Calcium phosphate ceramics have been used successfully as synthetic bone substitutes in orthopedics, dentistry, and maxillofacial surgery. One way of preparing these ceramics is the sintering of a calcium-deficient hydroxyapatite (CDHA), which can be obtained in different ways. Mechanochemistry is one possible means of synthesizing CDHA, with an expected molar calcium-to-phosphate (Ca/P) ratio +/- 0.005. The grinding can be carried out under dry or wet conditions. To optimize the experimental conditions of CDHA preparation by dry mechanosynthesis and for a better understanding of the DCPD/CaO mechanochemical reaction, we performed a kinetic study in which some of the experimental parameters were varied. Carried out with two different vertical rotating ball mills, this kinetic study showed that (1) experiments are reproducible and give as a final product a hydroxyapatite powder, formed of nano-sized crystals of around 20 nm, with a controlled Ca/P ratio; (2) the time for complete disappearance of DCPD and the time for complete reaction are in direct proportion to the mass of the ground powder; but (3) the time for complete disappearance of DCPD is independent of the Ca/P ratio while the time for complete reaction increases exponentially with the Ca/P ratio; and (4) the time for complete disappearance of DCPD corresponds to the time for complete reaction solely for Ca/P = 1.5. These observations suggest a reaction mechanism in two well differentiated stages: (First stage) CaO reacts with DCPD to give first an amorphous calcium phosphate (ACP) with a low Ca/P ratio that transforms into CDHA when its Ca/P ratio reaches 1.5. At the same time, CaO is hydrated into Ca(OH)(2) by the water produced by the reaction. (Second stage) If the Ca/P > 1.5 in the initial mixture, the excess Ca(OH)(2) is added to CDHA 1.5 by reacting with the HPO(4) group of CDHA until its Ca/P ratio reaches the expected value. The slower the reaction, the higher the Ca/P in the initial mixture.
By mixing CaHPO(4) x 2H(2)O (DCPD) and CaO with water or sodium phosphate buffers as liquid phase, a calcium phosphate cement was obtained. Its physical and mechanical properties, such as compressive strength, initial and final setting times, cohesion time, dough time, swelling time, dimensional and thermal behavior, and injectability were investigated by varying different parameters such as liquid to powder (L/P) ratio (0.35-0.7 ml g(-1)), molar calcium to phosphate (Ca/P) ratio (1.67-2.5) and the pH (4, 7, and 9) and the concentration (0-1 M) of the sodium phosphate buffer. The best results were obtained with the pH 7 sodium phosphate buffer at the concentration of 0.75 M. With this liquid phase, physical and mechanical properties depended on the Ca/P and L/P ratios, varying from 3 to 11 MPa (compressive strength), 6 to 10 min (initial setting time), 11 to 15 min (final setting time), 15 to 30 min (swelling time), 7 to 20 min (time of 100% injectability). The dough or working time was over 16 min. This cement expanded during its setting (1.2-5 % according to Ca/P and L/P ratios); this would allow a tight filling. Given the mechanical and rheological properties of this new DCPD/CaO-based cement, its use as root canal sealing material can be considered as classical calcium hydroxide or ZnO/eugenol-based pastes, without or with a gutta-percha point.
Hydraulic calcium phosphate cements (CPCs) that are used as osseous substitutes, set by an acid-base reaction between an acid calcium phosphate and a basic calcium salt (often a phosphate). In order to gain a better understanding of the setting of the monocalcium phosphate monohydrate-calcium oxide cement that we developed and in the aim to improve its mechanical properties, the setting reaction was studied by pH-metry. The two methods described in the literature were used. In the first, cement samples were prepared then crushed after different storage periods at 37 degrees C, 100% RH. The powder was then immersed in pure water with stirring and the pH was measured after equilibration. In the second technique, the starting materials were poured into water while stirring and the pH were followed over time. The two methods gave different results. The first procedure provided information concerning the pH of the surrounding liquid following the partial dissolution of the cement components, rather than any information about pH changes during setting. The second method is more appropriate to follow the pH variations during setting. In this second procedure, the effects of different parameters such as crushing time, stirring rate, liquid-to-powder (L/P) ratio and temperature were investigated. These parameters may impact substantially on the shape and position of the pH=f(t) curves. One or three pH jumps were observed during the setting depending on the composition of the liquid phase. The time at which these pH jumps occurred depended on the pH of the liquid phase, the concentration of the buffer, the crushing of starting materials, the L/P ratio and the temperature. Good linear correlations were obtained (i) between the time of the pH jumps and the L/P ratio and the temperature and (ii) between the time of the first pH jump and the compressive strength and the final setting time of the cements prepared with different liquid phases. It may be assumed in view of these correlations that the results obtained in dilute solution may be extrapolated to the conditions of cement sample preparation and that the mechanical properties of the cement are directly related to the phenomena that occur at the first pH jump which corresponds to precipitation of dicalcium phosphate dihydrate.
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