3D Imaging of Nanoparticles in an Inorganic Matrix Using TOF-SIMS Validated with STEM and EDX

Imaging nano-objects in complex systems such as nanocomposites using time-of-flight secondary ion mass spectrometry (TOF-SIMS) is a challenging task. Due to a very small amount of the material and a matrix effect, the number of generated secondary ions can be insufficient to represent a 3D elemental distribution despite being detected in a mass spectrum. Therefore, a model sample consisting of a ZrCuAg matrix with embedded Al nanoparticles is designed. A high mass difference between the light Al and heavy matrix components limits mass interference. The chemical structure measurements using a pulsed 60 keV Bi₃²⁺ beam or a continuous 30 keV Ga⁺ beam reveals distinct Al signal segregation. This can indicate a spatially resolved detection of single 10s of nanometer large particles and/or their agglomerates for the first time. However, TOF-SIMS images of 50 nm or smaller objects do not necessarily represent their exact size and shape but can rather be their convolutions with the primary ion beam shape. Therefore, the size of nanoparticles (25-64 nm) was measured using scanning transmission electron microscopy. Our studies prove the capability of TOF-SIMS to image chemical structure of nanohybrids which is expected to help building new functional materials and optimize their properties.