In this work, we used the depth resolution function (DRF) of the secondary ion mass spectrometry (SIMS) to deconvolve the boron depth profile of nanometer-thin embedded diamond layers. Thanks to an isotopic change within a thin layer, where carbon-12 (12C) and carbon-13 (13C) are substituted, the DRF was evaluated by a self-consistent algorithm. In a second step, this DRF was used to deconvolve the boron depth profile of a double delta-doped diamond analyzed under the same ion beam condition. The expected position, thickness, and boron concentration of the embedded layers were confirmed. This technique has enhanced the SIMS performance, and the depth resolution reached the nanometer range. Interfacewidths of boron-doped diamondmultilayerswere resolvedwell below 1 nm/decade over a large doping range, from 3 × 10^16 cm−3 to 1.2 × 10^21 cm−3, and confirmed a conformal growth layer by layer.