Journal
SYNTHETIC METALS
Volume 161, Issue 11-12, Pages 996-1000Publisher
ELSEVIER SCIENCE SA
DOI: 10.1016/j.synthmet.2011.03.006
Keywords
Charge transfer salt; Molecular conductors; Tetrathiafulvalene-chloranil; Polymorphism; Mechanochemistry; X-ray powder diffraction
Funding
- US D.O.E., Office of Science, Office of Basic Energy Sciences [DE-AC02-98CH10886]
- NSF [PHY-0755262]
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This work describes the synthesis of the green and black polymorphic forms of the tetrathiafulvalene-chloranil (TTF-CA) charge transfer salt as pure phases, by solvent-assisted mechanochemistry. Both materials were characterized using laboratory and high-resolution X-ray powder diffraction (XRPD), elemental analysis and scanning electron microscopy (SEM). The high-resolution XRPD pattern of the TTF-CA black polymorph was indexed with a triclinic lattice a = 10.756(5)angstrom, b = 11.057(4)angstrom, c = 6.614(2)angstrom, alpha = 101.36(2)degrees, beta = 93.69(3)degrees, gamma = 89.37(3)degrees, V = 769.6(5) angstrom(3). The chemical stability of these phases upon heating was investigated using thermogravimetric analysis (TGA), elemental analysis and X-ray powder diffraction (XRPD), indicating that both polymorphs undergo chemical decomposition, and ruling out the transition to an air-stable high temperature polymorph. (C) 2011 Elsevier B.V. All rights reserved.
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