Nanoparticles produced from gallium-based liquid metal alloys have been explored for developing applications in the fields of electronics, catalysis, and biomedicine. Nonetheless, physical properties, such as phase behavior at micro-/nanosize scale, are still significantly underexplored for such nanoparticles. Here, we conduct an in situ investigation of phase behavior for gallium-based liquid metal nanoparticles and discover the unprecedented coexistence of solid particles in spherical liquid metal shells without the support of a crystalline substrate. The particles can also transform into solid Janus nanoparticles after temperature cycling. In addition, we investigate the optical properties of the nanoparticles before and after phase separation using in situ electron energy-loss spectroscopy. Most importantly, we discover that increasing the content of indium within the nanoparticle can stabilize the solid-core/liquid-shell structure at room temperature. This study provides a foundation to engineer liquid metal nanoparticles for developing new applications in nanoscale optical platforms and shape-configurable transformers.Although various electronic, chemical, and biomedical applications have been demonstrated for nanoparticles made from gallium-based liquid metal alloys, fundamental physical properties such as phase behavior of such nanoparticles are still significantly underexplored. Here, Tang and coworkers present the in situ investigation of phase separation in binary and ternary spherical liquid metal nanoparticles upon cooling, and demonstrate the coexistence of solid core/liquid shell without the support of a crystalline substrate. This study provides insight into engineering such nanoparticles for the development of new applications.Despite gallium-based liquid metal alloys attracting extensive attention for various applications, their phase behavior at the nanoscale is still underexplored. Understanding the impact of phase separation in nanoparticles can be extremely useful for developing new structures and exploring suitable applications. Here, we report on the investigation of phase behavior for spherical nanoparticles made from gallium-based liquid metal alloys upon cooling. We discover the thermally stable coexistence of solid cores in spherical liquid metal shells without the support of a crystalline substrate at room temperature. Given the unique properties of liquid metal, together with the facile process for producing core-shell and Janus nanoparticles, this work will encourage further investigation of the properties of such nanoparticles for developing applications in the fields of electronics, catalysis, nanomedicine, and beyond.
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