TY - JOUR
T1 - Synthesis of zirconium titanate with an ordered M-fergusonite (beta) structure
AU - Troitzsch, Ulrike
AU - Christy, Andrew G.
AU - Ellis, David J.
PY - 2007/10
Y1 - 2007/10
N2 - We report a new zirconium titanate compound (Zr,Ti)O2 with 27.5-35 mol% titania (TiO2) formed from the oxides at 35-38 kbar, 1400-1500 °C. Crystal structure investigations at atmospheric conditions with powder X-ray diffraction (XRD) and transmission electron microscopy (TEM) revealed a monoclinic structure related to that of M-fergusonite (beta). Unit-cell dimensions (from 27.5 to 35 mol% TiO2): a=7.267(20)-7.340(2) Å, b=10.435(3)-10.429(1) Å, c=5.023(11)-5.040(1) Å, β=136.45(12)-137.55(1)°, V=262.44(92)-260.40(12) Å3, Z=4. Rietveld refinement (RF=1.55) of a sample with 32.8 mol% TiO2 indicates that site A is 8-fold coordinated, mostly occupied by Zr, while site B has 6-fold average coordination, occupied by Ti and Zr. Site B is at least partly ordered, as indicated by superstructure reflections 0 0 1 and -2 0 1 detected with TEM, reducing the space group from C2/c to C2. Pronounced streaking of selected diffraction spots is linked to the boundaries of lamellar domains in twin orientation, with twin planes either (200) or (20-2). Adjacent lamellae differ slightly in composition, causing subtle asymmetry of the twin diffraction patterns.
AB - We report a new zirconium titanate compound (Zr,Ti)O2 with 27.5-35 mol% titania (TiO2) formed from the oxides at 35-38 kbar, 1400-1500 °C. Crystal structure investigations at atmospheric conditions with powder X-ray diffraction (XRD) and transmission electron microscopy (TEM) revealed a monoclinic structure related to that of M-fergusonite (beta). Unit-cell dimensions (from 27.5 to 35 mol% TiO2): a=7.267(20)-7.340(2) Å, b=10.435(3)-10.429(1) Å, c=5.023(11)-5.040(1) Å, β=136.45(12)-137.55(1)°, V=262.44(92)-260.40(12) Å3, Z=4. Rietveld refinement (RF=1.55) of a sample with 32.8 mol% TiO2 indicates that site A is 8-fold coordinated, mostly occupied by Zr, while site B has 6-fold average coordination, occupied by Ti and Zr. Site B is at least partly ordered, as indicated by superstructure reflections 0 0 1 and -2 0 1 detected with TEM, reducing the space group from C2/c to C2. Pronounced streaking of selected diffraction spots is linked to the boundaries of lamellar domains in twin orientation, with twin planes either (200) or (20-2). Adjacent lamellae differ slightly in composition, causing subtle asymmetry of the twin diffraction patterns.
KW - Crystal structure
KW - Fergusonite
KW - Ordering
KW - Twinning
KW - Zirconium titanate
UR - http://www.scopus.com/inward/record.url?scp=35248862499&partnerID=8YFLogxK
U2 - 10.1016/j.jssc.2007.08.020
DO - 10.1016/j.jssc.2007.08.020
M3 - Article
SN - 0022-4596
VL - 180
SP - 2885
EP - 2895
JO - Journal of Solid State Chemistry
JF - Journal of Solid State Chemistry
IS - 10
ER -