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Stable abnormal N-heterocyclic carbenes and their applications

Although N-heterocyclic carbenes (NHCs) have been known as ligands for organometallic complexes since the 1960s, these carbenes did not attract considerable attention until Arduengo et al. reported the isolation of a metal-free imidazol-2-ylidene in 1991. In 2001 Crabtree et al. reported a few complexes featuring an NHC isomer, namely an imidazol-5-ylidene, also termed abnormal NHC (aNHCs). In 2009, it was shown that providing to protect the C-2 position of an imidazolium salt, the deprotonation occurred at the C-5 position, affording imidazol-5-ylidenes that could be isolated. Over the last ten years, stable aNHCs have been used for designing a range of catalysts employing Pd(II), Cu(I), Ni(II), Fe(0), Zn(II), Ag(I), and Au(I/III) metal based precursors. These catalysts were utilized for different organic transformations such as the Suzuki–Miyaura cross-coupling reaction, C–H bond activation, dehydrogenative coupling, Huisgen 1,3-dipolar cycloaddition (click reaction), hydroheteroarylation, hydrosilylation reaction and migratory insertion of carbenes. Main-group metal complexes were also synthesized, including K(I), Al(III), Zn(II), Sn(II), Ge(II), and Si(II/IV). Among them, K(I), Al(III), and Zn(II) complexes were used for the polymerization of caprolactone and rac-lactide at room temperature. In addition, based on the superior nucleophilicity of aNHCs, relative to that of their nNHCs isomers, they were used for small molecules activation, such as carbon dioxide (CO 2 ), nitrous oxide (N 2 O), tetrahydrofuran (THF), tetrahydrothiophene and 9-borabicyclo[3.3.1]nonane (9BBN). aNHCs have also been shown to be efficient metal-free catalysts for ring opening polymerization of different cyclic esters at room temperature; they are among the most active metal-free catalysts for ε-caprolactone polymerization. Recently, aNHCs successfully accomplished the metal-free catalytic formylation of amides using CO 2 and the catalytic reduction of carbon dioxide, including atmospheric CO 2 , into methanol, under ambient conditions. Although other transition metal complexes featuring aNHCs as ligand have been prepared and used in catalysis, this review article summarize the results obtained with the isolated aNHCs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

A mathematical analysis of carbon fixing materials that grow, reinforce, and self-heal from atmospheric carbon dioxide

Carbon fixing materials are a new class of self-healing, self-reinforcing materials we have introduced that utilize ambient CO 2 to chemically add to an ever extending carbon backbone. This class of materials can utilize biological or non-biological photocatalysts and support a wide range of potential backbone chemistries. However, there is no analysis to date that describes their fundamental limits in terms of chemical kinetics and mass transfer. In this computational study, we employ a reaction engineering, and materials science analysis to answer basic questions about the maximum growth rate, photocatalytic requirements and limits of applicable materials. Our proposed mathematical framework envelops three main functions required for carbon fixing materials: (1) adsorption of CO 2 from air, (2) photocatalytic reduction of CO 2 into selected monomers, and (3) polymerization of CO 2 -derived monomers. First, by performing a Damköhler number analysis, we derive criteria for the cross over from kinetic control to mass transfer limited growth, setting upper limits on performance of a potential photocatalyst. Next, we analyze photocatalytic reduction of CO 2 to single carbon products, using known catalytic pathways and kinetic data. We identify formaldehyde as a C1 intermediate having unique potential for incorporation into the material backbone of carbon fixing materials. As an example, we find that a diamond-shaped reaction network graph for CO 2 reduction, passing through CO and HCOOH intermediates, accurately describes kinetic data for cobalt-promoted TiO 2 nanoparticles at room temperature and 1 atm CO 2 . Finally, as an applied case study, we consider and analyze the example of a carbon fixing poly(oxymethylene) system with embedded catalyst promoting the photocatalytic reduction of CO 2 to formaldehyde. The latter then trimerizes to a trioxane monomer which subsequently polymerizes to polyoxymethylene. This reaction engineering analysis introduces benchmarks for carbon fixing materials with respect to achievable rates of photocatalysis, adsorption, and polymerization. These results should prove valuable for the design, evaluation, and benchmarking of this emergent and new class of environmentally sustainable materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Quantum effects on the dynamics and properties of soft materials

The quantum effects of nuclear and electronic motion play an important role in the structure, dynamics, and function of soft materials, yet they are difficult to capture with conventional classical simulations or static electronic–structure methods. In this work several complementary approaches for treating quantum effects in polymeric and soft–matter systems are demonstrated, with a focus being on the hydrogen-bonded networks, ion and charge transport, and photoactive chromophores. The proton transfer, tunneling, and isotope effects are captured within the reduced-dimensionality models by implementing grid-based nuclear quantum dynamics in terms of the discrete variable and Fourier bases. The nuclear quantum dynamics is extended to larger systems by employing the quantum trajectories and quantum–thermal bath schemes combined with on-the-fly electronic structure, enabling the description of high-dimensional polymeric environments at feasible cost. The dynamics in the electronic degrees of freedom, simulating the optical response in large chromophores such as chlorophylls, is performed using the real-time time-dependent density functional theory implemented in the real-space multigrid (RMG) code. These approaches are demonstrated on case studies of the proton and hydroxide transport in hydrated polymer membranes, charge transfer in conjugated polymers, and the optical spectra of chlorophyll chromophores relevant to polymerized chlorophyll materials and chlorophyll–polymer hybrids. The reviewed methods and applications highlight practical routes of including quantum effects in simulations of soft functional materials.

Garashchuk, Sophya [Univ. of South Carolina, Colum↗

A validation of the fibre orientation and fibre length attrition prediction for long fibre-reinforced thermoplastics

To improve the mechanical performance of polymeric parts, fibre reinforcement has established in industrial applications during the last decades. Next to the widely used Short Fibre-reinforced Thermoplastics (SFT) the use of Long Fibre-reinforced Thermoplastics (LFT) is increasingly growing. Especially for non-polar polymeric matrices like polypropylene (PP), longer fibres can significantly improve the mechanical performance. As with every kind of discontinuous fibre reinforcement the fibre orientations (FO) show a high impact on the mechanical properties. On the contrary to SFT where the local fibre length distribution (FLD) can be often neglected, for LFT the FLD show a high impact on the material’s properties and has to be taken into account in equal measure to the FOD. Recently numerical models are available in commercial filling simulation software and allow predicting both the local FOD and FLD in LFT parts. The aim of this paper is to compare i.) the FOD results and ii) the FLD results from available orientation- and fibre length attrition-models to those obtained from experimental data. The investigations are conducted by the use of different injection moulded specimens made from long glass fibre reinforced PP. In order to determine the FOD, selected part sections are examined by means of Computed Tomographic (CT) analyses. The fully three dimensional measurement of the FOD is then performed by digital image processing using grey scale correlation. The FLD results are also obtained by using digital image processing after a thermal pyrolytic separation of the polymeric matrix from the fibres. Further the FOD and the FLD are predicted by using a reduced strain closure (RSC) as well as an anisotropic rotary diffusion - reduced strain closure model (ARD-RSC) and Phelps-Tucker fibre length attrition model implemented in the commercial filling software Moldflow, Autodesk Inc., San Rafael, CA, USA.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Fabrication of large area flexible nanoplasmonic templates with flow coating

Here, we describe the development of a custom-built two-axis flow coater for the deposition of polymeric nanosphere monolayers used in the fabrication of large area nanoplasmonic films. The technique described here has the capability of depositing large areas (up to 7” x 10”) of self-assembled monolayers of polymeric nanospheres onto polyethylene terephthalate (PET) films. Here, three sets of film consisting of different diameter (ranging from 100 to 300 nm) polymeric nanospheres were used to demonstrate the capabilities of this instrument. To improve the surface wettability of the PET substrates during wet-deposition we enhanced the wettability by using a forced air blown-arc plasma treatment system. Both the local microstructure, as confirmed by scanning electron microscopy, describing monolayer and multilayer coverage, and the overall macroscopic uniformity of the resultant nanostructured film were optimized by controlling the relative stage to blade speed and nanosphere concentration. As this is a scalable technique, large area films such as the ones described here, have a variety of crucial emerging applications in areas such as energy, catalysis, and chemical sensing.

36 MATERIALS SCIENCE↗

Intermediate time sub-diffusion and stress relaxation in ring polymer melts

The slow dynamics of non-concatenated ring melts remains a frontier problem in polymer science with implications for many soft material environments including cellular biophysics. Here, in this work, we report large-scale simulations of model ring melts that analyze the monomer and center-of-mass (CM) mean square displacements (MSD) and stress relaxation function on intermediate time and length scales. The degree of dynamical slowing down is characterized by the maximally sub-diffusive fractional time scaling exponents. The data span an exceptionally wide range of ring degrees of polymerization and stiffnesses and are not successfully organized based on the classic measure linear chain entanglement, N/N e . Rather, we find that the crossover degree of polymerization, N D , based on ring macromolecular caging that successfully allows master curves to be constructed for the long-time CM self-diffusion constant also collapses these temporal dynamic scaling exponents. Different properties display different exponents and exhibit one or two regimes of linear variation with the logarithm of N D / N . A distinct crossover of the CM-MSD and stress relaxation exponents emerges at sufficiently large N or stiffness that is not found for the monomer MSD, indicating a novel form of dynamic decoupling. This crossover aligns with the predicted critical degree of polymerization for transitioning from a weak to strong caging regime, indicative of activated transport. The latter may reflect the emergence of an intermolecular collective contribution to stress in analogy with dense soft colloidal matter. Suggestions are made for future theoretical work to address the rich patterns of behavior discovered.

Anomalous diffusion↗

TOG–Tubulin Binding Specificity Promotes Microtubule Dynamics and Mitotic Spindle Formation

XMAP215, CLASP, and Crescerin use arrayed tubulin-binding tumor overexpressed gene (TOG) domains to modulate microtubule dynamics. We hypothesized that TOGs have distinct architectures and tubulin-binding properties that underlie each family’s ability to promote microtubule polymerization or pause. As a model, we investigated the pentameric TOG array of a Drosophila melanogaster XMAP215 member, Msps. We found that Msps TOGs have distinct architectures that bind either free or polymerized tubulin, and that a polarized array drives microtubule polymerization. An engineered TOG1-2-5 array fully supported Msps-dependent microtubule polymerase activity. Requisite for this activity was a TOG5-specific N-terminal HEAT repeat that engaged microtubule lattice-incorporated tubulin. TOG5–microtubule binding maintained mitotic spindle formation as deleting or mutating TOG5 compromised spindle architecture and increased the mitotic index. Mad2 knockdown released the spindle assembly checkpoint triggered when TOG5–microtubule binding was compromised, indicating that TOG5 is essential for spindle function. Our results reveal a TOG5-specific role in mitotic fidelity and support our hypothesis that architecturally distinct TOGs arranged in a sequence-specific order underlie TOG array microtubule regulator activity.

Byrnes, Amy E. (ORCID:0000000249254680)↗

Soft X‐ray Spectromicroscopic Investigation of Synthetic C‐S‐H and C 3 S Hydration Products

Calcium silicate hydrates (C‐S‐H), the primary binding phase in concrete, is the most prominent physiochemical factor controlling the mechanical and chemical properties in the production of concrete. This paper reports the local‐binding structure and morphological details of C‐S‐H as determined by high‐resolution X‐ray spectromicroscopy. Hydrated tricalcium silicate (C 3 S) was used to determine the properties and role of the outer products (Op) of C 3 S. C‐S‐H with different molar ratios of Ca/Si, were synthesized (Syn‐ CSH ) to quantitatively evaluate the effect of silicate polymerization on Ca L and Si K edge of C‐S‐H. Near edge X‐ray absorption fine structure ( NEXAFS ) spectroscopy of Syn‐ CSH showed no variation in peak positions and energy separation for CaL III, II edge for the Ca/Si ratios investigated. Compared to Syn‐ CSH , C 3 S, when hydrated for 17 d, had a similar local structure around Ca. Si K edge NEXAFS analysis on Syn‐ CSH showed a tendency for the peak positions of both the Si K edge and the peak induced by multiple scattering to shift to higher energy levels. The results also indicated that the distance between the two peaks increased with a decrease of the Ca/Si ratio in Syn‐ CSH . Silicate polymerization influenced the multiple scattering of distant shell atoms more than the binding energy of the core atoms. Op of C 3 S had a uniform and higher degree of silicate polymerization compared to the core area. The results imply that Op reduces the hydration process of C 3 S into the core area thereby playing a key role on the properties of concrete upon formation.

Bae, Sungchul↗

Experimental Investigation on the Performance Loss of Cross-Linked Polymers During Photo-Oxidative Aging

Abstract Polymeric substances have seen an unprecedented integration in countless applications and fields of life, subjecting them to a broad range of environmental conditions, which can cause a form of damage to the structural and mechanical properties of these components known as aging. In this study we investigate the effects of the degradation of polymeric materials due to the extended exposure to sunlight, which can be simulated through controlled photo-oxidative aging using ultraviolet (UV) radiation as the main catalyst of this phenomenon. The effects on mechanical behavior and chemical properties of four polymeric materials with different mechanical characteristics was accordingly monitored throughout the study. The materials range in hardness with the polyurethane adhesive being the hardest and acting plastically, followed by an acrylic which exhibits greater hardening with time, a polyurethane sealant, which behaves in an elastomeric manner, and a silicon sealant, which is the softest of the set. Samples were prepared and subjected to UV radiation at three different temperatures namely 45, 60 and 80°C, for different aging periods ranging from 1 day for higher temperatures to 150 days for lower ones. The samples were then subjected to the Fourier transform Infrared spectroscopy (FTIR) test to monitor the change in the chemical composition of the materials along the aging durations and conditions. The materials were then subjected to mechanical testing along two modes of mechanical loading, which are a simple tension until failure and a double-cyclic test with progressively increasing strain limits after every two successful cycles until the sample reaches failure. The samples are loaded at constant strain rates throughout both tests. These tests revealed the change of behavior of our materials along the aging periods and conditions. The changes in mechanical behavior vary across each individual material depending on the aging temperature and period, with the changes ranging from hardening to softening, embrittlement or an increase in the maximum strain the material can endure before failure. A general trend would be that most materials become harder after photo-oxidation, however due to the range of temperatures in the aging conditions, thermo-oxidation, which causes softening in some of the polymers, has an increasingly notable effect at higher temperatures. A visible correlation can be noted between the change in mechanical behavior and a change in absorbance of Infrared Radiation (IR) in the FTIR spectrum, as the greater the crosslinking throughout the polymer matrix, the lower the absorbance of IR radiation due to the increased stiffness of the overall macro-molecular structure.

Korayem, Abd-Elrahman↗

WE-AB-BRA-03: Non-Invasive Controlled Release from Implantable Hydrogel Scaffolds Using Ultrasound

Purpose: To control release of a model payload in acoustically responsive scaffolds (ARSs) using focused ultrasound (FUS). Methods: Fluorescently-labeled dextran (10 kDa) was encapsulated in sonosensitive perfluorocarbon (C{sub 6}F{sub 14} or C{sub 5}F{sub 12}) double emulsions (mean diameter: 2.9±0.1 µm). For in vitro release studies, 0.5 mL ARSs (10 mg/mL fibrin, 1% (v/v) emulsion) were polymerized in 24 well plates and covered with 0.5 mL medium. Starting one day after polymerization, ARSs were exposed to FUS (2.5 MHz, Pr = 8 MPa, 13 cycles, 100 Hz PRF) for 2 min daily. The amount of dextran released into the media was quantified. For in vivo studies, 0.25 mL ARSs were prepared as described previously and injected subcutaneously in the lower back of BALB/c mice. After polymerization, a subset of the implanted ARSs were exposed to FUS (as previously described). Animals were imaged longitudinally using a fluorescence imaging system to quantify the amount of dextran released from the ARSs. Results: In vitro: Over 6 days, +FUS displayed an 8.2-fold increase in dextran release compared to −FUS (−FUS: 2.7±0.6%; +FUS: 22.2±3.0%) for C{sub 6}F{sub 14} ARSs, and a 6.7-fold increase (−FUS: 5.0±0.8%; +FUS: 38.5±1.6%) for C{sub 5}F{sub 12}:C{sub 6}F{sub 14} ARSs. In vivo: +FUS displayed statistically greater dextran release compared to −FUS one day after implantation for C{sub 5}F{sub 12}:C{sub 6}F{sub 14} ARSs (−FUS: 55.1±1.5%; +FUS: 74.1±2.2%) and three days after implantation for C{sub 6}F{sub 14} ARSs (−FUS: 1.4±6.5%; +FUS: 30.4±5.4%). Conclusion: FUS enables non-invasive control of payload release from an ARS, which could benefit growth factor delivery for tissue regeneration. ARS are versatile due to their tunability (i.e. stiffness, emulsion composition, FUS pressure, FUS frequency, etc.) and can be modified to for optimal payload release. Future work will optimize ARS formulations for in vivo use to minimize payload release in the absence of FUS. This work was supported by NIH Grant R21 AR065010 (M.L. Fabiilli) and the Basic Radiologic Sciences Innovative Research Award (M.L. Fabiilli). A. Moncion is supported by the National Science Foundation Graduate Student Research Fellowship (Grant DGE 1256260).

60 APPLIED LIFE SCIENCES↗

The combined effect of temperature and seawater on the compression properties of carbon fiber vinyl ester composites for sandwich structures

For naval applications, composite sandwich structures are of significant interest, and are often manufactured using thin (2 to 4 mm) composite facings made from carbon or glass fiber reinforcement, attached to a thick (25 to 50 mm) section of PVC cellular foam or balsa wood-based core materials using a suitable polymeric resin. In the present study, we focus on the hygrothermal effect on the fiber-dominated compression properties of carbon fiber reinforced vinyl ester resin based polymeric composite (CF/VE), used as “skin” for a polymeric composite sandwich material. Hygrothermal conditioning is achieved by saturating samples in simulated seawater at 40°C. Compression properties are evaluated for coupons extracted along warp and fill undergoing- no conditioning, conditioning till saturation (up to 6 months), and long-term conditioning (2 years). Sea-water saturation yields in up to 12% drop in compression strength with a further 3–4% drop resulting from long-term conditioning. No statistically significant modulus degradation is noticed due to short or long-term hygrothermal exposure. The failure mechanism of the warp extracted coupon, which fails in a splitting failure mode originating due to the delamination between the 0/90 interface, or the fill extracted coupon, which fails due to the instability caused by tow micro-buckling, remains unchanged due to combined exposure (short or long-term) of seawater and temperature. The loss in strength is attributed to the degradation of the fiber-matrix interface, which is validated via conducting single fiber push-in tests with a nominal diameter of 7 micron for conditioned and unconditioned coupons.

Engineering↗

SISGR - Hydrogen Caged in Carbon-Exploration of Novel Carbon-Hydrogen Interactions

Hydrogen trapped in a carbon cage, captured through repulsive interactions, is a novel concept in hydrogen storage. Trapping hydrogen via repulsive interactions borrows an idea from macroscale hydrogen storage (i.e. compressed gas storage tanks) and reapplies these concepts on the nanoscale in specially designed molecular containers. Under extreme conditions of pressure, hydrogen solubility in carbon materials is expected to increase and carbon is expected to restructure to minimize volume via a mixed sp2/sp3 hydrogenated state. Thermodynamics dictate that pre-formed C-H structures will rearrange with increased pressure, yet the final carbon-hydrogen interactions may be dependent upon the mechanism by which hydrogen is introduced. Gas “trapping” is meant to denote gas present in a solid in a high density, adsorbed-like state, when the external pressure is much less than that necessary to provide a comparable fluid density. Trapping thus denotes a kinetically metastable state rather than thermodynamic equilibrium. This project probed mechanochemical means to polymerize select hydrocarbons in the presence of gases, in an attempt to form localized carbon cages that trap gases via repulsive interactions. Aromatic, polyaromatic, and hydroaromatic molecules expected to undergo cyclo-addition reactions were polymerized at high (~GPa) pressures to form extended hydrogenated amorphous carbon networks. Notably, aromatics with a pre-existing internal free volume (such as Triptycene) appeared to retain an internal porosity upon application of pressure. However, a high photoluminescence background after polymerization precluded in situ identification of trapped gases. No spectroscopic evidence was found after depressurization that would be indicative of pockets of trapped gases in a localized high-pressure environment. Control studies suggested this measurement may be insensitive to gases at low pressure. Similarly, no spectral fingerprint was found for gas-imbued spherical carbon nanoshells, even after chemical “capping” of the gas-imbued nanoshells to limit gas diffusivity. Subsequently, spectral probes of gas vibrational modes adsorbed in various carbon nanostructures (including activated carbons, single-wall carbon nanotubes, polymers of intrinsic microporosity (PIMs), and UV-irradiated PIMs with decreased pore size) were found only at high pressure. The vibrational mode of the adsorbed film became perturbed in high density films, and the perturbation was sensitive to surface functional groups, pore size, and pore dimension. Experimental results were corroborated with first-principle modeling using density functional theory. Development of semi-empirical correlations that relate the spectral features to pore dimension, geometry, and chemical potential of the adsorbed film are on-going.

08 HYDROGEN↗

Exploratory Project: Rigid nanostructured organic polymer monolith for in situ collection and analysis of plant metabolites from soil matrices

Plant metabolites released from litter leachates and root exudates enable plants to adapt and survive in a wide range of habitats by facilitating resource foraging and plant-organismal interactions, and could influence soil carbon storage. The biological functions of these plant inputs and the organismal interactions they facilitate in soil are strictly governed by their composition and molecular identity. Our current understanding about the molecular identity of exudates is based on physiological studies that are done in soil-less axenic cultures. On the other hand, ecological studies that rely on isotope labeling to track the fluxes of carbon from plants to soil have found the complexities of soil-microbe matrices as an insurmountable barrier to undertake any meaningful molecular level characterization of plant inputs. Although it is constantly advocated to undertake a molecular level identification of the dynamicity of plant metabolites in soils, the complexity of soil system has thus far prevented any such endeavors. We developed polymeric probes through in-situ polymerization of poly(styrene-co-vinylbenzyl chloride-co-divinylbenzene) to elucidate the chemical environment of the soil to which the plant roots are exposed. Hypercrosslinking of the polymeric probes through an in-situ Friedel-Crafts alkylation significantly increased the surface area and the sorption capacity of the probes. Surface functionalization of the probes using a hybrid approach was also attempted. The efficacy of these probes was tested using batch equilibration. Scanning electron microscopy revealed extensive modification of the surface of the probes through hypercrosslinking. The probes exhibited a lower site specific sorption (slope of Freundlich adsorption isotherm close to unity) and percent recovery of the sorbed compounds from the probes were >70, indicating a predominance of reversible sorption. Further we imparted specificity to this copolymer matrix by using molecular-template imprinting approach for the selective capture of less abundant plant metabolites from a crowded soil/litter leachate. Our results suggests that i) the root exudate pattern of plants is highly dependent on the nutrient status of the plant, with greater specificity of root exudation occurring in growing medium with low available form of nutrients, ii) the chemical composition of root exudation is a function of the distance of sampling from the source-roots, with the composition of root exudation being more enriched in polar metabolites farther from the source-roots, iii) Further we demonstrated that the compounds present in real root exudates diffuse farther from the source roots than those in artificial root exudates that are traditionally used. Thus, our project highlights how the soil matrix is instrumental in modifying the chemical composition of root exudates, and highlights that, apart from the plant physiology, the specificity and function of root exudates is also modified by environmental factors.

54 ENVIRONMENTAL SCIENCES↗

Final Report for Project titled High Thermal Conductivity Polymer Composites for Low-Cost Heat Exchangers

Heat exchangers (HXs) are critical components in a wide range of heat transfer applications, from HVAC (Heating Ventilation and Cooling) to automobiles to manufacturing plants. They require materials capable of transferring heat at high rates while also minimizing thermal expansion over the usage temperature range. Conventionally, metals are used for applications where effective and efficient heat exchange is required, since many metals exhibit thermal conductivity over 100 W/m K. While metal HXs are constantly being improved, they still have some inherent drawbacks due to their metal construction, in particular corrosion. Polymeric material can offer solution to such durability issues and allow designs that cannot be afforded by metal construction either due to complexity or cost. A major drawback of polymeric material is their low thermal conductivity (0.1-0.5? W/mK) that would lead to large system size. Recent improvements in the area of filled polymers have highlighted the possibility to greatly improve the thermal conductivity of polymeric materials while retaining their inherent manufacturing advantage, and have been applied to heat sink applications. Therefore, the objective of this project was to develop a robust review of materials for the manufacturing of industrial and commercial non-metallic heat exchangers. This review consisted of material identification, literature evaluation, as well as empirical and model characterization, resulting in a database of relevant material properties and characteristics to provide guidance for future heat exchanger development.

36 MATERIALS SCIENCE↗

Final Research Performance Report - Small Molecular Associative Carbon Dioxide (CO 2 ) Thickeners for Improved Mobility Control

The initial objective of this project was to promote the application of a CO 2 thickener for improved mobility control during CO 2 EOR based on solubility tests, viscosity tests, and core floods. Ultimately, it was demonstrated that the CO 2 -soluble polymeric thickeners are much better suited for use a CO 2 -soluble conformance control agents for diverting the flow of CO 2 away from thief zones. Our team generated several effective small molecule CO 2 thickeners with ARPA-e funding. Unfortunately, none of these small molecule thickeners could dissolve in CO 2 without the addition of unacceptably large amounts of hexane or toluene as a co-solvent Therefore none were viable candidates for the core flooding studies associated with NETL award. Therefore during the entire core flood testing program associated with this NETL award, our team used only the most promising polymeric CO 2 thickener, a polyfluoroacrylate (PFA). In order to produce an environmentally benign polymer, the monomer used to make the new polymers used in this study was a fluoroacrylate that contains only six fluorinated carbons. We verified CO 2 solubility with a phase behavior cell. The thickening potential of all polymer samples was substantiated with a falling ball viscometer and a falling cylinder viscometer at Pitt. Two different viscometers were used to determine the increase in CO 2 viscosity that could be achieved via the dissolution of PFA. Praxair, which has an interest in thickening CO 2 for pilot EOR projects and for waterless hydraulic fracturing, agreed to measure the viscosity of CO 2 -PFA solutions at no cost to the project. Falling cylinder viscometery was conducted at Pitt in our windowed high pressure phase behavior cell. Both apparatuses indicated that at very low shear rates the CO 2 viscosity increased by a factor of roughly 3.5 when 1wt% PFA was dissolved in the CO 2 2. Our team also planned thickener concentrations and compositions at Pitt for the core tests that were conducted at Special Core Analysis Laboratories, Inc., (SCAL) in Midland, TX, where the ability for PFA to reduce CO 2 mobility in a core was then tested. During the beginning of these tests, the PFA polymer was then shown to impart reasonable improvements in mobility control during the SCAL core tests; as the CO 2 -PFA solution displaced CO 2 from the core at a constant volumetric flow rate, the pressure drop increased as expected. However, as the test progressed, there was clear and surprising evidence of dramatic reductions in core permeability due to PFA adsorption, especially for sandstones. For example, as the CO 2 -PFA solution displaced pure CO 2 from sandstone and limestone cores, the pressure drop increased by factors of multiple hundreds to over a thousand. It was subsequently demonstrated that the PFA injected into the core either (a) adsorbed strongly and irreversibly onto the rock surfaces, (b) deposited/precipitated within the rock, thereby blocking pores in a manner that could be dislodged by large changes in flow rate or flow direction, or (c) remained in solution and passed completely through the core. The loss of PFA to the porous media and the unacceptably large increases in pressure drop both indicated that PFA was inappropriate for CO 2 EOR mobility control, where thickener adsorption must be minimized and mobility reductions of only 10-100-fold are typically required. However, we realized that because the CO 2 -PFA solution could greatly reduce the permeability of porous media, it could serve as a near wellbore conformance control agent for blocking “thief zones”, where adsorption is acceptable and dramatic increases in pressure drop are desirable. These effects were more dramatic for sandstone than for limestone. Therefore, these PFA fluoroacrylate polymers can serve as a CO 2 -soluble conformance control agent for CO 2 -EOR, especially in sandstone formations. This injection of a single phase solution of CO 2 -PFA for permeability reduction is (to the best of our knowledge) the first report of a CO 2 -soluble conformance control additive. We also demonstrated that the optimal strategy for using CO 2 -PFA solutions for conformance control is analogous to the application of water-based polymeric gels; the CO 2 -PFA solution should first be injected only in an isolated thief zone to induce dramatic reductions in permeability only in that thief zone, and then CO 2 should be injected into all of the zones. Finally, it was noted that given the propensity of PFA to adsorb onto sandstone, the adsorption of PFA from CO 2 -PFA solutions onto cement surfaces promote the sealing of extremely fine cracks in casing cement.

02 PETROLEUM↗

Survey Study of Trunk Materials for Direct ATRP Grafting

In previous study, we demonstrated a new method to prepare polymeric fiber adsorbents via a chemical-grafting method, namely atom-transfer radical polymerization (ATRP), and identified parameters affecting their uranium adsorption capacity. However, ATRP chemical grafting in the previous study still utilized conventional radiation-induced graft polymerization (RIGP) to introduce initiation sites on fibers. Therefore, the objective of the present study is to perform survey study of trunk fiber materials for direct ATRP chemical grafting method without RIGP for the preparation of fiber adsorbents for uranium recovery from seawater.

36 MATERIALS SCIENCE↗

PDRD Project 19039 - All metal vacuum scroll pump development for tritium

Currently the United States relies on a single source, foreign company, Eumeca (formerly Normetex) for the supply of an all metal vacuum scroll pump to process tritium. This “one of a kind”, all metal, vacuum scroll pump utilizes no “wetted”, polymeric materials that degrade prematurely when exposed to tritium. U.S. based vacuum scroll pump suppliers typically utilize a polymer, Teflon®, as a tip seal material at the edge of the scroll impellers for proper pump function. Teflon® is known to degrade within a relatively short time frame (approximately 1 year) when continually exposed to tritium gas. This degradation results in “flaking” of the Teflon® material which results in particulate contamination of the process gas stream. While filtration of the particulate is possible, doing so requires additional maintenance which is costly in a glovebox environment. In addition, filtration can degrade pumping system performance as particulate collects in the filter media over time. To date, all of the well established U.S and European based vacuum scroll pump manufacturers have been uninterested in developing an all metal vacuum scroll pump that does not use a polymeric scroll tip seal. This position is taken as the vacuum scroll pump manufacturers do not see a large enough market to make it profitable for them to develop and market an all metal vacuum scroll pump. In the mid 2000s, one company, Air Squared, Inc., a small Original Equipment Manufacturer (OEM) specializing in design and fabrication of custom scroll vacuum pumps and compressors, was willing to pursue the effort. The first design effort incorporated Vespel® as a polymeric tip seal material. Results of this effort led to realizing the affect that the Met-Bel MB-601 metal bellows pump has on performance when used as a backing pump for an all metal vacuum scroll pump without a scroll tip seal. As a result, Air Squared subsequently designed an all metal vacuum scroll pump without a tip seal material for evaluation. Although the initial, all metal version of the Air Squared pump was found deficient in regard to scroll impeller stiffness, which resulted in scroll contact, general design and pump performance was verified to be adequate. SRS PDRD Project 19039 was launched in 2019 as a 3rd attempt with Air Squared, Inc. in regard to development of an all metal vacuum scroll pump for consideration as an equivalent to the Eumeca/ Normetex pump. The effort specified 300 series stainless steel for the scroll impellers, all metal sealing, and design to meet tritium throughput and ultimate vacuum requirements. In addition, a 60 psig design pressure rating requirement was specified for the pump containment boundary. The 3rd generation Air Squared pump has been designed, fabricated, and has received preliminary testing. Preliminary testing has indicated proper leak tightness and pump performance. However, work continues regarding development of a pumping chamber containment bellows that can be subjected to 66 psig without damage to the bellows. Work will continue in 2020 and 2021 to pursue a pumping chamber containment bellows that meets the pressure rating requirement.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗