Lithium ion batteries have become ubiquitous in the modern world, powering devices such as cellular phones and vehicles. This thesis seeks to improve the powder X-ray diffraction capabilities of a combined X-ray absorption spectroscopy and powder X-ray diffraction (PXRD) experimental setup, used for investigating lithium ion battery cathode materials, at the Hard X-ray MicroAnalysis beamline in the Canadian Light Source. Determination of the atomic structure of ex situ orthosilicate cathode materials via Rietveld refinement is a goal, and provides a data quality benchmark for the improved setup. Instrumentation assembled for the improvement of the PXRD data, and equipment allowing for elevated temperature in situ measurements are discussed. And, the structure and polymorphism of Li2MSiO4 (M = Fe, Mn) from varying synthesis conditions is also explored.