Range Of Specimen Thicknesses Research Articles

Direct measurement of electrostatic potentials at the atomic scale: A conceptual comparison between electron holography and scanning transmission electron microscopy

Off-axis electron holography and first moment STEM are sensitive to electromagnetic potentials or fields, respectively. In this work, we investigate in what sense the results obtained from both techniques are equivalent and work out the major differences. The analysis is focused on electrostatic (Coulomb) potentials at atomic spatial resolution. It is shown that the probe-forming/objective aperture strongly affects the reconstructed electrostatic potentials and that, as a result of the different illumination setups, dynamical diffraction effects show a specific response with increasing specimen thickness. It is shown that thermal diffuse scattering is negligible for a wide range of specimen thicknesses, when evaluating the first moment of diffraction patterns.

Bandgap measurement of high refractive index materials by off-axis EELS

In the present work Cs aberration corrected and monochromated scanning transmission electron microscopy electron energy loss spectroscopy (STEM-EELS) has been used to explore experimental set-ups that allow bandgaps of high refractive index materials to be determined. Semi-convergence and –collection angles in the µrad range were combined with off-axis or dark field EELS to avoid relativistic losses and guided light modes in the low loss range to contribute to the acquired EEL spectra. Off-axis EELS further supressed the zero loss peak and the tail of the zero loss peak. The bandgap of several GaAs-based materials were successfully determined by simple regression analyses of the background subtracted EEL spectra. The presented set-up does not require that the acceleration voltage is set to below the Čerenkov limit and can be applied over the entire acceleration voltage range of modern TEMs and for a wide range of specimen thicknesses.

Effect of microscope parameter and specimen thickness of spatial resolution of transmission electron backscatter diffraction.

The spatial resolution of transmission electron backscatter diffraction (t-EBSD) with a standard conventional EBSD detector was evaluated quantitatively based on the calculation of the correlation coefficient of transmission patterns which were acquired across a twin boundary in the sample of austenitic steel. The results showed that the resolution of t-EBSD improved from tens of nanometres to below 10 nm with increasing accelerating voltage and thinning of specimen thickness. High voltage could enhance the penetration depth and reduce the scattering angle. And the thinning of specimen thickness would result in decreasing of the scattering events according to the theory of thermal diffuse scattering (TDS). In addition, the transmission patterns were found to be weak and noisy if the specimen was too thin, because of the decreasing intensity detected by the screen. Consequently, in this work, the best spatial resolution of 7 nm was achieved at 30 kV and 41 nm thickness. Moreover, the specimen thickness range was also discussed using Monte-Carlo simulation. This approach was helpful to account for the differences of measured spatial resolutions, by t-EBSD, of lamellas with different thickness.

Investigation on the rotational deformation of SEB specimens with various crack length to width ratio

A new CTOD calculation formula was proposed by using a correction factor for the blunted crack tip in the authors’ previous report[Kawabata et al(2016)], and the calculated CTOD by the formula significantly corresponded to the actual CTOD obtained by FE analysis in the wide range of specimen thicknesses. However, the use of the CTOD formula is limited to the frequently used crack depth-to-width ratio, a0/W, between 0.45 and 0.55, and this does not satisfy a strong demand for wider a0/W range. Meanwhile, ISO15653 covers a wider range of a0/W between 0.10 and 0.70, where J-based CTOD calculation formula has been specified in the annex-E of ISO15653. In this context, the plastic hinge model was investigated for a0/W between 0.05 and 0.70 by using FE analysis, and the analytical deformation of SEB specimens revealed that the plastic hinge model was applicable to the specimens even though their a0/W were out of the frequently used a0/W range from 0.45 and 0.55. Their rotational center points were almost steady when changing the applied load and the work hardening coefficient.

Recommended Specimen Dimensions and Boundary Conditions for Measurement of Hydrogen Permeation in Thick Carbon Steel Plates

The present work discusses the influence of specimen dimensions and boundary conditions on the deviation towards 2D diffusion during hydrogen permeation measurements on thick carbon steel plates. It was mathematically found and experimentally confirmed that hydrogen losses through lateral diffusion could significantly affect the validity of laboratory measurements on thick plates, since the common 1D simplification of diffusion equations is no longer valid. Based on a finite element analysis, two options are proposed to minimize the effects of side diffusion on permeation measurements. The first option, which encompasses ISO 17081 criteria, recommends optimum radii for hydrogen charging and extraction surfaces and is valid for a wide range of specimen thicknesses. The second option relies on modification of boundary conditions and consists of applying a hydrogen-diffusion barrier on the specimen side edges. This second option was experimentally tested and validated by means of an oxide layer deposited usi...

Fast characterization of two ultrasound longitudinal waves in cancellous bone using an adaptive beamforming technique.

The received signal in through-transmission ultrasound measurements of cancellous bone consists of two longitudinal waves, called the fast and slow waves. Analysis of these fast and slow waves may reveal characteristics of the cancellous bone that would be good indicators of osteoporosis. Because the two waves often overlap, decomposition of the received signal is an important problem in the characterization of bone quality. This study proposes a fast and accurate decomposition method based on the frequency domain interferometry imaging method with a modified wave transfer function that uses a phase rotation parameter. The proposed method accurately characterized the fast and slow waves in the experimental study, and the residual intensity, which was normalized with respect to the received signal intensity, was less than -20 dB over the bone specimen thickness range from 6 to 15 mm. In the simulation study, the residual intensity was less than -20 dB over the specimen thickness range from 3 to 8 mm. Decomposition of a single received signal takes only 5 s using a laptop personal computer with a single central processing unit. The proposed method has great potential to provide accurate and rapid measurements of indicators of osteoporosis in cancellous bone.

Compressive viscoelasticity of freshly excised mouse skin is dependent on specimen thickness, strain level and rate.

Although the skin’s mechanical properties are well characterized in tension, little work has been done in compression. Here, the viscoelastic properties of a population of mouse skin specimens (139 samples from 36 mice, aged 5 to 34 weeks) were characterized upon varying specimen thickness, as well as strain level and rate. Over the population, we observed the skin’s viscoelasticity to be quite variable, yet found systematic correlation of residual stress ratio with skin thickness and strain, and of relaxation time constants with strain rates. In particular, as specimen thickness ranged from 211 to 671 μm, we observed significant variation in both quasi-linear viscoelasticity (QLV) parameters, the relaxation time constant (τ1 = 0.19 ± 0.10 s) and steady-state residual stress ratio (G∞ = 0.28 ± 0.13). Moreover, when τ1 was decoupled and fixed, we observed that G∞ positively correlated with skin thickness. Second, as steady-state stretch was increased (λ∞ from 0.22 to 0.81), we observed significant variation in both QLV parameters (τ1 = 0.26 ± 0.14 s, G∞ = 0.47 ± 0.17), and when τ1 was fixed, G∞ positively correlated with stretch level. Third, as strain rate was increased from 0.06 to 22.88 s−1, the median time constant τ1 varied from 1.90 to 0.31 s, and thereby negatively correlated with strain rate. These findings indicate that the natural range of specimen thickness, as well as experimental controls of compression level and rate, significantly influence measurements of skin viscoelasticity.

Revised η-Factors andJ-CTOD Relationships for SE(B) Fracture Specimens Including 3D Effects and Implications for Fracture Toughness Measurements

AbstractThis work provides revised η-factors derived from CMOD records and J-CTOD relationships applicable to estimate the J-integral and CTOD in SE(B) specimens with varying crack size and specimen configuration. Very detailed non-linear finite element analyses for plane-strain and 3D models provide the evolution of load with increased crack mouth opening displacement, which is required for the estimation procedure. The analysis matrix considers SE(B) specimens with W=2B and W=B configurations with and without side grooves covering a wide range of specimen thickness, including a precracked Charpy (PCVN) specimen. Overall, the present results provide validation of the J and CTOD evaluation procedure currently adopted by ASTM E1820-11, while at the same time giving improved estimation equations for J and CTOD incorporating 3D effects which enter directly into more accurate testing protocols for experimental measurements of fracture toughness values using 3P SE(B) specimens.

Elemental mapping in achromatic atomic-resolution energy-filtered transmission electron microscopy.

We present atomic-resolution energy-filtered transmission electron microscopy (EFTEM) images obtained with the chromatic-aberration-corrected FEI Titan PICO at the Ernst-Ruska Centre, Jülich, Germany. We find qualitative agreement between experiment and simulation for the background-subtracted EFTEM images of the Ti-L2,3 and O-K edges for a specimen of SrTiO3 oriented down the [110] zone axis. The simulations utilize the transition potential formulation for inelastic scattering, which permits a detailed investigation of contributions to the EFTEM image. We find that energy-filtered images of the Ti-L2,3 and O-K edges are lattice images and that the background-subtracted core-loss maps may not be directly interpretable as elemental maps. Simulations show that this is a result of preservation of elastic contrast, whereby the qualitative details of the image are determined primarily by elastic, coherent scattering. We show that this effect places a constraint on the range of specimen thicknesses which could theoretically yield directly useful elemental maps. In general, interpretation of EFTEM images is ideally accompanied by detailed simulations.

Experimental study of annular bright field (ABF) imaging using aberration-corrected scanning transmission electron microscopy (STEM)

Experimental parameters used in the annular bright field (ABF) imaging method were tested using images simulated with the multislice method. Images simulated under identical conditions were found to agree well with experimental images. The ABF technique was shown to be relatively insensitive to the sample thickness and the defocus. In experimental ABF images, atomic columns exhibited dark contrast over a wide range of specimen thickness and defocus values, from 10 to 70nm and −20 to +20nm, respectively. A series of diffraction patterns at atomic columns, obtained using the diffraction imaging method, exhibited higher intensities in their central regions (0–11mrad) for light elements and in their peripheral regions (11–22mrad) for heavy elements. The results indicated that the contrast of light elements is enhanced by subtraction of the central region of the transmitted beam, since this is blocked by a circular mask in the ABF-STEM technique. Thus, the overall contrast of light elements is greatly improved, allowing them to be clearly visualized.

Determining the Stoichiometry of (K,Na)NbO3 Using Optimized Energy-Dispersive X-Ray Spectroscopy and Electron Energy-Loss Spectroscopy Analyses in a Transmission Electron Microscope

This paper describes an optimized analytical procedure for determining the composition of alkaline niobate-based lead-free piezoceramics by energy-dispersive X-ray spectroscopy (EDXS) in a transmission electron microscope (TEM). To discriminate the material-specific composition from the artifacts introduced during the EDXS/TEM analyses, the effects of radiation damage and the absorption of the characteristic X-ray lines were studied in detail. The optimized, quantitative EDXS analysis was tested on sodium potassium niobate with the nominal composition K0.5Na0.5NbO3 (KNN) by applying KNbO3 and NaNbO3 as standards. The results obtained indicate that KNbO3 is more radiation sensitive than NaNbO3. A similar degradation was confirmed in KNN, where the loss of potassium was higher than that of sodium. In addition, the degradation of the KNN was associated with a severe oxygen loss and the reduction of niobium. To achieve highly reliable, quantitative analyses and to preserve good counting statistics, the optimum conditions for the EDXS/TEM analyses were found at an electron dose rate of 0.4 pA/nm2 and an acquisition time of around 200 s in the specimen thickness range between 30 and 200 nm.

Local crystal structure analysis with several picometer precision using scanning transmission electron microscopy

We report a local crystal structure analysis with a high precision of several picometers on the basis of scanning transmission electron microscopy (STEM). Advanced annular dark-field (ADF) imaging has been demonstrated using software-based experimental and data-processing techniques, such as the improvement of signal-to-noise ratio, the reduction of image distortion, the quantification of experimental parameters (e.g. , thickness and defocus) and the resolution enhancement by maximum-entropy deconvolution. The accuracy in the atom position measurement depends on the validity of the incoherent imaging approximation, in which an ADF image is described as the convolution between the incident probe profile and scattering objects. Although the qualitative interpretation of ADF image contrast is possible for a wide range of specimen thicknesses, the direct observation of a crystal structure with deep-sub-angstrom accuracy requires a thin specimen (e.g., 10 nm), as well as observation of the structure image by conventional high-resolution transmission electron microscopy.

Fractal behavior throughout stretch zone of 15-5PH steel under elastic-plastic loading conditions

The topography of the fracture surface along the stretch zone of 15-5PH steel is analyzed for a range of specimen thicknesses, providing information on the changes in elastic-plastic behavior. The relationship between the stretch zone width, as a local toughness measurement, and fractal dimension is discussed along with the restrictions imposed by the stress field evolution. Image stacks for extended depth-of-field 3D reconstructions of the stretch zone region were acquired using a reflected light microscope. Significant correlations between the stretch zone width and fractal dimension with specimen thickness were found from measurements on elevation maps, especially at the center regions. This demonstrates that the stretch zone has heterogeneous topographic behavior depending on thickness and is more homogeneous under plane strain states. Finally, a general equation is suggested to describe the stretch zone width dependence on both the fractal dimension and material thickness.

Viscoelastic characterization of thin tissues using acoustic radiation force and model-based inversion

By means of the viscoelastodynamic model for a two-layer solid-fluid system and a detailed account of the locally induced acoustic radiation force, a rational analytical and computational framework is established for the viscoelastic characterization of thin tissues from high-frequency ultrasound (HFUS) measurements. For practical applications, the back-analysis is set up to interpret the frequency response function, signifying the tissue's axial displacement (captured by the imaging transducer) per squared voltage driving the ‘pushing’ transducer, as experimental input. On parametrizing the tissue's viscoelastic behavior in terms of the standard linear model, the proposed methodology is applied to a set of measurements performed on tissue-mimicking phantom constructs with thicknesses ranging from 0.5 to 4 mm. The results demonstrate that the model-based inversion, which carefully mimics the local boundary conditions and applied ultrasound excitation, yields viscoelastic properties for the phantom that are virtually invariant over the range of specimen thicknesses tested. Beyond its immediate application to in vitro viscoelastic characterization of thin excised tissues and tissue constructs, the proposed methodology may also find use in the characterization of skin or skin lesions over bone in vivo.

A steady-state Bi-substrate technique for measurement of the thermal conductivity of ceramic coatings

This paper presents a steady-state, bi-substrate technique for measurement of the through-thickness thermal conductivity of ceramic coatings, with a range of specimen thickness and porosity content. The technique is based on establishing unidirectional steady-state heat flow through the sample, sandwiched between a pair of (metallic) substrates with known thermal properties. Comparison between the heat fluxes passing through the two substrates allows a check to be made about the accuracy of the assumption of unidirectional heat flow. The interfacial conductances must be known and these can be estimated by testing samples of different thickness. Measured conductivities are likely to be more accurate if the interfacial conductance is relatively high. This is assisted by the introduction of a thin interfacial layer of a viscous, thermally conductive compound, or thermal pads of some sort, and by maintaining a suitable pressure across the setup. However, if such compounds (pastes) are used, then care must be taken to ensure that it does not enter the specimen via surface-connected pores, since this could significantly affect the measured conductivity. The reliability of the technique has been confirmed by testing fused silica samples of known thermal conductivity. It has also been applied to sprayed zirconia and plasma electrolytic oxide (PEO) alumina coatings. The values obtained were 1.05 ± 0.10 W m − 1 K − 1 and 1.63 ± 0.35 W m − 1 K − 1 , respectively.

Predicting Fatigue Crack Growth in the Residual Stress Field of a Cold Worked Hole

Abstract Cold working of holes generates compressive residual stresses resulting in a significant fatigue life improvement over a non-cold worked hole. Current fatigue life prediction methods for cold worked holes are based on two-dimensional (2-D) linear superposition of stress intensity factor, K, solutions of the non-cold worked hole and the residual stresses. Such predictions have shown various levels of agreement with the overall fatigue life and have generally underpredicted the crack growth over the majority of life. An inverse process was used to generate K solutions for the residual stresses of two experimental data sets using AFGROW and the crack growth data from the experiments. The inverse K solutions were inconsistent with the residual stress distribution indicating that it contained mechanisms or features not inherent to the 2-D weight function method. The predicted fatigue life was found to be very sensitive to a ± 1% variance in the inversely generated K solution. This sensitivity of the K method is a very important issue that must be addressed in the future. A 2-D FEA model indicated that the crack remained completely closed over a range of crack lengths despite experimental crack growth indicating that the model was not an accurate physical representation of the real crack. The results of this study combined with the significantly faster crack growth observed on the side of the hole corresponding to the entry side of the mandrel and the through thickness residual hoop stress variation show that the current methodology based on a 2-D assumptions is inadequate in predicting the fatigue crack growth from cold worked holes for the range of specimen thicknesses in this study. It is suggested that further research focus on incorporating the through thickness stress variance in a solution that predicts crack growth both in the radial and through thickness directions to capture the peculiar crack growth associated with cold working.

High-resolution quantitative X-ray microanalysis of Nb/AI multilayer thin films using the ζ-factor approach

Abstract The use of high-resolution X-ray microanalysis in the study of thin-film reactions provides composition information useful for understanding phase formation behaviour. The recently developed ζ-factor approach, in conjunction with data acquired on a high-spatial-resolution scanning transmission electron microscope, has been used successfully to obtain quantitative concentration profiles across layer interfaces in a Nb/AI multilayer. The use of the ζ-factor method permits efficient and simultaneous determination of the absorption correction and specimen thickness at each analysis point. The preparation of a suitable composition standard and the theory of the ζ-factor approach are also discussed. The ultimate result is a high-spatial-resolution X-ray line profile of the Nb-Al interface corrected for absorption in the specimen thickness range from 50 to 125 nm. The results demonstrate the potential of such an approach to other similar studies and represent a significant step towards the application o...

Experimental and theoretical study of the detection limits in electron energy-loss spectroscopy

We have developed a theoretical model that successfully predicts the spectral signal-to-noise ratios (SNRs) of inner-shell excitations in electron energy-loss spectroscopy of amorphous specimens by computing artificial spectra taking account of valence electron excitations as determined by the Ritchie–Howie model, inner-shell excitations from Hartree–Slater cross-sections and elastic scattering given by Lenz cross-sections together with the noise characteristics of the detection system. The consideration of multiple scattering in our model allows us to apply it to a wide range of specimen thicknesses and collection angles. We apply this model to the detection of minority elements which requires the correct identification of a weak signal on top of a large background in the presence of noise. The detectability of the minority element is judged by the confidence limits in the SNR of their characteristic excitation.

The gap correction for the resonant-mode dielectrometer

The calculation of dielectric constant from the frequency of a cylindrical resonant-mode dielectrometer is affected by the extension of the substrate into the gap beyond the cavity radius. An analysis of this gap effect is used to develop a correction calculation. As verification, we present measurements that cover a range of specimen thickness to cavity diameter ratios up to 0.1875 and dielectric constants from 1 to 154. Also included are measurements of sapphire, considered a standard dielectric. The algorithm developed results in a systematic error in the dielectric constant of less than one percent.

Definition of the spatial resolution of X-ray microanalysis in thin foils

The spatial resolution of X-ray microanalysis in thin foils is defined in terms of the incident electron beam diameter and the average beam broadening. The beam diameter is defined as the full width tenth maximum of a Gaussian intensity distribution. The spatial resolution is calculated by a convolution of the beam diameter and the average beam broadening. This definiyion of the spatial resolution can be related simply to experimental measurements of composition profiles across interphase interfaces. Monte Carlo calculations using a high-speed parallel supercomputer show good agreement with this definition of the spatial resolution and calculations based on this definition. The agreement is good over a range of specimen thicknesses and atomic number, but is poor when excessive beam tailing distorts the assumed Gaussian electron intensity distributions. Beam tailing occurs in low-Z materials because of fast secondary electrons and in high-Z materials because of plural scattering.