Co-grinding significance for calcium carbonate-calcium phosphate mixed cement. Part I: Effect of particle size and mixing on solid phase reactivity

In part I of this study we aim to evaluate and control the characteristics of the powders constituting the solid phase of a vaterite CaCO3-dicalcium phosphate dihydrate cement using a co-grinding process and to determine their impact on cement setting ability. An original methodology involving complementary analytical techniques was implemented to thoroughly investigate the grinding mechanism of separated or mixed reactive powders and the effects on solid phase reactivity. We showed that the association of both reactive powders during co-grinding improves the efficiency of this process in terms of the particle size decrease, thus making co-grinding adaptable to industrial development of the cement. For the first time the usefulness of horizontal attenuated total reflection Fourier transform infrared spectroscopy to follow the chemical setting reaction at 37 °C in real time has been demonstrated. We point out the antagonist effects that co-grinding can have on cement setting: the setting time is halved; however, progress of the chemical reaction involving dissolution-reprecipitation is delayed by 30 min, probably due to the increased contact area between the reactive powders, limiting their hydration. More generally, we can take advantage of the co-grinding process to control powder mixing, size and reactivity and this original analytical methodology to better understand its effect on the phenomena involved during powder processing and cement setting, which is decisive for the development of multi-component cements.