WO2025007191A1 - Joint soudé entre une membrane de séparation d'hydrogène métallique et un raccord métallique - Google Patents

Joint soudé entre une membrane de séparation d'hydrogène métallique et un raccord métallique Download PDF

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Publication number
WO2025007191A1
WO2025007191A1 PCT/AU2024/050727 AU2024050727W WO2025007191A1 WO 2025007191 A1 WO2025007191 A1 WO 2025007191A1 AU 2024050727 W AU2024050727 W AU 2024050727W WO 2025007191 A1 WO2025007191 A1 WO 2025007191A1
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WIPO (PCT)
Prior art keywords
metallic
weld
metal
separation membrane
hydrogen separation
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/AU2024/050727
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English (en)
Inventor
Sandy EDWARDS
David Viano
Matthew Langley
Riley INGLE
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.)
Commonwealth Scientific and Industrial Research Organization CSIRO
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Commonwealth Scientific and Industrial Research Organization CSIRO
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Filing date
Publication date
Priority claimed from AU2023902141A external-priority patent/AU2023902141A0/en
Application filed by Commonwealth Scientific and Industrial Research Organization CSIRO filed Critical Commonwealth Scientific and Industrial Research Organization CSIRO
Priority to CN202480044538.4A priority Critical patent/CN121464017A/zh
Priority to AU2024291411A priority patent/AU2024291411A1/en
Priority to KR1020267000417A priority patent/KR20260034655A/ko
Publication of WO2025007191A1 publication Critical patent/WO2025007191A1/fr
Anticipated expiration legal-status Critical
Pending legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/20—Bonding
    • B23K26/21—Bonding by welding
    • B23K26/211—Bonding by welding with interposition of special material to facilitate connection of the parts
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L13/00—Non-disconnectable pipe joints, e.g. soldered, adhesive, or caulked joints
    • F16L13/02—Welded joints
    • F16L13/0218—Welded joints having an inner or outer ring
    • F16L13/0236—Welded joints having an inner or outer ring having an outer ring
    • 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
    • B01D53/22—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 diffusion
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/003—Membrane bonding or sealing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/04—Tubular membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/022—Metals
    • B01D71/0221—Group 4 or 5 metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/005—Soldering by means of radiant energy
    • B23K1/0056—Soldering by means of radiant energy soldering by means of beams, e.g. lasers, electron beams [EB]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/19—Soldering, e.g. brazing, or unsoldering taking account of the properties of the materials to be soldered
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K15/00—Electron-beam welding or cutting
    • B23K15/0046—Welding
    • B23K15/0053—Seam welding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K15/00—Electron-beam welding or cutting
    • B23K15/0046—Welding
    • B23K15/0093—Welding characterised by the properties of the materials to be welded
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/0006—Working by laser beam, e.g. welding, cutting or boring taking account of the properties of the material involved
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/20—Bonding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K26/00—Working by laser beam, e.g. welding, cutting or boring
    • B23K26/20—Bonding
    • B23K26/21—Bonding by welding
    • B23K26/24—Seam welding
    • B23K26/28—Seam welding of curved planar seams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K9/00—Arc welding or cutting
    • B23K9/02—Seam welding; Backing means; Inserts
    • B23K9/028—Seam welding; Backing means; Inserts for curved planar seams
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K9/00—Arc welding or cutting
    • B23K9/23—Arc welding or cutting taking account of the properties of the materials to be welded
    • B23K9/232—Arc welding or cutting taking account of the properties of the materials to be welded of different metals
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L13/00—Non-disconnectable pipe joints, e.g. soldered, adhesive, or caulked joints
    • F16L13/007—Non-disconnectable pipe joints, e.g. soldered, adhesive, or caulked joints specially adapted for joining pipes of dissimilar materials
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
    • F16L13/00—Non-disconnectable pipe joints, e.g. soldered, adhesive, or caulked joints
    • F16L13/02—Welded joints
    • F16L13/0209—Male-female welded joints
    • 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
    • B01D53/22—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 diffusion
    • B01D2053/221—Devices
    • B01D2053/223—Devices with hollow tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/16—Hydrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/10—Single element gases other than halogens
    • B01D2257/102—Nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/406—Ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/502—Carbon monoxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/702—Hydrocarbons
    • B01D2257/7022—Aliphatic hydrocarbons
    • B01D2257/7025—Methane
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/58—Fusion; Welding
    • 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
    • B01D53/22—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 diffusion
    • B01D53/228—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 diffusion characterised by specific membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/02—Iron or ferrous alloys
    • B23K2103/04—Steel or steel alloys
    • B23K2103/05—Stainless steel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/18—Dissimilar materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/18—Dissimilar materials
    • B23K2103/26—Alloys of Nickel and Cobalt and Chromium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K2103/00—Materials to be soldered, welded or cut
    • B23K2103/50—Inorganic materials other than metals or composite materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K37/00—Auxiliary devices or processes, not specially adapted for a procedure covered by only one of the other main groups of this subclass
    • B23K37/04—Auxiliary devices or processes, not specially adapted for a procedure covered by only one of the other main groups of this subclass for holding or positioning work
    • B23K37/053—Auxiliary devices or processes, not specially adapted for a procedure covered by only one of the other main groups of this subclass for holding or positioning work aligning cylindrical work; Clamping devices therefor
    • B23K37/0536—Auxiliary devices or processes, not specially adapted for a procedure covered by only one of the other main groups of this subclass for holding or positioning work aligning cylindrical work; Clamping devices therefor for maintaining flanges on tubes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen; Reversible storage of hydrogen
    • C01B3/50—Separation of hydrogen or hydrogen-containing gases from gaseous mixtures, e.g. purification
    • C01B3/501—Separation of hydrogen or hydrogen-containing gases from gaseous mixtures, e.g. purification by diffusion
    • C01B3/503—Separation of hydrogen or hydrogen-containing gases from gaseous mixtures, e.g. purification by diffusion characterised by membranes

Definitions

  • a welded joint between a metallic hydrogen separation membrane to a metallic connector and the composition thereof is disclosed, as well as a method of joining a metallic hydrogen separation membrane to a metallic connector, e.g., sealably joining.
  • the joint may be particularly applicable for joining and sealing a tubular membrane, such as a vanadium-based tubular membrane, to a stainless steel gas fitting.
  • the joint could be used to join and seal any metallic type of hydrogen separation membrane to any type of metallic fitting or body.
  • Hydrogen (H2) does not occur naturally in great abundance, and in industrial practice it may be produced by the conversion of a hydrocarbon fuel such as coal, petroleum or natural gas, through the decomposition of ammonia (NH3), or from the electrochemical decomposition of water.
  • a hydrocarbon fuel such as coal, petroleum or natural gas
  • NH3 ammonia
  • Each of these production routes produces an impure gas stream containing H2 plus unreacted feed gases (e.g., CH4, H2O, NH3) and by-products such as CO2, CO and N2.
  • unreacted feed gases e.g., CH4, H2O, NH3
  • by-products such as CO2, CO and N2.
  • the H2 must be separated from this mixed gas stream.
  • Membrane-based separation technology can be used for the separation of H2 from mixed gas streams.
  • a membrane is a near two- dimensional structure which is selectively permeable to one species.
  • a membrane allows one species to selectively permeate (H2), while blocking other species (e.g. CO, CO2, H2O, N2 etc.).
  • Hydrogen-selective membranes can be created from inorganic, metallic or ceramic materials, each of which has characteristic hydrogen throughputs, operating temperatures and selectivity.
  • Palladium is the best known alloy membrane material, having an ability to permeate hydrogen between 300 to 600 °C whilst being tolerant to syngas species such as CO and H2O.
  • the high cost of palladium (AUD 80 to 160/g Pd (June 2023)), has driven research towards minimising its consumption, most notably through alloying with less-expensive metals, and minimising thickness by depositing very thin ( ⁇ 5 pm) layers on support structures with very fine pores.
  • vanadium has the widest alloying range, which means it has the widest scope for modifying the alloy properties to meet the demands of a vanadium- based membrane.
  • vanadium-based membranes is taught in the Applicant's United States patent publication No. US20150368762A1 .
  • Vanadium-based membranes are typically connected and sealed with another tube or pipe to provide a flow path for the extracted H2 and to prevent passage of non-H2 gas species through the membrane.
  • the sealing/joining of membranes to connections is crucial for the successful application of the V-based membrane technology in the separation of high purity hydrogen from a mixed gas feed containing hydrogen.
  • high purity hydrogen suitable for use in fuel-cell electric vehicles, FCEVs require >99.97% purity as set out in ISO 14687 standard as well as maximum limits on individual gas species such as NH3 and N2. Failure of seals results in contamination of the hydrogen product, which means the membranes are no longer ‘fit for purpose’ for producing high purity hydrogen.
  • connection and sealing technique for tubular vanadium-based membranes utilises brazing between a V-based membrane to a metallic fitting, for example an end cap or connection fitting.
  • a metallic fitting for example an end cap or connection fitting.
  • W02019000026A1 teaches a brazing technique for joining and sealing a vanadium-based membrane to a metallic connector in which a filler or brazing metal is used to form a bridging section of filler metal between the vanadium-based membrane and connector over the connection interface.
  • a welded joint and associated composition is described below, as well as an associated method, that may be used to join and seal a metallic hydrogen separation membrane to a metallic connector or fitting having a different composition, in particular being formed from a different metal or metal alloy, for example a stainless steel fitting.
  • a first aspect provides a welded joint between a metallic connector and at least a metallic core of a metallic hydrogen separation membrane.
  • the welded joint comprises a fusion weld formed from and between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane.
  • the metallic connector may be formed of a different metal or metal alloy to the metallic core of the hydrogen separation membrane.
  • the fusion weld may include a sealing portion that provides a continuous seal between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane.
  • the sealing portion may have a weld metal composition that comprises less than 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane.
  • the weld metal comprises the material from which the weld is composed.
  • a weld is formed from melted metal that forms a weld pool of that melted metal that subsequently cools and solidifies to form the weld metal that connects the adjoining components, here the metallic hydrogen separation membrane and metallic connector about a connection interface.
  • the weld metal therefore comprises the metal of that solidified weld pool.
  • the fusion weld of the welded joint comprises the welded joint between the metallic connector and the metallic core, and as such may be a fusion weld that includes the metallic composition of both the metallic connector and the metallic core.
  • the fusion weld formed between and from the metallic material of the metallic connector and the metallic core.
  • the fusion weld may be formed from the material from and between the metallic connector and the metallic core of the metallic hydrogen separation membrane.
  • a fusion weld of this type creates a weld pool that includes the materials of the metallic hydrogen separation membrane and the adjoining connector about that connection interface. This type of weld effectively fuses the two components together about that connection interface. The integrity of the seal may therefore largely depend on the properties of the fusion weld and the weld metal thereof that form that seal.
  • the sealing portion of the fusion weld is the portion of the weld metal that extends between and forms a continuous seal between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane.
  • the sealing portion may comprise at least 80% of the weld metal, for example from 80 to 99 % of the weld metal, or 80 to 100% of the weld metal.
  • the sealing portion may comprise at least 90% of the weld metal, for example from 90 to 99%, or from 90 to 100% of the weld metal.
  • the sealing portion may comprise at least 95% of the weld metal, for example from 95 to 99%, or from 95 to 100% of the weld metal.
  • the weld metal may include one or more isolated sections which may have a different composition due to that section being isolated from the full welding method/ treatment to which the majority of the main body of the weld metal is subjected.
  • the weld may for example include a heel, finger or other extended body which is isolated from the full welding method/ treatment to which the majority of the main body of the weld metal is subjected. Those isolated sections may not form part of the sealing portion of the weld metal.
  • a “continuous seal” means that the sealing portion of the weld between the metallic hydrogen separation membrane and the metallic connector connects these two components together with a welded joint that does not allow substantially any gas (including any hydrogen content therein) to pass through the welded joint and the connection between the metallic hydrogen separation membrane and the metallic connector formed by the welded joint.
  • a welded joint that does not allow substantially any gas (including any hydrogen content therein) to pass through the welded joint typically refers to a welded joint that holds pressure when the membrane is internally pressurised to 10 bara N2.
  • the weld may be tested to determine if the welded joint holds 10 bara N2 for at least 12 hr, preferably for at least 24 hr at room temperature. If applicable, leaks can be detected using a snoop leak detection test (see the description below for one example of this test using Swagelok Snoop Liquid Leak Detector).
  • the fusion weld may provide a continuous leak free seal between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane.
  • “leak free seal” should be understood to comprise a welded joint that does not allow substantially any gases to pass through the welded joint. Practically, the leak properties of a weld can be tested by pressure testing with a gas such as nitrogen (N2).
  • a leak free weld or a leak free welded joint is a weld that holds 10 bara N2 for at least 12 hr at room temperature. It should be appreciated that room temperature means at temperature of from 15 to 25 e C.
  • the leak proof properties of welded joint largely depend on the weld comprising the welded joint being continuous between the components about the connection interface and also being substantially defect free - i.e. free of cracks, inclusions, voids, through which gases, including the hydrogen content in those gases, may leak.
  • this first aspect addresses limitations previously thought to exist in welding metallic hydrogen separation membranes to metallic connectors formed from a different metal or metal alloy, for example vanadium based tubular hydrogen separation membranes to stainless steel connectors.
  • this type of fusion weld may be produced between the different metallic components to provide a reproducible continuous leak proof seal over a connection interface between the metallic hydrogen separation membrane and the adjoining connector.
  • the integrity of a fusion weld may be influenced by the final composition of the weld metal, particularly the final composition of the sealing portion of the fusion weld.
  • the metal from the metallic hydrogen separation membrane may comprise a metal or metal alloy which has a composition that can have deleterious effects on the composition of the weld metal if it comprises the substantive part of the weld metal.
  • the vanadium content of a vanadium based metallic hydrogen separations can produce a weld metal with undesirable defect forming properties when alloyed with stainless steel from the metal of a stainless steel based connector. It may therefore be preferable to reduce the mass contribution of the metal from the metallic hydrogen separation membrane within the weld metal composition, e.g., relative to the mass contribution of the connector material.
  • the sealing portion of the weld metal may comprise less than 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane.
  • 40% by mass of metal may be considered to refer to the average composition across the entire mass of weld metal of the welded joint provided by the sealing region.
  • the fusion weld may therefore be formed between the metallic hydrogen separation membrane and the metallic connector to be substantially free of cracks, inclusions, voids, when the weld metal of the sealing portion comprises less than 40% by mass of metal from the metallic hydrogen separation membrane.
  • the fusion weld may be formed between the metallic hydrogen separation membrane and the metallic connector to be free of cracks, inclusions, voids, when the weld metal of the sealing portion comprises less than 40% by mass of metal from the metallic hydrogen separation membrane. In some embodiments, the fusion weld may be formed between the metallic hydrogen separation membrane and the metallic connector which may be substantially leak free, or in some forms, leak free, when the weld metal of the sealing portion comprises less than 40% by mass of metal from the metallic hydrogen separation membrane.
  • the properties of the weld metal improves with even less mass contribution of the metal from the metallic core within the weld metal composition.
  • the weld metal of the sealing portion comprises less than 35% by mass of metal from the metallic core.
  • the weld metal of the sealing portion comprises less than 30% by mass of metal from the metallic core.
  • the weld metal of the sealing portion comprises less than 25% by mass of metal from the metallic core.
  • the weld metal of the sealing portion may comprise one of: less than 38%, less than 34%, less than 33%, less than 31 %, less than 28%, less than 23%, or less than 20% by mass of metal from the metallic core.
  • mass% used throughout this specification could be expressed in (and thus can be used interchangeably) with weight%.
  • the weight of a body is equal to the mass x gravity. When expressed in %, mass% is therefore equivalent to weight%.
  • the composition of the weld metal may be substantially homogenous across the volume of the weld metal of the sealing portion.
  • the weld metal of the sealing portion may have a substantially consistent or homogeneous volumetric composition throughout the entire volume/ material thereof in the of the sealing portion of the fusion weld.
  • compositional variation may exist in the weld metal, ideally, there are no isolated pockets in the weld metal of the sealing portion that have a composition that exceeds 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane, or the desired mass% limit as defined there above.
  • no portion of the volumetric composition of the weld metal of the sealing portion comprises no more than 40% by mass of metal from the metallic core, preferably no more than 35% by mass of metal from the metallic core. In some embodiments, no portion of the volumetric composition of the weld metal of the sealing portion comprises 30% by mass of metal from the metallic core, preferably no more than 25% by mass of metal from the metallic core. In some embodiments, no portion of the volumetric composition of the weld metal of the sealing portion comprises 35% by mass of metal from the metallic core, preferably no more than 20% by mass of metal from the metallic core. It should be appreciated that the volumetric composition comprises the composition across the full volume of the weld metal in the sealing portion of the welded joint.
  • the weld metal of the sealing portion may have a substantially homogenous composition throughout the volume of weld metal in embodiments.
  • the composition of weld metal of the welded joint may be substantially homogenous throughout the volume of weld metal.
  • the weld metal of the sealing portion may have a substantially uniform composition throughout the volume of weld metal.
  • the weld metal of the sealing portion may have a substantially homogenous composition throughout the volume of main body of the weld metal of the sealing portion.
  • the weld metal of the sealing portion may have a homogenous composition throughout the volume of main body of the weld metal of the sealing portion.
  • the main body of the weld metal of the sealing portion may be the volume or mass of metal spaced away from the perimeter or edges of the welded joint.
  • the main body of the weld metal of the sealing portion comprises an interior portion of the volume of weld metal of the welded joint.
  • the perimeter region and/or edge region of the weld metal typically includes a composition which transitions from the composition of the main body of the weld metal to the adjoining metal composition, and thus may not conform with the substantially homogenous of the main body of the weld metal.
  • the weld metal may include one or more isolated sections which may have a different composition due to that section being isolated from the full welding method/ treatment to which the majority of the main body of the weld metal is subjected. Those isolated sections also would not form part of the main body of the weld metal of the sealing portion.
  • the main body of the weld metal of the sealing portion therefore comprises at least 90% of the volume of the weld metal of the sealing portion, for example from 90 to 95 %, preferably 90 to 96 %, more preferably 90 to 98 % of the volume of the weld metal of the sealing portion.
  • a fusion weld typically substantially comprises a solidified mixture of the materials at and around the welded joint.
  • the fusion weld may substantially comprise the metals from the metallic hydrogen separation membrane and the metallic connector, preferably from the metallic core of the metallic hydrogen separation membrane and the metallic connector.
  • the balance of metal of the weld metal over the metal from the metallic hydrogen separation membrane typically comprises most if, not substantially all a metallic composition from the metallic connector.
  • the fusion weld may comprise an autogenous weld.
  • the weld metal substantially comprises the metal from the metallic connector and the metallic hydrogen separation membrane sourced from the metal at and proximate to the connection interface of that welded joint.
  • the welded joint may be formed as a fusion weld with at least one filler metal, preferably at least one filler wire.
  • the composition of that filler metal may be selected to enhance or optimise the properties of the weld metal.
  • the filler metal can be selected from at least one of: stainless steel, steel, aluminium-silicon, copper, copper alloy, gold-silver alloy, nickel alloy or silver.
  • the connector may be formed of/ from any suitable metal or metal alloy onto which it may be desired to mount the hydrogen separation membrane.
  • the connector may be comprised of at least one of: steel, stainless steel, nickel-chromium-iron alloy, brass, Inconel, Incoloy or a combination thereof.
  • suitable materials include austenitic stainless steel, preferably a 300 series stainless steel, for example 303, 304, or 316 stainless steel.
  • the metallic core of the hydrogen separation membrane may be the base metallic material from which the hydrogen separation membrane is formed.
  • the hydrogen separation membrane may comprise that core in and of itself (e.g., the hydrogen separation membrane may consist of a core).
  • the metallic core may include one or more further layers, for example coated layers over the surface of that metallic core.
  • the metallic hydrogen separation membrane and the metallic core thereof may comprise a metal capable of hydrogen separation through the dissociative chemisorption of hydrogen on the surface, and then hydrogen diffusion through the metal lattice driven by the partial pressure drop to the opposite side of the membrane, followed by the re-combination of hydrogen atoms and desorption of hydrogen from the permeate side.
  • Metallic membranes can separate and produce hydrogen (at high permeability, purity and recovery) from H2/CO2 mixtures, H2/N2/NH3 mixtures, or any other H2 containing gas mixtures.
  • at least the metallic core of the hydrogen separation membrane may comprise a group 5 (group V) based metal or metal alloy, preferably a vanadium, tantalum or niobium metal or metal alloy.
  • the hydrogen separation membrane may be formed from vanadium or a vanadium alloy.
  • the particular vanadium metal or alloy may be selected based on its suitability for use in a membrane separation device.
  • the hydrogen separation membrane comprises a vanadium alloy that comprises vanadium, aluminium having a content of greater than 0 to 10 at%, and Ta content of less than 0.01 at%, having a ductility of greater than 10% elongation, preferably greater than 1 1 % elongation.
  • the vanadium alloy can further comprise a grain refining element selected from Ti, Cr, Fe, Ni or B having a content of greater than 0 to 5 at%, preferably between 0.2 and 4.5 at%.
  • the grain refining element has a content from 0.1 to 2 at%, preferably from 0.1 to 2 at%, and more preferably from 0.1 to 1 at%.
  • the hydrogen separation membrane may have any suitable configuration.
  • the hydrogen separation membrane and the metallic core thereof may be tubular.
  • the metallic hydrogen separation membrane may comprise a thin walled hydrogen separation membrane, preferably a thin walled tubular hydrogen separation membrane.
  • the thin walled tubular hydrogen separation membrane may comprise tubular metallic core having an outer diameter of between 2 to 25 mm, preferably between 3 and 20 mm and a wall thickness of from 0.05 to 1 mm, preferably from 0.1 to 1 mm.
  • the metallic core of the hydrogen separation membrane may have a wall thickness of from 0.1 to 1 mm, preferably from 0.2 to 0.8 mm, more preferably from 0.2 to 0.5 mm. It is noted that in these thin walled embodiments, the welded joint may be characterised as a thick-to-thin welded joint.
  • the metallic core comprises a non-porous body, preferably a non-porous tube.
  • the metallic core that forms the core material of the hydrogen separation membrane may typically be formed from a non-porous, fluid tight body, such as a tube. It should be appreciated that hydrogen separation membranes formed from a group 5 based material or similar separates hydrogen through the diffusion of hydrogen through that material.
  • the permeation of hydrogen through a metallic membrane of this type consists of dissociation of hydrogen molecules (H2) to atoms (H) on the membrane, diffusion of H in the metal of the membrane, and recombination of H to H2 on the other side of the membrane.
  • the metallic core comprises a fluid tight body such as a gas-tight body, preferably a fluid-tight tube, such as a gas-tight tube.
  • the metallic core comprises a dense body, preferably a dense tube.
  • the metallic core comprises a solid body, preferably a solid tube.
  • the welded joint may be between the metallic core of the metallic hydrogen separation membrane and the metallic connector, or could be made between the metallic hydrogen separation membrane and the metallic connector. In some embodiments, the welded joint may be made between a metallic core that forms the main core material of the hydrogen separation membrane and the metallic connector before further layers are applied to the metallic core, to form the final metallic coated structure of the hydrogen separation membrane.
  • metallic core refers to the core metallic material that the hydrogen separation membrane may be formed from. That core material may be preferably coated with one or more layers to from the final metallic coated structure of the hydrogen separation membrane.
  • the metallic core of the hydrogen separation membrane may be coated in a Pd based coating, for example a Pd-coating or a Pd alloy coating, such as a Pd-Au based coating. That Pd based coating (for example a Pd coating, or a Pd-Au based coating) can be applied to the metallic core prior to forming the welded joint or after forming the welded joint with the connector.
  • the welded joint may be made between the hydrogen separation membrane (comprising the metallic core and any further layers already applied to the metallic core) and the metallic connector.
  • the metallic core may comprise a vanadium body, such as a vanadium tube that has at least one palladium or palladium alloy coating applied to one or more outer surfaces to form the final metallic coated structure of the hydrogen separation membrane.
  • the connector may have any suitable configuration.
  • the connector may comprise a metallic fitting, for example a connection fitting or end cap fitting, and preferably a metallic fluid connection fitting, more preferably a metallic gas connection fitting.
  • the connector may be tubular.
  • the connector may have any suitable dimensions.
  • the connector has a wall thickness of from 1 to 5 mm, preferably from 1 to 3 mm, or more preferably from 1 to 2 mm.
  • the connector formation of the connector may have any suitable configuration.
  • the connector formation may comprise a sloped or bevelled section configured to receive the end section of the hydrogen separation membrane thereon.
  • the connector formation may comprise an angled sloped end of the connector formation having a reduced diameter. This forms a ramped or curved section onto which at least the metallic core of the hydrogen separation membrane can be mounted.
  • the sloped or bevelled section may comprise a frustoconical shaped section.
  • the connection interface may comprise a substantially planar end face of the metallic core of the hydrogen separation membrane that may be arranged in parallel abutting or adjoining relationship to a substantially planar adjoining face of the connector formation.
  • connection configuration between the metallic core and/or metallic hydrogen separation membrane and metallic connector may have a variety of forms.
  • the metallic core of the metallic hydrogen separation membrane may be mounted on or against a connector formation of the connector, the metallic core and the connector formation contacting at a connection interface in which an end face of the metallic core may be proximate to, substantially abuts or overlaps an adjoining face of the connector formation; and the welded joint connects at least the metallic core of the hydrogen separation membrane and the connector about the connection interface.
  • connection configurations are also possible, and that the present invention should not be limited to this particular configuration.
  • the welded joint between at least the metallic core of the hydrogen separation membrane and the connector about the connection interface may comprise a fusion welded connection.
  • the welded joint may be formed using any suitable welding technique for example a laser welded connection, an arc welded connection such as TIG, or electron beam welding.
  • the welded joint may comprise a continuous weld which extends circumferentially around and over the connection interface. This forms a continuous fusion welded seal over the connection interface between at least the metallic core of the hydrogen separation membrane and the connector formation.
  • the weld may be autogenous (no filler material added).
  • a filler material may be used in the welded joint, for example at least one of stainless steel, steel, aluminium-silicon, copper, copper alloy, gold-silver alloy, nickel alloy or silver.
  • the end face of at least the metallic core of the hydrogen separation membrane at the connection interface may comprise a substantially square edge.
  • a square edge can be advantageous as this profile may be easy to consistently machine, improving reproducibility and repeatability.
  • the connector formation may comprise a tapered, sloped or bevelled section configured to receive the end section of the hydrogen separation membrane thereon.
  • the sloped of tapered section may be in the form of a frustoconical shaped section.
  • that tapered surface can have a taper angle of 15 to 60°, preferably 15 to 45°, more preferably 15° to 30°, and yet preferably around 30°.
  • the taper on the connector formation may be advantageously designed to allow for variations in both the diameter and thickness of the metallic core of the hydrogen separation membrane. Additionally, the taper angle may be optimised to enable further material of the connector to be melted into the weld pool, minimising concentration of the metal from the metallic core, for example vanadium, in the weld pool (to therefore minimise associated risk of cracking).
  • the weld may be joined and filled with the weld material in any suitable configuration.
  • the weld may be formed as an underfilled weld, i.e. comprises an underfilled weld. It should be appreciated that by underfilled, it is means that the welded joint does not extend above (stand proud of) the surface of the metallic core/ hydrogen separation membrane. The weld falls below the outer surface of the metallic core/ hydrogen separation membrane, preferably forming a dip or depression therein.
  • the first aspect may provide a welded joint between a metallic connector and at least a metallic core of a metallic hydrogen separation membrane, the welded joint comprising a fusion weld formed from and between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane that provides a continuous seal therebetween.
  • the metallic connector is formed of a different metal or metal alloy to the metallic core of the hydrogen separation membrane.
  • the weld metal of the welded joint comprises less than 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane.
  • Embodiments of the first aspect may provide a welded joint between a metallic connector and at least a metallic core of a metallic hydrogen separation membrane comprising a fusion weld formed from and between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane, wherein the connector is formed of a different metal or metal alloy to the metallic core of the hydrogen separation membrane, and wherein the fusion weld includes a sealing portion that provides a continuous seal between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane, the sealing portion having a weld metal composition that comprises less than 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane.
  • a second aspect provides a method of joining and sealing at least a metallic core of a hydrogen separation membrane to a metallic connector.
  • the method may be used to form a continuous welded seal, such as a fusion welded seal, between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane.
  • Such continuous welded seal may comprise a leak free welded seal.
  • the method may include mounting an end section of at least the metallic core of the metallic hydrogen separation membrane on or against a connector formation of a metallic connector, the connector being formed of a different metal or metal alloy to the metallic core.
  • the metallic core and the connector formation may contact at a connection interface in which an end face of at least the metallic core of the hydrogen separation membrane may be proximate to, substantially abuts or overlaps an adjoining face of the connector formation.
  • the method may include welding at least the metallic core of the hydrogen separation membrane to the connector to form a welded joint at and over the connection interface using a weld, such as a fusion weld, comprising a weld metal composition that comprises less than 40% by mass of metal from the metallic core.
  • At least the metallic core of the hydrogen separation membrane may be joined to the metallic (for example stainless steel) connector using a suitable joining or connection method, for example a welding method such as laser welding, an arc welding method such as TIG, or electron beam welding in a manner that creates a fusion weld comprising a weld metal composition that comprises less than 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane.
  • a suitable joining or connection method for example a welding method such as laser welding, an arc welding method such as TIG, or electron beam welding in a manner that creates a fusion weld comprising a weld metal composition that comprises less than 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane.
  • the weld metal of the sealing portion of the fusion weld may comprise less than 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane.
  • 40% by mass of metal refers to the average composition across the entire mass of weld metal of the sealing portion of the welded joint.
  • the properties of the weld metal improve with even less mass contribution of the metal from the metallic hydrogen separation membrane within the weld metal composition.
  • the weld metal of the sealing portion comprises at least one of: less than 35% by mass of metal from the metallic core; less than 30% by mass of metal from the metallic core; or less than 25% by mass of metal from the metallic core.
  • the weld metal of the sealing portion may comprise one of: less than 39%, less than 38%, less than 34%, less than 33%, less than 28%, less than 23%, or less than 20% by mass of metal from the metallic core of the metallic hydrogen separation membrane.
  • the weld metal may have a substantially consistent or homogeneous volumetric composition throughout the entire volume/ material thereof in the of the sealing portion of the fusion weld of the welded joint.
  • compositional variation may exist in the weld metal
  • no portion of the volumetric composition of the weld metal of the sealing portion comprises no more than 40% by mass of metal from the metallic core, preferably no more than 35% by mass of metal from the metallic core.
  • no portion of the volumetric composition of the weld metal of the sealing portion comprises 30% by mass of metal from the metallic core, preferably no more than 25% by mass of metal from the metallic core. In some embodiments, no portion of the volumetric composition of the weld metal of the sealing portion comprises 33% by mass of metal from the metallic core, preferably no more than 20% by mass of metal from the metallic core.
  • the weld metal of the sealing portion may have a substantially homogenous composition throughout the volume of weld metal in embodiments.
  • the composition of weld metal of the welded joint may be substantially homogenous throughout the volume of weld metal.
  • the weld metal of the sealing portion may have a substantially uniform composition throughout the volume of weld metal.
  • the weld metal of the sealing portion may have a substantially homogenous composition throughout the volume of main body of the weld metal.
  • the weld metal of the sealing portion may have a homogenous composition throughout the volume of main body of the weld metal It should be appreciated that the main body of the weld metal of the sealing portion may be the volume or mass of metal spaced away from the perimeter or edges of the welded joint.
  • the main body of the weld metal of the sealing portion comprises an interior portion of the volume of weld metal o the welded joint.
  • the perimeter region and/or edge region of the weld metal typically includes a composition which transitions from the composition of the main body of the weld metal to the adjoining metal composition, and thus may not conform with the substantially homogenous of the main body of the weld metal.
  • the main body of the weld metal therefore comprises at least 90% of the volume of the weld metal of the sealing portion, for example from 90 to 95 %, preferably 90 to 96 %, more preferably 90 to 98 % of the volume of the weld metal of the sealing portion.
  • the welded joint between at least the metallic core of the hydrogen separation membrane and the connector comprises a fusion welded connection.
  • the welded joint may be formed by at least one of: laser welding, electron beam welding, or an arc welding such as TIG, or electron beam welding.
  • the welded joint may comprise a continuous weld which extends circumferentially around and over the connection interface.
  • the welded joint may be formed using at least one continuous weld pass around the connection interface. This forms a continuous fusion welded seal over the connection interface between at least the metallic core of the hydrogen separation membrane and the connector formation.
  • the weld may be autogenous (no filler wire added).
  • a filler material may be used in the welded joint, for example at least one of aluminium-silicon, copper, copper alloy, gold-silver alloy, nickel alloy or silver.
  • the welded joint may be formed from a single weld pass at, around or proximate the connection interface.
  • the welded joint may be formed using at least two weld passes at, around or proximate the connection interface, one or both of which may be continuous weld passes.
  • the welded joint may be formed using two continuous weld passes at or around the connection interface.
  • the at least two weld passes may comprise: a first pass weld forming a first pass weld composition between the at least the metallic core of the hydrogen separation membrane and the connector; and a second pass weld, which may be used to dilute the first pass weld composition with more metal from the connector. In that way, the second pass weld may be used to reduce the composition of metal from the metallic core of the hydrogen separation membrane in the weld metal of the sealing portion, e.g., to be less than 40% by mass of metal from the metallic core.
  • the first pass weld may be used to substantially fuse the at least the metallic core of the hydrogen separation membrane to the connector.
  • the second pass weld may be used to form a continuous seal between the metallic core of the metallic hydrogen separation membrane and the connector.
  • the second pass weld may also be used to dilute the weld pool with more metal from the connector.
  • This second pass weld may therefore be configured to create a substantially homogenous weld metal composition (e.g., in a sealing portion of the weld, which may extend from membrane to connector).
  • the second pass may be used to introduce more metal mass from the connector material, and thus reduce the mass of metal of the metallic core in the weld metal of the sealing portion, and thus reduce the risk of cracking from the alloy composition that may result from an undesirable mass of metal from the metallic core.
  • this may be achieved by targeting the weld pool more on the connector material, i.e. further on the connector side of the connection interface.
  • remelting the weld pool in the second pass helps to distribute the metals more evenly throughout the weld pool, creating a more homogenous composition through the weld metal.
  • the at least two continuous weld passes comprise laser welding passes using a laser beam, and wherein the second weld pass employs a broader laser beam width for the laser relative to the laser beam width of the first pass.
  • the broader laser beam size may increase melting I dilution from connector metal and reduce the mass of metal of the from the metallic core in the weld pool to below the desired amount/ concentration (for example below 40 %).
  • the second pass may reduce the mass of metal of the from the metallic core in the weld pool to below at least one of: 38 % by mass of metal, 36 %, 35 %, 33%, 30 %, 25 %, or 20 %. In embodiments, the second pass may reduce the mass of metal of the from the metallic core in the weld pool to below 35%. In embodiments, the second pass may reduce the mass of metal of the from the metallic core in the weld pool to below 30 %. In embodiments, the second pass may reduce the mass of metal of the from the metallic core in the weld pool to below 25 %. In embodiments, the second pass may reduce the mass of metal of the from the metallic core in the weld pool to below 20 %.
  • the first pass weld may have welding focal point, for example a laser welding focal point, located on or proximate to the connector interface between the metallic hydrogen separation membrane and the connector.
  • a tight/narrow laser beam width may be used, for example that laser beam will be tighter/narrower than a subsequent second pass weld, where used (see below).
  • the function of the tight/narrow laser beam width may be to produce a focused and deep penetrating laser beam into that focal point.
  • the applied power of the laser may be applied following a number of waveforms. In embodiments, the applied power of the laser may follow a pulse wave form. That pulse waveform may have an initial peak, that decreases on a curve to reduce the applied laser power as the first pass weld progresses.
  • the second pass weld may have a laser focal point that is positioned further away from the connector interface between the metallic hydrogen separation membrane compared to the welding focal point of the first pass weld.
  • the welding focal point of the second pass weld may be located within the connector spaced away from the connector interface.
  • the welding focal point of this second pass may be located at a distance 1 /2 of the increase in beam diameter/ width of the laser beam width of the second pass weld, compared to the first pass weld. This may be used to ensure that the location of edge of the laser beam on the metallic hydrogen separation membrane remains the same for both the first and second passes.
  • the applied power of the laser may again be applied following a number of waveforms. In embodiments, the applied power of the laser may follow a pulse wave form. That pulse waveform may be applied with a constant laser power.
  • the connector, the metallic core, and the hydrogen separation membrane can have the features defined above for the first aspect.
  • the connector may be formed from any suitable metal, for example at least one of: steel, stainless steel, nickel-chromium-iron alloy, brass, Inconel, Incoloy or a combination thereof.
  • the metallic core and/or hydrogen separation membrane may comprise any suitable hydrogen separation metal or alloy.
  • at least the metallic core of the hydrogen separation membrane may comprise a group V based metal or metal alloy, preferably a vanadium, tantalum or niobium metal or metal alloy, more preferably vanadium or a vanadium alloy.
  • at least the metallic core of the hydrogen separation membrane may be formed from vanadium or a vanadium alloy for example a vanadium alloy that comprises vanadium, aluminium having a content of greater than 0 to 10 at%, and Ta content of less than 0.01 at%, having a ductility of greater than 10% elongation, preferably greater than 1 1 % elongation.
  • the vanadium alloy further comprises a grain refining element selected from Ti, Cr, Fe, Ni or B having a content of greater than 0 to 5 at%, preferably between 0.2 and 4.5 at%.
  • the metallic core of the hydrogen separation membrane may also be coated in a Pd based coating or a Pd-Au based coating.
  • the metallic core and the hydrogen separation membrane are tubular.
  • the connector may be tubular.
  • the connector formation may have any suitable configurations.
  • the connector formation comprises a sloped or bevelled section configured to receive the end section of at least the metallic core of the hydrogen separation membrane thereon.
  • the second aspect may provide method of joining and sealing at least a metallic core of a hydrogen separation membrane to a metallic connector comprising: mounting an end section of at least the metallic core of the metallic hydrogen separation membrane on or against a connector formation of a metallic connector, the connector being formed of a different metal or metal alloy to the metallic core of the hydrogen separation membrane, the metallic core and the connector formation contacting at a connection interface in which an end face of at least the metallic core of the hydrogen separation membrane is proximate to, substantially abuts or overlaps an adjoining face of the connector formation; welding at least the metallic core of the hydrogen separation membrane to the connector to form a welded joint at and over the connection interface using comprising a fusion weld, said fusion weld including a sealing portion that provides a continuous seal between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane, the sealing portion comprising having a weld metal composition that comprises less than 40% by mass of metal from the metallic core of metallic hydrogen separation membrane, thereby forming a continuous
  • a third aspect also relates to a gas separation membrane system incorporating a hydrogen separation membrane that may be joined and sealed to a connector formation using a welded joint according to the first aspect and/or a welded joint formed by the method of according to the second aspect.
  • the application of the sealing and joining arrangement of the present invention may be used to enable a hydrogen separation tubular membrane to be fitted into a catalytic membrane reactor (CMR) or membrane separator for use for selective separation of hydrogen gas from a mixed gas stream (with hydrogen and other gases), producing high purity hydrogen (suitable for FCEV refuelling applications) in the permeate stream from the membrane.
  • CMR catalytic membrane reactor
  • the associated method may provide a means to join the hydrogen separation membrane to other metallic structures (tube connections, tube ends, etc) to form a hydrogen separation system (in the form of a CMR), whilst maintaining sealing integrity, i.e. maintaining mechanical integrity I robustness through multiple cycles of operation.
  • a fourth aspect provides at least one of: a catalytic membrane reactor (CMR) or a membrane separator that includes at least one hydrogen separation membrane that may be joined and sealed to a connector using a welded joint according to the first aspect and/or a welded joint formed by the method of according to the second aspect.
  • CMR catalytic membrane reactor
  • membrane separator that includes at least one hydrogen separation membrane that may be joined and sealed to a connector using a welded joint according to the first aspect and/or a welded joint formed by the method of according to the second aspect.
  • the hydrogen separation membrane of this fourth aspect may have any suitable configuration selected based on the particular advantages that configuration can provide to a particular CMR or membrane separator configuration.
  • a CMR is essentially a two-dimensional device which channels syngas or alternatively ammonia (if catalytically cracking ammonia) along one dimension through a catalyst bed adjacent to a membrane.
  • Flat membranes can be easier and cheaper to produce than tubular membranes, but have a larger seal area, as the membranes are sealed around their outer edge. This sealing configuration provides a large sealing area and therefore can be prone to leaks between the raffinate and permeate gas streams.
  • a tubular membrane enables a tubular CMR to be used, and therefore can reduce the seal area. In tubular reactors seals are only required at each end of the tube. The joining and sealing method of the present invention can be used to provide these seals. Similar considerations are also applicable for membrane separator configurations.
  • the hydrogen separation membranes described in relation to each aspect may have a tubular configuration, for example comprising tubes. These tubular membranes may have any suitable dimensions as described above.
  • the thin-walled tube may comprise a tube having an outer diameter of between 2 to 25 mm, preferably between 3 and 20 mm and a wall thickness of from 0.05 to 1 mm, preferably from 0.1 to 1 mm.
  • the tubular membrane may comprise a thin-walled tube that comprises a vanadium alloy comprising vanadium, aluminium having a content of greater than 0 to 10 at%, and Ta content of less than 0.01 at%, having a ductility of greater than 10% elongation, preferably greater than 1 1 % elongation.
  • the hydrogen separation membrane may be coated in a Pd based coating or a Pd-Au based coating.
  • Figure 1 illustrates a cross-sectional view of one type of hydrogen separation membrane arrangement that includes a welded joint between a hydrogen separation membrane and connectorn.
  • Figure 1 A provides a schematic view illustrating the taper of the connector and square edge of the hydrogen separation membrane at a connection interface where a welded joint may be located.
  • Figure 2 illustrates forming a planar connection surface on the end of a vanadium-based tube for use in a joining and sealing arrangement.
  • Figure 3 provides an optical microscopy images of the cross-section of one welded joint between the end section of the vanadium-based membrane and a connector.
  • Figure 4 provides (4A) a schematic view of the connection interface between a hydrogen separation membrane and connector set up for a first weld pass to form the welded joint shown in Figure 1 ; and (4B) the pulse shape used for application of the laser beam.
  • Figure 5 provides (5A) a schematic view of the connection interface between a hydrogen separation membrane and connector set up for a second weld pass to form the welded joint shown in Figure 1 ; and (5B) the pulse shape used for application of the laser beam.
  • Figure 6 provides (A) an EDS line scan analyses (showing elemental composition, by mass %) of the weld pool; and (B) corresponding SEM images of weld cross sections (line 210 depicting the EDS line scan path), for a welded joint between a vanadium membrane tube and a stainless steel connector with only a single-pass weld.
  • Figure 7 provides (A) an EDS line scan analyses (showing elemental composition, by mass %) of the weld pool; and (B) corresponding SEM images of weld cross sections (line 215 depicting the EDS line scan path), for a welded joint between a vanadium membrane tube and a stainless steel connector following a second pass weld.
  • Figure 8 illustrates an example of one type of a laser welder that can be used to form the welded joint.
  • the laser welded has a modified shield, not shown, to accommodate 1100 mm long hydrogen separation membranes.
  • Figure 9 illustrates the Jig assembly for holding membranes and fittings for automated laser welding operations that can be used in the laser welder shown in Figure 8.
  • Figure 10 provides (A) an EDS line scan analyses (showing elemental composition, by mass %) of the weld pool; (B) SEM image of the joint along the EDS line scan path; and (C) corresponding SEM images of weld cross sections (line 410 depicting the EDS line scan path), for another welded joint between a vanadium membrane tube and a stainless steel connector with only a single-pass weld.
  • Figure 11 provides (A) an EDS line scan analyses (showing elemental composition, by mass %) of the weld pool; (B) SEM image of the joint along the EDS line scan path; and (C) corresponding SEM images of weld cross sections (line 415 depicting the EDS line scan path), for a welded joint between a vanadium membrane tube and a stainless steel connector following a second pass weld.
  • Figure 11 A provides a SEM backscatter image (AsB) showing the grain structure of the welded joint between a vanadium membrane tube and a stainless steel connector following a second pass weld which has been formed using a similar procedure to the welded joint shown in Figure 1 1 .
  • Figure 12 provides (A) an EDS line scan analyses (showing elemental composition, by mass %) of the weld pool; (B) SEM image of the joint along the EDS line scan path; and (C) corresponding SEM images of weld cross sections (line 410 depicting the EDS line scan path), for a welded joint between a vanadium membrane tube and an Inconel 600 connector with only a single-pass weld.
  • Figure 13 provides (A) an EDS line scan analyses (showing elemental composition, by mass %) of the weld pool; (B) SEM image of the joint along the EDS line scan path; and (C) corresponding SEM images of weld cross sections (line 415 depicting the EDS line scan path), for a welded joint between a vanadium membrane tube and an Inconel 600 connector following a second pass weld.
  • Figure 13A provides a SEM backscatter image (AsB) showing the grain structure of the welded joint between a vanadium membrane tube and an Inconel 600 connector following a second pass weld which has been formed using a similar procedure to the welded joint shown in Figure 13.
  • joints such as welded joints and a composition thereof, together with methods, used for joining and sealing a metallic hydrogen separation membrane (or at least the metallic core thereof) to a metallic connector formed from a different metal, for example stainless steel.
  • Hydrogen separation membranes comprise metallic membranes that can be configured to separate and produce hydrogen (at high permeability, purity and recovery) from H2/CO2 mixtures, H2/N2/NH3 mixtures, or any other H2 containing gas mixtures.
  • the metallic core of some of these hydrogen separation membranes may comprise a group 5 (group V) based metal or metal alloy such as a vanadium, tantalum or niobium metal or metal alloy.
  • group V group V
  • Useful examples of a suitable metallic core for a hydrogen separation membrane include vanadium or a vanadium alloy, which will be exemplified in the remainder of the specification for the rest of the specification.
  • the present invention may be more generally applied to other metallic hydrogen separation membranes, and in particular other group 5 metals or metal alloys.
  • MMT Metal Membrane Technology
  • Pd palladium
  • V vanadium
  • the vanadium tube forms the metallic core of this hydrogen separation membrane which can be coated in a Pd based coating, for example a Pd coating, or a Pd alloy coating such as a Pd-Au alloy catalytic coating.
  • Hydrogen separation membrane tubes may require seals on both ends to form a sealed hydrogen containing membrane, and to connect to H2 product take off tubes. This seal may be achieved by welding a metallic connector, typically a stainless steel fluid fitting to each end of the hydrogen separation membrane tube. The connector can be welded to the vanadium tube prior to the addition of the Rd/ Pd-Au based catalytic coating, or after that coating has been applied to the vanadium tube.
  • any connection between this type of hydrogen separation membrane tube and a connector ideally is configured with hydrogen expansion in mind.
  • Vanadium-based hydrogen -separation membranes for example vanadium-based hydrogen separation membrane tubes can have a linear (dimensional) expansion in the order of up to +5% and can volumetrically expand in the order of up to +15% when hydrogenated at conventional operating temperatures/pressures, compared to ambient conditions without hydrogen.
  • Other metallic hydrogen separation membranes such as those formed from group 5 metals and alloys thereof have similar linear and volumetric expansion when hydrogenated. This expansion can place significant strain and stress on a welded joint between these types of hydrogen separation membranes and an adjoining connector which can be significant enough to affect the integrity of the seal and join about the sealed welded joint.
  • the Applicant has developed a method of sealing and a hydrogen separation connection arrangement comprising (1 ) a welded joint (the subject of the present patent specification) that creates an advantageous continuous leak free seal between a hydrogen separation membrane and an adjoining connector/ fluid fitting; and (2) a constriction collar that can be advantageously used to mechanically limit the hydrogenated expansion of the hydrogen separation membrane at and proximate to the welded joint.
  • This constriction collar is the subject of the Applicant’s co-pending international patent application entitled “Arrangement for Joining and Sealing a Metallic Hydrogen Separation Membrane to a Metallic Connector” published as international patent publication W02024/007057, the contents of which should be understood to be incorporated into this specification by this reference.
  • Figure 1 illustrates one example of the overall hydrogen separation membrane arrangement 100 that includes the welded joint 130.
  • the illustrated arrangement 100 includes:
  • the hydrogen separation membrane exemplified here as a vanadium-based membrane 1 10, preferably comprises a vanadium or vanadium alloy tube, which may be configured for use as a hydrogen selective membrane, for example as taught in United States Patent No. 10,590,516 the contents of which should be understood to be incorporated into this specification by this reference.
  • the vanadium-based membrane may be formed from a metallic core tube comprising a vanadium or a vanadium alloy.
  • the particular vanadium metal or alloy may be selected based on its suitability for use in a membrane separation device.
  • the metallic core may comprise a vanadium alloy comprising: vanadium; aluminium having a content of greater than 0 to 10 at%; and Ta content of less than 0.01 at%, having a ductility of greater than 10% elongation, preferably greater than 1 1 % elongation.
  • the vanadium alloy can further comprise a grain refining element selected from Ti, Cr, Fe, Ni or B having a content of greater than 0 to 5 at%, preferably between 0.2 and 4.5 at%.
  • the grain refining element has a content from 0.1 to 2 at%, preferably from 0.1 to 2 at%, and more preferably from 0.1 to 1 at%.
  • this vanadium metallic core may be coated in a Pd based coating or a Pd-Au based coating, which forms a catalytic coating over the surface of that core material.
  • vanadium or vanadium alloys may equally be used for a hydrogen selective membrane/ hydrogen separation membrane.
  • the vanadium-based membrane 1 10 and metallic core thereof may comprise a non-porous tube, providing a solid fluid-tight body, for example a dense metal body, through which hydrogen diffusion to occur.
  • the illustrated vanadium-based membrane 1 10 has an outer diameter (D) about the longitudinal axis X-X. That outer diameter D is the outer diameter of the vanadium-based membrane when the vanadium -based membrane 110 is in an un-hydrogenated state (i.e. not in a hydrogenated expanded state).
  • the vanadium-based membrane 1 10 may comprise a thin-walled tube comprises a tube having an outer diameter of between 2 to 25 mm, and a wall thickness of from 0.1 to 1 mm.
  • other configurations could equally be used as discussed above.
  • a connector 120 may be fitted to each end of the hydrogen separation membrane tube to enable a fitting, such as a gas conduit or end cap, be connected thereon.
  • the illustrated connector 120 comprises a metallic fluid connection fitting (preferably a metallic gas connection fitting) formed from a different metal or metal alloy to the metallic core of the vanadium-based membrane 1 10.
  • suitable metal or metal alloys that the connector 120 can be formed from include one of steel, stainless steel, nickel-chromium- iron alloy, brass, Inconel, Incoloy or a combination thereof.
  • the illustrated connector 120 (the overall fitting) includes a connector formation 122 (the end section of connector 120 forming part of the connection interface with the vanadium-based membrane 1 10) configured to receive an end section 1 1 1 of at least the metallic core of the vanadium-based membrane 1 10 thereon.
  • the connector formation 122 comprises a sloped section in the form of a frustoconical shaped section.
  • the illustrated end section 11 1 of the vanadium-based membrane 1 10 may be configured with a square edge 1 1 1 A, as described below in more detail. However, again it should be appreciated that other end section configurations could equally be used.
  • the illustrated welded joint 130 may be located at and over a connection interface 132 between the end section 1 11 of at least the metallic core of the vanadium-based membrane 110 and the connector formation 122 where the end section 11 1 of the metallic core of the vanadium-based membrane 1 10 substantially abuts or overlaps an adjoining face of the connector formation 122.
  • This welded joint (also known as a welded connection) 130 may comprise a continuous weld which extends circumferentially around and over the connection interface 132.
  • the welded joint 130 may be formed using any selected welding technique the produces an advantageous weld metal composition between the connector and at least the metallic core of the vanadium-based membrane 1 10. Examples of different welding processes for forming this welded joint 130 are described in more detail below.
  • a constriction collar 140 may optionally also be used in the connection arrangement that is configured to extend from at least the connection interface 132 and welded joint 130 and extend axially over the vanadium-based membrane 1 10 relative to the longitudinal axis X-X.
  • the constriction collar 140 extends over the connection interface 132 and welded joint 130 and extends axially over the vanadium-based membrane 110 and at least part of the connector 120 relative to the longitudinal axis X-X.
  • the illustrated constriction collar 140 comprises a substantially cylindrically shaped tube.
  • the constriction collar can have any suitable overall shape and configuration. Again, the details of this constriction collar are covered in in the Applicant’s co-pending international patent application referenced above.
  • the illustrated welded joint 130 comprises a fusion weld.
  • this type of weld comprises a solidified mixture of the metals from at and around the welded joint 130.
  • the weld metal of the welded joint 130 is formed from a melted mixture of the metals from the metallic hydrogen separation membrane (exemplified as a vanadium tube 1 1 1 in Figure 3) and the metallic connector (exemplified as a stainless steel fitting 122 in Figure 3).
  • a further filler material may be used in the weld, to supplement material added in the weld pool forming the weld metal, for example one or more filler metals as discussed above.
  • the present example concerns the welded joint 130 over a connection interface 132 between the end section 1 11 of at least the metallic core of the vanadium-based membrane 1 10 and the connector formation 122.
  • This welded joint 130 may be formed using a variety of suitable welding techniques, for example fusion welding techniques, such as laser welding, electron beam welding, or arc welding or similar to create a weld to join and seal at least the metallic core of a hydrogen separation membrane 1 10 to a connector 120, for example a vanadium membrane to stainless steel fitting or fittings.
  • An advantageous weld may be formed between a metallic core of a metallic hydrogen separation membrane, and/or that membrane itself (e.g., with all layers attached) to a metallic connector that is substantially free of cracks, inclusions, voids, when the weld metal of the sealing portion of the welded joint 130 comprises less than 40% by mass of metal from the metallic hydrogen separation membrane.
  • the welded joint 130 may therefore be produced in a welding technique that controls the mass contribution of the metal from the at least the metallic core of the metallic hydrogen separation membrane within the weld metal composition to the desired compositional levels.
  • the integrity of a weld may be influenced by the final composition of the weld metal, particularly the final composition of the sealing portion of the weld.
  • the metal from the metallic hydrogen separation membrane may comprise a metal or metal alloy which has a composition that may have deleterious effects on the composition of the weld metal if it comprises the substantive part of the weld metal.
  • the vanadium content of a vanadium based metallic hydrogen separations may produce a weld metal with undesirable defect forming properties when alloyed with stainless steel from the metal of a stainless steel based connector.
  • V metal content e.g., vanadium content
  • 40% by mass of metal may be considered to refer to the average composition across the entire mass of weld metal of the sealing portion of the welded joint.
  • the properties of the weld metal may improve with even less mass contribution of the metal from the metallic core within the weld metal composition.
  • the weld metal of the sealing portion comprises less than 35% by mass of metal from the metallic core.
  • the weld metal of the sealing portion comprises less than 30% by mass of metal from the metallic core.
  • the weld metal of the sealing portion comprises less than 25% by mass of metal from the metallic core.
  • the weld metal of the sealing portion may comprises one of: less than 38%, less than 34%, less than 33%, less than 31 %, less than 28%, less than 23%, or less than 20% by mass of metal from the metallic core.
  • welded joint 130 may also be produced with a substantially homogenous composition across the volume of a sealing portion of the weld metal of the welded joint 130.
  • the sealing portion of the weld may be considered to be a portion of the weld metal that extends between and forms a continuous seal between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane.
  • the sealing portion may comprise the main portion of the weld metal of the welded joint 130.
  • the sealing portion 131 (as shown in the lighter broken lines in Figure 3) of that weld occupies more than least 80% of the weld metal.
  • This heel section 1 17A comprises an isolated section of that weld body at the bottom of the connection section which may have a different composition due to that section being isolated from the full welding method/treatment to which the majority of the main body of the weld metal is subjected.
  • the weld may include a heel, finger or other extended body which is isolated from the full welding method/treatment to which the majority of the main body of the weld metal is subjected.
  • the welded joint may comprise a weld body, which may itself comprise the sealing portion (e.g., providing sealing effect across the entirety of the joint from membrane to connector, and having less than 40% by mass of metal from the metallic core of the metallic hydrogen separation membrane).
  • the sealing portion may form a substantial portion of the weld body.
  • the weld body may, however, comprise other portions within that weld body (e.g., non-sealing portions), which may or may not affect sealing, and which in some cases may have different composition.
  • a “continuous seal” means that the sealing portion of the weld between the metallic hydrogen separation membrane and the metallic connector connects these two components together with a welded joint that does not allow substantially any gas (including any hydrogen content therein) to pass through the welded joint and the connection between the metallic hydrogen separation membrane and the metallic connector formed by the welded joint.
  • a welded joint that does not allow substantially any gas (including any hydrogen content therein) to pass through the welded joint typically refers to a welded joint that holds pressure when the membrane is internally pressurised to 10 bara N2.
  • the weld may be tested to determine if the welded joint holds 10 bara N2 for at least 12 hr, preferably for at least 24 hr at room temperature. It should be appreciated that room temperature means at temperature of from 15 to 25 e C. If applicable, leaks can be detected using a snoop leak detection test (see the description below for one example of this test using Swagelok Snoop Liquid Leak Detector).
  • the fusion weld may provide a continuous leak free seal between the metallic connector and at least the metallic core of the metallic hydrogen separation membrane.
  • “leak free seal” should be understood to comprise a welded joint that does not allow substantially any gases to pass through the welded joint.
  • a leak free weld or a leak free welded joint is a weld that holds 10 bara N2 for at least 12 hr at room temperature.
  • the leak proof properties of welded joint largely depend on the weld comprising the welded joint being continuous between the components about the connection interface and also being substantially defect free - i.e. free of cracks, inclusions, voids, through which gases, including the hydrogen content in those gases, may leak.
  • compositional variation may exist in the weld metal, ideally, there are no isolated pockets in the weld metal of the sealing portion 131 that have a composition that exceeds 40% by mass of metal from the metallic hydrogen separation membrane, or the desired mass% limit as defined there-above. It should be noted that that the weld may include small sections which may not have this substantially homogenous composition. In this sense, the sealing portion 131 of the weld metal (for example the light broken line section in Figure 7) may have a substantially homogenous composition across the volume of the weld metal therein. In many examples, the substantially homogenous composition of the sealing section will be within a main body 217 section of that sealing portion 131 .
  • the main body 217 of the weld metal of the sealing portion 131 may be the volume or mass of metal spaced away from the perimeter or edges of the welded joint i.e. an interior portion of the volume of weld metal of the welded joint.
  • the perimeter region and/or edge region of the weld metal typically includes a composition which transitions from the composition of the main body of the weld metal to the adjoining metal composition, and thus may not conform with the substantially homogenous of the main body of the weld metal.
  • the weld may also include an isolated section or portion, for example heel section 117A in Figure 3, which may have a different composition due to that section being isolated from the full welding method/ treatment to which the majority of the main body 1 17 of the weld metal is subjected.
  • This heel section 1 17A or any other similar isolated section does not form part of the main body 131 of the weld metal/ weld, nor forms part of the sealing portion 131 of the weld (e.g. any heel portion, or the like, does not affect the sealing function of the weld).
  • a number of welding techniques and procedures may be used to produce this weld metal composition.
  • One welding procedure that may be used to form the welded joint of the arrangement 100 illustrated in Figures 1 to 10, comprises the following methodology.
  • a suitable vanadium-based membrane tube 1 10 is cut to a suitable length.
  • the illustrated tube 110 may include an internal palladium coating, but no external coating.
  • the method would equally apply to vanadium-based membrane tube 1 10 without any internal palladium coating or with a vanadium-based membrane tube 1 10 that included coating layers on the inner and outer sides thereof.
  • One or both ends of the vanadium-based membrane tube 1 10 may be squared off to form an end face 1 1 1 A that may be suitable for use in the end section 1 11 of the vanadium-based membrane 1 10 that overlaps an adjoining face of the connector formation 122 of connector 120.
  • this may be achieved by clamping the vanadium-based membrane tube 1 10 in a jig 300 which holds the tube perpendicular to a work surface 302 of a planar grinding disc 304 (or other equivalent grinding arrangement).
  • This jig 300 may then be held on a planar grinding disc 304 and the end face 11 1 A ground until that end face 11 1 A of the tube 1 10 is square ( Figures 1 A, 2 and 4).
  • a square edge advantageously provides a profile that is easy to consistently machine, improving reproducibility and repeatability.
  • an optional abrasion step may be conducted where end sections 1 1 1 1 , including the end face 1 1 1 A of the tube 110 are abrased by sanding to remove any oxide at the surface of the end regions, exposing the vanadium for forming the weld.
  • the end section 1 11 of a vanadium-based membrane tube 1 10 may then be mounted over and on the ramped surface of connector formation 122 of the connector 120 (as shown in Figure 1 ) with the vanadium-based membrane tube 110 and the connector formation 122 contacting at a connection interface 132.
  • the taper on the connector formation 122 ( Figures 1 and 1 A) may be advantageously designed to allow for variations in both the diameter and thickness of the vanadium-based membrane tube 1 10.
  • a taper angle 6 of 15 to 60°, for example from 15 to 45°, or 15° to 30in the connector formation 122 may be used to assist in the formation of a weld pool between the vanadium-based membrane tube 1 10 and the connector formation 122.
  • the formation of a weld pool in this location may be useful in allowing further metal material from the connector 120, for example stainless steel, to be melted into the weld pool, and thus assist in minimising V- concentration in the weld pool (to therefore minimise associated risk of cracking).
  • 6 is around 30° ( Figure 1 A). However, it should be appreciated that other angles could be used as discussed above.
  • connection interface 132 may then be welded, for example laser welded, to join the vanadium-based membrane tube 1 10 to the connector 120.
  • an autogenous fusion welding procedure may be used to form an autogenous weld at the welded joint 130 where the weld pool melt material is formed from material in the connection joint area, for example vanadium and stainless steel for the exemplified the vanadium-based membrane tube 1 10 and the stainless steel connector 120.
  • This type of weld can have a number of useful advantages, for example enabling automation of the welding process.
  • the exclusion of a filler wire and the resulting underfilled weld profile may facilitate the design and use of a mechanical restriction (collar) over the welded joint, as described above and covered in the Applicant’s copending international patent application entitled “Arrangement for Joining and Sealing a Metallic Hydrogen Separation Membrane to a Metallic Connector” which claims priority from Australian provisional patent application No. 2022901905, the contents of which should be understood to be incorporated into this specification by this reference.
  • other welding techniques could equally be used.
  • a filler material could be used where desired or required.
  • FIG. 3 A cross-section of a finished welded joint 130 is illustrated in Figure 3.
  • the dashed line 310 indicates the original shape of the vanadium- based membrane 1 10 before welding and the dashed line 312 indicates the original shape of the connector section 122 of the stainless steel connector 120. Since the surface of the welded joint 130 is either flush or just below the surface of the vanadium-based membrane 110 and stainless steel connector 120, a close fitting constriction collar 140 may slide over the welded joint 130.
  • the particular configuration described may permit the profile of the weld pool to be positioned within the outer diameter of the joint/membrane/connector (e.g., relatively recessed within the outer diameter). This may permit ease of fitting any construction collar 140, or the like, without affecting unduly or damaging the joint, in use.
  • the welded joint 130 may be formed using any number of welding passes.
  • the welded joint 130 may be formed in a single weld pass.
  • a single weld may be used to fuse the tubular vanadium-based membrane 1 10 to the connector formation 122 of a stainless steel connector/ fitting 120 and to form a weld pool composition 130B having acceptable V-levels in the weld metal that minimise risk of cracking.
  • This may utilise a laser focal point 155 (see for example Figure 5(A)) that is positioned away from the connection interface 132 and further within the bulk of the stainless steel composition of the connector formation 122. This positioning may be used to ensure that the melt pool from the laser beam substantially includes stainless steel from the connector 120.
  • the welded joint may be formed in two welding passes - for example following the procedure described in more detail below. In yet other embodiments, three or more welding passes may be used to achieve the desired continuous weld and weld composition.
  • a two-pass welding technique is welded joint illustrated in Figures 4 to 7. This technique includes:
  • a first pass weld ( Figures 4 and 6) which may be performed to fill the space at the connection interface 132 between the connector formation 122 to the end 1 1 1 A of the vanadium-based membrane 110 with a first pass weld composition.
  • the first pass weld may also be used to fuse (e.g., positionally affix) the tubular vanadium-based membrane 1 10 to the connector formation 122 of a stainless steel connector/ fitting 120.
  • a taper may be provided on the connector formation which will assist in the formation of a weld pool between the connector formation 122 to the end 1 1 1 A of the vanadium-based membrane 1 10.
  • this first pass welded joint 130A may be prone to defects and associated cracking of the weld due to the small weld volume and high vanadium content.
  • the first pass weld may therefore be followed by:
  • a second pass weld ( Figures 5 and 7) which may be used to dilute the first pass weld composition of the weld pool 130B with more stainless steel and to create a substantially homogenous weld metal composition in the sealing portion 131 of the weld metal 130 that forms a continuous seal between the vanadium- based membrane 1 10 to the connector formation 122. This dilution aims to reduce the amount of V in the weld metal to acceptable compositional levels that minimise risk of cracking.
  • a second pass weld may also be used to remelt the weld pool, and thus help to distribute the metals more evenly throughout the weld pool, creating a more homogenous composition through the sealing portion of the weld metal.
  • a variety of parameters may be varied to achieve the desired composition of the weld metal.
  • the focal point and/or the configuration of the laser beam may be varied between the first pass weld and the second pass weld to assist in creating this continuous seal between the vanadium-based membrane 1 10 to the connector formation 122 and also reduce V-levels in the weld metal to acceptable compositional levels that minimise risk of cracking. This may be practically achieved by targeting the weld pool more on the connector material, i.e. further on the connector side of the connection interface during the second pass weld.
  • One example of the parameters that may be changed between the first pass weld and second pass weld are illustrated in Figures 4 and 5:
  • the first pass weld may have a focal point 150 ( Figure 4(A)) located on stainless steel of connector interface 132, and has a tight/narrow laser beam width BD1 which is tighter/narrower than the second pass to produce a focused and deep penetrating laser beam into that focal point 200.
  • a small/ narrower laser spot size may be used to heat the part just enough to create a melt. The heat conducts from the centre of the pool outward, so the pool is hotter in the centre and cooler on its edges.
  • the laser may be applied in a number of power forms.
  • the laser may be applied as a pulse 158, having an initial peak, that decreases on a curve to reduce the applied laser power as the first pass weld progresses.
  • the welded joint 130A created by this single weld pass may be used to fix the two components together, for example as shown in the formed weld is illustrated in Figure 6(A).
  • the second pass weld may be configured with a laser focal point 155 ( Figure 5(A)) that is positioned further away from the connection interface 132 and further within the bulk of the stainless steel composition of the connector formation 122.
  • the method may comprise affixing the membrane/connector, and then - as a second pass - controllably relocating a laser in a direction such that more connector material is heated and flows to the weld.
  • that controllable movement is performed axially in the X direction shown in 4.
  • the ease of controllable translation of the laser may help facilitate accurate and controllably composition of the weld pool.
  • the focal point 155 moves in the X direction (see Figures 4(A) and 5(A)) toward the fitting 120, preferably at a distance 1 /2 of the increase in beam diameter/ width so that the location of edge of the beam 150A on the vanadium tube side 1 10 remains the same for both the first and second passes.
  • This positioning may be used to ensure that the melt pool from the laser beam substantially includes stainless steel from the connector 120.
  • the second weld pass may also be configured with a broader beam width (broader spot size) for the laser compared to the first pass.
  • a broader beam width may be used to better control melting I dilution from stainless steel, e.g., and reduce the V-content to desired composition amounts (e.g., below 40% wt.)) Further, the composition may be evenly distributed throughout the weld pool, or at least the sealing portion thereof, which may help minimising the risk of cracking.
  • the laser may be applied in a number of suitable power forms. One example is shown in Figure 5(B), where the laser may be applied as a pulse 158A, that has a constant laser power. A cross-section of the resulting welded joint is illustrated in Figure 7(B).
  • repositioning of the focal point and wider beam size in the second pass weld may advantageously be used to assist in homogenising the metal composition in the pool, thereby reducing the V content compared to the first pass and assists with defect reduction.
  • the composition of weld metal of the welded joint becomes substantially much more homogenous throughout the volume of weld metal.
  • a small laser beam size produces a higher energy concentration on the area the beam impinges compared to broader beam.
  • a laser beam is round in cross section.
  • Figures 6 and 7 shows the difference in compositional profiles (vanadium, (V) vs. iron (Fe)) from energy dispersive spectroscopy (EDS) line scans across the weld pool following another example of a two pass welding method according to an embodiment of the present invention.
  • the first and second weld passes follow a similar welding procedure as described in Example 1 .
  • the data was not filtered or scaled to the assumption of a pure vanadium tube composition, and hence the mass percentage of the vanadium has not been scaled to 100%, but is rather scaled to 80%. This is to be compared to the data of Figures 10 to 13, where the assumption has been made that the vanadium tube is pure and has been used to scale/reference the vanadium concentration to 100%.
  • Figure 6 provides (a) an EDS line scan analyses (showing elemental composition, by mass %) of the weld after first pass ONLY (line 210 in Figure 6(b) depicts the EDS line scan path). This shows a non-homogeneous composition within the weld metal, with a vanadium content through the weld ranging from 62.5% by mass to 27% by mass. With only a first weld pass, the composition of the weld metal of the sealing portion 130A may have areas of high vanadium content that may produce regions in the weld pool where cracks are present (see for example the cracks shown in Figure 6(b)).
  • vanadium content As described above, it is generally preferable to have a vanadium content of less than 40% by weight/mass, and more preferably less than 35% by weight/mass. For stainless steel and Inconel, it is generally preferable to have a vanadium content of less than 35% by weight/mass to avoid cracking.
  • the corresponding SEM images of weld cross sections in Figure 6(b) shows that this variation in vanadium content leads to regions in the weld metal where the vanadium content is too high leading to cracks (for example cracks 220).
  • Figure 7 provides (a) an EDS line scan analyses (showing elemental composition, by mass % with line 215 in Figure (b) depicting the EDS line scan path of the weld pool showing that the vanadium content in the sealing portion of the weld metal is substantially reduced to below 20% by mass, and is substantially constant across the weld metal.
  • the composition of iron and vanadium is substantially homogeneous in the sealing portion of the weld metal.
  • the main body 217 of the weld metal shown by broken lines in Figure 7(A) - i.e. the volume or mass of metal spaced away from the perimeter or edges of the welded joint
  • this weld may also include an isolated portion - heel section 217A in Figure 3, which may have a different composition due to that section being isolated from the full welding method/ treatment to which the majority of the main body 217 of the sealing portion 131 of the weld metal 130 is subjected.
  • This heel section 217A does not form part of the sealing portion 131.
  • the heel section 217A was in a position that was not properly subjected to the second pass weld, thereby affecting the final composition of the metal in that section. Nevertheless, the corresponding SEM images of weld cross sections show that no cracks are evident in the weld metal of the sealing portion 131 .
  • FIG. 8 shows the laser welder 200 used to produce the welded joints illustrated in Figures 3, 6 and 7, being an Alpha ALW 200 closed laser welding device that (manufactured by Alphalaser, Germany) which includes a Class 4 laser (a pulsed Nd:YAG laser).
  • the laser welder 200 includes a modified guarding surrounding the laser to accommodate 1.1 m long membranes. Whilst not illustrated, a custom radiation shield with a port hole was designed to replace one of the laser welder doors.
  • the custom shield incorporates the existing laser welder safety interlocks which prevents the laser from operating if the shield door is open.
  • the laser welder 200 may be used to form an autogenous weld following an automated welding procedure that uses computer control of the welding process.
  • a jig assembly 250 that may be used for holding the tubular vanadium-based membrane 1 10 and the connector 120 for automated laser welding operations in the laser welder 200 ( Figure 8) is illustrated in Figure 9. However, it should be appreciated that other arrangements could equally be used.
  • the illustrated jig assembly 250 comprises a tailstock 280 mounted on linear rails 282 configured to hold the connector 120 concentric with the tubular vanadium-based membrane 1 10 mounted in a rotating chuck 270.
  • the chuck 270 may include jaws 272 formed from copper that grip the membrane 1 10 and which act as heat sinks.
  • the position of the tailstock 280 may be controlled via a computer that also controls and drives the laser welder using a suitable software interface, for example a computer running a custom LabVIEW program interface.
  • the tailstock 280 may be displaced along the rails 282 by a motor 284 which drives a threaded rod 286 connected to the tailstock 280.
  • the jig assembly 250 may be mounted on a moveable bed 290 of the laser welder 200.
  • the laser welder 200 may also include a shielding gas nozzle 260 for conveying shielding gas to the weld area during welding.
  • the connector 120 may be threaded into the tailstock 280, with the connector interface 122 extending outwardly prior to moving into the welding position to mating with the tubular vanadium-based membrane 1 10 ready for welding.
  • laser welding of the connection interface 132 may then take place.
  • the laser welder 200 may be operated to run the desired welding process, for example the single-pass or the two-pass welding process described above as an automated process. This automation may assist in ensuring consistency and repeatability of welds, minimising variation from human/ operator factors.
  • a connector is preferably welded to each end of the membrane.
  • a quality assurance I control QA/QC
  • Leak tests of individual membranes also known as the ‘snoop’ test - may be completed on some or in some case all of the produced and sampled membranes. This may be completed at any time, but it may be advantageous to conduct a snoop test close to or in some instances, immediately after the welding process.
  • membranes that have completed the laser welding process are given a temporary O-rings (not illustrated) and internally pressurised to 10 bara N2; the welded seals and membranes are then individually testing using Swagelok Snoop Liquid Leak Detector, where leaks in seals and vanadium tube are able to be detected through visible bubbling at the defect site.
  • Swagelok Snoop Liquid Leak Detector where leaks in seals and vanadium tube are able to be detected through visible bubbling at the defect site.
  • a variety of snoop testing arrangements/ apparatus can be completed. In some forms, the snoop testing apparatus (not illustrated) allow the membrane to rotate freely while pressurised so that the weld quality can be inspected.
  • tubular membrane using the above described welded joint may be incorporated into a tubular catalytic membrane reactor (CMR), for example as taught in United States Patent No. 10,590,516 again the contents of which should be understood to be incorporated into this specification by this reference.
  • CMR tubular catalytic membrane reactor
  • a CMR incorporating tubular membranes may be used to selectively extract hydrogen from hydrogen containing gases such as syngas to produce a raffinate (bydepleted syngas) and H2 permeate.
  • Example 1 Laser welding 3/8” vanadium tube to stainless steel fitting
  • a 3/8” vanadium tube was welded to a stainless steel fitting following the two weld pass technique as described above, using the laser welding system and jig illustrated and described in relation to Figures 8 to 9 comprising a laser welder 200 (Alpha ALW 200 closed laser welding device with a pulsed Nd:YAG laser).
  • Vanadium tube Outer Diameter (OD) 9.52mm (3/8”), Wall Thickness (WT) 0.25 -0.28mm; Edge ground square and surface abraded to remove oxide.
  • Laser parameters 210 V, 3ms pulse time, 35 Hz, 0.6 mm beam diameter
  • Laser parameters 210V, 3.4ms pulse time, 35Hz, 0.8mm beam diameter
  • the composition of the weld metal of the welded joint 330A following the first pass weld has areas of high vanadium content that can produce regions in the weld pool where cracks are present (see for example the cracks shown in Figure 10(B & C)).
  • the second pass weld ( Figure 11 ) has an EDS scan ( Figure 1 1 (A)) that shows that the vanadium content in the weld metal is substantially reduced to below 20% by mass, and is substantially constant across the weld metal.
  • the composition of iron and vanadium is substantially homogeneous in the weld metal, and in particular within the main body 417 of the sealing portion 331 ( Figure 1 1 ) of the weld metal 330.
  • the composition of iron and vanadium may be substantially homogeneous in the weld metal 330.
  • the main body 417 of the sealing portion 331 of weld metal 330 (the volume or mass of metal spaced away from the perimeter or edges of the welded joint as illustrated in the broken lines of Figure 1 1 ) has a substantially homogenous composition throughout its volume.
  • the corresponding SEM images ( Figure 1 1 (C)) show that no cracks are evident in the weld metal 330 of the sealing portion 331 .
  • Figure 1 1 A provides a SEM backscatter electron image (AsB) showing the grain structure of the welded joint between a vanadium membrane tube and a stainless steel connector following a second pass weld which has been formed using a similar procedure to the welded joint shown in Figure 1 1.
  • Figure 1 1 A confirms that this welding technique produced a substantial homogeneous composition, particularly in the main body 417 of the sealing portion 331 ( Figure 1 1 ) of the weld metal 330.
  • a backscattered electron image reveals the compositional difference in a specimen (difference in the average atomic number).
  • vanadium 310 is shown as a black shade
  • the stainless steel 320 is lighter in shade than the vanadium 310
  • the weld pool/ metal 330 has a grey shade that is in between vanadium and stainless steel.
  • the substantially uniform shade of grey in weld metal 330 suggests I supports claim of roughly homogeneous elemental composition throughout the cross-section of the weld metal, particularly within the main body of the weld metal 330.
  • a 3/8” vanadium tube was welded to an Inconel 600 fitting following the two weld pass technique described above, using the laser welding system and jig illustrated and described in relation to Figures 8 to 9 comprising a laser welder 200 (Alpha ALW 200 closed laser welding device with a pulsed Nd:YAG laser).
  • Vanadium tube Outer Diameter (OD) 9.52mm (3/8”), Wall Thickness (WT) 0.25 -0.28mm; Edge ground square and surface abraded to remove oxide.
  • INCONEL® (nickel-chromium-iron) alloy 600 (UNS N06600/W.Nr. 2.4816).
  • the vanadium tube was forced against the Inconel 600 fitting to form a single V joint preparation as shown in Figure 4(A).
  • Laser parameters 210 V, 3ms pulse time, 35 Hz, 0.6 mm beam diameter
  • Pulse shape as shown in Figure 4(B) Power: 51 .1 W
  • Laser parameters 210V, 3.4ms pulse time, 35Hz, 0.8mm beam diameter
  • the composition of the weld metal of the welded joint 530A following a first pass weld has large areas of high vanadium content that can produce regions in the weld pool where significant cracks are present (see for example the cracks shown in Figure 12(B & C)).
  • the second pass weld has an EDS scan (Figure 13(A)) that shows that the vanadium content in the weld metal 530, in particular the main body 617 of the sealing portion 531 ( Figure 13) of the weld metal 530 is substantially reduced to below 35% by mass, and is substantially constant across the weld metal.
  • the composition of nickel and vanadium is substantially homogeneous in the weld metal.
  • the composition of nickel and vanadium may be substantially homogeneous in the weld metal.
  • the main body 617 of the sealing portion 531 of weld metal 330 (the volume or mass of metal spaced away from the perimeter or edges of the welded joint as shown by the broken lines in Figure 13) has a substantially homogenous composition throughout its volume.
  • the corresponding SEM images ( Figure 13(C)) show that no significant cracks are evident in the weld metal of the welded joint 530.
  • Figure 13A provides a SEM backscatter image (AsB) showing the grain structure of the welded joint between a vanadium membrane tube and an Inconel 600 connector following a second pass weld which has been formed using a similar procedure to the welded joint shown in Figure 13.
  • Figure 13A confirms that this welding technique produced a substantial homogeneous composition, and in particular within the main body 617 of the sealing portion 531 ( Figure 13) of the weld metal 530.
  • a backscattered electron image reveals the compositional difference in a specimen (difference in the average atomic number).
  • vanadium 510 is shown as a black shade
  • the nickel (of Inconel 520) is lighter in shade than the vanadium 510
  • the weld pool/ metal 530 has a grey shade that is in between vanadium and nickel.
  • the substantially uniform shade of grey in weld metal 530 suggests I supports claim of roughly homogeneous elemental composition throughout the cross-section of the weld metal, particularly within the main body of the weld metal 530.
  • substantially means that a state or parameter that may not be 100%, but may be close to or for the most part 100%. Substantially may therefore be understood to mean that the state or parameter is a great or significant extent that state or parameter. Substantially may also be understood to mean that the state or parameter is to a large degree that state or parameter. Substantially may also be understood to mean that the state or parameter is for the most part that state or parameter, and/or essentially that state or parameter. In other words, substantially means that the parameter is approximate the perfect state of that parameter or state but may not be the perfect form of that parameter or state.

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Abstract

La présente invention concerne un joint soudé entre un raccord métallique et au moins un noyau métallique d'une membrane de séparation d'hydrogène métallique comprenant une soudure par fusion formée à partir du raccord métallique et d'au moins le noyau métallique de la membrane de séparation d'hydrogène métallique et entre ceux-ci, le raccord pouvant être constitué d'un métal ou d'un alliage métallique différent du noyau métallique de la membrane de séparation d'hydrogène, et la soudure par fusion comprenant une partie d'étanchéité qui fournit un joint continu entre le raccord métallique et au moins le noyau métallique de la membrane de séparation d'hydrogène métallique et le métal soudé de la partie d'étanchéité comprend moins de 40 % en masse de métal à partir du noyau métallique de la membrane de séparation d'hydrogène métallique.
PCT/AU2024/050727 2023-07-04 2024-07-04 Joint soudé entre une membrane de séparation d'hydrogène métallique et un raccord métallique Pending WO2025007191A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN202480044538.4A CN121464017A (zh) 2023-07-04 2024-07-04 金属氢分离膜与金属连接器之间的焊接接头
AU2024291411A AU2024291411A1 (en) 2023-07-04 2024-07-04 Welded joint between a metallic hydrogen separation membrane and a metallic connector
KR1020267000417A KR20260034655A (ko) 2023-07-04 2024-07-04 금속 수소 분리 멤브레인과 금속 커넥터 사이의 용접 접합부

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AU2023902141A AU2023902141A0 (en) 2023-07-04 Welded joint between a metallic hydrogen separation membrane and a metallic connector
AU2023902141 2023-07-04

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4551319A4 (fr) * 2022-07-07 2025-10-15 Commw Scient Ind Res Org Agencement servant à joindre et sceller une membrane métallique de séparation d'hydrogène à un connecteur métallique

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005246433A (ja) * 2004-03-04 2005-09-15 Ishikawajima Harima Heavy Ind Co Ltd 非晶質金属シートの接合方法及び接合装置並びに水素透過ユニット
US20060060084A1 (en) * 2004-09-20 2006-03-23 Edlund David J Hydrogen purification devices, components, and fuel processing systems containing the same
AT12132U1 (de) * 2010-11-10 2011-11-15 Plansee Se Anordnung zur gasabtrennung
US9616527B2 (en) * 2006-07-12 2017-04-11 L'Air Liquide, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Process for laser-arc hybrid welding aluminized metal workpieces
WO2019000026A1 (fr) * 2017-06-30 2019-01-03 Commonwealth Scientific And Industrial Research Organisation Procédé d'assemblage et d'étanchéité d'une membrane à base de vanadium à une section de connexion métallique

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005246433A (ja) * 2004-03-04 2005-09-15 Ishikawajima Harima Heavy Ind Co Ltd 非晶質金属シートの接合方法及び接合装置並びに水素透過ユニット
US20060060084A1 (en) * 2004-09-20 2006-03-23 Edlund David J Hydrogen purification devices, components, and fuel processing systems containing the same
US9616527B2 (en) * 2006-07-12 2017-04-11 L'Air Liquide, Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude Process for laser-arc hybrid welding aluminized metal workpieces
AT12132U1 (de) * 2010-11-10 2011-11-15 Plansee Se Anordnung zur gasabtrennung
WO2019000026A1 (fr) * 2017-06-30 2019-01-03 Commonwealth Scientific And Industrial Research Organisation Procédé d'assemblage et d'étanchéité d'une membrane à base de vanadium à une section de connexion métallique

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4551319A4 (fr) * 2022-07-07 2025-10-15 Commw Scient Ind Res Org Agencement servant à joindre et sceller une membrane métallique de séparation d'hydrogène à un connecteur métallique

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