WO2008101257A2 - Libération de gaz à partir de bouteilles à régulation interne - Google Patents

Libération de gaz à partir de bouteilles à régulation interne Download PDF

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Publication number
WO2008101257A2
WO2008101257A2 PCT/US2008/054336 US2008054336W WO2008101257A2 WO 2008101257 A2 WO2008101257 A2 WO 2008101257A2 US 2008054336 W US2008054336 W US 2008054336W WO 2008101257 A2 WO2008101257 A2 WO 2008101257A2
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WO
WIPO (PCT)
Prior art keywords
gas
gas supply
supply package
vessel
flow
Prior art date
Application number
PCT/US2008/054336
Other languages
English (en)
Other versions
WO2008101257A3 (fr
Inventor
Michael J. Wodjenski
Luping Wang
Jose I. Arno
Original Assignee
Advanced Technology Materials, Inc.
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 Advanced Technology Materials, Inc. filed Critical Advanced Technology Materials, Inc.
Publication of WO2008101257A2 publication Critical patent/WO2008101257A2/fr
Publication of WO2008101257A3 publication Critical patent/WO2008101257A3/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D83/00—Containers or packages with special means for dispensing contents
    • B65D83/14—Containers or packages with special means for dispensing contents for delivery of liquid or semi-liquid contents by internal gaseous pressure, i.e. aerosol containers comprising propellant for a product delivered by a propellant
    • B65D83/32—Dip-tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D83/00—Containers or packages with special means for dispensing contents
    • B65D83/14—Containers or packages with special means for dispensing contents for delivery of liquid or semi-liquid contents by internal gaseous pressure, i.e. aerosol containers comprising propellant for a product delivered by a propellant
    • B65D83/44—Valves specially adapted therefor; Regulating devices
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C2205/00—Vessel construction, in particular mounting arrangements, attachments or identifications means
    • F17C2205/03—Fluid connections, filters, valves, closure means or other attachments
    • F17C2205/0302—Fittings, valves, filters, or components in connection with the gas storage device
    • F17C2205/035—Flow reducers
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/32—Hydrogen storage

Definitions

  • the present invention relates to internally regulated material storage and gas dispensing vessels having a dispensing regulation device disposed in the interior of the vessel, e.g., a pressure-actuated gas dispensing assembly, and to improved gas delivery systems and methods utilizing such vessels.
  • gas supply packaging innovation utilizes a gas discharge regulating assembly, e.g., such as a set point pressure regulator, in the interior of the gas supply vessel.
  • a gas discharge regulating assembly e.g., such as a set point pressure regulator
  • Such internal regulator in use functions to control the pressure of the gas that is discharged from the vessel.
  • Gas supply packages of such type are commercially available from ATMI, Inc. (Danbury, CT, USA) under the trademark VAC and are more fully described in U.S. Patents 6,101,816 and 6,343,476.
  • the gas discharge regulating assembly in the interior volume of the vessel permits the storage of fluid in the vessel at high pressure, yet the gas discharge regulating assembly restricts discharge of gas to a set point or regulated pressure level that is substantially lower than the storage pressure of the bulk fluid in the vessel.
  • the internal gas discharge regulating assembly includes flow control elements designed to prevent particles from being discharged from the vessel with the dispensed vapor, and/or to prevent surges or throttling behavior in the gas dispensing operation.
  • the present invention relates to gas supply apparatus and methods utilizing internally regulated material storage and gas dispensing vessels having a dispensing regulation device disposed in the interior of the vessel, e.g., a pressure-actuated gas dispensing assembly.
  • the invention relates to a gas supply package, including: an elongate vessel defining a longitudinal axis of the vessel, and having an interior volume adapted to hold gas or a gas source material from which gas is available for discharge under dispensing conditions; and a gas discharge assembly secured to said vessel, for dispensing gas from said vessel under said dispensing conditions, said gas discharge assembly including a gas discharge member in said interior volume defining an elongate flow passage having a longitudinal axis, and at least one generally planar filter element in the flow passage for capture of particulates from gas flowing therethrough, wherein said flow passage and said at least one generally planar filter element are arranged to produce: a change in gas flow conductance in the vicinity of the filter element, and/or a direction of flow of gas at a non-zero angle with respect to the longitudinal axis of the vessel and/or to the longitudinal axis of the flow passage, for enhancement of capture efficiency of said filter element.
  • such gas supply package is
  • Another aspect of the invention relates to a gas supply system, comprising a gas supply package as described above, and flow circuitry coupled to the gas discharge assembly for transport of dispensed gas to a gas-utilization location.
  • the invention relates to a semiconductor manufacturing facility, comprising such a gas supply system.
  • the invention in another aspect relates to a fluid filter comprising a filter housing, a polymeric membrane supported on respective faces thereof by apertured support plates secured to said filter housing, and said filter housing arranged for flow of fluid therethrough, so that fluid entering the housing contacts each of the apertured support plates and said polymeric membrane for filtering of said fluid, prior to discharge thereof from the housing.
  • the term "membrane” means a sheet or web form article having pores therein, with such porosity extending through the sheet or web of the article, from one face to the other face thereof.
  • the pores constituting such porosity may be of any suitable sizes, shapes, lengths and pore size distributions.
  • the pores are suitably of a size that permits permeation of a target permeant species through the pores in the article, while one or more other species in mixture with the target permeant are blocked or occluded from such passage.
  • the pores most advantageously are of a size and distribution that permit the membrane to capture particulates so that they do not pass through the membrane.
  • the term "frit” as used herein refers to an article including or constituted of material that is formed under heat and/or pressure, from particles and/or otherwise divided or discontinuous bodies of material, to form a consolidated article that has porosity therein.
  • the porosity permit permeation of a target permeant species through the article, from an exterior surface portion of the article through the article to another exterior surface portion thereof, while one or more other species in mixture with the target permeant are blocked or occluded from such passage.
  • the membrane filters employed in the practice of the invention in preferred implementation do not perform any phase separation function, and preferably are constructed and arranged so that they do not contact liquid in use, or perform any liquid/gas separation operation.
  • FIG. 1 is a schematic cross-sectional elevation view of an internally regulated material storage and gas dispensing package of a type in which the improvements of the invention can be embodied.
  • FIG. 2 is a schematic elevation view of a valve head and an associated double regulator stick embodying improvements of the invention, in one embodiment thereof.
  • FIG. 3 is a schematic elevation view of a valve head and an associated stick embodying improvements of the invention, in one embodiment thereof.
  • FIG. 4 is a graph of out-of -package moisture outgassing, in parts per billion water, as a function of time, in minutes, for various filter media.
  • FIG. 5 is a graph of out-of -package oxygen outgassing, in parts per billion O 2 , as a function of time, in minutes, for various filter media.
  • FIG. 6 is a graph of 24-hour ambient air exposure showing water filtrate concentration, in parts per billion, as a function of time, in minutes, for various filter media.
  • FIG. 7 is a graph of differential pressure as a function of flow rate in standard liters per minute, for various filter media subjected to a differential pressure at 60 psig inlet pressure.
  • FIG. 8 is a micrograph of a PTFE filter medium.
  • FIG. 9 is a cross sectional side elevation view of a flow controller that may be employed in a gas supply package of the present invention.
  • FIG. 10 is a perspective view of the gas flow path through successive disc elements of the flow controller of FIG. 9.
  • FIG. 11 is a side elevation view, partially broken away, of a membrane-based filter, such as may be utilized in gas supply packages of the present invention, in various embodiments thereof.
  • FIG. 12 is a graph of differential pressure, as a function of flow rate at 23°C, for inlet pressures of 30 psig (upper line) and 60 psig (lower line).
  • FIG. 13 is a schematic front elevation view, partially broken away, of a gas supply package according to another embodiment of the invention.
  • FIG. 14 is a schematic elevation view, in cross-section, of a fluid supply package according to one embodiment of the invention, having two interiorly disposed regulators and a membrane filter assembly.
  • FIG. 15 is a schematic front elevation view, in cross-section, of a filter according to one embodiment of the invention.
  • FIG. 16 is a perspective view of the upper portion of the filter of FIG. 15.
  • FIG. 17 is a perspective view of the lower portion of the filter of FIG. 15.
  • FIG. 18 is a top plan view of an apertured plate of the filter of FIG. 15.
  • FIG. 19 is a bottom perspective view of the filter of FIG. 15.
  • the present invention relates to internally regulated gas supply package including a material storage and gas dispensing vessel having a dispensing regulation device, such as a pressure-actuated gas dispensing assembly, disposed in the interior of the vessel.
  • a dispensing regulation device such as a pressure-actuated gas dispensing assembly
  • the present invention in one aspect thereof relates to a gas supply package, including an elongate vessel defining a longitudinal axis of the vessel, and having an interior volume adapted to hold gas or a gas source material from which gas is available for discharge under dispensing conditions; and a gas discharge assembly secured to said vessel, for dispensing gas from said vessel under said dispensing conditions, said gas discharge assembly including a gas discharge member in said interior volume defining an elongate flow passage having a longitudinal axis, and at least one generally planar filter element in the flow passage for capture of particulates from gas flowing therethrough, wherein said flow passage and said at least one generally planar filter element are arranged to produce: a change in gas flow conductance in the vicinity of the filter element, and/or a direction of flow of gas at a non-zero angle with respect to the longitudinal axis of the vessel and/or to the longitudinal axis of the flow passage, for enhancement of capture efficiency of said filter element.
  • Such gas supply package preferably is devoid of sintered metal or frit gas filtration elements.
  • the gas supply package of the invention may be constructed so that the elongate flow passage longitudinal axis and the vessel longitudinal axis define an included acute angle therebetween that is in a range of from about 5° to about 25°.
  • the generally planar filter element in the gas supply package the invention may be constituted by or include a membrane filter element, such as a sheet of polymeric film material that is gas-permeable to the gas being dispensed from the gas supply package, but is effective as a barrier to prevent particulates from passing, so that the gas dispensed from the gas supply package is reduced in, and preferably substantially free of, particulates.
  • the gas supply package includes a membrane filter element that is positionally retained in the gas dispensing passage by apertured support plates producing a change in gas flow conductance in the vicinity of the filter element, and directional flow of gas into the apertures thereof., i.e., the solid portions of the apertured plate divert flow into the apertures.
  • the generally planar filter element of the gas supply package can be provided in an array of longitudinally spaced-apart disc elements in the tubular passage, at least one of which defines a gas flow opening producing directional flow of gas at a non-zero angle with respect to the longitudinal axis of the flow passage.
  • at least one disc element, and preferably multiple disc elements, in the array of longitudinally spaced- apart disc elements are equipped with slatted slot openings for inducing vortexial flow of gas in the tubular passage.
  • the gas supply package may be fabricated with the gas discharge member comprising a conduit, including a first conduit portion having a longitudinal axis that is coincident with the longitudinal axis of the vessel, and a second conduit portion having a longitudinal axis at a non-zero angle to the longitudinal axis of the vessel.
  • the second conduit in a preferred arrangement is below the first conduit portion and terminates at a lower end, with a housing containing the filter element therein being joined to the lower end of the second conduit portion.
  • the first conduit portion can be coupled to a pressure-actuated regulator, for discharging gas in response to a downstream gas pressure below a set point pressure of the pressure-actuated regulator.
  • the gas discharge member in the gas supply package can include a conduit coupled to a pressure-actuated regulator.
  • the gas discharge assembly of the gas supply package can include one, or more than one, pressure-actuated regulators in the interior volume of the vessel.
  • the vessel and the gas supply package can contain a storage medium for gas or a gas source material, from which the gas or gas source material is released under dispensing conditions and gas is flowed from the vessel to the desired gas-utilization location for such dispensed gas.
  • the storage material can be of any suitable type.
  • the storage material includes a physical adsorbent material.
  • the storage material includes an ionic liquid material.
  • the gas discharge assembly in the gas supply package of the invention can include a fluid filter in the interior volume of the vessel, in which the fluid filter includes a filter housing having a generally planar filter element mounted therein, positionally retained between upstream and downstream apertured support plates, as a composite assembly.
  • the generally planar filter element may comprise a polymeric membrane material.
  • polymeric materials that can be used are polyethylene terephthalate, polysulfone, polyimide and polytetrafluoroethylene.
  • the polymeric sheet material used as a filter element may have any suitable thickness, e.g., a thickness in a range of from 0.07 to 0.2 mm.
  • the vessel of the gas supply package in the use may be charged with a semiconductor manufacturing gas, e.g., gases such as arsine, ammonia, argon, boron trifluoride, boron trifluoride, diborane, carbon dioxide, carbon monoxide, hydrogen fluoride, phosphine, phosphorus trifluoride, silanes, silicon tetrachloride, silicon tetrafluoride, sulfur hexafluoride, halogen gases, hydride gases, metal organic compounds and oxide gases.
  • gases such as arsine, ammonia, argon, boron trifluoride, boron trifluoride, diborane, carbon dioxide, carbon monoxide, hydrogen fluoride, phosphine, phosphorus trifluoride, silanes, silicon tetrachloride, silicon tetrafluoride, sulfur hexafluoride, halogen gases, hydride gases, metal organic compounds and oxide gases.
  • the contained gas or gas source material may be stored, transported, and ultimately deployed at an intended use location.
  • the gas supply package may be coupled via a flow circuitry interconnecting the gas discharge assembly of the package with a gas-utilization location, for transport of dispensed gas to such location.
  • the use location may be a semiconductor manufacturing facility, in which the gas supply system including the gas supply package is utilized to provide high purity gas for the semiconductor manufacturing operation carried out in such facility.
  • the invention in another aspect relates to a fluid filter including a filter housing, a polymeric membrane supported on respective faces thereof by apertured support plates secured to the filter housing, with the filter housing arranged for flow of fluid therethrough, so that fluid entering the housing contacts each of the apertured support plates and the polymeric membrane for filtering of the fluid, prior to discharge thereof from the housing.
  • the polymeric membrane in a preferred embodiment comprises polytetrafluoroethylene, with each of the apertured support plates being arranged so that apertures therein are in register with apertures of the other of the apertured support plates, to facilitate gas flow through the filter.
  • FIG. 1 is a schematic cross-sectional elevation view of an internally regulated material storage and gas dispensing package 100 of a type in which the improvements of the invention can be embodied.
  • the package 100 includes a fluid storage and dispensing vessel 102 of generally cylindrical form, with a cylindrical sidewall 104 closed at its lower end by floor member 106. At the upper end of the vessel is a neck 108 including a cylindrical collar 110 defining and circumscribing a top opening (port) of the vessel. The vessel wall, floor member and neck thereby enclose an interior volume 128, as shown.
  • valve head assembly 114 At the neck of the vessel, a threaded plug 112 of the valve head assembly 114 is threadably engaged with the interior threaded opening of the collar 110.
  • the valve head assembly 114 includes a central fluid flow passage 120 joined in fluid flow communication with a central working volume cavity in the valve head assembly.
  • the central working volume cavity in turn is joined to outlet 124, which may be exteriorly threaded or otherwise constructed for attachment of a connector and associated piping, conduit, etc. thereto.
  • valve element 122 Disposed in the central working volume cavity is a valve element 122 that is joined to a hand wheel 126 in the embodiment shown, but may alternatively be joined to an automatic valve actuator or other controller or actuating means.
  • the valve head assembly 114 also features in the valve block a fill passage 116 communicating with fill port 118 and the interior volume 128 of the vessel.
  • the vessel 102 may thereby be charged with pressurized gas, following which the fill port is closed and capped, as shown.
  • the vessel may be filled with gas through the regulator, e.g., by setting the fluid pressure regulator at a suitably low pressure level so that the gas or vapor is at a pressure below the pressure regulator set point, using a conventional pressure regulator including a poppet element which may be biased with a biasing element such as a spring biasing element to a closed position, and which responds to pressure above the set point pressure by remaining closed, but which responds to pressure below the set point pressure by opening and allowing fluid flow therethrough.
  • a conventional pressure regulator including a poppet element which may be biased with a biasing element such as a spring biasing element to a closed position, and which responds to pressure above the set point pressure by remaining closed, but which responds to pressure below the set point pressure by opening and allowing fluid flow therethrough.
  • the fill operation may be carried out to load the vessel with fluid to be stored and subsequently dispensed, by establishing an interior pressure level in the vessel at which the poppet element of the pressure regulator disengages from its seat, thereby allowing gas to flow into the vessel, in reverse flow fashion to the dispensing mode of the system.
  • the vessel may be fabricated with only one port, which thus functions to permit egress of gas from the vessel for dispensing, as well as permitting filling of the vessel with the fluid in the first instance, through the single port.
  • the central fluid flow passage 120 in the valve head assembly 114 is joined at its lower end to a connector flow tube 130, to which in turn is joined to the regulator 132.
  • the regulator is set to maintain a selected pressure of the fluid discharged from the vessel.
  • a tubular fitting 136 which in turn is joined, e.g., by butt welding, to a filter unit 134 having a diffuser end cap 131 at its lower extremity.
  • the filter unit may be formed of stainless steel, with the diffuser wall being formed of a sintered stainless steel such as 316L stainless steel.
  • the filter unit has a wall porosity that permits removal of all particles greater than a predetermined diameter, e.g., greater than 0.003 micrometers at 30 standard liters per minute flow rate of gas from the system.
  • Filter units of such type are commercially available from Mott Corporation (Farmington, CT).
  • FIG. 2 is a schematic elevation view of a valve head 240 and an associated double regulator stick embodying improvements of the invention, in one embodiment thereof.
  • the stick comprises upper pressure regulator 242 and lower pressure regulator 244, and tubing 246 including a bend 248 intermediate the lower regulator 244 and membrane filter 250.
  • the included angle between the centerline of the stick above the bend 248 and the angles defined by the central axis of the tubing below the bend 248 may be in a range of from about 5 to 25°, more preferably in a range of from 8 to 15°, and most preferably a range of from 9 to 12°.
  • the dispensing structures of FIG. 2 is devoid of any frit or sintered metal filter components, instead utilizing a membrane filter in the tubing of the stick, proximate to the lower open end of such tubing, with such tubing having a slight bend therein.
  • FIG. 3 is a schematic elevation view of a valve head 260 and an associated stick embodying various features of the invention, in one embodiment thereof.
  • the tubing 264 of the stick below the regulator 262 has a 10° bend 266 so that the lower portion of the tubing below the bend is linear and describes and included angle between the central axis of the stick above the regulator, and the central axis of the tubing below the bend 266, which is 10° in this embodiment.
  • the lower angled portion of the tubing has a membrane filtration device 268 therein, as illustrated, and a bottom opening 270 allowing ingress of gas from the interior compartment of the gas dispensing vessel to flow upwardly in tubing 264 through the membrane filter 268 to the pressure regulator 262.
  • the regulator has a set point of appropriate pressure value, so that it opens when the valve of the valve head is open and the pressure regulator experiences a downstream pressure below its set point.
  • the bend 266 provides a minor damping of the fluid and has been found to enable good capture of particulates by the membrane filter 268, such as otherwise would adversely affect the regulator and downstream process in which the dispensed gas is used.
  • FIG. 4 is a graph of out-of -package moisture outgassing, in parts per billion water, as a function of time, in minutes, for various filter media.
  • Curve 1 represents the outgassing performance of a PTFE membrane
  • curve 2 represents a nickel frit
  • curve 3 a stainless steel frit
  • curve 4 a ceramic (Tos) filter
  • curve 5 a ceramic (Mem) filter.
  • the test methodology used to generate these curves was SEMASPEC 90120397B-STD. The results showed that the PTFE membrane was the only filter element to outgas moisture in the sub- 10 ppb regime, and that such membrane outperformed the nickel and stainless steel filters. None of the metal filters were capable of reaching ⁇ 10 ppb impurity levels after four hours of purging.
  • FIG. 5 is a graph of out-of -package oxygen outgassing, in parts per billion O 2 , as a function of time, in minutes, for the same various filter media tested in the out-of-package moisture outgassing test (curve 1 represents the outgassing performance of a PTFE membrane, curve 2 represents a nickel frit, curve 3 a stainless steel frit, curve 4 a ceramic (Tos) filter and curve 5 a ceramic (Mem) filter).
  • curve 1 represents the outgassing performance of a PTFE membrane
  • curve 2 represents a nickel frit
  • curve 3 a stainless steel frit
  • curve 4 a ceramic (Tos) filter
  • curve 5 a ceramic (Mem) filter
  • the test methodology used to generate the data shown in FIG. 5 was SEMASPEC 90120397B-STD.
  • the PTFE filter exhibited the lowest initial oxygen outgassing.
  • the PTFE and stainless steel filters remained ⁇ 1 ppm after a purge period of one hour.
  • FIG. 6 is a graph of 24-hour ambient air exposure showing water concentration, in parts per billion, as a function of time, in minutes, for various filter media.
  • This graph for water outgassing after 24-hour ambient exposure, contains data for the same membrane filters as used in the moisture outgassing and oxygen outgassing tests (curve 1 represents a PTFE membrane, curve 2 represents a nickel frit, curve 3 a stainless steel frit, curve 4 a ceramic (Tos) filter and curve 5 a ceramic (Mem) filter).
  • FIG. 7 is a graph of differential pressure as a function of flow rate in standard liters per minute, for various filter media subjected to a differential pressure at 60 psig inlet pressure.
  • the filter media included those used in the previous outgassing tests (curve 1 represents a PTFE membrane, curve 2 represents a nickel frit, curve 3 a stainless steel frit, curve 4 a ceramic (Tos) filter and curve 5 a ceramic (Mem) filter).
  • the test methodology used to generate the data shown in FIG. 7 was SEMASPEC 90120397B-STD. Of all filters tested, the PTFE filter at the lowest pressure differential at all inlet flow rates. The PTFE filter had 20% less pressure drop compared to the stainless steel filter, and approximately one-half of the pressure drop over the nickel filter.
  • a particle shed evaluation was conducted for the same type of membranes as used in the above-discussed outgassing tests (a PTFE membrane, a nickel frit, a stainless steel frit, a ceramic (Tos) filter and a different ceramic (Mem) filter).
  • the test methodology employed was that of SEMASPEC 9302151 IA-STD, involving 60 minutes steady flow, 60 minutes pulse flow, 10 minutes impaction and 30 minutes steady flow conditions.
  • the ceramic filters were determined to shed the most particles, and the PTFE membrane performed best, demonstrating its superiority to metal and ceramic filters.
  • Integrity testing performed on PTFE membranes involving pre-pulse and flush steps followed by a particle challenge (2 x 10 7 particles/minute), with continuous counting of downstream particles.
  • the PTFE membranes satisfied acceptance criteria of zero particles downstream.
  • FIG. 8 is a micrograph of a PTFE filter medium of the type used in the above- describe tests, showing the microstructure of such material.
  • FIG. 9 is a cross sectional side elevation view of a flow controller 200 that may be employed in a gas supply package of the present invention.
  • the flow controller includes a main cylindrical housing 202 that is coupled at one end to a smaller diameter cylindrical extension 218 having openings 220 therein, and at the other end to a smaller diameter cylindrical extension 208 having openings 210 therein.
  • the cylindrical extension 208 is reposed in and coaxial with a barrel section 204 having an open end 206 adapted for coupling with tubing of the stick in the interior volume of a gas supply vessel of the invention.
  • Within main cylindrical housing 202 are arranged a series of longitudinally spaced- apart transversely extending discs 212, 214 and 216 of differing conformation.
  • Disc 212 has a central opening therein for gas flow therethrough.
  • Disc 214 has a slot opening defined by segments of the disc that flair outwardly, in opposed fashion to one another, from the plane of the disc.
  • Disc 216 has a slot opening that is transversely offset in relation to the slot opening of discs of the type shown as disc 214, and is bounded by segments of the disc that flair outwardly, in opposed fashion to one another, from the plane of the disc.
  • FIG. 10 is a perspective view of the gas flow path through successive disc elements of the flow controller of FIG. 9.
  • the disc assembly 300 includes a top disc 302 having a slot opening 304 therein through which gas passes in the direction indicated by arrow A, as channeled by the louvered downwardly oriented tab to induce the vortexial flow illustrated between such top disc 302 and intermediate disc 306 having central opening 308 therein.
  • the gas then flows through the central opening 308 in the intermediate disc 306, and maintains its vortexial flow to the slot opening 312 bounded by the downwardly angled tab of the slot structure, so that the fluid is vortexially channeled as it egresses the slot opening.
  • the gas stream is channeled along an extended length flow path, relative to the length dimension of the flow controller and flow through such a controller lacking the disc elements with flow diverter angled slot structures.
  • FIG. 11 is a side elevation view, partially broken away, of a membrane-based filter 500, such as may be utilized in gas supply packages of the present invention, in various embodiments thereof.
  • the filter 500 includes an inlet tube 506 having an open end 502.
  • the inlet tube 506 is secured to the main housing 504 of the filter.
  • the main housing encloses an interior volume 512 in which is disposed one or more membrane filter elements 514, so that fluid entering the inlet tube 506 flows through the interior volume 512 of the housing 504 and is discharged to an outlet tube 508 having an open discharge end 510.
  • the filter 500 may be disposed in the interior volume of the gas supply package vessel, coupled at its outlet tube to the stick tube segment upstream of the regulator componentry, so that the open end 502 of the inlet tube 506 of the filter is arranged to receive gas to be dispensed from the vessel, and to effect flow damping and particulate removal therefrom.
  • FIG. 12 is a graph of differential pressure, as a function of flow rate at 23°C, for inlet pressures of 30 psig (upper line) and 60 psig (lower line), for flow through a filter of the type shown and described with reference to FIG.
  • Such filter achieved a downstream article concentration of less than 0.03 particles/ liter, for particles greater than 0.01 ⁇ m in diameter, and reduced volatiles to less than 10 ppb moisture.
  • the particle retention characteristic of the PTFE membrane was greater than 99.9999999% (9 LRV) removal of all particles at 30 standard liters per minute, as referenced at the most penetrating particle size.
  • the membrane filter utilized in the gas supply package of the invention may be of any suitable material of construction, preferably a polymeric material having a surface free energy that is comparable to that of polytetrafluoroethylene, as a vapor-permeable barrier structure.
  • the gas supply package of the present invention therefore enables the gas supply vessel to be devoid of any sintered metal matrix or metal frit barrier structures, and to utilize a vapor-permeable polymeric barrier structure that is much more efficient and less costly than such metal filter structures.
  • the vapor-permeable polymeric barrier material may be relatively thin in character, e.g., with a thickness in a range of from 0.07 to 0.2 mm in various embodiments, and with nominal pore size that may be on the order of 1 ⁇ m.
  • the invention in various embodiments provides a membrane filter that is self- cleaning in character, by generating asymmetric or transverse flows or flow components that sweep the surface of the membrane filter to effect cleaning thereof.
  • self- cleaning may be provided by a tubing conformation that is arranged to redirect a portion of the dispensed fluid stream across the filter surface, to remove any solids accumulation thereon.
  • the vortexial flow arrangement achieved by the disc elements in the flow controller of FIG. 9 serves to provide such self-cleaning capability, and can be adapted to a filter similarly constructed, in which one or more of the disc elements is replaced by a membrane element of the type shown in the filter of FIG. 11.
  • FIG. 13 is a schematic front elevation view, partially broken away, of a gas supply package 600 according to another embodiment of the invention.
  • the package includes a generally cylindrical vessel 602 enclosing an interior volume 604 for containment of a gas and/or gas source such as a liquid or solid for generating vapor that is discharged in the use of the package.
  • the interior volume 604 can in specific embodiments contain a storage medium for the gas and/or gas source, in which the gas and/or gas source is reversibly held, and from which gas can be extracted under dispensing conditions.
  • the storage medium can include or be constituted by a solid-phase physical adsorbent material, e.g., activated carbon, molecular sieve, a macroreticulate polymer, or other material having sorptive affinity for the gas and/or gas source, and from which gas is desorbable or otherwise extractible under dispensing conditions.
  • the storage medium can include or be constituted by an ionic liquid, in which the gas or a gas precursor can be retained for subsequent release under dispensing conditions.
  • the interior volume contains a porous carbon adsorbent, e.g., in a particulate form such as beads, pellets, particles, etc., to constitute a bed of the sorbent in the interior volume, or alternatively in a monolithic form, e.g., as bricks, blocks, discs, or other bulk form, in which one or more of the bulk form sorbent articles is arranged in the interior volume for storage of the gas or gas precursor, and desorptive release thereof in the dispensing mode of the package.
  • a porous carbon adsorbent e.g., in a particulate form such as beads, pellets, particles, etc.
  • a monolithic form e.g., as bricks, blocks, discs, or other bulk form
  • Desorption can be effected in any suitable manner, such as by pressure differential (pressure-mediated desorption), heating (thermally-mediated desorption) and/or concentration differential (mass transfer concentration gradient-mediated desorption, such as by flow of a carrier gas through the interior volume for contacting with the sorbent material).
  • the stick 620 in the interior volume 604 includes an upper conduit 621 interconnecting the regulator 622 with the valve head assembly 606.
  • the valve head assembly includes a valve head of block-like form as illustrated, containing a valve cavity in which is disposed a valve element that is translatable between fully open and fully closed valve positions by manual rotation of the handwheel 608 that is joined to a stem of such valve element.
  • the valve head also includes a discharge port 610 which may be coupled in fluid flow communication with a discharge line (not shown) for conveying the dispensed gas from the vessel to a downstream location of use, e.g., in a chemical vapor deposition or atomic layer deposition chamber.
  • Regulator 622 may be of any suitable type, e.g., a fixed set point regulator or alternatively a variable set point (adjustable) regulator.
  • the adjustable set point regulator may be internally adjustable in the enclosed volume of the vessel 602, or it may be externally adjustable, e.g., by a signal that is transmitted to the regulator from a location outside of the vessel.
  • the conduit 626 has a bore opening 634 therein, so that gas can flow upwardly in such conduit, in the direction indicated by arrow A, to the regulator for dispensing, when the valve in the valve head is opened, and the downstream pressure level is lower than the set point pressure of the regulator.
  • a membrane filter element 628 Disposed in conduit 626, in the upper portion of such conduit below the regulator 622, is a membrane filter element 628.
  • the membrane filter element is mounted in the bore of the conduit, extending transversely across the bore.
  • Such membrane filter element can be formed of PTFE or other suitable material.
  • a particulates disengagement chamber 630 that is characterized by a lower portion that is outwardly and upwardly flared.
  • the cross-sectional area of the flow passage defined by such chamber is increasing in the upward direction, to the intermediate portion of the chamber.
  • the velocity of the discharged gas stream is progressively reduced, to such extent as to allow disengagement of particulates from the gas stream. Disengaged particles then fall from the flow stream of dispensed gas onto the outwardly and upwardly flaring walls bounding the lower portion of the chamber.
  • the flow stream then flows through the upper portion of the chamber, with its progressively smaller cross-section in the upward direction.
  • the gas stream increases in superficial velocity as it flows vertically through the converging portion of chamber 630, and enters conduit 626 and is filtered by the membrane filter 628 extending transversely across the interior passage of such conduit, being substantially normal to the direction of gas flow through the conduit when the package is in dispensing operation.
  • the membrane filter 628 can be formed of any suitable material of construction, and preferably comprises a polymeric membrane of suitable porosity and permeability characteristics to achieve an ultra-clean character of the dispensed gas, in applications such as manufacture of microelectronic devices.
  • the polymeric membrane comprises a membrane filter of polytetrafluoroethylene (PTFE) or other polymeric membrane material, such as polysulfone, polyimide, etc.
  • PTFE polytetrafluoroethylene
  • the membrane filters 628 can be formed of carbon cloth, or other woven or nonwoven material, as suitable for the specific use intended.
  • the resultingly filtered gas then flows through regulator 622 when same is in a dispensing mode, through conduit 621 and through the passages of the valve in valve head assembly 606, for dispensing at the discharge port 610.
  • Discharge port 10 in use is appropriately joined to suitable flow circuitry for transfer to gas to a downstream use location.
  • conduit 626 below the regulator 622 may include a bend so that the portion of the stick below regulator 622 is oriented at an angle with respect to the longitudinal centerline of conduit 621 above the regulator.
  • the included angle between the angled conduit 646 and the longitudinal centerline of conduit 621 may be on the order of 10-30°.
  • the discharge port 610 of the gas supply package is coupled with appropriate flow circuitry for transport of the dispensed gas to a downstream use location.
  • Such flow circuitry may include piping, tubing, manifold structure, and flow monitoring and control devices, such as flow control valves, pressure monitoring sensors, additional regulators, temperature monitoring sensors, restricted orifice devices, pumps, sampling ports or chambers, etc.
  • flow monitoring and control devices such as flow control valves, pressure monitoring sensors, additional regulators, temperature monitoring sensors, restricted orifice devices, pumps, sampling ports or chambers, etc.
  • valve in the valve head assembly 606 then is opened, such as by manual rotation of the handwheel 608 or by operation of an actuator coupled thereto for automatic operation of the valve in the valve head assembly.
  • the regulator 622 then operates to initiate flow at a set point pressure characteristic of such device, if the pressure in the flow circuitry coupled with the gas supply package is below the set point pressure.
  • the regulator for such purpose may be of a type including an internal fixed-pressure and an external variable-pressure bellows assembly in contact with a pin and poppet assembly, in which the pin and poppet assembly is biased to a normally closed position by a spring mounted below the poppet.
  • the regulator opens when a lower-than-set point pressure is experienced by the bellows assembly, causing expansion of the bellows to translate the poppet from its normally biased-closed position to an open position enabling gas flow through the stick to the discharge port and externally coupled flow circuitry.
  • valve in the valve head assembly Upon completion of the dispensing operation, the valve in the valve head assembly
  • valve 606 is closed, e.g., by manual rotation of the handwheel 608 or by an automatic actuator coupled with the valve in the valve head assembly.
  • the gas source material in the vessel 602 may be of any suitable type, as useful for manufacturing of microelectronic products, production of semiconductors, cleaning of industrial process equipment, or other application for which the gas dispensed from the vessel is usefully employed.
  • the vessel 602 may contain arsine, boron trifluoride, phosphine, diborane, silane or metalorganic source reagents.
  • Membrane filters of such character exhibit no significant capillary action, and are highly efficient in respect of particle removal from gas streams.
  • the membrane filter components achieved a substantial advance in the art.
  • pressure- regulated vessels in which the pressure of the contained gas source material pressure was substantial, such as on the order of 50-2000 psi (0.34- 13.8 megaPascals) was that sintered metal plugs and thick frits were necessary to achieve satisfactory particle capture.
  • the present invention represents the unexpected discovery that membrane filters can be used to efficiently remove particulates from dispensed gas, without any significant deterioration or degradation of the membrane filter, even in extended use.
  • offsetting of the inlet of the stick from the center of the vessel interior volume has the unexpected advantage of improving the filtration capability of the membrane filter, since the flow of gas can be channeled by the bent stick conformation so that the dispensed gas stream has a radial velocity component that serves to sweep the surface of the membrane filter to provide improved filtration.
  • FIG. 14 is a schematic elevation view, in cross-section, of a fluid supply package 400 according to one embodiment of the invention, having two interiorly disposed regulators 410 and 412 and a membrane filter assembly 418.
  • the fluid supply package includes the vessel 406 defining an interior volume 408 therein, and having a gas discharge assembly including the valve head 402 and the interior double regulator flow circuitry.
  • the lower regulator 412 is coupled to a first conduit 414 that is coaxial with the longitudinal axis of the vessel 406, and a second conduit 416 that is coupled to the first conduit 414 as well as the filter assembly 418.
  • Second conduit 416 is disposed at an angle with respect to the longitudinal axis of the vessel, defining an included acute angle therewith.
  • FIGS. 15-19 illustrate an example of a suitable membrane filter that can be employed in the gas discharge assembly of the gas supply package of the present invention, as more fully described in U.S. Provisional Patent Application No. 60/901,876 filed February 16, in 2007 in the names of Anthony DiPrizio, Paul Matthews and Jose Arno for "A Fluid Filter With Polymeric Membrane And Metal Supports," the disclosure of which hereby is incorporated herein by reference.
  • the fluid filter of FIGS. 15-19 comprises a filter housing, a polymeric membrane supported on respective faces thereof by apertured support plates secured to said filter housing, with the filter housing being arranged for flow of fluid therethrough, so that fluid entering the housing contacts each of the apertured support plates and the polymeric membrane for filtering of the fluid, prior to discharge thereof from the housing.
  • the polymeric membrane comprises poly tetrafluoroe thy lene, and each of the apertured support plates is arranged so that apertures therein are in register with apertures of the other of said apertured support plates.
  • FIG. 15 is a schematic front elevation view, in cross-section, of a filter 700 according to one embodiment of the invention.
  • the filters 700 includes an upper housing member 702 cooperatively mating at threading 706 to lower housing member 704. Between the respective upper and lower housing members is mounted a filter assembly including a lower apertured support plate 708, a membrane filter element 712 reposed on the lower apertured support plate 708, and upper apertured support plate 710 reposed on the membrane filter element 712. The edges of this filter assembly are compressively secured in position by the respective upper and lower housing members.
  • the upper and lower housing members are provided with facing grooves in which are disposed respective O-rings 714 and 716, as illustrated.
  • the upper housing member 702 defines an upwardly convergent passage 722 communicating with upper cylindrical passage 724 in conduit 730.
  • the filter thus is arranged with a fluid inlet 720, from which fluid passes successively through the lower apertured plate 708, membrane filter element 712, and upper apertured plate 710, flowing into passage 722 and finally into passage 724.
  • FIG. 16 is a perspective view of the upper portion of the filter of FIG. 15, showing the threading 706a of the upper housing member 702 and conduit 730 containing passage 724 therein.
  • FIG. 17 is a perspective view of the lower portion of the filter of FIG. 15, showing the threading 706b of the lower housing member 704, and the interior aperture 732 for positioning of the upper and lower apertured plates.
  • FIG. 18 is a top plan view of the upper apertured plate 710 of the filter of FIG. 15, showing the apertures 744 therein.
  • the plate 710 has an outer un-apertured periphery 742 with extension elements 746 and 748, which are matably engageable with the interior apertures (e.g., aperture 732 is shown in FIG. 17) of the lower housing member of the filter.
  • FIG. 19 is a bottom perspective view of the filter of FIG. 15, showing the upper housing member 702 engaged with the lower housing members 704.
  • the filter element assembly
  • 760 includes lower apertured support plate 708 having aperture openings 744 therein, exposing the membrane element 712 to the influent gas flow, for passage through the filter element assembly comprising lower apertured support plate, membrane filter element and upper apertured support plate, and discharge through conduit 730.
  • FIGS. 15-19 is of an illustrative character, and that the membrane element can be supported or positionally retained in a variety of other ways, so that the membrane element is appropriately presented for filtering of the gas being dispensed from the associated source of same.
  • the gas supply package of the invention is usefully employed for storage of gases or gas source materials, and dispensing of gases for use in a wide variety of gas-utilizing processes and applications.
  • the dispensed gases can for example be hydride gases, halide gases, gaseous organometallic compounds, etchants, or other gases for the manufacture of microelectronic products such as semiconductor devices.
  • the gas supply package of the invention enables gases to be supplied in an ultra-pure condition, removing particulates and/or other contaminants that can adversely affect products manufactured using the dispensed gas.

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

La présente invention concerne un conditionnement d'alimentation en gaz, comprenant un récipient de stockage de matériau et de distribution de gaz définissant un volume intérieur conçu pour contenir un matériau source pour le gaz, une tige distributrice de gaz se trouvant dans le volume intérieur. Ladite tige comprend au moins un régulateur couplé à un passage d'écoulement, au moins un élément filtrant généralement plan étant disposé pour filtrer le gaz passant par ledit passage avant de s'écouler par le ou les régulateurs. Ledit passage et ledit ou lesdits éléments filtrants sont disposés pour produire : (i) un changement de la conductance du débit gazeux au voisinage de l'élément filtrant, et/ou (ii) un sens d'écoulement gazeux formant un angle non nul par rapport à l'axe longitudinal du récipient et/ou par rapport à l'axe longitudinal du passage d'écoulement, pour une amélioration de l'efficacité de capture dudit élément filtrant.
PCT/US2008/054336 2007-02-16 2008-02-19 Libération de gaz à partir de bouteilles à régulation interne WO2008101257A2 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US90187607P 2007-02-16 2007-02-16
US60/901,876 2007-02-16
US94987007P 2007-07-15 2007-07-15
US60/949,870 2007-07-15

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EP2898254A4 (fr) * 2012-09-21 2017-02-08 Entegris, Inc. Gestion de pression anti-pointes de récipients de stockage et de distribution de fluide à pression régulée
US9897257B2 (en) 2012-09-21 2018-02-20 Entegris, Inc. Anti-spike pressure management of pressure-regulated fluid storage and delivery vessels
KR102242962B1 (ko) 2012-09-21 2021-04-21 엔테그리스, 아이엔씨. 압력 조절식 유체 보관 및 운반 용기의 스파이크 압력 방지 관리
WO2014047522A1 (fr) 2012-09-21 2014-03-27 Advanced Technology Materials, Inc. Gestion de pression anti-pointes de récipients de stockage et de distribution de fluide à pression régulée
KR102373840B1 (ko) 2012-09-21 2022-03-11 엔테그리스, 아이엔씨. 압력 조절식 유체 보관 및 운반 용기의 스파이크 압력 방지 관리
EP3201512A4 (fr) * 2014-10-03 2018-03-14 Entegris, Inc. Récipient de fourniture de gaz à régulation de pression
CN112203778A (zh) * 2018-06-22 2021-01-08 林德有限责任公司 气缸阀以及用于抑制污染物在气缸和气缸阀中形成的方法
CN112203778B (zh) * 2018-06-22 2022-08-30 林德有限责任公司 气缸阀以及用于抑制污染物在气缸和气缸阀中形成的方法
WO2022232464A1 (fr) * 2021-04-30 2022-11-03 Entegris, Inc. Récipients et procédés de stockage et de distribution d'un réactif

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TW200900128A (en) 2009-01-01

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