Effect of ion milling on the perceived maturity of shale samples: Implications for organic petrography and SEM analysis

Sample polishing by argon ion beam is a widely used method for examining shale samples for inherent porosity characteristics; the high quality of these surfaces suggests that this technique may also be used for optical reflectance measurements to provide information about the thermal maturity of samples. Yet, the inevitable surface heating that this polishing method engenders has raised concerns that the measured reflectance properties are no longer those of the original sample. To explore the impact of ion milling on the maturity of shale samples as measured by vitrinite and solid bitumen reflectance, five different ion milling configurations were applied to a set of organic-rich New Albany Shale (Late Devonian-Early Mississippian) samples that range in maturity from immature to post-mature. Using two ion mill designs, edge milling vs planar milling, single and dual ion beams, variable acceleration voltages, and milling at room temperature vs samples cooled by liquid nitrogen, provided a wide range of beam heating scenarios. Reflectance of macerals was measured before and after ion milling to investigate whether and to what extent various ion-milling approaches change the reflectance values, and by extension the perceived thermal maturity of organic matter in these samples. Our results demonstrate that more aggressive milling methods, such as the use of multiple beams and higher acceleration voltages elevate reflectance values, and that this effect is most pronounced in immature samples and diminishes for samples of increasing original maturity. Specifically, for the two least mature samples, the most aggressive milling method (configuration D) increased reflectance of vitrinite from 0.48% to 0.58%, and from 0.58% to 0.74%. Increase of reflectance (perceived maturity) can be counteracted by reducing beam intensity (e.g., fewer beams, lower voltage) and cooling of samples with liquid nitrogen. The severity of heating artifacts depends partially on the ion mill design, and non-damaging settings must be determined experimentally for a given ion mill model. Because thermal alteration of organic matter typically involves the expulsion of volatiles, there is also a danger that ion beam heating of immature and oil window samples can skew the porosity characteristics of shale samples. Thus, determining non-damaging ion mill settings has the dual benefit of avoiding measuring false maturity levels and misleading porosity characteristics.