摘要： Due to their electrical and physical properties, Si1?XGeX materials are widely used in microelectronic devices. In particular, the Ge component found within Si1?XGeX compounds is important for enhancing carrier mobility and altering the lattice constant of metal-oxide-semiconductor field-effect transistors. In this study, magnetic sector secondary ion mass spectrometry (magnetic sector SIMS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) were used to determine the accurate concentrations of major compositions present within binary alloy samples. However, quantitative SIMS analysis is limited by the matrix effect, which influences the sputter yield of an element in a compound and alters the secondary ionization yields. Quantitative deviations that were due to the matrix effect were reduced by using Cs cluster ions (MCs+ and MCs2+) instead of elemental ions; the SIMS results using the elements were, therefore, compared with those using MCs+ and MCs2+ cluster ions. In the case of Fe1?XNiX alloys that have a less matrix effect compared to Si1?XGeX alloys, both the Cs primary ion beam (Cs+) and an oxygen primary ion beam (O2+) were used to measure the Fe1?XNiX compositions. The quantitative results from the two different primary ion beams were then compared to understand the ionization process. Deviations in the quantitative values gained with the O2+ beam were lower than those obtained using the Cs+ primary ions, meaning that using oxygen as the primary ion improves the accuracy in quantifying Fe1?XNiX compounds. Other reliable tools for analysis such as atom probe tomography and femtosecond laser ablation inductively coupled plasma mass spectrometry were also used in the quantitative analysis, with results that were consistent with the most accurate results obtained using magnetic sector SIMS and ToF-SIMS.