A differential thermal analysis (DTA) method has been developed that identifies and distinguishes surface and internal (volume) crystallization in glasses. This method is fast, convenient, and requires only a small quantity of sample, ∼500 mg, to identify the dominant crystallization, surface versus internal, in the glass. In this method, either the maximum height of the DTA crystallization peak, (δT”)p, or the ratio T2p/(ΔT)p, where Tp is the temperature at (δT)p and (ΔT)p the peak half width, is plotted as a function of particle size. The composition of the glasses that have been investigated in the present work include (in mol%) 33.3BaO 66.7SiO2 (BS2), 20Na2O‐80TeO2 (NT4), 22.2PbOll.lNb2O5 66.7TeO2 (PNT), 66.7PbO10.0Bi2O3‐23.3Ga2O3 (PBG), and xLi2O(100 ‐ x)SiO2 (lithium silicate, x = 33.3, 35, 37, and 40 mol%). Both (δT)p and T2p/(ΔT)p decrease with increasing particle size when surface crystallization is the dominant mechanism and increase when internal crystallization becomes predominant. The surface and internal crystallization have been identified by crystallizing the glasses at temperatures, as determined by DTA, and then examining the microstructure by scanning electron microscopy. The temperature at the crystallization peak maximum, Tp, shows no dependence on the crystallization mechanism (surface versus internal) and increases with increasing particle size for all the preceding glasses.
A novel calcium phosphate silicate bone cement (CPSC) was synthesized in a process, in which nanocomposite forms in situ between calcium silicate hydrate (C-S-H) gel and hydroxyapatite (HAP). The cement powder consists of tricalcium silicate (C(3)S) and calcium phosphate monobasic (CPM). During cement setting, C(3)S hydrates to produce C-S-H and calcium hydroxide (CH); CPM reacts with the CH to precipitate HAP in situ within C-S-H. This process, largely removing CH from the set cement, enhances its biocompatibility and bioactivity. The testing results of cell culture confirmed that the biocompatibility of CPSC was improved as compared to pure C(3)S. The results of XRD and SEM characterizations showed that CPSC paste induced formation of HAP layer after immersion in simulated body fluid for 7 days, suggesting that CPSC was bioactive in vitro. CPSC cement, which has good biocompatibility and low/no cytotoxicity, could be a promising candidate as biomedical cement.
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