Ammonia absorption in calcium graphite intercalation compound: in situ neutron diffraction, Raman spectroscopy and magnetization.

Ammonia absorption in calcium graphite intercalation compound: in situ neutron diffraction, Raman spectroscopy and magnetization.
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钙石墨插层化合物中的氨吸收:原位中子衍射、拉曼光谱和磁化。

DOI:
10.1039/b917992e
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发表时间:
2010
期刊:
PCCP
影响因子:
--
通讯作者:
Srinivas G
Srinivas G
中科院分区:
--
文献类型:
--
作者:
Srinivas G

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利用原位飞行时间中子衍射、拉曼光谱和磁化研究了氨化钙石墨插层化合物(Ca-GIC)的结构和超导性能。氨吸收是通过将预制的Ca-GIC暴露在不同压力下的氨蒸气中进行的。我们的原位中子衍射数据揭示了一个复杂的氨压力依赖的结构转变,其中二次氨化Ca-GIC相的生长以原始的CaC6和石墨为代价。氨的吸收本质上是不可逆的,在高温下对样品脱气导致酰胺钙和氢的形成。拉曼光谱和磁化研究表明,氨吸收不仅导致了较大的堆积无序,而且还降低了超导CaC6相分数。最后,我们提出了一个分子堆积模型,该模型考虑了观察到的氨吸收和伴随的结构相变。
The structure and superconducting properties of ammoniated calcium–graphite intercalation compound (Ca-GIC) have been investigated using in situ time-of-flight neutron diffraction, Raman spectroscopy and magnetization studies. Ammonia absorption has been carried out by exposing preformed Ca-GIC to ammonia vapour at various pressures. Our in situ neutron diffraction data reveal a complex ammonia pressure dependent structural transformation, in which the growth of secondary ammoniated Ca-GIC phases are observed at the expense of the pristine CaC6 and graphite. The ammonia absorption is irreversible in nature, and degassing the sample at elevated temperature leads to the formation of calcium amide and hydrogen. The Raman spectroscopy and magnetization studies show that the ammonia absorption not only leads to a large stacking disorder, but it also reduces the superconducting CaC6 phase fraction. Finally, we propose a molecular stacking model which accounts for the observed ammonia absorption and concomitant structural phase transitions.
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