This dissertation describes two-dimensional nuclear magnetic resonance theory and experiments which have been developed to study quadruples in the solid state. The technique of multiple-quantum magic-angle spinning (MQMAS) is extensively reviewed and expanded upon in this thesis. Specifically, MQMAS is first compared with another technique, dynamic-angle spinning (DAS). The similarity between the two techniques allows us to extend much of the DAS work to the MQMAS case. Application of MQMAS to a series of aluminum containing materials is then presented. The superior resolution enhancement through MQMAS is exploited to detect the five- and six-coordinated aluminum in many aluminosilicate glasses. Combining the MQMAS method with other experiments, such as HETCOR, greatly expands the possibility of the use of MQMAS to study a large range of problems and is demonstrated in Chapter 5. Finally, the technique switching-angle spinning (SAS) is applied to quadrupolar nuclei to fully characterize a quadrupolar spin system in which all of the 8 NMR parameters are accurately determined. This dissertation is meant to demonstrate that with the combination of two-dimensional NMR concepts and new advanced spinning technologies, a series of multiple-dimensional NMR techniques can be designed to allow a detailed study of quadrupolar nuclei in the solid state.

Thomson-scattering based x-ray radiation sources, in which a laser beam is scattered off a relativistic electron beam resulting in a high-energy x-ray beam, are currently being developed by several groups around the world to enable studies of dynamic material properties which require temporal resolution on the order of tens of femtoseconds to tens of picoseconds. These sources offer pulses that are shorter than available from synchrotrons, more tunable than available from so-called Ka sources, and more penetrating and more directly probing than ultrafast lasers. Furthermore, Thomson-scattering sources can scale directly up to x-ray energies in the few MeV range, providing peak brightnesses far exceeding any other sources in this regime. This dissertation presents the development effort of one such source at Lawrence Livermore National Laboratory, the Picosecond Laser-Electron InterAction for the Dynamic Evaluation of Structures (PLEIADES) project, designed to target energies from 30 keV to 200 keV, with a peak brightness on the order of 10{sup 18} photons {center_dot} s{sup -1} {center_dot} mm{sup -2} {center_dot} mrad{sup -2} {center_dot} 0.01% bandwidth{sup -1}. A 10 TW Ti:Sapphire based laser system provides the photons for the interaction, and a 100 MeV accelerator with a 1.6 cell S-Band photoinjector at the front end provides …