The present work, performed by means of ex-situ neutron diffraction measurements and combined with complementary Raman data, reports the first structural characterization of the recovered hydrogen hydrate during the transformation from the C₀ phase to ice XVII. The measurement of the position of the Bragg reflections in the neutron data allows to obtain the behaviour of the lattice parameters for the C₀ filled ice as a function of temperature during hydrogen release. From this analysis, we demonstrate the irreversibility of the structural changes passing from the pristine filled hydrate to the empty one, i.e. ice XVII. Meanwhile, we observe also the release of the spurious nitrogen molecules previously absorbed by the hydrate crystal when recovered at low temperature and ambient pressure. A significant release of guest molecules starts around 60 K, reaching the complete evacuation of the water structure above 100 K.

通过异位中子衍射测量并结合互补的拉曼数据进行的本工作报告了从C ₀相转变为冰XVII期间回收的水合氢的第一结构特征。中子数据中布拉格反射位置的测量允许获得C ₀晶格参数的行为氢气释放过程中填充的冰与温度的关系。从这一分析中，我们证明了从原始填充的水合物到空的水合物（即冰XVII）的结构变化的不可逆性。同时，当在低温和环境压力下回收时，我们还观察到先前被水合物晶体吸收的杂散氮分子的释放。客体分子大量释放开始于60 K左右，直至100 K以上的水结构完全排空。