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The use of a solvothermal process for the synthesis of tantalum carbide (TaC) and lanthanum hexaboride (LaB6) powders in fused-quartz test tubes is reported in order to demonstrate the synthesis of these powders using thermal and chemical ignition techniques and to prove that the process is of a self-propagating high-temperature synthesis type, obviating the need for an autoclave. X-ray powder diffraction showed phase pure powders with crystallite sizes of 25 and ∼80 nm, while dynamic light scattering showed average particle sizes of 97 and ∼130 nm, for TaC and LaB6, respectively. The data demonstrates that the powders have a very low level of agglomeration. Scanning electron microscopy shows that the TaC powders have a spherical morphology, while the LaB6 powders have a mixture of cubic and spherical morphologies.