A series of crystalline homometallic and heterometallic cobalt and nickel hydroxides and oxides were prepared using a continuous hydrothermal flow synthesis system. In all syntheses, the relevant metal salt solutions were pumped under high pressure to meet pH or other chemical modifiers (H2O2 or PVP) before the mixture was brought into contact with a feed of superheated (or supercritical) water, whereupon precipitation and particle growth occurred. The resulting nanoparticle (typically less than 100 nm in diameter) suspensions were collected from the outlet of the back-pressure regulator of the hydrothermal system. The collected suspensions were centrifuged, and the washed solids were freeze-dried prior to analyses. The nanopowders were characterized by a number of analytical methods including X-ray powder diffraction, Brunauer-Emmett-Teller (BET) surface area measurements, and simultaneous thermogravimetric analysis/differential scanning calorimetry.