Advantages of stereo imaging of metallic surfaces with low voltage backscattered electrons in a field emission scanning electron microscope

High emission current backscattered electron (HC-BSE) stereo imaging at low accelerating voltages (≤ 5 keV) using a field emission scanning electron microscope was used to display surface structure detail. Samples of titanium with high degrees of surface roughness, for potential medical implant applications, were imaged using the HC-BSE technique at two stage tilts of + 3° and − 3° out of the initial position. A digital stereo image was produced and qualitative height, depth and orientation information on the surface structures was observed. HC-BSE and secondary electron (SE) images were collected over a range of accelerating voltages. The low voltage SE and HC-BSE stereo images exhibited enhanced surface detail and contrast in comparison to high voltage (> 10 keV) BSE or SE stereo images. The low voltage HC-BSE stereo images displayed similar surface detail to the low voltage SE images, although they showed more contrast and directional sensitivity on surface structures. At or below 5 keV, only structures a very short distance into the metallic surface were observed. At higher accelerating voltages a greater appearance of depth could be seen but there was less information on the fine surface detail and its angular orientation. The combined technique of HC-BSE imaging and stereo imaging should be useful for detailed studies on material surfaces and for biological samples with greater contrast and directional sensitivity than can be obtained with current SE or BSE detection modes.     

Tilt dependence of the secondary electron emission at low excitation energy

Influence of the specimen's slope on the secondary electron emission has been experimentally studied. Strong deviations from the inverse cos law have been observed and corresponding phenomenological equation (taking into account this deviation) is suggested. The consequences of the dependence on the topography contrast of low- and high-voltage scanning electron microscopy (SEM) image, especially for three-dimensional (3-D) reconstruction, are considered.     

Choosing the optimum accelerating voltage (EO) to visualize submicron precipitates with a field emission scanning electron microscope

With the advent of field emission scanning electron microscopes (FESEM), the observation of small phases in the 5 to 50 nm range seems to be possible at low accelerating voltage using backscattered electron imaging mode. In this context, it is important to understand the contrast of multiphased materials at such low energy. A Monte Carlo program to simulate electron trajectories of multiphased materials (CASINO) was used to compute electron backscattering images. Simulations of images for various compositions of spherical precipitates embedded in a homogeneous matrix as a function of precipitate size and accelerating voltage are presented. These simulations show the concept of an optimum accelerating voltage to maximize the contrast of electron backscattering images. The results presented in this paper show that the contrast of backscattering images of multiphased images in the scanning electron microscope is not only a function of the atomic number difference, but that it is also strongly related to the geometry and the size of the phases.     

Development of high-resolution field emission scanning electron microscopy with multifunctions for chargeless observation of nonconducting surface

We have developed a fully digital field emission scanning electron microscope (FE-SEM) with multifunctions to compensate the charging up of nonconducting surfaces. High-voltage observation, minimum electron dose, variable scanning speed, averaging, integration, tuning of surface potential, and cyclotron movements of secondary electrons have been achieved. This FE-SEM was successfully applied to observe resist, diatomaceous earth, aluminum oxide, and zeolite surfaces. The accelerating voltage is changeable in a range from 0.5 to 30 kV, and the probe current on the sample can be varied from 2×10^-9 to l×10^-13A to supply optimum electron dose. By using a snorkel- type, strongly excited objective lens (OL) immersing the samples in the magnetic field, the secondary electrons are extracted from the sample. For guiding electrons into the built-in lens-type secondary electron detector (SED), newly developed accelerating and retarding electrodes are installed in the OL to tune the surface potential. Furthermore, this FE-SEM can select 10 scan speeds, and the averaging and integration of secondary electron image signals are possible under every selected scan speed.     

Traditional coating techniques in scanning electron microscopy compared to uncoated charge compensator technology: Looking at human blood fibrin networks with the ZEISS ULTRA Plus FEG‐SEM

Scanning electron microscopy (SEM) studies surface morphology. Biological material needs to be coated to render the material conductive, and gold coating is traditionally used, although other coating material like carbon and ruthenium vapors may also be used. With modern SEM technology (e.g., ZEISS ULTRA Plus FEG‐SEM), we are able to work at very low kilovolts and also view fine surface structure in much better detail than with previous older technology. Some machines also allow for the study of uncoated material, although this is usually not done with biological material. This study focuses on surface clarity by comparing gold, ruthenium vapor, and carbon coating techniques for biological material. Human fibrin networks are used as example. Uncoated specimens are also viewed with a ZEISS ULTRA Plus FEG‐SEM because of its unique nitrogen charge compensator, and here, the first micrographs for uncoated human fibrin networks versus carbon, gold, and ruthenium coating are shown. We conclude that gold coating for biological material is not preferable with the latest SEM machines, as this method forms gold islands on top of the biological material and therefore produces a false surface morphology. Microsc. Res. Tech., 2011. © 2010 Wiley‐Liss, Inc.     

Efficacy of in-office bleaching techniques combined with the application of a casein phosphopeptide-amorphous calcium phosphate paste at different moments and its influence on enamel surface properties

OBJECTIVES: The aim of this in vitro study was to investigate the efficacy of in‐office bleaching technique combined with the application of a casein phosphopeptide‐amorphous calcium phosphate (CPP‐ACP) paste (MI Paste–MI) at different moments and its influence on enamel surface properties. METHODS: Eighty bovine dental crowns were randomly allocated into eight groups (n = 10), and bleached with either 35% hydrogen peroxide (HP) or 37% carbamide peroxide (CP). Four different protocols of application of MI were considered: without MI, MI applied before bleaching, MI applied after bleaching, and MI applied both before and after bleaching. Bleaching effectiveness was measured by the VITA EasyShade spectrophotometer utilizing the CIEL*a*b* system (ΔE, ΔL*, Δa*, and Δb*). Color readings were measured at baseline, 7, 14, and 21 days. Hardness and roughness were measured at baseline (T0) and immediately after bleaching (T14). Data were subjected to the two‐way ANOVA for repeated measurements and Tukey's test at 5%. RESULTS: HP groups achieved the greatest color change. The application of a CPP‐ACP paste did not reduce the efficacy of bleaching peroxides. Samples bleached with CP showed decreased hardness at T14. Samples bleached with HP that received the application of MI before and before/after bleaching did not present hardness decrease at T14. Samples bleached with peroxides only and received MI after bleaching showed increased roughness at T14. CONCLUSIONS: The use of CPP‐ACP was able to prevent negative changes in roughness and hardness of bovine enamel when associated to hydrogen peroxide, and might be applied before/after the bleaching protocol. Microsc. Res. Tech. 75:1019–1025, 2012. © 2012 Wiley Periodicals, Inc.