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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Atomic layer deposition of nanofilms on porous polymer substrates: Strategies for success

Atomic layer deposition (ALD) is a versatile technique for engineering the surfaces of porous polymers, imbuing the flexible, high-surface-area substrates with inorganic and hybrid material properties. Previously reported enhancements include fouling resistance, electrical conductance, thermal stability, photocatalytic activity, hydrophilicity, and oleophilicity. However, there are many poorly understood phenomena that introduce challenges in applying ALD to porous polymers. In this paper, we address five common challenges and ways to overcome them: (1) entrapped precursor, (2) embrittlement, (3) film fracture, (4) deformation, and (5) pore collapse. These challenges are often interrelated and can exacerbate one another. To investigate these phenomena, we applied various ALD chemistries to porous polymers including polyethersulfone, polysulfone, polyvinylidene fluoride, and polycarbonate track-etched membranes. Reaction-diffusion modeling revealed why certain precursors and processing conditions result in embrittling subsurface material growth, entrapment of unreacted precursors, and nongrowth. We quantify the limits of ALD processing temperatures that are dictated by thermal expansion mismatch and can lead to fractured ALD films. The results herein allow us to make recommendations to avoid, mitigate, or overcome the difficulties encountered when performing ALD and plasma-enhanced ALD on porous polymers. We intend this article to serve as a “lessons learned” guide informed by previous experience to provide a better understanding of the difficulties and limitations of ALD on porous polymers and knowledge-based guidelines for successful depositions. This knowledge can accelerate future research and help experimentalists navigate and troubleshoot as they expose porous polymers to reactive precursor vapors.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Changes in environmental and engineered conditions alter the plasma membrane lipidome of fractured shale bacteria

ABSTRACT Microorganisms that persist in fractured shale reservoirs cause several problems including secreting foul gases and forming biofilms. Current biocontrol measures often fail due to limited knowledge of their in situ activities. The plasma membrane protects the cell, mediates many of its critical functions, and responds to intracellular cues and ecological perturbations through physicochemical modifications. As such, it provides valuable insight into the physiological adaptation of microorganisms in disturbed environmental systems. Here, we (i) demonstrate how changes in salinity and hydraulic retention time (HRT) influence the plasma membrane intact polar lipid (IPL) chemistry of model bacterium, Halanaerobium congolense WG10, and mixed microbial consortia enriched from shale-produced fluids and (ii) elucidate adjustments in membrane IPL chemistry during biofilm growth relative to planktonic cells. We incubated H. congolense WG10 in chemostats under three salinities (7%, 13%, and 20% NaCl), operated under three HRTs (19.2, 24, and 48 h), and in drip flow biofilm reactors under the same salinity gradients. Also, mixed microbial consortia in produced fluids were enriched in triplicate chemostat vessels under three HRTs (19.2, 24, and 72 h) and biofilm reactors. Lipids were analyzed by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Our results show that phosphatidylglycerols, cardiolipins, and phosphatidylethanolamines were predominantly enriched in planktonic H. congolense WG10 cells grown at hypersalinity (20%) compared to optimum (13%). In addition, several zwitterionic phosphatidylcholines and phosphatidylethanolamines were higher in abundance during biofilm growth. These observations suggest that microbial adaptation and biofilm formation in fractured shale are enabled by strategic plasma membrane IPL chemistry adjustments. IMPORTANCE Microorganisms inadvertently introduced into the shale reservoir during fracturing face multiple stressors including brine-level salinities and starvation. However, some anaerobic halotolerant bacteria adapt and persist for long periods of time. They produce hydrogen sulfide, which sours the reservoir and corrodes engineering infrastructure. In addition, they form biofilms on rock matrices, which decrease shale permeability and clog fracture networks. These reduce well productivity and increase extraction costs. Under stress, microbes remodel their plasma membrane to optimize its roles in protection and mediating cellular processes such as signaling, transport, and energy metabolism. Hence, by observing changes in the membrane lipidome of model shale bacteria, Halanaerobium congolense WG10, and mixed consortia enriched from produced fluids under varying subsurface conditions and growth modes, we provide insight that advances our knowledge of the fractured shale biosystem. We also offer data-driven recommendations for improving biocontrol efficacy and the efficiency of energy recovery from unconventional formations.

03 NATURAL GAS↗
DOE OSTI2020

Recent Progress to Understand and Improve Zeolite Stability in the Aqueous Medium

The work reviewed here attempts to summarize the growing literature on zeolite stability in hot liquid water. This required to first establish the nature, structure and interactions of the active sites in Brønsted and Lewis acidic microporous materials in the presence of liquid water. This understanding was then transferred to zeolite stability and catalyst deactivation. While early results correctly established Si–O–Si hydrolysis as the dominant pathway compared to the Si–O–Al hydrolysis observed in steaming, it also focused extensively on the positive role of framework and extra-framework Al in stabilizing zeolites. However, stability was instead found to more directly correlate with the number of internal structural defects and intraporous water concentration. Stabilization protocols for Brønsted acidic zeolites are described in detail. In the case of Lewis acidic zeolites, their inherent hydrophobic behavior (Si/M >100) makes them more resistant towards water, however, issues such as reversible carbonaceous species formation as well as irreversible metal leaching and fouling remain. Finally, we summarize the most important factors in designing robust and efficient zeolite catalysts made to withstand hot liquid water.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Durability Optimization of CO 2 Electrolyzers for Syngas Evolution

Recently, there has been an increased interest in mitigating anthropogenic CO 2 emissions through the electrochemical conversion of CO 2 into fuels and fuel feedstocks, including hydrogen gas (H 2 ), carbon monoxide (CO), and mixtures of the two to yield syngas. Commercial applications of these systems require high catalytic selectivity for the desired products, while exhibiting operational lifetimes exceeding thousands of hours. Advancements in this field have produced systems that display high selectivity of the desired products at faradaic efficiencies exceeding 95%. Despite the advancements made in CO 2 electrolysis, system durability remains a standing challenge in the field. CO 2 electrolyzer lifetimes are often limited by carbonate fouling, catalyst degradation, detrimental flooding of electrode microporous layers and anion exchange membrane (AEM) failures. In this report, a 5 cm 2 membrane electrode assembly (MEA) device is used to investigate potential failure modes and to optimize AEM CO 2 electrolyzer operation. Key findings of this study include the importance of CO 2 flow rate, use of a thin PiperION PTFE-reinforced membrane, optimizing compression to enhance contact under 40 in-lb compression, and the effect of more compressible, commercial iridium oxide anodes on system durability.

Abouremeleh, Mohammed H. [Lawrence Berkeley Nation↗
DOE OSTI2024

Moving toward automated µFTIR spectra matching for microplastic identification: addressing false identifications and improving accuracy

Abstract Infrared spectroscopy is a widely used tool for studying microplastics and identifying microparticles. Researchers rely on spectral libraries to differentiate between synthetic and natural materials. Unfortunately, spectral library matching is not perfect, and best practices require researchers to use time consuming, manual peak matching to assess spectral matches. Moving toward automated matching requires increased confidence in the matching process. Using spectra matching software may increase the efficiency of particle identification, however some matching strategies may confuse natural materials such as cotton, silk, and plant matter with common classes of synthetics such as polyesters and polyamides. In this experiment, we prepared 22 pristine sample materials from natural and synthetic sources and measured micro-Fourier transform infrared (µFTIR) spectra in transmission mode for each sample using a Thermo Nicolet iN10 MX instrument. The collected spectra were then input into two spectral library matching systems (Omnic Picta and Open Specy), using a total of five identification routines. Next, we placed a subset of four pristine microplastic materials in a biologically active river system for two weeks to simulate environmental samples. These simulated environmental samples were processed using 10% hydrogen peroxide for 24 h to remove organic contamination and then identified using the strongest performing library. We found that libraries with fewer sample spectra produced lower correlation matches and that using derivative correction greatly reduced the number of inaccuracies in identifying materials as either natural or synthetic. We also found that environmental fouling reduced the correlation value of library matches when compared to pristine particles, however the effect was not consistent across the four materials tested. Overall, we found that the accuracy of automated library matching in the tested systems and processing routines varied from 64.1 to 98.0% for distinguishing between natural and synthetic materials, and that a high Hit Quality Index (HQI) did not always correlate with accuracy. These results are important for the microplastic field, demonstrating a need to rigorously test spectral libraries and processing routines with known materials to ensure identification accuracy.

Kozloski, Rachel↗
DOE OSTI2020

First Ever Polymer Flood Field Pilot To Enhance The Recovery Of Heavy Oils On Alaska’s North Slope - Pushing Ahead One Year Later

In June 2018 the team embarked on an ambitious project to address the slow development pace of Alaska’s 20+ billion barrels heavy oil resource via the first ever polymer flood pilot. Following the successful commencement of the pilot in August 2018, the field demonstration, supporting laboratory experiments and numerical simulation have steadily progressed. A significant amount of valuable data and lessons learned have been collected, and are reported in this paper. The ongoing pilot and the research activities is making headway toward the primary objective of validating the use of polymer flooding for extracting heavy oil in Alaska’s challenging environment. The pilot is conducted in two pre-existing pairs of horizontal injectors and producers in an isolated fault block of the Schrader Bluff heavy oil reservoir at the Milne Point Field. A customized polymer blending and pumping unit injects HPAM polymer at a concentration of 1,750 ppm to achieve a target viscosity of 45 cP. Supporting coreflood laboratory experiments have focused on quantification of polymer retention in the rock, and effect of injection water salinity, polymer, and their combinations on oil recovery. The injection and production response of the pilot flood pattern is utilized to develop a history matched reservoir simulation model for forecasting oil recovery beyond the pilot. Finally, specially designed laboratory experiments address anticipated operating concerns regarding post-polymer breakthrough such as oil-water separation efficiency and polymer induced fouling of heater tubes. Polymer has been injected continuously since startup except for two short equipment modification shutdowns, and more recently a prolonged disruption due to polymer hydration issues at the J-pad field site. Cumulatively, over 600,000 lbs. of polymer has been injected, corresponding to ~7%PV. The two producers show significant decrease in the water cut, gradually increasing oil rate, and no polymer breakthrough. Two main observations from the coreflood are a significant uncertainty in polymer retention values, and positive oil recovery response to low salinity water (2,600 mg/liter TDS). The heterogeneity in the flood pattern presents some challenges in obtaining a robust history matched simulation model. Experimental results on produced fluids treatment indicate the formation of a dense polymer deposit, at certain conditions, on heating tubes that can negatively impact the heat transfer efficiency. The scientific knowledge, including the lessons learned during unanticipated shutdowns, quality control, logistics and field data that is being acquired from this effort has referential value for other planned EOR projects. Finally, by all indications, the polymer field pilot is steadily progressing toward achieving the ultimate goal of unlocking the massive heavy oil resources on Alaska North Slope (ANS).

Dandekar, Abhijit↗
DOE OSTI2024

Rejection of malathion by nanofiltration and reverse osmosis membranes exposed to foulant and two clean-in-place procedures

This research tested the treatment efficacy of an Energy Savings Nanofiltration 1 Low Fouling (ESNA 1-LF) nanofiltration (NF) and an Energy Saving Polyamide 2 (ESPA2) reverse osmosis (RO) membrane for removing malathion from water. Both membranes are of composite polyamide construction. The study included measuring malathion rejection using both pristine membranes and membranes exposed to a simulated secondary wastewater effluent foulant before and after two types of clean-in-place procedures. Across all conditions studied, malathion rejection ranged from 84 to 95% for the ESNA1-LF NF membrane and 77 to 94% for the ESPA2 RO membrane. Contact angle measurements were also collected for each membrane exposure condition. While the contact angle measurements indicated changes to the hydrophobicity of the selective layer of the membranes, they did not correlate to changes in the performance of malathion rejection. As expected, it was observed that malathion rejection improved with the introduction of foulant. Also, the clean-in-place procedures helped restore flux while maintaining malathion rejection.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Predicting initial trans-membrane pressure across cycles in the ultrafiltration process using random forest

With growing freshwater scarcity, direct potable reuse (DPR) systems that reclaim wastewater for drinking are becoming increasingly important for sustainable water supply. Reliable operation requires minimizing downtime in ultrafiltration (UF) units, where membrane fouling leads to elevated trans-membrane pressure (TMP). This study develops data-driven regression models based on random forest (RF) and autoregressive (AR) approaches to forecast the initial TMP at the start of each UF filtration cycle in a pilot-scale DPR system. The RF model consistently outperforms baseline methods, including historical mean, last observation carried forward, and AR models, across multiple forecast horizons, achieving the lowest root mean square error. To evaluate how different classes of process variables contribute to TMP dynamics over time, we examine the feature importance of independent input variables across multiple forecast horizons. This analysis provides insight into the temporal relevance of operational and sensor-derived features, guiding control and monitoring strategies. Additionally, the impact of hyperparameter tuning on TMP prediction performance is assessed for both direct and recursive RF modelling approaches. The proposed RF framework establishes a robust foundation for predictive monitoring and real-time optimization of UF operations, supporting sustainable and reliable water reuse.

direct potable reuse↗
DOE OSTI2020

Slag Management of Carbon Feedstock Used in Gasification FY17 TCF between Eastman Chemical and NETL (Final Report)

NETL, in collaboration with Eastman Chemical Corp (Kingsport, TN), targeted the joint evaluation and refinement of a slag management program developed by NETL (NETL IP, patent applied for) to control gasifier slag properties formed from ash in individual or combinations of different coal-based carbon feedstock materials and specific slag modifiers used in gasification. Slag forms from mineral or organic-metallic impurities in the carbon feedstock that melt at the high temperatures of gasification, coalescing to form a liquid (slag) that must flow from the gasifier. Slag additives, also known as slag modifiers, are often added to the carbon feedstock to modify the ash chemistry and achieve desired slag flow properties at target temperatures used in gasification. If slag does not flow from a gasifier, its buildup within the gasification chamber will cause either gasifier shutdown to physically remove the slag (consuming time and damaging the protective refractory lining), or the gasification temperature must be increased to lower slag viscosity so it can flow from the gasifier, leading to greater refractory wear/corrosion, along with increased fouling and downstream component wear. Because of these issues, gasification is typically targeted at the lowest temperature possible where slag will flow in a controlled manner (a temperature range called T100 for the lowest temperature, with T250 being the highest temperature where the slag has achieved the desired fluidity). That temperature range also needs to yield a desired syngas composition, highlighting the importance of knowing and being able to control carbon feedstock slag viscosity and the temperature of thermal breakdown of the carbon feedstock. Slag viscosity varies with changes in the gasification chamber temperature, oxygen partial pressure, and slag chemistry. The slag model work with Eastman Chemical targeted predicting and controlling molten coal ash slag behavior at specific gasification conditions. The final goal of the refined model was to develop/refine the NETL slag model so a gasifier operator would be able to predict slag behavior prior to purchasing or using a carbon feedstock and control slag properties once a carbon feedstock is being gasified, allowing a gasifier user to determine what mineral additives or blends of different carbon materials would be needed to achieve desired slag properties at targeted gasification conditions. For a given carbon feedstock and desired gasification condition, the actual gasification cost and slag behavior would be able to be predicted using the slag management program in advance of purchasing or using the carbon feedstock – allowing accurate control of slag ash behavior in real time. As part of the TCF project work with Eastman Chemical, the viscosity of several ash compositions of interest to them would be measured and used to populate the slag model, along with a large database of historical slag temperature, chemistry, and viscosity information they possess – information that would in-crease the predictive accuracy of the slag management model with slag ash chemistry of interest to them. As part of the model evaluation and refinement, the predictive model and its database will be installed on computers at Eastman Chemical and used to manage slag properties in a gasifier during real-time operation of their gasifier. In summary, success of the slag management program at Eastman Chemical would support its use by other gasifier operators to manage slag chemistry and properties over other desired gasification temperature ranges, allowing greater process control and efficiency of their carbon feedstock conversion during gasification.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2020

NH 4 OH Looping with Membrane CO 2 Absorber and Distributed Stripper for Enhanced Algae Growth

The University of Kentucky Center for Applied Energy (UK CAER) has devised a unique, integrated CO2 capture and utilization technology. CO2 from coal-fired power generation flue gas is first captured at half the operating cost of a typical aqueous CO2 capture system (CCS), distributed in an aqueous stream and then fixed by algae in bioreactors where the algae production is increased by 50% over that with a typical intermittent nutrient feeding system. Lower CCS operating cost is achieved by eliminating the flue gas pretreatment step for cooling and SO2 removal, eliminating steam extraction from the power generation steam cycle for solvent regeneration, and eliminating CO2 compression. Higher algae production is achieved by continuous, just-in-time nutrient feed to the bioreactors directly from a distributed solvent regenerator, which maintains the bioreactor pH for optimum growth. The process starts with a uniquely configured membrane absorber, where the flue gas is indirectly contacted with an ammonium hydroxide (NH4OH) solvent. Dissolved NH3 is attractive for both CO2 capture and as an algae nutrient. For CO2 capture it is inexpensive, has a low regeneration energy, is thermally- and oxidatively-stable and has a viscosity near that of water, which makes is easy to transport. Numerous studies have shown that the scrubbing capacity of NH3 is approximately 0.9-1.2 kg of CO2/kg of NH3, with a CO2 removal efficiency of ~99% and half the solvent regeneration energy than that of 30 wt% MEA[1, 2, 3]. NH3 is attractive as an algae nutrient due to its low cost. The rich NH4OH solvent is pumped to a set of distributed regenerators which are co-located with the algae bioreactors. Solvent pumping, transport and distribution reduces the balance of plant (BOP) cost compared to a typical aqueous CCS related to the flue gas duct and boost fan required to transport the flue gas. The energy required for the distributed solvent regeneration is supplied by solar-thermal panels eliminating the need for steam extraction from the power generation steam cycle. After solvent regeneration, the product stream contains both the CO2 captured from the flue gas and volatized NH3 from the solvent. This product stream is fed directly to the bioreactors, eliminating the need for compression of the CO2 stream. The relative amounts of CO2 and NH3 in the product stream are adjusted and controlled by a controlling the regeneration conditions (pressure and temperature). The continuous feed of the right ratio of nutrients overcomes the typical inhibition of algae growth resulting from frequent pH swings in the bioreactor due to unbalanced (intermittent) feeding systems for CO2 and N. Also, because the regenerators will operate at pressure and be located in close proximity to the bioreactors, there is no worry about pressure drop when sparging the gas into the algae. Sparging produces small bubbles which is beneficial for mass transfer efficiency. One known challenge when using an NH4OH solvent is high NH3 emission. Hydrophobic membranes are used for CO2 capture using an aqueous NH3 solution[4, 5] without the direct contact between flue gas and aqueous solution. Additionally, UK CAER CO2 capture and utilization process manages NH3 slip in three extra measures. First, NH3 slip is minimized by working with minimal species partial pressure, which is proportional to the concentration in the liquid. Hence, lowering the capture solvent concentration will lower the NH3 partial pressure. Second, UK CAER’s previous work has demonstrated that the addition of Zn2+ into NH3 solutions to chelate the NH3 can reduce NH3 volatility. Third, the configuration of the membrane CO2 absorber utilizes condensed water from the flue gas to continually wash the gas-side of the membrane to reduce fouling and recapture NH3 slip. Additional details about the UK CAER unique, integrated CO2 capture and utilization technology will be presented along with technology development plans. Diao, N., Q. Li, and Z. Fang. 2004. Heat transfer in ground heat exchangers with groundwater advection. International Journal of Thermal Sciences. 43: 1203-1211, He, Q., M. Chen, L. Meng, K. Liu, and W. Pan. 2004. Study on Carbon Dioxide Removal from Flue Gas by Absorption of Aqueous Ammonia. Western Kentucky University. Yeh, A.C., and H. Bai. 1999. Comparison of ammonia and monoethanolamine solvents to reduce CO2 greenhouse gas emissions. The Science of the Total Environment. 228: 121-133, Villeneuve, K., D. Roizard, J.C. Remigy, M. Iacono, and S. Rode. 2018. CO2 capture by aqueous ammonia with hollow fiber membrane contactors: Gas phase reactions and performance stability. Separation and Purification Technology, 199: 189-197, Toro Molina, C., and C. Bouallou. 2016. Carbon dioxide absorption by ammonia intensified with membrane contactors. Clean Techn Environ Policy 18, 2133–2146 (2016)

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2020

White Paper to Justify the Use of Strip Effluent in the Defense Waste Processing Facility During Slurry Mix Evaporator Processing

At the request of Savannah River Remediation (SRR), a white paper was written to assess whether it would be acceptable to process Strip Effluent (SE) in both the Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator (SME) in the Defense Waste Processing Facility (DWPF) for the nitric-glycolic acid flowsheet. Savannah River National Laboratory (SRNL) experimental data and DWPF Sludge Batch 9 (SB9) process data was reviewed, looking at batches which included Precipitate Reactor Feed Tank (PRFT) and/or Strip Effluent Feed Tank (SEFT) feeds that led to long processing times. These batches were reviewed looking for processing problems such as melter feed trips, foamovers, heating rod or steam coil fouling, missed Reduction/Oxidation (REDOX) targets, and other process anomalies.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Optimal Header Design for Diffusion Bonded Heat Exchangers

Microchannel heat exchangers have seen increasing adoption in many high-pressure applications in recent decades but are subject to particulate fouling from the relatively small channel size compared to traditional designs. Typical cleaning methods require process shutdown, heat exchanger removal, cleaning, then reassembly. The objective of this project was to refine and transfer technology to enable header design improvements for Cleaning-in-Place (CIP), allowing for reduced/negligible process interruption for the cleaning process. The technology transfer was from Sandia National Laboratories (Sandia) to Vacuum Process Engineering, Inc. (VPE). This primary purpose of CIP was developed while considering channel flow uniformity and heat exchanger cost. The project phases were to 1) capture and define potential improvement options, 2) evaluate options with both simulation and experiments, and 3) transfer design knowledge to the industry partner. These efforts resulted in improved header designs from the first known focused effort in this area. The improved designs will help the entire microchannel heat exchanger field that has applications in supercritical CO 2 power cycles, hydrogen (fuel cell) vehicle fueling, liquified natural gas processing, and more.

42 ENGINEERING↗
DOE OSTI2021

Subtask 2.6 – Optimization of Aerosol Mitigation Technology for Postcombustion CO 2 Capture

Growing concerns over the impact of CO 2 emissions from combustion sources on global climate change have prompted numerous research and development projects aimed at developing cost-effective technologies for CO 2 capture. One family of technologies being demonstrated at pilot and full scale globally is postcombustion CO 2 capture (PCCC) systems that employ amine-based solvents. The captured CO 2 can be compressed and permanently stored underground or used for enhanced oil recovery (EOR). The proximity of North Dakota’s lignite-fired fleet of power plants to potential CO 2 storage options creates a unique atmosphere for PCCC within the state. However, the aerosols present in lignite flue gas present a challenge for large-scale PCCC at North Dakota power plants. Aerosols can negatively impact the long-term performance of amine-based solvents for CO 2 capture. Amine-based solvents are volatile, and aerosols provide nucleation sites where amine vapors can condense. Because aerosols cannot be easily captured at the column outlet using conventional technologies, the amine-laden aerosols escape the system and lead to accelerated solvent losses. Moreover, aerosol components can chemically react with amines to form degradation products that can permanently deactivate the amine, cause fouling, and lead to hazardous emissions. Many of the elements that have been shown to catalyze solvent degradation are present in lignite coals and can exacerbate solvent replacement economics. Understanding this issue is critical to the implementation of solvent-based CO 2 capture systems as applied to lignite-fired generation systems. The Energy & Environmental Research Center (EERC) designed and carried out this project to optimize aerosol mitigation technology for PCCC at a lignite-fired power plant. To meet the goal of this project, the following objectives were identified: Determine the effectiveness of a wet electrostatic precipitator (WESP) on collection of aerosols at a low-rank coal-fired power station. Determine the impact of aerosols on the efficiency and degradation products of amine-based carbon capture systems fired with low-rank fuels. Work was conducted at Minnkota Power Cooperative’s (MPC’s) Milton R. Young (MRY) Station Unit 2 using a slipstream of flue gas from the outlet of the plant’s flue gas desulfurization (FGD) unit. To gather initial data for sizing and specifying a WESP for this system, a temporary pilot-scale WESP was rented and installed on-site. Several different conditions were tested to examine the impact of flow rate, voltage, and current on WESP performance. The WESP was effective at removing large particulate (>200 nm) but caused an increase in fine particulate (<75 nm). Fine particulate material at the inlet and outlet of the WESP was collected, analyzed, and showed that crystalline sulfates carried over from the plant’s FGD unit were being converted to fine aerosols and SO 2 was being converted to SO 3 through the WESP. Additionally, the high moisture content of the flue gas stream at this sample location also contributed to an overall increase in aerosol mass under some of the test conditions. Using the results from the rented WESP, the project team installed a smaller-scale WESP upstream of the EERC’s slipstream CO 2 capture system. Flue gas was routed through a pilot-scale FGD unit to remove SO 2 to very low levels (~1 ppm) and then through a direct contact cooler (DCC) to further cool the gas and to remove moisture. The gas exiting the DCC was then routed through the new WESP before passing to the CO 2 absorber columns. Fluor’s amine-based solvent was used to scrub CO 2 from the slipstream through a set of two absorber columns. The rich solvent was regenerated in a stripper column by heating to drive off captured CO 2 . The system operated using a catch-and-release method where the CO 2 was separated to provide data on the process, but the captured CO 2 was released back into the host site stack. Aerosols and sulfur species were measured at multiple locations throughout the pilot-scale system. The inlet FGD and DCC removed much of the particulate matter and gaseous sulfur upstream of the WESP. With this configuration, the WESP achieved >95% particulate capture. The new WESP did not show any of the increases in SO 3 or other aerosol species that had been consistently observed with the larger-scale WESP installed immediately downstream of the plant’s full-scale FGD unit. Particulate samples captured and analyzed from the WESP inlet did not show any presence of crystalline sulfate materials, indicating that the pilot-scale FGD and DCC were efficient at reducing carryover from the plant’s full-scale FGD unit. A set of parametric tests were conducted on the new WESP to assess the impacts of flow rate, voltage, number of online WESP fields, and gas-phase sulfur content on aerosol and sulfur transformations. The results showed that the WESP performed similarly well at all sets of conditions. Sulfur and particulate matter exiting the WESP were further reduced through the absorber column as the amine-based solvent captured some of the residual contaminants. Solvent analysis showed that these species were slowly concentrating in the solvent over the duration of the test. When the WESP was taken offline and the sulfur slip through the FGD allowed to rise, the sulfate content in the solvent rose sharply, showing that the extra FGD and WESP were effective at reducing sulfate and cation uptake. This would be expected to extend amine-based solvent life by slowing the formation of heat-stable salts and other degradation products. This subtask was cofunded through the EERC–U.S. Department of Energy Joint Program on Research and Development for Fossil Energy-Related Resources Cooperative Agreement No. DE-FE0024233. Nonfederal funding was provided by the North Dakota Industrial Commission and MPC.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2021

Microwave Plasma Flash Pyrolysis for Coal-to-Product Applications

Since 2010, the US coal industry has experienced a precipitous decline, with coal production volumes dropping by as much as 35% according to EIA. This decline is hardly surprising given that 90% of domestic coal use is allocated to electricity production: While coal generation supplied about 45% of the nation's power in 2010, its share is projected to fall to only 22% in 2020. Fortunately, alternative uses for coal as a feedstock rather than as energy source are available. Coal tar is an established feedstock for chemicals and high-value carbon products including carbon fiber and battery-grade graphites. At present, growth of these uses is constrained by the low availability, purity, and yields of currently available coal liquids, and high energy- and CO2-intensity of current methods of production (i.e. coking). Previously reported work conducted in a partnership with Pacific Northwest National Laboratory demonstrated technical and economic viability of flash pyrolysis of coal in a microwave plasma environment at bench scales targeting production of fuel feedstocks (synthetic oil). H Quest’s work since then indicated promise of microwave-derived coal liquids to be uniquely suited for the lower-cost production of carbon materials, including synthetic graphite, carbon fiber, and composites. Low bulk process temperatures, subsecond residence times, and ambient pressure operation enable small-scale deployment, reduce capital and operating costs, and suppress formation of impurities, including QI material, typical in conventional coal tars. With no inherent production of CO2 or water consumption, microwave plasma flash pyrolysis presents a viable route to the sustainable production of both platform chemicals and carbon-based materials. Most recently, H Quest developed a novel, ruggedized microwave plasma reactor, which departs from the proof-of-concept approach and addresses the problems typically encountered in scaling laboratory microwave plasma apparata (e.g. eliminating fragile quartz enclosures prone to coking and fouling). This reactor has been integrated with a 15kW microwave power supply, a pulverized coal injection system, and a product recovery system. A series of screening tests across a range of coals (including hv-, lv-bituminous and subbituminous PRB), entrainment gas flows and compositions and microwave energy inputs are performed to evaluate conversion rates within the novel, scaled-up system, confirm yields of liquid products, and to perform compositional (GC/MS and elemental) analyses of the products. Results of these tests will be presented and discussed.

Skoptsov, George↗
DOE OSTI2021

Fiscal Year 2021 Filtration of Hanford Tank 241-AP-107 Supernatant Samples Obtained at Prototypic Tank Level and Filtered at 16 °C

Bench-scale filtration testing of 8.5 liters of supernatant from Hanford waste tank 241-AP-107, chilled to 16 °C, was conducted using a backpulse dead-end filter (BDEF) filtration system equipped with a feed vessel and a Mott inline filter Model 6610 (Media Grade 5) in the hot cells of the Radiochemical Processing Laboratory at Pacific Northwest National Laboratory. This was done to assess the impact of a lower sampling location within the tank as well the lowered filtration temperature on supernatant stability and fouling. The as-received samples were transferred to 1.5-liter poly bottles and held at 16 °C for approximately 1 week prior to filtration. The feed was filtered through the BDEF system at a targeted flux of 0.065 gpm/ft 2 to match the prototypic operation of the TSCR system. During the initial period of filtration, the differential pressure required to effect filtration at 0.065 gpm/ft 2 increased until it reached 2 psid [the Tank Side Cesium Removal (TSCR) action limit] at 26 hours. After this, the filter was backpulsed to dislodge accumulated solids and reduce this pressure differential. An additional eight backpulses were conducted during the initial filtration period; each time, the target pressure was reached sooner than during the previous interval. Volume filtered decreased from 0.9 to 0.03 m 3 /m 2 over the course of 14 processing hours. After the ninth backpulse, the backpulse frequency had become unsustainable, and it was decided to perform an extensive filter cleaning. The filter was cleaned by draining the chilled AP-107 feed into chilled holding containers, introducing 0.1 M NaOH into the feed vessel, and recirculating the NaOH through the system for 20 minutes before allowing the system to soak for 2 hours without temperature control. A measurable decrease in filter resistance during this recirculation indicated that the 0.1 M NaOH was likely dissolving some of the solids that had deposited on the filter. Post cleaning, the filter resistance was effectively restored to initial conditions as the initial transmembrane pressure was restored to original levels. However, resumed processing of the AP-107 feed at 16 °C continued to result in an increased rate of filter resistance. An additional five backpulses were conducted (four during feed processing, one during subsequent cleaning) before the conclusion of the test. Solids concentrated from the backpulse solutions displayed sodium oxalate-type phases, Al-oxides and sodium Al-oxides/carbonates, iron oxides, and Ca-bearing phases (calcite). The scanning electron microscopy analyses also revealed a large distribution of particles, with some particles, notably sodium phosphate dodecahydrate, having diameters close to 0.5 mm.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Enhancing Steam-Side Heat Transfer via Microdroplet Ejection using Inorganic Coatings

During condensation of water on a superhydrophobic nanostructured surfaces, droplets coalesce and jump (droplet ejection) due to the release of excess surface energy. Meticulously designed nanostructured surfaces or coatings capable of droplet ejection can enhance heat transfer performance by easy removal of droplets during condensation. In the present work, the capabilities of the Nelumbo droplet ejection coatings technology currently used in commercial heat exchangers are explored and optimized for materials and conditions relevant to steam condensers. Specifically, this includes (1) adapting and optimizing the procedures and chemistries to deposit droplet ejecting coatings on materials used in the steam condenser, (2) testing of the heat transfer, durability, and fouling of the fabricated coatings under a variety of steam condenser relevant conditions, and (3) modeling of the impact of droplet dynamics and interfacial properties on heat transfer in steam condensers. We experimentally demonstrated that at low supersaturation conditions (S~1.02), developed superhydrophobic nanostructured surface gives a 40% higher peak heat transfer flux and a 17% higher peak overall heat transfer coefficient (U) with droplet ejection mechanism compared to the dropwise condensation mechanism on the same nanostructured surface. Though the experimentally observed droplet ejection mechanism was short-lived (~3 min) due to the limitation of the chiller to maintain a constant supersaturation condition in fabricated steam condenser. And large variations in water inlet temperature (+ to - 2 degrees C) caused flooding of nanostructure (Wenzel state) at higher supersaturation (S > or = 1.12). This is an important finding because typical supersaturation levels in field operation are over 1.8 and as such, either the flooding potential for these materials should be improved or operation at lower supersaturation may be required to maximize heat transfer efficiency. If supersaturation conditions can be maintained reliably in the steam condenser in addition to droplet ejection mechanism during condensation, this could provide a potential 2% reduction in water flow rate which equates to a savings of over 3900 gallons of water per minute for a 500 MW steam turbine and over $0.3MM savings annually given a 0.02 cent marginal water withdrawal cost. It is also worth noting that these savings are based on improvement of droplet ejection coatings over coatings capable of performing consistent dropwise mechanism in in-field surface condensers. Savings due to the droplet ejections coatings when compared to bare substrates could be much higher. Additionally, the present work provides the importance of steam condenser operating conditions and insights into the challenges in modeling the condensing droplet dynamics on surfaces.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2022

Improving Coal-Fired Plant Performance Through Integrated Predictive and Condition-Based Monitoring Tools

The project demonstrated the ability to improve boiler performance and reliability through the integrated use of condition-based monitoring (CBM) and predictions of the impacts of coal quality on boiler operations at a full-scale coal-fired power plant. The advanced tool developed actively monitors and manages coal quality and overall boiler conditions that maximizes availability and maintains generating capacity while reducing cost. The tool is used to forecast and alert plant operators and engineers about poor boiler conditions which may occur as a result of incoming coal and/or current power plant operating conditions. The Combustion System Performance Indices (CSPI) and CoalTracker (CT) programs predicts fireside performance of the plant including slagging, fouling, erosion, slag flow, strength development (sintering/densification), and slag layer thickness based on the composition of delivered coal. CT program is tailored for each plant and is used to track the coal from the point of delivery to the burner. The most successful application of the CSPI-CT has been at plants where the coal composition is determined through the use of a full stream elemental analyzers based on prompt gamma neutron analysis (PGNAA). The CSPI-CT program information is used by coal procurement, coal mining and plant operations personnel to select and blend coal properties for the best plant performance.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2021

Numerical Investigation of Enhanced Dehumidification Processes By Using Dielectrophoresis Principles in Moist Airflows

Dispersed particle-laden flows are encountered in many building and industrial applications, such as flow in a fluidized bed, hydrocarbon transportation in pipelines, and the fouling of air-cooled heat exchangers (Kuruneru et al., 2016; Ray et al., 2019; Wang et al., 2019). Computational fluid dynamic (CFD) models have been developed in recent years to depict particle-fluid and particle-particle interactions in laminar or turbulent flows with increasing accuracy and stability. One particular particle-laden system of interest for moisture control is electrically-enhanced condensation in air and water droplet flows. Electrically-enhanced condensation consists of the use of highly charged water droplets injected in the moist air. The droplets become electric seeds that attract polar water vapor molecules to their surfaces and promote condensation. The nucleation and growth of the charged droplets deplete the vapor phase near a droplet, which is compensated for by the dielectrophoresis flow and diffusion. Dielectrophoresis flow involves surrounding vapor at a distance of about 10 to 100 nm for droplets charged by an electrospray compared to ~2 nm for a single electron charge in a droplet. As the vapor molecules collapse on the surface of the droplets, their initial electrical charge decreases with time due to the neutralization of the ions. While the physics of this phenomena is well known, engineering models for predicting the condensation rates are not available. This work computationally investigates dehumidification of moist airflow in a converging rectangular duct. The objective is to develop an engineering model that predicts water vapor condensation by employing dielectrophoresis principles. We construct a Computational Fluid Dynamics (CFD) model of the duct with electrically-enhanced condensation. The model is implemented in the open-source software OpenFOAM. We utilize the Multi-Phase Particle-In-Cell (MP-PIC) method coupled with a Population Balance Equation (PBE) approach to simulate the particle-laden system. This methodology is an Eulerian-Lagrangian approach used to simulate the droplets' behavior in the humid air. The MP-PIC approach (Andrews and O'Rourke, 1996) mitigates the computational cost by parceling several fundamental particles with similar properties (such as types, sizes, and temperature) into one computational particle. Thus, the billions of particles can be substituted by millions of computational particles without significant loss of information. The PBE was considered with the Lagrangian frame to combine the particle distribution function used in MP-PIC (Kim et al., 2020). This approach preserves mass and energy conservation between the phases in the Eulerian and Lagrangian structures. The PBE in this procedure was directly linked to the discrete parcels, making the simulation of the particle distribution computationally efficient and robust. The MP-PIC-PBE approach used in the present work was applied to the dehumidification of air. Water droplets were injected in the air stream and forced to grow according to experimentally derived correlation. The experiments were conducted on a converging duct with the same geometry and boundary conditions used to build the CFD model. This approach enabled us to approximate the effect of dielectrophoresis phenomena on the droplet and air interface. This presentation will discuss the details of the new CFD model built for the duct, the implementation of the model in OpenFOAM CFD programming language, and the experimental validation of the newly developed model. The results revealed a moderate yet measurable increase in droplet diameter due to water vapor condensation at the vapor-liquid interface of the electrically charged droplets' surface. The seed water droplet particles grew in size by capturing the water vapor in the surrounding air. The OpenFOAM model predicted reductions of humidity in the air from 5 to 10 percent.

Yel Mahi, Maliha↗