In situ Synchrotron X-ray Powder Diffraction Study of the Early Hydration of α-tricalcium Phosphate/tricalcium Silicate Composite Bone Cement

Morejón-Alonso, Loreley; Motisuke, Mariana; Correa, José R.; Carrodeguas, Raúl García; Santos, Luís Alberto dos

doi:10.1590/1516-1439.302114

Cited by 8 publications

(8 citation statements)

References 18 publications

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“…The paste samples were cured previously at 20°C for 24 hours followed by curing at 60°C for the designated time. The cured pastes were placed on a 15 μm thick Kapton film which is positioned on a specialized temperature‐controlled sample holder as described for in‐situ XRD records of hydration of ordinary Portland cement . The temperature of the sample holder was raised from the room temperature to the temperature of 60°C within 2 minutes.…”

Section: Methodsmentioning

confidence: 99%

“…The cured pastes were placed on a 15 lm thick Kapton film which is positioned on a specialized temperature-controlled sample holder as described for in-situ XRD records of hydration of ordinary Portland cement. 21,22 The temperature of the sample holder was raised from the room temperature to the temperature of 60°C within 2 minutes. The XRD record was started when the holder temperature reached the designed temperature of 60°C.…”

Section: Methodsmentioning

confidence: 99%

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Conversion of calcium aluminate cement hydrates at 60°C with and without water

Zhang

et al. 2018

J Am Ceram Soc

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There have been different hypotheses about the transformation mechanisms of calcium aluminate cement hydrates and this work aims to clarify the long‐running debate about the conversion approaches. In this work, CAH10 and C2AH8 were produced from the pastes of calcium aluminate cement (CAC) cured for 24 hours at 10 and 20°C separately. And the cured pastes were continually cured at 60°C for 3 days with water and without water, respectively. The hydration of the pastes was halted by freeze‐drying, and the phases and microstructure of hydrates were investigated by XRD and SEM, respectively. The results indicate that CAH10 and C2AH8 converted into C3AH6 and AH3 in water presence at 60°C, but did not transform into C3AH6 and AH3 without water. It is confirmed that the conversion of CAH10 and C2AH8 to C3AH6 and AH3 happens through preceding solution of CAH10 and C2AH8 and subsequent precipitation of C3AH6 and AH3.

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Section: Methodsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Conversion of calcium aluminate cement hydrates at 60°C with and without water

Zhang

et al. 2018

J Am Ceram Soc

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“…To finalize this topic, one should mention that CaPO 4 might be added into self-setting calcium sulfate (plaster of Paris) formulations to improve their osteoconductivity [ 508 , 509 ]. Similarly, calcium silicates could be added to the self-setting CaPO 4 formulations [ 510 , 511 , 512 , 513 ].…”

Section: Biocomposites and Hybrid Biomaterials Containing Capo mentioning

confidence: 99%

Calcium Orthophosphate-Containing Biocomposites and Hybrid Biomaterials for Biomedical Applications

Dorozhkin¹

2015

JFB

125

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The state-of-the-art on calcium orthophosphate (CaPO4)-containing biocomposites and hybrid biomaterials suitable for biomedical applications is presented. Since these types of biomaterials offer many significant and exciting possibilities for hard tissue regeneration, this subject belongs to a rapidly expanding area of biomedical research. Through the successful combinations of the desired properties of matrix materials with those of fillers (in such systems, CaPO4 might play either role), innovative bone graft biomaterials can be designed. Various types of CaPO4-based biocomposites and hybrid biomaterials those are either already in use or being investigated for biomedical applications are extensively discussed. Many different formulations in terms of the material constituents, fabrication technologies, structural and bioactive properties, as well as both in vitro and in vivo characteristics have been already proposed. Among the others, the nano-structurally controlled biocomposites, those containing nanodimensional compounds, biomimetically fabricated formulations with collagen, chitin and/or gelatin, as well as various functionally graded structures seem to be the most promising candidates for clinical applications. The specific advantages of using CaPO4-based biocomposites and hybrid biomaterials in the selected applications are highlighted. As the way from a laboratory to a hospital is a long one and the prospective biomedical candidates have to meet many different necessities, the critical issues and scientific challenges that require further research and development are also examined.

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“…Synchrotron X-ray diffraction (SXRD) is a powerful tool for revealing detailed structural and morphological information by real-time monitoring of crystal evolution and phase transition. − The short exposure time makes it possible to provide fast data acquisition with high angular resolution and signal-to-noise ratio, thereby following rapid reactions. It has already been used to study the setting reaction of α-TCP-based cement, which however focused on the setting reaction after 24 h and even longer, as the setting of α-TCP-based cement is much slower than brushite cements.…”

Section: Introductionmentioning

confidence: 99%

“…20−25 The short exposure time makes it possible to provide fast data acquisition with high angular resolution and signal-to-noise ratio, thereby following rapid reactions. It has already been used to study the setting reaction of α-TCP-based cement, 26 which however focused on the setting reaction after 24 h and even longer, as the setting of α-TCP-based cement is much slower than brushite cements.…”

Section: ■ Introductionmentioning

confidence: 99%

In Situ Synchrotron X-ray Diffraction Analysis of the Setting Process of Brushite Cement: Reaction and Crystal Growth

Luo

Martínez-Casado

Balmès

et al. 2017

ACS Appl. Mater. Interfaces

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Brushite cements are fast self-setting materials that can be used as bone substitute materials. Although tracing their fast setting process is a challenge, it is important for the understanding of the same, which in turn is important for the material's further development and use in the clinics. In this study, the setting rate, phase formation, and crystal growth of brushite cements were quantitatively studied by in situ synchrotron powder X-ray diffraction (SXRD) on a time scale of seconds. The influence of reactant ratios and a retardant (citric acid) on the setting reaction were analyzed. To complement the in situ investigations, scanning electron microscopy was carried out for ex situ morphological evolution of crystals. The initial reaction followed a four-step process, including a fast nucleation induction period, nucleation, crystal growth, and completion of the setting. The brushite crystal size grew up to the micro scale within 1 min, and the brushite content increased linearly after the nucleation until all monocalcium phosphate monohydrate (MCPM; Ca(HPO)·HO) had dissolved within minutes, followed by a slow increase until the end of the monitoring. By adjusting the MCPM to the β-tricalcium phosphate (β-TCP, β-Ca(PO4)) ratio in the starting powders, the brushite/monetite ratio in the cements could be modified. In the presence of citric acid, the formation of brushite nuclei was not significantly retarded, whereas the increase in brushite content and the growth of crystal size were effectively hindered. The amount of monetite also increased by adding citric acid. This is the first time that the brushite setting process has been characterized in the first seconds and minutes of the reaction by SXRD.

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In situ Synchrotron X-ray Powder Diffraction Study of the Early Hydration of α-tricalcium Phosphate/tricalcium Silicate Composite Bone Cement

Cited by 8 publications

References 18 publications

Conversion of calcium aluminate cement hydrates at 60°C with and without water

Conversion of calcium aluminate cement hydrates at 60°C with and without water

Calcium Orthophosphate-Containing Biocomposites and Hybrid Biomaterials for Biomedical Applications

In Situ Synchrotron X-ray Diffraction Analysis of the Setting Process of Brushite Cement: Reaction and Crystal Growth

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