形态不同的纳米羟基磷灰石的合成和结构表征,The Journal of Physical Chemistry C

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形态不同的纳米羟基磷灰石的合成和结构表征
The Journal of Physical Chemistry C ( IF 3.3 ) Pub Date : 2022-07-25 , DOI: 10.1021/acs.jpcc.2c02383
Yuan Li ₁ , Marielle A. Deguzman ₁ , John E. Heise ₁ , Gregory P. Holland ₁

Affiliation

选择性地开发了具有不同形态和晶相的纳米级羟基磷灰石 (HAP)，包括高度结晶的纳米棒、单晶纳米线和具有 c 或 a(b) 晶格平面的纳米片，并合成了半无定形形式并对其进行了结构表征。粉末 X 射线衍射、电子显微镜和多核魔角旋转 (MAS) 固态核磁共振 (ssNMR) 用于确定体积和表面物质的结构。质子 MAS ssNMR 提供了对表面羟基缺陷位点的深入了解，与其他 HAP 形式相比，这些位点在以 c 晶格平面为主的纳米片中明显更丰富。通过一系列的水合和氨基酸吸附实验，有人提出，这些羟基缺陷可能是与表面钙位点结合的 OH 基团，可能在生物矿化过程中很重要。对于 a(b) 晶格平面优先的 HAP 样本，¹ H MAS NMR 揭示了这些环境的低群体，其光谱主要由结构羟基和物理吸附水控制，而具有选择性发展的 a(b) 晶格平面的纳米片形态揭示了相当多的表面相关缺陷羟基群体。这项工作为纳米级 HAP 的结构和表面化学提供了相当多的新见解，其中表面羟基环境对形态暴露的晶格平面表现出强烈的依赖性。

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Synthesis and Structural Characterization of Morphologically Distinct Nanoscale Hydroxyapatites

Nanoscale hydroxyapatites (HAPs) with different morphologies and crystal phases including highly crystalline nanorods, single-crystal nanowires, and nanosheets with the c or a(b) lattice planes were selectively developed and a semiamorphous form was synthesized and structurally characterized. Powder X-ray diffraction, electron microscopy, and multinuclear magic angle spinning (MAS) solid-state nuclear magnetic resonance (ssNMR) were used for structure determination of the bulk and surface species. Proton MAS ssNMR provides considerable insights into surface hydroxyl defect sites that are significantly more abundant in c-lattice plane-dominated nanosheets compared to the other HAP forms. Through a series of hydration and amino acid adsorption experiments, it is proposed that these hydroxyl defects are likely to be OH groups that bind to surface calcium sites and may be important in biomineralization processes. For a(b) lattice plane-preferred HAP samples, the ¹H MAS NMR reveals a low population of these environments with a spectrum dominated by structural hydroxyls and physisorbed water, while nanosheet morphologies with the a(b) lattice plane selectively developed reveal a considerably higher population of surface-associated defect hydroxyls. This work provides considerable new insights into the structure and surface chemistry of nanoscale HAP where surface hydroxyl environments show a strong dependence upon the morphologically exposed lattice planes.

更新日期：2022-07-25

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