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Control of excess heat production in Pd-impregnated alumina powder

Control of excess heat production in Pd-impregnated alumina powder. O. Dmitriyeva 1,2 , R. Cantwell 1 , M. McConnell 1 , G. Moddel 2 1 Coolescence, LLC, Boulder, CO, USA 2 University of Colorado – Boulder, CO, USA. Motivation. Excess heat in Pd-impregnated materials with D 2 1-5

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Control of excess heat production in Pd-impregnated alumina powder

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  1. Control of excess heat production in Pd-impregnated alumina powder O. Dmitriyeva1,2, R. Cantwell1, M. McConnell1, G. Moddel2 1 Coolescence, LLC, Boulder, CO, USA 2 University of Colorado – Boulder, CO, USA 10th Workshop - Siena

  2. Motivation • Excess heat in Pd-impregnated materials with D2 1-5 • Evidence of exothermic H/D exchange chemical reactionin water4,5 1 Y. Arata, Z. Chang, Establishment of the "Solid Fusion" reactor, J. High Temp Soc., 34 (2008) 85-93. 2 Y. Sasaki, A. Kitamura, Y. Mioshi, T. Nohmi, A. Taniike, A. Takahashi, R.Seto, Y. Fujita, Proceedings of ICCF15, (2009) 94-99. 3 T. Hioki, H. Azuma, T.Nishi, A. Itoh, J. Gao, S. Hibi, T. Motohiro, J. Kasagi, Proceedings of ICCF15, (2009) 88-93. 4 D. Kidwell, D. Knies, A. Moser, D. Domingues ICCF15, (2009) 100-109. 5 O. Dmitriyeva, R. Cantwell, M. McConnell, and G. Moddel, ACS National Meeting and Exposition, Anaheim, 2011 10th Workshop - Siena

  3. Motivation • Excess heat in Pd-impregnated materials with D2 1-5 • Evidence of H/D exchange chemical reactionin water4,5 Questions to answer • Control excess heat by controlling amount of water? • Enough water to account for excess heat? 10th Workshop - Siena

  4. Gas-loading system • Precision of temperature control 10 mK • 6 g of material • Pressurized up to 1200 torr • Temperatures 40 - 390oC to vacuum pump pressure gauge reference Ma sample under test temperature acquisition thermistors isothermal chamber HP 5890 gas chromatographer H2 D2 10th Workshop - Siena

  5. Excess heat generation 1200 0 Endothermic heat Exothermic heat Excess heat = Exothermic heat + Endothermic heat 10th Workshop - Siena

  6. Material fabrication • Oxide supports: • alumina: Fisher Scientific P/N: CAS 1344-28-1 74-177 μ particle size • high crystalline α-alumina: American Elements P/N AL-OX-O2-P.30UM 30-50 μ particle size • 2% Pd by weight in by wet impregnation of different precursors: • Pd(NH3)4Cl2 • H2PdCl4 commercially available 5% Pd in alumina Acros Organic CAS:7440-05-3 average particle size 5 nm 20 nm O. Dmitriyeva, R. Cantwell, M. McConnell, and G. Moddel, “Mechanisms for heat generation during deuterium and hydrogen loading of palladium nanostructures”, ICCF-16, Chennai, India, 2011, in press 10th Workshop - Siena

  7. H/D exchange reaction D. Kidwell, D. Knies, A. Moser, D. Domingues, Yes, Virginia there is heat, but it is most likely of chemical origin, Proceedings of the 15th International Conference on Condensed Matter Nuclear Science, (2009) 100-109. 10th Workshop - Siena

  8. Heating and cooling due to H/D exchange Qexcess endothermic deuteriumruns deuterium runs hydrogen runs Qexcess exothermic exothermic heat recharged 10th Workshop - Siena

  9. Presence of water Thermogravimetric analysis Summary 8% of mass lost by 400ºC Residual gas analysis (RGA): H2O weight 100% 95% 90% derivative 0 200 400 600 800 1000 Temperature (ºC) 10th Workshop - Siena

  10. Experimental schedule 10th Workshop - Siena

  11. Experimental schedule 10th Workshop - Siena

  12. Experimental schedule 390C 300C 250C 200C 350C 150C 40C 100C 5 hours 10th Workshop - Siena

  13. Experimental schedule 390C 300C 250C 200C 350C 150C 40C 100C 5 hours 40C 10th Workshop - Siena

  14. Experimental schedule 10th Workshop - Siena

  15. Reactivation of heat production • Average weight increase • 3.6 – 5% 5 hours 10th Workshop - Siena

  16. Reactivation of heat production 10th Workshop - Siena

  17. Heat available from water 10th Workshop - Siena

  18. Summary • H/D exchange responsible for at least some of excess heat • reaction nulled by 390˚C bakeout • reaction reactivated by moisture reabsorption • Calculations show enough water to account for excess heat in our experiment 10th Workshop - Siena

  19. Conclusion Baking out the material in vacuum for prolonged time prior to any contact with gases is a way to eliminate potential H/D exchange energy contribution 10th Workshop - Siena

  20. BACKUP SLIDES 10th Workshop - Siena

  21. Water content during bakeout 10th Workshop - Siena

  22. H/D exchange confirmed … by RGA Pressure (torr ×10-6) 10th Workshop - Siena Run #

  23. H/D exchange confirmed … by nuclear magnetic resonance (NMR) 10th Workshop - Siena

  24. H/D exchange confirmed … by Fourier transform infrared spectroscopy (FTIR) 10th Workshop - Siena

  25. H/D exchange reaction D2 H2 3. reversed spillover 1. spillover H D Pd H 2b) exchange D H D D 2a) H H D H O O Alumina substrate O O O D. Kidwell, D. Knies, A. Moser, D. Domingues, Yes, Virginia there is heat, but it is most likely of chemical origin, Proceedings of the 15th International Conference on Condensed Matter Nuclear Science, (2009) 100-109. 10th Workshop - Siena

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