• 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.

• Journal of the Korean institute of surface engineering
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• v.50 no.2
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• pp.98-107
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• 2017

Pd-based membranes have been widely used in hydrogen purification and separation due to their high hydrogen diffusivity and infinite selectivity. However, it has been difficult to fabricate thin and dense Pd-based membranes on a porous stainless steel(PSS) support. In case of a conventional PSS support having the large size of surface pores, it was required to use complex surface treatment and thick Pd coating more than $6{\mu}m$ on the PSS was required in order to form pore free surface. In this study, we could fabricate thin and dense Pd membrane with only $3{\mu}m$ Pd layer on a new PSS support manufactured by metal injection molding(MIM). The PSS support had low surface roughness and mean pore size of $5{\mu}m$. Pd membrane were prepared by advanced Pd sputter deposition on the modified PSS support using fine polishing and YSZ vacuum filling surface treatment. At temperature $400^{\circ}C$ and transmembrane pressure difference of 1 bar, hydrogen flux and selectivity of $H_2/N_2$ were $11.22ml\;cm^{-2}min^{-1}$ and infinity, respectively. Comparing with $6{\mu}m$ Pd membrane, $3{\mu}m$ Pd membrane showed 2.5 times higher hydrogen flux which could be due to the decreased Pd layer thickness from $6{\mu}m$ to $3{\mu}m$ and an increased porosity. It was also found that pressure exponent was changed from 0.5 on $6{\mu}m$ Pd membrane to 0.8 on $3{\mu}m$ Pd membrane.

• Membrane Journal
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• v.34 no.2
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• pp.140-145
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• 2024

In modern times, when a change in the energy paradigm is required, hydrogen is an attractive energy source. Among these hydrogen purification technologies, technology using a membrane is attracted attention as a technology that can purify high purity hydrogen at low cost. However, palladium(Pd), which is mostly used because of its excellent hydrogen separation performance, is very expensive, so a replacement material is needed. In this study, a alloy membrane was manufactured from an alloy of niobium (Nb), which has high hydrogen permeability but is weak to hydrogen embrittlement, and nickel (Ni) and zirconium (Zr), which have low hydrogen permeability but are highly durable. Hydrogen permeation characteristics were confirmed under conditions of 350~450 ℃ at 1 to 4 bar. The maximum hydrogen permeation flux was 0.69 ml/cm²/min for the Ni₄₈Nb₃₂Zr₂₀ alloy membrane without Pd coating, and 13.05 ml/cm²/min for the Pd coated alloy membrane.

• 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.

• Membrane Journal
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• v.32 no.6
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• pp.456-464
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• 2022

Hydrogen permeation performance was analyzed by manufacturing Pd and Pd-Cu membranes through electroless plating. As a support for the Pd and Pd-Cu membranes, α-Al₂O₃ ceramic hollow fiber were used. Pd-Cu membrane was manufactured through sequential electroless plating, and then annealing was performed at 500°C, for 18 h in a hydrogen atmosphere to make Pd and Cu alloy. After annealing, the Pd-Cu membrane confirmed that the alloy was formed through EDS (Energy Dispersive X-ray Spectroscopy) and XRD (X-ray Diffraction) analysis. In addition, the thickness of the Pd and Pd-Cu plating layers were measured to be about 3.21 and 3.72 µm, respectively, through SEM (Scanning Electron Microscope) analysis. Hydrogen permeation performance was tested for hydrogen permeation in the range of 350~450°C and 1~4 bar in hydrogen single gas and mixed gas (H₂, N₂). In a single hydrogen gas, Pd and Pd-Cu membranes have flux of up to 54.42 and 67.17 ml/cm²⋅ min at 450 °C and 4 bar. In the mixed gas, it was confirmed that the separation factors of 1308 and 453 were obtained under the conditions of 450 °C and 4 bar.

• 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.

• Transactions of the Korean hydrogen and new energy society
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• v.21 no.4
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• pp.264-270
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• 2010

Recently, the most promising methods for high purity hydrogen production are membranes separation such as polymer, metal, ceramic and composites. It is well known that Pd and Pd-alloys membranes have excellent properties for hydrogen separation. However, it has hydrogen embrittlement and high cost for practical applications. Therefore, most scientists have studied new materials instead of Pd and Pd-alloys. On the other hand, TiN powders are great in resistance to acids and chemically stable under high operating temperature. In order to get specimens for hydrogen permeation, the TiN powders synthesized were consolidated together with Co, Ni powders by hot press sintering (HPS). During the consolidation of powders at HPS, heating rate was 10 K/min and the pressure was 10 MPa. It was characterized by XRD, SEM. Also, we estimated the hydrogen permeability by Sievert's type hydrogen permeation membrane equipment.

• 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.

• 한국신재생에너지학회:학술대회논문집
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• 2007.11a
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• pp.79-79
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• 2007

• 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.