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All sourcesNASA NTRSDOE OSTI
DOE OSTI2013

Large-scale Manufacturing of Nanoparticulate-based Lubrication Additives for Improved Energy Efficiency and Reduced Emissions

This project was funded under the Department of Energy (DOE) Lab Call on Nanomanufacturing for Energy Efficiency and was directed toward the development of novel boron-based nanocolloidal lubrication additives for improving the friction and wear performance of machine components in a wide range of industrial and transportation applications. Argonne's research team concentrated on the scientific and technical aspects of the project, using a range of state-of-the art analytical and tribological test facilities. Argonne has extensive past experience and expertise in working with boron-based solid and liquid lubrication additives, and has intellectual property ownership of several. There were two industrial collaborators in this project: Ashland Oil (represented by its Valvoline subsidiary) and Primet Precision Materials, Inc. (a leading nanomaterials company). There was also a sub-contract with the University of Arkansas. The major objectives of the project were to develop novel boron-based nanocolloidal lubrication additives and to optimize and verify their performance under boundary-lubricated sliding conditions. The project also tackled problems related to colloidal dispersion, larger-scale manufacturing and blending of nano-additives with base carrier oils. Other important issues dealt with in the project were determination of the optimum size and concentration of the particles and compatibility with various base fluids and/or additives. Boron-based particulate additives considered in this project included boric acid (H 3 BO 3 ), hexagonal boron nitride (h-BN), boron oxide, and borax. As part of this project, we also explored a hybrid MoS 2 + boric acid formulation approach for more effective lubrication and reported the results. The major motivation behind this work was to reduce energy losses related to friction and wear in a wide spectrum of mechanical systems and thereby reduce our dependence on imported oil. Growing concern over greenhouse gas emissions was also a major reason. The transportation sector alone consumes about 13 million barrels of crude oil per day (nearly 60% of which is imported) and is responsible for about 30% of the CO 2 emission. When we consider manufacturing and other energy-intensive industrial processes, the amount of petroleum being consumed due to friction and wear reaches more than 20 million barrels per day (from official energy statistics, U.S. Energy Information Administration). Frequent remanufacturing and/or replacement of worn parts due to friction-, wear-, and scuffing-related degradations also consume significant amounts of energy and give rise to additional CO 2 emission. Overall, the total annual cost of friction- and wear-related energy and material losses is estimated to be rather significant (i.e., as much as 5% of the gross national products of highly industrialized nations). It is projected that more than half of the total friction- and wear-related energy losses can be recovered by developing and implementing advanced friction and wear control technologies. In transportation vehicles alone, 10% to 15% of the fuel energy is spent to overcome friction. If we can cut down the friction- and wear-related energy losses by half, then we can potentially save up to 1.5 million barrels of petroleum per day. Also, less friction and wear would mean less energy consumption as well as less carbon emissions and hazardous byproducts being generated and released to the environment. New and more robust anti-friction and -wear control technologies may thus have a significant positive impact on improving the efficiency and environmental cleanliness of the current legacy fleet and future transportation systems. Effective control of friction in other industrial sectors such as manufacturing, power generation, mining and oil exploration, and agricultural and earthmoving machinery may bring more energy savings. Therefore, this project was timely and responsive to the energy and environmental objectives of DOE and our nation. In this project, most of the boron-based materials with known and potential anti-friction and -wear properties have been manufactured as colloidal additives and tested for their effectiveness in controlling friction and wear. Unlike other anti-friction and -wear additives, which consist of zinc, molybdenum, sulfur, phosphorus, and even chlorine, lubricious boron compounds considered in this project are made of boron, oxygen, nitrogen, and hydrogen, which are more environmentally benign. Among others, boric acid is a natural mineral (known in mineralogy as "sassolite"). Based on our earlier exploratory research, it was found to offer the best overall prospect in terms of performance improvements, environmental friendliness, and ease of manufacturing and, hence, cost effectiveness. Hexagonal boron nitride and borax also offered good prospects for improving the tribological properties of lubricated sliding surfaces. Boron oxide particles were found to be rather hard and somewhat abrasive and, hence, were not considered beyond the initial screening studies. In our bench-top tribological evaluation, we also demonstrated that those additives which worked well with engine oils could work equally well with very common gear oils. When added at appropriate concentrations, such gear oils were found to provide significant resistance to micropitting and scuffing failures in bench-top tribological test systems. Their traction coefficients were also reduced substantially and their scuffing limits were improved considerably. Such impressive tribological behavior of boron-based additives may have been due to their high chemical affinities to interact with sliding contact surfaces and to form slick and protective boundary films. Indeed, our surface studies have confirmed that most of the boron-based nanoparticulate additives prepared in our project possess a strong tendency to form a boron-rich boundary film on sliding contact surfaces. It is believed that the formation of such slick and highly durable boundary films is perhaps one of the fundamental reasons for their superior anti-friction, -wear, and -scuffing performance. Boron-based additives developed under this project have shown potential to reduce or replace the uses of environmentally unsafe sulfur- and phosphorus-bearing anti-wear and friction additives, such as zinc dialkyl dithiophosphate (ZDDP) and molybdenum dialkyl dithiocarbamate (MoDTC), in current lubricating oils. Because ZDDP and MoDTC were suspected of adversely impacting the performance of after-treatment catalysts in current engines, the Environmental Protection Agency (EPA) and other regulatory agencies are demanding that the concentrations of these catalysts in current oils be curtailed drastically. The boron-based nano-additives developed in this project may help reduce the use of ZDDP and MoDTC additives and, hence, help ease the poisoning effects on after-treatment catalysts. When used as lubricity additives, these boron additives can chemically interact with sliding or contacting surfaces and form a protective and slick boundary film, which can, in turn, help reduce friction and wear and increase resistance to scuffing. In the cases of traditional anti-friction and -wear additives mentioned, such protective boundary films result from phosphorus, sulfur, and other elements in the additive package, and again they have been under increased scrutiny in recent years, mainly because of their adverse effects on after-treatment devices. Overall, the boron-based nano-additive technology of this project was shown to hold promise for a broad range of industrial and transportation applications where lower friction and higher resistance to wear and scuffing are needed. Due to more stringent operating conditions of modern machinery, rolling, rotating, and sliding components have been failing to meet the projected lifetimes, mainly because of failures related to mechanical wear, corrosion, and scuffing. The novel boron-based additive technology developed under this project may help such machine components to function reliably by cutting down the friction and wear losses and by increasing resistance to scuffing.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2014

Erosion-Corrosion of Iron and Nickel Alloys at Elevated Temperature in a Combustion Gas Environment

This paper reports on the results of a study that compares the erosion-corrosion behavior of a variety of alloys (Fe- 2¼Cr 1Mo, 304 SS, 310 SS, Incoloy 800, Haynes 230 and a Fe 3 Al) in a combustion environment. Advanced coal combustion environments, with higher temperatures, are driving re-examination of traditional and examination of new alloys in these hostile environments. In order to simulate conditions in advanced coal combustion boilers, a special erosion apparatus was used to allow for impingement of particles under a low abrasive flux in a gaseous environment comprised of 20 % CO 2 , 0.05 % HCl, 77 % N 2 , 3 % O 2 , and 0.1 % SO 2 . Tests were conducted at room temperature and 700 °C with ~ 270 μm silica, using an impact velocity of 20 m/s in both air and the simulated combustion gas environment. The erosion-corrosion behavior was characterized by gravimetric measurements and by examination of the degraded surfaces optically and by scanning electron microscopy (SEM). At room temperature most of the alloys had similar loss rates. Not surprisingly, at 700 °C the lower chrome-iron alloy had a very high loss rate. The nickel alloys tended to have higher loss rates than the high chrome austenitic alloys.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2014

Application of Super-Hydrophobic Coating for Enhanced Water Repellency of Ballistic Fabric

The objective of this work was to demonstrate that a superhydrophobic coating technology developed at Oak Ridge National Laboratory (ORNL) increases the water repellency of ballistic fabric beyond that provided by existing water repellency treatments. This increased water repellency has the potential to provide durable ballistic fabric for body armor without adding significant weight to the armor or significant manufacturing cost. Specimens of greige and scoured ballistic fabric were treated with a superhydrophobic coating and their weights and degree of water repellency were compared to specimens of untreated fabric. Treatment of both greige and scoured ballistic fabrics yielded highly water repellent fabrics. Our measurements of the water droplet contact angles gave values of approximately 150 , near the lower limit of 160 for superhydrophobic surfaces. The coatings increased the fabric weights by approximately 6%, an amount that is many times less than the estimated weight increase in a conventional treatment of ballistic fabric. The treated fabrics retained a significant amount of water repellency following a basic abrasion test, with water droplet contact angles decreasing by 14 to 23 . Microscopic analysis of the coating applied to woven fabrics indicated that the coating adhered equally well to fibers of greige and scoured yarns. Future evaluation of the superhydrophobic water repellent treatment will involve the manufacture of shoot packs of treated fabric for ballistic testing and provide an analysis of manufacturing scale-up and cost-to-benefit considerations.

superhydrophobic water repellent coating treatment↗
DOE OSTI2014

Results of stainless steel canister corrosion studies and environmental sample investigations

This progress report describes work being done at Sandia National Laboratories (SNL) to assess the localized corrosion performance of container/cask materials used in the interim storage of used nuclear fuel. The work involves both characterization of the potential physical and chemical environment on the surface of the storage canisters and how it might evolve through time, and testing to evaluate performance of the canister materials under anticipated storage conditions. To evaluate the potential environment on the surface of the canisters, SNL is working with the Electric Power Research Institute (EPRI) to collect and analyze dust samples from the surface of in-service SNF storage canisters. In FY 13, SNL analyzed samples from the Calvert Cliffs Independent Spent Fuel Storage Installation (ISFSI); here, results are presented for samples collected from two additional near-marine ISFSI sites, Hope Creek NJ, and Diablo Canyon CA. The Hope Creek site is located on the shores of the Delaware River within the tidal zone; the water is brackish and wave action is normally minor. The Diablo Canyon site is located on a rocky Pacific Ocean shoreline with breaking waves. Two types of samples were collected: SaltSmart™ samples, which leach the soluble salts from a known surface area of the canister, and dry pad samples, which collected a surface salt and dust using a swipe method with a mildly abrasive ScotchBrite™ pad. The dry samples were used to characterize the mineralogy and texture of the soluble and insoluble components in the dust via microanalytical techniques, including mapping X-ray Fluorescence spectroscopy and Scanning Electron Microscopy. For both Hope Creek and Diablo Canyon canisters, dust loadings were much higher on the flat upper surfaces of the canisters than on the vertical sides. Maximum dust sizes collected at both sites were slightly larger than 20 μm, but Phragmites grass seeds ~1 mm in size, were observed on the tops of the Hope Creek canisters. At both sites, the surface dust could be divided into fractions generated by manufacturing processes and by natural processes. The fraction from manufacturing processes consisted of variably-oxidized angular and spherical particles of stainless steel and iron, generated by machining and welding/cutting processes, respectively. Dust from natural sources consisted largely of detrital quartz and aluminosilicates (feldspars and clays) at both sites. At Hope Creek, soluble salts were dominated by sulfates and nitrates, mostly of calcium. Chloride was a trace component and the only chloride mineral observed by SEM was NaCl. Chloride surface loads measured by the Saltsmart™ sensors were very low, less than 60 mg m –2 on the canister top, and less than 10 mg m –2 on the canister sides. At Diablo Canyon, sea-salt aggregates of NaCl and Mg-SO 4 , with minor K and Ca, were abundant in the dust, in some cases dominating the observed dust assemblage. Measured Saltsmart™ chloride surface loads were very low (<5 mg m –2 ); however, high canister surface temperatures damaged the Saltsmart™ sensors, and, in view of the SEM observations of abundant sea-salts on the package surfaces, the measured surface loads may not be valid. Moreover, the more heavily-loaded canister tops at Diablo Canyon were not sampled with the Saltsmart™ sensors. The observed low surface loads do not preclude chloride-induced stress corrosion cracking (CISCC) at either site, because (1) the measured data may not be valid for the Diablo Canyon canisters; (2) the surface coverage was not complete (for instance, the 45º offset between the outlet and inlet vents means that near-inlet areas, likely to have heavier dust and salt loads, were not sampled); and (3) CISCC has been experimentally been observed at salt loads as low as 5-8 mg/m 2 . Experimental efforts at SNL to assess corrosion of interim storage canister materials include three tasks in FY14. First, a full-diameter canister mockup, made using materials and techniques identical to those used to make interim storage canisters, was designed and ordered from Ranor Inc., a cask vendor for Areva/TN. The mockup will be delivered prior to the end of FY14, and will be used for evaluating weld residual stresses and degrees of sensitization for typical interim storage canister welds. Following weld characterization, the mockup will be sectioned and provided to participating organizations for corrosion testing purposes. A test plan is being developed for these efforts. In a second task, experimental work was carried out to evaluate crevice corrosion of 304SS in the presence of limited reactants, as would be present on a dustcovered storage canister. This work tests the theory that limited salt loads will limit corrosion penetration over time, and is a continuation of work carried out in FY13. Laser confocal microscopy was utilized to assess the volume and depth of corrosion pits formed during the crevice corrosion tests. Results indicate that for the duration of the current experiments (100 days), no stifling of corrosion occurred due to limitations in the amount of reactants present at three different salt loadings. Finally, work has been carried out this year perfecting an instrument for depositing sea-salts onto metal surfaces for atmospheric corrosion testing purposes. The system uses an X-Y plotter system with a commercial airbrush, and deposition is monitored with a quartz crystal microbalance. The system is capable of depositing very even salt loadings, even at very low total deposition rates.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Analysis of Dust Samples Collected from an Unused Spent Nuclear Fuel Interim Storage Container at Hope Creek, Delaware

In July, 2014, the Electric Power Research Institute and industry partners sampled dust on the surface of an unused canister that had been stored in an overpack at the Hope Creek Nuclear Generating Station for approximately one year. The foreign material exclusion (FME) cover that had been on the top of the canister during storage, and a second recently-removed FME cover, were also sampled. This report summarizes the results of analyses of dust samples collected from the unused Hope Creek canister and the FME covers. Both wet and dry samples of the dust/salts were collected, using SaltSmart(TM) sensors and Scotch-Brite(TM) abrasive pads, respectively. The SaltSmart(TM) samples were leached and the leachate analyzed chemically to determine the composition and surface load per unit area of soluble salts present on the canister surface. The dry pad samples were analyzed by X-ray fluorescence and by scanning electron microscopy to determine dust texture and mineralogy; and by leaching and chemical analysis to deter mine soluble salt compositions. The analyses showed that the dominant particles on the canister surface were stainless steel particles, generated during manufacturing of the canister. Sparse environmentally - derived silicates and aluminosilicates were also present. Salt phases were sparse, and consisted of mostly of sulfates with rare nitrates and chlorides. On the FME covers, the dusts were mostly silicates/aluminosilicates; the soluble salts were consistent with those on the canister surface, and were dominantly sulfates. It should be noted that the FME covers were w ashed by rain prior to sampling, which had an unknown effect of the measured salt loads and compositions. Sulfate salts dominated the assemblages on the canister and FME surfaces, and included Ca-SO 4 , but also Na-SO 4 , K-SO 4 , and Na-Al-SO 4 . It is likely that these salts were formed by particle - gas conversion reactions, either prior to, or after, deposition. These reactions involve reaction of carbonate, chloride, or nitrate salts with at mospheric SO 2 , sulfuric acid, or a mmonium sulfate to form sulfate minerals. The Na-Al-SO 4 phase is unusual, and may have formed by reaction of Na-Al containing phases in aluminum smelter emissions with SO 2 , also present in smelter emissions. An aluminum smelter is located in Camden, NJ, 40 miles NE of the Hope Creek Site.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Atomically Bonded Transparent Superhydrophobic Coatings

Maintaining clarity and avoiding the accumulation of water and dirt on optically transparent surfaces such as US military vehicle windshields, viewports, periscope optical head windows, and electronic equipment cover glasses are critical to providing a high level of visibility, improved survivability, and much-needed safety for warfighters in the field. Through a combination of physical vapor deposition techniques and the exploitation of metastable phase separation in low-alkali borosilicate, a novel technology was developed for the fabrication of optically transparent, porous nanostructured silica thin film coatings that are strongly bonded to glass platforms. The nanotextured films, initially structurally superhydrophilic, exhibit superior superhydrophobicity, hence antisoiling ability, following a simple but robust modification in surface chemistry. The surfaces yield water droplet contact angles as high as 172°. Moreover, the nanostructured nature of these coatings provides increased light scattering in the UV regime and reduced reflectivity (i.e., enhanced transmission) over a broad range of the visible spectrum. In addition to these functionalities, the coatings exhibit superior mechanical resistance to abrasion and are thermally stable to temperatures approaching 500°C. The overall process technology relies on industry standard equipment and inherently scalable manufacturing processes and demands only nontoxic, naturally abundant, and inexpensive base materials. Such coatings, applied to the optical components of current and future combat equipment and military vehicles will provide a significant strategic advantage for warfighters. The inherent self-cleaning properties of such superhydrophobic coatings will also mitigate biofouling of optical windows exposed to high-humidity conditions and can help decrease repair/replacement costs, reduce maintenance, and increase readiness by limiting equipment downtime.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Materials and Additive Manufacturing for Energy Efficiency in Wind Turbine and Aircraft Industries

The purpose of this project was to develop surface treatments which will inhibit the formation of ice on turbine blades and propellers. ORNL worked with Piedmont Propulsion Systems, LLC and First Aviation Services Inc. to demonstrate a new surface treatment for two primary markets, aviation and wind turbines, as well as secondary markets such as power lines, bridges, boats, roofs and antennas among others. Exploring alternative surface treatments for wind turbines will provide anti-icing properties and erosion/abrasion prevention properties similar to those for aviation applications. A series of superhydrophobic coating materials was synthesized and successfully applied on anti-ice tape materials that could be used in a wide range of wind turbine and aviation applications to prevent ice accumulation. The coatings developed in this project were based on superhydrophobic particles of different geometries and sizes that were homogeneously dispersed in polymeric binders. The superhydrophobic features of the coatings are volumetric and their abrasion resistance was evaluated. Future research will involve the demonstration of anti-icing properties of the surface treatment developed in this project.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2012

Wireless link and microelectronics design for retinal prostheses

This project focuses on delivering power and data to the artificial retinal implant inside the eye and the implant microstimulator electronics which delivers the current pulses to stimulate the retinal layer to elicit visual perception. Since the use of invasive means such as tethering wires to transmit power and data results in discomfort to the patients which could eventually cause infection due to the abrasion caused by the wire and contact of the internals of the eye to the external environment, a completely wireless approach is used to transfer both power and data. Power is required inside the eye for the microelectronic implant which uses a dual voltage supply scheme (positive and negative) to deliver biphasic (anodic and cathodic) current pulses. Data in the form of digital bits from the data transmitter external to the eye, carries information about the amplitude, phase width, interphase delay, stimulation sequence for each implant electrode. The data receiver unit decodes the digital stream and the microstimulator unit generates the appropriate current stimuli. Since the external unit consisting of the power transmitter can experience coupling a variation with the power receiver due to the patient’s movements, a closed loop approach is used which varies the transmitted power dynamically to automatically compensate for such movements. This report presents the salient features of this research activities and results.

42 ENGINEERING↗
DOE OSTI2018

Advanced SOFC quality control and the role of manufacturing defects on stack reliability

Atrex Energy rolled out first commercial SOFC generator products in 2013. Following that we embarked on implementation of mass production in order to ramp up productivity and lower the costs in the meantime. To ensure the goal of mass production, an accurate, cost effective and consistent quality control methodology needs to be in place. The aim of this DOE funded project is to devise a machine and methodology for cell quality control using modern non-destructive testing methods and cell rejection criterion based on the empirical determination of the role of manufacturing flaws on stack degradation and reliability. The work scope encompasses two goals aimed at 1) developing automatable techniques for objective flaw detection and 2) developing an understanding of the ramifications of flaws on stack and cell reliability. By accomplishing these two goals it is likely that an advanced stage Quality Control (QC) device can be developed. This project scope encompasses: 1) Invention of a high speed automated instrument for spatial mapping of surface and sub-surface imperfections in production cells (ex situ) using modern imaging techniques. 2) Identification of rejection criteria upon which to screen cells from production by: a. Magnification of the effect of production defects on cell degradation through fabrication and testing of micro-cells which encompass these imperfections. b. The long term testing of full size production cells both as single cells and in small stacks, in order to correlate the (in situ) performance and degradation with the imperfection type (identified ex-situ) and hence be able to classify imperfections as actual defects. We first built a defect library with the cells containing imperfections classified and documented. The cells with various imperfections were tested to evaluate the imperfection potential impact on cell electrochemical performance. Evaluations were conducted on minicell, single cell and stack levels. On minicell level, pinhole, scratch, crack, contamination, and pop-out were investigated. We found: (1) none of the imperfections causes calamity type failure, (2) pinholes do not show measurable effect on minicell performance, (3) imperfection such as electrolyte abrasion, scratch, and pop out cause minicell potential to fluctuate by different degrees; the cells with such imperfections exhibit sensitivity of potential to high fuel utilization and “self healing” behavior. On single cell level we evaluated the effect of long crack and high population pinholes. The cell with a long crack does not show performance compromise at start. There is no potential fluctuation or sensitivity to high fuel utilization or catastrophic failure. The voltage degradation due to thermal cycle is slightly higher than normal cells. The cells with high population pinholes perform surprisingly as well as normal cells over a period of 3,500h. Even when subjected to cyclic load condition, the cells 4 show negligible degradation. Our cells appear to have “self immunization” feature which fends off the adversary effects of certain imperfections. Defects were also evaluated on stack level. Two stacks were made each with ten defect cells. The first stack was tested for 13,2000h under steady load condition while the second was tested for 9,000h under transient load conditions. We found: (1) voltage fluctuation and sensitivity to thermal cycle were not observed in contrast to minicell test, (2) of the various cracks examined, including longitudinal cracks, circumferential crack, crack near closed and open ends, none exhibited distinguishable impact on performance, (3) defect cells exhibited higher degradation rates on average under steady load condition; Individually some defect cells performed similarly or better than reference cells, (4) under steady load condition all the cells degrade monotonically with degradation rate increasing with time, (5) under cyclic (transient) load condition, both defect and reference cells exhibit complex dynamic behaviors, (6) fuel loss (leak) was measured occasionally for stack 1, the cells with crack showed the highest fuel loss increase, nevertheless, no correlation with performance degradation could be established with certainty, and (7) no catastrophic failure ever happened other than incremental degradation. Posttest inspection and microanalysis were carried out; the observations are summarized in what follows: (1) Electrolyte pinholes, some scratches and IC porosity became undetectable after testing. (2) The cathode covering the popout defects is intact without any cracking or delamination. (3) The scratch was covered by cathode in pristine state; Ni oxide or NiO-YSZ filled the space where electrolyte was missing. After >10,000h operation, the cathode that used to cover the scratch was missing but the size of the scratch remains unchanged; there is a fairly dense Ni oxide layer on top of the scratch. (4) All of the cracks remain their original dimensions. Current collector kept longitudinal cracks closed which mitigated the adversary effect of crack on cell performance/durability. (5) The crack at open end showed some deterioration manifested by a small oxidation zone in the vicinity of the crack. Wide spectrum of imaging techniques were surveyed and evaluated to detect tubular SOFC defects. Optical methods, with and without assistance of expression technique, were applied to detect all kinds of defects. Thermograph method in combination of CO2 leak, ultra-sound and electric potential was also extensively evaluated to detect surface and under-surface defects such as short circuit. Based on these works, laser camera has been selected to build the final QC machine vision inspection system. The Gocator laser profile sensor was setup to generate 2D surface intensity images of tubular SOFC surface which were analyzed with Sherlock machine vision software supplied by Teledyne Dalsa. The Gocator output was integrated with the Sherlock software and enabled live images to be imported by a Common Vision Blox driver. The Sherlock software was programmed to detect various surface defects from the surface intensity images generated by the Gocator. These measurements are subsequently used to make pass or fail decisions.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2018

The Effect of Aging on the Delamination Fracture Energy of Glass Solar Reflectors

Thin metal and metal oxide films deposited on glass or polymer substrates have been widely applied to manufacture front surfaced solar reflectors such as those used in the concentrated solar power (CSP) systems due to the facts that they are highly transparent, resistant to ultraviolet (UV) light and abrasion, and chemically inert. However, the reliable operation over long periods of outdoor exposure of such solar reflectors depends on the adequate adhesion between each layer to prevent delamination and subsequent failure. We report results from measurements of the delamination fracture energy (DFE) of the weakest interface in both as-deposited and aged reflectors, where the reflector construction consists of a glass/copper/silver/oxide stack. In this study, DFE was measured using a width-tapered beam method and the test results showed that the weakest interface of this solar reflector is the copper-glass interface, with a delamination fracture energy of approximately 4.4 J/m 2 . In order to verify the test results, finite element (FE) simulations were run using the commercial software package ABAQUS 6.14 based on the cohesive zone model (CZM). In the simulations, the DFE derived from the delamination measurement was treated as an input and the delamination forces from the FE simulations were compared to the experimental results. The good agreement between the tested and simulated delamination force indicated that this width-tapered beam method is accurate even for very small DFE, making it appropriate to test the DFE of front surfaced glass solar reflectors. Additionally, in order to study the aging effect on the DFE, accelerated aging tests were conducted using samples with different protective coatings, one group of samples with alumina ( Al 2 O 3 ) protective coating and the other group with titania ( TiO 2 ) protective coating. The DFE after 50 and 100 hours of accelerated aging were measured. The test results showed that the copper-glass interface would still be the weakest interface for all samples after aging, and the DFE for samples with Al 2 O 3 protective coating was unchanged whereas the copper-glass interface was found to undergo statistically significant change after both 50 and 100 hours of aging for samples with TiO 2 protective coating. We found that DFE at the copper/glass interface decreased after 50 hours of aging then increased after 100 hours of aging. The origin of this non-monotonic response of TiO 2 coated reflectors under accelerated aging conditions is unknown.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Stereolithographic Fabrication of a Flow Cell For Improved Neurochemical Sensor Testing

The human brain remains a mystery to researchers. Scientists at Lawrence Livermore National Laboratory (LLNL) have developed highly sensitive and flexible multimodal multielectrode arrays (MEAs) with the potential to be both powerful diagnostic and therapeutic tools when dealing with neurological ailments such as Alzheimers, Parkinson’s, Post Traumatic Stress Disorder, and Traumatic Brain Injuries. These MEAs include biosensors in addition to electrodes for electrical stimulation and recording. The transition from the traditional rigid neural probes to the flexible MEAs has led LLNL researchers on the search for alternative testing and characterization methods for flexible devices in vitro. The rigid devices have been shown to be more abrasive and damaging to the brain when implanted, but due to their rigidity – are more robust and resilient to noise artifacts in in vitro testing. The flexible MEAs, similar in size and flexibility to a human hair, cause much less damage in the brain but have had a difficult time maintaining their integrity and collecting data without high-levels of noise due to the formation of inertial eddies (due to increased turbulent flow) moving the flexible MEA during in vitro testing. The goal of this project was to design a fluidic cell to allow for a more constant electrochemical testing & characterization of biosensors on these flexible MEAs. Design and fabrication of the fluidic cell was through the use of CAD software and a stereolithography printer using clear photopolymer resin (appropriate for biomedical use and quality resolution). Flow cells facilitate analyte delivery to biosensor surfaces in a more constant and controlled fashion, allowing for –in this case –a better electrodeposition of thin-film Platinum-Iridium (Pt-Ir) on MEAs of 16 Platinum disc electrodes 50µm in diameter. Platinum-Iridium alloy electrodes have been widely used in biomedical and industrial applications. Iridium adds mechanical stiffness to platinum. PtIr is a FDA approved electrode material for human implantable devices.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Slippery Omniphobic Covalently Attached Liquids for Extreme Anti-Scaling

Fouling is amajor unresolved problem in a varietyof industries including power generation, water desalination,and hydrometallurgy. In a heat exchanger, the accumulated salt scale could lead to a decrease in heat transfer, corrosion, blockage of flow and increasedpressure drop, resulting in higher operation costsand shortened equipment lifetime. The added operational costs due to active scale removal techniques such as mechanical abrasion and chemical inhibitors are responsible for 0.25% of the GDP in industrialized nations.Herewe utilize slippery omniphobic covalently attached liquids (SOCAL) dip coating on aluminum substrates to minimize surface energyand surface roughness, hence maximizingthe energy barrier for scale formation. To enable SOCAL surfacebinding on aluminum, we started by depositinga nanoscale(500 nm thick)adhesion layer of SiO2using scalable and cost-effective electrophoretic deposition (EPD), followed by SOCAL grafting to the SiO2.The EPD SiO2coating chemistry was tailored to achieve a smoothsurface finish which, combined with the low surface energyof the SOCAL coating, translated to extreme anti-scaling performance. Thermal degradation testing in an ambient environment revealed the covalently bonded SOCAL coatingswithstand temperatures of 100°C. To characterize scaling, we utilized CaSO4and CaCO3scale tests, showing up to 20X less scaling than uncoated aluminum. Descaling tests revealed that our SOCAL coatings dramatically decrease scale adhesion, resulting in rapid removal of scale buildup in highly supersaturated conditions. To investigate manufacturability, two alternate methods of SiO2deposition were tested, including physical vapor deposition and spin-on glass, with great success in coating smooth metallic substrates, but limited success due to the inability to coat arbitrarily shaped surfaces. Our work not only demonstrates a facile method of tailoring interfacial energy and roughness to control fouling, it develops cost-effective, scalable,and high performing anti-fouling coating applicable to aluminum surfacesfor a variety of applications.

Zhao, Hanyang↗
DOE OSTI2018

HIGH-STRENGTH LIGHTWEIGHT ENGINES FOR HEAVY-DUTY DIESEL TRUCKS

This project with Cummins supports the development of next generation heavy duty diesel engines that can achieve a 50% or better Break Thermal Efficiency (BTE). The fuel efficiency roadmap for the 50% BTE engine considers six main areas for efficiency improvement in the baseline engine, several of which involve making more efficient use of thermal energy (heat) in the engine. Increased operating temperatures and improved thermal management are expected to enable significant increases in $power$ $density$, thus resulting in greater power output for the same sized engine or engine downsizing (or light weighting) for the same power output. However, it has become apparent that several key components will be exposed to temperatures beyond the capabilities of current engine and exhaust materials, requiring the availability of the next generation of high temperature materials to allow the engine to reach the targeted efficiencies, commercially viable durability, and emission targets. The objective of this project was to identify and/or develop key materials, and evaluate their critical properties to enable the design and development of a lightweight, higher efficiency engine, with enhanced temperature capability and reduced heat-loss to the atmosphere in order to facilitate waste heat recovery and improved efficiency. An increase in the temperature capability of exhaust manifold materials, and piston materials were identified as having a positive influence on the efficiency of the next generation diesel engines. Since the current materials (High SiMo cast irons used in exhaust manifolds, and 4140 steel in pistons) are already operating near their limits of their temperature and strength capabilities, it was determined that new materials with the right combination of properties are required for these components. Oxidation and constrained thermal fatigue tests were used to down-select CF8C plus (CF8CP), a cast austenitic stainless steel, for exhaust manifolds capable of operating at higher temperatures. A prototype exhaust manifold was fabricated using CF8CP and successfully tested in a marine engine. A functionally graded multiple-layer thermal barrier coating system was designed with four layers of mixed bondcoat alloy (NiCoCrAlYHfSi) and yttria stabilized zirconia (YSZ) and was shown to reduce the effective thermal conductivity of the coating-substrate (steel and Ti-6Al-4V) system. The graded alloy and YSZ mixture were intended to achieve better match of thermal expansion coefficient (CTE) and minimize thermal stresses. Such coatings can increase the temperature capability of pistons fabricated from steel and Ti-alloys. Effect of oil additives and friction conformal contact friction tests showed there was a 15-30% reduction in friction by the polymer-graphite composite coating compared to the uncoated steel piston. Standalone Mn-P coating had little beneficial impact. Changing the oil from CJ-4 to PC-11 had little impact on the friction behavior in boundary lubrication. Wear behavior was tested under a point contact configuration with a high contact pressure. The candidate CK-4 oil showed similar or slightly better lubricity compared to the CJ-4 oil while the candidate FA-4 oil decisively increased the piston skirt wear. Although both coatings prevented scuffing failure observed for the uncoated steel skirt in a base oil without an additive package, they surprisingly caused a higher piston wear rate when tested in any of the fully formulated engine oil. The detrimental impact was attributed to the Mn-P film, either as a standalone coating, or a coating interlayer. The porous and brittle Mn-P film was broken during the wear test and the released hard Mn-P grains are suspected to cause third-body abrasion to accelerate the wear process. This work also evaluated the feasibility of developing an improved high temperature, low mass, cost-neutral turbocharger compressor wheel for heavy-duty engine applications from TiAl using additive manufacturing, utilizing its unique ability to fabricate high strength, low weight structures. This work has shown that the phase transforming nature of the TiAl alloys enable obtaining equiaxed microstructures in the as-built state without the need for tedious beam parameter manipulations. The HIPed structures have good RT tensile properties that will enable them to be surface machined to the required tolerance that can 2 then be heat treated to obtain the desired microstructures. Additionally, the negligible residual stresses stemming from the high build chamber temperatures ensure the parts are formed without cracks (one of the major issues in traditional manufacturing of these intermetallics).

33 ADVANCED PROPULSION SYSTEMS↗
DOE OSTI2019

Additive Manufacturing Fabrication of PEEK Counter-Current Centrifugal Contactor Components

Additive manufacturing (AM, also known as 3D printing) offers significant advantages for the fabrication of annular centrifugal contactor-separator (CCS) stages, particularly when complemented by post-processing via traditional machining. The shortcomings of 3D printing of CCSs are offset by its low cost, quick turnaround, and ability to manufacture enhanced mixing sections and multistage modules. High-density acrylic materials show promise for improved chemical resistance and mechanical properties. The demonstration of the MOEX process using acrylic AM CCS stages confirmed their full functionality and showed significant flexibility in geometry design while using relatively low-cost plastic materials. Over the past two years, AM has been used to produce low-cost centrifugal contactor components, ranging from bench-scale laboratory testing to a full-scale industrial process with on-hand availability of spare parts and great flexibility in design modifications and quick testing and implementation. However, the shortcomings of stereo lithography assembly (SLA)-printed acrylic components became apparent rather quickly. By the completion of the initial MOEX demonstration using the 9-stage 2-cm CCS bank, nearly half of the rotors had begun to fail from pitting and cracking. These problems were most likely caused by swelling of the rotor due to liquid absorption, resulting in improper excess run out, mechanical abrasion, and chemical exposure of the roughened surface. Additional deterioration of the acrylic stages was later discovered when the interiors of the acrylic housings began to experience flaking and delamination as the plastic dried out several weeks after the tests. All of these issues caused severe limitations to the lifespan of the CCS stages, which are acceptable for R&D but undesirable for commercial-scale production.

42 ENGINEERING↗
DOE OSTI2020

High Temperature Erosion In Particle Based CSP Systems

Particle based concentrated solar power plants are increasingly being considered as an alternative to molten salts. Although these particle based systems provide the inherent safety and enhanced lifetime from reduced corrosion compared to molten salt systems, they bring in complexities associated with surface erosion from falling particle impact and sliding motion along the surfaces. Past research on particle related erosion has been limited to high velocity applications and doesn’t necessarily coincide with the operating conditions in CSP systems. In our work, we evaluate characterize the rate of erosion for particles and containment materials at 800ºC. Three different types of erosion resulting from a) impact of solid particles on receiver, particle storage, and heat exchanger walls; b) abrasion erosion from particle sliding motion along walls; and c) attrition erosion as the particles breakdown from particle-to-particle contact and particle-to-wall interactions are evaluated and compared across a varied spectrum of particle and containment material spectrum. From the results, It is noted that temperature plays a key role in the rate of erosion experienced by any material. With the increase in temperature, materials become more ductile and are more readily sheared away from particle impinging or sliding motion. Furthermore, the particles themselves have higher susceptibility to breakdown which also lowers particle thermal absorptance and thus efficiency as heat transfer fluid.

14 SOLAR ENERGY↗
DOE OSTI2020

Report of the Condition of a General Electric Transportation Systems Gearbox

Wind power plant operations and maintenance (O&M) costs remain an appreciable contributor to the overall cost of wind energy. Premature of wind turbine gearboxes failures are often a result of abrasive wear, micropitting, scuffing, white-etch cracks, and macropitting issues. Micropitting is a fatigue phenomenon that occurs in Hertzian contacts in both gears and rolling-element bearings that operate in mixed or micro elastohydrodynamic lubrication regimes. Micropitting is influenced by and manifests itself in many different ways depending on operating conditions such as load, speed and operating temperature, and on factors such as gear geometry and accuracy, tooth flank roughness, percentage of tooth sliding, and lubricant composition. Despite much research by many investigators, micropitting remains complex, unpredictable, and difficult to control and remains a problem in wind turbine gearboxes. The purpose of this report is to document and describe the micropitting damage observed in a wind turbine gearbox, thereby facilitating further analysis and examination in future reports.

17 WIND ENERGY↗
DOE OSTI2020

High Temperature Erosion Modeling in Particle Based CSP Systems

1. Introduction. Wear and erosion damage of materials from solid particle and surface interactions is a major issue in various industries. Although more common in mining and oil and gas production, erosion is becoming a critical issue in renewable technologies as well such as particle based concentrated solar thermal power (CSP) systems. In particle based CSP systems, solid particles are used to absorb solar energy and as thermal storage. However, these particles may cause significant amount of wear to system components while through the system at high temperatures. This damage can be costly, and therefore, requires a greater understanding of solid particle erosion in CSP systems. Throughout the years, models and tools have been developed to predict and control erosion in industries such as oil and gas production. However, these erosion models and erosion prediction tools have been mainly developed based on erosion data for much higher velocities and lower temperatures, i.e. the operating conditions for which the existing models have been built are not pertinent to those expected in CSP system. It is known that erosion depends on many factors such as material properties, erodent particle properties, and particle impact speed and angle. However, the effect of temperature on erosion is not vastly investigated. In this work, a temperature-based correlation is introduced that will be used to modify the existing erosion models to predict erosion rates at velocities and temperatures relevant to Gen3 CSP systems. The existing models are first validated against erosion experiments run at low temperatures and low velocities. Subsequently, a temperature correction term is developed that can extend the existing models to high temperatures, based on the available experimental data showing the effect of temperature on impact erosion. 2. Erosion Models. Continuing sequence of impacts from solid particles on surfaces would result in loss of material due to mechanical interaction between solid surface and particles. Erosion equations have been developed to predict erosion under different conditions and erosion mechanism, including cutting and deformation erosion. These models are mainly either mechanistic, empirical, and semi-mechanistic models, when the latter combine the theory of the erosion mechanism and particle motion with the available experimental data. One of the first empirical correlation was introduced by American Petroleum Institute (API) Recommended Practice (RP) 14E [1]. This correlation was very conservative, and several improved empirical and semi-mechanistic equations were developed in the years following. More recently, the models introduced by Erosion/Corrosion Research Center (E/CRC) at the University of Tulsa and Arabnejad. et al. [2] are frequently used in the literature and industry, as they account for many parameters affecting erosion including particle impact speed and angle, material density and hardness, and particle size and shape. However, both these models were developed based on data at relatively high velocities and also do not take into account any mechanical changes in material associated with thermal cycling at high temperatures. 3. Erosion Prediction at High Temperatures. In this work, the accuracy of Arabnejad et al. model and E/CRC model is investigated to predict impact erosion at conditions relevant to Gen3 CSP systems. Two significant deviations expected in Gen3 systems compared to operating conditions used to build these models are particle impact velocities and system temperature. As a first step, the performance of these models was validated at low velocities and temperatures. Impact erosion experiments were conducted on SS316 coupons using HSP 40/70 ceramic particles. Assuming particle rate of 1 kg/s/m, 0.0254 m of particle curtain thickness, and particle velocity of 1.5 m/s in the system, an overall erosion of 0.59 mm/year was calculated. The experimental results were subsequently compared to those from computational simulations and erosion of 0.47 mm/year was obtained using the Arabnejad et al. model. The results indicated that the models work well at low velocities and low temperature conditions. To account for temperature effect, a mathematical correlation was developed using data published by DUCOM [3] for Inconel 600 eroded by alumina particles at high velocities. The correlation was applied to both Arabnejad et. al model and the E/CRC model. The prediction results from these modified models were within 20% of this experimental data. Predictions of of erosion by the modified E/CRC model at three different temperatures are made. Similar to the calculation at low temperature, a typical CSP system with 1 kg/s/m of particle flow rate per unit length of the particle curtain and a curtain thickness of 0.0254 m is assumed. The annual thickness loss calculations were run for different particle impact velocities, assuming a uniform particle impact area equal to the cross-sectional area of the curtain (particle-particle interactions and dispersion of particles are not considered in obtaining the results). It is observed that erosion increases exponentially as temperature increases. Furthermore, it is also noted that, erosion changes non-linearly with impact velocity. Currently, experiments are also being conducted to measure erosion of SS316 at 800 ºC with HSP 40/70 particles at low impact velocities. We expect to use the results from high temperature testing to further improve the temperature correlation function. Similar models are also being developed for abrasion erosion resulting from particle sliding along the surfaces as well as attrition from particle to particle and particle to surface interactions. References. [1] Institute, A. P. (1991). API Recommended Practice for Design and Installation of Offshore Production Platform Piping System, API RP 14E. [2] Arabnejad, H., Mansouri, A., Shirazi, S. A., and McLaury, B. S. (2015a). Development of mechanistic erosion equation for solid particles. Wear, 332–333, 1044–1050. http://doi.org/10.1016/j.wear.2015.01.031. [3] https://ducom.com/high-temperature-erosion-evaluating-sample-wear/

14 SOLAR ENERGY↗
DOE OSTI2020

Falling particle impact erosion testing for particle based CSP systems

CSP systems are currently being examined as an effective method for using solar energy to generate electricity. While much of this research has been conducted using molten salt as the heat transfer medium, in recent years, solid particles have been posited as a cheaper and more energy efficient heat transfer medium for use in CSP systems. Many researchers have looked into the effectiveness of solid particles as a heat transfer medium. However, a concern with the use of particles is that the falling particles will impact various components within the CSP system, such as the hopper, the heat exchanger, and the insulating material, resulting in surface erosion and damage. With repeated impacts from falling particles, material from the surfaces under impact is removed. The degree of erosion depends on whether the substrate is made of brittle or ductile material. Furthermore, factors such as particle shape, size, hardness, concentration, impact angle, particle velocity, and substrate hardness will contribute to the erosion process and determine how much and how quickly erosion will takes place in a system. Three types of erosion will be observed simultaneously: impact erosion from particle impact on receiver, particle storage, and heat exchanger walls, abrasion erosion from particle sliding motion along walls, and attrition erosion as the particles breakdown from particle-to-particle contact and particle-to-wall interactions. It is imperative to understand each of these erosions individually for a more comprehensive understanding and prediction of CSP system durability. In this work, we developed an experimental test setup capable of measuring impact erosion at conditions relevant to 1MW CSP plant. Subsequently, Impact erosion measurements were performed for three different candidate substrate materials at low particle velocities using HSP 40/70 ceramic particles.

14 SOLAR ENERGY↗