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At least 19 records

Sequestering Rare Earth Elements and Precious Metals from Seawater Using a Highly Efficient Polymer Adsorbent Derived from Acrylic Fiber

An amidoxime and carboxylate containing polymer adsorbent derived from acrylic fiber has shown extremely high efficiencies for extracting critical materials and precious metals from seawater. Among 50 extractable elements, the lanthanides, cobalt, and palladium were ranked near the top with KD values in the order of 107, about an order of magnitude higher than that of uranium. The KD value of the lanthanides increased linearly with the atomic number indicating charge density is a factor controlling trivalent lanthanide extractability in seawater. The data given in this report provides crucial information regarding the strategies of ocean mining of critical materials and precious metals.

36 MATERIALS SCIENCE↗

Development of a Lower Cost, High Volume, Commercially Available, Precursor for Lower Cost Carbon Fiber for Automotive and Wind Blade Applications

Essentially all carbon fibers used in structural applications are presently manufactured from solution spun polyacrylonitrile (PAN) precursor. Solution spinning is accomplished at relatively low temperatures using very large amounts of environmentally unfriendly solvents that impart major impact to line speed and costs involved with handling and reclaiming the solvents and associated “waste streams” required in spinning and extracting those solvents. Dralon and others have demonstrated the dry spinning of PAN in the production of some acrylic fibers for textile applications, but to this point it has not been demonstrated in the production of carbon fibers. In dry spinning, the PAN polymer is also dissolved into similar solvents, although typically less solvent is utilized to maintain a somewhat higher solids content of 20-50%. The use of lower overall solvent quantities and elimination of the need for solvent/water separation simplifies and reduces the cost of solvent recovery operations. Other portions of the precursor production and carbon fiber manufacturing processes are quite similar. The work described in this report demonstrated that dry spun acrylic fiber can be an attractive candidate for carbon fiber precursor of potential interest to applications looking to capture the specific stiffness (stiffness per unit mass) and specific strength (strength per unit mass) of carbon fiber when produced at a discount relative to commercial carbon fibers in the market today. Dralon has determined that the dry spinning process utilized for producing fibers used as precursors in this project requires 27% less energy versus producing comparable fibers via the industry standard wet spinning process. Identification of carbon fiber manufacturers, as well as applications development and targeted marketing, will be required to achieve significant in-roads into mission areas of interest to DOE, such as automotive applications and wind turbine blades. In support of that activity, initial data produced in this project indicate the innovative approach as described in this report can meet at least the baseline property requirements identified for these applications.

36 MATERIALS SCIENCE↗

IACMI Project 4.7: Pultruded Textile Carbon Fiber for Spar Caps (Final Report)

The primary objective of this project was to demonstrate the potential to significantly reduce the cost of wind turbine blades with carbon fiber reinforced polymer (CFRP) structure. Applicability of textile carbon fibers (TCF) were evaluated for use in pultruded spar cap (SC) elements as a path to cost reduction for utility scale wind turbine blades. In earlier work for the Department of Energy (DOE) Wind Energy Technologies Office (WETO), a collaboration of Sandia National Laboratory (SNL), Oak Ridge National Laboratory (ORNL), and Montana State University has demonstrated potential for pultruded TCF to compete with infused fiberglass and commercially available carbon fiber pultruded sections for spar cap construction. In the design cases evaluated, the TCF sections fared well when compared on cost per unit composite stiffness and cost per unit composite compressive strength for those designs [1]. Both stiffness and compressive strength tend to be key factors in the design of blade composite Spar Cap which carry the bulk of the blade structural loads in bending. Spar Cap design tends to distribute largely symmetric tensile and compressive stresses to opposite sides of the spar structure, but since carbon fiber composite compressive strength is typically 20-50% lower than tensile strength, the compressive loading reaches failure levels well before the tensile loading. Stiffness is critical in containing the large tip deflection in high wind loading situations. However, materials and process development were very limited in the earlier study and the work in this project was expanded to make the comparative information more representative of what will be required in order to make further inroads towards implementation. Similar to that study, this project team confirmed that the primary materials of interest for pultruded spar cap elements should be thermoset (TS) resins reinforced by carbon fibers, utilizing as high a percentage of TCF as practical to benchmark cost and performance against commercial carbon fibers. To make the closest comparison possible and eliminate specific test article size, resin selection, and equipment/operational nuance effects, the team planned to pultrude sections with 100% commercially available carbon fiber (Panex 35 carbon fiber from Zoltek) as well as samples utilizing high fractions of TCF. The resin system chosen was based on formulations recommended by large wind industry supplier Hexion and consisted of Hexion resin RSL-4597, curing agent CCA-138, and internal mold release additive 117, along with common kaolin filler ASP400P from BASF. As commonly deployed in spar cap configurations, the team had a mold built to pultrude a rectangular spar cap element of 100mm width and 3mm thickness. The extremely limited number of samples produced for the earlier study were produced with a “generic” epoxy utilized for a variety of applications by the pultruder contracted to produce test articles for demonstration purposes. More importantly, those samples were produced at a fiber fraction only slightly over 50%. Based on feedback from our industrial advisory team for that project and strongly recommended by this project team, the consensus is that it is highly desirable to obtain fiber fractions of 65-68% for significant penetration in wind blade spar cap. Although this requirement has yet to be exhaustively confirmed in readily available information, this was established as a project goal and informally decided we needed to exceed 60% fiber fraction to gain serious industry consideration. Previous TCF pultrusion trials have been challenged by the lack of robust TCF packages, resulting in non-uniform tension across and between tows, as well as excess labor and waste for removal of interleaved paper. The non-uniform tension and associated intermingling of tows in textile acrylic fiber tows and associated difficulties created from broken filaments in carbon fiber conversion inhibit the ordered packing necessary to enhance fiber fraction elevation. (These “cross-overs” are not considered undesirable for textile applications and there is some sense that they might be advantageous for those applications). In addition to work that is ongoing at the acrylic fiber manufacturers to improve their formats, The Institute of Advanced Composites Manufacturing Innovation (IACMI) Project 6.12 (report PA16-0349-6.12-01) [2] has developed and demonstrated a more robust packaging and creeling approach that at least partially addresses these issues, thus improving control of the TCF feed into the pultrusion unit. It was hoped that these and other improvements currently being implemented would allow us to achieve fiber fractions at least approaching these fiber fraction targets. During this project, sections utilizing 100% commercially available carbon fiber reinforcement were produced as a baseline, as well as sections reinforced with about 94% TCF and the balance being commercially available fiber for comparison. The most important finding was that similar to results reported in the earlier WETO-funded project and results from tests of TCF reported at IACMI meetings, this work demonstrated that sections pultruded with TCF in an epoxy resin frequently utilized in actual spar cap production had stiffness and compressive strengths largely comparable to similar sections pultruded with a commercially available carbon fiber also frequently utilized in the wind industry. Although the amount of that data is limited, some of the tensile strength results were actually closer than would have been expected based on fiber strength results provided by the TCF and commercial fiber producers. The actual test data are reported and discussed in detail in Section 5. The pultruded sections dominated by TCF reinforcement were approximately 8-10% lower in fiber fraction than for the sections produced using commercial fiber alone, making direct comparison difficult. The COVID-19 project has provided significant insight into the current state-of-the-art with various TCF product forms. The data obtained in this project will guide the planned improvements at the precursor level, especially in attaining uniform tensioning and payout to facilitate enhanced fiber fractions and overall processability of the TCF composites. The project team is providing guidance to stakeholders concerning the attributes, needs, and potential demand for TCF in wind blade spar caps. Results achieved in this project are consistent with findings in the related work cited [1] and support this guidance and the high potential for this product type. TCF precursor-producing partners continue to express interest in enhancing their product forms and the team looks forward to working with these improved materials as they become available.

42 ENGINEERING↗

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Testing and Characterization to Develop a Mechanistic Explanation for Unsaturated Drift of Fiber Optic Sensors during High-Dose Irradiation

The primary limitation for any optical fiber-based sensor for nuclear reactor applications is radiation-induced attenuation (RIA) of the transmitted and/or reflected signals. Based on several recent studies, RIA is tolerable for some fused silica optical fibers with the proper choice of sensing wavelength and fiber dopants. For extreme temperature applications (> 1000°C), sapphire optical fibers have been proposed; however, recent optical transmission measurements performed on bulk sapphire samples showed prohibitively large RIA. For some sensors, radiation-induced dimensional changes in the fiber materials can also cause significant drift. Moreover, the drift that was observed in numerous experiments performed in the High Flux Isotope Reactor (HFIR), the Advanced Test Reactor, the Massachusetts Institute of Technology Reactor, and other international facilities far exceeded what would be expected based on compaction of fused silica glass. Clearly, additional work is needed to better understand the origins of both RIA and radiation-induced drift in both silica and sapphire optical fiber-based sensors before these sensors can be reliably deployed for nuclear applications. This work evaluated the underlying mechanisms that may be responsible for RIA and drift in silica and sapphire materials. First, detailed characterization was performed on bulk fused silica glass samples that were previously irradiated to different neutron fluences at different temperatures to better understand the structural changes that drive radiation-induced drift in the absence of coating effects that are discussed later. Results show that the non-monotonic compaction that occurs with increasing neutron fluence continues up to fast neutron fluences approaching 10 22 n/cm 2 , which has important implications for physics-based models that may be used to compensate for the sensor drift. Initial Raman spectroscopy and synchrotron x-ray diffraction provide insights into the nature of the structural changes. Next, detailed characterizations were performed on silica fibers with various coatings that were subjected to several different thermal treatments. The hypothesis is that the coatings convert to carbon-rich materials that compact under irradiation, putting a large compressive strain on the fiber. Out-of-pile testing confirms that both polyimide and acrylate fiber coatings convert to glassy carbon (GC) materials when heated under inert conditions, and the degree of order (i.e., graphitization) increases with increasing temperature. The results provide increasingly strong evidence that the combination of polymeric coatings and inert (or vacuum) conditions render fiber optic sensors susceptible to significant radiation-induced drift that would not otherwise exist in uncoated fibers. Finally, transmission electron microscopy was performed on bulk sapphire samples that were irradiated to two neutron fluences at different temperatures to gain insights into the potential mechanisms driving the prohibitive RIA at higher neutron fluences and temperatures. Contrary to previous hypotheses, results show that scattering from radiation-induced voids cannot explain the observed RIA. Similarly, models for scattering losses from dislocation loops also do not agree with the experimental results. Instead, fitting to the experimental data shows that increased absorption from aluminum vacancy centers is the most likely explanation for the the prohibitively large RIA that was observed at high irradiation temperature and dose. In addition, the voids that formed in these single-crystal samples were found to align along the basal plane (a-axis) as opposed to that seen in previous observations of c-axis alignment in polycrystalline samples, which could have important implications for anisotropic swelling and other phenomena that could affect sensor performance at high neutron fluence.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

High-resolution fiber imaging for pulsed power experiments

This work presents a novel approach for imaging the visible emissions from plasmas in pulsed power experiments using high-resolution plastic optical fibers. The diagnostic consists of a 2 mm diameter core commercial cable constructed of 13 000 individual acrylic fibers. The fibers are fused together to create a single high-resolution bundle. Different designs were investigated to cover a wide range of resolutions and fields of view (3–700 µm and 0.05–45 mm, respectively). The system was tested on the 1-MA Mykonos accelerator at Sandia National Laboratories and successfully imaged visible emission from a hybrid x-pinch target. Diagnostic development and preliminary results are presented.

Fulford, K. W. (ORCID:0000000309691832)↗

Melt-Spun PAN Precursor for Cost-Effective Carbon Fibers in High Pressure Compressed Gas Tankage

The objective of this program was to synthesize melt-spinnable polyacrylonitrile (PAN) precursor that will lead to carbon fiber 25% less expensive than carbon fiber produced from conventional PAN precursor when produced in large volumes. The carbon fiber produced from this precursor needs to achieve ≥ 700 ksi tensile strength with this cost reduction to replace the incumbent fiber. In this program, the technology for producing precursor and then converted carbon fiber (CF) capable of meeting the 700 ksi target was to be demonstrated at a small scale in tows, containing ≥ 100 filaments. If this program moved on to a “Phase 2”, the processes would be scaled up to produce and test Type IV compressed gas storage tanks capable of meeting the 700-bar ultimate targeted FOA performance level. Precursor fiber production typically contributes a large fraction (~50%) to finished CF manufactured cost. Presently, all high strength CFs are manufactured from solution spun PAN precursor, accomplished at low temperatures using large amounts of environmentally unfriendly solvents that impart major impact to line speed and costs involved with handling and reclaiming the solvents and associated “waste streams” required in spinning and extracting those solvents. PAN melt spinning was demonstrated by the company BASF in CF precursor production and used in production of some other acrylic fibers, but significant production challenges remain for meeting the established CF metrics. Melt spinning requires use of plasticizers to suppress the melt temperature of the predominantly PAN formulation to a point sufficiently below the temperature of significant cross-linking. Fortunately, BASF and this team’s earlier work had demonstrated acrylic formulations melt spun with combinations of plasticizing solvents at much lower solvent levels. This project team made significant progress in understanding technical issues and identifying formulation pathways in earlier work in this area where >250ksi strength was achieved. The goal of this program was to pursue a more comprehensive approach with a larger, more diverse team having greater equipment design and overall production capabilities to push rapidly beyond the science to resolve remaining “engineering” issues associated with establishing stable, continuous processes for precursor fiber leading to enhanced, cost-effective CF and composite tank production.

36 MATERIALS SCIENCE↗

Empirical Characterization and Modeling of Cohesive – to – Adhesive Shear Fracture Mode Transition due to Increased Adhesive Layer Thicknesses of Fiber Reinforced Composite Single – Lap Joints

Here, to ensure a strong adhesive bond, most standards and adhesive manufacturers specify a maximum adhesive gap of 1 mm when bonding fiber reinforced composite structures. In manufacturing large components, such as joining two halves of wind turbine blades, meeting this gap tolerance specification is impractical; gaps larger than 10 mm are common in large adhesively bonded composite structures using state-of-the-art manufacturing techniques. Currently, there is a lack of fundamental understanding of the failure mechanics of adhesive gaps larger than 3 mm. To create such understanding, glass fiber - acrylic thermoplastic composite panels bonded using different epoxy adhesives within single-lap joint samples with adhesive thicknesses of 0.1 mm, 0.3 mm, 1 mm, 3 mm, 5 mm, and 10 mm were sheared to failure. A transition from cohesive to adhesive failure was observed to occur about 1 mm to 3 mm joint thicknesses. Plotting the shear stress normalized by the ratio of the joint width to thickness as a function of the joint thickness normalized by the joint length is shown to result in the ability to fit simple empirically derived models of the cohesive-to-adhesive failure transition, regardless of the adhesive. Furthermore, using these normalized variables, all the observed cohesively failed specimens collapse to a single master curve, as do the adhesively failed specimens.

36 MATERIALS SCIENCE↗

Bacteria/virus filter membrane

Hollow acrylate fiber membrane that filters bacterial and viral organisms can be used with closed-cycle life-support systems for underwater habitations or laboratories. Membrane also has applications in fields of medicine, gnotobiotics, pharmaceutical production, and industries and research facilities that require sterile water. Device eliminates need for strong chemicals or sterilizing agents, thereby reducing costs.

Lysaght, M. S.↗

Infusible thermoplastic resin based sandwich structures for wind blade applications and the influence of scrim on facesheet to core interface debonding

Infusible thermoplastic Elium® family of resins from Arkema have garnered much attention in recent years as a possible replacement for thermoset resins in laminate and sandwich composite manufacturing for wind blade applications due to its ease of recyclability and the ability to utilize existing manufacturing processes without imposing complicated variations. However, physical and mechanical properties of the proposed Elium® based thermoplastic composites must be comparable to existing epoxy (thermoset) based composites using manufacturing processes relevant for large wind turbine blades. A 13-meter-long demonstration blade was manufactured for that purpose and sandwich samples were obtained from that project for a detailed study. This paper details three-point flexural properties of unidirectional E-glass fiber reinforced acrylic and epoxy based sandwich panels with identical balsa wood core materials. In addition, to evaluate the relative merit considering debond failure mode, the interfacial critical strain energy release rate, predominantly in mode-1, was compared via single cantilever beam testing. In sandwich composites constructed with balsa wood core material, resin uptake by the balsa core is traditionally impeded via the insertion of a scrim material at the facesheet to core interface. Results revealed that inclusion of scrim mesh layer at the facesheet to core interface reduced flexural properties and strain energy release rates in panels infused with acrylic resin but did not significantly reduce these properties in epoxy infused facesheets.

Engineering↗

Technology Validation of Optical Fiber Cables for Space Flight Environments

Periodically, commercially available (COTS) optical fiber cable assemblies are characterized for space flight usage under the NASA Electronic Parts and Packaging Program (NEPP). The purpose of this is to provide a family of optical fiber cable options to a variety of different harsh environments typical to space flight missions. The optical fiber cables under test are evaluated to bring out known failure mechanisms that are expected to occur during a typical mission. The tests used to characterize COTS cables include: (1) vacuum exposure, (2) thermal cycling, and (3) radiation exposure. Presented here are the results of the testing conducted at NASA Goddard Space Flight Center on COTS optical fiber cables over this past year. Several optical fiber cables were characterized for their thermal stability both during and after thermal cycling. The results show how much preconditioning is necessary for a variety of available cables to remain thermally stable in a space flight environment. Several optical fibers of dimensions 100/140/172 microns were characterized for their radiation effects at -125 C using the dose rate requirements of International Space Station. One optical fiber cable in particular was tested for outgassing to verify whether an acrylate coated fiber could be used in a space flight optical cable configuration.

Ott, Melanie N.↗

Infusible Thermoplastic Composites for Wind Turbine Blade Manufacturing: Fatigue Life of Thermoplastic Laminates under Ambient and Low-Temperature Conditions

Traditionally, thermoset resins such as polyesters (PE) and epoxies are used as the polymer matrix for construction of wind turbine blades. However, concern about their end-of-life treatment garners interest to use thermoplastics for increased recyclability. However, the high viscosity of molten thermoplastics inhibits their use in manufacturing wind turbine blades with injection or compression molding. A recently developed, infusible, reactive thermoplastic resin overcomes this technological barrier. Toward verifying that this recyclable resin is suitable for use in wind turbine blades, a dataset of R?=?0.1 and R?=?10 fatigue data for glass fiber-reinforced acrylic composites is provided and equal fatigue life to industry standard epoxy and unsaturated PE resin systems is demonstrated. Specifically, R?=?0.1 fatigue data for acrylic composites at room temperature and -30?degrees C for verification of low-temperature performance are tabulated. To elucidate failure mechanisms, in situ mechanical testing with X-ray computed tomography demonstrates that damage accumulation occurs by crack propagation along the fiber-matrix interface under cyclic loading. Infrared (IR) thermography predicts failure points in composites specimens with porosity defects introduced from nonideal manufacturing processes. Furthermore, these manufacturing defects are shown to compromise the fatigue life of the acrylic laminates by an order of magnitude.

effect of defects↗

Dopant, coating, and grating effects in silica optical fibers under extreme neutron irradiation

Radiation effects on fiber Bragg gratings (FBGs) have been studied but data gaps related to the effects of displacement damage resulting from high fast neutron fluence remain. In this work, Type-I and Type-II FBGs inscribed in optical fibers with various core dopants (Ge and F) and fiber coatings (acrylate, polyimide) were monitored in situ during 75 days of neutron irradiation to a peak fast (>0.1 MeV) neutron fluence of 3 X 10 21 n fast /cm 2 . Further, the reflected intensity of the Type-I FBGs inscribed in a Ge-doped core fiber decreased by > 30 dB within 7 h of irradiation (10 19 n fast /cm 2 ), whereas Type-II FBGs inscribed in a pure silica core fiber eventually approached >40 dB attenuation after accumulating a fast neutron fluence on the order of 10 20 n fast /cm 2 . Type-II FBGs inscribed in F-doped core fiber improved stability: the attenuation approached an equilibrium value in the range of 10 to 20 dB.

47 OTHER INSTRUMENTATION↗

Production of Uranium from Seawater Using a Novel Polymer Adsorbent – Process Development and Cost Analysis (Final Scientific/Technical Report SBIR Phase II)

Research in developing techniques for extracting uranium from seawater is of considerable current interest. One reason which drives scientists to develop techniques of sequestering uranium from ocean is the prediction that the land-based uranium reserves would be depleted by the end of this century based on the current production rate. Uranium exists in seawater at a very low concentration (about 3 ppb) and as highly stable uranyl tris-carbonato complexes, primarily in the form Ca 2 [UO 2 (CO 3 ) 3 ]. Because of the enormous volume of seawater, the total amount of uranium in ocean is estimated to be a thousand times greater than the land-based uranium resources. As early as 1964, the idea of extracting uranium from seawater was discussed by Davies et al. in a Nature paper. In the past decades, many different materials were tested to evaluate their ability for sequestering uranium from seawater. Among them, amidoxime and carboxylate containing polymer fiber adsorbents appear most promising because of their high uranium adsorption capacity and stability in seawater. The carboxylate groups are necessary to make the polymer adsorbent hydrophilic whereas the amidoxime groups provide strong coordination sites for uranyl ions. Moreover, according to theoretical analysis, the adsorbability of uranium may involve synergistic effects of both amidoxime and carboxyl groups in the fiber adsorbent.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Process modifications for improved carbon fiber composites: Alleviation of the electrical hazards problem

Attempts to alleviate carbon-fiber-composite electrical hazards during airplane crash fires through fiber gasification are described. Thermogravimetric and differential scanning calorimetric experiments found several catalysts that caused fibers to combust when composites were exposed to test fires. Composites were tested in the 'Burn-Bang' apparatus and in high voltage electrical detection grid apparatus. In a standard three minute burn test modified composites released no fibers, while state-of-the-art composites released several hundred fiber fragments. Expected service life with and without catalytic modification was studied and electron microscopy and X-ray microanalysis furnished physical appearance and chemical composition data. An acrylic acid polymer fiber coating was developed that wet the carbon fiber surface uniformly with the catalyst, providing a marked contrast with the uneven coats obtained by solution-dipping.

Ramohalli, K.↗

Effect of temperature on optical fiber transmission

Results are presented concerning the effects of temperature on the transmission properties of various optical fibers including a silicone plastic clad, an acrylic plastic clad, and CVD step-index fibers both with and without polyurethane jackets. Results are presented for the normalized transmitted power vs temperature, the index of refraction vs temperature, and induced attenuation coefficients vs temperature. The data show that the intrinsic transmission of a CVD fiber is independent of temperature over the -110 to +150 C range. Plastic clad fused silica fibers are subject to transmission losses at lower temperatures due to changes in the optical index of the cladding polymer. Acrylic-clad and plastic-clad silica fibers also show transmission losses at lower temperatures, but to lesser extents.

Yeung, W. F.↗

Electrospun Si and Si/C Fiber Anodes for Li-Ion Batteries

Due to structural changes in silicon during lithiation/delithiation, most Li-ion battery anodes containing silicon show rapid gravimetric capacity fade upon charge/discharge cycling. Herein, we report on a new Si powder anode in the form of electrospun fibers with only poly(acrylic acid) (PAA) binder and no electrically conductive carbon. The performance of this anode was contrasted to a fiber mat composed of Si powder, PAA binder, and a small amount of carbon powder. Fiber mat electrodes were evaluated in half-cells with a Li metal counter/reference electrode. Without the addition of conductive carbon, a stable capacity of about 1500 mAh/g (normalized to the total weight of the anode) was obtained at 1C for 50 charge/discharge cycles when the areal loading of silicon was 0.30 mgSi/cm2, whereas a capacity of 800 mAh/g was obtained when the Si loading was increased to ~1.0 mgSi/cm2. On a Si weight basis, these capacities correspond to >3500 mAh/gSi. The capacities were significantly higher than those found with a slurry-cast powdered Si anode with PAA binder. There was no change in fiber anode performance (gravimetric capacity and constant capacity with cycling) when a small amount of electrically conductive carbon was added to the electrospun fiber anodes when the Si loading was ≤1.0 mgSi/cm2.

Mondal, Abhishek N.↗

Glassy carbon formation from pyrolysis of polymeric coatings on fiber-optic sensors

Deploying fiber-optic sensors in nuclear reactors requires a detailed understanding of radiation effects on the fiber materials and the transmitted signals. Previous work has shown large wavelength shifts in the reflected spectra obtained from polymer-coated fiber-optic temperature sensors exposed to high neutron fluences. The sensor drift resulting from these wavelength shifts cannot be explained by radiation effects on fused silica glass. These shifts are hypothesized to be caused by the conversion of the polymeric fiber coating to a glassy carbon via radiolysis and/or pyrolysis and subsequent radiation-induced compaction. Here, thermal degradation of these polymeric coatings was studied to provide insight into the potential origins of the sensor drift phenomenon. Acrylate- and polyimide-coated fibers were heated under various temperatures (250–1300 °C) and environments (oxidative and inert), and the resulting coating products were characterized via mass-loss data, scanning electron microscope imaging, and Raman spectroscopy. Results suggest that the polymer decomposition product of both coating types, at least under inert conditions, is indeed a glassy carbon. Analytical models that account for radiation-induced glassy carbon coating compaction show significant compressive fiber strains and predicted wavelength shifts that agree well with experimental measurements, providing additional evidence that supports the hypothesized origins of the sensor drift.

36 MATERIALS SCIENCE↗