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Magnetic resonance studies on amorphous and crystalline lanthanum aluminoborates

机译:非晶和结晶铝硼酸镧的磁共振研究

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The development of an LaAl_(2.03)B_4O_(10.5) (124) crystalline phase from amorphous xerogels and glasses doped with iron and gadolinium has been characterised by magic angle spinning nuclear magnetic resonance (MAS NMR) and electron paramagnetic resonance (EPR) spectroscopies. The crystallisation of amorphous precursors takes place between 760 and 860 deg C in the case of xerogels and around 1000 deg C for glasses. The magnetic resonance results indicate that the local structure dramatically changes when crystalline phases are developed in amorphous precursors. The major changes are evidenced in the boron environment. In amorphous precursors boron atoms are predominantly three-coordinated, while in the crystalline samples almost only tetra-coordinated species are detected. As regards aluminium, it occurs in amorphous samples as hexa-, penta- and tetra-coordinated, while in the crystalline samples it appears preponderantly penta-coordinated. Three different sites for Fe~(3+) ions were identified in crystalline samples by EPR measurements with only one preponderant site for Gd~(3+) ions.
机译:LaAl_(2.03)B_4O_(10.5)(124)晶相由非晶态干凝胶和掺杂铁和g的玻璃形成,其特征在于魔角旋转核磁共振(MAS NMR)和电子顺磁共振(EPR)光谱。在干凝胶的情况下,无定形前体的结晶发生在760至860摄氏度之间,对于玻璃而言,发生在1000摄氏度左右。磁共振结果表明,当在非晶态前体中形成结晶相时,局部结构会发生巨大变化。硼环境已证明存在重大变化。在非晶态前体中,硼原子主要是三配位的,而在晶体样品中,几乎只检测到四配位的物种。关于铝,它在无定形样品中以六,五和四配位形式出现,而在结晶样品中,它以五配位形式出现。通过EPR测量在晶体样品中鉴定出Fe〜(3+)离子的三个不同位点,而Gd〜(3+)离子仅一个优势位点。

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