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Influence of Cu2+-doping in β-TCP on the hydration kinetics of brushite cement investigated by Rietveld analysis and heat flow calorimetry

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- Plenary Lecture Test Ploetz 1 Alexia Ploetz
- Poster Investigating Dynamic Biological Processes with High-Speed, High-Resolution Correlative AFM-Light Microscopy 1 Oilibhe Pabsch
- Poster Corrosion behaviour of potencially biodegradable ternary alloy Zn-Mg-Ca 1 Dipl.-Ing. Jan Pinc
- Poster Multi scale topography in titanium alloys by electron beam technique: influence on the tissue adhesion and bacterial contamination 1 Dr. Fernando Warchomicka
- Poster Cytotoxicity of gold nanorods and nanoribbons in context of biomedical applications 1 Marika Musielak
- Poster Preliminary studies of synthesis of gold nanoribbons using selected dicationic surfactants 1 Joanna Patalas
- Poster Diclofenac release from a silicon based hydrogel for contact lenses controlled by a layer-by-layer coating 1 Prof. Ana Serro
- Poster Synthesis, solubility and optical activity of chiral poly(2,4-disubstituted-2-oxazoline)s 1 Mengshi Yang
- Poster Influence of Cu2+-doping in β-TCP on the hydration kinetics of brushite cement investigated by Rietveld analysis and heat flow calorimetry 1 Karla Späth
- Poster Analytical investigation of the influence of micro- and nanoplastic particles in crop plants by electron microscopic imaging and spectroscopy 1 Dr. Jörg Wissler
- Poster Influence of fluoride corrosion attack on the metal-porcelain bond strength of TiCr20 compared to titanium 1 Christine Schille
- Poster Bacterial nanocellulose loaded with frankincense extract as natural wound dressing to treat local dermal inflammations 1 Berit Karl
- Poster Graded functionalization of polydopamine coated fiber mats as potential implant for tendon-bone-transition 1 Sarah Oehmichen
- Poster Enhancing the functionalities of bioactive glass-based scaffolds by novel polymeric coatings 1 Dr. Liliana Liverani
- Poster Durability analysis of the cryopreservation of DNA origami nanostructures 1 Yang Xin
- Poster Effects of staple age on DNA origami nanostructure assembly and stability 1 Charlotte Kielar
- Poster Dual-setting brushite-silica gel cements – Variations of the monomer precursors and tuning of the setting parameters 1 Ib Holzmeister
- Poster Novel QCM-D/microscopy set-up for real-time analysis of bacterial binding onto biomaterial-coated sensors 1 Dr. Zeqian Xu
- Poster Chairside plasma activation of encapsulated implants: how fast is it? 1 Miguel Angel Garcia Chame
- Poster Nanostructured high-pressure laminate surfaces to reduce transmission pathways of pathogens in public transportation 1 Christian Helbing
- Poster Biomineralization of Recombinant Spider Silk Films 1 Vanessa J. Neubauer
- Poster Modification of bacterial cellulose to enhance anti-inflammatory wound dressing properties 1 Uwe Beekmann
- Poster Absolute Characterization of Synthetic Macromolecules used in Biomaterials Science Applications 1 Mandy Grube
- Poster Biodegradable thermoplastic materials for bimodal imaging containing the mineral present in the human body 1 Zaneta Górecka
- Poster Nano-rough titanium surfaces created by wet alkaline etching and PVD and their influence on bacterial adhesion as well as protein adsorption 1 Michaela Schürmann
- Poster Effective strategies for the controlling and dealing with transmission pathway of pathogens in air traffi 1 Christian Helbing
- Poster Cytotoxicity evaluation of biodegradable Zn-4Cu alloy using L929, Saos-2 and TAg cell lines 1 Ping Li
- Poster Influence of pulsed bias voltage on the tribological and morphological properties of a-C coatings deposited by an anodic arc method 1 Dipl.-Ing. Ingo Erdmann

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Brushite (CaHPO4∙2H2O) formation in calcium phosphate generally occurs under acidic conditions. One example is the acid-base-reaction of monocalcium phosphate monohydrate (MCPM, Ca(H2PO4)2∙H2O) and β-tricalcium phosphate (β-TCP, β-Ca3(PO4)2), which react with H2O according to (1).

Ca(H2PO4)2∙H2O + β-Ca3-xCux(PO4)2 + 7 H2O → 4 CaHPO4∙2H2O (1)

Because of the very rapid reaction of this cement system, a setting retarder is necessary. Phytic acid (IP6, C6H6(OPO3H2)6) is an additive to decelerate the reaction, while further improving injectability of the cement pastes [1].The use of Cu2+ as dopant for β-Ca3(PO4)2 leads to increased microbacterial activity, hence preventing inflammation [2] and has positive effects on angiogenesis and wound healing [3].

The limit of substitution of Cu2+ ions in the structure of β-Ca3(PO4)2 was investigated by Rietveld refinement of powder XRD samples with different amounts of Cu2+ doping up to 20 mol-%. Its effect on the hydration was investigated by isothermal heat flow calorimetry and quantitative in-situ XRD. β-TCP was mixed with MCPM with a molar ratio of β-TCP/MCPM = 1.62 and a water to solid ratio of 0.3 ml/g. The amount of IP6 was set at 2 wt.-% referred to the solid content, all measurements were conducted at 23 °C.

Rietveld refinement showed a significant decrease of the lattice parameters a and c with an increasing amount of Cu2+ up to 15 mol-% for Ca2+. Furthermore the refinement of the site occupancies showed an incorporation of Cu2+ ions at the Ca(5) and Ca(3) atom site. For Cu2+ amounts above 15 mol-% the formation of the secondary phase Ca3Cu3(PO4)4 was observed, whereby the limit of solid solution could be set between 10 and 15 mol-%. Heat flow calorimetry and in-situ XRD measurements showed a clear increasing retardation of the reaction with increasing amount of Cu2+ in the dry powder. Besides a significant decrease of the reaction degree could be determined.

Consequently, the studies provided a deeper understanding of Cu2+ doping in the crystal structure of β-TCP and demonstrated a large impact of Cu2+ on the hydration of β-TCP and MCPM.

[1] Hurle K, Weichhold J, Brueckner M, Gbureck U, Brueckner T, Goetz-Neunhoeffer F. Acta Biomaterialia 2018; 80: 378-89.

[2] Matsumoto N, Sato K, Yoshida K, Hashimoto K, Toda Y. Acta Biomaterialia 2009; 5(8): 3157–64.

[3] Barralet J, Gbureck U, Habibovic P, Vorndran E, Gerard C, Doillon Ch J. Tissue Engineering Part A 2009; 15(7): 1601–9.


Karla Späth
Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU)
Additional Authors:
  • Dr. Katrin Hurle
    Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU)
  • Prof. Dr. Friedlinde Goetz-Neunhoeffer
    Friedrich-Alexander-Universität Erlangen-Nürnberg (FAU)