X-ray and neutron scattering

Abstract:

We present a structural and magnetic study of two batches of polycrystalline LiNi_0.8Mn_0.1Co_0.1O₂ (commonly known as Li NMC 811), a Ni-rich Li ion battery cathode material, using elemental analysis, X-ray and neutron diffraction, magnetometry, and polarized neutron scattering measurements. We find that the samples, labeled S1 and S2, have the composition Li_1-xNi_0.9+x-yMn_yCo_0.1O₂, with x = 0.025(2), y = 0.120(2) for S1 and x = 0.002(2), y = 0.094(2) for S2, corresponding to different concentrations of magnetic ions and excess Ni²⁺ in the Li⁺ layers. Both samples show a peak in the zero-field-cooled (ZFC) dc susceptibility at 8.0(2) K, but the temperature at which the ZFC and FC (field-cooled) curves deviate is substantially different: 64(2) K for S1 and 122(2) K for S2. The ac susceptibility measurements show that the transition for S1 shifts with frequency whereas no such shift is observed for S2 within the resolution of our measurements. Our results demonstrate the sample dependence of magnetic properties in Li NMC 811, consistent with previous reports on the parent material LiNiO₂. We further establish that a combination of experimental techniques is necessary to accurately determine the chemical composition of next-generation battery materials with multiple cations.

Abstract:

Metal-organic framework (MOF) glasses have become a subject of interest as a distinct category of melt quenched glass, and have potential applications in areas such as ion transport and sensing. In this paper we show how MOF glasses can be combined with inorganic glasses in order to fabricate a new family of materials composed of both MOF and inorganic glass domains. We use an array of experimental techniques to propose the bonding between inorganic and MOF domains, and show that the composites produced are more mechanically pliant than the inorganic glass itself.

Abstract:

The book contains a comprehensive account of the theory and application of neutron scattering for the study of the structure and dynamics of condensed matter. All the principal experimental techniques available at national and international neutron scattering facilities are covered. The formal theory is presented, and used to show how neutron scattering measurements give direct access to a variety of correlation and response functions which characterize the equilibrium properties of bulk matter. The determination of atomic arrangements and magnetic structures by neutron diffraction and neutron optical methods is described, including single-crystal and powder diffraction, diffuse scattering from disordered structures, total scattering, small-angle scattering, reflectometry, and imaging. The principles behind the main neutron spectroscopic techniques are explained, including continuous and time-of-flight inelastic scattering, quasielastic scattering, spin-echo spectroscopy, and Compton scattering. The scattering cross-sections for atomic vibrations in solids, diffusive motion in atomic and molecular fluids, and single-atom and cooperative magnetic excitations are calculated. A detailed account of neutron polarization analysis is given, together with examples of how polarized neutrons can be exploited to obtain information about structural and magnetic correlations which cannot be obtained by other methods. Alongside the theoretical aspects, the book also describes the essential practical information needed to perform experiments and to analyse and interpret the data. Exercises are included at the end of each chapter to consolidate and enhance understanding of the material, and a summary of relevant results from mathematics, quantum mechanics, and linear response theory, is given in the appendices.