Dehydration of Ca3Al2(SiO4)y(OH)4(3-y) (0<y<0.176) studied by neutron thermodiffractometry

Hydrogarnet (Ca12Al2(OH)(12)) and katoite of composition Ca3Al2(SiO4)(0.176)(OH)(11.3) were obtained by hydration of tricalcium aluminium oxide, and for katoite synthesis, by addition of amorphous silica. The thermal dehydration was monitored in situ, by neutron thermodiffractometry, from room temperature to 700 degrees C at atmospheric pressure and at a heating rate of 2 degrees C/min. On heating, powder neutron diffraction patterns were collected every 300 s. Cell parameters were fitted by the Pawley method. Hydrogarnet decomposed to yield Ca12Al14O32 (OH)-mH(2)O and Ca(OH)(2) that eventually transformed to CaO. For katoite, phases of formula Ca12Al14-ySiyO32(O,OH)(1+y/2) related to mayenite were formed. Complementary annealing experiments, for 10 h, at higher temperatures and subsequent quenching lead to the formation of mayenite and traces of Ca3SiO5. Thermogravimetric curves were in agreement with the thermodiffractometry experiments. Also, neutron diffraction data allowed to measure thermal expansion coefficients, at atmospheric pressure, between 25 and 250 degrees C for hydrogarnet and katoite: 1.89 x 10(-5) +/- 0.09 and 1.63 x 10(-5) +/- 0.07 degrees C-1, respectively. (C) 2008 Published by Elsevier Ltd.