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DOE OSTI2019

Position sensitive alpha detector for an associated particle imaging system

Associated Particle Imaging (API) is a nuclear technique that provides for the nondestructive determination of 3D isotopic distributions. The method is based on the detection of the alpha particles associated with the neutron emitted in the deuterium-tritium (DT) fusion reaction, which provides information regarding the direction and time of the emitted 14 MeV neutron. Inelastic neutron scattering leads to characteristic gamma-ray emission from certain isotopes, for example 12 C, that can be correlated with the neutron interaction location. An API system consisting of a sealed-type neutron generator, gamma detectors, and a position-sensitive alpha detector is under development for the nondestructive quantification of carbon distribution in soils. This paper describes the design of the alpha detector, detector response simulations, and first experimental results. The alpha detector consists of a Yttrium Aluminum Perovskite (YAP) scintillator mounted on the inside of a neutron generator tube. The scintillation light propagates through a sapphire window to a position-sensitive photomultiplier tube mounted on the outside. The 16x16 output signals are connected through a resistive network for a 4-corner readout. The four readout channels are amplified, filtered, and then digitized for the calculation of the alpha position. First test findings demonstrate that an excellent alpha position resolution, better than the 1 mm FWHM required by the application, can be achieved with this detector design.

47 OTHER INSTRUMENTATION↗

NASA NTRS2004

Optical Calibration Process Developed for Neural-Network-Based Optical Nondestructive Evaluation Method

A completely optical calibration process has been developed at Glenn for calibrating a neural-network-based nondestructive evaluation (NDE) method. The NDE method itself detects very small changes in the characteristic patterns or vibration mode shapes of vibrating structures as discussed in many references. The mode shapes or characteristic patterns are recorded using television or electronic holography and change when a structure experiences, for example, cracking, debonds, or variations in fastener properties. An artificial neural network can be trained to be very sensitive to changes in the mode shapes, but quantifying or calibrating that sensitivity in a consistent, meaningful, and deliverable manner has been challenging. The standard calibration approach has been difficult to implement, where the response to damage of the trained neural network is compared with the responses of vibration-measurement sensors. In particular, the vibration-measurement sensors are intrusive, insufficiently sensitive, and not numerous enough. In response to these difficulties, a completely optical alternative to the standard calibration approach was proposed and tested successfully. Specifically, the vibration mode to be monitored for structural damage was intentionally contaminated with known amounts of another mode, and the response of the trained neural network was measured as a function of the peak-to-peak amplitude of the contaminating mode. The neural network calibration technique essentially uses the vibration mode shapes of the undamaged structure as standards against which the changed mode shapes are compared. The published response of the network can be made nearly independent of the contaminating mode, if enough vibration modes are used to train the net. The sensitivity of the neural network can be adjusted for the environment in which the test is to be conducted. The response of a neural network trained with measured vibration patterns for use on a vibration isolation table in the presence of various sources of laboratory noise is shown. The output of the neural network is called the degradable classification index. The curve was generated by a simultaneous comparison of means, and it shows a peak-to-peak sensitivity of about 100 nm. The following graph uses model generated data from a compressor blade to show that much higher sensitivities are possible when the environment can be controlled better. The peak-to-peak sensitivity here is about 20 nm. The training procedure was modified for the second graph, and the data were subjected to an intensity-dependent transformation called folding. All the measurements for this approach to calibration were optical. The peak-to-peak amplitudes of the vibration modes were measured using heterodyne interferometry, and the modes themselves were recorded using television (electronic) holography.

Decker, Arthur J.↗

NASA NTRS1989

Generic system components of the Thiokol ultrasonic RSRM case-to-insulation bondline inspection system

Qualification testing of the Ultrasonic Redesigned Solid Rocket Motor Bondline Inspection Systems (URBIS) was conducted at the Thiokol Nondestructive Evaluation Test Facility M337A and at the Rotation Process Storage Facility at Kennedy Space Center. The test was performed on portions of the URBIS that are generic to redesigned solid rocket motor case-to-insulation bondline inspections. Testing began on Feb. 13, 1989 and was completed on May 26, 1989. The main purpose of the test was to verify that each URBIS performed to the manufacturer's specifications in the same manner and to make any procedural changes necessary for specific redesigned solid rocket motor inspections. All five URBISs passed every stage of the qualification test. Each URBIS is now qualified for use on redesigned solid rocket motors. Verifying the fact that each URBIS obtains and analyzes data in a similar fashion has eliminated concerns about variations in data between the five systems. The following recommendations were made as a result of this test: (1) each URBIS should be located within a stable environment; (2) an electronic preventative maintenance program should be established for each URBIS; (3) when the URBIS is being utilized to perform transducer analysis, the URBIS equipment setting should match the equipment setting noted on the manufacturer-supplied transducer certification sheet; and (4) optimum scan velocities for each inspection technique (clevis, capture feature, pinhole and membrane) should be determined through further testing.

Cook, M.↗

NASA NTRS1999

An Ultrasonic Technique to Determine the Residual Strength of Adhesive Bonds

In this work, ultrasonic techniques to nondestructively evaluate adhesive bond degradation have been studied. The key to the present approach is the introduction of an external factor which pulls the adhesive bond in the nonlinear range, simultaneously with the application of an ultrasonic technique. With the aid of an external static tensile loading, a superimposed longitudinal wave has.been used to obtain the slopes of the stress-strain curve of an adhesive bond at a series of load levels. The critical load, at which a reduction of the slope is detected by the superimposed longitudinal wave, is an indication of the onset of nonlinear behavior of the adhesive bond, and therefore of bond degradation. This approach has been applied to the detection of adhesive bond degradation induced by cyclic fatigue loading. Analogously to the longitudinal wave case, a superimposed shear wave has been used to obtain the effective shear modulus of adhesive layers at different shear load levels. The onset of the nonlinear behavior of an adhesive bond under shear loading has been detected by the use of a superimposed shear wave. Experiments show that a longitudinal wave can also detect the nonlinear behavior when an adhesive bond is subjected to shear loading. An optimal combination of ultrasonic testing and mechanical loading methods for the detection of degradation related nonlinear behavior of adhesive bonds has been discussed. For the purpose of a practical application, an ultrasonic technique that uses a temperature increase as an alternative to static loading has also been investigated. A general strain-temperature correspondence principle that relates a mechanical strain to a temperature has been presented. Explicit strain-temperature correspondence relations for both the tension and shear cases have been derived. An important parameter which quantifies the relation between the wave velocity and temperature has been defined. This parameter, which is indicative of adhesive bond nonlinearity and which can be conveniently obtained by an ultrasonic measurement, has been used as an indication of adhesive bond degradation. Experimental results have shown that the temperature increase method is a convenient and productive alternative to static loading. A technique which uses the reflected waveform data to obtain the fundamental ultrasonic parameters (transit time, reflection coefficient and attenuation coefficient) of an adhesive bond has also been presented.

Achenbach, J. D.↗

DOE OSTI2016

Utilization of the Differential Die-Away Self-Interrogation Technique for Characterization and Verification of Spent Nuclear Fuel

New nondestructive assay techniques are sought to better characterize spent nuclear fuel. One of the NDA instruments selected for possible deployment is differential die-away self-interrogation (DDSI). The proposed DDSI approach for spent fuel assembly assay utilizes primarily the spontaneous fission and (α, n) neutrons in the assemblies as an internal interrogating radiation source. The neutrons released in spontaneous fission or (α,n) reactions are thermalized in the surrounding water and induce fission in fissile isotopes, thereby creating a measurable signal from isotopes of interest that would be otherwise difficult to measure. The DDSI instrument employs neutron coincidence counting with 3He tubes and list-mode-based data acquisition to allow for production of Rossi-alpha distributions (RADs) in post-processing. The list-mode approach to data collection and subsequent construction of RADs has expanded the analytical possibilities, as will be demonstrated throughout this thesis. One of the primary advantages is that the measured signal in the form of a RAD can be analyzed in its entirety including determination of die-away times in different time domains. This capability led to the development of the early die-away method, a novel leakage multiplication determination method which is tested throughout the thesis on different sources in simulation space and fresh fuel experiments. The early die-away method is a robust, accurate, improved method of determining multiplication without the need for knowledge of the (α,n) source term. The DDSI technique and instrument are presented along with the many novel capabilities enabled by and discovered through RAD analysis. Among the new capabilities presented are the early die-away method, total plutonium content determination, and highly sensitive missing pin detection. Simulation of hundreds of different spent and fresh fuel assemblies were used to develop the analysis algorithms and the techniques were tested on a variety of spontaneous fission-driven fresh fuel assemblies at Los Alamos National Laboratory and the BeRP ball at the Nevada National Security Site. The development of the new, improved analysis and characterization methods with the DDSI instrument makes it a viable technique for implementation in a facility to meet material control and safeguards needs.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

Probability of Detection Study to Assess the Performance of Nondestructive Inspection Methods for Wind Turbine Blades.

Wind turbine blades pose a unique set of inspection challenges that span from very thick and attentive spar cap structures to porous bond lines, varying core material and a multitude of manufacturing defects of interest. The need for viable, accurate nondestructive inspection (NDI) technology becomes more important as the cost per blade, and lost revenue from downtime, grows. NDI methods must not only be able to contend with the challenges associated with inspecting extremely thick composite laminates and subsurface bond lines, but must also address new inspection requirements stemming from the growing understanding of blade structural aging phenomena. Under its Blade Reliability Collaborative program, Sandia Labs quantitatively assessed the performance of a wide range of NDI methods that are candidates for wind blade inspections. Custom wind turbine blade test specimens, containing engineered defects, were used to determine critical aspects of NDI performance including sensitivity, accuracy, repeatability, speed of inspection coverage, and ease of equipment deployment. The detection of fabrication defects helps enhance plant reliability and increase blade life while improved inspection of operating blades can result in efficient blade maintenance, facilitate repairs before critical damage levels are reached and minimize turbine downtime. The Sandia Wind Blade Flaw Detection Experiment was completed to evaluate different NDI methods that have demonstrated promise for interrogating wind blades for manufacturing flaws or in-service damage. These tests provided the Probability of Detection information needed to generate industry-wide performance curves that quantify: 1) how well current inspection techniques are able to reliably find flaws in wind turbine blades (industry baseline) and 2) the degree of improvements possible through integrating more advanced NDI techniques and procedures. _____________ S a n d i a N a t i o n a l L a b o r a t o r i e s i s a m u l t i m i s s i o n l a b o r a t o r y m a n a g e d a n d o p e r a t e d b y N a t i o n a l T e c h n o l o g y a n d E n g i n e e r i n g S o l u t i o n s o f S a n d i a , L L C , a w h o l l y o w n e d s u b s i d i a r y o f H o n e y w e l l I n t e r n a t i o n a l , I n c . , f o r t h e U . S . D e p a r t m e n t o f E n e r g y ' s N a t i o n a l N u c l e a r S e c u r i t y A d m i n i s t r a t i o n u n d e r c o n t r a c t D E - N A 0 0 0 3 5 2 5 .

17 WIND ENERGY↗

DOE OSTI2015

Image reconstruction of single photon emission computed tomography (SPECT) on a pebble bed reactor (PBR) using expectation maximization and exact inversion algorithms: Comparison study by means of numerical phantom

Single Photon Emission Computed Tomography (SPECT) is a well-known imaging technique used in medical application, and it is part of medical imaging modalities that made the diagnosis and treatment of disease possible. However, SPECT technique is not only limited to the medical sector. Many works are carried out to adapt the same concept by using high-energy photon emission to diagnose process malfunctions in critical industrial systems such as in chemical reaction engineering research laboratories, as well as in oil and gas, petrochemical and petrochemical refining industries. Motivated by vast applications of SPECT technique, this work attempts to study the application of SPECT on a Pebble Bed Reactor (PBR) using numerical phantom of pebbles inside the PBR core. From the cross-sectional images obtained from SPECT, the behavior of pebbles inside the core can be analyzed for further improvement of the PBR design. As the quality of the reconstructed image is largely dependent on the algorithm used, this work aims to compare two image reconstruction algorithms for SPECT, namely the Expectation Maximization Algorithm and the Exact Inversion Formula. The results obtained from the Exact Inversion Formula showed better image contrast and sharpness, and shorter computational time compared to the Expectation Maximization Algorithm.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Process-dependent anisotropic thermal conductivity of laser powder bed fusion AlSi10Mg: impact of microstructure and aluminum-silicon interfaces

Purpose AlSi10Mg alloy is commonly used in laser powder bed fusion due to its printability, relatively high thermal conductivity, low density and good mechanical properties. However, the thermal conductivity of as-built materials as a function of processing (energy density, laser power, laser scanning speed, support structure) and build orientation, are not well explored in the literature. This study aims to elucidate the relationship between processing, microstructure, and thermal conductivity. Design/methodology/approach The thermal conductivity of laser powder bed fusion (L-PBF) AlSi10Mg samples are investigated by the flash diffusivity and frequency domain thermoreflectance (FDTR) techniques. Thermal conductivities are linked to the microstructure of L-PBF AlSi10Mg, which changes with processing conditions. The through-plane exceeded the in-plane thermal conductivity for all energy densities. A co-located thermal conductivity map by frequency domain thermoreflectance (FDTR) and crystallographic grain orientation map by electron backscattered diffraction (EBSD) was used to investigate the effect of microstructure on thermal conductivity. Findings The highest through-plane thermal conductivity (136 ± 2 W/m-K) was achieved at 59 J/mm 3 and exceeded the values reported previously. The in-plane thermal conductivity peaked at 117 ± 2 W/m-K at 50 J/mm 3 . The trend of thermal conductivity reducing with energy density at similar porosity was primarily due to the reduced grain size producing more Al-Si interfaces that pose thermal resistance. At these interfaces, thermal energy must convert from electrons in the aluminum to phonons in the silicon. The co-located thermal conductivity and crystallographic grain orientation maps confirmed that larger colonies of columnar grains have higher thermal conductivity compared to smaller columnar grains. Practical implications The thermal properties of AlSi10Mg are crucial to heat transfer applications including additively manufactured heatsinks, cold plates, vapor chambers, heat pipes, enclosures and heat exchangers. Additionally, thermal-based nondestructive testing methods require these properties for applications such as defect detection and simulation of L-PBF processes. Industrial standards for L-PBF processes and components can use the data for thermal applications. Originality/value To the best of the authors’ knowledge, this paper is the first to make coupled thermal conductivity maps that were matched to microstructure for L-PBF AlSi10Mg aluminum alloy. This was achieved by a unique in-house thermal conductivity mapping setup and relating the data to local SEM EBSD maps. This provides the first conclusive proof that larger grain sizes can achieve higher thermal conductivity for this processing method and material system. This study also shows that control of the solidification can result in higher thermal conductivity. It was also the first to find that the build substrate (with or without support) has a large effect on thermal conductivity.

Engineering↗

DOE OSTI2015

Applying fast calorimetry analysis on spent fuel calorimeter - 15620

Swedish Nuclear Fuel and Waste Management Company (SKB) is responsible for the back-end of the Swedish nuclear industry. This includes transport of spent fuel by boat from the power plants to the Central Interim Storage Facility for Spent Fuel (Clab), and in the future, encapsulation of the spent fuel and further transportation to a geological repository. In order to ensure safety for the planned geological repository, the decay heat has to be well known. For this purpose the SKB has performed calorimetric measurements on over 200 pressurized water reactor (PWR) and boiling water reactor (BWR) assemblies since 2003. The results from earlier analyses have been used to improve computer codes predicting heat as well as to acquire deeper knowledge about the fuel inventory. The work complements research being done as part of the Next Generation of Safeguards Initiative - Spent Fuel project, whose purpose is to develop and test nondestructive assay (NDA) technologies to improve safeguards measurements of spent nuclear fuel. The project is working to accomplish multiple goals, one of which is to determine the heat content of spent fuel assemblies. To shorten the measurement time, the temperature increase method was used instead of the equilibrium temperature method. In the temperature increase method, the temperature inside of the calorimeter is lowered below the surrounding water temperature before the measurement, and the temperature is allowed to increase due to the higher surrounding water temperature during the measurement. The rate of the temperature increase when the temperature is the same as the surrounding temperature is then compared to a calibration curve where an electric heater has been used in the same way. The price for the higher throughput is less accuracy and dependency of fuel geometry since the heat flow will be different for different fuel types, especially between PWR and BWR assemblies. Recently at Los Alamos National Laboratory, more sophisticated analysis methods have been considered for the use of calorimetry for treaty verification. These methods aim to predict the equilibrium temperature based on early data and therefore be able to shorten the measurement time while maintaining good accuracy and eliminate the dependency on fuel geometry. Even though the techniques show promise for future calorimetry of spent fuel, certain design features of the current system have been identified to interfere with the accuracy of equilibrium measurements in general such as changing pool temperatures and heat leakage during calibration. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2026

Nondestructive ultrasonic characterization of a triple-weld-bead wire arc additively manufactured ER70S-6 S-curved wall

Understanding build-scale microstructural variation in wire arc additive manufacturing (WAAM) of low-carbon steels is essential for ensuring consistent structure–property relationships throughout large components. Conventional destructive characterization techniques, such as scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD), are time-intensive and limited to localized regions, making comprehensive evaluation of large WAAM structures challenging. In this study, a nondestructive ultrasonic approach was employed to characterize a 252 mm tall ER70S-6 S-curved WAAM wall produced using a triple-bead deposition strategy. Optical and SEM analysis revealed a repeating dual-region microstructure consisting of uniform polygonal ferrite at melt pool centers and heterogeneous ferrite with coarse and fine grains near melt pool boundaries, attributed to cyclic thermal conditions. Longitudinal ultrasonic backscatter imaging was used to evaluate the continuity of this periodicity along the full build height. The ultrasonic response exhibited a consistent repeating pattern that correlated with the observed layer-wise microstructural variation. X-ray computed tomography confirmed the absence of detectable porosity, indicating that ultrasonic contrast is primarily governed by grain morphology. Overall, the results indicate that longitudinal backscatter ultrasound is a promising nondestructive characterization technique for validating microstructural variations along the s-curved WAAM wall, with significant potential for microstructure optimization and process control.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Nanoscale x-ray imaging of circuit features without wafer etching

Modern integrated circuits (ICs) employ a myriad of materials organized at nanoscale dimensions, and certain critical tolerances must be met for them to function. To understand departures from intended functionality, it is essential to examine ICs as manufactured so as to adjust design rules ideally in a nondestructive way so that imaged structures can be correlated with electrical performance. Electron microscopes can do this on thin regions or on exposed surfaces, but the required processing alters or even destroys functionality. Microscopy with multi-keV x-rays provides an alternative approach with greater penetration, but the spatial resolution of x-ray imaging lenses has not allowed one to see the required detail in the latest generation of ICs. X-ray ptychography provides a way to obtain images of ICs without lens-imposed resolution limits with past work delivering 20–40-nm resolution on thinned ICs. We describe a simple model for estimating the required exposure and use it to estimate the future potential for this technique. Here we show that this approach can be used to image circuit detail through an unprocessed 300-μm-thick silicon wafer with sub-20-nm detail clearly resolved after mechanical polishing to 240-μm thickness was used to eliminate image contrast caused by Si wafer surface scratches. Here, by using continuous x-ray scanning, massively parallel computation, and a new generation of synchrotron light sources, this should enable entire nonetched ICs to be imaged to 10-nm resolution or better while maintaining their ability to function in electrical tests.

36 MATERIALS SCIENCE↗

DOE OSTI2022

WIRE-21 Sensor Irradiation Experiment Ready for HFIR Insertion

The ability to deploy new nuclear fuels for current or future reactor concepts requires a wealth of data regarding fuel performance during normal operation, anticipated operational occurrences, and design-basis accidents. Most of these data have historically been collected during experiments in materials test reactors, ideally with online instrumentation to collect as much data as possible. However, advanced instrumentation could also allow for in situ monitoring of fuel operating conditions during commercial reactor operation to maximize fuel utilization, reduce unnecessary conservativism in design margins, and improve operator understanding of limiting peaking factors. The latter approach would complicate fuel handling, particularly during refueling, unless the instrumentation could be placed inside the fuel rods and transmitted wirelessly to a receiver located outside the fuel’s primary pressure boundary. To this end, Westinghouse Electric Company (WEC) developed wireless sensors based on inductive coupling that can transmit information regarding fuel centerline temperatures and rod internal pressures wirelessly from within a fuel rod to a nearby instrument thimble. After testing these sensors in lower-power university research reactors, the next step is to perform high neutron fluence testing to characterize the performance of these wireless sensors under conditions that are more representative of the intended application—in this case, light-water reactors (LWRs). The removable Be (RB) positions of the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) provide the neutron flux, experiment volume, and access to instrument leads required to achieve these sensor testing goals. This report summarizes the design, analysis, and assembly of the Wireless Instrumented RB Experiment 2021 (WIRE-21). This is the most highly instrumented irradiation experiment ever performed in HFIR. The experiment will use seven different sensing techniques to measure temperature, pressure, neutron flux, and neutron fluence during reactor operation. In addition to WEC’s wireless temperature and pressure sensors, WIRE-21 includes an array of thermocouples, self-powered neutron detectors, spatially distributed fiber optic temperature sensors, passive SiC temperature monitors, and flux wires. The design of WIRE-21 and the cabling that was installed in HFIR also provide the infrastructure to enable accelerated, economical testing of advanced sensor technologies while leveraging the extremely high neutron flux that is available in HFIR. The containment for WIRE-21 is similar to previous RB irradiation vehicles but includes a few modifications, most notably the use of integrated compression seals to pass a larger number of sensor leads through the experiment’s pressure boundary. In addition to the sensor leads, inert gas lines are passed into the experiment to enable active temperature control and the ability to pneumatically actuate a bellows-driven pressure sensor. WIRE-21 is targeting component temperatures (300–350°C) and neutron fluence levels (~10 22 n/cm 2 ) that would be expected in the plenum region of LWR fuels, except for the active sensing region of the wireless temperature sensor, which is targeting LWR fuel centerline temperatures (~800–1,100°C). WIRE-21 was successfully assembled, passed all nondestructive examination, and was delivered to HFIR for insertion during upcoming cycle 498 (April 2022).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Interpretation of Indications Generated by Small Welding Discontinuities in Ultrasonic Time of Flight Diffraction Technique

The article presents results of research on non-destructive ultrasonic time of flight diffraction technique TOFD and metallographic examinations of selected cross-sections of a MAG welded joint. The main objective was to compare the results of TOFD and metallographic examination at the locations where a large number of point-like indications, located on specific depths, have been detected on TOFD images and analyse the impact of this type of indication on results of a welded joint evaluation. Considered, that the indications have not exhibited separations between upper and lower diffraction signals, because of their small heights, measuring of height of indications in those cases was impossible. In all cases, the occurrence of discontinuities of 0.16–0.78 mm in height, in locations indicated by TOFD has been confirmed.

42 ENGINEERING↗

DOE OSTI2019

Exploiting Acoustic Anisotropy to Detect Recrystallization in a Ni Single Crystal Using Ultrasonic Nondestructive Inspection

Ultrasonic inspection was used to detect regions of recrystallization (RX) within a single crystal of Ni. RX can produce polycrystalline regions within single-crystal (SX) materials. Because RX regions act as initiator sites for failure by fatigue-crack growth in otherwise SX Ni-based superalloys, RX is an issue of direct concern for the service life of high-performance turbine blades. Detection and discrimination of RX regions in single-crystal materials are significant challenges for current nondestructive inspection technologies. The present study leverages the elastic anisotropy of single crystals, which produces acoustic anisotropy, to ultrasonically detect and characterize RX regions produced within single-crystal specimens. Single crystals of pure Ni were processed to create controlled regions of RX. These specimens were ultrasonically examined in an immersion tank using a high-resolution, polyvinylidene fluoride transducer to detect acoustic impedance changes across the boundaries between different crystals (i.e., grains) within the RX region. Data from time-of-flight and absolute peak amplitude measurements were used to create acoustic images that were compared against electron microscope images of the RX regions. The ultrasonic inspection technique described here successfully detected not only the locations of RX regions, but also the approximate sizes and shapes of the RX regions.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Characterization of commercial proton exchange membrane materials after exposure to beta and gamma radiation

Proton Exchange Membrane (PEM) type electrolysis cells have a potential use for tritium removal and heavy water upgrading. AECL is currently exposing various commercial PEM materials to both gamma (Cobalt-60 source) and beta (tritiated water) radiation to study the effects of radiation on these materials. This paper summarizes the testing methods and results that have been collected to date. The PEM materials that are or have been exposed to radiation are: Nafion 112, 212, 117 and 1110. Membrane characterization pre- and post- exposure consists of non-destructive inspection (FTIR, SEM/XPS), mechanical (tensile strength, percentage elongation, and modulus), electrical (resistance), or chemical (ion-exchange capacity - IEC). It has appeared that the best characterization techniques to compare exposed versus unexposed membranes were IEC, ultimate tensile strength and percent elongation. These testing techniques are easy and cheap to perform. The non-destructive tests, such as SEM and FTIR did not provide particularly useful information on radiation-induced degradation. Where changes in material properties were measured after radiation exposure, they would be expected to result in poorer cell performance. However, for modest γ-radiation exposure, all membranes showed a slight decrease in cell voltage (better performance). In contrast, the one β-radiation exposed membrane did show the expected increase in cell voltage. The counterintuitive trend for γ-radiation exposed membranes is not yet understood. Based on these preliminary results, it appears that γ- and β-radiation exposures have different effects.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2015

Meso-scale magnetic signatures for nuclear reactor steel irradiation embrittlement monitoring

Verifying the structural integrity of passive components in light water and advanced reactors will be necessary to ensure safe, long-term operations of the existing U.S. nuclear fleet. This objective can be achieved through nondestructive condition monitoring techniques, which can be integrated with plant operations to quantify the “state of health” of structural materials in real-time. While nondestructive methods for monitoring many classes of degradation (such as fatigue or stress corrosion cracking) are relatively advanced, this is not the case for degradation caused by irradiation. The development of nondestructive evaluation technologies for these types of degradation will require advanced materials characterization techniques and tools that enable comprehensive understanding of nuclear reactor material microstructural and behavioral changes under extreme operating environments. Irradiation-induced degradation of reactor steels causes changes in their microstructure that impacts their micro-magnetic properties. In this paper, we describe preliminary results of integrating advanced material characterization techniques with meso-scale computational models. In the future, this will help to provide an interpretive understanding of the state of degradation in structural materials. Microstructural data are presented from monocrystalline Fe and are correlated with variable-field magnetic force microscopy and micro-magnetic measurements. Ongoing research is focused on extending the measurements and models on thin films to gain insights into the structural state of irradiated materials and the resulting impact on magnetic properties. Preliminary conclusions from these correlations are presented, and next steps described.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2022

Material Characterization of Grade 91 Steel Welds using, Micro-resolution Ultrasonic Imaging System

Grade 91 (9Cr-1Mo-V) steel is a common structural material for fossil-fuel fired and nuclear power plants because of its creep strength and oxidation resistance at high temperatures. In this research, we studied the feasibility of correlating the high-resolution images obtained from the immersion ultrasonic imaging technique to microstructure regions in Grade 91 steel plate weldments. The high-resolution ultrasonic images presented in this paper were generated using a 20-MHz focused transducer as the transmitter, and a laser vibrometer as the receiver in the through transmission configuration to produce longitudinal and shear waves. This nondestructive evaluation (NDE) method was used to identify the Fusion Zone (FZ), Heat-Affected Zone (HAZ), and Base Metal (BM) regions of Grade 91 cold metal transfer (CMT) and flux core arc welds (FCAW). The ultrasonic imaging results were analyzed using beam propagation amplitudes and homogeneity, which in turn were used to relate the different microstructure regions of the FCAW and CMT welded samples. With this study, we were able to identify highly susceptible microstructures in the weld that could potentially promote creep type failures.

20 FOSSIL-FUELED POWER PLANTS↗

DOE OSTI2016

Sensitivity analysis of high resolution gamma-ray detection for safeguards monitoring at natural uranium conversion facilities

Under the policies proposed by recent International Atomic Energy Agency (IAEA) circulars and policy papers, implementation of safeguards exists when any purified aqueous uranium solution or uranium oxides suitable for isotopic enrichment or fuel fabrication exists. Under IAEA Policy Paper 18, the starting point for nuclear material under safeguards was reinterpreted, suggesting that purified uranium compounds should be subject to safeguards procedures no later than the first point in the conversion process. In response to this technical need, a combination of simulation models and experimental measurements were employed in previous work to develop and validate gamma-ray nondestructive assay monitoring systems in a natural uranium conversion plant (NUCP). In particular, uranyl nitrate (UO 2 (NO 3 ) 2 ) solution exiting solvent extraction was identified as a key measurement point (KMP). Passive nondestructive assay techniques using high resolution gamma-ray spectroscopy were evaluated to determine their viability as a technical means for drawing safeguards conclusions at NUCPs, and if the IAEA detection requirements of 1 significant quantity (SQ) can be met in a timely manner. Building upon the aforementioned previous validation work on detector sensitivity to varying concentrations of uranyl nitrate via a series of dilution measurements, this work investigates detector response parameter sensitivities to gamma-ray signatures of uranyl nitrate. The full energy peak efficiency of a detection system is dependent upon the sample, geometry, absorption, and intrinsic efficiency parameters. Perturbation of these parameters translates into corresponding variations of the 185.7 keV peak area of the 235 U in uranyl nitrate. Such perturbations in the assayed signature impact the quality or versatility of the safeguards conclusions drawn. Given the potentially high throughput of uranyl nitrate in NUCPs, the ability to assay 1 SQ of material requires uncertainty «1%. Accounting for material self-shielding properties, pipe thickness, and source-detector orientation is instrumental in determining the robustness of gamma-ray detection in the process monitoring of uranyl nitrate in NUCPs. Monte Carlo models and ray-tracing models were employed to determine the sensitivity of the detected 185.7 keV photon to self-shielding properties, pipe thickness, and source-detector geometry. Considering the implementation of the detection of 1 SQ, diversion of 1 SQ becomes essentially undetectable given the systematic uncertainty, in addition to considerations such as propagating uncertainties due to pipe offset/position, as well as minor variations in pipe thickness. Consequently, pipe thickness was the most sensitive variable in affecting full energy efficiency of the 185.7 keV signature peak with up to 8% variation in efficiency for ±0.5 mm changes in Schedule 40 304L stainless steel piping. Furthermore, computation of the attenuation correction factor of the uranyl nitrate solution [CF(AT) (i.e. εsample)] using Parker's method using with the approximation for the geometrical factor κ≈π/4 was validated through experimental, Monte Carlo and ray-tracing calculations for a uranyl nitrate filled transfer pipe segment. Furthermore, quantifying sensitivity in detector position, as well as voiding effects due to bubbly flow or laminar flow with an air gap in the uranyl nitrate becomes increasingly important as considerations from (static) design-scale measurements translate into (dynamic) field operations tests.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗