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Investigating the structure of biomass-derived non-graphitizing mesoporous carbons by electron energy loss spectroscopy in the transmission electron microscope and X-ray photoelectron spectroscopy

机译:通过电子能量损失光谱研究透射电子显微镜和X射线光电子谱的电子能量损失光谱研究生物质衍生非石墨介孔碳的结构

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摘要

We have investigated the microstructure and bonding of two biomass-based porous carbon chromatographic stationary phase materials (alginic acid-derived Starbon® and calcium alginate-derived mesoporous carbon spheres (AMCS) and a commercial porous graphitic carbon (PGC), using high resolution transmission electron microscopy, electron energy loss spectroscopy (EELS), N2 porosimetry and X-ray photoelectron spectroscopy (XPS). The planar carbon sp 2-content of all three material types is similar to that of traditional nongraphitizing carbon although, both biomass-based carbon types contain a greater percentage of fullerene character (i.e. curved graphene sheets) than a non-graphitizing carbon pyrolyzed at the same temperature. This is thought to arise during the pyrolytic breakdown of hexauronic acid residues into C5 intermediates. Energy dispersive X-ray and XPS analysis reveals a homogeneous distribution of calcium in the AMCS and a calcium catalysis mechanism is discussed. That both Starbon® and AMCS, with high-fullerene character, show chromatographic properties similar to those of a commercial PGC material with extended graphitic stacks, suggests that, for separations at the molecular level, curved fullerene- like and planar graphitic sheets are equivalent in PGC chromatography. In addition, variation in the number of graphitic layers suggests that stack depth has minimal effect on the retention mechanism in PGC chromatography.
机译:我们使用高分辨率透射率研究了两种基于生物质的多孔碳色谱固定相材料(藻酸衍生的Starbon®和藻酸钙衍生的介孔碳球(AMCS)和商业多孔石墨碳(PGC)的微观结构和键合电子显微镜,电子能量损失谱(EELS),N2孔隙率法和X射线光电子能谱(XPS)。三种材料类型的平面碳sp 2-含量均与传统的非石墨化碳相似,尽管这两种都是基于生物质的碳两种类型的富勒烯特征(即弯曲的石墨烯片)比在相同温度下热解的非石墨化碳具有更高的百分率特性,认为这是在将六糖醛酸残基热分解为C5中间体时产生的。分析揭示了AMCS中钙的均匀分布,并讨论了钙催化机理。具有高富勒烯特征的arbon®和AMCS具有类似于具有扩展石墨堆叠的商用PGC材料的色谱特性,表明对于分子水平的分离,弯曲的富勒烯状和平面石墨片在PGC色谱中是等效的。另外,石墨层数的变化表明,堆叠深度对PGC色谱中的保留机理影响最小。

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