SEM characterization of silicon nanostructures: can we meet the challenge?

The current semiconductor technology road map for device scaling champions a 4.5 nm gate length in production by 2022. The scanning electron microscope (SEM) as applied to critical dimensions (CD) metrology and associated characterization modes such as electron beam-induced current and cathodoluminescence (CL) has proved to be a workhorse for the semiconductor industry during the microelectronics era. We review some of the challenges facing these techniques in light of the silicon nanotechnology road map. We present some new results using voltage contrast imaging and CL spectroscopy of top-down fabricated silicon nanopillar/nanowires (<100 nm diameter), which highlight the visualization challenge. However, both techniques offer the promise of providing process characterization on the 10-20 nm scale with existing technology. Visualization at the 1 nm scale with these techniques may have to wait for aberration-corrected SEM to become more widely available. Basic secondary electron imaging and CD applications may be separately addressed by the He-ion microscope.     

Biodegradable Lubricants: What Does ‘Biodegradable’ Really Mean?

A minimum level of biodegradability for either the base fluid(s) or the formulated product is stipulated in all the major schemes for defining an environmentally acceptable lubricant (EAL). Unfortunately, there are many standard tests for assessing biodegradability, while differences in the test conditions and how biodegradation is measured (e.g., carbon dioxide evolution, oxygen consumption, loss of parent material) affect the level of biodegradation measured. This means that the stated biodegradability of the base fluid (or any other component) of an EAL will be dependent on both its molecular properties and the test method used. This paper describes suitable test methods for assessing the biodegradability of EALs and gives examples of the confusion that can arise with the different test methods. It is recommended that ‘biodegradable’ for an EAL is defined as achieving at least 60% ThCO₂ (net CO₂ production as percentage of theoretical maximum) after 28 days, when tested according to OECD Test Guideline 301 B (CO₂ evolution test).     

Segmentation of SEM images of multiphase materials: When Gaussian mixture models are accurate?

Scanning electron microscopy has been a powerful technique to investigate the structural and chemical properties of multiphase materials on micro and nanoscale due to its high-resolution capabilities. One of the main outcomes of the SEM-based analysis is the calculation of the fractions of material components constituting the multiphase material by means of the segmentation of their back scattered electron SEM images. In order to segment multiphase images, Gaussian mixture models (GMMs) are commonly used based on the deconvolution of the image pixel histogram. Despite its extensive use, the accuracy of GMM predictions has not been validated yet. In this paper, we proceed to a systematic study of the evaluation of the accuracy and the limitations of the GMM method when applied to the segmentation of a four-phase material. To this end, first, we build a modelling framework and propose an index to quantify the accuracy of GMM predictions for all phases. Then we apply this framework to calculate the impact of collective parameters of image histogram on the accuracy of GMM predictions. Finally, some rules of thumb are concluded to guide SEM users about the suitability of using GMM for the segmentation of their SEM images based only on the inspection of the image histogram. A suitable histogram for GMM is a histogram with number of peaks equal to the number of Gaussian components, and if that is not the case, kurtosis and skewness should be smaller than 2.35 and 0.1, respectively.     

Seeing is believing? When scanning electron microscopy (SEM) meets clinical dentistry: The replica technique.

In restorative dentistry, the in situ replication of intra‐oral situations, is based on a non‐invasive and non‐destructive scanning electron microscopy (SEM) evaluation method. The technique is suitable for investigation restorative materials and dental hard‐ and soft‐tissues, and its interfaces. Surface characteristics, integrity of interfaces (margins), or fracture analysis (chipping, cracks, etc.) with reliable resolution and under high magnification (from ×50 to ×5,000). Overall the current study aims to share detailed and reproducible information about the replica technique. Specific goals are: (a) to describe detailed each step involved in producing a replica of an intra‐oral situation, (b) to validate an integrated workflow based on a rational sequence from visual examination, to macrophotography and SEM analysis using the replica technique; (c) to present three clinical cases documented using the technique. A compilation of three clinical situations/cases were analyzed here by means the replica technique showing a wide range of possibilities that can be reached and explored with the described technique. This guidance document will contribute to a more accurate use of the replica technique and help researchers and clinicians to understand and identify issues related to restorative procedures under high magnification.     

When,what and how image transformation techniques should be used to reduce error in Particle Image Velocimetry data?

Particle Image Velocimetry is commonly used to compute velocity fields in several areas including fluid mechanics, hydraulics and geophysics. However, acquired images often contain deformations caused either by camera lenses or placement. In this work the most popular digital transformation methods used to remove/reduce these deformations are benchmarked and suggestions tailoring specific transformations to different types of deformations are made. This article also shows the reduction of the error associated to the first and second order statistics, in the case of two-dimensional Particle Image Velocimetry, when the transformation techniques are applied to the computed velocity fields, and not the raw images, a common option in available commercial software.     

Is Scanning Electron Microscopy/Energy Dispersive X‐ray Spectrometry (SEM/EDS) Quantitative?

Scanning electron microscopy/energy dispersive X‐ray spectrometry (SEM/EDS) is a widely applied elemental microanalysis method capable of identifying and quantifying all elements in the periodic table except H, He, and Li. By following the “k‐ratio” (unknown/standard) measurement protocol development for electron‐excited wavelength dispersive spectrometry (WDS), SEM/EDS can achieve accuracy and precision equivalent to WDS and at substantially lower electron dose, even when severe X‐ray peak overlaps occur, provided sufficient counts are recorded. Achieving this level of performance is now much more practical with the advent of the high‐throughput silicon drift detector energy dispersive X‐ray spectrometer (SDD‐EDS). However, three measurement issues continue to diminish the impact of SEM/EDS: (1) In the qualitative analysis (i.e., element identification) that must precede quantitative analysis, at least some current and many legacy software systems are vulnerable to occasional misidentification of major constituent peaks, with the frequency of misidentifications rising significantly for minor and trace constituents. (2) The use of standardless analysis, which is subject to much broader systematic errors, leads to quantitative results that, while useful, do not have sufficient accuracy to solve critical problems, e.g. determining the formula of a compound. (3) EDS spectrometers have such a large volume of acceptance that apparently credible spectra can be obtained from specimens with complex topography that introduce uncontrolled geometric factors that modify X‐ray generation and propagation, resulting in very large systematic errors, often a factor of ten or more. SCANNING 35: 141‐168, 2013. ¹ Published 2012 Wiley Periodicals, Inc.     

Do universal adhesives provide the benefits from double-application or an extra bonding layer in composite repair?

This study aimed to determine whether the application of extra hydrophobic resin (EHR) or double layer (DL) improves microtensile bond strength (μTBS) of two universal adhesives to composite resin. Composite blocks were fabricated and exposed to thermal cycles. The specimens were horizontally sectioned into two halves. Scotch Bond Universal (SBU) and Clearfil S3 Bond Universal (CSBU) were applied to the ground composite surface according to the manufacturers' instructions, or with DL application or EHR application. The repair composite was incrementally placed to bonded planes. Composite sticks were achieved and tensed with a universal testing machine, followed by examining the fracture surfaces by a scanning electron microscope. Data were evaluated by Weibull analysis (shape and scale [σ_θ and σ_0.10] parameters) using the maximum likelihood method. The σ_θ and σ_0.10, respectively, estimate strength at 63.2 and 10% probability of failure. Shape parameter values showed significant differences among treatments. DL application of CSBU did not affect μTBS values at σ_θ of failure but caused to decrease μTBS values at σ_0.10 of failure. DL application of SBU reduced μTBS values at σ_θ of failure. DL or EHR coating did not improve μTBS of SBU. EHR application increased μTBS of CSBU, whereas DL application did not benefit.