27Al and 1H Solid State NMR Studies Show Evidence of TiAl3 and TiH2 in Ti-doped NaAlH4

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Previous X-ray Diffraction (XRD) and Nuclear Magnetic Resonance (NMR) studies on Ti-doped NaAlH{sub 4} revealed the reaction products of two heavily doped (33.3 at.%) samples that were solvent-mixed and mechanically-milled. This investigation revealed that nano-crystalline or amorphous Al{sub 2}O{sub 3} forms from the possible coordination of aluminum with oxygen atom of the furan ring system from added tetrahydrofuran (THF) in the solvent-mixed sample, and that TiAl{sub 3} forms in mechanically-milled samples. The present paper provides a more sophisticated NMR investigation of the these materials. On heavily doped (33.3 at.%) solvent-mixed samples, {sup 27}Al Magic Angle Spinning (MAS) NMR {sup 27}Al … continued below

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Herberg, J; Maxwell, R & Majzoub, E May 26, 2005.

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Previous X-ray Diffraction (XRD) and Nuclear Magnetic Resonance (NMR) studies on Ti-doped NaAlH{sub 4} revealed the reaction products of two heavily doped (33.3 at.%) samples that were solvent-mixed and mechanically-milled. This investigation revealed that nano-crystalline or amorphous Al{sub 2}O{sub 3} forms from the possible coordination of aluminum with oxygen atom of the furan ring system from added tetrahydrofuran (THF) in the solvent-mixed sample, and that TiAl{sub 3} forms in mechanically-milled samples. The present paper provides a more sophisticated NMR investigation of the these materials. On heavily doped (33.3 at.%) solvent-mixed samples, {sup 27}Al Magic Angle Spinning (MAS) NMR {sup 27}Al multiple quantum MAS (MQMAS) indicates the presence of an oxide layer of Al{sub 2}O{sub 3} on the surfaces of potentially bulk nanocrystalline Ti, nanocrystalline TiAl{sub 3}, and/or metallic aluminum. The {sup 1}H MAS NMR data also indicate the possible coordination of aluminum with the oxygen atom in the THF. On heavily doped samples that were mechanically milled, {sup 27}Al MAS NMR and static NMR confirms the presence of TiAl{sub 3}. In addition, the {sup 1}H MAS NMR and {sup 1}H spin-lattice relaxation (T{sub 1}) measurements are consistent with the presence of TiH{sub 2}. These results are in agreement with recent XAFS measurements indicating both Al and H within the first few coordination shells of Ti in the doped alanate.

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  • Journal Name: Journal of Alloys and Compounds; Journal Volume: 417

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  • Report No.: UCRL-JRNL-212589
  • Grant Number: W-7405-ENG-48
  • Office of Scientific & Technical Information Report Number: 884770
  • Archival Resource Key: ark:/67531/metadc892002

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  • May 26, 2005

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Herberg, J; Maxwell, R & Majzoub, E. 27Al and 1H Solid State NMR Studies Show Evidence of TiAl3 and TiH2 in Ti-doped NaAlH4, article, May 26, 2005; Livermore, California. (https://digital.library.unt.edu/ark:/67531/metadc892002/: accessed April 27, 2025), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; crediting UNT Libraries Government Documents Department.

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