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At least 127 records · Page 7

Influence of thread construction on strength of ceramic sewing threads

The effects of two thread construction variables, yarn twist and polymeric sizing, on break strength were obtained for a silica thread and two types of aluminoborosilicate (ABS) threads at temperatures ranging from 23 C to 1200 C. It was shown that increasing the degree of twist for the silica thread produced an optimum twist level until all the yarn finish was removed. The break strength of both ABS threads was inversely proportional to the degree of twist caused by increased filament breakage with increasing twist that was controlled by the gradual removal of the polymeric processing aids. At elevated temperatures, above 950 C, strength loss was observed for both ABS threads because of the presence of a glass phase that softens and causes fiber deformation. This was not observed for the silica thread at similar test temperatures because of the higher viscosity of the pure silica glass phase.

Sawko, Paul M.↗

Iron-Catalyzed Cross-[2 + 2] Cycloaddition of Butadiene and α,ω-Dienes for Ductile and Chemically Recyclable Poly(oligocyclobutanes)

Poly(divinyloligocyclobutanes) (pDVOCBs) are a distinct class of butadiene-derived, chemically recyclable polyolefins prepared from iron-catalyzed [2 + 2] cycloaddition followed by ruthenium-catalyzed ADMET polymerization. These polymers are highly crystalline, with high melting temperatures and unique rotator phases. The high degree of crystallinity in these materials not only leads to high stiffness over a broad temperature range but also results in brittle failure for polymers of modest molecular weights. Iron-catalyzed cross-[2 + 2] cycloaddition of butadiene and α,ω-dienes was accomplished, where the number of methylene units between the four-membered rings was systematically varied. Subsequent ADMET polymerization of the resulting telechelic oligomers provided a new class of chemically recyclable polyolefins that exhibit distinct thermomechanical properties. Specifically, methylene units induce changes in crystallinity that, in combination with the increased molecular weight, favored the formation of stable necks upon tensile deformation, with ∼10× enhanced ductility and improved toughness compared to pDVOCB. Through combined experimental and computational studies, the effects of methylene spacers on the crystal-to-rotator transition of the cyclobutane polymers were established. Ultimately, these methylene-modified cyclobutane polymers expand the range of properties and potential applications of this class of recyclable polyolefins.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Moisture resistant and anti-reflection optical coatings produced by plasma polymerization of organic compounds

The need for protective coatings on critical optical surfaces, such as halide crystal windows or lenses used in spectroscopy, has long been recognized. It has been demonstrated that thin, one micron, organic coatings produced by polymerization of flourinated monomers in low temperature gas discharge (plasma) exhibit very high degrees of moisture resistence, e.g., hundreds of hours protection for cesium iodide vs. minutes before degradation sets in for untreated surfaces. The index of refraction of these coatings is intermediate between that of the halide substrate and air, a condition for anti-reflection, another desirable property of optical coatings. Thus, the organic coatings not only offer protection, but improved transmittance as well. The polymer coating is non-absorbing over the range 0.4 to 40 microns with an exception at 8.0 microns, the expected absorption for C-F bonds.

Hollahan, J. R.↗

Improved Fire-Resistant Resins for Laminates

Fire-resistant resins for fabricating laminates with inorganic fibers, especially graphite fibers, are formed from bisimides containing main-chain phosphorus and olefinic end groups. Bisimides are thermally polymerized to form resins and laminates virtually imcombustible in pure oxygen at 300 degrees C. New resins are suitable for many applications requiring good adhesion and excellent resistance to heat, fire, solvents and chemicals.

Fohlen, G. M.↗

Bisimide amine cured epoxy /IME/ resins and composites. II - Ten-degree off-axis tensile and shear properties of Celion 6000/IME composites

Bisimide amines (BIAs), which are presently used as curing agents in a state-of-the-art epoxy resin, are oligomeric and polymeric mixtures. A series of composites consisting of the novel BIA-cured epoxy resin reinforced with Celion 6000 graphite fibers were fabricated and evaluated, and the ten-degree, off-axis uniaxial tensile and shear properties of these composites were determined. The use of the intralaminar shear strain-to-failure was used in the calculation of resin shear strain-to-failure. Study results indicate that several of these novel composite systems exhibit shear strain properties that are superior to those of the control composite system of the present experiments, which employed a sulfone curing agent.

Scola, D. A.↗

High-Fidelity and High-Performance Computational Simulations for Rapid Design Optimization of Sulfur Thermal Energy Storage

Industrial process heating (IPH) accounts for approximately 70% of US manufacturing energy use and is primarily produced by fossil fuel combustion. Approximately 1500 TWht (approximately 60%) of IPH demand is in the temperature range of 100-300. Industrial applications in this temperature range include drying, hydrothermal processing, thermal enhanced oil recovery, food and beverage, bioethanol production, etc. Cost-effective thermal energy storage (TES) that increases the utilization of waste and renewable heat (solar, geothermal, etc.) could provide significant energy savings and reliable heat sources, decrease emissions, and increase US manufacturing competitiveness through reductions in fuel consumption. TES development has historically been dominated by technologies suitable for deployment with concentrating solar power (CSP). State-of-the-art thermal storage deployed commercially with power tower CSP plants uses a 60%/40% NaNO3/KNO3 molten salt and operates between temperatures of approximately 280 degrees Celsius and 570 degrees Celsius using a two-tank configuration. However, these nitrate salts are unsuitable for operation outside of this temperature range due to a high freezing point of approximately 220 degrees Celsius, and limits on high-temperature salt stability and corrosion resistance of containment alloys. Other materials being investigated for TES include those based on: (1) sensible energy storage (various molten salt compositions, inert solid particles, rocks or pebble beds, sulfur, water, concrete, graphite, etc.), (2) latent energy storage in materials that undergo solid-liquid phase change at relevant temperatures (organic materials for low-temperature applications, inorganic salts and/or metals for high-temperature applications), or (3) thermochemical energy storage (hydrides, hydroxides, carbonates, metal oxides, etc.). The application temperature and challenges pertaining to storage material and/or containment cost, energy density, long-term thermal and cyclic stability, and charge/discharge heat transfer effectiveness drive material selection for a given IPH or electricity generation application. Sulfur is a cheap commodity at $80/ton compared to $1100 - 1300/ton for conventional salts. When using a metric of storage cost per kWh, sulfur costs around 2-3 $/kWh. Previous sulfur TES development focused on high temperature (>600 degrees) concentrated solar power applications with sulfur encapsulated in pipes and flow of gaseous HTF (air) in the shell side. However, for lower-temperature IPH applications in the range of approximately 100-300 degrees Celsius Element 16 adopted a compact and scalable TES design with molten sulfur in the shell and HTF pipes submerged in the molten sulfur bath. The low-cost molten sulfur TES for dispatchable IPH has deployment potential for broad applications. The spatial and temporal evolution of the HTF and sulfur temperature is critical to the TES system performance, and thus detailed modeling can improve understanding of the performance and facilitate design improvements. Using high performance computing and computational fluid dynamics (CFD) a low-cost molten sulfur thermal energy storage (TES) system for industrial process heating (IPH) applications was developed. The unique challenges in CFD modeling of sulfur TES are the sharp property changes of sulfur relevant to the working temperatures. Above 159, liquid sulfur undergoes polymerization, and the viscosity of sulfur rapidly increases by several orders of magnitude between 159 degrees Celsius and 188 degrees Celsius, followed by a decrease in viscosity beyond 188 degrees Celsius due to thermal bound dissociation. In addition, various concentrations of H2S impurities can also modify sulfur viscosity. This numerical challenge is especially relevant to transient simulation of the sulfur TES charging and discharging processes as the extreme property variations limit the applicability of traditional heat transfer correlations. Transient CFD simulations including the temperature-dependent sulfur properties and geometric complexity of the TES design were used to predict the effect of natural convection during charging and discharging on the heat transfer process, sulfur temperature uniformity, charge/discharge rates, and performance of the storage devices. The CFD model was validated with experimental results for a full charge and discharge cycle. The work will show 3D and 2D simulation comparisons aimed to facilitate rapid design iterations and a machine learning based design optimization approach.

CFD↗

Solid composites containing polymeric matrix with carbon fibers embedded therein

A functionalized carbon fiber having covalently bound on its surface a partially cured epoxy or amine-containing sizing agent, wherein at least a portion of epoxide or amine groups in the sizing agent are available as uncrosslinked epoxide or amine groups, which corresponds to a curing degree of epoxide or amine groups of no more than about 0.6. Composites comprised of these functionalized carbon fibers embedded in a polymeric matrix are also described. Methods for producing the functionalized carbon fibers and composites thereof are also described.

36 MATERIALS SCIENCE↗

Power Electronics Materials and Bonded Interfaces - Reliability and Lifetime

Advanced packaging technologies are currently being designed and developed by the power electronics industry however, the maximum operating temperature is still limited to 175 degrees Celsius for the silicon carbide devices. Bonded materials such as sintered copper and polymeric materials are potential candidates for high temperature operation, but it is critical to characterize and evaluate its reliability under harsh operating conditions. In this project, we discuss the results of the accelerated experiments conducted on sintered copper and polymeric materials. Additionally, a novel framework to develop the lifetime prediction model of bonded interfaces through employing statistical and machine learning models are described. In this task, scanning acoustic microscope images of bonded interfaces obtained under thermal cycling experiments are used as the data.

ENGINEERING↗

A Rapid Survey of the Compatibility of Selected Seal Materials with Conventional and Semi-Synthetic JP-8

Since the synthesis of a liquid hydrocarbon fuel from coal by Franz Fischer and Hans Tropsch in 1923, there has been cyclic interest in developing this fuel for military and commercial applications. In recent years the U.S. Department of Defense has taken interest in producing a unified battlespace fuel using the Fischer Tropsch (FT) process for a variety of reasons including cost, quality, and logistics. In the past year there has been a particular emphasis on moving quickly to demonstrate that an FT fuel can be used in the form of a blend with conventional petroleum-derived jet fuel. The initial objective is to employ this semi-synthetic fuel with blend ratios as high as 50 percent FT with longer range goals to use even high blend ratios and ultimately a fully synthetic jet fuel. A significant concern associated with the use of a semi-synthetic jet fuel with high FT blend ratios is the effect these low aromatic fuels will have on fuel-wetted polymeric materials, most notably seals and sealants. These materials typically swell and soften to some degree when exposed to jet fuel and the aromatic content of these fuels contribute to this effect. Semi-synthetic jet fuels with very low aromatic contents may cause seals and sealants to shrink and harden leading to acute or chronic failure. Unfortunately, most of the material qualification tests are more concerned with excessive swelling than shrinkage and there is little guidance offered as to an acceptable level of shrinkage or other changes in physical properties related to low aromatic content. Given the pressing need for guidance data, a program was developed to rapidly survey the volume swell of selected fuel-wetted materials in a range of conventional and semi-synthetic jet fuels and through a statistical analysis to make a determination as to whether there was a basis to be concerned about using fuels with FT blend ratios as high as 50 percent. Concurrent with this analysis data was obtained as to the composition of the fuel absorbed in fuel-wetted materials through the use of GC-MS analysis of swollen samples as well as other supporting data. In this presentation the authors will present a summary of the results of the volume swell and fuel absorbed by selected O-rings and sealants as well as a description of the measurement protocols developed for this program.

Graham, John L.↗

Vacuum Baking To Remove Volatile Materials

Outgassing reduced in some but not all nonmetallic materials. Eleven polymeric materials tested by determining outgassing species as temperature of conditioned and unconditioned materials raised to 300 degrees C. Conditioning process consisted of vacuum bake for 24 hours at 80 degrees C in addition to usual cure. Baking did not change residual gas percentage of water molecules.

Muscari, J. A.↗

Polyenamines for Films, Coatings, and Adhesives

Easy process makes polymers with good mechanical properties. Synthesis involves Michael-type addition polymerization of two diacetylenic diketones, with various aromatic diamines in m-cresol at 60 to 130 degrees C. Technique provides synthetic route to high-molecular-weight polyenamines with moderate thermal stability and good mechanical properties. Polyenamines produced exhibit potential for use as films, coatings, adhesives, molding compounds, and composite matrices.

Hergenrother, Paul M.↗

Stretchable and wearable polymeric heaters and strain sensors fabricated using liquid metals

Wearable electronic devices (WEDs) are receiving significant attention because of the increasing interest in soft robotics, electronic skin, and wearable sensors. Liquid metals (LMs) are compelling for WEDs owing to their metallic conductivity, fluidic nature, and low toxicity. For this study, we fabricated stretchable and soft WEDs using LM (eutectic gallium-indium alloy) wires (LMWs) patterned via force wetting through custom-made stencils on an elastic substrate. LMWs can generate thermal energy via Joule heating upon current application and deliver it to the substrate, resulting in wearable polymeric heaters. The LM mixed with carbonyl iron particles (CIPs) can also be patterned while preserving fluidic behavior. The degree of thermal energy generated through the LMWs can be manipulated as a function of the CIP concentration in the LM and geometrical factors of the electrode patterns, i.e., width and length. An elastic film patterned with LMWs attached to the human body exhibits changes in the effective electrical resistance depending on applied strain, demonstrating potential as a wearable strain sensor. This LM utilized WED that can generate thermal energy upon current application through the LMWs and detect the bodily motion has significant potential for application in wearable thermotherapy, electronic skin, and soft sensors.

47 OTHER INSTRUMENTATION↗

Plasma polymerization of an ethylene-nitrogen gas mixture

A procedure has been developed whereby nitrogen can be incorporated into an organic film from an ethylene-nitrogen gas mixture using an internal electrode capacitively coupled radio frequency reactor. The presence of nitrogen has been shown directly by infrared transmittance spectra and electron spectroscopic chemical analysis data, and further indirect evidence was provided by dielectric measurements and by the reverse osmosis properties of the film. Preparation of a nitrogen containing film did not require vapor from an organic nitrogen containing liquid monomer. Some control over the bonding and stoichiometry of the polymer film was provided by the added degree of freedom of the nitrogen partial pressure in the gas mixture. This new parameter strongly affected the dielectric properties of the plasma polymerized film and could affect the reverse osmosis behavior.

Hudis, M.↗

Command of active and responsive elastomers by topological defects and patterns

The project resulted in the development of stimuli-responsive elastomer coatings formed by photopolymerized liquid crystal molecules. The molecular orientation of the liquid crystal elastomers is coupled to rubber-like elasticity. The project developed an approach to produce complex patterns of molecular orientation in elastomers by employing photopatterning technique based on plasmonic metamasks that convert unpolarized incoming light into a transmitted light beam with spatially-varying linear polarization. The polarization-modulated light beam aligns the film of azodye molecules, which serves as the substrate for liquid crystal elastomer coating. The alignment of the azodye molecules follows the polarization pattern with a phase shift of the alignment direction by 90 degrees. The azodye substrate imposes orientation of molecules in the adjacent liquid crystal layer which is preserved after the monomers are polymerized into a liquid crystal elastomer. By using differently aligned substrates one could produce various patterns of molecular orientation in the elastomer, which dictate the mechanical properties of the elastomers and their response to external stimuli such as temperature, humidity, and ultraviolet irradiation. In particular, the predesigned molecular orientation produces deterministically defined topography response of the liquid crystal coatings, in which their free surface changes from flat to either locally elevated or locally compressed, depending on whether the pre-inscribed molecular orientation is predesigned with a splay or bend deformation. The research established that the mechanism of this deterministic relation between the dynamic topography and pre-inscribed molecular orientation is rooted in the change of the tensorial order parameter that characterizes the degree of orientational order, and in the contraction/expansion of polymer molecules in response to the order parameter changes. In particular, lowering the order causes contraction of polymer globules. The work demonstrated that the dynamic topography of elastomer coatings with three-dimensional pattern of orientational order includes up and down motion of the material (along the normal to the coating) and also shifts in lateral directions. We demonstrate that the deterministic relationship between the orientational patterns and variations of coatings’ profile is caused by forces that are mathematically equivalent to active forces in the system of “pullers” or “pushers” in active matter, demonstrating universality of the out-of-equilibrium behavior. The project resulted in theoretical models that predictively describe the dynamic response of coatings. The topography of liquid crystal elastomers is sensitive to stimuli such as temperature, ultraviolet irradiation, and humidity. The applicability of the patterned approach to produce dynamic coatings was expanded from nematic elastomers to their smectic counterparts. The project combined a battery of imaging techniques to unveil the dynamic properties of the coatings, ranging from the state-of-the-art dynamic holographic microscopy to fluorescent confocal polarizing microscopy and polscope microscopy. The research uncovered potential applications of dynamic elastomer coatings, such as control placement of colloidal particles, engineering of living tissues with alignment patterns of cells that follow the orientational order of elastomer coatings. The approach developed in the project can be used to design programmable dynamic coatings with functionalities that mimic biological tissues such as skin.

36 MATERIALS SCIENCE↗

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 ↗

Calcium Sulfate and Calcium Carbonate Scaling of Thin-Film Composite Polyamide Reverse Osmosis Membranes with Surface-Tethered Polyacrylic Acid Chains

The gypsum and calcite scaling propensities of the thin-film composite polyamide (PA-TFC) reverse osmosis (RO) membrane, modified with a tethered surface layer of polyacrylic acid (PAA) chains, was evaluated and compared to the scaling of selected commercial RO membranes. The tethered PAA layer was synthesized onto a commercial polyamide membrane (i.e., base-PA) via atmospheric pressure plasma-induced graft polymerization (APPIGP). The PAA nano-structured (SNS) base-PA membrane (SNS-PAA-PA) was scaled to a lesser degree, as quantified by a lower permeate flux decline and surface imaging, relative to the tested commercial membranes (Dow SW30, Toray SWRO, and BWRO). The cleaning of gypsum-scaled membranes with D.I. water flushing achieved 100% water permeability recovery for both the SNS-PAA-PA and Dow SW30 membranes, relative to 92–98% permeability restoration for the Toray membranes. The calcium carbonate scaling of SNS-PAA-PA membranes was also lower relative to the commercial membranes, but permeability recovery after D.I. water cleaning was somewhat lower (94%) but consistent with the level of surface scale coverage. In contrast, the calcite and gypsum-scaled membrane areas of the commercial membranes post-cleaning were significantly higher than for the SNS-PAA-PA membrane but with 100% permeability recovery, suggesting the potential for membrane damage when mineral scaling is severe.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Hydrocarbon polymeric binder for advanced solid propellant

A series of DEAB initiated isoprene polymerizations were run in the 5-gallon stirred autoclave reactor. Polymerization run parameters such as initiator concentration and feed rate were correlated with the molecular weight to provide a basis for molecular weight control in future runs. Synthetic methods were developed for the preparation of n-1,3-alkadienes. By these methods, 1,3-nonadiene was polymerized using DEAB initiator to give an ester-telechelic polynonadiene. This was subsequently hydrogenated with copper chromite catalyst to give a hydroxyl terminated saturated liquid hydrocarbon prepolymer having greatly improved viscosity characteristics and a Tg 18 degrees lower than that of the hydrogenated polyisoprenes. The hydroxyl-telechelic saturated polymers prepared by the hydrogenolysis of ester-telechelic polyisoprene were reached with diisocyanates under conditions favoring linear chain extension gel permeation chromatography was used to monitor this condensation polymerization. Fractions having molecular weights above one million were produced.

Potts, J. E.↗