HIGH TEMPERATURE PRESSURE PROCESSING OF MIXED ALANATE COMPOUNDS Page: 4 of 14
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Molten state processing (MSP), an SRNL patented technique, was used to heat ball
milled mixtures under high hydrogen gas pressure (usually 4500 psi) in order to
synthesize possible new phases.[12, 13] The premise is that the high H2 pressure will
favor the formation of products with high hydrogen content, following Le Chatelier's
principle. Vanadium forms hydrides rather easily, so vanadium powder was heated under
vacuum/hydrogen cycles to create VHo si for use in these experiments.[14]
3. Results and Discussion
Table 1 provides a comprehensive list of the various mixtures that were
investigated in this study. The mixtures we have explored include NaAlH4, LiAlH4,
MgH2 and Mg2NiH4 as the primary materials, with addition of alkali(ne) hydrides, and/or
early third row transition metals (V, Cr, Mn) and occasionally TiCl3. The metals Cr and
Mn were chosen because they do not easily form hydrides under the conditions of our
experiment, so the effect of a transition metal in "metal" form could be examined.
Vanadium, immediately to the left of Cr on the periodic table, does form a hydride so
VHo.gi was used to explore the difference in chemical reactions of a transition metal
versus a transition metal hydride additive. Experimental parameters such as
stoichiometry, temperature of ball milling, use of hand milling, and temperature of MSP
were varied to study the effects of these parameters on the products. Starting materials
are abbreviated SM for brevity in the table, and this indicates that all of the starting
materials are seen in the XRD pattern of the indicated reaction step.
3a. Mixtures of alanates and transition metals:
Mixtures with Cr metal:
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Berseth, P; Ragaiy Zidan, R; Donald Anton, D; Kirk Shanahan, K & Ashley Stowe, A. HIGH TEMPERATURE PRESSURE PROCESSING OF MIXED ALANATE COMPOUNDS, article, June 7, 2007; [Aiken, South Carolina]. (https://digital.library.unt.edu/ark:/67531/metadc889040/m1/4/: accessed April 17, 2024), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; crediting UNT Libraries Government Documents Department.