WO2013137300A1 - Agent d'élimination de composé de silanol, procédé d'élimination de composé de silanol, filtre chimique, et dispositif d'exposition à la lumière - Google Patents

Agent d'élimination de composé de silanol, procédé d'élimination de composé de silanol, filtre chimique, et dispositif d'exposition à la lumière Download PDF

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Publication number
WO2013137300A1
WO2013137300A1 PCT/JP2013/056970 JP2013056970W WO2013137300A1 WO 2013137300 A1 WO2013137300 A1 WO 2013137300A1 JP 2013056970 W JP2013056970 W JP 2013056970W WO 2013137300 A1 WO2013137300 A1 WO 2013137300A1
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silanol compound
activated carbon
oxygen
functional group
containing functional
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PCT/JP2013/056970
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English (en)
Japanese (ja)
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太年 下津
俊 石川
章博 今井
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ニチアス株式会社
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/72—Organic compounds not provided for in groups B01D53/48 - B01D53/70, e.g. hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28069—Pore volume, e.g. total pore volume, mesopore volume, micropore volume
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • C01B32/354—After-treatment
    • C01B32/372—Coating; Grafting; Microencapsulation
    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
    • G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
    • G03F7/70—Microphotolithographic exposure; Apparatus therefor
    • G03F7/708—Construction of apparatus, e.g. environment aspects, hygiene aspects or materials
    • G03F7/70908—Hygiene, e.g. preventing apparatus pollution, mitigating effect of pollution or removing pollutants from apparatus
    • G03F7/70925—Cleaning, i.e. actively freeing apparatus from pollutants, e.g. using plasma cleaning
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/102—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/55—Compounds of silicon, phosphorus, germanium or arsenic
    • B01D2257/553—Compounds comprising hydrogen, e.g. silanes

Definitions

  • the present invention relates to a silanol compound removing agent for removing a silanol compound, such as removal of a silanol compound in air to be treated containing the silanol compound.
  • HMDS hexamethyldisilazane
  • Patent Document 1 Japanese Patent Laid-Open No. 2009-295765 discloses that silanols are brought into contact with a fibrous inorganic compound having a hydroxyl group, and the silanols are chemically bonded to the fibrous inorganic compound. A method for purifying a substrate to be collected and removed is disclosed.
  • Patent Document 2 Japanese Patent Application Laid-Open No. 2011-166085
  • adsorbents composed of a porous body, and at least a part of the large number of adsorbents includes a metal catalyst (platinum or palladium).
  • a supported chemical filter is disclosed.
  • the chemical filter employs a method in which a silanol compound is dimerized in a filter portion on which a metal catalyst is supported, and the dimer is adsorbed on a filter portion on which the metal catalyst is not supported.
  • Patent Document 3 Japanese Patent Application Laid-Open No. 2012-30164 discloses a dehumidifying unit that dehumidifies air containing a silanol compound to a relative humidity of 33% or less, and air dehumidified by the dehumidifying unit.
  • An air purification system comprising a chemical filter for filtering and removing the silanol compound is disclosed.
  • Cited Document 1 a mechanism for maintaining the surface temperature of the inorganic fiber compound at 70 to 300 ° C. is necessary, and it is not practical to mount it on an exposure apparatus or the like in which the temperature and humidity are extremely precisely controlled. It will also be expensive.
  • Cited Document 2 an expensive metal catalyst is used, a part on which the metal catalyst is supported, and a part for adsorbing the dimer of the silanol compound are required, so that the filter layer becomes thick. It is not economical.
  • an object of the present invention is to provide a silanol compound removing agent having a high effect of removing a silanol compound, in particular, a high effect of removing a silanol compound in air to be treated.
  • the subject of this invention is providing the removal method of the silanol compound with the high removal effect of the silanol compound in to-be-processed air.
  • the present inventors have made contact with a silanol compound, particularly trimethylsilanol, by contacting activated carbon into which an oxygen-containing functional group has been introduced.
  • the silanol compound can be dimerized by the action of the functional group, and by dimerizing the silanol compound, it can be easily adsorbed on the activated carbon, and the amount of oxygen-containing functional group in the activated carbon is in a specific range.
  • the removal effect of silanol compounds, particularly trimethylsilanol compounds is increased, and the present invention has been completed.
  • the present invention (1) is activated carbon having an oxygen-containing functional group, and the amount of the oxygen-containing functional group per 1 g of the activated carbon having the oxygen-containing functional group is 0.5 mmol / g or more.
  • a silanol compound removing agent is provided.
  • this invention (2) produced
  • a method for removing a silanol compound characterized in that the silanol compound in the air to be treated is removed by adsorbing the dimer of the silanol compound to activated carbon having the oxygen-containing functional group. is there.
  • the present invention (3) carries out the silanol compound removal method of the present invention (2), characterized in that activated carbon having an oxygen-containing functional group of 0.5 mmol / g or more per gram is used.
  • a chemical filter is provided.
  • the present invention (4) provides an exposure apparatus having the chemical filter of the present invention (3).
  • a silanol compound removing agent having a high effect of removing a silanol compound, in particular, a high effect of removing a silanol compound in air to be treated.
  • the removal method of the silanol compound with the high removal effect of the silanol compound in to-be-processed air can be provided.
  • the chemical filter with the high removal effect of the silanol compound in to-be-processed air can be provided.
  • the silanol compound removing agent of the present invention is activated carbon having an oxygen-containing functional group, and the amount of the oxygen-containing functional group per 1 g of the activated carbon having the oxygen-containing functional group is 0.5 mmol / g or more. Silanol compound remover.
  • the silanol compound removing agent of the present invention is activated carbon having an oxygen-containing functional group, that is, activated carbon into which an oxygen-containing functional group has been introduced. That is, the activated carbon having an oxygen-containing functional group is activated carbon in which an oxygen-containing functional group is bonded to a carbon atom of the activated carbon.
  • the silanol compound removing agent of the present invention is activated carbon that has been oxidized, and activated carbon into which an oxygen-containing functional group has been introduced by oxidation.
  • oxygen-containing functional group examples include a carbonyl group, a hydroxyl group, a lactone group, a carboxyl group, a quinone group, and a carboxylic anhydride group.
  • the activated carbon having an oxygen-containing functional group preferably has at least one or more of a carbonyl group, a hydroxyl group, a lactone group and a carboxyl group as the oxygen-containing functional group, and at least a carbonyl group, a hydroxyl group It is particularly preferable to have a lactone group and a carboxyl group.
  • the amount of the oxygen-containing functional group per 1 g of the activated carbon having an oxygen-containing functional group is 0.5 mmol / g or more, preferably 0.8 to 3.0 mmol / g, particularly preferably 1.0 to 2.5 mmol / g. It is. When the amount of the oxygen-containing functional group per 1 g of the activated carbon having the oxygen-containing functional group is within the above range, the effect of removing the silanol compound is enhanced.
  • the amount of oxygen-containing functional groups per 1 g of activated carbon having oxygen-containing functional groups and the amount of each functional group are measured as follows. First, activated carbon having an oxygen-containing functional group is vacuum-dried for 8 to 10 hours in a constant temperature dryer adjusted to 115 ° C., and then allowed to cool in a desiccator containing silica gel as a desiccant. Next, four 50 ml stoppered Erlenmeyer flasks (A, B, C, D) are prepared, and 1 g of cooled activated carbon is accurately weighed to 0.1 mg in each Erlenmeyer flask.
  • an N / 10 sodium hydrogen carbonate aqueous solution was added to the Erlenmeyer flask (D)
  • an N / 10 sodium carbonate aqueous solution was added to the Erlenmeyer flask (C)
  • an N / 10 sodium hydroxide aqueous solution was added to the Erlenmeyer flask (B)
  • an Erlenmeyer flask (A ) 25 ml of N / 10 sodium ethoxide ethanol solution is added to the solution and shaken at 160 rpm at 25 ° C. for 24 hours.
  • the supernatant and precipitate are separated by centrifugation, and 10 ml of the supernatant is accurately weighed into a 20 ml beaker and titrated with N / 10 hydrochloric acid until the pH is 4 using a pH meter.
  • the consumption of each base per gram of activated carbon is calculated from the hydrochloric acid titration amount according to the following formula.
  • the substance removed by the silanol compound removing agent of the present invention is a silanol compound contained in the air to be treated.
  • a silanol compound is a compound having a silanol group (—Si—OH).
  • a silanol compound having a molecular weight of 300 or less is preferable, and a silanol compound having a molecular weight of 200 or less is particularly preferable.
  • examples of the silanol compound include trimethylsilanol and triethylsilanol.
  • the silanol compound removing agent of this invention has a remarkable effect especially when to-be-processed air contains a trimethylsilanol.
  • the BET specific surface area of the activated carbon having an oxygen-containing functional group is preferably 500 to 2000 m 2 / g, particularly preferably 800 to 1700 m 2 / g.
  • the silanol compound removal effect is enhanced.
  • the average pore diameter of the activated carbon having an oxygen-containing functional group is preferably 0.4 to 3.0 nm, particularly preferably 0.6 to 2.5 nm.
  • the total pore volume of the activated carbon having an oxygen-containing functional group is preferably 0.30 to 2.00 cm 3 / g, particularly preferably 0.40 to 1.50 cm 3 / g.
  • Examples of a method for producing activated carbon having an oxygen-containing functional group include a method of oxidizing activated carbon in a gas phase or a liquid phase.
  • the BET specific surface area of the raw material activated carbon is preferably 600 to 2000 m 2 / g, particularly preferably 900 to 1800 m 2 / g.
  • the average pore diameter of the raw material activated carbon is preferably 0.4 to 3.0 nm, particularly preferably 0.6 to 2.5 nm.
  • the total pore volume of the starting activated carbon is preferably 0.30 to 2.00 cm 3 / g, particularly preferably 0.40 to 1.50 cm 3 / g.
  • a method of oxidizing activated carbon in the gas phase a method of oxidizing activated carbon with ozone gas, a method of oxidizing with chlorine gas, a method of air oxidation by heating in air, a combination of oxygen treatment and nitrogen oxide treatment, oxygen Examples thereof include low-temperature plasma treatment with gas or air.
  • activated carbon is converted into ozone aqueous solution, nitric acid aqueous solution, hydrogen peroxide aqueous solution, sulfuric acid solution, chloric acid solution, iodic acid solution, hypochlorous acid solution, bromine aqueous solution, permanganic acid.
  • the method of immersing in a potassium solution etc. is mentioned.
  • the oxidized activated carbon is thoroughly washed with pure water and dried at about 80 to 120 ° C.
  • the oxidation conditions of the activated carbon are selected as appropriate, but the condition that the amount of the oxygen-containing functional group per 1 g of activated carbon is 0.5 mmol / g or more, preferably 0.8 to 3.0 mmol / g, particularly A condition of 1.0 to 2.5 mmol / g is preferably selected.
  • the silanol compound removing agent of the present invention is used for removing a silanol compound such as removal of a silanol compound in air to be treated containing the silanol compound.
  • the silanol compound removing agent of the present invention is activated carbon having an oxygen-containing functional group
  • the silanol compound and the oxygen-containing functional group come into contact with the oxygen-containing functional group, for example, by contact with the air to be treated containing the silanol compound.
  • the unshared electron pair of the oxygen atom of the oxygen-containing functional group in the activated carbon having an oxygen-containing functional group is bonded to the hydrogen atom of the silanol group in the silanol compound. It is considered that two silanol compounds in which a hydrogen atom of a silanol group is bonded to an unshared electron pair of an oxygen atom of an oxygen-containing functional group present in the vicinity undergoes dehydration condensation to dimerize.
  • the dimerization reaction is “2R 3 SiOH ⁇ R 3 SiOSiR 3 + H 2 O”.
  • the present inventors have found that dimerization of the silanol compound occurs even at a low temperature of 5 to 40 ° C., preferably 10 to 30 ° C., due to the action of the oxygen-containing functional group introduced into the activated carbon, and that the silanol compound is dimerized. As a result, the molecular weight of the object to be removed can be increased, so that it can be easily adsorbed on the activated carbon.
  • the amount of the oxygen-containing functional group per 1 g of the activated carbon having an oxygen-containing functional group is 0.5 mmol / g or more, preferably 0.8 to 3.0 mmol / g, particularly preferably 1.0 to 2.5 mmol.
  • silanol compound remover of the present invention even low molecular weight silanol compounds such as trimethylsilanol, which have been conventionally considered difficult to adsorb and remove with activated carbon due to the low molecular weight, are adsorbed on activated carbon. Can be removed. Further, according to the silanol compound removing agent of the present invention, it is possible to remove the silanol compound such as removal of the silanol compound from the air to be treated at a low temperature of 5 to 40 ° C., preferably 10 to 30 ° C.
  • the silanol compound removing agent of the present invention exhibits an excellent silanol compound removing effect in removing silanol compounds in air to be treated containing a silanol compound having a relative humidity of 45% or less.
  • the lower limit of the relative humidity is not particularly limited, but the relative humidity is preferably 15% or more, particularly preferably 20% or more, and further preferably 25% or more.
  • Examples of the method for removing the silanol compound in the air to be treated using the silanol compound removing agent of the present invention include a method of bringing the silanol compound removing agent of the present invention into contact with the air to be treated containing the silanol compound.
  • the air to be treated that is treated with the silanol compound removing agent of the present invention is not particularly limited.
  • silanol such as air in an optical system installation space of an exposure apparatus for semiconductor production, air in a clean room for semiconductor production, etc. Air containing a compound.
  • the silanol compound contained in the air to be treated is a compound having a silanol group (—Si—OH), and examples thereof include trimethylsilanol and triethylsilanol.
  • the silanol compound removing agent of this invention has a remarkable effect especially when to-be-processed air contains a trimethylsilanol.
  • the content of the silanol compound in the air to be treated is not particularly limited. For example, in the case of air in the optical system installation space of an exposure apparatus for manufacturing a semiconductor, it is usually 0.3 to 8.0 ppb.
  • the silanol compound removing agent of the present invention is suitably used as a silanol compound removing agent for carrying out the silanol compound removing method of the present invention described below. That is, the silanol compound removal method of the present invention is such that the silanol compound remover of the present invention is brought into contact with the treated air containing the silanol compound to dimerize the silanol compound, and the dimer of the generated silanol compound is dimerized.
  • a silanol compound removing method comprising removing a silanol compound in the air to be treated by adsorbing a body to activated carbon having the oxygen-containing functional group.
  • activated carbon having an oxygen-containing functional group of 0.5 mmol / g or more per 1 g is brought into contact with the air to be treated containing the silanol compound to dimerize the silanol compound.
  • the silanol compound removal method is characterized in that the silanol compound in the air to be treated is removed by adsorbing the dimer of the silanol compound to the activated carbon having the oxygen-containing functional group.
  • the activated carbon having an oxygen-containing functional group according to the method for removing a silanol compound of the present invention is the same as the activated carbon having an oxygen-containing functional group according to the silanol compound removing agent of the present invention.
  • activated carbon having an oxygen-containing functional group is brought into contact with the air to be treated containing the silanol compound.
  • the air to be treated is not particularly limited, but is air containing a silanol compound such as air in an optical system installation space of an exposure apparatus for semiconductor manufacturing, air in a clean room for semiconductor manufacturing, and the like.
  • the silanol compound contained in the air to be treated is a compound having a silanol group (—Si—OH).
  • a silanol compound having a molecular weight of 300 or less is preferable, and a silanol compound having a molecular weight of 200 or less is particularly preferable.
  • examples of the silanol compound include trimethylsilanol and triethylsilanol.
  • the content of the silanol compound in the air to be treated is not particularly limited.
  • it is usually 0.3 to 8.0 ppb.
  • the method of bringing the air to be treated into contact with the activated carbon having an oxygen-containing functional group is not particularly limited.
  • the activated carbon having an oxygen-containing functional group is formed by filling activated carbon having an oxygen-containing functional group into a filling container. Examples thereof include a method of allowing the air to be treated to pass through the activated carbon layer, a method of supporting the activated carbon having an oxygen-containing functional group on a carrier, and allowing the air to be treated to pass through the carrier.
  • the temperature when the air to be treated is brought into contact with activated carbon having an oxygen-containing functional group is 5 to 40 ° C., preferably 10 to 30 ° C.
  • the supply amount of the air to be treated when the air to be treated is brought into contact with the activated carbon having the oxygen-containing functional group is appropriately selected depending on the content of the silanol compound in the air to be treated, the amount of the activated carbon having the oxygen-containing functional group, etc. Is done.
  • the activated carbon having an oxygen-containing functional group is brought into contact with the treated air containing the silanol compound to bring the activated carbon having an oxygen-containing functional group into contact with the activated carbon having the oxygen-containing functional group.
  • the unshared electron pair of the oxygen atom of the oxygen-containing functional group and the hydrogen atom of the silanol group in the silanol compound are bonded to each other, and then to the unshared electron pair of the oxygen atom of the oxygen-containing functional group present in the vicinity
  • Two silanol compounds to which the hydrogen atom of the silanol group is bonded are considered to undergo dehydration condensation and dimerization.
  • the dimerization reaction is “2R 3 SiOH ⁇ R 3 SiOSiR 3 + H 2 O”.
  • the present inventors have found that dimerization of the silanol compound occurs even at a low temperature of 5 to 40 ° C., preferably 10 to 30 ° C., due to the action of the oxygen-containing functional group introduced into the activated carbon, and that the silanol compound is dimerized. Since the molecular weight of the object to be removed can be increased, it can be easily adsorbed on the activated carbon, and the amount of oxygen-containing functional groups in the activated carbon is within a specific range, thereby removing the silanol compound. Found to be higher.
  • the amount of the oxygen-containing functional group per 1 g of the activated carbon having an oxygen-containing functional group is 0.5 mmol / g or more, preferably 0.8 to 3.0 mmol / g, particularly preferably 1.0 to 2.5 mmol. It was found that the effect of removing the silanol compound is enhanced by setting the amount to / g. Therefore, according to the silanol compound removal method of the present invention, even low molecular weight silanol compounds, such as trimethylsilanol, which have been conventionally considered difficult to adsorb and remove with activated carbon due to low molecular weight, are adsorbed on activated carbon. Can be removed. Further, according to the silanol compound removal method of the present invention, the silanol compound in the air to be treated can be removed at a low temperature of 5 to 40 ° C., preferably 10 to 30 ° C.
  • Activated carbon having an oxygen-containing functional group of 0.5 mmol / g or more per gram is an excellent silanol compound particularly in removing silanol compounds in air to be treated containing a silanol compound having a relative humidity of 45% or less. Demonstrate the removal effect. Therefore, in the method for removing a silanol compound of the present invention, the relative humidity of the air to be treated containing the silanol compound is preferably 45% or less.
  • the lower limit of the relative humidity is not particularly limited, but the relative humidity is preferably 15% or more, particularly preferably 20% or more, and further preferably 25% or more. That is, in the silanol compound removal method of the present invention, the relative humidity of the air to be treated containing the silanol compound is preferably 15 to 45%, particularly preferably 20 to 45%, and further preferably 25 to 45%.
  • the chemical filter of the present invention is a chemical filter for carrying out the method for removing a silanol compound of the present invention, and is activated carbon having an oxygen-containing functional group of 0.5 mmol / g or more per gram (silanol compound removing agent of the present invention). Activated carbon having an oxygen-containing functional group according to the method for removing a silanol compound of the present invention) is used.
  • the activated carbon having an oxygen-containing functional group according to the chemical filter of the present invention is the same as the activated carbon having an oxygen-containing functional group according to the silanol compound removing agent of the present invention.
  • Examples of the chemical filter of the present invention include a chemical filter in which activated carbon having an oxygen-containing functional group of 0.5 mmol / g or more per gram is filled in a gas-permeable filling container to form an activated carbon layer.
  • the chemical filter of the present invention includes a chemical filter in which activated carbon having an oxygen-containing functional group of 0.5 mmol / g or more per 1 g is supported on a carrier.
  • the carrier on which the activated carbon having an oxygen-containing functional group is supported is not particularly limited and is used as a carrier for a chemical filter.
  • an inorganic fibrous base material (paper) composed of inorganic fibers is formed into a honeycomb structure or a pleated structure
  • an organic fibrous base material (paper) composed of organic fibers is honeycomb.
  • examples thereof include an organic fibrous carrier molded into a structure or a pleated structure.
  • a pleated structure is preferable because it can increase the amount of activated carbon per unit volume and has a low pressure loss.
  • the method for supporting activated carbon having oxygen-containing functional groups is not particularly limited.
  • the activated carbon having an oxygen-containing functional group may be supported on a carrier by using a binder, or an inorganic fiber
  • Activated carbon having oxygen-containing functional groups may be supported by a sheet of quality or organic fiber so as to be supported.
  • air to be treated containing a silanol compound for example, air in an optical system installation space of an exposure apparatus for manufacturing a semiconductor, air in a clean room for manufacturing a semiconductor, etc.
  • the activated carbon having an oxygen-containing functional group of 0.5 mmol / g or more per gram particularly in the removal of the silanol compound in the air to be treated containing a silanol compound having a relative humidity of 45% or less, Since the chemical filter of the present invention in which such activated carbon is used exhibits an excellent silanol compound removal effect, the removal of the silanol compound in the treated air containing the silanol compound having a relative humidity of 45% or less In, it has excellent silanol compound removal performance.
  • the exposure apparatus of the present invention is an exposure apparatus having the chemical filter of the present invention.
  • the chemical filter according to the exposure apparatus of the present invention is the same as the chemical filter of the present invention.
  • the structure of the exposure apparatus of the present invention is not particularly limited, and may be any exposure apparatus that is usually used for semiconductor manufacturing.
  • the exposure apparatus of the present invention is provided with an optical system installation space in which an optical system member and an exposure object are installed and can be shielded from external air. Further, the exposure apparatus of the present invention extracts the air in the optical system installation space and returns the air in the optical system installation space back to the optical system installation space and the air in the clean room in the optical system installation space. And an external air intake path for intake.
  • the chemical filter of the present invention is installed in each of the circulation path and the external air intake path.
  • the exposure apparatus of the present invention includes a relay lens system, a condenser lens system, a projection optical system lens (hereinafter also referred to as an optical system member), and an installation portion for an exposure object.
  • the optical system member and the exposure object are installed in a small chamber that can be cut off from the outside air, so that the space of the installation part in which the optical system member and the exposure object are installed ( Hereinafter, it is also referred to as an optical system installation space.) Is cut off from outside air.
  • air in the optical system installation space is extracted and returned to the optical system installation space, and the air circulation path in the optical system installation space and the air in the clean room are taken into the optical system installation space.
  • An external air intake path, and the chemical filter of the present invention is installed in each of the circulation path and the external air intake path.
  • the air in the optical system installation space extracted from the optical system installation space in the circulation path is extracted by passing through the chemical filter installed in the circulation path.
  • silanol compounds in the air in the optical system installation space particularly trimethylsilanol, are removed.
  • the air from which silanol compounds such as trimethylsilanol have been removed is returned to the optical system installation space again.
  • the air taken in from the clean room passes through the chemical filter installed in the external air intake path, so that the air in the clean room taken in The silanol compound, especially trimethylsilanol, is removed.
  • the air from which silanol compounds such as trimethylsilanol have been removed is supplied to the optical system installation space.
  • an N / 10 sodium hydrogen carbonate aqueous solution was added to the Erlenmeyer flask (D)
  • an N / 10 sodium carbonate aqueous solution was added to the Erlenmeyer flask (C)
  • an N / 10 sodium hydroxide aqueous solution was added to the Erlenmeyer flask (B)
  • an Erlenmeyer flask (A ) 25 ml of N / 10 sodium ethoxide ethanol solution was added to the solution and shaken at 160 rpm at 25 ° C. for 24 hours.
  • Base consumption (mmol / g) (0.1 ⁇ (10 ⁇ HCl titration) ⁇ 25) / 10
  • the consumption of sodium bicarbonate is D (mmol / g)
  • the consumption of sodium carbonate is C (mmol / g)
  • the consumption of aqueous sodium hydroxide is B (mmol / g)
  • the consumption of sodium ethoxide is A (Mmol / g)
  • the oxygen-containing functional group amount per 1 g of activated carbon is “A (mmol / g)”
  • the carbonyl group amount is “AB (mmol / g)”.
  • the amount of lactone group is “CD (mmol / g)”
  • the amount of carboxyl group is “D (mmol / g)”.
  • ⁇ Trimethylsilanol removal test> As shown in FIG. 1, a test sample having a thickness of 5 mm (length in the aeration direction of the air to be treated) is inserted in a hollow glass tube 2 having an inner diameter of 20 mm and a length of 300 mm by a support member 4. A layer (activated carbon layer) 3 was formed to produce a trimethylsilanol removal test apparatus 1.
  • Example 3 and Comparative Example 3 150 ppb trimethylsilanol-containing air (temperature: 23 ° C., relative humidity: 45% (Example 1 and Comparative Example 1), 35% (Example 2 and Comparative Example 2), or 25% (Example 3 and Comparative Example) Example 3)) was supplied from the gas inlet 21 and discharged from the gas outlet 22, and the air to be treated was vented to the test sample layer 3 at a wind speed of 0.3 m / sec.
  • Trimethylsilanol removal rate (%) ((trimethylsilanol concentration at the inlet side ⁇ trimethylsilanol concentration at the outlet side) / trimethylsilanol concentration at the inlet side) ⁇ 100
  • Example 1 Oxidation was performed by exposing 50 g of activated carbon a having a crushed shape average particle size of 32/60 mesh (0.25 to 0.50 mm) and a specific surface area of 1500 m 2 / g in a 1% ozone atmosphere for 8 hours.
  • the amount of oxygen-containing functional groups of the obtained activated carbon A having oxygen-containing functional groups was measured, the amount of oxygen-containing functional groups was 1.57 mmol / g, the amount of carbonyl groups was 0.35 mmol / g, and the amount of hydroxyl groups was 0.59 mmol. / G, the amount of lactone groups was 0.33 mmol / g, and the amount of carboxyl groups was 0.30 mmol / g.
  • the specific surface area of the obtained activated carbon A having an oxygen-containing functional group was 1500 m 2 / g, the average pore diameter was 0.7 nm, and the total pore volume was 0.78 cm 3 / g.
  • the trimethylsilanol removal test apparatus 1 shown in FIG. 1 is filled with activated carbon A having an oxygen-containing functional group and 150 ppb of trimethylsilanol containing 150 ppb of trimethylsilanol containing air at a temperature of 23 ° C. and a relative humidity of 45%. Trimethylsilanol removal test was performed using air. The results are shown in Table 1 and FIG.
  • Example 1 (Analysis of adsorption amount of dimer of silanol compound)
  • activated carbon after the trimethylsilanol removal test in Example 1, after 234.1 hours test, in Comparative Example 1 after 99.3 hours test
  • 0.1 g was collected in a vial.
  • 2 mL of dichloromethane was added to the vial and shaken for extraction.
  • the extract was quantitatively analyzed by GC-MS, and the ratio of the trimers of trimethylsilanol and trimethylsilanol in the substance adsorbed on the activated carbon was determined.
  • Example 1 trimethylsilanol was 12 mass%, and the dimer of trimethylsilanol was 88 mass%.
  • Comparative Example 1 trimethylsilanol was 76% by mass, and trimethylsilanol dimer was 24% by mass.
  • Example 2 In the same manner as in Example 1, activated carbon A having an oxygen-containing functional group was obtained.
  • the trimethylsilanol removal test apparatus 1 shown in FIG. 1 is filled with activated carbon A having an oxygen-containing functional group, and 150 ppb of trimethylsilanol containing 150 ppb of trimethylsilanol containing air at a temperature of 23 ° C. and a relative humidity of 35%. Trimethylsilanol removal test was performed using air. The results are shown in Table 3 and FIG.
  • Comparative Example 2 Activated carbon a used in Comparative Example 1 was prepared. Next, activated carbon a is filled in the trimethylsilanol removal test apparatus 1 shown in FIG. 1, and 150 ppb of trimethylsilanol-containing air having a temperature of 23 ° C. and a relative humidity of 35% is used as 150 ppb of trimethylsilanol-containing air. A silanol removal test was conducted. The results are shown in Table 4 and FIG.
  • Example 3 In the same manner as in Example 1, activated carbon A having an oxygen-containing functional group was obtained. Next, the trimethylsilanol removal test apparatus 1 shown in FIG. 1 is filled with activated carbon A having an oxygen-containing functional group, and 150 ppb of trimethylsilanol containing 150 ppb of trimethylsilanol containing air at a temperature of 23 ° C. and a relative humidity of 25%. Trimethylsilanol removal test was performed using air. The results are shown in Table 5 and FIG.
  • Comparative Example 3 Activated carbon a used in Comparative Example 1 was prepared. Next, activated carbon a is filled in the trimethylsilanol removal test apparatus 1 shown in FIG. 1, and trimethylsilanol-containing air having a temperature of 23 ° C. and a relative humidity of 25% is used as 150 ppb of trimethylsilanol-containing air. A silanol removal test was conducted. The results are shown in Table 6 and FIG.
  • Relative humidity Relative humidity of air containing trimethylsilanol used in the test

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Abstract

L'agent d'élimination de composé de silanol ci-décrit est caractérisé en ce que c'est un charbon actif ayant un groupe fonctionnel contenant de l'oxygène, et en ce qu'il a au moins 0,5 mmol/g dudit groupe fonctionnel contenant de l'oxygène par gramme de charbon actif. L'agent d'élimination de composé de silanol selon l'invention a un effet élevé d'élimination de composé de silanol.
PCT/JP2013/056970 2012-03-13 2013-03-13 Agent d'élimination de composé de silanol, procédé d'élimination de composé de silanol, filtre chimique, et dispositif d'exposition à la lumière WO2013137300A1 (fr)

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WO2014077305A1 (fr) * 2012-11-16 2014-05-22 ニチアス株式会社 Agent d'élimination de composés de silanol
CN110467183A (zh) * 2019-09-09 2019-11-19 上海纳米技术及应用国家工程研究中心有限公司 高效去除空气中苯的柱状活性炭的制备工艺及其产品和应用
WO2023117432A1 (fr) * 2021-12-20 2023-06-29 Asml Netherlands B.V. Alimentation en gaz de purge

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JPH02118121A (ja) * 1988-10-25 1990-05-02 Osaka Gas Co Ltd ピッチ系活性炭素繊維およびその製造方法
JP2009295765A (ja) * 2008-06-05 2009-12-17 Ebara Corp シラノール類を捕集除去する気体浄化方法と装置
WO2011099616A1 (fr) * 2010-02-15 2011-08-18 ニッタ株式会社 Filtre chimique comprenant un agent d'imprégnation acide
JP2011166085A (ja) * 2010-02-15 2011-08-25 Nitta Corp 金属触媒担持ケミカルフィルタ
JP2011212531A (ja) * 2010-03-31 2011-10-27 Kuraray Chemical Co Ltd アルキルシラノール除去材及びそれを製造する方法
JP2012030163A (ja) * 2010-07-29 2012-02-16 Nitta Corp 空気浄化システム
JP2012055807A (ja) * 2010-09-07 2012-03-22 Kureha Corp トリメチルシラノール用吸着剤、及びそれを担持したケミカルフィルタ

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JPH02118121A (ja) * 1988-10-25 1990-05-02 Osaka Gas Co Ltd ピッチ系活性炭素繊維およびその製造方法
JP2009295765A (ja) * 2008-06-05 2009-12-17 Ebara Corp シラノール類を捕集除去する気体浄化方法と装置
WO2011099616A1 (fr) * 2010-02-15 2011-08-18 ニッタ株式会社 Filtre chimique comprenant un agent d'imprégnation acide
JP2011166085A (ja) * 2010-02-15 2011-08-25 Nitta Corp 金属触媒担持ケミカルフィルタ
JP2011212531A (ja) * 2010-03-31 2011-10-27 Kuraray Chemical Co Ltd アルキルシラノール除去材及びそれを製造する方法
JP2012030163A (ja) * 2010-07-29 2012-02-16 Nitta Corp 空気浄化システム
JP2012055807A (ja) * 2010-09-07 2012-03-22 Kureha Corp トリメチルシラノール用吸着剤、及びそれを担持したケミカルフィルタ

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014077305A1 (fr) * 2012-11-16 2014-05-22 ニチアス株式会社 Agent d'élimination de composés de silanol
CN110467183A (zh) * 2019-09-09 2019-11-19 上海纳米技术及应用国家工程研究中心有限公司 高效去除空气中苯的柱状活性炭的制备工艺及其产品和应用
WO2023117432A1 (fr) * 2021-12-20 2023-06-29 Asml Netherlands B.V. Alimentation en gaz de purge

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