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These are a set of slides that deal with membrane degradation accelerated stress test. Specifically, the following topics are covered: membrane degradation FCTT drive cycle; membrane ASTs; current membrane ASTs damage mechanisms; proposed membrane AST, RH cycling in H 2 /Air; current proposed AST; 2min/2min AST damage mechanism; 30sec/45sec RH cycling at OCV.
To verify the 15-year reliability of the Navy half-watt radioisotope thermoelectric generator (RTG), bismuth-telluride thermoelectric converters were submitted to testing at high temperatures which accelerated the degradation and caused failure of the converters. Metallographic diagnostic examination of failed units verified failure mechanisms. Results of diagnostic examinations are presented.
Qualification testing of solar photovoltaic (PV) modules per IEC 61215 standard encompasses a set of well-defined accelerated stress tests (irradiation, environmental, mechanical and electrical) with strict pass/fail criteria based on functionality/performance, electrical and mechanical safety, and visual requirements. The qualification testing does not identify all the possible reliability failures or durability issues witnessed in the actual field. However, it does identify the major/catastrophic design quality issues (infant mortality), which could occur early in a module’s field life. Unfortunately, in the industry, there is no consensus-based standard or protocol available to validate manufacturers’ warranty period claims based on the end-of-life wear-out failure mechanisms. Being able to predict the field degradation rates and lifetime using mode-specific accelerated tests on moderately field-aged modules, for example 10 years, for certain commonly occurring degradation modes would be a powerful contribution to all the stakeholders of the PV industry. There is a need to formulate guidelines to find the correlation of accelerated testing with field degradation for individual degradation modes observed in the field. Potential approaches to fulfill this need were experimented in this project and are presented in this report. Two of the most commonly seen degradation modes – encapsulant browning and solder bond thermomechanical fatigue – are addressed in this report through presenting the accelerated testing methods and physical modelling approaches. Two accelerated test methods (UV and thermal cycling) were designed to induce the wear-out mechanisms in the modules and not infant mortality failures. To focus on the wear-out failure modes, the tests were performed on field-aged modules, instead of fresh modules, with known degradation rates and degradation modes. The degradation rates were measured based on the degradation rates of individual cell parameters (short-circuit current, I sc and series resistance, R s ) instead of the degradation rate of maximum power (P max ) which cannot be used to study any specific/limited degradation mode as the P max degradation could be caused by many different degradation modes. The key characteristic parameter considered for encapsulant discoloration and solder bond degradation is I sc and R s , respectively. The developed physical models/equations relating the testing degradation data and field weather data were utilized to determine the acceleration factor (AF) and to predict the degradation rate for a specific degradation mode of PV modules installed in two different climates, Arizona (hot) and New York (cold). The predicted degradation rates for encapsulant browning and solder bond degradation have also been validated against the actual measured field degradation rates. UV testing cost reduction: To determine acceleration factor, single UV chamber was used for accelerated UV testing at three different temperatures simultaneously, instead of three chambers for three temperatures (or one chamber sequentially which is an extremely time-consuming approach). A passive heating approach was successfully used to achieve and maintain multiple temperatures in the accelerated UV chamber. Foam insulation boards of varying thicknesses were utilized to obtain three different temperatures for UV testing. However, these foam materials tend to disintegrate in the presence of moisture. To alleviate this problem, silicone heating blankets with temperature controls and humidifier can be used if the UV testing is to be performed under hot-humid conditions instead of conventional hot-dry conditions. Thermal cycling testing cost reduction: Single thermal cycling chamber was used for accelerated thermal cycling testing at three different upper temperatures simultaneously, instead of three chambers for three upper temperatures (or one chamber sequentially which is an extremely time-consuming approach). An active heating approach based on silicone heating blankets was successfully used to achieve and maintain multiple upper temperatures in the accelerated thermal cycling chamber. Such blankets provide stable temperature control and thereby more reliable and repeatable for replicate experiments.
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Accelerated degradation tests can be used as the basis for predicting the performance or state of health of products and materials at use conditions over time. Measurements acquired at accelerated levels of stress are used to develop models that relate to the degradation of one or more performance measures. Frequently, products/materials of interest are subjected to variable stress levels during their lifetimes. However, testing is usually performed only at a few fixed stress levels. In such cases, cumulative degradation models are developed and assessed by using data acquired under those fixed stress conditions. The degradation rate at any stress condition within the range of the model can be estimated by the derivative of the cumulative model at that stress condition. It follows that, to predict cumulative degradation over variable use conditions, one might integrate the fluctuating degradation rate over time. Existing approaches for doing this consider degradation rates that depend only on the current stress level. Here, we propose to allow the degradation rate to also depend on the current state of health as indicated by the associated performance measure(s). The resulting modeling approach is capable of portraying a broader range of degradation behavior than existing approaches. The assertion of memoryless degradation by using this or any other approach should be assessed experimentally with data acquired under variable stress in order to increase confidence that the integrated rate model is accurate. In this article, we demonstrate the additional capability of the proposed approach by developing empirical memoryless rate-based degradation models to predict resistance increase and capacity decrease in lithium-ion cells that are being evaluated for use in electric vehicles. Here, we then assess the plausibility of these models.
Electron-spin-resonance (ESR) spectroscopy and Arrhenius plots used to determine maximum safe temperature for accelerated testing of photothermal degradation of polymers. Aging accelerated by increasing illumination, temperature, or both. Results of aging tests at temperatures higher than those encountered in normal use valid as long as mechanism of degradation same throughout range of temperatures. Transition between different mechanisms at some temperature identified via transition between activation energies, manifesting itself as change in slope of Arrhenius plot at that temperature.
An extensive search and evaluation of electrochemically stable catalyst supports (including metal oxides like RuO2-SiO2, RuO2-TiO2, and ITO was perfomed during the 4 years of the project. The suports were also catalyzed by deposition of Pt and tested for its performance and electrochemical stability in RDE and fuel cell experiments. For testing the electrochemical stability and fuel cell performance of the catalysts and supports, we have employed the protocols in use at the Department of Energy and Nissan Technological Center North America (NTCNA). The use of such procedures allows a precise and reproducible estimation of the performance and stability of the materials and permits comparisons among laboratories and DOE funded projects. RuO2-SiO2 catalyst supports showed no loss in surface area during start-stop stability tests that were performed by cycling the electrode potential between 0 V to 1.8 V for 1000 cycles. Catalyzed support (40% Pt/RuO2-SiO2; 1:1 mole ratio) were tested in a PEFC, resulting in a current density of 750 mA/cm2 at 0.6 Volts, and a maximum power density of 570 mW/cm2. Measurements were conducted at 80 ºC with 75% relative humidity of the inlet gases (H2/O2); Pt loadings were 0.4 mg/cm2 at the cathode and 0.2 mg/cm2 at the anode. Start-stop stability tests for support and catalyzed support performed in RDE and PEFC set-ups have confirmed RuO2-TiO2 support stability. The beginning of life performance was exactly equal to end of life performance (in an MEA that has been subjected to severe start-stop cycling for 10,000 start/stop cycles between 1 V to 1.5 V). This result was in sharp contrast to baseline Pt/C catalyst that showed significant performance deterioration after accelerated stability tests. The Pt/TRO showed minimal loss in performance upon exposure to start-stop cycles. The loss in cell voltage at 1 A/cm2 at 100% RH was almost 700 mV for Pt/C whereas it was only ca. 15 mV for Pt/TRO. 40% RH data (of inlet gases) revealed a similar trend in terms of stability – exceptional stability for Pt/TRO as opposed to very poor stability for Pt/HSAC. These observations were attributed to the much higher stability of the TRO support compared to Carbon. The carbon dioxide concentration in the cathode exit stream during the accelerated degradation test with Pt/TRO (start-stop protocol) was extremely low (between 3 to 10 ppm of CO2). In contrast, the CO2 emission levels from a conventional Pt/C catalyst were found to be approx. 200 ppm. This observation was a clear indicator that the main source of carbon being oxidized to carbon dioxide in an MEA was the carbon catalyst support, and not the gas diffusion layer or the graphite flow fields. Indium tin oxide (ITO) was also evaluated as a catalyst support for PEFCs. Pt/ITO was very stable under start-up/shutdown accelerated degradation protocol (RDE tests in perchloric acid). The ECSA change was less than 4% over 10,000 cycles. The load cycling accelerated protocol (from 0.6 to 0.95 V vs. RHE) resulted in a loss of approximately 34% of the initial ECSA after 10,000 cycles. However, fuel cell testing resulted in a very low performing catalyst. XPS spectroscopy was employed to investigate the changes in the catalysts occuring during fuel cell operation. It was observed a shift of In 3d5/2 and In 3d3/2 peaks towards higher binding energies. This can be explained by the formation of hydroxides or oxy-hydroxides in the surface of the catalyst. O1s spectrum for Pt/ITO catalyst after being operated in the fuel cell, also confirmed the formation of significant amounts of surface hydroxides (12 to 16%). The presence of surface hydroxides in the catalyst increased the electrode resistivity affecting fuel cell performance. NTCNA performed a detailed analysis of transport phenomena (reactants and products to/from the Pt active sites) in both commercial catalyst and Pt/RTO (in order to have a better understanding at the basic level). The proton resistance (Rionomer) in Pt/C and Pt/RTO cathode catalyst layers were 150 and 12 mΩ-cm2, respectively. Pt/RTO catalyst layer has about an order or magnitude lower proton transfer resistance than Pt/C catalyst layer. Since the ionomer/support ratio that was used in formulating the ink for both catalysts was the same (0.9), it is expected that the volumetric coverage of ionomer of both catalysts will be significantly different due to the disparity in the surface areas (Pt/C had ~ 800 m2/g, while Pt/RTO had ~ 50 m2/g). The differences in the ionomer volumetric coverage and the ionomer film thickness may explain the significantly higher proton conductivity in the Pt/RTO catalyst layer when compared to Pt/HSAC. It is therefore very important to optimize the ionomer loadings when synthesizing new catalyst supports (and never rely on values for carbon-based commercial catalysts). Finally, NTCNA has elaborated a cost model for non-carbon support materials considering their durability benefits. Material costs for production of Pt/ RuO2-TiO2 electrodes were compared to Pt/C. RuO2-TiO2 support was more expensive than carbon but the total material cost was still dominated by platinum cost. Though ruthenium is considered a precious metal, its cost is far less than platinum. It should also be noted that ruthenium only makes up 38% of the mass of the support, while the rest is inexpensive TiO2. After considering the durability advantages of Pt/RTO, cost model showed that even with almost double the Pt loading (0.35 vs 0.18 mgPt/cm2), Pt/RTO ($22.7/kWnet) is only slightly more expensive than Pt/C ($21.9/kWnet).
Platinum monolayer (Pt ML ) core–shell electrocatalysts for the oxygen reduction reaction (ORR) have attracted great attention because of their exceptional activity and stability for promising practical applications in fuel cells. In this paper, we describe our in-depth investigation of the relationship between the ORR activity and structure of the Pt ML /Pd/C catalyst during the stability test. By virtue of the rotating disk electrode technique, an accelerated degradation test with the potential window of 0.65 to 1.05 V was applied to the Pt ML /Pd/C to interrogate its long-term reliability in the ORR, the change of its electrochemical surface area, and its surface composition and components. The Pt ML /Pd/C catalyst displayed a volcano-like mass/dollar activity profile in the stability test up to 100k cycles. The overall loss of the activity was recorded to be as low as 17% of the initial value. The ORR activity increased in the initial 20k cycles because the freshly prepared Pt ML did not entirely encompass the whole Pd core, but it was integrated to a full coverage with a more stable configuration during the potential cycling owing to its self-healing property. Then, the activity decreased at a much slower rate than the standard Pt/C because the Pd–Pt core–shell structure due to its structural self-retaining property remained intact and impeded the electrochemical Ostwald ripening of the entire particles. Changes in the morphology and configuration of Pt ML were mapped by combining our experimental investigation with model analyses. Finally, the proposed self-healing and self-retaining mechanisms account for the structure-dependent stability in the ORR and play cornerstone roles in formulating ORR core–shell electrocatalysts.
This report presents a preliminary plan to guide the qualification testing of advanced heat exchanger (HX) components for nuclear-to-industrial heat transfer applications. The objective is to establish a defensible, physics-based methodology that integrates computational modeling, targeted experimentation, and in-service inspection considerations to demonstrate component performance and reliability under representative reactor conditions. The analysis identifies Sodium-cooled Fast Reactor (SFR) and High-Temperature Gas-cooled Reactor (HTGR) systems as reference configurations in terms of temperature, pressure, and chemical environment. Within these operating envelopes, dominant degradation mechanisms— including creep–fatigue interaction, flow-induced vibration, corrosion, and diffusion-bond deterioration—were evaluated to define test requirements. A comprehensive computationalexperimental framework is proposed to support life prediction and qualification activities. The framework couples high-fidelity structural-mechanics, thermal-hydraulic, and fluid-structure interaction models with accelerated degradation testing to produce a traceable linkage between microstructural evolution, mechanical performance, and remaining useful life (RUL). The approach adheres to established Verification, Validation, and Uncertainty Quantification (VVUQ) standards (ASME V&V 10/20; NUREG-2152) and incorporates a digital-twin architecture for continuous model refinement through data assimilation. The plan further outlines testing methodologies, including pre-test analyses, test-loop design parameters, and sensor placement strategies that maximize information yield while maintaining mechanistic fidelity. Complementary sections describe in-service inspection (ISI), on-line monitoring (OLM), and structural-health-monitoring (SHM) techniques applicable to compact HX geometries typical of advanced reactors. Collectively, these activities establish the technical foundation for demonstrating 40-60-year equivalent service life of advanced heat exchangers in support of the U.S. Department of Energy’s Advanced Reactor and Integrated Energy Systems programs. The forthcoming phase will execute the defined pre-test analyses, initiate hardware fabrication, and implement the integrated testing campaign to validate the proposed qualification methodology.
To understand and develop models for silicon photovoltaic module degradation, accelerated testing is often used, however, outdoor field testing is necessary for validation. Outdoor field testing publications are often limited by the lack of a pristine, control module to compare the fielded module to. In this work, commercially available modules were purchased from seven different manufacturers for outdoor fielding then destructive characterization to investigate packaging material degradation on
On-line monitoring and tracking of nuclear plant system and component degradation is being investigated as a method for improving the safety, reliability, and maintainability of aging nuclear power plants. Accurate prediction of the current degradation state of system components and structures is important for accurate estimates of their remaining useful life (RUL). The correct quantification and propagation of both the measurement uncertainty and model uncertainty is necessary for quantifying the uncertainty of the RUL prediction. This research project developed and validated methods to perform RUL estimation throughout the lifecycle of plant components. Prognostic methods should seamlessly operate from beginning of component life (BOL) to end of component life (EOL). We term this "Lifecycle Prognostics." When a component is put into use, the only information available may be past failure times of similar components used in similar conditions, and the predicted failure distribution can be estimated with reliability methods such as Weibull Analysis (Type I Prognostics). As the component operates, it begins to degrade and consume its available life. This life consumption may be a function of system stresses, and the failure distribution should be updated to account for the system operational stress levels (Type II Prognostics). When degradation becomes apparent, this information can be used to again improve the RUL estimate (Type III Prognostics). This research focused on developing prognostics algorithms for the three types of prognostics, developing uncertainty quantification methods for each of the algorithms, and, most importantly, developing a framework using Bayesian methods to transition between prognostic model types and update failure distribution estimates as new information becomes available. The developed methods were then validated on a range of accelerated degradation test beds. The ultimate goal of prognostics is to provide an accurate assessment for RUL predictions, with as little uncertainty as possible. From a reliability and maintenance standpoint, there would be improved safety by avoiding all failures. Calculated risk would decrease, saving money by avoiding unnecessary maintenance. One major bottleneck for data-driven prognostics is the availability of run-to-failure degradation data. Without enough degradation data leading to failure, prognostic models can yield RUL distributions with large uncertainty or mathematically unsound predictions. To address these issues a "Lifecycle Prognostics" method was developed to create RUL distributions from Beginning of Life (BOL) to End of Life (EOL). This employs established Type I, II, and III prognostic methods, and Bayesian transitioning between each Type. Bayesian methods, as opposed to classical frequency statistics, show how an expected value, a priori, changes with new data to form a posterior distribution. For example, when you purchase a component you have a prior belief, or estimation, of how long it will operate before failing. As you operate it, you may collect information related to its condition that will allow you to update your estimated failure time. Bayesian methods are best used when limited data are available. The use of a prior also means that information is conserved when new data are available. The weightings of the prior belief and information contained in the sampled data are dependent on the variance (uncertainty) of the prior, the variance (uncertainty) of the data, and the amount of measured data (number of samples). If the variance of the prior is small compared to the uncertainty of the data, the prior will be weighed more heavily. However, as more data are collected, the data will be weighted more heavily and will eventually swamp out the prior in calculating the posterior distribution of model parameters. Fundamentally Bayesian analysis updates a prior belief with new data to get a posterior belief. The general approach to applying the Bayesian method to lifecycle prognostics consisted of identifying the prior, which is the RUL estimate and uncertainty from the previous prognostics type, and combining it with observational data related to the newer prognostics type. The resulting lifecycle prognostics algorithm uses all available information throughout the component lifecycle.
Designing acid-stable oxygen evolution reaction electrocatalysts is key to developing sustainable energy technologies such as polymer electrolyte membrane electrolyzers but has proven challenging due to the high applied anodic potentials and corrosive electrolyte. This work showcases advanced nanoscale microscopy techniques supported by complementary structural and chemical characterization to develop a fundamental understanding of stability in promising SrIrO 3 thin film electrocatalyst materials. Cross-sectional high-resolution transmission electron microscopy illustrates atomic-scale bulk and surface structure, while secondary ion mass spectrometry imaging using a helium ion microscope provides the nanoscale lateral elemental distribution at the surface. After accelerated degradation tests under anodic potential, the SrIrO 3 film thins and roughens, but the lateral distribution of Sr and Ir remains homogeneous. A layer-wise dissolution mechanism is hypothesized, wherein anodic potential causes the IrO x -rich surface to dissolve and be regenerated by Sr leaching. Finally, the characterization approaches utilized herein and mechanistic insights into SrIrO 3 are translatable to a wide range of catalyst systems.
The failure mechanisms of electrically conductive adhesives (ECAs) in solar modules are difficult to study since the ECA layer is not easily accessible within the module package. In this work, we present two complementary imaging modalities—X-ray radiography and X-ray microcomputed tomography (XCT)—that reveal important morphological features of the ECA within a shingled module. X-ray radiography uses single X-ray projections to provide fast and non-destructive imaging of the shingled interconnection, illuminating the alignment of the ECA relative to the busbars, the size and shape of the ECA, and the presence of voids within it. Through X-ray radiography, we observed, for example, that the average void coverage area of ECA segments reduced from 36.7% to 4.4% when an ECA was cured for 60 s prior to module lamination. XCT is a three-dimensional imaging technique that can identify regions in which the ECA makes electrical contact to busbars on cells and regions in which the ECA has cracked, among other features. XCT can also be used to image the individual metal particles within ECA, from which the metal volume fraction of an ECA was found here to be 70.4%. This is a quantity that is not often reported by ECA manufacturers but is important to ensure isotropic conduction. As X-ray projections can be performed non-destructively on full modules, the technique may be used to pinpoint ECA failures in accelerated degradation testing. XCT is complementary and is suited to forensic analysis of failing modules.
In this paper, we report on the electrochemical behavior and corrosion resistance of as-prepared aluminum alloy, A360 (AlSi10Mg), fabricated by additive manufacturing, with and without a trivalent chromium process conversion coating. Selective laser melting was the 3D printing process used for the alloy build. The corrosion suppression provided by the coating system was assessed through electrochemical measurements and accelerated degradation testing during a 14-day continuous neutral salt-spray exposure. The results indicate that the conversion coating can be formed by solution pretreating (degreasing and deoxidation) the alloy (X-Z plane perpendicular to the build plane) with its native surface roughness (as-prepared) followed by immersion for 10, 15 or 20 min in the coating bath. All three immersion times provide an equivalent level of corrosion protection to the alloy. The conversion coating suppresses both anodic and cathodic currents, increases the polarization resistance, and provides both anodic and cathodic corrosion protection to the as-prepared alloy. The conversion-coated specimens exhibit good stand-alone corrosion resistance during a 14-day neutral salt-spray exposure with corrosion intensity values (g/m 2 -year) ~10x lower than values for the uncoated, as-prepared alloy specimens.
The main objectives for this project were to formulate, validate and disseminate a new procedure based on Environmental X-ray Photoelectron Spectroscopy (EXPS) for the accelerated degradation testing of metal hybrid perovskite (MHP) PV materials. With this capability, we can aid US efforts to improve MHP tolerance for illumination in damp heat conditions. This capability will benefit the public by supporting new industry efforts to create stable MHP formulations.
This project seeks to develop device design, materials composition, and processing tools and parameters to fabricate semi-transparent perovskite solar cells and modules for application in stand-alone products or added to other solar cells in a mechanically stacked tandem configuration. This technology presents significant advanced manufacturing challenges and opportunities in getting to scale, including development of perovskite inks, scalable perovskite and heterojunction deposition and annealing processes, heterojunction composition, transparent electrode composition and deposition process, anti-reflection layer composition and deposition process, and cell to module integration processes. Modification 5: The proposed project seeks to develop device design, materials composition, and processing tools and parameters to fabricate semi-transparent perovskite solar cells and modules for application in stand-alone products or added to other solar cells in a mechanically-stacked tandem configuration. This technology presents significant advanced manufacturing challenges and opportunities in getting to scale, including development of perovskite inks, scalable perovskite and heterojunction deposition and annealing processes, heterojunction composition, transparent electrode composition and deposition process, passivation layers including in module scribes, anti-reflection layer composition and deposition process, and cell to module integration processes. Advanced metrology and characterization will be performed on perovskite films, cells and module. Furthermore, we will examine module or materials recycling for circular economy considerations. Modifcation 6: Gigahertz frequency microwave pump-probe spectroscopies are highly sensitive to thin film semiconductor photoconductivity of individual and stacks of layers that comprise perovskite solar cells. As such, these techniques will be used to qualify reproducibility and quality correlations during the manufacturing process. Modification 7: Mechanical adhesion of top contacts within perovskite modules significantly impacts the durability of the module when exposed to accelerated degradation testing. The adhesion between the perovskite/transport layer interface and the transport layer/top contact interface are both very sensitive small changes in processing. ALD processing conditions of the transport layer will be tuned to optimize the mechanical adhesion within the perovskite module stack.
In this study, we highlight some important factors in the specimen preparation methods for evaluating photovoltaic backsheet properties after accelerated aging. Two different sequences are considered: Method (I) cut-then-age: cut into 1-cm wide strips and then expose to stress, and Method (II) age-then-cut: expose a larger sheet to stress and then cut into 1-cm widths for mechanical property measurements. We also compare the effect of three cutting methods, (a) tensile specimen punch, (b) paper cutter, and (c) fresh razor blade. Several commercial backsheets were evaluated, with stress exposures including (a) pressure cooker test (PCT), (b) dry ultraviolet (UV) radiation exposure, and (c) UV combined damp heat tests. Fourier transform infrared spectrometer (FTIR) and intrinsic viscosity (IV) were used to analyze the materials on unstressed materials and samples exposed to PCT. The results show that both the cutting method and the time of cutting have an impact on the backsheet mechanical properties. Additionally, under UV exposure, Method II, age-then-cut, generally resulted in a higher average value, with more variation than Method I; however, if the side strips from Method II were excluded, the variation dropped to the same level. This is because the specimens at the sides of the sheet get additional damage from UV light from the exposed sides of the sample. In contrast to UV exposure, PCT specimens prepared by Method II result in lower average values and higher variability. This is attributed to embrittlement through the bulk of the sample where the cutting of embrittled specimens appears to result in more edge defects which can then initiate a break at smaller strains. The data suggest that for UV exposures, the specimens should be cut after aging and the exposed side specimens discarded, and that for PCT exposures, the specimens should be cut before the exposure.
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