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At least 1,513 records · Page 84

Growth of Hexagonal Boron Nitride from Molten Nickel Solutions: A Reactive Molecular Dynamics Study

Metal flux methods are excellent for synthesizing high-quality hexagonal boron nitride (hBN) crystals, but the atomic mechanisms of hBN nucleation and growth in these systems are poorly understood and difficult to probe experimentally. Here, we harness classical reactive molecular dynamics (ReaxFF) to unravel the mechanisms of hBN synthesis from liquid nickel solvent over time scales up to 30 ns. These simulations mimic experimental conditions by including relatively large liquid nickel slabs containing dissolved boron and a molecular nitrogen gas phase. Overall, the reaction takes place almost exclusively on the surface of the liquid nickel, owing to the low solubility of nitrogen in bulk nickel and the intermediate species’ preference for the metal–gas interface. The formation of hBN invariably begins by reaction of dinitrogen with nickel-solvated boron atoms at the surface, forming intermediate N–N–B species, which typically evolve into B–N–B units through a short-lived intermediate where a single nitrogen atom is coordinated by one nitrogen and two boron atoms. The resulting B–N–B units, in turn, coalesce with growing hBN nuclei and carry nitrogen between hBN nanocrystals in an Ostwald ripening process. The amount of hBN produced on the tens of nanosecond time scale depends critically on the boron concentration, while having a much weaker dependence on the N 2 pressure for the regime considered (N 2 pressures of 2.5–10 MPa, Ni–B solutions with 6–12% boron by atom fraction). The highest rate of hBN formation occurs at the lowest temperature considered (1750 K, just above the melting point of nickel), while no hBN sheets are formed at 2000 K or above. An analysis of the transition pathways for nitrogen atoms shows that the final step, incorporation of small B–N motifs into larger hBN sheets, is the rate-limiting step in the regimes considered. While raising the temperature from 1750 to 2000 K has little effect on the formation of intermediates (N–N–B, B–N–B, etc.), the lack of large hBN sheets at temperatures >1900 K is explained by decreased probability of the final step and increased probability of breakup of hBN into B–N motifs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Leveraging Triphenylphosphine-Containing Polymers to Explore Design Principles for Protein-Mimetic Catalysts

Complex interactions between noncoordinating residues are significant yet commonly overlooked components of macromolecular catalyst function. While these interactions have been demonstrated to impact binding affinities and catalytic rates in metalloenzymes, the roles of similar structural elements in synthetic polymeric catalysts remain underexplored. Using a model Suzuki–Miyuara cross-coupling reaction, we performed a series of systematic studies to probe the interconnected effects of metal–ligand cross-links, electrostatic interactions, and local rigidity in polymer catalysts. To achieve this, a novel bifunctional triphenylphosphine acrylamide (BisTPPAm) monomer was synthesized and evaluated alongside an analogous monofunctional triphenylphosphine acrylamide (TPPAm). In model copolymer catalysts, increased initial reaction rates were observed for copolymers untethered by Pd complexation (BisTPPAm-containing) compared to Pd-cross-linked catalysts (TPPAm-containing). Further, incorporating local rigidity through secondary structure-like and electrostatic interactions revealed nonmonotonic relationships between composition and the reaction rate, demonstrating the potential for tunable behavior through secondary-sphere interactions. Lastly, through rigorous cheminformatics featurization strategies and statistical modeling, we quantitated relationships between chemical descriptors of the substrate and reaction conditions on catalytic performance. Collectively, these results provide insights into relationships among the composition, structure, and function of protein-mimetic catalytic copolymers.

Catalysts↗

Electrolyte and Cutoff Potential Effects on Cycle Life of Li4Ti5O12/LiNi0.9Mn0.1O2 Batteries for Behind-the-Meter Storage Applications

Behind-the-Meter Storage (BTMS) is a stationary battery energy storage system that is connected to the electrical distribution system on the customer's side of the utility's service meter. BTMS systems are used to store electrical energy from the grid as well as inconstant, renewable energy, such as local solar and wind generation. A successful BTMS system will allow the customer to pair their energy generation and storage to optimize electrical consumption from the grid, improving reliability and minimizing cost. For BTMS applications, batteries must be designed and optimized with different set of criteria from other leading segments of the Li-ion battery market, like transportation, due the system being stationary and proximal to the residential or commercial building it's benefitting. BTMS applications prioritize safety, cost (low/no-critical materials), reliability (20-year calendar life), and durability (10,000 cycle life), while having the ability to (minimally) compromise energy density and rate capability. Lithium titanate (Li4Ti5O12-, LTO) is a promising anode candidate for BTMS applications due to its high safety and capacity retention, while maintaining a reasonable 160 mAhg-1 reversable capacity and composition of relatively abundant materials. (1) Specifically, LTO has a high working voltage which helps to prevent Li dendrite formation, improving safety. Furthermore, LTO also has negligible lithiation-based volume change, leading to less mechanical pulverization, or loss of active material, upon cycling. For the cathode, materials with little or no Co are of high interest due to the high cost and low abundance of Co. LiMn2O4 (LMO) has been paired with LTO for BTMS applications in the past due to its safety, low cost (abundancy), and reasonably high operating voltage. (2-4) However, the low capacity of LMO limits energy density and specific energy. While not the highest priority for BTMS applications, increasing energy density will enable deployment in space constrained BTMS applications and decrease total cost. LiNi0.9Mn0.1O2 (LN-MO) is a recently developed material with promise due to its high operating voltage and relatively low price. (5) However, Ni-rich layered oxides, including LNMO, tend to struggle with capacity retention during high-voltage cycling due to mechanical pulverization, irreversible phase transitions, and unstable solid-electrolyte interphase. The study presented here focuses on building an understanding of how electrolyte solvent and varied cutoff potentials will impact the cycle life of LTO/LN-MO cells. Specifically, a comparison is provided between ethylene carbonate (EC), ethyl methyl carbonate (EMC), fluoroethylene carbonate (FEC), and Gen2 electrolyte solvents with 1M Lithium hexafluorophosphate (LiPF6) salt, cycling to two upper termination potentials, 2.6V and 2.7V. Electrochemical testing and diagnostics (e.g., differential capacity analysis, area specific impedance, constant voltage hold, and rate capability) and post-mortem characterization will be used to understand the aging behavior and failure mechanisms of the 8 cell combinations (four electrolytes and two voltage cutoffs). Cells with FEC electrolyte showed a lower initial capacity compared to cells with Gen2, EMC, and EC cycling at both voltages; however, the cells with FEC showed consistent trends in capacity retention with 2.6V and 2.7V termination potentials, while the cells with the other electrolytes showed much higher rates of capacity loss when cycling to the higher voltage. These results indicate that FEC may play a role in improving durability of high-voltage, Ni-rich electrode systems for use in high-cycle applications, such as BTMS.

electrolyte↗

Self-Propagating Frontal Polymerization in Water at Ambient Pressure

Advances in polymer chemistry have led to the development of monomers and initiation agents that enable propagating free-radical polymerization fronts to exist. These fronts are driven by the exothermicity of the polymerization reaction and the transport of heat from the polymerized product to the reactant monomer/solvent/initiator solution. The thermal energy transported to the reactant solution causes the initiator to decompose, yielding free radicals, which start the free radical polymerization process as discussed in recent reviews. The use of polymerization processes based on propagating fronts has numerous applications. Perhaps the most important of these is that it enables rapid curing of polymers without external heating since the polymerization process itself provides the high temperatures necessary to initiate and sustain polymerization. This process also enables more uniform curing of arbitrarily thick samples since it does not rely on heat transfer from an external source, which will necessarily cause the temperature history of the sample to vary with distance from the surface according to a diffusion-like process. Frontal polymerization also enables filling and sealing of structures having cavities of arbitrary shape without having to externally heat the structure. Water at atmospheric pressure is most convenient solvent to employ and the most important for practical applications (because of the cost and environmental issues associated with DMSO and other solvents). Nevertheless, to our knowledge, steady, self-propagating polymerization fronts have not been reported in water at atmospheric pressure. Currently, polymerization fronts require a high boiling point solvent (either water at high pressures or an alternative solvent such as dimethyl sulfoxide (DMSO) (boiling point 189 C at atmospheric pressure.) Early work on frontal polymerization, employed pressures up to 5000 atm in order to avoid boiling of the monomer/solvent/initiator solution. High boiling point solutions are needed because in order to produce a propagating front, a high front temperature is needed to produce sufficiently rapid decomposition of the free radical initiator and subsequent free radical polymerization and heat release at a rate faster than heat losses remove thermal energy from the system. (While the conduction heat loss rate increases linearly with temperature, the free radical initiator decomposition is a high activation energy process whose rate increases much more rapidly than linearly with temperature, thus as the temperature decreases, the ratio of heat loss to heat generation increases, eventually leading to extinction of the front if the temperature is too low.) In order to obtain atmospheric pressure frontal polymerization in water, it is necessary to identify a monomer/initiator combination that is water soluble and will not extinguish even when the peak temperature (T*) is less than 100 C. In this work acrylic acid (AA) was chosen as the monomer because is it one of the most reactive monomers and can polymerize readily at low temperatures even without initiators. Ammonium persulfate (AP) was chosen as the initiator because it decomposes readily at low temperatures, produces relatively few bubbles and is commercially available. The propagation rates and extinction conditions of the fronts are studied for a range of AA and AP concentrations. Small amounts of fumed silica powder (Cab-o-sil, Cabot Corporation) were added to the solutions to inhibit buoyancy induced convection in the solutions; future studies will investigate the effects of buoyant convection within the solutions.

Olten, Nesrin↗

Bench-scale Development of a Transformational Graphene Oxide-based Membrane Process for Post-combustion CO 2 Capture

Graphene-based materials, such as graphene and graphene oxide (GO), have been considered as next-generation membrane materials. GTI Energy and The State University of New York at Buffalo (UB) have been developing a transformational GO-based membrane process (designated as GO2) that integrates a high CO 2 /N 2 selectivity membrane (GO-1) and a high CO 2 flux membrane (GO-2) for post-combustion CO 2 capture. An innovative membrane structure, consisting of GO nanochannels intercalated by single-walled carbon nanotube (SWCNT), was developed. The membrane prepared on hollow fiber substrate showed CO 2 permeance as high as 1,300 GPU with CO 2 /N 2 selectivity >200. The membranes were successfully scaled up to effective area of 50-100 cm 2 . The 50-100 cm 2 membranes showed CO 2 /N 2 selectivity ≥200 and CO 2 permeance ≥1,000 GPU for the GO-1 type, and CO 2 /N 2 selectivity ≥20 and CO 2 permeance ≥2,500 GPU for the GO-2 type. The CO 2 capture performance of the GO-based membranes was tested using a simulated flue gas. The testing results indicate that the GO-based membranes are stable in the presence of flue gas contaminants. The GO-based membranes were then further scaled up to a surface area of 1,000 cm 2 . Good stability was achieved during an integrated testing with GO-1 and GO-2 membranes using simulated flue gas. A bench-scale system was designed, constructed, and tested at the National Carbon Capture Center (NCCC). Good stability was achieved during testing of a single-stage process with >10 shutdowns/startups at NCCC. During the integrated testing, the membranes showed good stability at 50°C and 57°C. 70-90% CO 2 removal efficiencies and ≥95% CO 2 purity were validated during the steady state operation at NCCC. Techno-economic analysis indicates the GO2 membrane-based process technology provides a reduction in both the levelized cost of electricity (LCOE) and cost of capture when compared to the reference B12B case presented in the Cost and Performance Baseline for Fossil Energy Plants Volume 1: Bituminous Coal and Natural Gas to Electricity study prepared by the National Energy Technology Laboratory (NETL), before considering any system optimization or improvement opportunities. The benefits are primarily driven by a reduction in the equipment costs of the CO 2 capture process vs. the solvent-based reference process in NETL Case B12B as well as a decrease in the base plant size.

20 FOSSIL-FUELED POWER PLANTS↗

Molecular Weight Dependence of Block Copolymer Micelle Fragmentation Kinetics

The effect of molecular weight (M) on the fragmentation kinetics of micelles formed by 1,2-polybutadiene-block-poly(ethylene oxide) (PB-PEO) copolymers was studied in the ionic liquid 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl)imide. A series of six samples, with total M ranging from 10 4 to 10 5 g mol –1 and nearly constant composition (f PEO ≈ 0.4), were examined; all six formed spherical micelles with PEO coronas. Nonequilibrium PB-PEO micelles were prepared by direct dissolution, a process that systematically produces nanoparticles with mean aggregation numbers more than twice the equilibrium values. When subjected to high temperature annealing (170 °C), the average micelle radius was found to decrease substantially, as determined by temperature-jump dynamic light scattering (T-jump DLS) and time-resolved small-angle X-ray scattering (TR-SAXS). Furthermore, the characteristic fragmentation times (τ) were found to increase strongly with increasing degree of polymerization N, as τ ~ N 1.8 . This result compares favorably with the prediction of a previously untested model.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

The Influence of Alkyl Spacers and Molecular Weight on the Charge Transport and Storage Properties of Oxy‐Bithiophene‐Based Conjugated Polymers

Conjugated polymers (CPs) with polar side chains can conduct electronic and ionic charges simultaneously, making them promising for bioelectronics, electrocatalysis and energy storage. Recent work showed that adding alkyl spacers between CP backbones and polar side chains improved electronic charge carrier mobility, reduced swelling and enhanced stability, without compromising ion transport. However, how alkyl spacers impact polymer backbone conformation and, subsequently, electronic properties remain unclear. In this work, we design two oxy-bithiophene-based CP series, each featuring progressively extended alkyl spacer lengths and two distinct molecular weight (MW) distributions. Using operando characterisations, we evaluate the (spectro)electrochemical and swelling properties of the polymer thin films, and their performance in organic field-effect transistors and organic electrochemical transistors. Surprisingly, alkyl spacers negatively impact the hole mobility of our polymers, with higher MW amplifying this effect. Using molecular dynamics simulations, we show that it is thermodynamically favourable for adjacent non-polar alkyl spacers to aggregate in polar electrolytes, leading to backbone twisting. Further spectroscopic measurements corroborate this prediction. Our findings demonstrate the active interactions between side chain structure, MW and electrolyte/solvent polarity in influencing polymer performance, underscoring the importance of considering solvation environment effects on polymer conformation when designing new mixed conducting CPs for electrochemical applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Cryogenic Carbon Capture™ Technoeconomic Analysis

The Cryogenic Carbon Capture™ (CCC) process significantly decreases cost and energy demands for CO 2 separation and pressurization to 150 bar compared to alternatives. The process is a post-combustion technology that cools CO 2 -laden flue gas to desublimation temperatures (-100 to -135 °C), separates solid CO 2 —that forms from the flue gas—from the light gases, uses the cold products to cool incoming gases in a recuperative heat exchanger, compresses the solid/liquid CO 2 to final pressures (100–200 bar), and delivers a compressed CO 2 stream separated from an atmospheric pressure light-gas stream. The overall energy and economic costs are about 30-50% lower than most competing processes that involve air separation units (ASUs), solvents, or similar technologies. In addition, the CCC process enjoys several ancillary benefits, including (a) it is a minimally invasive Bolton technology, (b) it provides highly efficient removal of most pollutants (Hg, SOx, NO 2 , HCl, etc.), and (c) possible energy storage capacity. This report outlines the process details and economic and energy comparisons relative to other well-documented alternatives. This paper presents the results of a detailed techno-economic comparison of CCC with amine-based systems. The comparison uses identical financial and economic assumptions similar process assumptions as the detailed analyses published by US DOE in the greenfield analysis. Specifically, the comparison assumes power plants that produce the same net output, one equipped with and a second without carbon capture. Separately, the paper compares similar analyses for retrofitting existing systems using typical plant characteristics in the US (initial capital costs have been paid, high plant utilization), though there are no DOE estimates available for direct comparison. Financial and technical assumptions for all comparisons are maintained as close to the DOE reference studies as possible. The results demonstrate about 30-50% lower costs and energy demands for capture from greenfield coal plants. Natural gas plants produce substantially lower CO 2 concentrations which makes the cost of capturing a ton of CO 2 at the same capture rate as the coal plant higher for all processes while the cost of CO 2 capture per unit of power generation is lower. However, CCC maintains about the same absolute energy and cost advantages for NG as for coal compared to amine systems. Finally, the costs of retrofitting a station are compared to those of building a new station with and without capture. The retrofit costs are comparable to (slightly lower than) new plant costs without capture. In all cases operating and capital cost comparisons show that the CCC process can be retrofitted to a variety of plants to cost effectively reduce CO 2 emissions. Further process integration into the upstream processes and unique process features like water recovery, and integrated energy storage bring the effective cost of carbon capture using the CCC process down further and increase its advantages over alternatives. This technoeconomic analysis shows that the CCC process has the potential to the be lowest cost carbon capture technology under development today.

20 FOSSIL-FUELED POWER PLANTS↗

Atomistic Insights into Lithium–Glyme Solvate Ionic Liquids: Effects of Chain Length and Anion Coordination

For this study, mixtures of lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) in diglyme (G2), triglyme (G3) and tetraglyme (G4) at solvate ionic liquid (SIL) concentrations were investigated using classical molecular dynamics (cMD) simulations with a physically motivated force-field specifically developed for modeling these systems. The structural and dynamical properties of the mixtures were computed and analyzed. Lithium solvation shells, radial distribution functions, and X-ray structure factors were studied across the different SIL systems. Translational diffusion and rotational relaxation times were also evaluated, exhibiting similar trends with increasing glyme chain length. The results are consistent with experimental data and in good agreement with previous computational studies on G3 and G4. These findings validate the accuracy of the force field in modeling glyme systems and its use for describing the [Li(G2) 4/3 ][TFSI] mixture. Additionally, the thermal and electrochemical stability of these electrolytes were systematically examined. The thermal stability appears to be governed by cooperative interactions among glyme molecules, while the electrochemical stability is primarily influenced by Li + -anion interactions, which vary significantly with glyme chain length. Overall, the study sheds light on the crucial role of the anion in these glyme-based SILs and offers valuable insights into Li + -glyme systems at SIL concentrations, highlighting their promise as potential Li-ion battery electrolytes.

anions↗

Competitive Adsorption of Lubricant Base Oil and Ionic Liquid Additives at Air/Liquid and Solid/Liquid Interfaces

Oil-soluble ionic liquids (ILs) have been proved as effective additives in lubricant oils through tribological experiments and post-test analytical analyses. Here, surface structures of lubricant base oil, oil-soluble ILs, and their mixtures at the air/liquid and solid/liquid interfaces have been studied using sum frequency generation (SFG) vibrational spectroscopy. At the air/base oil and air/IL interfaces, the alkyl chains of the studied compounds were shown to be conformationally disordered and their terminal methyl groups point outward at the liquid surface. The base oil dominates the air/(base oil + IL) interface due to its higher surface excess propensity and larger bulk concentration. At the solid (silica) surface, ILs adopt a structure with their charged headgroups in contact with the silica surface, while their alkyl chains are more conformationally ordered or packed compared to the air/IL interface. At the interface between silica and (base oil + IL) mixtures, ILs also preferentially adsorb to the silica surface with their layer structures somewhat different from those of ILs alone. These results showed that ILs can adsorb onto the solid surface even before tribological contacts are made. The insights obtained from this SFG study provide a better understanding of the role of ionic liquids in lubrication.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Using Separation-Enhanced Isotope Ratio Mass Spectrometry to Enable Increased Renewable Carbon Content in Transportation Fuels (CRADA 525)

Stable isotope ratio measurements of carbon atoms using isotope ratio mass spectrometry (IRMS) can be an effective tool for quantifying biogenic carbon in co-processed fuels, with results approaching the precision and accuracy of accelerator mass spectrometry (AMS). The lower cost of an IRMS may enable deployment to refineries, improving access and analysis turnaround times (≤2 hours), and, by extension, provide data that can allow process optimization to maximize renewable carbon in desired refinery products. This project explored the integration of chemical separation with IRMS analyses to enable highly detailed tracking of biogenic carbon into fuel product streams separated by boiling point range, chemical class, or specific compound. Forty-nine fuels and fuel components of fossil and biogenic origin, spanning gasoline and diesel boiling point ranges, were received from three refiners and were analyzed for their δ 13 C values via IRMS. Results spanned a 13 C range from ca. 10‰ to 44‰ and reflect materials derived from sustainable sources (e.g., C4 or C3 plants, animal-based pathways, syngas) or from fossil-derived fuels. Common ranges are approximately 18‰ to 9‰ and approximately 30‰ to 20‰ for C4 and C3 plants, respectively, and approximately 34‰ to 24‰ and approximately 70‰ to 33‰ for petroleum-derived fuels and methane, respectively. Fuel-like standards were developed and tested using direct-injection elemental analyzer (EA) IRMS for liquid fuels. This method was compared with the published methods, yielding statistically similar results. Four blend curve sets were produced ranging from 0% to 100% of a fuel containing biogenic carbon, focusing on 0% to 10% biogenic carbon. Linear fits were the most applicable for two of the four blend curve sets; however, two sets were found to exhibit slightly quadratic behavior, which was more pronounced in low biogenic blend samples, necessitating second-order fits. The origin of the slight quadratic behavior remains unclear; however, the discussion points to possible interpretations. CanmetENERGY thoroughly characterized a majority of the samples using one- and two-dimensional gas chromatography (GC and GC×GC, respectively) and other analyses. Selected samples were subjected to solid phase extraction (SPE) for saturate, olefin, aromatic, and polar (SOAP) analysis, and the resulting solvent-diluted fractions containing saturates and aromatics were returned to Pacific Northwest National Laboratory (PNNL), where the solvent was removed via evaporation or physical separation using GC techniques. Characterization and separations provided an understanding of saturate and aromatic content, as well as boiling point ranges for each sample and sample fraction. Samples resulting from SPE were examined using EA-IRMS and gas chromatography combustion IRMS (GC-C-IRMS) analyses. Both approaches suggest that the range in values between end-members can be increased by selecting the paraffinic or aromatic fraction of the end-member or by selecting among individual compounds resulting from GC separation of the paraffinic fractions. Considerable work remains to put these approaches into practice and statistically validate the benefit for using a fraction or individual compound over bulk analysis of a sample. However, initial results suggest that separations provide advantages for samples having blend ratios of less than 10% biogenic blendstocks. 13 C results showed statistically similar biofuel blend results to those obtained at PNNL, although additional work is needed to obtain better reproducibility. Select samples were sent to Los Alamos National Laboratory (LANL) for IRMS measurements and Beta Analytics for AMS measurements. This work suggests that IRMS and AMS yield closely comparable results and in some circumstances, IRMS could serve as a surrogate for AMS. While additional work is needed to better resolve statistical advantages for separations and better show the comparable nature of IRMS and AMS in both the biogenic carbon analysis of bulk chemical classes, initial results from this study suggest that these should be pursued in order to proliferate this approach for quantifying biogenic carbon in transportation fuels to the refinery level, thereby potentially enabling process optimization in co-processing scenarios.

09 BIOMASS FUELS↗

Uranyl Naphthylsalophen and Pyrasal Complexes: Oxo Ligands Acting as Hydrogen Bond Acceptors in the Solid State

Uranium is most stable when it is exposed to oxygen or water in its +6 oxidation state as the uranyl (UO 2 2+ ) ion. This ion is subsequently particularly stable and very resistant to functionalization due to the inverse trans effect. Uranyl oxo ligands are typically not considered good hydrogen bond acceptors due to their weak Lewis basicity; however, the ligands bound in the equatorial plane greatly affect the strength of the oxo ligands’ hydrogen bonding. Here, in this work, new naphthylsalophen and pyrasal complexes of uranium were synthesized and crystallized for characterization in the solid state. The bond lengths and angles of the uranyl ion and the ligand conformation are compared. In the solid state, one of the pyrasal complexes showed a hydrogen bond directly from a water molecule to the uranyl oxo ligand, which resulted in an asymmetric lengthening of the U–O yl bonds from 1.789 to 1.862 Å and 1.784 to 1.844 Å.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Fabrication and Modification of Nanoporous Silicon Particles

Silicon-based nanoporous particles as biodegradable drug carriers are advantageous in permeation, controlled release, and targeting. The use of biodegradable nanoporous silicon and silicon dioxide, with proper surface treatments, allows sustained drug release within the target site over a period of days, or even weeks, due to selective surface coating. A variety of surface treatment protocols are available for silicon-based particles to be stabilized, functionalized, or modified as required. Coated polyethylene glycol (PEG) chains showed the effective depression of both plasma protein adsorption and cell attachment to the modified surfaces, as well as the advantage of long circulating. Porous silicon particles are micromachined by lithography. Compared to the synthesis route of the nanomaterials, the advantages include: (1) the capability to make different shapes, not only spherical particles but also square, rectangular, or ellipse cross sections, etc.; (2) the capability for very precise dimension control; (3) the capacity for porosity and pore profile control; and (4) allowance of complex surface modification. The particle patterns as small as 60 nm can be fabricated using the state-of-the-art photolithography. The pores in silicon can be fabricated by exposing the silicon in an HF/ethanol solution and then subjecting the pores to an electrical current. The size and shape of the pores inside silicon can be adjusted by the doping of the silicon, electrical current application, the composition of the electrolyte solution, and etching time. The surface of the silicon particles can be modified by many means to provide targeted delivery and on-site permanence for extended release. Multiple active agents can be co-loaded into the particles. Because the surface modification of particles can be done on wafers before the mechanical release, asymmetrical surface modification is feasible. Starting from silicon wafers, a treatment, such as KOH dipping or reactive ion etching (RIE), may be applied to make the surface rough. This helps remove the nucleation layer. A protective layer is then deposited on the wafer. The protective layer, such as silicon nitride film or photoresist film, protects the wafer from electrochemical etching in an HF-based solution. A lithography technique is applied to pattern the particles onto the protective film. The undesired area of the protective film is removed, and the protective film on the back side of the wafer is also removed. Then the pattern is exposed to HF/surfactant solution, and a larger DC electrical current is applied to the wafers for a selected time. This step removes the nucleation layer. Then a DC current is applied to generate the nanopores. Next, a large electrical current is applied to generate a release layer. The particles are mechanically suspended in the solvent and collected by filtration or centrifuge.

Ferrari, Mauro↗

Demonstration of Scaled-Production of Rare Earth Oxides and Critical Materials from U. S. Coal-Based Sources (Final Report)

The project objective was to demonstrate scaled production of high purity rare earth oxides (REO), nominally exceeding 90% grade, from coal refuse sources using innovative technologies that reduce cost and improve environmental outcomes relative to traditional rare earth processing technologies. The project utilized a critical material pilot plant constructed and tested as part of a previous U.S. Department of Energy project. Target performance criteria was a 50% reduction in production cost based on previous optimum values, 150% increase in recovery and greater than 2% concentrates of rare earth oxides, cobalt and manganese. Concentrate production goals were to produce a rare earth mix oxide product at a rate of 200 grams per day having a minimum purity of 50% as well as products of cobalt and manganese having a minimum purity of 2%. A previous pilot plant investigation identified acid cost as the major contributor to an operating cost that made the recovery of rare earth and other critical metals from bituminous coal sources economically challenging. As such, acid cost reduction was a major target using bio-oxidation reactors to produce sulfuric acid from naturally occurring coal pyrite. Based on laboratory data, a bio-oxidation circuit was designed for the pilot plant to produce 7.5 l/min of acid using two 11-m3 (3000 gallon) reactors equipped with 40 hp aerators for air dispersion. The pilot-scale tests revealed that acid concentration equivalent to as high as 1.0 M sulfuric acid could be continuously produced. However, the bio-acid contained exceptionally high iron concentrations, which complicated downstream processing of the pregnant leach solution (PLS). A TEA of the bio-oxidation circuit showed that production cost was approximately $0.13 per kg acid equivalent if produced using a four-day retention time in the reactors. This value represents a 48% reduction from that of purchased bulk sulfuric acid. Calcination (or roasting) studies were conducted on coarse refuse from West Kentucky No. 13 and Fire Clay coal seam sources. The test results revealed the potential to increase recovery by nearly 100% using temperatures between 500°C to 700°C with light REE recovery value being the most improved. Acid baking of the calcined products using sulfuric acid at 250°C increased heavy rare earth recovery from around 40% to 80% while decreasing the acid requirements by over 50%. The existing pilot plant was upgraded for the pilot scale demonstration of REE and CM recovery. The primary feedstocks were West Kentucky No.13 and heap leach pregnant leach solution (PLS) while a secondary feedstock was a lignite waste material from a construction sand operation. The pilot scale operation started with PLS generation through leaching followed by iron and aluminum removal, nominally at 3.3 and 4.5 pH, respectively. Leaching lixiviants used for the test were industrial grade sulfuric acid or bio-acid generated at the pilot scale facility. For most of the tests, the solid feed rate was 200 lb/hr whereas lixiviant was added at 2 gpm to provide an optimal residence time of 45 minutes. Following the contaminant removal step, several different process schematics were tested with the goal of maximizing REE recovery and purity. In the first test, direct processing of aluminum precipitation raffinate for REE recovery using oxalic acid at pH 1.5 was investigated. Overall REE recovery was approximately 45%. Unfortunately, elevated calcium content in the PLS significantly impacted the RE-Oxide product grade. Similarly, high calcium content decreased both the product purity and grades of CM products. As such, a new flowsheet was tested with the same initial process schematic but different precipitation stages for REEs and CMs at pH 6.0 and 9.0, respectively. It was noted that the overlapping precipitation behavior of Co, Ni and Zn with REEs limited the applicability of this process schematic. While this change increased the RE-Oxide grade from 36% in the first test to 87%, the loss of critical metals to the REE cake and bypass of the REEs to the CM cake significantly impacted the recovery of both REEs and CMs. Therefore, the modified process flowsheet combined oxalic acid precipitation stage raffinate and redissolved CM cake filtrate to maximize both the recovery and purity of the products. Consequently, a RE-Oxide product with 85% purity and CM cakes with over 19% Co, 38% Ni, 14% Zn and 9% Mn content were generated with significantly higher recoveries. While the modified process flowsheet improved recoveries and grades, elemental losses observed in separate precipitation and redissolution losses inspired the adaptation of a single precipitation stage at pH 9.0 for both REEs and CMs. This change was anticipated to maximize the REE recovery while minimizing the costs associated with separated redissolution and processing stages. As expected, REE recovery in this new circuit arrangement was over 56% with a product grade of over 87% RE-Oxide content. Similarly, Co, Ni, Mn, and Zn recoveries of 54%, 40%, 67%, and 66%, respectively, were achieved. Unfortunately, the elevated calcium content present in the solution due to its precipitation at pH 9.0 caused a decrease in the CM cake quality. Therefore, the final process flowsheet involved the addition of calcium oxalate precipitation following the oxalic acid precipitation stage, which effectively eliminated calcium contamination of the CM products. Finally, the pilot scale experiments conducted using bio-acid achieved comparable REE leaching recoveries to the conventional sulfuric acid leaching. Elevated iron concentration in the solution caused the co-precipitation of REEs with the iron and aluminum cake, resulting in the REE losses. Furthermore, elevated iron content bypassing the iron and aluminum precipitation stages contaminated the metal sulfide and manganese cake, respectively. A techno-economic analysis was performed based on a commercial facility capable of treating 500 tph of coal-based material. The production cost for West Kentucky No. 13 coarse refuse material ranged from approximately $500-$700/kg of total rare earth oxide whereas the lignite source had significantly lower production cost of $100-$300/kg. The significant difference in cost was due to the easier leaching characteristics of the lignite material and the higher feed concentrations. All process scenarios resulted in a negative net present value (NPV). For the lignite feedstock, laboratory REE leach recovery values were about 30% higher than the pilot plant data. Using the lab leach results, a positive net present value was achieved and the production cost decreased from $100-$300 $/kg to less than $150/kg of total REO.

01 COAL, LIGNITE, AND PEAT↗

Tuning the Mechanical Properties of Crosslinked Copolymers via Sequence and Solvent‐Selective Swelling for Vat Photopolymerization

Block copolymers (BCPs) offer distinct advantages for vat photopolymerization by enabling mechanically programmable network structures through microphase-separated morphologies that can be kinetically trapped during curing, yielding properties unattainable in homogeneous resins. However, the respective roles of repeat-unit sequence and solvent environment, together with their interplay in directing network formation and mechanical performance, remain unclear. Here, we synthesize a series of CO 2 -based polycarbonate copolymers comprising a crosslinkable glassy poly(vinyl cyclohexene carbonate) (PVCHC, A block) and a non-crosslinkable soft poly(propylene carbonate) (PPC, B block). The polymer sequence is systematically varied (ABA, BAB, and statistical), and solvent choice controls block-selective swelling to jointly control gelation behavior, microphase morphology, and mechanical response through changes in the accessibility and local environment of photocrosslinkable vinyl groups during network formation, as revealed by photorheology and small angle x-ray scattering. By tuning polymer sequence and curing solvent, we transform nominally identical formulations from brittle to highly ductile materials, achieving a three-orders-of-magnitude range in toughness (0.003 to 9.1 MJ m −3 ). These results establish clear structure–processing–property relationships and identify polymer sequence and selective solvation as powerful strategies for programming both printability and performance of block copolymer resins for additive manufacturing.

additive manufacturing↗

Carbamoylation as an Effective Tool in the Analysis of the Soman Nerve Agent Marker Pinacolyl Alcohol in Soil Matrices by EI-GC-MS and LC-HRMS

Pinacolyl alcohol (PA) is a Schedule 2 chemical commonly featured in most proficiency tests (PTs) administered by the Organisation for the Prohibition of Chemical Weapons (OPCW) due to its direct as well as forensic link to the nerve agent Soman. Therefore, its detection by Chemical Weapons Convention (CWC) inspection teams during on-site investigations is a strong indicator of the past or latent presence of Soman in the environment. Its small molecular weight (102), early elution time, and poor ionization profile make PA a challenging analyte to detect particularly at low concentrations (∼1–10 μg/g). In this work, 1,1′-carbonyldimidazole (CDI) has been used to effectively modify PA for the first time in two different soil matrices (Virginia type A soil and silt sediment) at two separate concentrations (1 and 10 μg/g) for its subsequent detection by EI-GC-MS and LC-HRMS methods. For the EI-GC-MS analysis, the PA carbamate derivative (PIC) exhibits improved chromatography relative to PA such as improved peak shape, increased molecular weight (196 for PIC and 102 for PA) and increased retention time (16.9 min for PIC and ∼4.1 min for PA). In addition, the derivatization also improves the detection of PA by LC-HRMS as the PIC product possesses protonation sites (i.e., imidazole ring) relative to none exhibited by PA. More importantly, the carbamoylation proceeds under mild conditions (55 °C, no base) and rapidly (3 h), characteristics that make it an appealing protocol for the analysis of PA during OPCW PTs or real case scenarios particularly in instances where it is present at low concentrations. It is anticipated that the protocol can be applied to the forensic analysis of this important Soman marker in various environmental matrices.

Chemistry↗

Charge Transport in Solvated Donor–Acceptor Functionalized Peptoids: Molecular Dynamics and Rate Theory

Scalable solar-energy conversion requires photoactive materials that combine the efficiency of natural photosynthetic systems with the stability and processability needed for practical applications. Achieving reliable charge transport in soft, self-assembled organic materials remains challenging, as structural fluctuations and environmental effects strongly influence charge-transfer (CT) rates. Here, we present a broadly applicable computational framework for evaluating CT rates in the condensed phase, combining Fermi’s golden rule rate theory with inputs from all-atom molecular dynamics (MD) simulations and first-principles electronic-structure calculations. The approach does not rely on system-specific parametrization and is applicable to a wide range of soft and disordered materials. We demonstrate the applicability and usefulness of the framework on redox-active peptoids functionalized with iron–porphyrin (Fe–P) complexes, a bioinspired platform with programmable donor–acceptor units and tunable three-dimensional organization. The calculated CT rates exhibit strong sensitivity to molecular conformation, with variations spanning several orders of magnitude. This dependence is shown to arise from the pronounced variation in diabatic electronic coupling with the relative orientations and separations of the Fe–P complexes across the conformational ensemble. The framework provides a consistent route for connecting atomistic structure to CT kinetics in the condensed phase and enables analysis of structure–rate relations in organic semiconducting systems.

Charge transfer↗

A Fundamental Economic Assessment of Recovering Rare Earth Elements and Critical Minerals from Acid Mine Drainage Using a Network Sourcing Strategy

In recent years, acid mine drainage (AMD) has emerged as a promising unconventional source of rare earth elements (REEs) and other critical minerals (CMs) such as cobalt and manganese. In this regard, AMD provides a natural heap leaching effect that extracts and concentrates REE/CM from the host strata creating a partially enriched feedstock suitable for downstream extraction, separation, and recovery. While several prior studies have described processes and approaches for the valorization of AMD, very few have described the supply chain and infrastructure requirements as well as the associated economic assessment. To that end, this paper provides a fundamental economic assessment of REE/CM recovery from AMD using a network sourcing strategy in addition to a robust, flexible feedstock separations and refining facility. The methodology of this paper follows that of a typical techno-economic analysis with capital and operating costs estimated using AACE Class IV (FEL-2) guidelines. To demonstrate the range of possible outcomes, four pricing scenarios were modeled including contemporary prices (September, 2021) as well as the minimum and maximum prices over the last decade. In addition, five production scenarios were considered reflecting variations in the product suite, ranging from full elemental separation to magnet REE and CM production only (i.e., Pr, Nd, Tb, Dy, Y, Sc, Co, and Mn). The results of this analysis show that, with the exception of the minimum price scenario, all operational configurations have positive economic indicators with rates of return varying from 25% to 32% for the contemporary price scenario. The optimal configuration was determined to be production of Co, Mn, and all REEs except for mischmetal, which is not recovered. Sensitivity analysis and Monte Carlo simulation show that capital cost and HCl consumption are the two major factors influencing rate of return, thus indicating opportunities for future technology development and cost optimization. Implications of the study and a cooperative profit-sharing model for sourcing are also described.

42 ENGINEERING↗