Low voltage and variable-pressure scanning electron microscopy of fractured composites.
ABSTRACT Uncoated fracture surfaces of carbon-epoxy composites are investigated using a variable-pressure environmental scanning electron microscope (VP-ESEM), under optimized conditions for topographic description, image quality and sample preservation. Always using freeware or open source programs, parameters for low-voltage and low vacuum are stipulated with the support of Monte Carlo simulations combined to topographic measurements, tailoring the VP-ESEM setup for visualization of fine relief details. Based on topographic information from atomic force microscope (AFM) images, finest fracture steps were measured. These were the references to optimize and define boundaries for applied beam voltages and chamber pressures, restricted by the beam penetration depth and gas-electron interactions, guided by Monte Carlo simulations and signal-to-noise measurements. For VP mode, ideal chamber pressure was found around 30-40Pa at 3keV beam voltage and 6mm working distance. Lower pressures will cause noise due to electron charging and gas excess provokes resolution degradation and noise due to positive charging and electron beam scattering, raising the skirt radius. When a larger working distance is necessary, it can be compensated by adjusting the detector bias and the probe current, or even lowering chamber pressure, but the signal-to-noise ratio will certainly change. Monte Carlo simulations provided a good approach to optimize imaging conditions under low vacuum and low voltage for fractographic analysis of carbon-epoxy composites.
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ABSTRACT: A LEO SUPRA 35VP FESEM has been modified to significantly improve image quality in the low pressure mode of operation. It is further shown that the same conversion can allow the machine to operate also as a fully fledged environmental scanning electron microscope with specimen chamber pressures in excess of 2000Pa. This is achieved by a diamagnetic insert with a thin pressure limiting aperture at the bottom of the pole-piece. The insert allows the use of various size apertures in addition to the existing 1mm differential diaphragm.Micron 07/2012; 44. DOI:10.1016/j.micron.2012.06.014 · 2.06 Impact Factor
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ABSTRACT: The methodology for fracture analysis of polymeric composites with scanning electron microscopes (SEM) is still under discussion. Many authors prefer to use sputter coating with a conductive material instead of applying low-voltage (LV) or variable-pressure (VP) methods, which preserves the original surfaces. The present work examines the effects of sputter coating with 25 nm of gold on the topography of carbon-epoxy composites fracture surfaces, using an atomic force microscope. Also, the influence of SEM imaging parameters on fractal measurements is evaluated for the VP-SEM and LV-SEM methods. It was observed that topographic measurements were not significantly affected by the gold coating at tested scale. Moreover, changes on SEM setup leads to nonlinear outcome on texture parameters, such as fractal dimension and entropy values. For VP-SEM or LV-SEM, fractal dimension and entropy values did not present any evident relation with image quality parameters, but the resolution must be optimized with imaging setup, accompanied by charge neutralization. SCANNING 00: 1-9, 2012. © 2012 Wiley Periodicals, Inc.Scanning 05/2013; 35(3). DOI:10.1002/sca.21048 · 1.44 Impact Factor