Rutherford backscattering spectrometry is a primary reference method for the quantity of materials, but has a limit‐of‐detection (LOD) presently at ∼1015 at/cm2 for analyses with traceable accuracy near 1%. A multidetector assembly is demonstrated which increases the count rate without decreasing the signal/noise due to pulse pile-up. A LOD of 6 × 1012 at/cm2 is achieved with the multidetector assembly and applied to quantify the onset of an atomic layer deposition (ALD) process for an in-depth study of the growth selectivity of ALD Ru on a‐C:H and on SiCN. Besides, the spectrometer enables <10 min measurements on a Ru layer of 2.7 nm, permitting wafer mapping.

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