Zonal and sectorial heterogeneities in natural diamonds provide information on the growth conditions and post-growth changes. Cathodoluminescence (CL) microscopy revealed these heterogeneities in a very detailed manner with high spatial resolution. In this study, factors affecting the CL images of two natural diamonds were analyzed and the results of cathodoluminescence studies in steady-state (SS-CL) and scanning modes were compared. SS-CL was observed using an optical microscope, and scanning mode was evaluated via SEM (SEM-CL). It was demonstrated that the relative brightness of the <111> and <100> growth sectors in diamond crystals depends on the nature of defects in them and on the method of image detection (steady-state/scanning versus color/panchromatic). The differences between SS-CL and SEM-CL images can be attributed to the kinetics of luminescence and spectral sensitivity of the detectors. It was established that the nature of lattice defects around small inclusions can be changed (e.g., the intensity of blue luminescence from nitrogen-vacancy defects (N3V) decreases due to their transformation into nitrogen–hydrogen defects (N3VH). The hydrogen disproportion between the sectors is caused by different growth mechanisms. Hydrogen atoms in the diamond matrix can affect the kinetics of transformation of the defects by transforming a part of N3V to N3VH.
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