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At least 163 records · Page 9
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Critical review of functionalized silica sorbent strategies for selective extraction of rare earth elements from acid mine drainage

We report the ubiquitous and growing global reliance on rare earth elements (REEs) for modern technology and the need for reliable domestic sources underscore the rising trend in REE-related research. Adsorption-based methods for REE recovery from liquid waste sources are well-positioned to compete with those of solvent extraction, both because of their expected lower negative environmental impact and simpler process operations. Functionalized silica represents a rising category of low cost and stable sorbents for heavy metal and REE recovery. These materials have collectively achieved high capacity and/or high selective removal of REEs from ideal solutions and synthetic or real coal wastewater and other leachate source. These sorbents are competitive with conventional materials, such as ion exchange resins, activated carbon; and novel polymeric materials like ion-imprinted particles and metal organic frameworks (MOFs). This critical review first presents a data mining analysis for rare earth element recovery publications indexed in Web of science, highlighting changes in REE recovery research foci and confirming the sharply growing interest in functionalized silica sorbents. A detailed examination of sorbent formulation and operation strategies to selectively separate heavy (HREE), middle (MREE), and light (LREE) REEs from the aqueous sources is presented. Selectivity values for sorbents were largely calculated from available figure data and gauged the success of the associated strategies, primarily: (1) silane-grafted ligands, (2) impregnated ligands, and (3) bottom-up ligand/silica hybrids. These were often accompanied by successful co-strategies, especially bite angle control, site saturation, and selective REE elution. Recognizing the need to remove competing fouling metals to achieve purified REE “baskets,” we highlight techniques for eliminating these species from acid mine drainage (AMD) and suggest a novel adsorption-based process for purified REE extraction that could be adapted to different water systems.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1978

High temperature adhesives for bonding Kapton

Experimental polyimide resins have been developed and evaluated as potential high temperature adhesives for bonding Kapton polyimide film. Lap shear strengths of 'Kapton'/'Kapton' bonds were obtained as a function of test temperature, adherend thickness, and long term aging at 575K (575 F) in vacuum. Glass transition temperatures of the polyimide/'Kapton' bondlines were monitored by thermomechanical analysis.

Saint Clair, A. K.↗
NASA NTRS1994

Modeling of delamination damage evolution in laminated composites subjected to low velocity impact

This study examines the delamination evolution, under quasi-static conditions, of laminated polymeric composites with mechanically nonlinear resin rich interfaces. The constitutive behavior of the interface is represented by two models developed by Needleman and Tvegaard. These models assumed that the interfacial tractions, a function of only the interfacial displacement, will behave similarly to the interatomic forces generated during the interatomic seperation. The interface material's parameters control the load at which the delamination growth initiates and the final delamination size. A wide range of damage accumulation responses have been obtained by varying the model parameters. These results show that Tvergaard's model has been found to be better suited of the two models in predicting damage evolution for the configurations examined.

Lo, David C.↗
DOE OSTI2026

Tailored Silicone Network Architecture for Ultimate Mechanical Reinforcement

Hydrosilylation cured silicone elastomers are subject to reaction inefficiency, leading to incomplete and non-uniform crosslink networks, restricting the potential of mechanical reinforcement. This work investigates pre-synthesized, functional PDMS architectures as additives to improve ultimate mechanical performance relative to conventional single-step curing. Three custom, functional structures were prepared: a partially crosslinked PDMS scaffold (Structure A), a bottle-brush PDMS (Structure B), and a star-shaped PDMS derived from an MQ resin (Structure C). Rheological characterization was used to identify the ultimate design space and proper stoichiometric ratio for Structure A, and confirm successful formation of all structures for suitable incorporation into a base silicone formulation at 30wt%. Mechanical tests indicated that all three structures increased in ultimate tensile strength relative to their single-step counterparts, with Structure A providing additional improvements to toughness (432 vs. 258 kJ/m3) and ultimate elongation (158 vs. 115%). Furthermore, Structure B remained very soft in the unfilled state, while Structure C provided hardness (23 vs. 18 Shore A) and stiffness (780 vs. 420 kPa Young’s modulus) increases. In silica filled systems, Structure A retained increased strength but reduced elongation, while Structure B indicated strong reinforcement in terms of strength, toughness, and stiffness. Thermal analysis on the cure profiles of these materials suggested that pre-formation of network architectures enable a more complete reaction than a single-step process (15.9 vs. 15.1 J/g). Ultimately, these results indicate that tailoring PDMS architecture before the final cure can improve ultimate mechanical properties via improved network development in silicone elastomers. Furthermore, this work offers a promising strategy for designing higher-performance, more tunable silicone formulations.

36 MATERIALS SCIENCE↗
NASA NTRS1995

Neural Network Burst Pressure Prediction in Graphite/Epoxy Pressure Vessels from Acoustic Emission Amplitude Data

Acoustic emission (AE) data were taken during hydroproof for three sets of ASTM standard 5.75 inch diameter filament wound graphite/epoxy bottles. All three sets of bottles had the same design and were wound from the same graphite fiber; the only difference was in the epoxies used. Two of the epoxies had similar mechanical properties, and because the acoustic properties of materials are a function of their stiffnesses, it was thought that the AE data from the two sets might also be similar; however, this was not the case. Therefore, the three resin types were categorized using dummy variables, which allowed the prediction of burst pressures all three sets of bottles using a single neural network. Three bottles from each set were used to train the network. The resin category, the AE amplitude distribution data taken up to 25 % of the expected burst pressure, and the actual burst pressures were used as inputs. Architecturally, the network consisted of a forty-three neuron input layer (a single categorical variable defining the resin type plus forty-two continuous variables for the AE amplitude frequencies), a fifteen neuron hidden layer for mapping, and a single output neuron for burst pressure prediction. The network trained on all three bottle sets was able to predict burst pressures in the remaining bottles with a worst case error of + 6.59%, slightly greater than the desired goal of + 5%. This larger than desired error was due to poor resolution in the amplitude data for the third bottle set. When the third set of bottles was eliminated from consideration, only four hidden layer neurons were necessary to generate a worst case prediction error of - 3.43%, well within the desired goal.

Hill, Eric v. K.↗
DOE OSTI2024

Refractive index matching base resin for extremely fine three-dimensional ceramic structures

An optically clear resin for additive manufacturing includes an optically clear ceramic precursor having a pre-defined refractive index. Each molecule of the ceramic precursor has at least two photopolymerizable functional groups, at least one of the photopolymerizable functional groups being functionalized with a refractive index-tuning group thereby causing the ceramic precursor to have the pre-defined refractive index.

Mettry, Magi↗
DOE OSTI2023

Fluorescent aggregate structure revealed in bisphenol F epoxy thermoset

Bisphenol F (BPF) epoxy resin is a prepolymer component of thermosets used in construction of reinforced carbon fiber composites (RCFC). The fluorescence of this resin can provide information about chemical and structural alterations of the thermoset from thermal or mechanical damage. While some work has investigated the fluorescence spectra of bisphenol A epoxy resin, a structural analog of BPF, none have studied BPF. The purpose of this study is to investigate the baseline fluorescence spectra of the BPF epoxy resin for features that could be utilized for monitoring damage and structural alterations. Bisphenol F epoxy resin was found to have two emission peaks with a broad peak centered at 410 nm and a sharp peak centered at 550 nm. The broad emission peak was identified as the fluorescence from BPF epoxy monomer while the sharp emission peak was found to be from an aggregate structure present in the epoxy resin. It is hypothesized that this structure is an H-aggregate based on the emission features and structural stability of the aggregate compared to the alternative J-aggregate which was determined via density functional theory calculations. The H-aggregate was found to persist into one of the cured thermoset formulations evaluated but was lost when exposed to elevated temperatures below thermal degradation of the thermoset. This loss of aggregate structure was due to polymer network rearrangement. This new fluorescence signature can be used as an indicator of polymer network rearrangement from thermal exposure which may alter the expected material performance and precede thermal degradation.

36 MATERIALS SCIENCE↗
NASA NTRS1987

Ketimine modifications as a route to novel amorphous and derived semicrystalline poly(arylene ether ketone) homo- and copolymers

A series of amine terminal amorphous poly(arylene ether ketone) oligomers of controlled molecular weights (2-15 K) were synthesized. These oligomers have been found to undergo 'self-crosslinking' reactions upon heating above 220 C, via the reaction of the terminal amine groups with the in-chain keto carbonyl functionalities. The resulting networks are ductile, chemically resistant, and nonporous. The networks obtained via generated ketimine functionality were characterized by solid state NMR. They have also been found to be remarkably stable toward hydrolysis. Ketimine functional bishalide monomers have also been synthesized. Such monomers have been utilized to synthesize a wide variety of amorphous poly(arylene ether) ketimine polymers. A high molecular weight hydroquinone functional poly(arylene ether) ketimine has been acid treated to regenerate a poly(arylene ether ketone) backbone in solution. This novel procedure thus allows for the synthesis of important matrix resins under relatively mild conditions.

Mohanty, D. K.↗
NASA NTRS1987

Vibratory response of a stiffened, floor equipped, composite cylinder

A structural modal analysis has been performed on a composite, filament wound cylindrical shell with floor, using a Computer Aided Test (CAT) system. The twelve foot (3.66 m) long shell is five and one half feet (1.68 m) in diameter and includes a half inch thick plywood floor attached to the shell 69 degrees from the vertical centerline through the bottom of the shell. The shell is composed of carbon fibers embedded in an epoxy resin. The cylinder is supported by two heavy, rigid endcaps simulating simply supported end conditions. Modal frequencies of the shell and floor have been extracted by measuring the frequency response functions from impulse excitation by an impact hammer. Reasonable agreement is obtained between the measured structural modal frequencies and mode shapes and analytical results from a computerized prediction model. The effects of floor location, fiber orientation, and skin thickness on the resonance frequencies of the shell and floor have been predicted for a stiffened and unstiffened cylinder.

Grosveld, Ferdinand W.↗
NASA NTRS2000

Mechanical Properties of LaRC(tm) SI Polymer for a Range of Molecular Weights

Mechanical testing of an advanced polyimide resin (LaRC(tm)-SI) with known variations in molecular weight was performed over a range of temperatures below the glass transition temperature. Elastic and inelastic properties were characterized as a function of molecular weight and test temperature. It was shown that notched tensile strength is a strong function of both temperature and molecular weight, whereas stiffness is only a strong function of temperature. The combined analysis of calculated yield stress and notched tensile strength indicated that low molecular weight materials tended to fail in a brittle manner, whereas high molecular weight materials exhibited ductile failure. The microphotographs of the failure surfaces also supported these findings.

Whitley, Karen S.↗
NASA NTRS2009

Functionalizing CNTs for Making Epoxy/CNT Composites

Functionalization of carbon nanotubes (CNTs) with linear molecular side chains of polyphenylene ether (PPE) has been shown to be effective in solubilizing the CNTs in the solvent components of solutions that are cast to make epoxy/CNT composite films. (In the absence of solubilization, the CNTs tend to clump together instead of becoming dispersed in solution as needed to impart, to the films, the desired CNT properties of electrical conductivity and mechanical strength.) Because the PPE functionalizes the CNTs in a noncovalent manner, the functionalization does not damage the CNTs. The functionalization can also be exploited to improve the interactions between CNTs and epoxy matrices to enhance the properties of the resulting composite films. In addition to the CNTs, solvent, epoxy resin, epoxy hardener, and PPE, a properly formulated solution also includes a small amount of polycarbonate, which serves to fill voids that, if allowed to remain, would degrade the performance of the film. To form the film, the solution is drop-cast or spin-cast, then the solvent is allowed to evaporate.

Chen, Jian↗
NASA NTRS2016

Properties of Multifunctional Hybrid Carbon Nanotube/Carbon Fiber Polymer Matrix Composites

For aircraft primary structures, carbon fiber reinforced polymer (CFRP) composites possess many advantages over conventional aluminum alloys due to their light weight, higher strength- and stiffness-to-weight ratios, and low life-cycle maintenance costs. However, the relatively low electrical and thermal conductivities of CFRP composites fail to provide structural safety in certain operational conditions such as lightning strikes. Carbon nanotubes (CNT) offer the potential to enhance the multi-functionality of composites with improved thermal and electrical conductivity. In this study, hybrid CNT/carbon fiber (CF) polymer composites were fabricated by interleaving layers of CNT sheets with Hexcel® IM7/8852 prepreg. Resin concentrations from 1 wt% to 50 wt% were used to infuse the CNT sheets prior to composite fabrication. The interlaminar properties of the resulting hybrid composites were characterized by mode I and II fracture toughness testing. Fractographical analysis was performed to study the effect of resin concentration. In addition, multi-directional physical properties like thermal conductivity of the orthotropic hybrid polymer composite were evaluated.

Cano, Roberto J.↗
NASA NTRS1983

The nonlinear viscoelastic response of resin matrix composites

The current paper describes the utilization of a thermodynamic based analytical nonlinear viscoelastic approach to represent lamina properties. Test data to verify the analysis for both transverse and shear properties of a T300/934 composite are presented. Master curves as a function of stress level and temperature are generated. Favorable comparisons between the traditional graphical and the current analytical approaches are shown.

Hiel, C. C.↗
NASA NTRS2007

Sequestration of Single-Walled Carbon Nanotubes in a Polymer

Sequestration of single-walled carbon nanotubes (SWCNs) in a suitably chosen polymer is under investigation as a means of promoting the dissolution of the nanotubes into epoxies. The purpose of this investigation is to make it possible to utilize SWCNs as the reinforcing fibers in strong, lightweight epoxy-matrix/carbon-fiber composite materials. SWCNs are especially attractive for use as reinforcing fibers because of their stiffness and strength-to-weight ratio: Their Young s modulus has been calculated to be 1.2 TPa, their strength has been calculated to be as much as 100 times that of steel, and their mass density is only one-sixth that of steel. Bare SWCNs cannot be incorporated directly into composite materials of the types envisioned because they are not soluble in epoxies. Heretofore, SWCNS have been rendered soluble by chemically attaching various molecular chains to them, but such chemical attachments compromise their structural integrity. In the method now under investigation, carbon nanotubes are sequestered in molecules of poly(m-phenylenevinylene-co-2,5-dioctyloxy-p-phenylenevinylene) [PmPV]. The strength of the carbon nanotubes is preserved because they are not chemically bonded to the PmPV. This method exploits the tendency of PmPV molecules to wrap themselves around carbon nanotubes: the wrapping occurs partly because there exists a favorable interface between the conjugated face of a nanotube and the conjugated backbone of the polymer and partly because of the helical molecular structure of PmPV. The constituents attached to the polymer backbones (the side chains) render the PmPV-wrapped carbon nanotubes PmPV soluble in organic materials that, in turn, could be used to suspend the carbon nanotubes in epoxy precursors. At present, this method is being optimized: The side chains on the currently available form of PmPV are very nonpolar and unable to react with the epoxy resins and/or hardeners; as a consequence, SWCN/PmPV composites have been observed to precipitate out of epoxies while the epoxies were being cured. If the side chains of the PmPV molecules were functionalized to make them capable of reacting with the epoxy matrices, it might be possible to make progress toward practical applications. By bonding the side chains of the PmPV molecules to an epoxy matrix, one would form an PmPV conduit between the epoxy matrix and the carbon nanotubes sequestered in the PmPV. This conduit would transfer stresses from the epoxy matrix to the nanotubes. This proposed load-transfer mode is similar to that of the current practice in which silane groups are chemically bonded to both the epoxy matrices and the fibers (often glass fibers) in epoxymatrix/fiber composites.

Bley, Richard A.↗
DOE OSTI2025

Chlorocobaltate-Enabled Selective Separation of CoCl 2 from Mixed Chloride and Nitrate Salts of Mn, Co, and Ni

Described here is the effect of anionic metalates─chlorocobaltate and nitratocobaltate─on the heat-driven separation of the critical element cobalt from potentially competing transition metal salts. Resins bearing the hexadentate glycolamide receptor L (PS-L) exhibit sorption capacities, Q = 1.33 mmol/g for CoCl 2 and Q = 0.66 mmol/g for Co(NO 3 ) 2 , as inferred from sorption isotherm studies. This trend runs counter to the typical Hofmeister series for anion selectivity. Ion chromatographic analysis of a mixed CoCl 2 /Co(NO 3 ) 2 solution revealed an increase in chloride content from 55 mol % to 90 mol % after a single thermally driven catch-and-release cycle. This chloride-selective behavior was recapitulated in a mixed-metal cation, mixed-anion system containing the chloride and nitrate salts of Mn(II), Co(II), and Ni(II) at near-equimolar concentrations. PS-L also displayed enhanced selectivity for Co using this mixed stock solution as observed by ICP-OES. In contrast, for a nitrate-only solution containing Mn(II), Co(II), and Ni(II), PS-L showed increased affinity for Mn, with its proportion rising from 36.6 mol % to 58.1% after a single catch-and-release cycle. Density functional theory calculations support the suggestion that the enhanced uptake of Co(II) in chloride-rich media arises from the high thermodynamic stability of [CoCl 4 ] 2– , which facilitates its outer-sphere coordination to cationic resin-bound cobalt species. Single crystal X-ray crystallographic analyzes of L•MCl 2 (M = Mn, Co, Ni) and L•M(NO 3 ) 2 (M = Mn, Co) confirmed metal complexation by L in the solid state and the concomitant formation of metalate counteranions. Here, the present study highlights a relatively simple approach for separating cobalt from its transition metal congeners.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2004

Effects of Molecular Structure in Macroscopic Mechanical Properties of an Advanced Polymer (LARC(sup TM)-SI)

Mechanical testing of an advanced polymer resin with known variations in molecular weight was performed over a range of temperatures below the glass transition temperature. The elastic properties, inelastic elongation behavior, and notched tensile strength all as a function of molecular weight and test temperature were determined. It was shown that notched tensile strength is a strong function of both temperature and molecular weight, whereas stiffness is only a strong function of temperature.

Nicholson, Lee M.↗
NASA NTRS2013

Unibody Composite Pressurized Structure

An integrated, generic unibody composite pressurized structure (UCPS) combined with a positive expulsion device (PED), consisting of an elastomeric bladder for monopropellant hydrazine, has been quasi-standardized for spacecraft use. The combination functions as an all-composite, non-metallic, propellant tank with bladder. The integrated UCPS combines several previous innovations - specifically, the linerless, all-composite cryogenic tank technology; all-composite boss; resin formulation; and integrated stringer system. The innovation combines the UCPS with an integrated propellant management device (PMD), the PED or bladder, to create an entirely unique system for in-space use. The UCPS is a pressure vessel that incorporates skirts, stringers, and other structures so that it is both an in-space hydrazine tank, and also a structural support system for a spacecraft in a single, all-composite unit. This innovation builds on the progress in the development of a previous SBIR (Small Business Innovation Research) Phase I with Glenn Research Center and an SBIR III with Johnson Space Center that included the fabrication of two 42-in. (≈107-cm) diameter all-composite cryogenic (LOX and liquid methane) UCPS test tanks for a lunar lander. This Phase II provides hydra zine compatibility testing of the elastomeric bladder, a see-through PED to validate the expulsion process and model, and a complete UCPS-based PED with stringers and skirts that will be used to conduct initial qualification and expulsion tests. This extends the UCPS technology to include hydrazine-based, in-space pro - pulsion applications and can also be used for electric propulsion. This innovation creates a system that, in comparison to the traditional approach, is lower in weight, cost, volume, and production time; is stronger; and is capable of much higher pressures. It also has fewer failure modes, and is applicable to both chemical and electric propulsion systems.

Rufer, Markus↗
NASA NTRS1995

A new technique for ground simulation of hypervelocity debris

A series of hypervelocity damage experiments were preformed on spacecraft materials. These experiments employed a technique which accelerates micro flyer plates simulating space debris traveling at 3 to 8 km/sec. The apparatus used to propel the micro flyer plates was compact and fit well into a space environmental chamber equipped with instrumentation capable of analyzing the vapor ejected from the sample. Mechanical damage to the sample was also characterized using optical and scanning electron microscpopy. Data for this work was obtained from hypervelocity impacts on a polysulfone resin and a graphite polysulfone composite. Polysulfone was selected because it was flown on the Long Duration Exposure Facility (LDEF) which spent several years in low earth orbit (LEO). Chemistry of the vapor produced by the impact was analyzed with a time of flight mass spectrometer, (TOFMS). This represents the first time that ejected vapors from hypervelocity collisions were trapped and analyzed with a mass spectrometer. With this approach we are able to study changes in the vapor chemistry as a function of time after impact, obtain a velocity measurement of the vapor, and estimate a temperature of the surface at time of impact using dynamic gas equations. Samples of the vapor plume may be captured and examined by transmission electron microscopy. Studies were also conducted to determine mechanical damage to a graphite polysulfone composite and a polysulfone resin. Impact craters were examined under optical and scanning electron microscopes. The collision craters in the matrix were typical of those shown in conventional shock experiments. However, the hypervelocity collisions with the graphite polysulfone composite were remarkably different than those with the resin.

Roybal, R.↗