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Synchrotron Studies for Tackling Technical Challenges in the Hydrogen Economy

Synchrotron Studies for Tackling Technical Challenges in the Hydrogen Economy { Research into Novel Materials for Emerging Energy Applications } Tabbetha A. Dobbins 1,2 1. Institute for Micromanufacturing, Louisiana Tech University, Ruston, LA

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Synchrotron Studies for Tackling Technical Challenges in the Hydrogen Economy

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  1. Synchrotron Studies for Tackling Technical Challenges in the Hydrogen Economy {Research into Novel Materials for Emerging Energy Applications} Tabbetha A. Dobbins1,2 1. Institute for Micromanufacturing, Louisiana Tech University, Ruston, LA 2. Dept. of Physics, Grambling State University, Grambling, LA November 5, 2009 Institute for Micromanufacturing Louisiana Tech University

  2. “A (n) Inconvenient Truth” (about Energy Production) • The Fossil Fuel-based economy has limitations; • An alternative fuel cell energy infrastructure (PEM Fuel Cells and Solid Oxide Fuel Cells) will penetrate energy markets; • Technical challenges facing the PEM fuel cell are nevertheless substantial; • Creative solutions are needed to tackle our societal need for “cleaner and greener” energy. H2 Fuel??? ? Animation courtesy of: http://www.humboldt.edu 2

  3. Target Performance Image from Satyapal, Petrovic, Thomas (Scientific American, April 2007) Targets Table Reproduction from Millikan and Rossmeissl Aug. 14, 2002 Workshop 3

  4. DoE Targets for Hydrogen Storage Materials 4

  5. Advanced Photon Source (APS) at Argonne National Laboratory Synchrotron (High Flux) X-rays Source at CAMD (LSU in Baton Rouge, LA) • 1.3Mile, 7GeV ring of electrons in storage ring. • 38 experimental sectors • Small-Angle X-ray Scattering (SAXS), 3D Imaging • Collaborators: Jan Ilavsky and Francesco DeCarlo • 0.3 Mile, 1-2GeV ring of electrons in storage ring. • 15 experimental sectors • X-ray Absorption Spectroscopy, 3D Imaging, and SAXS • Collaborators: Amitava Roy Synchrotron Accelerators

  6. Synchrotron Radiation Facilities in the US SRC CHESS NSLS ALS APS SURF SSRL CAMD Is the only SR source in the South!

  7. Some Grand Challenge Areas in H2 Storage Research • Catalysis: What is role of transition catalysts in the hydrogen discharge and recharge reaction? How are non-reversible products formed and what are their roles in catalysis? • Kinetics: What fundamental limits hydrogen desorption kinetics? What are mass transport limitations in hydrogen storage materials? • Improved Research Tools: What instrumentation developments are needed for improved examination of atomic local structure (0.1 – 2nm) and microstructure (2nm – 1000 mm)? 7

  8. Research Highlights Fundamental Materials Research Problems– (1) Role of Catalyst still not well understood; (2) Slow diffusion and reaction rates should be addressed. 3D Imaging of Interphase Boundary Area between LiBH4/MgH2 and TiN/NaAlH4 Dobbins T.A., Decarlo F., Ziao, X., Ukpai W., Narase Gowda S. (To be published) Formation of TiAlx Alloys during introduction of TiCl3 catalyst to NaAlH4 Dobbins T.A., Abrecht M., Uprety Y., Moore K., ”An X-ray Photoemission Electron Microscopy Study of the Formation of Ti-Al Phases in 4 mol % TiCl3 Catalyzed NaAlH4 During High Energy Ball Milling”, Nanotechnology, 20, 204014 (2009). Microwave irradiation for desorption of H2 from NaAlH4 Krishnan R., Agrawal D., Dobbins T.A.,“Microwave Irradiation Effects on Reversible Hydrogen Desorption in Sodium Aluminum Hydrides (NaAlH4)”, Journal of Alloys and Compounds, 470 [1-2] 250 (2009). TiCl3 dopant mitigating Na+ and Al3+ diffusion rates in NaAlH4 Dobbins, T.A., Bruster E.B., Oteri, E.U., Ilavsky J., ”Ultrasmall-Angle X-ray Scattering (USAXS) Studies of Morphological Trends in High Energy Milled NaAlH4 Powders”, Journal of Alloys and Compounds 446-447 pp 248-254 (2007). Thin polymer films containing Ti3+ overlayed onto NaAlH4 Kamineni V., Lvov Y.M., Dobbins T.A. “Layer-by-Layer Nanoassembly Using Formamide as a Working Solvent”, Langmuir23 pp 7423-27 (2007). 8

  9. 3D Imaging (Computed X-ray Tomography) 2 NaAlH4 + 2TiN 2TiAl + 2 NaN + 4 H2(g) 50 mol % TiN in NaAlH4 (17 keV) (imaged at CAMD) • Tomography can guide this work by yielding interfacial contact area. • Tomography also Offers a means to define active crystallographic surfaces (coupled with Wulff construction of images and by DFT). 9

  10. TiAl3 TiAl 125 minute mill time 25 minute mill time 5 minute mill time 1 minute mill time 0 minute mill time (blended) EXAFS: TiAl and TiAl3 formation during introduction of TiCl3 catalyst to NaAlH4 Radial Distribution Function Normalized Absorption TiAl3 10

  11. Ti Cl 5mm 5mm Na Al 5mm 5mm X-ray Photoemission Electron Microscopy (XPEEM): TiAlx formation during high energy milling Al K-edge Spectra 25 Minute Mill Ti L-edge Spectra NaAlH4+4 mol % TiCl3 after high energy milled for 25 minutes. XPEEM data were collected at the VLS PGM beamline at the Synchrotron Radiation Center (SRC), Madison, WI. (Collaborator: Michael Abrecht) 11

  12. Small-Angle X-ray Scattering (SAXS) (a) (b) SAXS Data 0 min mill time 1 min mill time (c) (d) 5 min mill time 25 min mill time SEM images of undoped NaAlH4 powders blended for 2 minutes in dry N2 glovebox and milled for (a) 0 minutes; (b) 1 minute; (c) 5 minutes; and (d) 25 minutes. Quantitative Parameter to describe microstructure (in terms of surface area) • p~-3 for High surface area. • p~-4 smoother colloidal particle (lowest surface area) • SA~rDs~rpr6 In Collaboration with Jan Ilavsky (Advanced Photon Source) 12 Dobbins, T.A., Bruster E.B., Oteri, E.U., Ilavsky J., JALCOM 446-447 p 248 (2007).

  13. Summary and Future Plans: • Dept. of Energy: Energy Frontier Research Center • The Center for Atomic-Level Catalyst Design. (Lead: James Spivey @ LSU) • Center involves 8 institutions in the U.S. (LaTech, GSU, GaTech, UFl, Penn State, Tulane and abroad (Univ. of Utrecht). • The overall objective of LaTech/GSU work is to explore catalyst structure-property relationships which dictate fuel conversion reaction mechanisms and reaction rates using synchrotron x-ray scattering and x-ray absorption spectroscopy. • NSF Faculty Early Career Development Award • The objective of this proposal is to understand the influence of catalytic additives in enhancing atomic mobility and desorption rates in metal hydrides (specifically, NaAlH4 and LiBH4) by incorporating x-ray and neutron studies. • Two new courses cross-listed at LaTech, LSU and GSU. • (1) Synchrotron Studies and (2) Alternative Energy • High school design challenge: Design H2 tank for Fuel Cell Vehicle. X-ray Data for unique Insight into structure of materials Synchrotron Courses for training new generation of students in formal setting Undergraduate Student Mentoring High School Fuel Cell Workshops C

  14. Acknowledgments Graduate Students: Corisma Robinson (XANES); Vimal Kamineni (EXAFS/XANES) Shathabish Narase Godwa (Neutron Studies) Undergraduate Students: Youaraj Uprety (XPEEM Analysis); Kristan Moore (X-ray Diffraction); Whitney Fisher (Tomography); Collaborators: • CAMD (EXAFS/XANES): Amitava Roy and Greg Merchan • CAMD (Tomography): Kyunming Ham and Les Butler • SRC (XPEEM): Michael Abrecht • APS (USAXS): Jan Ilavsky • APS (Tomography): Francesco Decarlo and Xianghui Xiao • LaTech IfM: Daniela Mainardi, Phani Krisha Dathara, Yuri Lvov Funding Sources: • Department of Energy, Office of Basic Energy Sciences (Contract No.: DE-FG02-05ER46246). • National Science Foundation, Division of Materials Research (Contract No.: DMR-0508560). • National Science Foundation, CAREER Award Program (Contract No.: DMR-0847464). • Louisiana State Board of Regents Support Fund, RCS Program • Louisiana State Board of Regents Support Fund, PFUND Program www2.latech.edu/~tdobbins 14

  15. Thank You. www2.latech.edu/~tdobbins 15

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