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Materials Innovations in an Emerging Hydrogen Economy Cocoa Beach FL 26 February 2008 H ollow G lass M icrosphere s (HGMS) Designed for Storing Hydrogen Delbert E. Day MO-SCI Corp Rolla MO & James E. Shelby New York State College of Ceramics Alfred University. OUTLINE. Introduction

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OUTLINE

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  1. Materials Innovations in an EmergingHydrogen EconomyCocoa Beach FL26 February 2008Hollow Glass Microspheres (HGMS) Designed for Storing HydrogenDelbert E. DayMO-SCI CorpRolla MO&James E. ShelbyNew York State College of CeramicsAlfred University

  2. OUTLINE Introduction What are HGMS and how are they made? Why use HGMS for hydrogen storage? Gas storage and release from HGMS Thermal release Photo-induced outgassing (release) Photo-induced release from soda lime glass doped with FeO, NiO or CoO Conclusions

  3. HGMS Applications • Commercially available • Paint filler, polymer/rubber filler, foam filler, oil well drilling mud, bowling balls, etc. • Laser fusion targets --- H2 D2 • Strict specifications on size, shape, wall thickness, and surface smoothness (achieved internal pressure of 10,000 psi) • Containers for hydrogen storage (Teitel-1977) Shelby and Hall

  4. Why Use HGMS for Hydrogen Storage? Non-toxic Mechanically strong Low cost Reusable Light weight Environmentally friendly Chemically durable High hydrogen mass density, 6 to 14 wt% Commercially available Ultra pure hydrogen Fire safe—non-explosive

  5. Manufacturing of HGMS Prepare precursor particles Gas-evolution (Blowing) Melt & spheridize particles Collect & size N2, H2O,CO2,SO2 Glass types: Soda Lime Borosilicate High Silica Heated tube or flame

  6. Manufacturing of HGMS Prepare precursor particles Gas-Evolution (Blowing) Melt and spheridize particles Collect and size N2, H2O,CO2,SO2 Glass types:: Soda Lime Borosilicate High Silica Heated tube or flame

  7. Appearance of as-made HGMS made from doped amber soda lime glass 5 wt % CoO 5 wt % FeO Back scattered image (200X) Shelby, Raszewski, & Hall

  8. Concepts of Gas Storage & Release Using HGMS Gas Filling Stage Gas Release H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 H2 High Pressure-High Temperature Gas Low Pressure-Ambient Temperature

  9. GLASSES USED TO MAKE HGMS Ave dia* Ave wall* Bulk density thickness g/cc Clear “soda lime” 131 2.3 0.41 Amber “soda lime” 38 1.9 0.46 Amber “soda lime” + 1 or 5 wt % FeO 60 1.3 0.25 “ “ NiO 133 2.8 0.25 “ “ CoO 62 0.9 0.19 * Microns Soda lime glass contained 9 wt % B2O3 Sulfate blowing agent

  10. Residual Gas Analyzer instrument used to measure hydrogen release from filled HGMS Spl in 6 mm tube (10 to 90 mg) Shelby and Hall

  11. What is Photo – Induced Gas Release (Outgassing)? IR/Visible Radiation H2 H2 H2 H2 H2 H2 H2 H2 Hollow Glass Microspheres 800 – 2300 nm light is most effective 250 W Infrared Light Bulb Shelby & Hall

  12. Comparison of photo-induced H2 outgassing at 25oC vs. thermally induced outgassing by heating at 150°C (soda lime HGMS containing 5 wt% FeO). Photo-induced @ 25oC thermal—150oC Shelby & Hall

  13. Switch – like photo-induced H2 outgassing for HGMS containing 5 wt% FeO. 15 seconds ON/OFF cycle Lamp on full time after 780 seconds 5 minutes ON/OFF cycle Max release decreases with each cycle due to lower pressure in HGMS

  14. Effect of Dopant on Photo-induced H2 Release • CoO is more effective than FeO in photo-induced release • Rate of H2 release increases with increasing concentration of CoO. 700 torr Temp. 25 0C Shelby & Hall

  15. Photo-induced H2 release from HGMS of different diameter (microns) 5 % CoO >100 100>x>50 <50 Snyder, Wachtel, et.al. Lamp on

  16. Dependence of photo-induced release on fill pressure 5 % CoO 77,600 torr (1500psi) spl=10 mg 700 torr spl=90mg Snyder, Wachtel, et.al. Lamp on

  17. H2 retained in 5 wt% FeO HGMS after 5 weeks at 25oC or 50°C. 5 wks Thermally outgassed at25°C Shelby & Hall After 5 wks 97% retained at ~25°C and 92% at 50oC

  18. Conclusions Photo induced release offers many advantages for hydrogen storage >>fast response (10 to 20s) at ambient temperature >>release rate easily controlled >>no expected limit for on-off cycles Hydrogen retention > 90% after 5 wks at 50oC (122oF) HGMS have survived 5000 psi fill pressure (10wt% H2)

  19. Acknowledgements We thank the Department of Energy (DOE), contract DE-FG36-05GO15007, for funding this work.

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