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An in situ XAS study on the incorporation of metal ions into AlPO4-5 framework in hydrothermal synthesis process

机译:水热合成过程中金属离子掺入AlPO4-5骨架的原位XAS研究

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The in situ X-ray Absorption Spectroscopy (XAS) was employed to probe the incorporation of transition metal ions, such as Mn2+, Fe3+, Co2+ and Ni2+, from precursor gel to AlPO4-5 framework in hydrothermal synthesis process. With the crystallization, the number of coordinated oxygen around metal ions changes from 6 to 4, associated with a decrease in the coordination distance of metal ions to oxygen, as revealed by XAS. However, these metal ions are different in the incorporation behaviour and mechanism. The transition of Co2+ into the tetrahedral framework of AlPO4-5 is completed at 150 oC with the emergence of longrange ordered microporous structure, while the incorporation of Mn2+ and Fe3+ is much more difficult and starts after the build-up of microporous structure. On the other hand, the existence of Si4+ in the precursor gel has also considerable influences on the synthesis process.
机译:利用原位X射线吸收光谱法(XAS)研究了水热合成过程中从前体凝胶到AlPO4-5骨架的过渡金属离子如Mn2 +,Fe3 +,Co2 +和Ni2 +的掺入。通过结晶,如XAS所示,金属离子周围的配位氧数从6变为4,这与金属离子与氧的配位距离减小有关。但是,这些金属离子的结合行为和机理不同。随着长程有序微孔结构的出现,Co2 +过渡到AlPO4-5的四面体构架完成,而Mn2 +和Fe3 +的引入要困难得多,并且要在微孔结构建立后才能开始。另一方面,前体凝胶中Si4 +的存在对合成过程也有相当大的影响。

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