• Applied Chemistry for Engineering
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• v.16 no.2
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• pp.282-287
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• 2005

Palladium membranes, which are permselective to hydrogen separation, were used for the hydrogen purification and in membrane reactors for improving conversions by shifting the reaction equilibrium. Palladium/ceramic composite membranes were prepared by electroless plating technique and then etched in titanium chloride ($TiCl_4$) as a post treatment to enhance the membrane's durability. These membranes were used for membrane reactors in water gas shift (WGS) reaction. CO conversions for the membrane reactor were obtained according to experimental parameters and compared to the traditional reactor without a palladium/ceramic membrane. As a result, CO conversion using palladium membrane reactor at an appropriate condition was over 20~25% greater than that without the membrane reactor. The stability in the long-term test of up to 120 h for WGS reaction with the membrane reactor was good without the degredation of CO conversion.

• Journal of the Korean institute of surface engineering
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• v.37 no.5
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• pp.243-248
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• 2004

A palladium-nikel(Pd-Ni) alloy composite membrane has been fabricated on microporous nickel support formed with nickel powder. Plasma surface treatment process is introduced as pre-treatment process instead of HCI activation. Pd coating layer was prepared by dc magnetron sputtering deposition after $H_2$ plasma surface treatment. Palladium-nickel alloy composite layer had a fairly uniform and dense surface morphology. The membrane was characterized by permeation experiments with hydrogen and nitrogen gases at temperature of 773 K and pressure of 2.2psi. The hydrogen permeance was 6 ml/minㆍ$\textrm{cm}^2$ㆍatm and the selectivity was 120 for hydrogen/nitrogen($H_2$/$N_2$) mixing gases at 773 K.

• Proceedings of the Membrane Society of Korea Conference
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• 2003.07a
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• pp.25-28
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• 2003

Low cost composite metallic membranes for the hydrogen separation and production have been prepared by using thin Pd-Ag foils reinforced by metallic (stainless steel and nickel) structures. Especially, “supported membranes” have been obtained by a diffusion welding procedure in which Pd-Ag thin foils have been joined with perforated metals (nickel) and expanded metals (stainless steel): in these membranes the thin palladium foil assures both the high hydrogen permeability and the perm-selectivity while the metallic support provides the mechanical strength. A second studied method of producing "laminated membranes" consists of coating non-noble metal sheets with very thin palladium layers by diffusion welding and cold-rolling. Palladium thin coatings over these metals reduce the activation energy of the hydrogen adsorption process and make them permeable to the hydrogen. In this case, the dense non-noble metal has been used as a support structure of the thin Pd-Ag layers coated over its surfaces: a proper thickness of the metal assures the mechanical strength, the absence of defects (cracks, micro-holes) and the complete hydrogen selectivity of the membrane. membrane.

• 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.

• Membrane Journal
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• v.21 no.2
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• pp.148-154
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• 2011

Metal-ceramic composite membrane have been developed to separate hydrogen from mixed gases, particularly product streams generated during coal gasification and methane reforming. Cermet membrane was fabricated with palladium as hydrogen-permeable metal and $Y_2O_3$-stabilized $ZrO_2$ (YSZ) as ceramic supporter. As-prepared membrane showed dense structure with continuous channel of palladium. The hydrogen flux of Pd/YSZ membrane have been measured in the range of 0.5~2 atm with 100% hydrogen gas. The results indicate that the hydrogen flux was 0.333 mL/$min{\cdot}cm^2$ at $450^{\circ}C$ and 2 atm. The crack was formed in the surface and cross-section of membrane.

• Journal of the Korean institute of surface engineering
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• v.37 no.5
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• pp.289-295
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• 2004

A dense palladium-nikel (Pd-Ni) alloy composite membrane has been fabricated on microporous nickel support mixed with submicron/micron nickel powder instead of mesoporous stainless steel support. Plasma treatment process is introduced as pre-treatment process instead of HCI activation. Pd-Ni alloy composite membrane prepared by electro plating was fairly a uniform and dense surface morphology. The membrane was characterized by permeation experiments with hydrogen and nitrogen gases at temperature 773 K and pressure 2.2 psi. The results showed that hydrogen ($H_2$) permeance was 27 ml/$\textrm{cm}^2$ㆍatmㆍmin and hydrogen/ nitrogen ($_H2$$N_2$) selectivity was 8 at 773 K.

• Applied Chemistry for Engineering
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• v.17 no.5
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• pp.458-464
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• 2006

The Pd-Ni-Ag alloy composite membrane using modified porous stainless steel (PSS) as a substrate was prepared by a electroless plating technique. In this work, we have introduced the intermediate layer between Pd-based alloy and a metal substrate. As an intermediate layer, the mixtures of nickel powder and inorganic sol such as $SiO_{2}$ sol, $Al_{2}O_{3}$ sol, and $TiO_{2}$ sol were used. The intermediate layers were coated onto a PSS substrate according to various membrane preparation conditions and then $N_{2}$ fluxes through the membranes with different intermediate layers were measured. The surface morphology of the intermediate layer in the mixture of nickel powder and inorganic sol was analyzed using scanning electron microscope (SEM). Finally, the Pd-Ni-Ag alloy composite membrane using the support coated with the mixture of nickel powder and silica as an intermediate layer was fabricated and then the gas permeances for $H_{2}$ and $N_{2}$ through the Pd-based membrane were investigated. The selectivity of $H_2/N_2$ was infinite and the $H_{2}$ flux was $1.39{\times}10^{-2}mol/m^2{\cdot}s$ at the temperature of $500^{\circ}C$ and trans-membrane pressure difference of 1 bar.

• Journal of Hydrogen and New Energy
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• v.27 no.3
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• pp.270-275
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• 2016

A simple solid state incorporation method was employed in order to incorporate Pd nanocatalyst into a Nafion film for polymer electrolyte membrane fuel cell (PEMFC) via the reduction of palladium (II) bis (acetylacetonate), $Pd(acac)_2$. It was sublimed, penetrated into Nafion film and then reduced to Pd nanoparticles simultaneously in a glass reactor of N2 atmosphere at $180^{\circ}C$ for 1, 3 and 5 min. This reaction was took place without any reducing agent and any solvent. The morphology of the Pd nanoparticles was observed by transmission electron microscopy (TEM), and Pd distribution was analyzed by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). And 23% modification of tensile strength of Pd/Nafion composite film was measured by universal testing machine and I-V curve was estimated by using a unit cell with $5{\times}5cm^2$ active area.

• Journal of the Korean institute of surface engineering
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• v.45 no.6
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• pp.248-256
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• 2012

A Pd-based hydrogen membranes for hydrogen purification and separation need high hydrogen perm-selectivity. The surface roughness of the support is important to coat the pinholes free and thin-film membrane over it. Also, The pinholes drastically decreased the hydrogen perm-selectivity of the Pd-based composite membrane. In order to remove the pinholes, we introduced various surface pre-treatment such as alumina powder packing, nickel electro-plating and micro-polishing pre-treatment. Especially, the micro-polishing pretreatment was very effective in roughness leveling off the surface of the porous nickel support, and it almost completely plugged the pores. Fine Ni particles filled surface pinholes with could form open structure at the interface of Pd alloy coating and Ni support by their diffusion to the membrane and resintering. In this study, a $4{\mu}m$ surface pore-free Pd-Cu-Ni ternary alloy membrane on a porous nickel substrate was successfully prepared by micro-polishing, high temperature sputtering and Cu-reflow process. And $H_2$ permeation and $N_2$ leak tests showed that the Pd-Cu-Ni ternary alloy hydrogen membrane achieved both high permeability of $13.2ml{\cdot}cm^{-2}{\cdot}min^{-1}{\cdot}atm^{-1}$ permation flux and infinite selectivity.

• Korean Chemical Engineering Research
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• v.44 no.2
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• pp.160-165
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• 2006

A Pd-Cu-Ni alloyed hydrogen membrane has fabricated on porous nickel support formed by nickel powder. Porous nickel support made by sintering shows a strong resistance to hydrogen embrittlement and thermal fatigue. Plasma surface modification treatment is introduced as pre-treatment process instead of conventional HCl wet activation. Nickel was electroplated to a thickness of $2{\mu}m$ in order in to fill micropores at the nickel support surface. Palladium and copper were deposited at thicknesses of $4{\mu}m$ and $0.5{\mu}m$, respectively, on the nickel coated support by DC sputtering process. Subsequently, copper reflow at $700^{\circ}C$ was performed for an hour in $H_2$ ambient. And, as a result PdCu-Ni composite membrane has a pinhole-free and extremely dense microstructure, having a good adhesion to the porous nickel support and infinite hydrogen selectivity in $H_2/N_2$ mixtures.