PALLADIUM AND PALLADIUM ALLOY MEMBRANES ...

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CAMP Internal Report-LIT 3 June, 2011

PALLADIUM AND PALLADIUM ALLOY MEMBRANES: Sortable Matrix L.G. Twidwell, K. Konen

Center for Advanced Mineral and Metallurgical Processing (www.camp-montanatech.net) Metallurgical and Materials Engineering Department School of Mines Montana Tech of The University of Montana, Butte, MT 59701 (www.mtech.edu) email [email protected]

INTENT OF REPORT The intent of this report is to provide an extensive list of palladium and palladium alloy membrane experimental hydrogen transport data in a spreadsheet format that allows the user to sort the information into categories of specific interest to the user; and, an extensive bibliography of referenced publications (most of which are hyperlinked to PDF publications for Montana University personnel use only).

BACKGROUND The attached spreadsheet atlas contains over 750 entries gleamed from the literature. This is a rather miniscule amount of the data available in the literature but is by far more than anything else that has been published. Two other documents are available that may be of interest to the reader. They are: “A Literature Guide to Palladium and Palladium Alloy Membranes” and “Recipes for Electroless Plating of Palladium and Palladium Alloy Membranes”. The documents are available upon request through the CAMP website (www.camp-montanatech.edu). In addition to the spreadsheet atlas we have included a Bibliography that list many more publications than those referenced in the report. For detailed information on specific topics you will likely want to refer to the referenced publications; to facilitate this we have collected most of the referenced publications as PDFs. The PDF publications are hyperlinked to the references in the present report and in each of the two previous reports specified above. The PDFs are included on a DVD supplied with each printed report. The reports containing the hyperlinked references are only available for use by the CAMP and Montana University system researchers and cannot be used nor sent off-campus. However, each non-hyperlinked report contains a bibliography that lists the referenced papers and collection of the publications can be made by the user through the internet. Some of the PDF publications must be purchased through vendor organizations such as Science Direct; however, many are available and can be downloaded free. Description of Matrix This report contains the sortable matrix as a Microsoft Excel file. Lists of abbreviations and nomenclature used in the matrix tabulation are presented in the following tables. The following information has been tabulated (when available) in the Matrix file: type of membrane (palladium or palladium alloys); composition of membrane (PdAg, PdAu, PdCu, PdCuAg and others); thickness of membrane (µm); method of membrane preparation (electroless, foil, electroplating, sputtered, and others); hydrogen test conditions including retentate (feed) and permeate (discharge) pressures, and temperature of test; and test results including permeance, permeability, hydrogen flux, and selectivity; and source of information (publication reference and year).

Nomenclature Nomenclature

k, permeability



k , permeance

Units

Comments n

mol H2/(msP )

2

n

mol H2/(m sP )

2

mol H2/(m s) (most used) at Pa, T1 J or NH2, flux

3

2

ft H2/(ft hr) 3

2

cm H2/(m s) 3

2

m H2/(m s)

n, pressure exponent

Pa, total pressure PH2, partial pressure of hydrogen PH2 perm, partial pressure of hydrogen on permeate (discharge) side PH2 ret, partial pressure of hydrogen on retentate (feed) side T, temperature XM, membrane thickness α, selectivity

Usually 0.5 to 1, much of the literature reports results at 0.5

This is the most used unit combination. mol H2 – moles of hydrogen gas m – meter Pn – pressure in pascals “n” – pressure exponet Permeance Is the slope of a plot of flux versus the th difference in the n root of the pressure on the retentate and permeate sides of the membrane , n i.e. the slope of a plot of H2 flux versus [(PH2, ret) n (PH2, perm) ]. It is also the permeability divided by the membrane thickness, e.g. k/XM. Xm – membrane thickness in meters. s - seconds 2

To Convert from other units to mol H2/(m s) at T1, Ppascal multiply by: -5

o

1.018*10 Ppascal/T1 K -7

o

-1

o

1.202*10 *Ppascal/T1 K 1.202*10 *Ppascal/T1 K If “n” is 0.5 the hydrogen transport is controlled by bulk diffusion through the membrane. Greater values for “n” denote that the transport is influenced by other factors than just bulk diffusion through the membrane, such as, surface contamination, hydrogen flow through defects or grain boundaries, resistance of the substrate support material, lattice defects, presence of alloying elements, or thermal treatment history.

atm, psi, or kPa (most used) atm, psi, or kPa atm, psi, or kPa atm, psi, or kPa o

K meters (m) or microns (µm) α=mol % H2/mol %N2,He,other gases or in some cases the ratio of hydrogen flux/gas constituent flux

Abbreviations in Matrix H2 Test Conditions

Pd Membrane Type

µm

Method

Substrate

ToK

Test Results

P H2, ret

P H2, per

kPa

kPa

n

k

Reference N H2

yr

Selectivity H2/N2

Thickness

Pd or Pd Alloy

k'

In Tabulation

Real

permeability, mol H2 /(msPan) Porous stainless steel=PSS Ceramic=Ceram Al2O3=α or γ

electroless=elp electroplating=ep sputtering=sput foil=foil cathode vapor deposition=CVD photocatalytic deposition=PCD laser synthesis=ls

Pressure on retentive (feed) side

Pressure on permeate (discharge) side

Pressure exponent =0.5-1

permeance, mol H2 /(m 2 sPan)

Last name of first author, eg Rothenberger et al. (2004, ref

Flux, mol H2 /(m 2 s) year of ref paper, eg 2000

Awareness of Data We have collected and tabulated data primarily from two major sources, i.e. from tables presented by various authors to compare their test results to those presented by other researchers and from tabulated results in publications where the authors summarized their specific study results. Therefore, the reader may want to refer to the original publications (easily done using the hyperlinking feature) for more detailed results. For example, we have tabulated the results as presented by the authors from comparative and summarized tables, however, each paper contains much more data in graphs and in the authors discussion of results. Comparative Tabulated Results Various authors have recalculated the results from other investigators to allow them to make comparisons to their study results, e.g. Rothenberger et al. (2004) present a very useful tabulation comparing permeance, permeability, and flux based on a common calculation basis “A secondary objective of this study was to compare the performance of the membrane at high hydrogen partial pressure conditions with the numerous prior studies of thin supported palladium films characterized at low hydrogen partial pressure conditions. Although membrane permeance or permeability can be compared directly if the membranes are characterized by the same exponent value (e.g., n = 0.5), membranes with different hydrogen partial pressure exponent values should be compared by calculating the hydrogen flux at standard hydrogen partial pressures gradients on the retentate and sweep sides. Therefore, the hydrogen flux across each membrane was evaluated at “standard conditions” (a hydrogen pressure gradient of 100 kPa) as a means of comparing their performances.” The authors present an example of how using the standard conditions influence the value of the measurement “The results, though useful, must be viewed with a degree of caution. The permeability and permeance relationships are a very broad measure of material behavior. They are particularly sensitive to the choice of the best fit exponent, n. For example, the flux of the 2 NETL-Ma-1-21.3 membrane at 673K was 4.8 × 10−2mol/m s when calculated using the permeability relationship with 2 n = 0.5, but 3.5 × 10−2 mol/m s when calculated using the best fit exponent of n = 0.61 (Table 2). These two values, differing by almost 40%, were calculated from the same set of experimental data, with the only difference being how the original data was fit.” Rothenberger et al. (2004). Another example is the tabulation by Howard et al. (2004) who reported the results of a number of investigators for palladium/copper alloys. The specific data presented by the individual investigators were converted to common units and to values determined using the common “n” value of 0.5 Some authors have prepared comparative tables that required the conversion of specific investigators reported units 3 2 3 2 2 for permeance, permeability or flux to a common basis, e.g. for fluxes of m /m /hr or cm /cm /hr to mol/m /s or visa versa. Also, in some cases authors have extrapolated data to their temperature of interest from data collected over a

different temperature range. The comparative tabulations presented by authors are included in the present matrix with units as reported in their publication.

Spreadsheet Results

The major tabulation sheet is the one titled “Original Master Data Summary”. We have sorted the entries by metal, temperature, flux, permeance, membrane thickness, method of membrane formation (see these results on the included Excel sheets). One printout for the “by metal” sorted matrix is attached with this report. The user may want to sort using other criteria. If you as the user see some interesting data entries you can get the details from the specific PDF. In fact, probably the value of this work will be the convenience for you (or your graduate students) to look at specific publications without having to dig them out of a bibliography. Bibliography Abate, Salvatore, Gabriele Centi, Siglinda Perathoner, Dangsheng S. Su, Gisela Weinberg, 2010. The Influence of the Nanostructure on the Effect of CO2 on the Properties of Pd-Ag Thin-Film for H2 Separation, Applied Catalyst A: General, doi:10:1016/j.apcata.2010.08.005, 11 p. Ackerman, F.J., G.J. Koskinas, 1972. Permeation of Hydrogen and Deuterium Through Palladium–Silver Alloys, J. Chem. Eng. Data 17, 51. Adhkari, S., S. Fernando, 2006. Hydrogen Membrane Separation Techniques, Ind. Eng. Chem. Res., 45, 875-81. Ahmad, A.L., M.A.T. Jaya, C.J.C. Derek, M.A. Ahmad, 2011. Synthesis and Characterization of TiO2 Membrane with Palladium Impregnation for Hydrogen Separation, J. Membrane Science, 366, 166-75. Ahmad, A.L., N.N.N. Mustafa, 2007. Sol-Gel Synthesized of Nanocomposite Palladium-Alumina Ceramic Membrane for H2 Permeability: Preparation and Characterization, Int. J. Hydrogen Energy, 32, 2010-2021. Akis, B.C., E.E. Engwall, I.P. Mardilovich, Y.H. Ma, 2003. Effect of the in situ Formation of an Intermetallic Diffusion Barrier Layer on the Properties of Composite Palladium Membranes, ACS Fuel Chem. Div. Preprints, 48(1), 337. Alqasmi, R.A., S. Paasch, H.-J. Schaller, 1999. Thermodynamic Properties of Pd-Y and Pd-Gd Intermetallic Phases, J. Alloys and Compounds, 283, 173-177. Amandusson, H., L.-G. Ekedahl, H. Dannetun, 2001. Hydrogen Permeation through Surface Modified Pd and PdAg Membranes, J. Membrane Science, 193, 35-47. Amandusson, H. Hydrogen Extraction with Palladium Membrane, 2000. PhD Dissertation No. 651, Linkopings University, Sweden, p 38. Amano, M., C. Nishimura, M. Komaki, 1990. Effects of High Concentration CO and CO2 on Hydrogen Permeation Through The Palladium Membrane, Mater. Trans. JIM, 31, 404. Armor, J.N., 1998. Applications of Catalytic Inorganic Membrane Reactors to Refinery Products, J. Membrane Science, 147, 217-233. ASM, Binary Phase Diagrams, The Metals Handbook, Volume 3, American Society for Metals, Metals Park, Ohio, 1992, p 257. Augustine, A.S., Yi H. Ma, N.K. Kazantzis, 2011. High Pressure Palladium Membrane Reactor for the High Temperature Water-Gas Shift Reaction, Int. J. Hydrogen Energy, doi:10.1016/j.ihydene.2011.01.172, 11p. Ayturk, M.E., Yi Hua Ma, 2009. Electroless Pd and Ag Deposition Kinetics of the Composite Pd and Pd/Ag Membranes Synthesized from Agitated Plating Baths, J. Membrane Science, 330, 233-45. Ayturk, M.E., E.A. Payzant, S.S. Speakman, Y.H. Ma, 2008. Isothermal Nucleation and Growth Kinetics of Pd/Ag Alloy Phase via in situ Time-Resolved High-Temperature X-ray Diffraction (HTXRD) Analysis, J. Membrane Science, 316, 97-111. Ayturk, M.E., E.E. Engwall, Y.H. Ma, 2007. Microstructure Analysis of the Intermetallic Diffusion Induced Alloy Phases in Composite Pd/Ag/Porous Stainless Steel (PSS) Membranes, Ind. Eng. Chem. Res., 46 (12), 4295-4306 Ayturk, M. Engin, Ivan P. Mardilovich, Erik E. Engwall, Yi Hua Ma, 2006. Synthesis of Composite Pd-Porous Stainless Steel (PSS) Membranes with a Pd/Ag Intermetallic Diffusion Barrier, J. Membrane Science, 285, (1-2), 385-394.

Basile, A., F. Gallucci, A. Iulianelli, G.F. Tereschenko, M.M. Ermilova, N.V. Orekhova, 2008. Ti-Ni-Pd Dense Membranes-The effect of the Gas Mixtures on the Hydrogen Permeation, J. Membrane Science, 310, 44-50. Basile, A., F. Gallucci, S. Tosti, 2008. Synthesis, Characterization, and Applications of Palladium Membranes, Membrane Science Tech., 13, 225-323. (Review) Basile, Angelo, Fausto Gallucci, Luca Paturzo, 2005. Hydrogen Production from Methanol by Oxidative Steam Reforming Carried out in a Membrane Reactor, catalysis Today, 104, 251-59. Basile, Angelo, Luca Paturzo, Fortunato Lagana, 2001. The Partial Oxidation of Methanol to syngas in a Palladium Membrane Reactor: Simulation and Experimental Studies, Catalysis Today, 67, 65-75. Bernardo, P., G. Barbieri, E. Drioli, 2010. Evaluation of Membrane Reactor with Hydrogen-Selective Membrane in Methane Steam Reforming, Chemical Engineering Science, 65, 1159-1166. Berseneva, F., N.I. Timofeev, A.B. Zakharov, 1993. Alloys of Palladium with Metals of the Platinum Group as Hydrogen-Permeable Membrane Components at High Temperatures of Gas Separation, Int. J. Hydrogen Energy, 18 (1), 15-18. Bhargav, Atul, Gregory S. Jackson, Richard J. Ciora Jr., Paul T.K. Liu, 2010. Model Development and Validation of Hydrogen Transport through Supported Palladium Membranes, J. Membrane Science, 356, 123-132. Bhandari, R., Yi Hua Ma, 2009. Pd-Ag Membrane Synthesis: The Electroless and Electro-plating Conditions and their Effect on the Deposits Morphology, J. Membrane Science, 334, 50-63. Bhargav, Atul, Gregory S. Jackson, 2009. Thermokinetic Modeling and Parameter Estimation for Hydrogen Permeation through Pd0.77Ag0.23 Membranes, Int. J. of Hydrogen Energy, 34, 5164-5173. Bhatia, B. and D. S. Sholl, 2005. Chemisorption and Diffusion of Hydrogen and Nickel on Flat and Stepped Nickel Surfaces, J. Chem. Phys., 122, 204707. Bhatia, B., X. Luo, C. A. Sholl, and D. S. Sholl, 2004. Diffusion of Hydrogen in Cubic Laves Phase HfTi2Hx, J. Phys. Condens. Matter, 16, 8891. Bosko, M.L., F. Ojeda, E.A. Lombardo, L.M. Cornaglia, 2009. NaA Zeolite as an Effective Diffusion Barrier in Composite Pd/PSS Membranes, J. Membrane Science, 331, 57-65. Bosko, María L., David Yepes, Silvia Irusta, Pierre Eloy, Patricio Ruiz, Eduardo A. Lombardo, Laura M. Cornaglia, 2007. Characterization of Pd-Ag Membranes after Exposure to Hydrogen Flux at High Temperatures, J. Membrane Science, 306, 56-65. Brunetti, A., G. Barbieri, E. Drioli, 2009. Upgrading of a Syngas Mixture for Pure Hydrogen Production in a Pd-Ag Membrane Reactor, Chemical Engineering Science, 64, 3448-3454. Bryden, K.J., J.Y. Ying, 2002. Nanostructured Palladium-Iron Membranes for Hydrogen Separation and Membrane Hydrogenation Reactions, J. Membrane Science, 203, 29-42. Bryden, K.J., J.Y. Ying, 1995. Nanostructured Palladium Membrane Synthesis by Magnetron Sputtering, Material Science and Engineering, A204, 140. Cai, Q., 1997. Non-Cyanide Electroless Gold Plating, Applicable Technology Market, 4, 7-8. CAMP, 2011. Fuel Cell Design and Manufacturing Technology Development, Center for Advanced Mineral and Metallurgical Processing, www.camp-montanatech.net, 2011. Caravella, Alessio, Giuseppe Barbieri, Enrico Drioli, 2008. Modeling and Simulation of Hydrogen Permeation through Supported Pd-Alloy Membranes with a Multicomponent Approach, Chemical Engineering Science, 63, 2149-60. Castelli, S., L. Bimbi, M. De Grancesco, A. Iasonna, S. Tosti, V. Violante, 1998. Deposition of a Pd-Ag Film Alloy on th Macroporous Ceramic Supports, Proceedings of the 20 SOFT, Marseille, Fusion Tech., 2, 993-996. Catalano, Jacopo, Marco Giacinti Baschetti, Giulio C. Sarti, 2010. Hydrogen Permeation in Palladium-Based Membranes in the Presence of Carbon Monoxide, J. Membrane Science, 362, 221-33. Catalano, Jacopo, Marco Giacinti Baschetti, Giulio C. Sarti, 2009. Influence of the Gas Phase Resistance on Hydrogen Flux through Thin Palladium-Silver Membranes, J. Membrane Science, 339, 57-67. Chabot, J., et al., 1988. Fuel Cleanup System—Poisoning of Palladium–Silver Membranes by Gaseous Impurities, Fusion Technol. 14, 614. Chang, Hsin-Fu, Wen-Ju Pai, Ying-Ju Chen, Wen-Hsiung Lin, 2010. Autothermal Reforming of Methane for Producing High-Purity Hydrogen in a Pd/Ag Membrane Reactor, Int. J. Hydrogen Energy, 35, 12986-92. Checchetto, R., N. Bazzanella, B. Patton, A. Miotello, 2004. Palladium Membranes Prepared by R.F. Magentron Sputtering for Hyrdogen Purification, Surface Coating Tech., 177/178, 73.

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