Aluminum Chloride as effective dopant in Amide-based systems
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1 Multifunctionality of metal hydrides for energy storage developments and perspectives 8 th -2 st September - Warsaw University of Technology - POLAND Aluminum Chloride as effective dopant in Amide-based systems Dr. Sebastiano Garroni
2 What is ICCRAM? Dr. Santiago Cuesta-Lopez 2
3 What is ICCRAM? 3
4 What is ICCRAM? 4
5 What is ICCRAM? 5
6 Materials for hydrogen storage Chen P. et al., Nature Reviews Materials, 6059 (206). 2 T.R. Jensen et al., Chem. Soc. Rev., 207,46, H. Wang, G. Wu, H. Cao, C. Pistidda, A.-L. Chaudhary, S. Garroni, M. Dornheim, and P. Chen, Adv. Energy Mater. 207, 7,
7 Materials for hydrogen storage: M-N-H LiNH 2 (s) + LiH(s) <-> Li 2 NH(s) + H 2 (g) Chen P, et al., Interaction of hydrogen with metal nitrides and imides. Nature 2002;420-42:
8 Materials for hydrogen storage: M-N-H Advantages: Good gravimetric capacity (6.5 wt. %) Good reversibility (Pressure < 5.0 MPa; Temperature ~ 300 C) Promising thermodynamic properties (calculated: kj/mol H 2 ; experimental: 66 kj/mol H 2 ) Disadvantages: Slow desorption kinetic Release of NH 3 Strategies: Particle size reduction by ball milling. Nanoconfinement Addition of Metal Halide LiNH 2 (s) + LiH(s) <-> Li 2 NH(s) + H 2 (g) Chen P, et al., Interaction of hydrogen with metal nitrides and imides. Nature 2002;420-42: Leng H, Wu Z, Duan W, Xia G, Li Z. Int J Hydrogen Energy 202;37:
9 Materials for hydrogen storage: M-N-H Advantages: Good gravimetric capacity (6.5 wt. %) Good reversibility (Pressure < 5.0 MPa; Temperature ~ 300 C) Promising thermodynamic properties (calculated: kj/mol H 2 ; experimental: 66 kj/mol H 2 ) Disadvantages: Slow desorption kinetic Release of NH 3 Strategies: Particle size reduction by ball milling. Nanoconfinement Addition of Metal Halide AlCl 3 LiNH 2 (s) + LiH(s) <-> Li 2 NH(s) + H 2 (g) Chen P, et al., Interaction of hydrogen with metal nitrides and imides. Nature 2002;420-42: Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,:
10 Effect of AlCl 3 on the LiNH 2 + LiH system 300 C, 0. bar H 2 Undoped 0.03 AlCl 3 -doped Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,:
11 Effect of AlCl 3 on the LiNH 2 + LiH system 0.03 AlCl 3 -doped Undoped 300 C, 7 bar H 2 Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,:
12 Effect of AlCl 3 on the LiNH 2 + LiH system 275 C, 0. bar H 2 Undoped 0.03 AlCl 3 -doped Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,:
13 Effect of AlCl 3 on the LiNH 2 + LiH system 275 C, 7 bar H AlCl 3 -doped Undoped Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,:
14 Cyclability DESORPTION 300 C 275 C 96% 84% 98% 96% 92% 79% 54% 28% cycle 4 cycle Undoped AlCl3-doped Undoped AlCl3-doped Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,:
15 Cyclability ABSORPTION 88% 300 C 275 C 99% 00% 89% 99% 00% 53% 4% cycle 4 cycle Undoped AlCl3-doped Undoped AlCl3-doped Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,:
16 Cyclability comparison with KF DESORPTION AlCl 3 KF 2 92% 67% 4 cycle Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,: Y.L. Teng et al., In J. Hydrogen Energy,206, 4,
17 Temperature, C Desorption temperatures other additives Maximum Desorption Peak Temperature AlCl 3 KF Fernandez Albanesi L, Arneodo Lorochette P, Gennari FC. Int J Hydrogen Energy 203;38,: Y.L. Teng et al., In J. Hydrogen Energy,206, 4, G. Wu et al., Progress in Natural Science: Materials International, 207, 27, 39. 7
18 2LiNH 2 (s) MgH 2 (s) system AlCl 3 KF 2 8
19 Mg(NH 2 ) 2 (s) 2LiH (s) system Mg(NH 2 ) 2 (s) 2LiH (s) AlCl 3 9
20 Structural Investigation LiNH 2 (s) +.6LiH(s) AlCl 3 Initial mixture: hand mix of the starting reagents Ball milled for 5 hours AlCl 3 KF 2 Annealing at different temperatures Goal: Which is the active phase? Characterization: XRD FT-IR MAS NMR Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
21 Structural Investigation: XRD LiNH 2 (s) +.6LiH(s) AlCl 3 AlCl 3 KF 2 Initial mixture Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
22 Structural Investigation: XRD LiNH 2 (s) +.6LiH(s) AlCl 3 AlCl 3 KF 2 Initial mixture Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
23 Structural Investigation: XRD LiNH 2 (s) +.6LiH(s) AlCl 3 AlCl 3 KF 2 After 5h ball milling Initial mixture Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
24 Structural Investigation: XRD LiNH 2 (s) +.6LiH(s) AlCl 3 FCC-type AlCl 3 KF 2 After 5h ball milling Initial mixture Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
25 Structural Investigation: FT-IR LiNH 2 (s) +.6LiH(s) AlCl 3 AlCl 3 KF 2 After 5h ball milling FCC-type Al-N-H N-H Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
26 Structural Investigation: MAS NMR LiNH 2 (s) +.6LiH(s) AlCl 3 KF AlCl AlCl AlCl 3 FCC-type After 5h ball milling Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,: Janot R, et al, Decomposition of LiAl(NH2)4 and reaction with LiH for a possible reversible hydrogen storage. J Phys Chem C 2007;:
27 Structural Investigation: MAS NMR LiNH 2 (s) +.6LiH(s) AlCl 3 KF AlCl AlCl AlCl 3 FCC-type After 5h ball milling 0 ppm Al-N-H species 2 Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,: Janot R, et al, Decomposition of LiAl(NH2)4 and reaction with LiH for a possible reversible hydrogen storage. J Phys Chem C 2007;:
28 Structural Investigation: Upon annealing - XRD LiNH 2 (s) +.6LiH(s) AlCl 3 AlCl 3 KF 2 50 C under 7 bar H 2 I2 3 Fm-3m Mixture as-milled 5h Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
29 Structural Investigation: Upon annealing - XRD LiNH 2 (s) +.6LiH(s) AlCl 3 AlCl 3 KF 2 50 C under 7 bar H 2 I2 3 a = Å Fm-3m a = Å Mixture as-milled 5h Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
30 Structural Investigation: Upon annealing - XRD AlCl Reaction 3 between LiNH KF 2 2 +LiCl 30
31 Structural Investigation: Upon annealing - XRD AlCl 3 KF 2 R C under 7 bar H 2 I C under 7 bar H 2 Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
32 LiNH AlCl 3 AlCl 3 KF 2 50 C under 7 bar H 2 Mixture as-milled 5h Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
33 LiNH AlCl 3 under 7 bar H 2 AlCl 3 KF 2 50 C 300 C + 0.5h 300 C + h 300 C + 2h Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
34 LiNH AlCl 3 Ball to powder ratio = : AlCl 3 KF 2 Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
35 LiNH AlCl 3 Ball to powder ratio = : 0.8 *0 4 hits AlCl 3 KF *0 4 hits 9000 hits 800 hits 300 hits Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
36 LiNH AlCl 3 Ball to powder ratio = : 0.8 *0 4 hits R R R C R C R C R AlCl 3 AlCl 3 KF *0 4 hits 9000 hits 800 hits 300 hits Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
37 LiNH AlCl 3 Ball to powder ratio = : R R R AlCl 3 KF 2 C R C R C R Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
38 LiNH AlCl 3 AlCl 3 60 sec BM t-linh KF 2 R-3 2 I2 3 Rhombohedral R-3, a = Å and c = 8.96 Å, 60.0 wt% Cubic, I2 3, a = Å, 25.0 wt% SAME PHASES OBSERVED UPON ANNEALING OF THE SOLID SOLUTION!!! Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
39 LiNH AlCl 3 AlCl 3 60 sec BM t-linh KF 2 R-3 2 I2 3 Rhombohedral R-3, a = Å and c = 8.96 Å, 60.0 wt% Cubic, I2 3, a = Å, 25.0 wt% Formation of the 2 new phases takes place in few seconds, suggesting the occurrence of a MSR!! Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
40 Mechanochemical reactions AlCl 3 KF 2 S.A. Humphry-Baker, S. Garroni, F. Delogu and C. Schuh, Nature Materials, 206, DOI: 0.038/NMAT
41 Mechanically induced self-propagating reaction, MSR Exothermic powder mixtures Activation period: size reduction, mixing, and defect formation AlCl 3 KF 2 The MSR (mechanically induced self-propagating reaction) is ignited when the powder reaches a well defined critical state. Once started, the reaction propagates through the powder charge as a combustion process. TiC, TiS, PbTe, PbS, CdSn, ZnSn, etc Laszlo Takacs, Progress in Materials Science 47 (2002)
42 MSR in the LiNH 2 +xalcl 3 Quartz vial AlCl 3 KF 2 Termocouple 42
43 MSR in the LiNH 2 +xalcl 3 Quartz vial AlCl 3 KF 2 43
44 MSR in the LiNH 2 +xalcl 3 AlCl 3 KF 2 44
45 MSR in the LiNH 2 +xalcl 3 AlCl 3 KF 2 Termocouple Rotation speed Mass of ball Amount of AlCl 3 45
46 MSR in the LiNH 2 +xalcl 3 MSR data vs milling rotation speed AlCl 3 KF 2 46
47 MSR in the LiNH 2 +xalcl 3 MSR data vs milling rotation speed AlCl 3 KF 2 47
48 No MSR MSR in the LiNH 2 +xalcl 3 MSR data vs milling sphere mass AlCl 3 KF 2 48
49 MSR in the LiNH 2 +xalcl 3 MSR data vs milling sphere mass AlCl 3 KF 2 No MSR! 49
50 No MSR! MSR in the LiNH 2 +xalcl 3 MSR data vs AlCl 3 content AlCl 3 KF
51 MSR in the LiNH 2 +xalcl 3 MSR data vs AlCl 3 content AlCl 3 KF 2 5
52 MSR in the LiNH 2 +xalcl 3 FT-IR: Gases AlCl 3 KF 2 52
53 MSR in the LiNH 2 +xalcl 3 FT-IR: Powders AlCl 3 KF 2 53
54 Conclusions AlCl 3 represents a good additive to improve the hydrogen sorption properties of the MNH 2 based systems Among the halide-baed AlCl 3 additives, AlCl KF 3 2 is one of the most performing The active phase is mainly composed by Li-Al-N-H-Cl Two new hydrogen phases have been discovered These phases can be obtained after a thermal annealing of the solid solution FCC produced by ball milling (5h) or In few seconds by MSR For the first time a MSR took place in complex hydride based systems 54
55 Conclusions Both the crystal structures of the new hydride phases are not solved AlCl 3 KF 2 No MSR reaction occurred with LiH. Why? Thermodanymic data about the new phases are still missing New opportunities in the synthesis of amide-based phases as hydrogen storage materials NaNH 2 + xalcl 3?, Mg(NH 2 ) 2 + xalcl 3?... 55
56 Acknowledgments Prof. Gabriele Mulas Prof. Stefano Enzo PhD stduent Nina Senes Lucia Pisano AlCl 3 KF 2 Prof. Fabiana Gennari Dr. Luisa Fernandez Dr. Nadia Gamba Dr. Guillermina Amica Cooperation project Italia-Argentina Development and optimization of materials for hydrogen storage based on Li-N-H systems. Superivsors: Sebastiano Garroni and Fabiana Gennari
57 Acknowledgments Prof. Gabriele Mulas Prof. Stefano Enzo Dr. Antonio Valentoni PhD stduent Nina Senes Lucia Pisano AlCl 3 KF 2 Prof. M.D. Barò Prof. S. Suryach Prof. Fabiana Gennari Dr. Luisa Fernandez Dr. Nadia Gamba Dr. Guillermina Amica Dr. Emilio Napolitano Dr. Claudio Psitidda PhD student Antonio Santoru Prof. Martin Dornheim Prof. Chiara Milanese Prof. Marini Dr. Alessandro Girella 57
58 Acknowledgments 58
59 Acknowledgments Thank you for your attention 59
60 Acknowledgments Thank you for your attention 60
61 Structural Investigation: Upon annealing MAS NMR 300 C under 7 bar H AlCl3 AlCl 3 KF AlCl 3 Fernandez Albanesi L, Garroni S., Arneodo Lorochette P, Nolis, P., Mulas G., Enzo S., Barò M.D., Gennari FC. Int J Hydrogen Energy 205;40,:
62 Materials for hydrogen storage 62
63 Improving hydrogen storage properties: catalysts Chen P, et al., Interaction of hydrogen with metal nitrides and imides. Nature 2002;420-42: Chen P. et al., Nature Reviews Materials, 6059 (206) 63
64 LiNH AlCl 3 Ball to powder ratio = 20: AlCl 3 KF 2 Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
65 LiNH AlCl 3 Ball to powder ratio = 20: AlCl 3 KF 2 Fernandez Albanesi L, Garroni S., G., Enzo S., Gennari FC. : Dalton Trans., 206, 45,
66 Incorporation of AlCl3 AlCl 3 KF 2 Li 2 NH (with the origin shifted by ¼, ¼, ¼) LiNH 2 LiNH 2 (with vacant lithium side showed in red) The ball milling of LiNH 2 with AlCl 3 easy creates Li +x NH 2-x amide-imide solid solutions David WIF, Jones MO, Gregory DH, Jewell CM, Johnson SR, Walton A, et al. A mechanism for non-stoichiometry in the lithium amide/lithium imide hydrogen storage reaction. J Am Chem Soc 2007;29:594e60. 66
67 Incorporation of AlCl3 AlCl 3 KF 2 Al 3+ Li 2 NH (with the origin shifted by ¼, ¼, ¼) LiNH 2 LiNH 2 (with vacant lithium side showed in red) The Al 3+ ions could replace sites normally reserved for Li + (in the cubic description, 50% are empty). David WIF, Jones MO, Gregory DH, Jewell CM, Johnson SR, Walton A, et al. A mechanism for non-stoichiometry in the lithium amide/lithium imide hydrogen storage reaction. J Am Chem Soc 2007;29:594e60. 67
68 Incorporation of AlCl3 AlCl 3 KF 2 Al 3+ Cl - Li 2 NH (with the origin shifted by ¼, ¼, ¼) LiNH 2 LiNH 2 (with vacant lithium side showed in red) To keep electro neutrality, the Cl ions could occupy the other empty sites David WIF, Jones MO, Gregory DH, Jewell CM, Johnson SR, Walton A, et al. A mechanism for non-stoichiometry in the lithium amide/lithium imide hydrogen storage reaction. J Am Chem Soc 2007;29:594e60. 68
69 SR-XPRD AlCl 3 KF 2 69
70 SR-XPRD AlCl 3 KF 2 70
71 SR-XPRD AlCl 3 KF 2 AlCl 3 :NH 3 2LiNH 2 + AlCl 3 AlCl 3 :NH 3 + Li 2 NH LiCl LiNH 2 + AlCl 3 LiCl + Al + H 2 /NH 3 (????) LiH + AlCl 3 LiCl + Al + H 2 (????) 7
72 SR-XPRD AlCl 3 KF 2 LiAlCl 4 LiCl + AlCl 3 LiAlCl 4 72
73 SR-XPRD AlCl 3 KF 2 73
74 SR-XPRD AlCl 3 KF 2 74
75 SR-XPRD AlCl 3 KF 2 75
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