• Membrane Journal
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• v.32 no.2
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• pp.116-125
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• 2022

In this experiment, an α-Al₂O₃ ceramic hollow fiber was used as a support, and a hydrogen membrane plated with Pd and Pd-Ag was manufactured through electroless plating. The Pd-Ag membrane was annealed at 500℃ for 10 h to form an alloy of Pd and Ag. It was confirmed that it became a Pd-Ag alloy through EDS (Energy Dispersive X-ray Spectroscopy) analysis. Also, the thickness of the Pd, Pd-Ag plating layer was measured to be about 8.98 and 9.29 ㎛ through SEM (Scanning Electron Microscope) analysis respectively. Hydrogen permeation experiment was performed using the H₂ gas and mixed gas (H₂ and N₂) in the range of 350~450℃ and 1-4 bar using the prepared hydrogen membrane. Under the H₂ gas condition, the Pd and Pd-Ag membrane has a flux of up to 21.85 and 13.76 mL/cm²·min and also separation factors of 1216 and 361 were obtained in the mixed gas at 450℃ and 4 bar conditions respectively.

• Membrane Journal
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• v.34 no.1
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• pp.50-57
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• 2024

In this experiment, Pd-Ag-Cu membrane was manufactured using electroless plating on an α-Al₂O₃ support. Pd, Ag and Cu were each coated on the surface of the support through electroless plating and heat treatment was performed for 18 h at 500℃ in H₂ in the middle of electroless plating to form Pd alloy. The surface of the Pd-Ag-Cu membrane was observed through Scanning Electron Microscopy (SEM), and the thickness of the Pd membrane was measured to be 7.82 ㎛ and the thickness of the Pd-Ag-Cu membrane was measured to be 3.54 ㎛. Energy dispersive X-ray spectroscopy and X-ray diffraction analysis confirmed the formation of a Pd-Ag-Cu alloy with a composition of Pd-78wt%, Ag-8.81wt% and Cu-13.19wt%. The gas permeation experiment was conducted under the conditions of 350~450℃ and 1~4 bar in H₂ single gas and H₂/N₂ mixed gas. The maximum H₂ flux of the hydrogen separation membrane measured in H₂ single gas is 74.16 ml/cm²·min at 450℃ and 4 bar for the Pd membrane and 113.64 ml/cm²·min at 450℃ and 4 bar for the Pd-Ag-Cu membrane. In the case of the separation factor measured in H₂/N₂ mixed gas, separation factors of 2437 and 11032 were measured at 450℃ and 4 bar.

• Proceedings of the Membrane Society of Korea Conference
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• 1999.07a
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• pp.43-47
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• 1999

Pd-ceramic composite membranes and catalytic membrane reactors(CMR) have been studied for hydrogen purification and recovery in th fusion reactor fuel cycle. The development of techniques for coating microporous ceramic tubes with Pd and Pd/Ag layers is described: composite membranes have been produced by electroless deposition (Pd/Ag film of 10-20${\mu}{\textrm}{m}$) and rolling of thin metal sheet (Pd and Pd/ Ag membranes of 50-70 ${\mu}{\textrm}{m}$). Experimental results on electroless membranes showed that the metallic film presented some defects and the membranes had not complete hydrogen selectivity . Then the catalytic membrane reactors with electroless membranes can be applied for some industrial processes that do not require a complete separation of the hydrogen (i.e. in the dehydrogenation of hydrocarbons). The rolled thin Pd/Ag membranes separated the hydrogen from the other gas with a complete selectivity and exhibited a slightly larger (about a factor 1.7) mass transfer resistance with respect to the electroless membranes. Experimental tests confirmed the good performances in terms of durability.

• Applied Chemistry for Engineering
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• v.20 no.1
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• pp.104-108
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• 2009

In this study, for the flow of carbon dioxide/hydrogen mixture through a tubular type Pd-Ag membrane, hydrogen partial pressure, velocity profile, and concentration profile were simulated as a function of inlet flow rate using computational fluid dynamics (CFD) technique. The simulation results indicated that the mole fraction of carbon dioxide increased slowly in the longitudinal direction as the flow rate increased. In addition, the effects of inlet flow rate and the length of membrane on hydrogen recovery were investigated. At lower flow rate and for longer membrane, the hydrogen recovery was larger.

• Korean Membrane Journal
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• v.1 no.1
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• pp.1-7
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• 1999

Pd-ceramic composite membranes and catalytic membrane reactors(CMR) have been studied for hydrogen and its isotopes (deuterium and tritium) purification and recovery in the fusion reactor fuel cycle. Particularly a closed-loop process has been studied for recovering tritium from tritiated water by means of a CMR in which the water gas shift reaction takes place. The development of the techniques for coating micro-porous ceramic tubes with Pd and Pd/Ag thin layers is described : P composite membranes have been produced by electroless deposition (Pd/Ag film of 10-20 $\mu$m) and rolling of thin metal sheets (Pd and Pd/Ag membranes of 50-70 $\mu$m). Experimental results of the electroless membranes have shown a not complete hydrogen selectivity because of the presence of some defects(micro-holes) in the metallic thin layer. Conversely the rolled thin Pd and Pd/ag membranes have separated hydrogen from the other gases with a complete selectivity giving rise to a slightly larger (about a factor 1.7) mass transfer resistance with respect to the electroless membranes. Experimental tests have confirmed the good performances of the rolled membranes in terms of chemical stability over several weeks of operation. Therefore these rolled membranes and CMR are adequate for applications in the fusion reactor fuel cycle as well as in the industrial processes where high pure hydrogen is required (i.e. hydrocarbon reforming for fuel cell)

• 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 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.

• 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.

• Proceedings of the Membrane Society of Korea Conference
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• 2000.04a
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• pp.13-20
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• 2000

• Applied Chemistry for Engineering
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• v.16 no.5
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• pp.641-647
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• 2005

The partial oxidation of methane is one of important processes for hydrogen production. As a membrane reactor, palladium-silver (Pd-Ag) alloy membrane prepared by electroless plating technique was employed for partial oxidation of methane. The experimental variables were reaction temperature, $O_2/CH_4$ mole ratio, $CH_4$ feed rate, and $N_2$ sweep gas flow rate. The methane conversions increased with the reaction temperatures in the range of 350 to $730^{\circ}C$. The highest methane conversion and CO selectivity were obtained at the condition of $O_2/CH_4$ mole ratio of 0.5 and $730^{\circ}C$ using commercially available nickel/alumina catalyst. The Pd-Ag membrane reactor showed higher methane conversions, 10~40% higher, compared to those in a traditional reactor.