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A new method for characterizing lithium niobate +/-Z ferroelectric polarization domains using Auger electron spectroscopy (AES) is presented. The domains of periodically poled samples are found to be differentiable using the peak amplitude of the Auger oxygen KLL transition, with -Z domains having a larger peak-amplitude as compared to +Z domains. The peak amplitude separation between domains is found to be dependent on the primary beam current, necessitating a balance between the insulating samples charging under the primary beam and achieving sufficient signal to noise in amplitude separation. AES amplitude-based domain characterization is demonstrated for fields of view (FOV) ranging from 1 $\mathrm{\mu <\#comment/>}$m to 78 $\mathrm{\mu <\#comment/>}$m. Domain spatial resolution of 91 nm is demonstrated at 1 $\mathrm{\mu <\#comment/>}$m FOV. 

Auger electron spectroscopy (AES) as a method to characterize the ferroelectric polarization domains in magnesium-doped lithium niobate crystals is demonstrated. Preliminary measurements on a test sample show a clearly identifiable relative shift in the energy of the Auger oxygen KLL transition peak between poled (inverted) and un-poled domains. Auger electrons detected from the negative polarization domains (-Z) have a higher energy than those from the positive domains indicating a lower ionization energy at the -Z domain surface. The degree of electron energy separation between the −Z and +Z domains was found to be dependent on proximity to the domain boundary and was potentially diminished by the accumulated charge under the incident primary beam. Polarization domain resolution is demonstrated on both the micron and millimeter scale, suggesting potential applicability of this technique to surface investigation and domain structure characterization of nonlinear optical devices such as periodically poled lithium niobate.