Study of Negative Thermal Expansion and Shift in Phase Transition Temperature in Ti 4+ - and Sn 4+ -Substituted ZrW 2 O 8 Materials Klaartje De Buysser,* Isabel Van Driessche, ² Bart Vande Putte, Paul Vanhee, Joseph Schaubroeck, and Serge Hoste ² Department of Inorganic and Physical Chemistry, Building S3 Ghent UniVersity Krijgslaan 281, 9000 Ghent, Belgium, and Faculty of Applied Engineering Sciences, UniVersity College Ghent, Schoonmeersstraat 52, 9000 Ghent, Belgium Received August 23, 2007 The negative-thermal-expansion material ZrW 2 O 8 is known to undergo an order-disorder phase transition which affects its expansion behavior. In this study, Ti 4+ and Sn 4+ are examined as possible substituting ions for the Zr 4+ position in ZrW 2 O 8 . This substitution leads to a decrease in cell parameters, as the ionic radii of the substituents are smaller than the Zr 4+ ionic radius. A remarkable decrease in transition temperature is noticed. DSC is used to quantify the enthalpy and entropy changes during the phase transition in order to reveal the mechanisms behind this decrease. It is shown that the strength of the M-O bond plays an important role, as it is a partner in the rigid unit mode motion and the order-disorder transition mechanism. Introduction ZrW 2 O 8 is known as an isotropic negative-thermal- expansion material in its entire kinetic stability range (-273 to 825 °C). 1 This behavior is in contrast with the asymmetry of the vibrational potential well which leads to positive thermal expansion in most solid materials. Contraction upon heating is not exceptional among solids, as it can be seen for example in tetrahedrally bonded crystals at low temper- ature and -quartz at high temperatures. 2,3 ZrW 2 O 8 is formed by corner-linked ZrO 6 and WO 4 polyhedra which are connected by two-fold-coordinated oxygen atoms. In the WO 4 tetrahedra, one oxygen atom remains singly coordinated. The polyhedra are arranged in an open-framework structure. RUMs, or rigid unit modes, can occur within these polyhedra. These are low-energy vibrations of the polyhedra without distortion of the intra- hedral bond distances or angles. These RUMs have been associated with a possible mechanism behind the large nega- tive thermal expansion behavior exhibited by the ZrW 2 O 8 crystal structure. 4-10 The isotropy of the thermal expansion is caused by the cubic crystal structure of R-ZrW 2 O 8 (P2 1 3) with WO 4 tetrahedra aligned along the [111] axis. ZrW 2 O 8 undergoes an order-disorder transition at 150-160 °C from cubic R to cubic (Pa3 h). The direction in which the WO 4 tetrahedra point becomes dynamically disordered in the high-temper- ature phase. The phase transition also affects the thermal expansion coefficient, but the negative thermal expansion is maintained: R-phase )-10 × 10 -6 °C -1 and -phase ) -4 × 10 -6 °C -1 . 11 The use of ZrW 2 O 8 to tailor the thermal expansion of composite materials is described in the literature. 12-22 * To whom correspondence should be addressed. E-mail: Klaartje.DeBuysser@Ugent.be. ² Ghent University Krijgslaan. University College Ghent. (1) Evans, J. S. O.; Mary, T. A.; Vogt, T.; Subramanian, M. A.; Sleight, A. W. Chem. Mater. 1996, 8, 2809. (2) Taylor, R. E. In Data series on material properties, 1st ed.; Ho, Y., Ed.; ASM International: Materials Park, OH, 1998. (3) Callister, W. D. XXXXX, 5th ed.; Anderson, W., Ed.; Wiley and Sons: Danvers, 2000; p 661. (4) Barrera, G. D.; Bruno, J. A. O.; Barron, T. H. K.; Allan, N. L. J. Phys.-Condens. Mat. 2005, 17, R217. (5) Evans, J. S. O.; David, W. I. F.; Sleight, A. W. Acta Crystallogr. B 1999, 55, 333. (6) Gallardo-Amores, J. M.; Amador, U.; Moran, E.; Alario-Franco, M. A. Int. J. Inorg. Mater. 2000, 2, 123. (7) Noailles, L. D.; Peng, H. H.; Starkovich, J.; Dunn, B. Chem. Mater. 2004, 16, 1252. (8) Sleight, A. W. Inorg. Chem. 1998, 37, 2854. (9) Allen, S.; Ward, R. J.; Hampson, M. R.; Gover, R. K. B.; Evans, J. S. O. Acta Crystallogr. B 2004, 60, 32. (10) Tao, J. Z.; Sleight, A. W. J. Solid State Chem. 2003, 173, 442. (11) Mary, T. A.; Evans, J. S. O.; Vogt, T.; Sleight, A. W. Science 1996, 272, 90. (12) Kofteros, M.; Rodriguez, S.; Tandon, V.; Murr, L. E. Scripta Mater. 2001, 45, 369. (13) Yilmaz, S.; Dunand, D. C. Compos. Sci. Technol. 2004, 64, 1895. Inorg. Chem. 2008, 47, 736-741 736 Inorganic Chemistry, Vol. 47, No. 2, 2008 10.1021/ic701660w CCC: $40.75 © 2008 American Chemical Society Published on Web 12/21/2007