• Journal of the Korean institute of surface engineering
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• v.39 no.6
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• pp.255-262
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• 2006

Pd-Cu alloy membrane for hydrogen separation was fabricated by sputtering and Cu reflow process. At first, the Pd and Cu was continuously deposited by sputtering method on oxidized Si support, the Cu reflow process was followed. Microstructure of the surface and permeability of the membrane was investigated depending on various reflow temperature, time, Pd/cu composition and supports. With respect to our result, Pd-Cu thin film (90 wt.% Pd/10 wt.% Cu) deposited by sputtering process with thickness of $2{\mu}m$ was heat-treated for Cu reflow The voids of the membrane surface were completely filled and the dense crystal surface was formed by Cu reflow behavior at $700^{\circ}C$ for 1 hour. Cu reflow process, which is adopted for our work, could be applied to fabrication of dense Pd-alloy membrane for hydrogen separation regardless of supports. Ceramic or metal support could be easily used for the membrane fabricated by reflow process. The Cu reflow process must result in void-free surface and dense crystalline of Pd-alloy membrane, which is responsible for improved selectivity oi the membrane.

• Membrane Journal
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• v.21 no.4
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• pp.345-350
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• 2011

No investigation has yet been accomplished to screen the boron-doped effects on vanadium based metal membranes. The synthesis, hydrogen permeation properties and chemical stability of a novel Pd-coated $V_{99.8}B_{0.2}$ alloy membrane are presented in this report. Hydrogen permeation experiments have been performed to investigate the hydrogen transport properties through the Pd-coated $V_{99.8}B_{0.2}$ alloy membrane in the absolute pressure range 1.0~3.0 bar under pure hydrogen, hydrogen-carbon dioxide gas mixture at $400^{\circ}C$. The maximum hydrogen permeation flux was $48.5mL/min/cm^2$ for a 0.5 mm thick membrane under pure hydrogen. This results offer new direction in the synthesis of novel non-Palladium-based metal membranes for hydrogen separation in water-gas shift reaction.

• Journal of the Korea Institute of Military Science and Technology
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• v.20 no.4
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• pp.528-535
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• 2017

Fuel cells have been spotlighted in the world for being highly efficient and environmentally friendly. A hydrogen which is the fuel of fuel cell can be obtained from a number of sources. Hydrogen source for operating the polymer electrolyte membrane fuel cell(PEMFC) in the current underwater environment, such as a submarine and unmanned underwater vehicles are currently from the metal hydride cylinder. However, metal hydride has many limitations for using hydrogen carrier, such as large volume, long charging time, limited storage capacity. To solve these problems, we suggest diesel reformer for hydrogen supply source. Diesel fuel has many advantages, such as high hydrogen storage density, easy to transport and also well-infra structure. However, conventional diesel reforming system for PEMFC requires a large volume and complex CO removal system for lowering the CO level to less than 10 ppm. In addition, because the preferential oxidation(PROX) reaction is the strong exothermic reaction, cooling load is required. By changing this PROX reactor to hydrogen separation membrane, the problem from PROX reactor can be solved. This is because hydrogen separation membranes are small and permeable to pure hydrogen. In this study, we conducted the pressurized diesel reforming and water-gas shift reaction experiment for the hydrogen separation membrane application. Then, the hydrogen permeation experiments were performed using a Pd alloy membrane for the reformate gas.

• Journal of the Korean institute of surface engineering
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• v.48 no.1
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• pp.11-22
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• 2015

Pd alloy hydrogen membranes for hydrogen purification and separation need thermal stability at high temperature for commercial applications. Intermetallic diffusion between the Pd alloy film and the porous metal support gives rise to serious problems in long-term stability of Pd alloy membranes. Ceramic barriers are widely used to prevent the intermetallic diffusion from the porous metal support. However, these layers result in poor adhesion at the interface between film and barrier because of the fundamentally poor chemical affinity and a large thermal stress. In this study, we developed Pd alloy membranes having a dense microstructure and saturated composition on modified metal supports by advanced DC magnetron sputtering and heat treatment for enhanced thermal stability. Experimental results showed that Pd-Cu and Pd-Ag alloy membranes had considerably enhanced long-term stability owing to stable, dense alloy film microstructure and saturated composition, effective diffusion barrier, and good adhesive interface layer.

• Journal of the Korean institute of surface engineering
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• v.51 no.5
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• pp.277-290
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• 2018

In this study, Pd-Ni-Ag alloy hydrogen separation membranes were fabricated by Pd/Ag/Pd/Ni/Pd multi-layer sputter deposition on the modified MIM(Metal Injection Molding)-PSS(Porous Stainless Steel) support and followed heat treatment. Nickel, used as an alloying element in Pd alloy membranes, is inexpensive and stable material in a hydrogen isotope environment at high temperature up to 1123 K. Hydrogen perm-selectivity of Pd-Ni-Ag alloy membranes is affected not only by composition of membrane films but also by other factors such as surface properties of PSS support, microstructure of membrane films and inter-diffused impurities from PSS support. In order to clarify the effect of surface Ni composition on hydrogen perm-selectivity of Pd-Ni-Ag alloy membranes, the other effects were significantly minimized by the formation of dense and homogeneous Pd-Ni-Ag alloy membranes. Hydrogen permeation test showed that hydrogen permeability decreased from $7.6{\times}10^{-09}$ to $1.02{\times}10^{-09}mol/m{\cdot}s{\cdot}Pa^{0.5}$ as Ni composition increased from 0 to 16 wt% and the selectivity for $H_2/N_2$ was infinite.

• Proceedings of the Materials Research Society of Korea Conference
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• 2008.05a
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• pp.11.1-11.1
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• 2008

• Journal of the Korean institute of surface engineering
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• v.49 no.3
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• pp.286-300
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• 2016

Pd-Ag alloy membranes have attracted a great deal of attention for their use in hydrogen purification and separation due to their high theoretical permeability, infinite selectivity and chemical compatibility with hydro-carbon containing gas streams. For commercial application, Pd-based membranes for hydrogen purification and separation need not only a high perm-selectivity but also a stable long-term durability. However, it has been difficult to fabricate thin, dense Pd-Ag alloy membranes on a porous stainless steel metal support with surface pores free and a stable diffusion barrier for preventing metallic diffusion from the porous stainless steel support. In this study, thin Pd-Ag alloy membranes were prepared by advanced Pd/Ag/Pd/Ag/Pd multi-layer sputter deposition on the modified porous stainless steel support using rough polishing/$ZrO_2$ powder filling and micro-polishing surface treatment, and following Ag up-filling heat treatment. Because the modified Pd-Ag alloy membranes using rough polishing/$ZrO_2$ powder filling method demonstrate high hydrogen permeability as well as diffusion barrier efficiency, it leads to the performance improvement in hydrogen perm-selectivity. Our membranes, therefore, are expected to be applicable to industrial fields for hydrogen purification and separation owing to enhanced functionality, durability and metal support/Pd alloy film integration.

• Membrane Journal
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• v.22 no.1
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• pp.1-7
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• 2012

We make a studyof the hydrogen permeability and chemical stability of $Nb_{56}Ti_{23}Ni_{21}$ metal alloy membrane. For this purpose, we produced the $Nb_{56}Ti_{23}Ni_{21}$ membrane which has 10 mm diameter and 0.5 mm thick, and experiment the hydrogen transport properties under two kinds of feed gas ($H_2$ 100%; $H_2$ 60% + $CO_2$ 40%) at $450^{\circ}C$C with variation of absolute pressure.The maximum hydrogen permeation flux was $5.58mL/min/cm^2$ in the absolute pressure 3 bar under pure hydrogen. And each case of feed gases about gas composition, the permeation fluxes were satisfied with Sievert's law, and the hydrogen permeation flux decreased with decrease of hydrogen partial pressure irrespective of temperature and pressure. After permeation test, we experiment the stability and durability of $Nb_{56}Ti_{23}Ni_{21}$ alloy membrane for carbon dioxide by XRD analysis.

• Transactions of the Korean hydrogen and new energy society
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• v.19 no.4
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• pp.359-366
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• 2008

Hydrogen as a high-quality and clean energy carrier has attracted renewed and ever-increasing attention around the world in recent years, mainly due to developments in fuel cells and environmental pressures including climate change issues. In this processes for hydrogen production from fossil fuels, separation and purification is a critical technology. $(Ni_{60}-Nb_{40})_{95}-Pd_5$ alloy ingots were prepared by arc-melting the mixture of pure metals in an Ar atmosphere. Melt-spun ribbons were produced by the single-roller melt-spinning technique in an Ar atmosphere. Amorphous structure and thermal behavior were characterized by XRD and DSC. The permeability of the $(Ni_{60}-Nb_{40})_{95}-Pd_5$ amorphous alloy membrane was characterized by hydrogen permeation experiments in the temperature range 623 to 773 K and pressure of 2 bars. The maximum hydrogen permeability was $3.54{\times}10^{-9}[mol{\cdot}m^{-1}s^{-1}{\cdot}pa^{-1/2}]$ at 773 K for the $(Ni_{60}-Nb_{40})_{95}-Pd_5$ amorphous alloy.

• Corrosion Science and Technology
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• v.6 no.3
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• pp.133-139
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• 2007

Nickel powder was coated with aluminum nitrate solution to increase the thermal stability of a porous nickel support and control the nickel content in the Pd-Cu-Ni ternary alloyed membrane. Raw nickel powder and alumina coated nickel powder were uniaxialy pressed by home made press with metal cylindrical mold. Though the used nickel powder prepared by pulsed wire evaporation (PWE) method has a good thermal stability, the porous nickel support was too much sintered and the pores of porous nickel support was plugged at high temperature (over $800^{\circ}C$) making it not suitable for the porous support of a palladium based composite membrane. In order to overcome this problem, the nickel powder was coated by alumina and alumina modified porous nickel support resists up to $1000^{\circ}C$ without pore destruction. Furthermore, the compositions of Pd-Cu-Ni ternary alloy membrane prepared by magnetron sputtering and Cu-reflow could be controlled by not only Cu-reflow temperature but also alumina coating amount. SEM analysis and mercury porosimeter analysis evidenced that the alumina coated on the surface of nickel powder interrupted nickel sintering.