Effect of electrical charging on scanning electron microscopy-energy dispersive X-ray spectroscopy analysis of insulating materials

• In SEM-EDX analysis, ionic liquid prevents charging below probe current of 100 nA.
• Ionic liquid provides suitable qualitative value at probe current of 10 nA.
• Cu·K and Zr·L lines were detected in charged samples in SEM-EDX analysis.

We investigated the conditions under which we can obtain reasonable qualitative results in scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDX) analysis of trace elements in insulating materials using a diluted ionic liquid (EMI-CH3COO) and changing probe current. Below 100 nA, electrical charging of insulating materials was prevented. The probe current of 10 nA was suitable for qualitative analysis because the intensities of peaks from these materials were strong enough to detect trace elements at the concentration of 0.1 wt.% in the sample without interference by sum peaks. Diluted EMI-CH3COO can also be used for SEM-EDX quantitative analysis of insulating materials as discharging agents. In contrast, when insulating materials were electrically charged, the obtained spectra contained characteristic X-rays of the insulating materials with low energies and of materials other than the samples such as the sample stage and the collimator in the X-ray detector. This is because electrons from the electron beam were decelerated by and deflected from the insulating materials. By coating the insulating materials with the diluted EMI-CH3COO, the deceleration and deflection of the electron beam were prevented.