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基于磷酸改性碳化硅氧的非晶态材料的光谱研究。

Spectroscopic studies on phosphate-modified silicon oxycarbide-based amorphous materials.

作者信息

Gawęda Magdalena, Jeleń Piotr, Bik Maciej, Szumera Magdalena, Olejniczak Zbigniew, Sitarz Maciej

机构信息

NOMATEN CoE, NOMATEN MAB, National Centre for Nuclear Research, A. Soltana 7 Str., 05-400 Otwock-Świerk, Poland.

AGH University of Science and Technology, Faculty of Materials Science and Ceramics, A. Mickiewicza 30 Av, 30-059 Kraków, Poland.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2023 Apr 15;291:122341. doi: 10.1016/j.saa.2023.122341. Epub 2023 Jan 8.

Abstract

Vibrational spectroscopy is the most effective, efficient and informative method of structural analysis of amorphous materials with silica matrix and, therefore, an indispensable tool for examining silicon oxycarbide-based amorphous materials (SiOC). The subject of this work is a description of the modification process of SiOC glasses with phosphate ions based on the structural examination including mainly Infrared and Raman Spectroscopy. They were obtained as polymer-derived ceramics based on ladder-like silsesquioxanes synthesised via the sol-gel method. With the high phosphate's volatility, it was decided to introduce the co-doping ions to create [AlPO] and [BPO] stable structural units. As a result, several samples from the SiPOC, SiPAlOC and SiPBOC systems were obtained with various quantities of the modifiers. All samples underwent a detailed structural evaluation of both polymer precursors and ceramics after high-temperature treatment with Fourier-transformed infrared spectroscopy (FTIR), Raman spectroscopy, X-ray diffraction (XRD) and magic angle spinning nuclear magnetic resonance (MAS-NMR). Obtained results proved the efficient preparation of desired materials that exhibit structural parameters similar to the unmodified one. They were X-ray-amorphous with no phase separation and crystallisation. Spectroscopic measurements confirmed the presence of the crucial Si-C bond and how modifying ions are incorporated into the SiOC network. It was also possible to characterise the turbostratic free carbon phase. The modification was aimed to improve the bioperformance of the materials in the context of their future application as bioactive coatings on metallic implants.

摘要

振动光谱是对含二氧化硅基体的非晶态材料进行结构分析的最有效、高效且信息丰富的方法,因此也是研究基于碳氧化硅的非晶态材料(SiOC)不可或缺的工具。本工作的主题是基于结构检测(主要包括红外光谱和拉曼光谱)来描述磷酸根离子对SiOC玻璃的改性过程。它们是通过溶胶 - 凝胶法合成的基于梯形倍半硅氧烷的聚合物衍生陶瓷。鉴于磷酸根挥发性高,决定引入共掺杂离子以形成[AlPO]和[BPO]稳定结构单元。结果,获得了来自SiPOC、SiPAlOC和SiPBOC体系的几个含有不同数量改性剂的样品。所有样品在高温处理后,通过傅里叶变换红外光谱(FTIR)、拉曼光谱、X射线衍射(XRD)和魔角旋转核磁共振(MAS - NMR)对聚合物前驱体和陶瓷进行了详细的结构评估。所得结果证明了能有效制备出具有与未改性材料相似结构参数的所需材料。它们是X射线非晶态的,无相分离和结晶现象。光谱测量证实了关键的Si - C键的存在以及改性离子如何融入SiOC网络。还能够表征乱层状游离碳相。这种改性旨在改善材料在未来作为金属植入物生物活性涂层应用方面的生物性能。

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