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首页> 外文期刊>Acta biomaterialia >Furthering the understanding of silicate-substitution in α-tricalcium phosphate: An X-ray diffraction, X-ray fluorescence and solid-state nuclear magnetic resonance study
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Furthering the understanding of silicate-substitution in α-tricalcium phosphate: An X-ray diffraction, X-ray fluorescence and solid-state nuclear magnetic resonance study

机译：进一步理解α-磷酸三钙中的硅酸盐取代：X射线衍射，X射线荧光和固态核磁共振研究

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摘要

High-purity (SupT) and reagent-grade (ST), stoichiometric and silicate-containing α-tricalcium phosphate (α-TCP: ST0/SupT0 and Si-TCP x = 0.10: ST10/SupT10) were prepared by solid-state reaction based on the substitution mechanism Ca3(PO4)(2-x)(SiO 4)x. Samples were determined to be phase pure by X-ray diffraction (XRD), and Rietveld analysis performed on the XRD data confirmed inclusion of Si in the α-TCP structure as determined by increases in unit cell parameters; particularly marked increases in the b-axis and β-angle were observed. X-ray fluorescence (XRF) confirmed the presence of expected levels of Si in Si-TCP compositions as well as significant levels of impurities (Mg, Al and Fe) present in all ST samples; SupT samples showed both expected levels of Si and a high degree of purity. Phosphorus (31P) magic-angle-spinning solid-state nuclear magnetic resonance (MAS NMR) measurements revealed that the high-purity reagents used in the synthesis of SupT0 can resolve the 12 expected peaks in the 31P spectrum of α-TCP compared to the low-purity ST0 that showed significant spectral line broadening; line broadening was also observed with the inclusion of Si which is indicative of induced structural disorder. Silicon (29Si) MAS NMR was also performed on both Si-TCP samples which revealed Q0 species of Si with additional Si Q1/Q2 species that may indicate a potential charge-balancing mechanism involving the inclusion of disilicate groups; additional Q4 Si species were also observed, but only for ST10. Heating and cooling rates were briefly investigated by 31P MAS NMR which showed no significant line broadening other than that associated with the emergence of β-TCP which was only realised with the reagent-grade sample ST0. This study provides an insight into the structural effects of Si-substitution in α-TCP and could provide a basis for understanding how substitution affects the physicochemical properties of the material.
机译：通过固相反应制得高纯度（SupT）和试剂级（ST），化学计量和含硅酸盐的α-磷酸三钙（α-TCP：ST0 / SupT0和Si-TCP x = 0.10：ST10 / SupT10）基于Ca3（PO4）（2-x）（SiO 4）x的取代机理。通过X射线衍射（XRD）确定样品为纯相，对XRD数据进行的Rietveld分析证实，如晶胞参数增加所确定的，α-TCP结构中包含Si。特别观察到b轴和β角明显增加。 X射线荧光（XRF）证实所有ST样品中Si-TCP组合物中均存在预期水平的Si，并且存在明显水平的杂质（Mg，Al和Fe）。 SupT样品显示出预期的Si水平和高纯度。磷（31P）魔角旋转固态核磁共振（MAS NMR）测量显示，合成SupT0所用的高纯试剂可解析α-TCP的31P光谱中的12个预期峰。显示光谱线明显展宽​​的低纯度ST0;伴随着Si的引入，还观察到线变宽，这表明诱导的结构紊乱。还在两个Si-TCP样品上进行了硅（29Si）MAS NMR分析，揭示了Si的Q0物种和其他Si Q1 / Q2物种，这可能表明潜在的电荷平衡机制涉及二硅酸盐基团的引入。还观察到其他Q4 Si物种，但仅对于ST10。通过31P MAS NMR简短地研究了加热和冷却速率，除仅与试剂级样品ST0实现的与β-TCP的出现有关的谱线扩宽外，没有显着谱线展宽。这项研究提供了对α-TCP中Si取代的结构效应的见解，并可以为理解取代如何影响材料的物理化学性质提供基础。

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