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Studies on Hydrogen Storage in Carbon Materials

Studies on Hydrogen Storage in Carbon Materials. Store and generate. B.Viswanathan*, S. Ramaprabhu # , P.Selvam*, Prathap Haridass $ , S. Rajalakshmi & , K.S.Dhathatreyan & and Pani @ * National Centre for Catalysis Research, Department of Chemistry

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Studies on Hydrogen Storage in Carbon Materials

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  1. Studies on Hydrogen Storage in Carbon Materials Store and generate B.Viswanathan*, S. Ramaprabhu#, P.Selvam*, Prathap Haridass$, S. Rajalakshmi &, K.S.Dhathatreyan& and Pani@ *National Centre for Catalysis Research, Department of Chemistry #Alternative Energy and Nanotechnology Laboratory (AENL), Nano Functional Materials Technology Centre (NFMTC), Department of Physics $Department of Materials and Metallurgical Engineering Indian Institute of Technology Madras, Chennai 600 036 &ARC Centre for Fuel Cell Technology, and @Nanoram

  2. HYDROGEN FUTURE: FACTS AND FALLACIES: CAUTION [M. Aulice Scibioh and B. Viswanathan, Bulletin of the Catalysis Society of India, vol.3, pp.72-81(2004)] A transition to a ‘hydrogen economy’ is a sea change in our energy infrastructure and is not to be taken lightly. As an energy carrier, hydrogen is to be compared to electricity, the only wide spread and viable alternative. When hydrogen is employed to transmit renewable electricity, only 50% can reach the end user due to losses in electrolysis, hydrogen compression and the fuel cell. The rush into a hydrogen economy is neither supported by energy efficiency arguments nor justified with respect to economy or ecology. In fact, it appears that hydrogen will not play an important role in a sustainable energy economy because the synthetic energy carrier cannot be more efficient than the energy from which it ismade. Renewable electricity is better distributed by electrons than by hydrogen. Consequently, the hasty introduction of hydrogen as an energy carrier cannot be a stepping stone into a sustainable energy future. The opposite may be true. Because of the wastefulness of a hydrogen economy, the promotion of hydrogen may counteract all reasonable measures of energy conservation. Even worse, the forced transition to a hydrogen economy may prevent the establishment of a sustainable energy economy based on an intelligent use of precious renewable resources.

  3. Transition to Hydrogen Economy • Production • Storage Metal Hydride MOF Choice limited • Distribution Petrol dispensing station

  4. Transition to a “Hydrogen Economy” • Broad-based use of hydrogen as a fuel – Energy carrier analogous to electricity – Produced from variety of primary energy sources – Can serve all sectors of the economy: transportation, power, industry, buildings and residential – Replaces oil and natural gas as the preferred end-use fuel – Makes renewable and nuclear energy “portable” (e.g. transportation needs) • Advantages: – Inexhaustible – Clean – Universally available to all countries Before and Now

  5. Hydrogen Storage some Directions

  6. Situation and Questions • Production, storage and application - challenges of hydrogen economy • Solid state storage – remarkable but not reproducible • 6.5 wt% - desired level (according to original DOE standards) • Demands consistent and innovative practice • Are the carbon materials appropriate for solid state hydrogen storage? • If this were to be true, what type of carbon materials or what type of treatments for the existing carbon materials are suitable to achieve desirable levels of solid state hydrogen storage? • What are the stumbling blocks in achieving the desirable solid state hydrogen storage? • Where does the lacuna lie? Is it in our theoretical foundation of the postulate or is it in our inability to experimentally realize the desired levels of storage?

  7. Why carbon materials for solid state hydrogen storage? Coordination number is variable/expandable Promote new morphologies Covalent character retention Variable hybridization possible Geometrical possibilities/size considerations Meta-stable state Similar to biological architectures “Haeckelites” Boron and nitrogen doped graphitic arrangements promise important applications.

  8. Hydrogen storage capacity reported in carbon nanostructures

  9. A plot of the reported hydrogen storage capacities of CNTs from the literature versus their year of publication. Reprinted with . Seung Jae Yang , Haesol Jung , Taehoon Kim , Chong Rae Park, Recent advances in hydrogen storage technologies based on nanoporous carbon materials, Progress in Natural Science: Materials International, Volume 22, Issue 6, 2012, 631 – 638, http://dx.doi.org/10.1016/j.pnsc.2012.11.006

  10. Research objectives • Processing of carbon based nanostructured materials • Doping of Nitrogen/Boron on carbon based nanostructured materials • 3. Dispersion of Pd metal nanoparticles on Boron/Nitrogen doped carbon • based nanostructured materials • 4. Characterization of these materials by XRD, SEM, HRTEM, XPS • 6. Measurement of the hydrogen absorption/adsorption and kinetics of • sorption using pressure reduction facility • 7. Development of novel low cost Carbon based materials with a hydrogen • storage capacity of 4-5 wt% hydrogen at room temperature and • moderate pressure

  11. Hydrogen exfoliated Graphene 20 nm 5 nm

  12. Materials investigated for hydrogen storage Pristine carbon nanostructures Few layer graphene (G) Chemical modifications Acid functionalization Nitrogen/Boron doping Nitrogen / Boron doped Few layer graphene (N-G) Acid functionalized Few layer graphene (f-G) Pd transition metal doping Pd metal nanoparticles decorated Nitrogen doped few layer graphene (Pd/N-G) Pd metal nanoparticles decorated acid functionalized few layer graphene (Pd/f-G)

  13. NITROGEN DOPING Acid functionalization leads to the agglomeration of graphene sheets Nitrogen Plasma • Treating Graphene with nitrogen plasma for 30 min using RF sputtering • Chamber pressure ~ 0.05 mbar • RF power ~ 120 W • Aluminum disc was used as target

  14. Characterizations of Pd/acid functionalized graphene FTIR Pd/f-Graphene Graphene G Pd/f-Graphene f-Graphene Graphene Pd/f-Graphene Graphene XRD Pd/f-G Pd nanoparticle size ~ 6.6 nm Pd metal loading is 20 wt% Graphene C GO Pd Graphite O

  15. Characterizations of Pd/nitrogen doped graphene Raman spectra XPS spectra Pd/N-G N-G Graphene(G) High resolution XPS spectra of (a) C 1s (b) N 1s (c) Pd 3d and (d) O 1s orbital of Pd/N-G C Nitrogen content in Pd/N-G :7 atomic % Pd Pd metal loading is 20 wt% O

  16. Microscopes images of Pd/nitrogen doped graphene N-Graphene Pd/N-Graphene N-Graphene Pd/N-Graphene Pd nanoparticle size ~ 3.1 nm

  17. Hydrogen adsorption isotherms of graphene composites Graphene N-Graphene H (wt%) Note the comparison between Graphene and heteroatom containing graphene

  18. Hydrogen adsorption isotherms of graphene composites Pd/f-Graphene Pd/N-Graphene Pd/B-Graphene

  19. Comparison of hydrogen adsorption isotherm values for different carbon nanocomposites

  20. MECHANISM Increase in hydrogen storage capacity of Pd/chemically modified graphene samples are due to • Nitrogen/Boron doping effect on graphene support and Pd nanoparticles Nitrogen/Boron doping can induce atomic charge density over graphene surface that enhances the interaction between carbon atoms and hydrogen molecules. Nitrogen/Boron doping of graphene surface leads to high dispersion, small particle size and strengthened interaction of catalyst metal nanoparticles over the support.

  21. SUMMARY • Graphene and GNP were chemically modified by acid functionalization and nitrogen doping for the dispersion of 3d transition metal nanoparticles. • Nitrogen doping provides high dispersion, small particle size and strengthened interaction of catalyst metal nanoparticles over the support. • Pd nanoparticles decorated Boron doped graphene gives an hydrogen storage capacity of 5.0 wt% at room temperature and 3.2 MPa pressure. • Enhancement in hydrogen storage capacity of Pd-Graphene nanocomposite is due to heteroatom doping and spillover mechanism. Future plan Work is in progress to achieve 5.0 wt% at room temperature and 2.0 MPa pressure.

  22. Studies on Hydrogen storage in carbon materials( No.103/140/2008-NT) PI Prof.B.Viswanathan, Head, NCCR, Department of Chemistry, IIT Madras, Chennai Co-PI: • Dr.K.S.Dhathathreyan, CFCT,ARCI, • Prof.A.R.Phani, NanoRam MNRE 5th Aug 2014 (CFCT ARCI)

  23. Major Equipments procured TGA with MS, Sieverts apparatus and ASAP MNRE 5th Aug 2014 (CFCT ARCI)

  24. Before Carbonization After Carbonization Lemon Outer Activated carbons from different precursors MNRE 5th Aug 2014 (CFCT ARCI)

  25. Characterisation and hydrogen absorption studies MNRE 5th Aug 2014 (CFCT ARCI)

  26. Schematic of Hydrogen storage Apparatus Part -2 Part - 1 • Manifold Pressure Gauge (0-150 bar) • H2 gas inlet • 3. Vacuum pump • 4. Connecting channel • 5. Reaction Chamber • 6. Vent • 7. RC pressure Gauge (0-25 bar) 1 7 P Man. V Man P RC. (V RC + Vman+ Vtub- Vsam ) 6 ∆nH2 = Z (PMan,T) R. TMan Z (PRC,T) R. TRC 2 5 The total amount of hydrogen adsorbed by the sample can be : 3 4 MNRE 5th Aug 2014 (CFCT ARCI)

  27. Hydrogen storage capacity for corn cob , Jute , TSC, Cotton MNRE 5th Aug 2014 (CFCT ARCI)

  28. Hydrogen storage datalog of Cotton-800-2hr MNRE 5th Aug 2014 (CFCT ARCI)

  29. Consolidated data of all the samples at RT and at 40 bar MNRE 5th Aug 2014 (CFCT ARCI)

  30. PUBLICATIONS Publications • Vinayan B P., Rupali Nagar, K. Sethupathi and S. Ramaprabhu, The Journal of Physical Chemistry C, 115, 15679, (2011). • Vinayan B P, K. Sethupathi and S. Ramaprabhu, Transactions of the Indian Institute of Metals, 64, 169, (2011). • Vinayan B P, K.Sethupathi and S.Ramaprabhu, Journal of Nanoscience and Nanotechnology, 12, 1, (2012) • Vinayan B P, Rupali Nagar, and S. Ramaprabhu, Langmuir,  28,7826, (2012). • Transition metal - graphene based hydrogen storage nanomaterial (Indian patent) filed (2012). • Chemically modified- carbon based hydrogen storage material (patent) to be filed (2014).

  31. Publications/ Paper 1. Activated carbons derived from Tamarind seeds- T.Rameshkumar, N.Rajalakshmi and K.S.Dhathathreyan, Communicated (2013) 2. Pt loaded on carbon derived from corn cobs for hydrogen storage - R.Karthikeyan, N.Rajalakshmi and K.S.Dhathathreyan Communicated (2013) 3. . Jute fibres based activated carbons for Hydrogen storage , M. Vivekanandan, T.Rameshkumar, N.Rajalakshmi and K.S.Dhathathreyan - Communicated (2013) 4. Carbon from Cotton as hydrogen storage medium– T.Rameshkumar, N.Rajalakshmi and K.S.Dhathathreyan In preparation (2014) 5. Hydrogen storage from composites based on Mg and activated carbon derived from tamarind seeds(2014). Conferences: 6. T.Ramesh, G.Subashini, N.Rajalakshmi and K .S.Dhathathreyan , Activated Carbon from Tamarind Seeds- Promising Hydrogen storage material , Paper presented at the National conference on Advanced materials , NCAMA-2013 at NIT, Trichy during 4th and 5th April 2013

  32. Boron substituted carbon materials and hydrogen absorption capacity for comparison purpose ( by another independent group)

  33. IIT Entrance THANK YOU FOR YOUR KIND ATTENTION NCCR IIT Research Park NCCR

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