Structural Aspects of the Dehydration and Dehydroxylation of gamma-Titanium Phosphate, gamma-Ti(PO(4))(H(2)PO(4)).2H(2)O.
The thermal transformations of gamma-titanium phosphate, gamma-Ti(PO(4))(H(2)PO(4)).2H(2)O, have been studied using thermogravimetric analysis, differential scanning calorimetry, X-ray powder diffraction, and temperature-resolved in-situ powder diffraction. The transformation sequence goes from gamma-Ti(PO(4))(H(2)PO(4)).2H(2)O over a new partially dehydrated form gamma'-Ti(PO(4))(H(2)PO(4)).(2-x)H(2)O (x approximately 1) to the anhydrous form beta-Ti(PO(4))(H(2)PO(4)) and then through a two-step condensation process where layered titanium pyrophosphate, Ti(PO(4))(H(2)P(2)O(7))(0.5), is formed first and finally cubic titanium pyrophosphate TiP(2)O(7). The dehydration of gamma-Ti(PO(4))(H(2)PO(4)).2H(2)O and the dehydroxylation/condensation process from beta-Ti(PO(4))(H(2)PO(4)) to layered titanium pyrophosphate,Ti(PO(4))(H(2)P(2)O(7))(0.5), was followed in-situ. A new partially dehydrated phase, gamma'-Ti(PO(4))(H(2)PO(4)).(2-x)H(2)O (x approximately 1), which forms at approximately 50 degrees C has been detected and characterized. The unit cell is monoclinic with the lattice parameters a = 23.670(1) Å, b = 6.264(1) Å, c = 5.036(1) Å, beta = 102.41(1) degrees, and Z = 4. Layered titanium pyrophosphate, Ti(PO(4))(H(2)P(2)O(7))(0.5), which forms at 375 degrees C has been characterized. The unit cell is monoclinic with lattice parameters a = 16.271(3) Å, b = 6.319(1) Å, c = 5.122(1) Å, beta = 90.59(2) degrees, and Z = 4.
Krogh Andersen
Anne Marie
AM
Department of Chemistry, SUNY at Stony Brook, Stony Brook, New York 11794.
Norby
Poul
P