Introducing fluorocarbon vapor in the air above an aqueous dispersion of clusters of nanodiamonds induces their disaggregation, a prerequisite for most of their biomedical uses. Furthermore, the fluorocarbon gas promotes the adsorption of nanodiamonds at the gas/water interface. As an example of the benefits that can be gained from our findings relative to the implementation of nanomaterials for practical uses, we investigated the role that the fluorocarbon gas may play in the generation of microbubbles, which are currently actively investigated in ultrasound-mediated diagnosis and therapy. Remarkably, the fluorocarbon gas enables the production of microbubbles shelled only with nanodiamonds, in the absence of any other surfactant, which could not be achieved without the fluorocarbon being present. This demonstrates that a supernatant gas can decisively affect the adsorption of nanoparticles from an aqueous phase to an air/water interface, likely through physical adsorption at the nanodiamond surface. The investigations involved solid-state NMR and FTIR, microbubble generation experiments with acoustic attenuation monitoring, and bubble profile analysis tensiometry on spontaneously adsorbed Gibbs films. Perspectives include control of aggregation of nanodiamonds and their retrieval from aqueous dispersions and applications in multimodal diagnostic imaging, bioimaging, and therapeutic cell tracking. It is proposed that the disaggregating potency of fluorocarbons can be applied to other nanomaterials, providing a simple and effective means of alleviating aggregation.