Beta-gallia rutile (BGR) intergrowths, generally expressed as Ga4Tin-4O2n-2, where n is an odd integer ≥ 5, are under investigation for their potential in photocatalytic and photovoltaic applications. Solid state reactions are the traditional processing method for these materials, however this method generally produces greater-than-micron sized powders. Because high surface area is needed for the envisioned application, a method that produces a smaller particle sizes is desired. In these experiments, we explore the use of hydrothermal synthesis for preparing BGR powders from various titanium-containing precursors, including titanium dioxide (rutile and anatase), titanium isopropoxide, and dihydrobis (ammonium lactato) titanium IV. Temperature, pressure, pH, and concentration variables were also modified to observe the effects on synthesized powders. Powder morphology was observed using SEM imaging, while particle size was determined using dynamic light scattering and surface area measurements. In addition, X-ray diffraction was used to determine phase purity and crystallite size.