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At least 361 records · Page 20

Nondestructive evaluation of composites by optical time domain reflectometry in imbedded optical fibers

The use of imbedded optical fibers to obtain dynamic two-dimensional dynamic-strain measurements by optical time-domain reflectometry (OTDR) in laminated composites is described. The fundamental principles of OTDR are reviewed, and the basic parameters resolution and dynamic range are defined. Results of OTDR measurements on 30-cm square plates of 0/90/90/0-deg graphite epoxy composite with type 1506 optical fibers imbedded in a serpentine pattern between (and parallel to the reinforcing fibers of) the 90-deg plates are presented in graphs and briefly characterized. It is estimated that processing the OTDR data with simple techniques could permit strain detection of the order 0.00001 at sampling rates as high as 1/ms.

Claus, R. O.↗

Dynamic dielectric analysis - A nondestructive cure process monitoring method

The cure processes of TGDDM-based epoxy thermosets and polysulfone thermoplastic resins were monitored by means of computer-controlled dynamic dielectric measurements made at frequencies 5 Hz to 5 million Hz. The values of capacitance and conductance were recorded, and the data were used to calculate the complex permittivity, an intensive property which is characteristic of the material's state of cure and independent of the amount of material measured. The frequency dependence of the complex permittivity value was used to determine the conductivity and mean relaxation time. The conductivity which is also an intensive variable and is independent of sample size, was correlated with the viscosity in both the epoxy and polysulfone systems.

Kranbuehl, D. E.↗

Nondestructive determination of radionuclides in lunar samples using a large low-background gamma-ray spectrometer and a novel application of least-squares fitting

Dual-parameter gamma ray spectrometer systems with large volume Nal (Tl) crystals and low backgrounds were used for nondestructive determination of K, Th, U and cosmic ray produced radionuclides in 60 lunar samples. The total weight of samples measured with this system is 28 kg, and the individual sample weights varied from 2 to 2300 g. Samples from Apollo 11, 12, 14, 15 and 16 were measured. Operation of the spectrometers in the coincidence mode and analyzing single coincidence spectra permits the simultaneous determination of 8-10 radionuclides in each lunar sample.

Eldridge, J. S.↗

Bonding and nondestructive evaluation of graphite/PEEK composite and titanium adherends with thermoplastic adhesives

Bonded single overlap shear specimens were fabricated from Graphite/PEEK (Polyetheretherketone) composite adherends and titanium adherends. Six advanced thermoplastic adhesives were used for the bonding. The specimens were bonded by an electromagnetic induction technique producing high heating rates and high-strength bonds in a few minutes. This contrasts with conventionally heated presses or autoclaves that take hours to process comparable quality bonds. The Graphite/PEEK composites were highly resistant to delamination during the testing. This allowed the specimen to fail exclusively through the bondline, even at very high shear loads. Nondestructive evaluation of bonded specimens was performed ultrasonically by energizing the entire thickness of the material through the bondline and measuring acoustic impedance parameters. Destructive testing confirmed the unique ultrasonic profiles of strong and weak bonds, establishing a standard for predicting relative bond strength in subsequent specimens.

Hodges, W. T.↗

Ultrasonic modulus determination in composite media

A nondestructive test procedure for determining the elastic properties of anisotropic media is presented. The technique is based on transit time measurements for multiple angles of incidence and a numerical solution of the resulting coupled nonlinear equations for modulus determination. Methods for compensating for energy flux deviation from the wave normal and the resulting differences group and phase velocity are devised.

Kline, R. A.↗

Fiber Optic Bragg Grating Sensors for Thermographic Detection of Subsurface Anomalies

Conventional thermography with an infrared imager has been shown to be an extremely viable technique for nondestructively detecting subsurface anomalies such as thickness variations due to corrosion. A recently developed technique using fiber optic sensors to measure temperature holds potential for performing similar inspections without requiring an infrared imager. The structure is heated using a heat source such as a quartz lamp with fiber Bragg grating (FBG) sensors at the surface of the structure to detect temperature. Investigated structures include a stainless steel plate with thickness variations simulated by small platelets attached to the back side using thermal grease. A relationship is shown between the FBG sensor thermal response and variations in material thickness. For comparison, finite element modeling was performed and found to agree closely with the fiber optic thermography results. This technique shows potential for applications where FBG sensors are already bonded to structures for Integrated Vehicle Health Monitoring (IVHM) strain measurements and can serve dual-use by also performing thermographic detection of subsurface anomalies.

Allison, Sidney G.↗

Gas-Phase Composition as a Predictive Metric for Calendar Life Behavior of Next-Generation Silicon Anodes

The expansion of renewable technologies and electrification of the transportation sector is driving increased demand for next-generation battery materials that provide higher power and energy density with superior cycling and calendar life stability. Silicon (Si) has a theoretical capacity nearly 10x that of graphite, and is therefore a promising anode material candidate to meet these rigorous performance demands. While leading Si anode battery demonstrations are approaching target metrics for cycle life, a series of complex and interrelated modes of reactivity lead to reduced calendar life and therefore challenge practical adoption of these materials. Deconvoluting the degradation processes that impact Si calendar life is critical to informing the rational and accelerated design of improved Si materials. In the present work, we employ novel sampling techniques and GC-MS-FID characterization to measure gas-phase composition during initial Si cycling, which we tie to selective mechanisms of Si passivation. We utilize a tiered analysis approach to identify and quantify the gas-phase reaction products associated with three advanced Si material candidates under practical operating conditions. Ex situ analysis of Si powders (pure chemical reactivity) is coupled with nondestructive in situ sampling of Si electrodes in a practical pouch-cell format (coupled chemical and electrochemical reactivity). We link the observed gas-phase species evolution to electrochemical behavior and measured calendar life of the three Si materials. Further, we evaluate the voltage-resolved evolution of gas-phase species for one such Si nanomaterial, where nonmonotonic gas generation implies competition between passivating reaction pathways. The measured gas-phase compositional data serves as a critical input for our advanced electrochemical SEI models to identify favorable vs unfavorable reaction pathways to stabilize Si. In addition to bolstering a fundamental understanding of Si reactivity, the present approach informs specific and quantifiable gas-phase metrics tied to calendar life improvements in Si, which can streamline and accelerate the process of next-generation material development.

DIRECT ENERGY CONVERSION,ENERGY STORAGE↗

Nondestructive ultrasonic characterization of two-phase materials

The development of ultrasonic methods for the nondestructive characterization of mechanical properties of two phase engineering materials are described. The primary goal was to establish relationships between the nonlinearity parameter and the percentage of solid solution phase in two phase systems such as heat treatable aluminum alloys. The acoustoelastic constant was also measured on these alloys. A major advantage of the nonlinearity parameter over that of the acoustoelastic constant is that it may be determined without the application of stress on the material, which makes the method more applicable to inservice nondestructive characterization. The results obtained on the heat treatable 7075 and the work hardenable 5086 and 5456 aluminum alloys show that both the acoustoelastic constant and the acoustic nonlinearity parameter change considerable with the volume fraction of second phase precipitates in these aluminum alloys. A mathematical model was also developed to relate the effective acoustic nonlinearity parameter to volume fraction of second phase precipitates in an alloy. The equation is approximated to within experimental error by a linear expression for volume fractions up to approx. 10%.

Salama, Kamel↗

BWR Spent Nuclear Fuel Acquisition and Testing to Support DOE-NE High Burnup Spent Fuel Data Project

The Office of Spent Fuel and Waste Disposition (SFWD) within the US Department of Energy (DOE) Office of Nuclear Energy (NE) established the Spent Fuel and Waste Science and Technology (SFWST) campaign to conduct research and development (R&D) activities related to the storage, transportation, and disposal of spent nuclear fuel (SNF) and high-level radioactive waste. The SFWST program was created within SFWD to address issues of extended or long-term SNF storage and transportation. Some near-term objectives of SFWST are to use a science-based, engineering-driven approach to: Support the enhancement of the technical bases to support the continued safe and secure dry storage of SNF for extended periods; Support the enhancement of the technical bases for retrieving SNF after extended dry storage; Support the enhancement of the technical bases for transporting high burnup (HBU) fuel and transporting low burnup fuel and HBU fuel after dry storage DOE-NE, in partnership with the Electric Power Research Institute, developed the High Burnup Spent Fuel Data Project to perform a large-scale demonstration and laboratory-scale testing of HBU pressurized water reactor (PWR) fuels (exceeding 45 gigawatt-days per metric ton of uranium [GWd/MTU]). Under this project, 25 sister rods—which are rods that have the same design, power histories, and other characteristics—were removed from assemblies at the North Anna Nuclear Power Station and sent to Oak Ridge National Laboratory (ORNL) in January 2016. ORNL performed detailed nondestructive examination (NDE) on all 25 rods. The NDE consisted of visual examinations, gamma and neutron scanning, profilometry and rod length measurements, and eddy current examinations. After completing the NDE, 10 of the sister rods were delivered to Pacific Northwest National Laboratory (PNNL) in a NAC International, Inc. legal-weight truck cask in September 2018 for destructive examination (DE). To date, SFWD work has focused on the PWR fuel that is part of the Sister Rod Test program. No boiling water reactor (BWR) fuel has been tested in the program, and the data needs that were identified for the PWR fuel have not been collected for BWR fuel. The goal to obtain six to nine BWR rods and test them at ORNL will support closing this important data gap. BWR fuel comprises approximately 56% of the total fuel assemblies currently in storage at nuclear power plants in the United States. BWR nuclear fuel and cladding designs and manufacturing are significantly different from PWRs. Differences include the following: BWR fuel pellets are larger than PWR pellets; Variations of Zircaloy-2 (including liners) are used instead of the Zircaloy-4 cladding materials used in PWRs; Clad manufacturing and stress-relief processes are different between PWRs and BWRs; The fuel rod dimensions are different because larger rod diameters and thicker cladding are used in BWRs; BWR fuel typically has lower internal rod pressures and sees vastly different operating conditions than PWR fuel (i.e., two-phase flow); BWR assemblies are “canned,” meaning each assembly is surrounded by a metal fuel channel; BWR cladding is often composed of an inner pure Zr liner that has widely different mechanical properties than the Zircaloy-2 alloy and exhibits a stronger affinity for hydrogen; The BWR SNF generally has more total hydrogen in the cladding/liner than typical PWR fuel; The construction of the PWR and BWR assemblies is vastly different; BWR rods are solidly attached to the assembly nozzles and experience a much different vibration and shock load than PWR rods, which are “floating” within a grid system attached to guide tubes, and the rods sit loosely on the bottom end plates. These numerous differences will affect the way the BWR SNF responds under dry storage preparation processes (e.g., vacuum drying) and during transportation. The results collected in the PWR experimental program must be compared with a subset of similar data collected on BWR SNF to establish a technical basis for whether the larger PWR database is sufficient to bound the BWR SNF end-of-life conditions as is currently assumed for several fuel/clad properties. Changes that occur in both fuel types at HBU could exacerbate any mechanical property differences. As the fuel burnup increases, several changes occur that might affect the performance of the fuel, cladding, and assembly hardware in storage and transportation. These changes include increased cladding corrosion layer thickness, increased cladding hydrogen content, increased cladding creep strains, increased fission gas release, and the formation of the HBU structure at the surface of the fuel pellets. The Nuclear Regulatory Commission (NRC) limits the current maximum rod-averaged burnup to 62 GWd/MTU due to these changes and the lack of data at higher burnups.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Superconducting Material Growth for Radio-Frequency (RF) Cavities

Superconducting radio-frequency (SRF) cavities, usually manufactured from Niobium (Nb), are vital components of modern particle accelerators because of their ability to achieve high acceleration gradients with little power dissipation. Naturally forming Nb surface oxides significantly alter cavity performance by changing surface resistance. A nondestructive characterization of oxide thickness is helpful for relating surface processing treatments to cavity performance. This work develops a protocol to measure Nb oxide thickness using Angle-Resolved X-ray Photoelectron Spectroscopy (ARXPS) while correcting instrumental errors. Using uniform bulk standard samples (Silver, Aluminum oxide, and Germanium), we determined a baseline correction factor to account for analyzer-related intensity evolution as the measurement angle increases. The correction factor was then applied to Nb 3d ARXPS data. Applying the Strohmeier equation to the corrected data yielded a Nb2O5 thickness of 6.04 nm, closely matching the 5.5 (±.05) nm value obtained from cross-sectional transmission electron microscopy. Our approach will bring a method to incorporate inherent errors in the thickness measurements using ARXPS and can be broadly applied to improve the accuracy of thickness measurements in a wide range of heterostructures.

Lambert, Nathan [Fermilab]↗

Advanced NDE research in electromagnetic, thermal, and coherent optics

A new inspection technology called magneto-optic/eddy current imaging was investigated. The magneto-optic imager makes readily visible irregularities and inconsistencies in airframe components. Other research observed in electromagnetics included (1) disbond detection via resonant modal analysis; (2) AC magnetic field frequency dependence of magnetoacoustic emission; and (3) multi-view magneto-optic imaging. Research observed in the thermal group included (1) thermographic detection and characterization of corrosion in aircraft aluminum; (2) a multipurpose infrared imaging system for thermoelastic stress detection; (3) thermal diffusivity imaging of stress induced damage in composites; and (4) detection and measurement of ice formation on the space shuttle main fuel tank. Research observed in the optics group included advancements in optical nondestructive evaluation (NDE).

Skinner, S. Ballou↗

A Diagnosis-Prognosis Feedback Loop for Improved Performance Under Uncertainties

The feed-forward relationship between diagnosis and prognosis is the foundation of both aircraft structural health management and the digital twin concept. Measurements of structural response are obtained either in-situ with mounted sensor networks or offline using more traditional techniques (e.g., nondestructive evaluation). Diagnosis algorithms process this information to detect and quantify damage and then feed this data forward to a prognostic framework. A prognosis of the structure's future operational readiness (e.g., remaining useful life or residual strength) is then made and is used to inform mission- critical decision-making. Years of research have been devoted to improving the elements of this process, but the process itself has not changed significantly. Here, a new approach is proposed in which prognosis information is not only fed forward for decision-making, but it is also fed back to the forthcoming diagnosis. In this way, diagnosis algorithms can take advantage of a priori information about the expected state of health, rather than operating in an uninformed condition. As a feasibility test, a diagnosis-prognosis feedback loop of this manner is demonstrated. The approach is applied to a numerical example in which fatigue crack growth is simulated in a simple aluminum alloy test specimen. A prognosis was derived from a set of diagnoses which provided feedback to a subsequent set of diagnoses. Improvements in accuracy and a reduction in uncertainty in the prognosis- informed diagnoses were observed when compared with an uninformed diagnostic approach.

Leser, Patrick E.↗

Microwave Photoelasticity: A Resonant Wavelength Approach Applied to PEEK Polymer

Every nondestructive testing (NDT) technique has its unique set of advantages and limitations. Currently, the only existing noncontact NDT method capable of measuring sub-surface stresses, in optically opaque materials, at near-real-time speeds and over large areas is Microwave Photoelasticity (MP). This paper presents a new MP approach, which correlates changes in resonant wavelengths to changes in stress. In addition to a theoretical outline of the approach, the design and operation of an instrument capable of conducting these measurements is described. Finally, the technique is demonstrated by conducting measurements on polyetheretherketone, commonly known as PEEK, polymer. Between the W-Band frequencies of 105 to 115 GHz, PEEK’s stress-optic-coefficient was determined to be of 𝐶𝐶 = −0.20 ± 0.02 1/GPa.

Schemmel, Peter J.↗

Superconducting Material Growth for Radio-Frequency (RF) Cavities

Superconducting radio-frequency (SRF) cavities, usually manufactured from Niobium (Nb), are vital components of modern particle accelerators because of their ability to achieve high acceleration gradients with little power dissipation. Naturally forming Nb surface oxides significantly alter cavity performance by changing surface resistance. A nondestructive characterization of oxide thickness is helpful for relating surface processing treatments to cavity performance. This work develops a protocol to measure Nb oxide thickness using Angle-Resolved X-ray Photoelectron Spectroscopy (ARXPS) while correcting instrumental errors. Using uniform bulk standard samples (Silver, Aluminum oxide, and Germanium), we determined a baseline correction factor to account for analyzer-related intensity evolution as the measurement angle increases. The correction factor was then applied to Nb 3d ARXPS data. Applying the Strohmeier equation to the corrected data yielded a Nb2O5 thickness of 6.04 nm, closely matching the 5.5 (±.05) nm value obtained from cross-sectional transmission electron microscopy. Our approach will bring a method to incorporate inherent errors in the thickness measurements using ARXPS and can be broadly applied to improve the accuracy of thickness measurements in a wide range of heterostructures.

Lambert, Nathan [Fermilab]↗

Field‐Induced Ferroelectric Phase Evolution During Polarization “Wake‐Up” in Hf 0.5 Zr 0.5 O 2 Thin Film Capacitors

Abstract As an emerging nonvolatile memory technology, HfO 2 ‐based ferroelectrics exhibit excellent compatibility with silicon CMOS process flows; however, the reliability of polarization switching in these materials remains a major challenge. During repeated field programming and erase of the polarization state of initially pristine HfO 2 ‐based ferroelectric capacitors, the magnitude of the measured polarization increases, a phenomenon known as “wake‐up”. In this study, the authors attempt to understand what causes the wake‐up effect in Hf 0.5 Zr 0.5 O 2 (HZO) capacitors using nondestructive methods that probe statistically significant sample volumes. Synchrotron X‐ray diffraction reveals a concerted shift in HZO Bragg peak position as a function of polarization switching cycle number in films prepared under conditions such that they exhibit extremely large (≈3000%) wake‐up. In contrast, a control sample with insignificant wake‐up shows no such peak shift. Capacitance – voltage measurements show evolution in the capacitance loop with switching cycle number for the wake‐up sample and no change for the control sample. Piezoresponse force microscopy measurements are utilized to visualize the domain switching with wake‐up. The combination of these observations clearly demonstrates that wake‐up is caused by a field‐driven phase transformation of the tetragonal phase to the metastable ferroelectric orthorhombic phase during polarization switching of HZO capacitors.

36 MATERIALS SCIENCE↗

A Tool Measuring Remaining Thickness of Notched Acoustic Cavities in Primary Reaction Control Thruster NDI Standards

Stress corrosion cracking in the relief radius area of a space shuttle primary reaction control thruster is an issue of concern. The current approach for monitoring of potential crack growth is nondestructive inspection (NDI) of remaining thickness (RT) to the acoustic cavities using an eddy current or remote field eddy current probe. EDM manufacturers have difficulty in providing accurate RT calibration standards. Significant error in the RT values of NDI calibration standards could lead to a mistaken judgment of cracking condition of a thruster under inspection. A tool based on eddy current principle has been developed to measure the RT at each acoustic cavity of a calibration standard in order to validate that the standard meets the sample design criteria.

Sun, Yushi↗

Sub-10 nm Probing of Ferroelectricity in Heterogeneous Materials by Machine Learning Enabled Contact Kelvin Probe Force Microscopy

Reducing the dimensions of ferroelectric materials down to the nanoscale has strong implications on the ferroelectric polarization pattern and on the ability to switch the polarization. As the size of ferroelectric domains shrinks to the nanometer scale, the heterogeneity of the polarization pattern becomes increasingly pronounced, enabling a large variety of possible polar textures in nanocrystalline and nanocomposite materials. Critical to the understanding of fundamental physics of such materials and hence their applications in electronic nanodevices is the ability to investigate their ferroelectric polarization at the nanoscale in a nondestructive way. We show that contact Kelvin probe force microscopy (cKPFM) combined with a k-means response clustering algorithm enables to measure the ferroelectric response at a mapping resolution of 8 nm. In a BaTiO 3 thin film on silicon composed of tetragonal and hexagonal nanocrystals, we determine a nanoscale lateral distribution of discrete ferroelectric response clusters, fully consistent with the nanostructure determined by transmission electron microscopy. Moreover, we apply this data clustering method to the cKPFM responses measured at different temperatures, which allows us to follow the corresponding change in the polarization pattern as the Curie temperature is approached and across the phase transition. This work opens up perspectives for mapping complex ferroelectric polarization textures such as curled/swirled polar textures that can be stabilized in epitaxial heterostructures and more generally for mapping the polar domain distribution of any spatially highly heterogeneous ferroelectric materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Optimal Methods for Estimating Cactus Pear Biomass Using Cladode Dimensions of Morphologically Diverse Accessions

Current allometric methods for photosynthetic-stem (cladode) plants, such as cactus pear (Opuntia spp.), require refinement to be used in field settings in which diverse accessions are grown. We analysed cladode dimensional data using 14 accessions representing four species and two hybrids to quantify statistically significant morphological differences among accessions and derived cross-accession models to approximate cladode fresh weight. A Box model using cladode dimensions (e.g., length, width, thickness and diameter) and factorial combinations of these measures (e.g., length*width*thickness*diameter vs. fresh weight) resulted in the highest coefficient of determination (R 2 = 0.95 general fit) across all accessions for estimating fresh weight along with parsimony estimates using the Schwarz–Bayes Criterion (SBC), which assesses the most consistent performance on individual accessions. A Fitting-box modelling approach used the measured cladode area captured using ImageJ (R 2 = 0.93 general fit). Lastly, an Elliptical model used an elliptical approximation for the measured area and performed well over all accessions (R 2 = 0.94 general fit) while avoiding extensive manual measurements. These models meet or exceed the performance of previously published approaches when applied across morphologically diverse accessions, providing efficient tools for nondestructive estimation of cactus pear biomass under the conditions tested.

Opuntia↗