The variable pressure scanning electron microscope (VP-SEM) allows imaging of insulators without the need for a conductive coating, due to charge neutralization at the surface from recombination of positive ions and surface electrons. Varying certain parameters such as pressure, bias, and working distance creates incomplete neutralization, and localized charging develops called charge contrast. Although the exact mechanism creating charge contrast imaging (CCI) is unknown, it is agreed that it is related to an optimum charge compensation. The behavior of the CCI is still vague, which presents a problem for determining the mechanisms. This article provides user-friendly methods of finding the optimum levels of charge contrast in the VP-SEM. We show that the CCI is obtained at optimum operating conditions where the specimen current is between 2.5 nA and 3.5 nA. The specimen current is a function of secondary electrons (SE) emission and ionization potential, producing an ion flux. Therefore an optimum specimen current represents the balanced conditions of SE emission and ion flux. Controlling the pressure, working distance, bias, scan rate, and beam current allows the microscopist to set the specimen current at this optimum level for charge contrast imaging. All the work was performed on gibbsite using the S3000N VP-SEM from Hitachi.

In variable pressure scanning electron microscopy (VPSEM) the current data suggests that considerable caution is required in the interpretation of X-ray data from nonconductive samples, depending on the operating conditions. This article reviews some of the documented approaches and presents data that illustrate the nature and magnitude of the effects of charge above, on, and in the sample on the detected X-ray emissions from the sample and from elsewhere within the VPSEM specimen chamber. The collection of reliable and reproducible X-ray data has been found to require relatively high specimen chamber gas pressures, at the upper end of or beyond the available pressures for most VPSEMs. It is also shown that sample characteristics, including composition, strongly influence local charge effects, which can significantly affect the primary electron landing energy and consequently the resultant emitted X-ray signal under low pressure environments.

Charge contrast images (CCI) of synthetic gibbsite obtained on an environmental scanning electron microscope gives information on the crystallization process. Furthermore, X-ray mapping of the same grains shows that impurities are localized during the initial stages of growth and that the resulting composition images have features similar to these observed in CCI. This suggests a possible correlation between impurity distributions and the emission detected during CCI. X-ray line profiles, simulating the spatial distribution of impurities derived from the Monte Carlo program CASINO, have been compared with experimental line profiles and give an estimate of the localization. The model suggests that a main impurity, Ca, is depleted from the solution within approximately 3–4 μm of growth.