammable gas for combustion
  • 5 is air
  • 6 is atmospheric discharge gas
  • 7 is a precombustion chamber
  • 8 is a combustion chamber
  • 9 is a combustion gas cooling apparatus
  • 10 is an alkali scrubber
  • 11 is an exhaust blower.
  • exhaust gas containing fluorine gas or halogen fluoride gases emitted from etching or cleaning steps is burned in a combustion chamber having a fluoride passivation film formed on its surface. That is, the invention encompasses a treatment to render harmless exhaust gas emitted from semiconductor fabrication processes including fluorine gas or halogen fluoride gases as well as gases such as SiH 4 used as film-forming gases or other gases, at a prescribed temperature.
  • the treatment process of the invention can notably reduce the amount of carbon dioxide and NO x gases as decomposition by-products emitted from abatement systems, by allowing an adequate harmless-rendering treatment to be carried out under conditions with reduced fuel feed and lower combustion temperature compared to the ordinary combustion conditions when no fluorine gas or halogen fluoride gases are present, or in other words, it permits treatment to be carried out on compounds which can be easily rendered harmless so that operation may be carried out under such suitable conditions.
  • a combustion-type abatement system is used for simultaneous abatement treatment of film-forming gases such as SiH 4 , SiH 2 Cl 2 , NH 3 , PH 3 , WF 6 , Si(OC 2 H 5 ) 4 , NF 3 , H 2 , B 2 H 6 , CH 4 , C 2 H 2 and the like, cleaning gases or other gas components emitted in semiconductor fabrication processes, which are commonly used in steps of semiconductor fabrication, along with the fluorine gas and halogen fluoride gases.
  • the components to be treated in the exhaust gas may be fluorine gas or halogen fluoride gas alone.
  • the concentration of the fluorine gas or halogen fluoride gas in the exhaust gas is preferably no greater than 5 vol %.
  • Operation of the combustion-type abatement system of the invention can accomplish harmless rendering of toxic gas components and conversion to substances which are easily removed by decomposition, under operating conditions with 10-30% lower fuel feed and a combustion temperature of more than 50° C. below the combustion conditions employed when the introduced exhaust gas contains no fluorine gas or halogen fluoride gases (for example, combustion conditions necessary for decomposition of nitrogen trifluoride gas).
  • a combustion temperature of more than 50° C. below the combustion conditions employed when the introduced exhaust gas contains no fluorine gas or halogen fluoride gases (for example, combustion conditions necessary for decomposition of nitrogen trifluoride gas).
  • the combustion treated exhaust gas is finally fed to wet abatement equipment such as an alkali scrubber connected to the exhaust duct of the combustion-type abatement tower for absorption treatment of hydrogen halides such as hydrogen fluoride, NO x or other decomposed substances such as silicon tetrafluoride.
  • wet abatement equipment such as an alkali scrubber connected to the exhaust duct of the combustion-type abatement tower for absorption treatment of hydrogen halides such as hydrogen fluoride, NO x or other decomposed substances such as silicon tetrafluoride.
  • the exhaust gas treatment system of the invention is equipped with an exhaust gas introduction port, a fuel introduction port, a precombustion chamber, a combustion chamber, an air introduction port and an exhaust duct, and a fluoride passivation film is formed on at least the surface of the combustion chamber.
  • FIG. 1 shows an embodiment of a treatment system for carrying out the exhaust gas treatment process of the invention, which employs a combustion decomposition treatment system whereby a mixed exhaust gas containing fluorine gas or halogen fluoride gases is passed through a flame wall and introduced into a supporting gas vortex stream.
  • the material of the system shown in FIG. 1 must be a highly corrosion resistant material to withstand a flow of fluorine gas or halogen fluoride gases.
  • the combustion chamber 8 is preferably formed of nickel or a nickel-rich alloy or Monel metal, and a fluoride passivation film is preferably formed on its surface.
  • the combustion chamber 8 may be formed of ordinary stainless steel or a steel material, with the surface thereof having a thin-film composed of nickel, nickel alloy electroplating, electrocast plating or nickel alloy electroless plating or a ceramic thin-film composed of alumina or aluminum nitride, which are materials with excellent fluorine gas resistance and heat resistance for spray coating or the like, and a fluoride passivation film formed over the surface of the thin-film.
  • a nickel-boron based electroless plating treatment is preferred to achieve excellent heat resistance.
  • the precombustion chamber 7 also preferably has a fluoride passivation film formed on its surface in the same manner.
  • the system parts are preferably subjected to passivation treatment with fluorine gas beforehand.
  • the proximity of the zone in which the exhaust gas is burned is exposed to particularly high temperatures by heat radiation and heat transmission from the combustion zone.
  • These areas are therefore preferably constructed with nickel or a nickel-rich alloy or Monel metal.
  • An ordinary stainless steel or steel material may be subjected to anti-corrosion treatment such as nickel electroplating, electrocast plating or nickel alloy electroless plating.
  • the system members are also preferably subjected to passivation treatment with fluorine gas, beforehand, in the same manner.
  • the passivation treatment with fluorine gas may be according to a publicly known method, and for example, the method described in Japanese Unexamined Patent Publication No. 11-92912 may be used.
  • the surface of the nickel used for the system parts may be first subjected to forced oxidation and the oxidized film then reacted with fluorine gas to form a fluoride passivation film.
  • the system part used is a stainless steel surface with a nickel thin-film formed thereover, it may be subjected to oxidation and fluorination treatment in the same manner to form a fluoride passivation film on the surface.
  • exhaust gas containing fluorine gas or halogen fluoride gases which is emitted from etching or cleaning steps is introduced into a combustion apparatus equipped with a combustion chamber having a fluoride passivation film formed on its surface, and combustion of the exhaust gas therein allows efficient treatment of the exhaust gas.
  • the invention further provides a semiconductor device fabrication process comprising an etching or cleaning step employing fluorine gas or halogen fluoride gases as the etching gas or cleaning gas and an abatement step wherein the gas containing fluorine gas or halogen fluoride gases emitted from the previous step is burned, the abatement step being carried out in a combustion chamber having a fluoride passivation film formed on its surface.
  • the stainless steel combustion chamber of a combustion-type abatement system and the parts surrounding it were subjected to nickel plating and fluoride passivation treatment, and a combustion-abatement experiment was conducted using fluorine gas.
  • the combustion-type abatement system operating conditions and fluorine introduction conditions are shown in Table 1, and the results of compositional analysis of the exhaust gas emitted after combustion and abatement are shown in Table 2.
  • the combustion chamber temperature was measured with a thermocouple attached to the combustion chamber outer wall.
  • the nitrogen monoxide and nitrogen dioxide concentrations in the exhaust gas after combustion were measured with a gas detector tube, and the hydrogen fluoride gas concentration was measured by infrared spectroscopy.
  • the nitrogen trifluoride was measured using a detector.
  • the exhaust gas after combustion contained absolutely no nitrogen monoxide or nitrogen dioxide, and the total amount of fluorine introduced into the combustion-type abatement system reacted and was converted to hydrogen fluoride gas.
  • the absence of combustion reaction products other than hydrogen fluoride gas, water vapor and carbon dioxide in the combustion exhaust gas was confirmed by infrared spectroscopy and inductively coupled plasma-atomic emission spectroscopy of the sample solution.
  • the operating conditions shown in Table 3 are indicated as the combustion operating conditions under which no nitrogen trifluoride gas was detected in the exhaust gas.
  • the total amount of the nitrogen trifluoride introduced into the combustion-type abatement system reacted and was converted to hydrogen fluoride gas, but nitrogen monoxide and nitrogen dioxide were both produced in the exhaust gas far in excess of permissible concentrations.
  • Example 1 After completing operation of the combustion and abatement, the metal surfaces inside the combustion chambers of Example 1 and Comparative Examples 1, 2, 3, 4 and 5 were analyzed. The measurement was conducted with an energy dispersive X-ray spectroscope. TABLE 13 Detected metals (mass %) Ni Fe Cr Other Example 1 100 0 0 0 Comp. Ex. 1 100 0 0 0 Comp. Ex. 2 100 0 0 0 Comp. Ex. 3 7.7 75.8 16.5 0 Comp. Ex. 4 100 0 0 0 Comp. Ex. 5 7.5 73.5 19 0 Reference SUS316L 12 69.5 16 Mo 2.5 Reference SUS304 8 74 18 0
  • Example 1 The inner surfaces of the precombustion chambers were also subjected to metal surface analysis after the combustion-abatement experiments of Example 1 and Comparative Examples 1, 2, 3, 4 and 5. The measurement was conducted with an energy dispersive X-ray spectroscope. TABLE 14 Detected metals (mass %) Ni Fe Cr Other Example 1 100 0 0 0 Comp. Ex. 1 100 0 0 0 Comp. Ex. 2 100 0 0 0 Comp. Ex. 3 7.9 88.1 7.9 0 Comp. Ex. 4 100 0 0 0 Comp. Ex. 5 9.6 75.8 14.7 0 Reference SUS316L 12 69.5 16 Mo 2.5 Reference SUS304 8 74 18 0
  • Comparative Example 3 was confirmed to have considerable loss of Cr from the material.
  • the Cr concentration was slightly lower in Comparative Example 5 as well.
  • Microscopic observation revealed cracks and peeling of the fluoride formed film, by formation and gasification of Cr fluorides as well as by secondary fluoride-forming reactions converting the stainless steel material Fe from the bivalent to trivalent form.
  • the precombustion chambers When the stainless steel damage conditions of the combustion chambers and precombustion chambers were compared, the precombustion chambers all had greater changes in Cr concentration than the combustion chambers, whether with fluorine gas or nitrogen trifluoride, and the appearances were also notably impaired. This is attributed to predominance of oxidation reaction by oxidizing flame during combustion of the fuel gas in the combustion chamber, and particularly at the wall sections.
  • the treatment process of the invention it is possible to accomplish treatment of fluorine gas or halogen fluoride gases when these are emitted at high concentration or high volume, or when they are in combination with other gases having differing properties, to accomplish simultaneous treatment using the same abatement system.
  • the process of the invention is preferably used in a semiconductor fabrication process and, because, it allows efficient and economical abatement treatment with due consideration to safety and preservation of the environment, it has high potential value for industry.

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  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Treating Waste Gases (AREA)
  • Incineration Of Waste (AREA)
  • Drying Of Semiconductors (AREA)
US10/474,765 2002-02-14 2003-02-13 Method for treating exhaust gas Abandoned US20050115674A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2002-037344 2002-02-14
JP2002037344A JP4172938B2 (ja) 2002-02-14 2002-02-14 排ガスの処理方法および処理装置
PCT/JP2003/001507 WO2003069228A1 (fr) 2002-02-14 2003-02-13 Procede de traitement de gaz d'echappement

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US (1) US20050115674A1 (ja)
JP (1) JP4172938B2 (ja)
KR (1) KR100544760B1 (ja)
CN (1) CN1259524C (ja)
AU (1) AU2003211966A1 (ja)
HK (1) HK1066262A1 (ja)
TW (1) TW592797B (ja)
WO (1) WO2003069228A1 (ja)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120100491A1 (en) * 2009-01-30 2012-04-26 Central Glass Company, Limited Semiconductor Production Equipment Including Fluorine Gas Generator
US20140054464A1 (en) * 2012-08-20 2014-02-27 Sabic Innovative Plastics Ip B.V. Real-time online determination of caustic in process scrubbers using near infrared spectroscopy and chemometrics
GB2554406A (en) * 2016-09-26 2018-04-04 Edwards Korea Ltd Plasma abatement
US10168049B2 (en) * 2014-05-15 2019-01-01 Tokyo Electron Limited Method for preventing explosion of exhaust gas in decompression processing apparatus
US10844301B2 (en) * 2015-11-04 2020-11-24 Haffner Energy Method for producing a synthesis gas
CN113767281A (zh) * 2019-11-27 2021-12-07 昭和电工株式会社 由质谱仪测定含卤素氟化物气体中的氟气浓度的测定方法

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JP4751091B2 (ja) * 2005-04-08 2011-08-17 関東電化工業株式会社 排ガスの処理方法
GB0509944D0 (en) * 2005-05-16 2005-06-22 Boc Group Plc Gas combustion apparatus
JP4912163B2 (ja) * 2007-01-12 2012-04-11 ステラケミファ株式会社 フッ化不動態膜を形成した炭素鋼又は特殊鋼及びその形成方法
JP2010276307A (ja) * 2009-05-29 2010-12-09 Japan Pionics Co Ltd 熱分解装置
CN102163643B (zh) * 2010-10-09 2013-01-02 浙江哈氟龙新能源有限公司 废气处理热循环烘干***
CN106884134B (zh) * 2015-12-16 2020-07-03 中国科学院上海应用物理研究所 一种镍基合金的表面钝化处理方法
CN106524191A (zh) * 2016-10-31 2017-03-22 江苏优瑞德环境科技有限公司 含氟烷烃废气焚烧处理工艺及装置
CN113785190A (zh) * 2019-11-27 2021-12-10 昭和电工株式会社 由紫外光谱法测定含卤素氟化物气体所含的氟气浓度的测定方法
CN112827341B (zh) * 2020-12-25 2022-05-17 北京京仪自动化装备技术股份有限公司 一种半导体工艺的废气处理***及其废气的处理方法

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US5183647A (en) * 1988-04-11 1993-02-02 Mitsui Toatsu Chemicals, Inc. Method for purifying nitrogen trifluoride gas
US5009963A (en) * 1988-07-20 1991-04-23 Tadahiro Ohmi Metal material with film passivated by fluorination and apparatus composed of the metal material
US6039261A (en) * 1990-09-24 2000-03-21 Pavese; Guy Process for improving the combustion of a blow-type burner
US5510093A (en) * 1994-07-25 1996-04-23 Alzeta Corporation Combustive destruction of halogenated compounds
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120100491A1 (en) * 2009-01-30 2012-04-26 Central Glass Company, Limited Semiconductor Production Equipment Including Fluorine Gas Generator
US20140054464A1 (en) * 2012-08-20 2014-02-27 Sabic Innovative Plastics Ip B.V. Real-time online determination of caustic in process scrubbers using near infrared spectroscopy and chemometrics
US9084975B2 (en) * 2012-08-20 2015-07-21 Sabic Global Technologies B.V. Real-time online determination of caustic in process scrubbers using near infrared spectroscopy and chemometrics
US20150251131A1 (en) * 2012-08-20 2015-09-10 Sabic Global Technologies B.V. Real-Time Online Determination Of Caustic In Process Scrubbers Using Near Infrared Spectroscopy And Chemometrics
US9636629B2 (en) * 2012-08-20 2017-05-02 Sabic Global Technologies B.V. Real-time online determination of caustic in process scrubbers using near infrared spectroscopy and chemometrics
US10168049B2 (en) * 2014-05-15 2019-01-01 Tokyo Electron Limited Method for preventing explosion of exhaust gas in decompression processing apparatus
US10844301B2 (en) * 2015-11-04 2020-11-24 Haffner Energy Method for producing a synthesis gas
GB2554406A (en) * 2016-09-26 2018-04-04 Edwards Korea Ltd Plasma abatement
CN113767281A (zh) * 2019-11-27 2021-12-07 昭和电工株式会社 由质谱仪测定含卤素氟化物气体中的氟气浓度的测定方法
EP4067300A4 (en) * 2019-11-27 2024-01-03 Resonac Corp METHOD FOR MEASURING THE FLUORINE GAS CONCENTRATION IN HALOGEN FLUORIDE CONTAINING GAS USING A MASS SPECTROMETER
US11984308B2 (en) 2019-11-27 2024-05-14 Resonac Corporation Method for measuring concentration of fluorine gas in halogen fluoride-containing gas using mass spectrometer

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Publication number Publication date
TW592797B (en) 2004-06-21
CN1498328A (zh) 2004-05-19
JP4172938B2 (ja) 2008-10-29
CN1259524C (zh) 2006-06-14
WO2003069228A1 (fr) 2003-08-21
KR20030085596A (ko) 2003-11-05
AU2003211966A1 (en) 2003-09-04
JP2003236337A (ja) 2003-08-26
HK1066262A1 (en) 2005-03-18
KR100544760B1 (ko) 2006-01-24
TW200303236A (en) 2003-09-01

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