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 °C at atmospheric pressure and at a heating rate of 2 °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)·mH2O 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 °C for hydrogarnet and katoite: 1.89 × 10−5 ± 0.09 and 1.63 × 10−5 ± 0.07 °C−1, respectively.This research was supported by MCYT under the projects MAT-2003-08331-CO2-01 and MAT2006-12749-C02-01-02. We thank ILL for beam time granted (experiment number 5-25-83) and Dr. J. Campo for his assistance in collecting ND data. We also thank to Dr. D. Sheptyakov for experimental assistance in collecting the neutron diffraction data at SINQ (experiment number II/02 S-18).Peer reviewe