Critical Considerations for TOF‐SIMS Sample Preparation and Parameter Optimization

Rationale Time‐of‐flight secondary ion mass spectrometry (TOF‐SIMS) is an ultrasensitive surface analysis technique capable of providing comprehensive elemental and molecular characterization of sample surfaces. The selection of appropriate sample preparation methods and optimal instrument parameters is critical for obtaining accurate and reliable analytical results. Methods This article systematically discusses three key aspects of the TOF‐SIMS surface analytical technique: essential considerations in sample preparation, optimization of spectral acquisition parameters, and configuration of depth profiling parameters. Results Through representative case studies, we elucidate the fundamental principles and practical considerations for TOF‐SIMS sample preparation and measurement optimization, thereby establishing a framework for acquiring high‐quality TOF‐SIMS data. Conclusions Sample preparation and processing are critical for ensuring the validity of TOF‐SIMS detection results, while selecting appropriate testing parameters facilitates the acquisition of authentic and valid sample information. The presented methodology in this paper serves as a valuable reference for ensuring data reliability in TOF‐SIMS analyses.