Nondestructive Characterization Research Articles

Recent Progress in Ultrasonic Nondestructive Characterization of Material Microstructures: A Review

The scattering and attenuation of high frequency ultrasonic wave in polycrystalline materials such as metal and ceramics have implication of material microstructures. Many studies have recently developed sophisticate forward models that corelate ultrasonic scattering and attenuation with different types of polycrystalline materials. Furthermore, some studies have proposal effective methodologies to nondestructively determine polycrystal microstructures from ultrasonic measurements, namely solving the inversion problems. Its applications cover titanium alloys in aerospace, carbon steels in transportation, additively manufactured components and machineries, to name a few. This paper reviews recent progress in ultrasonic nondestructive characterization of metal microstructures, including voids, grain size, crystallographic texture and grain boundary.

Non-destructive characterization of silicon nanowires and nanowire coatings using mid-infrared spectroscopy

Silicon nanowires (SiNWs) have attracted much attention owing to their potential applications in electronics and photonics, while remaining as a cost-effective material platform. Key material properties in engineering SiNWs for different applications include their length, density, and presence of oxides or other chemicals on the surface. However, monitoring these properties is challenging, as scanning electron microscopy and atomic force microscopy (AFM), which directly image the wires, require destructive cleaving of the sample. This paper uses polarized, variable-angle Fourier Transform IR reflectance spectroscopy as a nondestructive technique to characterize the areal density and length of metal-assisted chemically etched SiNW arrays. In addition to the ability to characterize “as-etched” wires, we show that IR spectroscopy can also measure few-nanometer thick layers of aluminum oxide (AlOx) grown radially around the length of the SiNWs utilizing atomic layer deposition. Despite sample inhomogeneities, an effective medium theory (EMT) model can determine the length and density of the NWs for a range of lengths between 3 and 14 μm. The EMT can also reproduce the experimentally measured vibrational bands for coated NWs, demonstrating that IR spectroscopy can also evaluate the presence of molecular contaminants on the wires.

In-situ rapid nondestructive characterization of multiple irregular three-dimensional grain boundary structures and electrical properties by nanorobot with SEM in ZnO

To address the problem of spatial quantification of irregular grain boundaries, a unique approach for the nondestructive characterization of multiple irregular three-dimensional grain boundaries is proposed using nanorobots with scanning electron microscopy (SEM) to accomplish in-situ rapid synchronized quantification of structures and electrical properties. By constructing a three-dimensional trigonometric geometric mapping relationship, multiple irregular three-dimensional grain boundary structures and electrical properties can be rapidly quantified. Experimental results demonstrate that it is feasible to accomplish in-situ rapid nondestructive characterizations. The two-dimensional profile shapes of the targeted grain boundaries at each layer exhibit irregular and non-uniform features in the Y-Z plane. The hypotenuse length between the virtual space tilting lines presents a three-dimensional characteristic in the X-Z plane. The spatial tilt angle of the virtual space tilting line can be calculated using the right-triangle relation. The unequal numbers of grains along the same tilted hypotenuse direction with equal lengths directly illustrate the existence of irregular and nonlinear grain boundaries in bulk ZnO ceramics. The relatively uniform spatial sizes of the grain boundary illustrate the coupled spatial characteristics existing in the irregular micro-structures. The relatively uniform equivalent circuit fitting parameters confirmed the existence of relatively uniform doping components in bulk ZnO ceramics. Furthermore, this method provides a unique approach for the rapid nondestructive quantitative analysis of multiple three-dimensional irregular grain boundaries in bulk polycrystalline materials.

Polydimethylsiloxane (PDMS)-assisted non-destructive transient thermoreflectance characterizations.

The conventional pump-probe thermoreflectance (pump-probe TR) techniques are routinely performed on a thin (typically <100nm) metal transducer deposited on samples, ensuring the most fundamental principle of thermoreflectance: the reflectance change (∆R/R) of the sample surface is directly and linearly related to the temperature change (∆T) within a finite temperature range. However, general metal coating methods may damage the sample by forming a mixed layer with the sample. In this article, we present a non-destructive pump-probe transient thermoreflectance (TTR) characterization using the polydimethylsiloxane (PDMS)-assisted metal transfer technique. Our method utilizes PDMS dry transfer to transfer common transducer metals (Au and Al) to the target substrate. This method effectively avoids impurities and damage to the sample. In particular, we have utilized Au as a transition layer to study the application of Al transfer in TTR measurements. The substrate thermal conductivity measurement results show that they can all be used for TTR measurement, and the thermal boundary conductance results show that the transferred metals have low bonding to the substrate. In addition, Al/Au can be transferred over a large area at room temperature compared to Au. After measurement, the samples can be restored to their original state by a simple cleaning method. This method provides a simple and reliable way to characterize samples without metal coating for TTR.

In-Line Test Structures and Non-destructive Characterization of Electromigration-Driven Phase Evolution in Microscale Solder Joints

In-Line Test Structures and Non-destructive Characterization of Electromigration-Driven Phase Evolution in Microscale Solder Joints

Non-destructive depth reconstruction of Al-Al2Cu layer structure with nanometer resolution using extreme ultraviolet coherence tomography

Non-destructive cross-sectional characterization of materials systems with a resolution in the nanometer range and the ability to allow for time-resolved in-situ studies is of great importance in material science. Here, we present such a measurements method, extreme ultraviolet coherence tomography (XCT). The method is non-destructive during sample preparation as well as during the measurement, which is distinguished by a negligible thermal load as compared to electron microscopy methods. Laser-generated radiation in the extreme ultraviolet (XUV) and soft x-ray range is used for characterization. The measurement principle is interferometric and the signal evaluation is performed via an iterative Fourier analysis. The method is demonstrated on the metallic material system Al-Al2Cu and compared to electron and atomic force microscopy measurements. We also present advanced reconstruction methods for XCT, which even allow for the determination of the roughness of outer and inner interfaces.

Synergistic Effect of CO2 in Accelerating the Galvanic Corrosion of Lithium/Sodium Anodes in Alkali Metal-Carbon Dioxide Batteries.

Rechargeable alkali metal-CO2 batteries, which combine high theoretical energy density and environmentally friendly CO2 fixation ability, have attracted worldwide attention. Unfortunately, their electrochemical performances are usually inferior for practical applications. Aiming to reveal the underlying causes, a combinatorial usage of advanced nondestructive and postmortem characterization tools is used to intensively study the failure mechanisms of Li/Na-CO2 batteries. It is found that a porous interphase layer is formed between the separator and the Li/Na anode during the overvoltage rising and battery performance decaying process. A series of control experiments are designed to identify the underlying mechanisms dictating the observed morphological evolution of Li/Na anodes, and it is found that the CO2 synergist facilitates Li/Na chemical corrosion, the process of which is further promoted by the unwanted galvanic corrosion and the electrochemical cycling conditions. A detailed compositional analysis reveals that the as-formed interphase layers under different conditions are similar in species, with the main differences being their inconsistent quantity. Theoretical calculation results not only suggest an inherent intermolecular affinity between the CO2 and the electrolyte solvent but also provide the most thermodynamically favored CO2 reaction pathways. Based on these results, important implications for the further development of rechargeable alkali metal-CO2 batteries are discussed. The current discoveries not only fundamentally enrich our knowledge of the failure mechanisms of rechargeable alkali metal-CO2 batteries but also provide mechanistic directions for protecting metal anodes to build high-reversible alkali metal-CO2 batteries.

Ultrasonic Guided Wave Scattering Spectra by Hybrid Global–Local Modeling for Nondestructive Evaluation in Composites With Varying Defect Features

Abstract The nondestructive characterization and monitoring of defects in composite structures by ultrasonic guided waves are hindered by the complexity of the interaction. Efficient computational modeling of propagating ultrasonic guided waves in waveguides with discontinuities is necessary to properly tune inspections and correctly interpret the scattering behavior. This paper studies the influence of different defect types in composite plates on ultrasonic guided wave scattering. Employing a hybrid global–local method, the energy spectra of transmitted and reflected waves in defected composite plates are numerically analyzed over a broad frequency range. Through parametric analyses of defect dimensions and locations, the resulting trends of the effect of specific defect features on the scattering behavior, as well as the importance of observing scattering on a broad frequency range, are accurately computed and highlighted. The presented findings indicate the potential for effective defect characterization and monitoring.

Non-destructive characterization of pore structure and chloride diffusion coefficient of cementitious materials with modified non-contact electrical resistivity method

The intricate pore structure of cement-based materials passively influences chloride ion transport and mechanical properties. Existing non-contact electrical resistivity measurement (NC-ERM) methods lack precision for rigorous studies. the NC-ERM was upgraded in this research, which is suitable for assessing the pore structure and transport characteristics of hardened cementitious substrates. The results obtained from this method closely correspond to those obtained from CEMHYD3D, Mercury intrusion porosimetry (MIP), and other methods. Additionally, the impact of mixture proportions on the resistivity, pore structure parameters, and chloride ion diffusion coefficient of cementitious materials is discussed. With an increase in sand ratio and sand-to-stone ratio, the resistivity exhibits an initial rise followed by a decline. Chloride diffusion of 5 wt% NaCl-saturated specimens is 1.2–1.3 times higher than 3.5 wt% NaCl. This study provides a novel non-destructive, convenient and accurate method for characterising the pore structure and testing the transport properties of cementitious materials.

Interdisciplinary methodology for the characterisation of archaeological metal grave goods from the Museum of Patagonia by PIXE, DRX, and SEM/EDS

AbstractWe present a study of a selection of metal ornaments belonging to archaeological funerary goods from Patagonic Indigenous groups. They are part of the ‘Andrés Giai’ Collection, under the guard of the Museum of Patagonia (Nahuel Huapi National Park [PNNH]; National Parks Administration [APN]), Argentina. The absence of contextual information and its current conservation status motivated the design of an interdisciplinary methodology to develop an Integral Conservation Plan that considered the selection of analytical techniques. Here, we implemented complementary nondestructive characterisation techniques such as particle induced X‐ray emission (PIXE), X‐ray diffraction (XRD) and scanning electron microscopy coupled with energy dispersive X‐ray spectroscopy (SEM/EDS). We developed a methodology enabling us to characterise each piece with respect to its metallic composition and degradation products, and in certain cases, their manufacturing process. These findings have contributed with essential information for the tailored conservation treatment proposal. Moreover, they provided key information in regard to the reconstruction of contextual data for each piece. In addition, the methodology proposed for the Integral Conservation Plan takes into account an optimisation of the techniques to be used in order to minimise unnecessary handling of goods whilst ensuring an appropriate use of technological and economic resources whilst minimising time on potentially unconclusive measurements and results.

Non-destructive characterization of dislocation density in annealed pure iron using nonlinear ultrasonic combined with recurrence quantification analysis

Non-destructive characterization of dislocation density in annealed pure iron using nonlinear ultrasonic combined with recurrence quantification analysis

Nondestructive material characterization and component identification in sheet metal processing with electromagnetic methods

Electromagnetic methods for non-destructive evaluation (NDE) are presented, with which sheet metal components can be identified and their material properties can be characterized. The latter is possible with 3MA, the Micromagnetic Multiparametric Microstructure and stress Analyser. This is a combination of several micromagnetic NDE methods that make it possible to analyse the microstructure in a ferromagnetic material and to determine quantitative values of the mechanical material properties or the stress state. In the case of cold forming, the 3MA application for pre-process testing of sheet metal is discussed. Based on the 3MA information, the formability of the sheets can be predicted. To apply 3MA in-line, the influence of the relative speed and the relative distance between the 3MA probe head and the sheet was investigated. In a second study, a spatially resolved eddy current (EC) method was used to create an image of the intrinsic material microstructure of a component for its identification and traceability. It turned out, that these intrinsic fingerprint images can still be recognized even after subsequent plastic deformation or coating of the surface. This enabled the development of a marker-free traceability method for sheet metal processing. It is based on a low-cost array sensor and a specimen identification using robust and partly redundant features of the fingerprint images processed by machine learning (ML).

Pore-scale physics of ice melting within unconsolidated porous media revealed by non-destructive magnetic resonance characterization

Melting of ice in porous media widely exists in energy and environment applications as well as extraterrestrial water resource utilization. In order to characterize the ice-water phase transition within complicated opaque porous media, we employ the nuclear magnetic resonance (NMR) and imaging (MRI) approaches. Transient distributions of transverse relaxation time T2 from NMR enable us to reveal the substantial role of inherent throat and pore confinements in ice melting among porous media. More importantly, the increase in minimum T2 provides new findings on how the confinement between ice crystal and particle surface evolves inside the pore. For porous media with negligible gravity effect, both the changes in NMR-determined melting rate and our theoretical analysis of melting front confirm that conduction is the dominant heat transfer mode. The evolution of mushy melting front and 3D spatial distribution of water content are directly visualized by a stack of temporal cross-section images from MRI, in consistency with the corresponding NMR results. For heterogeneous porous media like lunar regolith simulant, the T2 distribution shows two distinct pore size distributions with different pore-scale melting dynamics, and its maximum T2 keeps increasing till the end of melting process instead of reaching steady in homogeneous porous media.

Evaluation of a Local Acoustic Resonance Method for Coating Thickness Determination on Stochastic Metal Hybrid Foams

Novel cellular materials promise a combination of high strength and low specific weight for sustainable and energy‐efficient material design. Inhomogeneities of the materials, such as varying coating thickness, are inherent to the production process but require advanced characterization in order to better understand mechanical properties. Herein, global and local acoustic analysis for nondestructive characterization of local coating thickness on an open‐porous hybrid metal foam system is studied. Experiments and numerical simulations are carried out to evaluate vibration behavior stimulated by a low‐energy impact. The novelty of the work is the use of local excitation and analysis of decay times to determine coating thickness gradients. This qualitative measurement can inform and speed up the material development process due to its simplicity, speed, and low cost. Furthermore, it provides a basis for quality control when scaling up the technology of metal hybrid foams for industrial applications.

Non-destructive characterization of additive manufacturing components with computed tomography and 3D X-ray microscopy

Non-destructive characterization of additive manufacturing components with computed tomography and 3D X-ray microscopy

Quantitative Nondestructive Evaluation of Cold Spray Manufactured Aluminum Alloy 6061 and Copper Samples

Cold spray (CS) is a solid-state process for depositing thick layers of material via the successive high-velocity impact of powder particles onto a solid surface, which leads to high rates of deformation, interparticle bonding, and coating build-up. Although CS is finding commercial utilization in non-load-bearing repair and coating applications, clear nondestructive characterization procedures are necessary to realize its potential in load-bearing structural applications. In this study, the viability of electrical conductivity and through thickness ultrasound wave velocity measurement methods was studied to serve as a means for nondestructive quantitative measurement for quality control in CS and potentially other additive manufacturing (AM) methods. Eddy current, ultrasound, porosity, hardness, and uniaxial tensile strength tests were conducted on CS deposited layers of aluminum alloy 6061 and copper on aluminum alloy 6061 and commercially pure copper substrates, respectively. CS gas dynamic parameters were intentionally and systematically varied to result in corresponding discrete differences in mechanical properties of deposits. Ultrasound measurements of longitudinal wave velocity and eddy current electrical conductivity measurements showed good correlation with process conditions, microstructural characterization results, and destructive mechanical tests (hardness, tensile). The results of this work show that ultrasound wave velocity and electrical conductivity correlate well with increased particle impact velocity in CS deposited aluminum and copper blocks, which evidently show an incremental decrease in porosity, increase in hardness, and increase in tensile strength. The outlined ultrasound and eddy current nondestructive testing methods present effective means for quantitative assessment of cold spray deposited structures while intact with the substrate.

Online state of health estimation for lithium-ion batteries based on gene expression programming

Lithium-ion battery is a kind of energy storage devices with complex internal reaction and many factors affecting its performance. Accurate prediction of its SOH (State of Health) is of great significance to prolong its service life and improve safety performance. However, the current prediction for SOH has the difficulties of selecting health factors and using data-driven methods with opaque mechanisms. In this paper, a data-driven model will be established with the capacity change during aging of lithium-ion batteries as a health indicator to realize precise prediction of capacity degradation. Firstly, the feature parameters were extracted and analyzed from the battery cyclic aging test dataset. Two in-situ nondestructive characterization methods, incremental capacity analysis curve and differential thermal voltammetry curve, were utilized to resolve the evolution paths of the feature parameters. After that, a data-driven battery capacity degradation estimation is realized based on the GEP (Gene Expression Programming) algorithm, the performance is compared with the existing vehicle-end and cloud-end models, and a higher-accuracy SOH stacking model is developed with an increase of less than 1 ms in computational time. The results indicated that the GEP model proposed in this paper has obvious advantages in terms of physical explain-ability, computational efficiency and robustness.

A Study of Synthesis and Characterization Techniques for Iron Oxide (FeO) Nanoparticles

Nanoparticles, especially iron oxide nanoparticles, are pivotal in various applications due to their magnetic properties. This research focuses on the synthesis and characterization of iron oxide (FeO) nanoparticles. The study delves into the versatile applications of these nanoparticles, ranging from magnetic colloids to bio-functional uses, highlighting their significance in magnetic bio-separation, magnetic resonance imaging (MRI), and precision drug delivery. The experimental design employs diverse synthesis techniques, emphasizing the gel-evaporation, co-precipitation, reverse micelles, and hydrothermal methods. These approaches offer control over the size and shape of nanoparticles, crucial for tailoring their physicochemical properties. Detailed exploration of the polyol technique and micro-emulsion method provides insights into their mechanisms and the resulting nanoparticles' characteristics. The synthesis of nanoparticles through hydro-thermal conditions is also investigated, elucidating the influence of reaction parameters on particle size and morphology. For comprehensive characterization, various techniques are employed. X-ray Diffraction (XRD) determines crystal structures, while Scanning Electron Microscopy (SEM) and Transmission Electron Microscopy (TEM) offer morphological and topographical insights. Photoluminescence (PL) is utilized for non-destructive optical characterization, analyzing electron-hole pair generation and recombination. Experimental data is collected using advanced equipment such as the FESEM-Hitachi S4800, JEM 3010 TEM, and a Horiba Jobin Yvon system. XRD scans cover a range of 10 to 75 degrees, SEM provides high-resolution 3D images, TEM allows atomic-level resolution, and PL spectra are acquired for liquid samples.This comprehensive study contributes to the understanding of iron oxide nanoparticles, their synthesis techniques, and their potential applications in various fields. The findings offer valuable insights for researchers and practitioners involved in nanomaterial science, catalysis, and biomedical applications.

Polarization sensitive optical side leakage radiometry for distributed characterization of anti-resonant hollow-core fibers.

A novel technique referred to as optical side leakage radiometry is proposed and experimentally demonstrated for non-destructive and distributed characterization of anti-resonant hollow-core optical fibers with high spatial resolution. Through in-depth analysis of the leakage light collection, we discover a unique polarization dependence, which is validated by our experiment. By leveraging this effect and employing Fourier filtering, this method enables accurate quantification of propagation attenuations for fundamental and higher order modes (with the uncertainty of <1 dB/km), identification of localized defects (with the resolution of ∼5 cm), and measurement of ultra-low spectral phase birefringence (at the level of 10-7) in two in-house-fabricated nested antiresonant nodeless hollow-core fibers. Such a fiber characterization approach, boasting unprecedently high accuracy and a potentially wide dynamic range, holds the potential to become an indispensable diagnosis tool for monitoring and assisting the manufacture of high-quality anti-resonant hollow-core fiber.

Acoustoelastic characterization of plates using zero group velocity Lamb modes

Acoustoelasticity, a characteristic of material anharmonicity, gives rise to a link between wave propagation velocity and the stress state in materials. Ultrasonic techniques to monitor this coupling, particularly with high sensitivity and in a noncontact manner, can have widespread application both in the quantification of applied and residual stress and in the characterization of nonlinear material behavior through measurement of higher order elastic constants. Here, we use a laser ultrasonic technique to excite and detect zero group velocity (ZGV) Lamb wave resonances in aluminum plates under uniaxial loading. A laser line source is used to excite these resonances at different orientations with respect to the applied load, and the signals are detected using an interferometer. The effects of stress and source orientation on ZGV resonance frequencies are validated using the theory of acoustoelastic Lamb wave propagation. In addition, a model-based inversion technique is used to extract Murnaghan's third-order elastic constants from measurements of the stress dependence of the first two ZGV modes generated parallel and perpendicular to the applied load. Laser generation and detection of ZGV resonances is shown to be an effective and powerful approach for the noncontact and nondestructive acoustoelastic characterization of elastic waveguides.