The preparation of hard material samples with the necessary size and shape is critical to successful material analysis. X-ray nanotomography requires that samples are sufficiently thin for X-rays to pass through the sample during rotation for tomography. One method for producing samples that fit the criteria for X-ray nanotomography is focused ion beam/scanning electron microscopy (FIB/SEM) which uses a focused beam of ions to selectively mill around a region of interest and then utilizes a micromanipulator to remove the milled-out sample from the bulk material and mount it on a sample holder. In this article the process for preparing X-ray nanotomography samples in multiple shapes and sizes is discussed. Additionally, solid-oxide fuel cell anode samples prepared through the FIB/SEM technique underwent volume-independence studies for multiple properties such as volume fraction, average particle size, tortuosity and contiguity to observe the characteristics of FIB/SEM samples in X-ray nanotomography.