Two new vanadyl pyrophosphate precursors were produced in a single ste
p operation using a counterflow diffusion flame burner. The technique
consists of adding a vanadium and a phosphorus halide to the fuel stre
am of hydrogen-oxygen flames. Particles nucleate and grow in the flame
to an average diameter between 5 and 30 nm. Upon exiting the flame, p
owders are collected on two stainless steel strips and their crystalli
ne structures are analyzed by x-ray diffraction and Fourier-transform
infrared spectroscopy. A strong effect of flame temperature on the cry
stalline structure of the powders produced is observed. When a high te
mperature flame is used, the powder collected is a mixture of VOPO4 .
2H(2)O and (VOPO4)(1-x)(VOHPO4)(x) . 2.6H(2)O. This mixture forms gamm
a-VOPO4 upon subsequent reheating at 750 degrees C in a oxidizing atmo
sphere, and transforms into (VO)(2)P2O7 in an oxygen-free atmosphere a
t 700 degrees C. When a lower temperature flame is used, the powder co
llected is (VOPO4)(1-x)(VOHPO4)(x) . 2.9H(2)O, which transforms at 750
degrees C into beta-VOPO4 in an oxidizing atmosphere and to (VO)(2)P2
O7 at 700 degrees C in an oxygen-free atmosphere. Structural differenc
es between the two vanadyl pyrophosphates are observed. These differen
ces are discussed in terms of the ability of (VO)(2)P2O7 to accommodat
e various disordered and polytypic structures. (C) 1996 Academic Press
, Inc.