Three-dimensional device (FinFET) doping requirements are challenging due to fin sidewall doping, crystallinity control, junction profile control, and leakage control in the fin. In addition, physical failure analyses of FinFETs can frequently reach a “dead end” with a No Defect Found (NDF) result when channel doping issues are the suspected culprit (e.g., high Vt, low Vt, low gain, sub-threshold leakage, etc.). In new technology development, the lack of empirical dopant profile data to support device and process models and engineering has had, and continues to have, a profound negative impact on these emerging technologies. Therefore, there exists a critical need for dopant profiling in the industry to support the latest technologies that use FinFETs as their fundamental building block [1]. Here, we discuss a novel sample preparation method for cross-sectional dopant profiling of FinFET devices. Our results show that the combination of low voltage (<500eV), shallow angle (~10 degree) ion milling, dry etching, and mechanical polishing provides an adequately smooth surface (Rq<5Å) and minimizes surface amorphization, thereby allowing a strong Scanning Capacitance Microscopy (SCM) signal representative of local active dopant (carrier) concentration. The strength of the dopant signal was found to be dependent upon mill rate, electrical contact quality, amorphous layer presence and SCM probe quality. This paper focuses on a procedure to overcome critical issues during sample preparation for dopant profiling in FinFETs.