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Surface and related bulk properties of titania nanoparticles recovered from aramid-titania hybrid films: A novel attempt

机译:从芳族聚酰胺-二氧化钛杂化膜中回收的二氧化钛纳米粒子的表面和相关体积性质:一种新的尝试

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5 and 10 wt%-TiO_2-containing aramid-titania hybrid films were prepared using sol-gel processing improved by the inclusion of 3-isocyanato-propyltriethoxysilane (ICTOS) to strengthen bonding of the titania species to the polymer backbone and, hence, lessen its agglomeration. The films were thermally degraded by heating at 450 ℃ in a dynamic atmosphere of air. The solid residues were found by thermogravimetry, X-ray diffractometry and electron microscopy to consist dominantly of uniformly agglomerated rod-like anatase-TiO_2 nanoparticles, irrespective of the titania content of the film. The recovered titania particle morphology and surface microstructure were examined by field emission scanning and high-resolution transmission electron microscopy, respectively. Whereas, the particle surface chemistry and texture were assessed, respectively, by means of X-ray photoelectron spectroscopy and N_2 sorptiometry. The recovered titanias were found, irrespective of the film content of titania, to enjoy not only a high temperature (up to 800℃) stable nanoscopic anatase bulk structure, but also a high-temperature stable surface chemical composition (lattice Ti~(4+) and O~(2-), and adsorbed OH/ CH_X species), (101)-faceted microstructure and highly accessible (145-112 m~2/g), uniform mesoporous texture with average pore diameter in the narrow range of 3.9-6.3 nm. Increasing the calcination temperature up to 1100℃ enhances an anatase → rutile transition, the extent of which is larger the higher the titania content of the film.
机译:使用溶胶-凝胶工艺制备了5和10 wt%的含TiO_2的芳族聚酰胺-二氧化钛杂化膜,该工艺通过加入3-异氰酸根合丙基三乙氧基硅烷(ICTOS)来增强二氧化钛与聚合物主链的键合,从而减少了这种现象。它的聚集。薄膜在动态空气中于450℃加热而热降解。通过热重法,X射线衍射法和电子显微镜发现固体残留物,主要由均匀团聚的棒状锐钛矿-TiO_2纳米颗粒组成,而与膜的二氧化钛含量无关。通过场发射扫描和高分辨率透射电子显微镜分别检查了回收的二氧化钛颗粒形态和表面微观结构。而分别通过X射线光电子能谱和N_2吸光光度法评估了颗粒表面化学和织构。发现回收的二氧化钛,无论二氧化钛的膜含量如何,不仅具有高温(最高800℃)稳定的纳米锐钛矿整体结构,而且具有高温稳定的表面化学成分(晶格Ti〜(4+ )和O〜(2-)以及吸附的OH / CH_X物种),(101)切面的微结构和高度可及的(145-112 m〜2 / g),均匀的介孔织构,平均孔径在3.9的窄范围内-6.3 nm。将煅烧温度提高到1100℃会增强锐钛矿→金红石的转变,薄膜的二氧化钛含量越高,其程度越大。

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