WO2001070366A1 - Dégazeur et procédé de dégazage - Google Patents

Dégazeur et procédé de dégazage Download PDF

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Publication number
WO2001070366A1
WO2001070366A1 PCT/JP2001/002295 JP0102295W WO0170366A1 WO 2001070366 A1 WO2001070366 A1 WO 2001070366A1 JP 0102295 W JP0102295 W JP 0102295W WO 0170366 A1 WO0170366 A1 WO 0170366A1
Authority
WO
WIPO (PCT)
Prior art keywords
liquid
tubular body
tubular
flow path
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.)
Ceased
Application number
PCT/JP2001/002295
Other languages
English (en)
Japanese (ja)
Inventor
Naoyuki Nakamoto
Toshiyuki Nakagawa
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Priority to AU2001242757A priority Critical patent/AU2001242757A1/en
Publication of WO2001070366A1 publication Critical patent/WO2001070366A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/0031—Degasification of liquids by filtration

Definitions

  • the present invention relates to a degassing apparatus and a degassing method for performing degassing by using a tubular membrane through which a dissolved gas in a liquid to be treated permeates, and particularly to a liquid used in a semiconductor device manufacturing process.
  • TECHNICAL FIELD The present invention relates to a degassing apparatus and a degassing method that are useful in a degassing step for performing degassing from a chemical in a gas state.
  • PECVD plasma vapor deposition
  • a gaseous or liquid chemical (precursor) is used as a processing gas.
  • This processing gas is supplied to a gas dispersion head of a deposition station in a reactor, is turned into plasma, and is deposited on a semiconductor substrate to form a thin film.
  • a chemical is supplied in liquid form, it passes through a vaporizer before entering the reactor and is gasified.
  • liquid chemical delivery systems must meet two important criteria. Firstly, liquid chemicals are supplied at a predetermined flow rate at a uniform and stable pressure, and secondly, liquid chemicals are accurately supplied. It does not contain particles and gas when it is gasified so that the liquid can be measured at a high rate. In particular, in a supply system using a pump as a supply source, there are problems such as impurities and difficulties in controlling the pressure and flow rate uniformly, so that gas pressure is used.
  • the main method is to supply liquid chemicals stored in containers.
  • a liquid to be treated (liquid to be supplied) is passed through a tubular membrane (tube) from which dissolved gas can be separated.
  • a deaerator for removing dissolved gas from a liquid to be treated by reducing the pressure of the space outside the tubular membrane.
  • a degassing device As a device for removing dissolved gas, a degassing device as shown in FIG. 4 is known.
  • This apparatus has a horizontal housing 23 provided with a supply port 24 at one end and a discharge port 25 at the other end.
  • a large number of tubular hollow fiber membranes 22 are arranged side by side from one end to the other end at a predetermined interval in an internal space 23 in the housing 23. Module is configured.
  • These hollow fiber membranes 22 are provided with a common decompression port 27, and the housing is provided with an inlet port 2 for supplying a sweep gas to the internal space as necessary. 6 are provided.
  • the liquid to be treated is supplied into the internal space 21 from the supply port 24 and discharged from the discharge port 25, while being discharged through the pressure reducing port 27. 22
  • Dissolved gas present in the processing liquid is sucked into the membrane module and removed from the liquid to be treated.
  • the problem of discharging air bubbles in the degassing process as described above is a problem common to other degassing processes, not limited to degassing at the time of supplying a chemical solution in a semiconductor device manufacturing process.
  • an object of the present invention is to provide a deaerator and a deaeration method capable of effectively removing generated bubbles from a liquid to be treated.
  • a deaerator includes a tubular body having a supply port through which a liquid is supplied and a discharge port through which a liquid is discharged.
  • the flow path is inserted into the tubular body, defines a flow path from the supply port to the discharge port between the tubular body and the liquid flowing through the flow path by being depressurized.
  • at least one tubular membrane through which the dissolved gas in the liquid is permeable At least in part, the downstream side is located lower than the upstream side, and constitutes a bubble blocking portion that prevents generated bubbles from flowing to the downstream side.
  • tubular body and the tubular membrane may have any cross-section, but a circular cross-section is preferable, and it is preferable that both have a concentric tubular configuration.
  • a tubular membrane through which the dissolved gas in the liquid to be treated permeates is inserted into the tubular body, and a liquid flow path such as the liquid to be treated is formed outside the tubular membrane.
  • the pressure difference between the inside and outside of the membrane causes the dissolved gas to pass through the tubular membrane, thereby removing the dissolved gas from the liquid to be treated. it can.
  • at least a part of the tubular body is disposed such that the downstream side is located below the upstream side, and a bubble blocking portion is provided to prevent generated bubbles from flowing to the downstream side.
  • the bubbles can be prevented from flowing downstream due to the buoyancy of the generated bubbles.
  • the bubbles in the case of forming the flow path of the liquid to be treated inside the tubular membrane, if the bubbles become large to some extent, the bubbles will not easily rise in the liquid to be treated due to the buoyancy of the bubbles.
  • the bubbles since the flow path of the liquid to be treated is formed outside the tubular membrane, the bubbles easily rise due to buoyancy, and the bubbles are effectively prevented from flowing downstream. Can be done. As a result, it is possible to provide a deaerator in which generated bubbles are hardly discharged together with the processing liquid.
  • a heating means is preferably provided on at least a part of the outer periphery of the tubular body.
  • the inside of the tubular body can be efficiently heated, the gas permeability of the tubular membrane can be increased, and degassing can be performed efficiently.
  • the relationship between the liquid to be treated and the dissolved gas is such that the solubility is lower at a higher temperature, the bubbles are generated more aggressively by heating, so that the liquid to be dissolved can be removed from the liquid to be treated. Dissolved gas can be removed more efficiently.
  • the degassing apparatus according to any one of the above uses, and thus, due to the above-described effects, generated bubbles are not easily discharged together with the processing liquid. Degassing method.
  • the degassing method of the present invention is particularly useful as a method for degassing a liquid chemical used in a semiconductor manufacturing process where the presence of dissolved gas is particularly problematic. This is a useful technique.
  • FIG. 1 is a cross-sectional view showing a main part of an example of the deaerator of the present invention.
  • FIG. 2 is a schematic configuration diagram showing an example of use of the deaerator of the present invention.
  • 3A and 3B are a side view and a perspective view, respectively, showing a main part of a deaerator according to another embodiment.
  • FIG. 4 is a cross-sectional view showing an essential part of an example of a conventional deaerator.
  • FIG. 1 is a cross-sectional view showing a part of a degassing apparatus according to an embodiment.
  • This apparatus does not allow a liquid to be treated to pass through but allows the dissolved gas in or around it to permeate. It has a linear main tubular membrane 1 formed of a material capable of being extended vertically, and a main tubular body 2 in which the tubular membrane 1 is coaxially inserted.
  • the outer diameter of the tubular membrane 1 is much smaller than the inner diameter of the tubular body 2, and as a result, an annular flow for flowing the liquid to be treated is provided between the tubular membrane 1 and the tubular body 2.
  • Road 3 is formed.
  • the tubular membrane 1 may be any as long as it allows the dissolved gas in the liquid to be treated to permeate, and is a nonporous membrane that has been conventionally used as a degassing separation membrane. And hollow or hollow fiber membranes made of porous membranes. Specifically, a fluororesin such as PTF E. F E P or P F A, or a polyethylene, polypropylene or polyamide separation membrane can be suitably used.
  • the outer surface of the tubular membrane 1 and the inner surface of the Z or tubular body 2 turbulence the flow of the liquid to be treated in the flow path 3 therebetween, so that the liquid to be treated and the tubular membrane 1 are separated from each other.
  • the outer surface of the tubular membrane 1 is formed with irregularities, such as a ganella tube.
  • liquid to be treated for example, in the case of a liquid chemical used in a manufacturing process of a semiconductor device, tetraethyl orthosilicate Salt, trimethyl phosphite, trimethyl borate, triethyl phosphite, triethyl borate, tetrax (ethyl) aminotita And the like.
  • tetraethyl orthosilicate Salt trimethyl phosphite
  • trimethyl borate triethyl phosphite
  • triethyl borate trietrax (ethyl) aminotita And the like.
  • the dissolved gas include helium, nitrogen, neon, argon, carbon dioxide, oxygen and the like.
  • any material may be used as the material of the tubular body 2 as long as there is no inconvenience such as being corroded by the liquid to be treated, but in consideration of corrosion resistance and the like, fluorine resin, SUS, or the like is used. I like it.
  • the cross-sectional area of the tubular flow path 3 is determined by the inner diameter of the tubular body 2 and the outer diameter of the tubular membrane 1, and in the illustrated example, the inner diameter of the tubular body 2 is about 3 to 3 Omm, Preferably, the diameter is 1 to: about LO mm, and the ratio of the two (the former and the latter) is about 4 to 1.2.
  • the tubular body 2 is arranged in a substantially vertical direction such that the downstream side is located below the upstream side, and substantially the entirety of the main tubular body 2 serves as the bubble blocking portion FP.
  • the tubular body 2 may be arranged so that the downstream side is located below the upstream side.
  • a gas reservoir 10 is formed by an auxiliary tubular body 10a extending vertically to be continuous with the main tubular body 2, and an auxiliary fluid connected to the main tubular membrane 1 therein.
  • a tubular membrane 1a is arranged.
  • the auxiliary tubular body 10 a is the same member as the main tubular body 2. They may be formed integrally or may be formed separately and connected.
  • the auxiliary tubular membrane la may be formed integrally with the same member as the main tubular membrane 1, or may be formed separately and connected.
  • the upper end of the auxiliary tubular body 10a is joined to the male side of the resin pipe joint 5, the auxiliary tubular membrane 1a is inserted through the male side, and sealed by tightening the female side.
  • the generated air bubbles rise and collect in the internal space 10 b of the gas reservoir 10, but the accumulated gas is reduced by reducing the pressure inside the auxiliary tubular membrane 1 a. Is removed through the tubular membrane 1a.
  • the upper end of the auxiliary tubular membrane 1a is connected to a pressure reducing pipe 7 via a pipe joint 6 (various fittings).
  • the pressure reducing pipe 7 is connected to a pressure reducing device such as a vacuum pump (not shown). (Omitted).
  • the pressure-reducing pipe 7 is formed of a metal or the like that is difficult for gas to permeate.
  • the boundary between the main tubular body 2 and the auxiliary tubular body 10a is branched into a T shape, and the supply pipe 8 is integrally branched or connected via a supply port. .
  • the lower end of the main tubular body 2 is also branched into a T shape, and a discharge pipe 9 is integrally branched or connected via a discharge port.
  • the liquid to be treated is supplied to the supply pipe 8 from a supply device connected thereto.
  • the liquid to be treated is supplied from a supply port to a flow path 3 formed outside the tubular membrane 1, flows downward in this flow path, and is then discharged to the outside via a discharge pipe 9.
  • the liquid to be treated is degassed while the dissolved gas contained in the liquid to be treated permeates through the tubular membrane 1 while flowing through the flow path 3.
  • the air bubbles generated during this time move upward and temporarily accumulate in the gas storage part 10, and the air bubbles that have accumulated are discharged to the outside through the auxiliary tubular membrane la. Can be done. Bubbles in the liquid to be treated, which are supplied from the supply pipe 8 to the flow path 3, can be similarly discharged through the gas reservoir 10.
  • the main tubular membrane 1 and the main tubular body 2 also extend continuously below the branch portion of the discharge pipe 9 and have the same sealing structure as the upper end.
  • the lower end of the extended portion of the main tubular membrane 1 may be sealed, but a valve may be provided so that a sweep gas can be supplied as necessary.
  • a sweep gas nitrogen gas or the like which is difficult to permeate through the tubular membrane 1 can be suitably used.
  • a heating means is provided on at least a part of the outer peripheral portion of the main tubular body 2 as shown in FIG.
  • an electric heating wire 11 wound around the outer periphery of the tubular body 2 an electric heating heater, or the like can be used.
  • the liquid to be treated is heated from 25 ° C. to 50 ° C., so that the gas permeability coefficient is 1.8 in helium.
  • the ratio is 2.7 times with oxygen and 2.7 times with nitrogen, increasing the degassing effect.
  • FIG. 1 This liquid supply system has a supply source 12, a deaerator DG, and a liquid mass mouth opening controller 17.
  • One end of the supply source 12 is connected to a sealed container 15 filled with the liquid 13 to be treated and a supply source (not shown) for supplying a pressurized gas 14, and the other end is connected to the container 1.
  • the 5 has a gas supply pipe 15a opened in the space above 5 and a liquid discharge pipe 15b connected to the base end of the supply pipe 8 and opened in the liquid to be treated in the container 15 .
  • a supply source 12 by supplying a pressurized gas into the container 15 through the supply pipe 15 a, the liquid 13 to be treated in the container is pressurized. Then, it is discharged to the supply pipe 8 via the discharge pipe 15b.
  • the gas 14 is Helium
  • the liquid 13 to be treated is tetraethyl orthosilicate (TEOS).
  • TEOS tetraethyl orthosilicate
  • Other gases and other liquids that do not chemically react with each other can be used in place of helium and TEOS.
  • TMP trimethyl phosphite
  • TMB trimethyl borate
  • helium gas 14
  • STEOS liquid to be treated 13
  • the flow of the liquid to be treated is interrupted, and the liquid measurement in the liquid is erroneous.
  • the deaerator DG having the above-described configuration effectively removes the helium gas dissolved in the liquid to be processed, which is supplied to the liquid mass flow controller 17. For this reason, the pressure reducing pipe 7 of the deaerator DG is exhausted by an exhaust pump 16 connected thereto. Degassed treatment The liquid is supplied to the liquid mass flow controller 17 via the discharge pipe 9 of the deaerator DG.
  • the liquid mass flow controller 17 is provided so that the liquid 1 can be accurately measured at a desired flow rate and at a uniform pressure for the user. Used to distribute 3.
  • the liquid mass flow controller 17 is any controller known to those skilled in the art.
  • the outlet of the liquid mass opening / cont opening / opening 17 is connected to the PEC VD reactor 18 and to the vaporizer 19 provided in the PEC VD reactor 18.
  • the liquid to be treated 13 is vaporized by a vaporizer to become a gas to be treated, and then sent to a gas dispersion head (not shown).
  • a plurality of liquid mass flow controllers 17 and PECVD reactors 18 may be provided as necessary, and the liquid to be treated is supplied to each pair simultaneously or selectively. Can be done.
  • the length of the main tubular membrane 1 at the portion to be degassed may be determined, for example, as follows. From the scale and number of PECVD reactors 18, calculate the maximum flow rate of the liquid 13 to be treated by the supply source 12 and calculate the maximum flow rate from the solubility of the gas 14 in the liquid 13 to be treated. Find the maximum dissolved amount corresponding to the amount of gas that should be removed per unit time. In a test, degassing is performed with a degassing device equipped with a unit-length main tubular membrane 1, and the above-mentioned gas amount to be removed is divided by the obtained degassing flow rate per unit time. Thus, the length of the tubular membrane 1 is used as a guide.
  • the maximum flow rate of 500 m 1 / min considering the solubility of helium gas, when the inner diameter of the main tubular body 2 is 1 O mm and the outer diameter of the main tubular membrane 1 is 6 mm, the length is 1 to 3 About m is enough for degassing.
  • FIGS. 3A and 3B Next, another embodiment of the present invention will be described with reference to FIGS. 3A and 3B.
  • a straight tubular body is vertically arranged to form a bubble blocking portion, and a gas reservoir is provided at the upper end thereof, and a tubular membrane is arranged inside.
  • the main tubular body 2 may be arranged as shown in FIG. 3A so as to easily increase the effective length for degassing.
  • the main tubular body 2 is arranged in a predetermined shape in a vertical plane, for example, bent in an inverted N-shape, and air bubbles are prevented at two vertically arranged tubular body portions.
  • a section FP is formed, and the portion of the tubular body 2 disposed therebetween can be degassed.
  • the structure of the decompression pipe 7, the supply pipe 8, the gas reservoir 10 and the discharge pipe 9 is the same as that described above, but in this embodiment, the curved S section at the upper end of the downstream bubble prevention section FP is used. 10 'has the same function as the gas reservoir 10.
  • the degassing device is mainly configured using a straight tubular body.
  • a diagram is used.
  • the degassing device may be configured by using a tubular body 2 arranged in a spiral.
  • the axis of the helix in the horizontal direction, it is possible to effectively form the bubble blocking portion FP in which the downstream side of the tubular body 2 is located below the upstream side.
  • a spirally arranged tubular The vicinity of the upper end of the body 2 can be used as the gas reservoir 10.
  • Other configurations are the same as those described above.
  • the degassing apparatus and the degassing method of the present invention are not only used for the PECVD system, but are also applicable to any degassing process that requires the supply of bubbles and a liquid containing no dissolved gas. Can be used. For example, it can be used to supply various reaction raw material liquids, produce high-purity liquids, and produce ultrapure water.
  • the deaerator of the present invention forms the flow path of the liquid to be treated outside the tubular membrane, the degassing device easily rises due to the buoyancy of the bubbles and effectively prevents the bubbles from flowing to the downstream side. be able to. As a result, the generated bubbles are not easily discharged together with the processing liquid.
  • a degassed liquid is used, for example, it can be effectively used in the field of semiconductor manufacturing equipment.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Chemical Vapour Deposition (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

Cette invention a trait à un dégazeur comportant un corps tubulaire pourvu d'un orifice d'alimentation permettant l'introduction de liquide, un orifice d'évacuation permettant l'évacuation du liquide ainsi qu'au moins un film tubulaire inséré dans le corps tubulaire, définissant un circuit d'écoulement allant de l'orifice d'alimentation vers l'orifice d'évacuation entre le film tubulaire et le corps tubulaire, mais interdisant, du fait de la réduction de la pression, au liquide de passer dans le circuit d'écoulement. Ce système permet, par contre, au gaz dissous dans le liquide d'être soumis à une perméation. Une partie au moins du circuit d'écoulement se trouve du côté inférieur, en aval, afin de constituer une barrière empêchant les bulles d'air produites de s'écouler vers l'aval.
PCT/JP2001/002295 2000-03-22 2001-03-22 Dégazeur et procédé de dégazage Ceased WO2001070366A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001242757A AU2001242757A1 (en) 2000-03-22 2001-03-22 Deaerator and deaerating method

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2000-79387 2000-03-22
JP2000079387A JP4375766B2 (ja) 2000-03-22 2000-03-22 脱気装置及び脱気方法

Publications (1)

Publication Number Publication Date
WO2001070366A1 true WO2001070366A1 (fr) 2001-09-27

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PCT/JP2001/002295 Ceased WO2001070366A1 (fr) 2000-03-22 2001-03-22 Dégazeur et procédé de dégazage

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JP (1) JP4375766B2 (fr)
AU (1) AU2001242757A1 (fr)
WO (1) WO2001070366A1 (fr)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003268552A (ja) * 2002-03-18 2003-09-25 Watanabe Shoko:Kk 気化器及びそれを用いた各種装置並びに気化方法
WO2007008950A2 (fr) * 2005-07-13 2007-01-18 Systec, Llc Degazeur/debulleur integre
US7682421B2 (en) * 2006-10-12 2010-03-23 Celgard Llc Degassing a liquid using a gravity fed apparatus
JP2008205506A (ja) * 2008-05-12 2008-09-04 Watanabe Shoko:Kk 気化器及びそれを用いた各種装置並びに気化方法
JP6829649B2 (ja) * 2017-04-27 2021-02-10 大陽日酸株式会社 堆積物の除去方法、及び堆積物の除去装置
CN118636223B (zh) * 2024-08-14 2024-10-11 大连天薇管业有限公司 一种环保型克拉管加工检测系统

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0252989A (ja) * 1988-08-15 1990-02-22 Japan Menburen Syst Kk 熱交換器
JPH06254304A (ja) * 1993-02-26 1994-09-13 Fuji Photo Film Co Ltd 感光性塗布液の脱気方法及び装置
JPH11319407A (ja) * 1998-05-14 1999-11-24 Micro Galaxy:Kk 真空脱気装置

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0252989A (ja) * 1988-08-15 1990-02-22 Japan Menburen Syst Kk 熱交換器
JPH06254304A (ja) * 1993-02-26 1994-09-13 Fuji Photo Film Co Ltd 感光性塗布液の脱気方法及び装置
JPH11319407A (ja) * 1998-05-14 1999-11-24 Micro Galaxy:Kk 真空脱気装置

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JP4375766B2 (ja) 2009-12-02
AU2001242757A1 (en) 2001-10-03
JP2001259306A (ja) 2001-09-25

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