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Tricalcium Phosphate: an X-Ray Diffraction, Solid State NMR and ATR-FTIR Study

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Tricalcium Phosphate: an X-Ray Diffraction, Solid State NMR and ATR-FTIR Study Journal of Functional Biomaterials Article Strontium and Zinc Substitution in β-Tricalcium Phosphate: An X-ray Diffraction, Solid State NMR and ATR-FTIR Study Elisa Boanini 1 , Massimo Gazzano 2,* , Carlo Nervi 3 , Michele R. Chierotti 3 , Katia Rubini 1, Roberto Gobetto 3 and Adriana Bigi 1 1 Department of Chemistry “Giacomo Ciamician”, Alma Mater Studiorum-University of Bologna, 40126 Bologna, Italy; [email protected] (E.B.); [email protected] (K.R.); [email protected] (A.B.) 2 ISOF-CNR, via Gobetti 101, 40129 Bologna, Italy 3 Department of Chemistry, University of Torino, via P. Giuria 7, 10125 Torino, Italy; [email protected] (C.N.); [email protected] (M.R.C.); [email protected] (R.G.) * Correspondence: [email protected]; Tel.: +39-051-2099552 Received: 27 March 2019; Accepted: 28 April 2019; Published: 5 May 2019 Abstract: β-tricalcium phosphate (β-TCP) is one of the most common bioceramics, widely applied in bone cements and implants. Herein we synthesized β-TCP by solid state reaction in the presence of increasing amounts of two biologically active ions, namely strontium and zinc, in order to clarify the structural modifications induced by ionic substitution. The results of X-ray diffraction analysis indicate that zinc can substitute for calcium into a β-TCP structure up to about 10 at% inducing a reduction of the cell parameters, whereas the substitution occurs up to about 80 at% in the case of strontium, which provokes a linear increase of the lattice constants, and a slight modification into a more symmetric structure. Rietveld refinements and solid-state 31P NMR spectra demonstrate that the octahedral Ca(5) is the site of β-TCP preferred by the small zinc ion. ATR-FTIR results indicate that zinc substitution provokes a disorder of β-TCP structure. At variance with the behavior of zinc, strontium completely avoids Ca(5) site even at high concentration, whereas it exhibits a clear preference for Ca(4) site. The infrared absorption bands of β-TCP show a general shift towards lower wavenumbers on increasing strontium content. Particularly significant is the shift of the infrared 1 symmetric stretching band at 943 cm− due to P(1), that is the phosphate more involved in Ca(4) coordination, which further supports the occupancy preference of strontium. Keywords: β-tricalcium phosphate; zinc; strontium; ionic substitutions; Rietveld refinement; solid-state NMR; ATR-FTIR 1. Introduction β-tricalcium phosphate, β-Ca3(PO4)2 (β-TCP) is the stable polymorph of tricalcium phosphate at temperatures lower than 1125 ◦C. At higher temperatures, it undergoes a thermal transition into the α form [1]. β-TCP is synthesized by solid state reaction at high temperature, alternatively it can be prepared by thermal transition of other calcium phosphates. Although this phase is not present in physiologically calcified biological tissues, it has been found in pathological calcifications and it can be obtained as a product of thermal conversion of the poorly crystalline hydroxyapatite (HA), which constitutes the inorganic phase of bone [2]. Actually, β-TCP both alone and in combination with synthetic HA, is widely applied as a biomaterial for the treatment of defects of the skeletal system [3]. The properties, as well as the relative stability, of calcium phosphates can be modified by functionalization with foreign ions [4]. The number of studies on ionic substitution into HA structure J. Funct. Biomater. 2019, 10, 20; doi:10.3390/jfb10020020 www.mdpi.com/journal/jfb J. Funct. Biomater. 2019, 10, x FOR PEER REVIEW 2 of 15 J. Funct. Biomater. 2019, 10, 20 2 of 15 structure is particularly relevant, due to its high flexibility, which supports a great variety of cationic, as well as anionic, substitutions [4–8]. is particularlyThe rhombohedral relevant, due structure to its high of flexibility,β-TCP, space which group supports R3c, is a without great variety any doubt of cationic, less flexible as well than as anionic,HA lattice; substitutions however, [4 –it8 ].can host several ionic replacements, especially the replacement of calcium ionsThe with rhombohedral bivalent cations structure [9–14]. of βCalcium-TCP, space ions group in β-TCP R3c, occupy is without five any different doubt lesscation flexible sites: thanCa(1), HACa(2) lattice; and however, Ca(3) are it on can general host several positions ionic with replacements, eight to nine especially coordinated the replacement oxygens, whereas of calcium both ions Ca(4) withand bivalent Ca(5) are cations on special [9–14 ].positions, Calcium with ions inanβ effective-TCP occupy multiplicity five diff erentof 1/3 cationof the sites:other Ca(1),cation Ca(2)sites. andCa(5) Ca(3)exhibits are on an general approximately positions octahedr with eightal coordination, to nine coordinated Ca(4) oxygens,site is only whereas half occupied both Ca(4) and and exhibits Ca(5) a arequite on special distorted positions, nine coordination with an effective (Figure multiplicity 1) [15]. ofPhosphorus 1/3 of the other exhi cationbits three sites. crystallographically Ca(5) exhibits an approximatelydifferent positions, octahedral with coordination,the multiplicity Ca(4) of P(1) site isequal only to half 1/3 occupied of those andof P(2) exhibits and P(3), a quite since distorted it is on a ninespecial coordination position. (Figure1)[ 15]. Phosphorus exhibits three crystallographically different positions, with the multiplicity of P(1) equal to 1/3 of those of P(2) and P(3), since it is on a special position. Figure 1. Coordination geometry of the five different cation sites of β-TCP [15]. Bonds at 3.0 0.1 Å Figure 1. Coordination geometry of the five different cation sites of β-TCP [15]. Bonds at 3.0± ± 0.1 Å length are dotted. length are dotted. In this paper we investigated the structural modifications induced on β-TCP structure by functionalizationIn this paper with we two investigated bivalent cations, the structural namely strontium modifications and zinc. induced Both theseon β-TCP ions arestructure of great by biologicalfunctionalization interest:strontium with two hasbivalent been cations, reported namely to display strontium a beneficial and zinc. action Both in the these treatment ions are of of bone great diseasesbiological characterized interest: strontium by abnormally has been high reported mass to resorption, display a beneficial such as osteoporosis action in the [ 16treatment,17]; zinc of hasbone beendiseases shown characterized to inhibit osteoclast by abnormally proliferation high mass [18] and resorption, it has been such reported as osteoporosis to display [16,17]; antibacterial zinc has propertiesbeen shown [19]. to Moreover, inhibit osteoclast their beneficial proliferation effect on [18] bone and cells it has has been also beenreported observed to display when coupledantibacterial to β-TCPproperties [20–24 [19].]. In Moreover, particular, their strontium-substituted beneficial effect onβ bone-TCP cells (SrTCP) has also added been with observed mesenchymal when coupled stem cellsto β has-TCP been [20–24]. shown In toparticular, improve strontium-substituted bone formation and fusionβ-TCP across(SrTCP) the added transverse with mesenchymal processes, both stem incells osteoporotic has been andshown non-osteoporotic to improve bone animal formation models and [ 25fusion]. The across possible the transverse substitution processes, of these both two in cationsosteoporotic into β-TCP and non-osteoporotic structure has been animal previously models investigated. [25]. The possible Heat treatmentsubstitution of poorlyof these crystalline two cations HAinto synthesized β-TCP structure in the presence has been of zincpreviously produced investigat Zn substituteded. Heatβ -TCPtreatment (ZnTCP) of uppoorly to a Zncrystalline content ofHA aboutsynthesized 9 at% [26 in]. the The presence results of of Rietveld zinc produced refinement Zn indicatedsubstituted a linearβ-TCP decrease (ZnTCP) of up the to lattice a Zn constantcontent of andabout a preference 9 at% [26]. of The Zinc results for the of Ca(5) Rietveld site. refinement Evidences ofindicated preference a linear for the decrease octahedral of the Ca(5) lattice site constant were obtainedand a preference also by combination of Zinc for ofthe near-edge Ca(5) site. X-ray Evidences absorption of preference fine structure for the (NEXAFS) octahedral measurements Ca(5) site were andobtainedab-initio alsocalculations by combination with X-rayof near-edge refinement X-ray of absorption ZnTCP synthesized fine structure by (NEXAFS) solid state measurements reaction up toand a zinc ab-initio content calculations of about 3.3with at% X-ray [27 ].refinement These data of areZnTCP in agreement synthesized with by thesolid results state reaction of a study up ofto a first-principleszinc content calculationsof about 3.3 which at% [27]. indicated These that data Ca(4) are and in Ca(5)agreement are the with favored the results substitution of a sitesstudy of of divalentfirst-principles cations: thecalculations lower coordination which indicated number that and Ca bond(4) and lengths Ca(5) ofare Ca(5), the favored are preferred substitution by smaller sites of sizeddivalent cations cations: such as the Zn lower and Mg, coordination whereas larger-sized number and ones, bond such lengths as Sr of and Ca(5), Ba, favor are preferred the Ca(4) by site smaller [28]. Onsized the othercations hand, such on asthe Zn basisand Mg, of the whereas refinement larger-siz resultsed ofones, zinc such doped as biphasicSr and Ba, calcium favor the phosphate Ca(4) site J. Funct. Biomater. 2019, 10, 20 3 of 15 (BCP) Gomes et al. (2011) [29] concluded that Zn is incorporated into β-TCP structure by substituting calcium ions both in Ca(5) and in Ca(4) sites. Strontium substitution to calcium into β-TCP has been obtained by thermal treatment of calcium deficient apatite up to 20 at% and by solid state reaction up to 80 at% [9,30]. However, detailed structural analysis on strontium substituted β-TCP (SrTCP) was performed only up to a Sr substitution of about 33 at% and indicated a preferential occupation of the Ca(4) site [31,32].
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