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Advanced solid-state H-1/P-31 NMR characterization of pyrophosphate-doped calcium phosphate cements for biomedical applications: The structural role of pyrophosphate
Stockholm Univ, Dept Mat & Environm Chem, SE-10691 Stockholm, Sweden.
Stockholm Univ, Dept Mat & Environm Chem, SE-10691 Stockholm, Sweden.
Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Applied Materials Sciences.
Stockholm Univ, Dept Mat & Environm Chem, SE-10691 Stockholm, Sweden.ORCID iD: 0000-0001-7109-5068
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2019 (English)In: Ceramics International, ISSN 0272-8842, E-ISSN 1873-3956, Vol. 45, no 16, p. 20642-20655Article in journal (Refereed) Published
Abstract [en]

From a suite of advanced magic-angle spinning (MAS) NMR spectroscopy and powder X-ray diffraction (PXRD) experiments, we present a comprehensive structural analysis of pyrophosphate-bearing calcium phosphate cements that are investigated for bone-inductive biomedical implants. The cements consist mainly of poorly ordered monetite (CaHPO4), along with minor Ca orthophosphate phases, and two distinct pyrophosphate constituents: crystalline beta-Ca2P2O7 and amorphous calcium pyrophosphate (ACPP), the latter involving one water bearing portion and another anhydrous component. Independent 2D MAS NMR experiments evidenced close contacts between the amorphous pyrophosphates and the monetite phase, where ACPP is proposed to form a thin layer coating the monetite particles. Heteronuclear H-1-P-31 and homonuclear P-31-P-31 correlation NMR experimentation enabled us to detect, identify, and quantify even minor cement constituents (less than or similar to 2 mol%) that could not be ascertained by the Rietveld method. Quantitative phase analyses of the cements, as determined independently by P-31 NMR and PXRD, are contrasted and discussed.

Place, publisher, year, edition, pages
ELSEVIER SCI LTD , 2019. Vol. 45, no 16, p. 20642-20655
Keywords [en]
Bioceramics, Monetite cement, DCPA, Amorphous calcium pyrophosphate, P-31 NMR, H-1 NMR, 2D homonuclear/heteronuclear correlation, NMR spectroscopy, Rietveld refinement, Cement structure
National Category
Ceramics
Identifiers
URN: urn:nbn:se:uu:diva-395715DOI: 10.1016/j.ceramint.2019.07.047ISI: 000488148100128OAI: oai:DiVA.org:uu-395715DiVA, id: diva2:1365608
Funder
Swedish Foundation for Strategic Research , RMA15-0110Available from: 2019-10-25 Created: 2019-10-25 Last updated: 2019-10-25Bibliographically approved

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Pujari-Palmer, MichaelEngqvist, Håkan

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