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Doping of brushite cements with metal ions can entail many positive effects on biological and physicochemical properties. Cu2+ ions are known to exhibit antibacterial properties and can additionally have different positive effects on cells as trace elements, whereas high Cu2+ concentrations are cytotoxic. For therapeutical applications of bone cement, a combination of good biocompatibility and sufficient mechanical properties is required. Therefore, the aim of this study was to investigate different physicochemical and biological aspects, relevant for application, of a brushite cement with Cu2+‐doped β‐tricalcium phosphate, monocalcium phosphate monohydrate and phytic acid as setting retarder. Additionally, the ion release was compared with a cement with citric acid as setting retarder. The investigated cements showed good injectability coefficients, as well as compressive strength values sufficient for application. Furthermore, no antibacterial effects were detected irrespective of the Cu2+ concentration or the bacterial strain. The cell experiments with eluate samples showed that the viability of MC3T3‐E1 cells tended to decrease with increasing Cu2+ concentration in the cement. It is suggested that these biological responses are caused by the difference in the Cu2+ release from the hardened cement depending on the solvent medium. Furthermore, the cements showed a steady release of Cu2+ ions to a lesser extent in comparison with a cement with citric acid as setting retarder, where a burst release of Cu2+ was observed. In conclusion, despite the anticipated antibacterial effect of Cu2+‐doped cements was lacking and mammalian cell viability was slightly affected, Cu2+‐concentrations maintained the physicochemical properties as well as the compressive strength of cements and the slow ion release from cements produced with phytic acid is considered advantageous compared to citric acid‐based formulations. [ABSTRACT FROM AUTHOR]

It was analysed how a low Na5P3O10 (STPP) concentration influences the hydration of a calcium aluminate cement. It is known that the hydration of a CAC‐Calcite system precipitates C2AHX as a precursor phase at 23°C during hydration before the formation of hemi‐ or monocarbonate and the additional formation of CAH10 and AH3. In our study the addition of 0.2 and 1.0 wt.% STPP (bwoc) to a CAC‐Calcite system at 23 °C and with a w/b of 0.33 was investigated and is compared with mixes without STPP addition. Heat flow calorimetry data showed that STPP accelerates the main reaction. Moreover, an additional heat flow event within the first 30 minutes was detected by STPP addition. However, from the results of QXRD analysis, crystalline hydrate phases are formed only during the main reaction. These are CAH10, C2AHX, AH3, hemicarbonate and monocarbonate. STPP shows an influence on the amount of crystalline C2AHX, otherwise, no difference in the qualitative phase content is observed. Gillmore‐Needle‐Testing (IMETER device) could observe an accelerated hardness development during the early heat flow event despite initially reduced viscosity. Pore water studies and thermodynamic modelling (PhreeqC) indicate the formation of an amorphous C‐P‐H phase during this early heat flow event. [ABSTRACT FROM AUTHOR]

The influence of water loss during the hydration of calcium aluminates on the phase development is investigated at 60°C. This is relevant for applications in which calcium aluminate cement (CAC) based formulations are exposed to quick drying during hydration. The presented results provide new insights into the well‐known conversion processes occurring in CAC pastes. Using in situ XRD two different routes of the development of initially formed C2AH8 are determined: (a) transformation to C3AH6 + AH3 in the presence of sufficient free water and (b) dehydration to C2AH5 at a lack of free water. Moreover, the influence of precuring of the pastes at 23°C before heating to 60°C is investigated. The increasing loss of free water with increasing precuring time resulting from both, precipitation of hydrate phases and evaporation, causes incomplete hydration of CA or CA2 as well as dehydration of C2AH8 instead of conversion into C3AH6. Comparative investigations of sealed samples always revealed complete hydration of CA and CA2 as well as complete conversion of C2AH8. [ABSTRACT FROM AUTHOR]

C3S and CA are the main phases of OPC and Fe‐rich CAC, respectively. The objective of this research was to investigate the influence of CA on C3S hydration, representing an under sulfated OPC‐rich binder, and to shed light on the underlying hydration mechanisms. To this end, C3S was blended with 1‐30 wt‐% CA and the pastes (w/c 0.5) were investigated by heat flow calorimetry, in situ X‐ray diffraction and analysis of the pore solution chemistry. CA additions ≥5 wt‐% reveal a separation into three distinct heat flow maxima, whereas additions ≤3 wt‐% just retard the start of the main reaction. The silicate reaction (dissolution of C3S and precipitation of C–S–H with or without CH) can be retarded for 4 to ≥22 hours in comparison to pure C3S depending on the admixed CA content. The start of the silicate reaction seems to be related to a decrease in Al‐ and increase in Ca‐concentration in the pore solution. However, it can be shown in this study that C3S is able to dissolve even at high Al concentrations in the pore solution. [ABSTRACT FROM AUTHOR]

Abstract: This study was performed to understand the influence of a critical amount of CA on the kinetics of C3S hydration. For this purpose, monoclinic C3S was blended with 15 wt.% CA and investigated by heat flow calorimetry and in situ XRD at 23°C at a water to cement ratio of 0.5. The binary mixture shows 3 distinct heat flow maxima where the underlying C3S dissolution is proceeding stepwise. The C3S dissolution rates during the 3 steps are varying strongly, depending on the hydrate phase precipitated during the respective reaction step. Comparison of these dissolution rates with a pure C3S reference sample allows the conclusion that the dissolution rate of pure C3S after the heat flow maximum might be governed by either the remaining available reactive surface of C3S or a diffusion‐controlled process, which would both be influenced by the respective hydrate phase precipitating on the C3S surface. [ABSTRACT FROM AUTHOR]

Hydration of partially amorphized α-TCP powders with Sr2+ concentrations ranging from 0 to 10 mol% substitution for Ca2+ was analyzed by isothermal calorimetry and quantitative in-situ XRD. Hydration of both crystalline α-TCP and amorphous TCP (ATCP) forming CDHA was retarded to an increasing extent with increasing Sr2+ content. Sr2+ slightly reduced the crystallite size (XRD coherent scattering domains) of the CDHA formed during hydration, while the size of crystals visible under SEM was not noticeably affected. Reaction enthalpies of Δ HR(Sr-α-TCP→Sr-CDHA) = 122 ± 8 J/gTCP and Δ HR(Sr-ATCP→Sr-CDHA) = 257 ± 8 J/gTCP were determined for the hydration of crystalline α-TCP and ATCP containing 5 mol% Sr2+ substitution for Ca2+. This is comparable with the corresponding reaction enthalpies previously obtained for undoped samples, which are 106 ± 7 J/gTCP for α-TCP and 250 ± 7 J/gTCP for ATCP. [ABSTRACT FROM AUTHOR]

An in situ framework for 1 H time-domain nuclear magnetic resonance analysis was developed and applied on alite and OPC hydration. Highly time-resolved quantitative data on the evolution of proton reservoirs during hydration was collected for up to 40 h. Reservoirs could be clearly assigned to mobile (mix water), intermediate (C-S-H) and rigid fractions (CH, ettringite). Comparison of determined fraction quantities with data from in situ XRD measurements and heat flow calorimetry show very good agreement. During alite hydration at 23 °C, a bulk water content of 4 H 2 O in C 1.7 SH x was confirmed. T2 relaxation times of the mobile fraction shifted towards shorter times from the start of the main reaction until the maximum of the heat flow. Microstructure evolution is nearly finished at that point in time. T2 relaxation times are severely shortened for iron-containing OPC, but are still evaluable. [ABSTRACT FROM AUTHOR]