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Quantitative phase analyses of biomedical pyrophosphate-bearing monetite and brushite cements by solid-state NMR and powder XRD
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).ORCID iD: 0000-0001-7797-7387
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).ORCID iD: 0000-0003-3242-0205
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).ORCID iD: 0000-0001-7109-5068
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2020 (English)In: Ceramics International, ISSN 0272-8842, E-ISSN 1873-3956, Vol. 46, no 8, p. 11000-11012Article in journal (Refereed) Published
Abstract [en]

We present a comprehensive composition analysis of calcium phosphate cements (CPCs) incorporating increasing amounts of bioactive pyrophosphate species (up to 17 wt% P2O7). These cements comprise primarily poorly ordered monetite (CaHPO4) or brushite (CaHPO4 center dot 2H(2)O) and are investigated for enhanced osteoinductive bone/tooth implants. The specimens were characterized by magic-angle spinning (MAS) P-31 and H-1 nuclear magnetic resonance (NMR) spectroscopy along with powder X-ray diffraction (PXRD). P-31 MAS NMR was employed to quantify the major monetite/brushite constituents, the crystalline and amorphous pyrophosphates, as well as various minor orthophosphate by-products. The NMR-derived contents of the crystalline phases accorded well with those from Rietveld analyses of the corresponding PXRD data. The amounts of crystalline and amorphous pyrophosphate depended on the precise cement precursor mixture and preparation conditions, which together with their distinct structural roles may enable the design of cements with a tunable P2O74 - release into aqueous solutions.

Place, publisher, year, edition, pages
2020. Vol. 46, no 8, p. 11000-11012
Keywords [en]
Calcium phosphate cement, Amorphous calcium pyrophosphate, P-31 NMR, H-1 NMR, Rietveld analysis, Biomedical implant
National Category
Physical Chemistry Inorganic Chemistry
Identifiers
URN: urn:nbn:se:su:diva-194827DOI: 10.1016/j.ceramint.2020.01.116ISI: 000528481900126OAI: oai:DiVA.org:su-194827DiVA, id: diva2:1579207
Available from: 2021-07-08 Created: 2021-07-08 Last updated: 2021-11-22Bibliographically approved
In thesis
1. Structural characterization of complex inorganic materials using solid-state NMR spectroscopy
Open this publication in new window or tab >>Structural characterization of complex inorganic materials using solid-state NMR spectroscopy
2021 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Over the past decades, advancements in technology have relied greatly on the development of new functional inorganic materials. Detailed structural characterization of these materials is key for the understanding and also prediction of chemical and physical properties. The structural characterization of complex inorganic materials is typically conducted by a combination of multiple methods. Solid-state NMR brings several advantages because it is element-specific, non-destructive and allows local-chemical-structure elucidation for composite materials, disordered and interfacial structures. This thesis focuses on the application of solid-state NMR for structural characterization of two classes of complex inorganic materials. 

Calcium phosphate cements (CPCs) have been widely applied as bone-substitution materials. The structures of the setting cements are vital for understanding their behaviors in setting and bone-regeneration processes and functions of different additives. In this thesis two types of CPCs, with different additives, were investigated. The different components in the cements could be identified and quantified with solid-state NMR. Correlation spectra were established that helped in probing the structural relationship between different phases. 

Mixed-anion perovskite compounds AB(O,X)3 (X = N, F, H, OH, etc.) have been intensively investigated because of their unique properties for different applications as introduced by the mixed anion environment for the transition metal component B. Because of the lability of hydride oxyhydrides emerged as versatile precursors for the synthesis of other mixed-anion compounds and oxynitrides are extensively investigated for their photocatalytic activity and dielectric properties. In this thesis the oxyhydrides BaTiO3-xHx and SrVO2H were synthesized and their subsequent conversions to oxynitrides were investigated. Solid-state NMR was used to probe the local chemical environments of H and N incorporated in the perovskite anion substructure. 1H NMR proved especially to be useful in the quantification of H which is very difficult to accomplish by other methods.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry, Stockholm University, 2021. p. 78
Keywords
solid-state NMR, materials characterization, inorganic materials, Calcium phosphate cements, bone-substitution materials, Mixed-anion compounds, perovskite, Oxyhydride materials, Oxynitride materials, Barium titanate, Strontium vanadate
National Category
Inorganic Chemistry
Research subject
Inorganic Chemistry
Identifiers
urn:nbn:se:su:diva-194830 (URN)978-91-7911-556-2 (ISBN)978-91-7911-557-9 (ISBN)
Public defence
2021-09-27, online via Zoom, public link is available at the department website, 10:00 (English)
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Supervisors
Available from: 2021-09-02 Created: 2021-07-08 Last updated: 2021-11-22Bibliographically approved

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Guo, HuaYu, YangStevensson, BaltzarEdén, Mattias

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