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首页> 外文期刊>Journal of Materials Science >Electron spin resonance study of Mo(V) ion species incorporated into aluminosilicate nanospheres with solid core/mesoporous shell structure
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Electron spin resonance study of Mo(V) ion species incorporated into aluminosilicate nanospheres with solid core/mesoporous shell structure

机译：具有固态核/介壳结构的铝硅酸盐纳米球中Mo（V）离子物种的电子自旋共振研究

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摘要

Silica spheres with sub-micrometer sized solid core and mesoporous shell (SCMS) structure were synthesized, and aluminum was incorporated into the mesoporous shell framework by impregnation method to generate SCMS aluminosilicate (AlSCMS) nanospheres. The impregnation of aluminum into the SCMS spheres generates the acid sites on the framework due to the presence of Al3+ ions. The AlSCMS was then used to support molybdenum ion species on the mesoporous shell framework. A solid-state reaction of MoO3 with AlSCMS followed by thermal reduction generated paramagnetic Mo(V) species. The dehydration produced a Mo(V) species that is characterized by electron spin resonance with g e > g ⊥ > g ||. The structural properties of active sites in the AlSCMS were characterized by means of XRD, UV–Vis, 27Al MAS NMR, FT-IR, and energy dispersive X-ray spectrometric measurements. Upon O2 adsorption, the Mo(V) ESR signal intensity decreased, and a new O2 − radical was generated. The Mo species in the dehydrated Mo-AlSCMS is found to exist as oxo-molybdenum species, (MoO2)+ or (MoO)3+. Since the AlSCMS has a low framework negative charge, the MoO2 + with a low positive charge can be easily stabilized and thus seems to be more probable in the AlSCMS framework.
机译：合成了具有亚微米级固体核和介孔壳（SCMS）结构的二氧化硅球，并通过浸渍法将铝掺入介孔壳骨架中，生成了SCMS硅铝酸盐（AlSCMS）纳米球。由于Al 3 + 离子的存在，铝浸入SCMS球中会在骨架上产生酸位。然后将AlSCMS用于在中孔壳骨架上支撑钼离子物种。 MoO 3 与AlSCMS固相反应，然后热还原生成顺磁性Mo（V）物种。脱水产生了一个Mo（V）物种，其特征是电子自旋共振，其中g e ⊥ || 。通过XRD，UV-Vis， 27 Al MAS NMR，FT-IR和能量色散X射线光谱分析对AlSCMS活性位的结构进行了表征。吸附O 2 后，Mo（V）ESR信号强度降低，并生成新的O 2 -自由基。发现脱水的Mo-AlSCMS中的Mo物种为（-MoO 2 ） + 或（MoO） 3 + 。由于AlSCMS具有较低的框架负电荷，因此具有较低正电荷的MoO 2 + 可以很容易地稳定下来，因此在AlSCMS框架中似乎更有可能。

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