β-tricalcium bis(orthophosphate) [Ca
3(PO
4)
2] (β-TCP) was mechanochemically treated with a mortar grinder in three different atmospheres of air, wet N
2, and wet CO
2. H
2O and CO
32- were incorporated into ground β-TCP, the amount of which depended on both the grinding time and the atmosphere. As the grinding time of β-TCP increased, it hydrolyzed easily to Ca-deficient hydroxyapatite. The apatite-formation ratio for β-TCP ground in wet CO
2 was remarkably lower than that for β-TCP ground in air or wet N
2. The role of H
2O and CO
32- in the hydrolysis of ground β-TCP was investigated by calorimetry together with spectroscopy. In calorimetry for each ground β-TCP, a strong exothermic band was observed, which was followed by a broad exothermic band. It is considered that the first band corresponds to the process of adsorption of H
2O in the solvent onto the fresh surface of ground β-TCP and the second broad band corresponds to the apatite-formation process. With increasing amount of H
2O incorporated into ground β-TCP, both the heat evolution of the first exothermic band and the apatite-formation ratio increased linearly. The H
2O incorporated into ground β-TCP promotes the dissolution of β-TCP and apatite formation. In terms of the effect of the incorporated CO
32- on hydrolysis, the incorporated CO
32- prevents not only apatite formation but also the dissolution of β-TCP.
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