Analysis of Water Ice in Nanoporous Copper Needles Using Cryo Atom Probe Tomography

The application of atom probe tomography (APT) to frozen liquids is limited by difficulties in specimen preparation. Here, we report on the use of nanoporous Cu needles as a physical framework to hold water ice for investigation using APT. Nanoporous Cu needles are prepared by electropolishing and dealloying Cu–Mn matchstick precursors. Cryogenic scanning electron microscopy and focused ion beam milling reveal a hierarchical, dendritic, highly wettable microstructure. The atom probe mass spectrum is dominated by peaks of Cu+ and H(H2O)n+ up to n ≤ 3, and the reconstructed volume shows the protrusion of a Cu ligament into an ice-filled pore. The continuous Cu ligament network electrically connects the apex to the cryostage, leading to an enhanced electric field at the apex and increased cooling, both of which simplify the mass spectrum compared to previous reports.