Outgassing rates of two solid rocket fuels in vacuum
Outgassing rate measurements on stored composite fuels of polybutadiene acrylic acid and polyurethane binders
COMPOSITE PROPELLANT↗
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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
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Impact of melt viscosity on filler dispersion in elastomeric nanocomposites
Compounding of commercial nanocomposites usually involves the addition of viscosity enhancers such as binder resins in ink jet inks, and paints. Contrary to this, plasticizers such as process oils are added to reduce the melt viscosity and ease processability of reinforced elastomers. Nanofillers such as silica and carbon black are typically added to reinforce rubber and enhance performance of automotive tire treads. Filler dispersion has traditionally been qualitatively (indirectly) assessed by measuring the properties of reinforced elastomers. While dispersion can be quantified by examining filler agglomeration through surface roughness measurements and microscopy, the size-scale dependence for these hierarchical fillers has usually been ignored. Here, we have recently devised a method to quantify nano-scale dispersion of fillers using Ultra small-angle X-ray scattering (USAXS) techniques. This method is advantageous since it directly links the controllable processing/compounding parameters such as the mixing speed, mixer geometry, residence time (or mixing duration), melt density, flow gap distance, and melt viscosity to nano-scale dispersion. While our previous studies have explored the impact of different processing parameters, this study specifically investigates the impact of melt viscosity on nano-scale filler dispersion in elastomer compounds. Commercially available polybutadienes with different Mooney viscosities were used in conjunction with different grades and amounts of process oils to modify the melt viscosity.
Carbon black↗
Designing a Block Copolymer Membrane for Selective Transport of Lactic Acid from Aqueous Mixtures
We report the design and synthesis of a triblock copolymer-based membrane for enabling selective transport of lactic acid from aqueous solutions. This is relevant to the production of polylactic acid, one of the few biodegradable and biobased polymers with sufficient mechanical strength for practical applications. The end blocks are positively charged with negatively charged lactate counterions. The middle block is polybutadiene (PBD). Due to microphase separation, the charged blocks form channels for transporting lactic acid. The mechanical integrity of the membrane is controlled by cross-linking the PBD block. Transport of lactic acid and water across the membrane was studied by placing the membrane between two chambers, a feed chamber containing aqueous lactic acid solutions, and a receiving chamber containing pure water. The lactic acid concentration in the receiving chamber was monitored as a function of time using conductivity, HPLC, and NMR. The corresponding flux of water from the receiving chamber to the feed chamber was measured using an NMR-based approach. The lactic acid and water permeabilities through our membrane were (1.12 ± 0.05) × 10–8 and (8.58 ± 0.75) × 10–9 cm2 s–1. To our knowledge, there are no reports of lactic acid permeabilities through any membrane in the literature. The separation factor of our membrane, αLA/water, 1.305 ± 0.123, is comparable to that of membranes used for selective transport of ethanol, despite the fact that lactic acid is a much larger molecule than ethanol. Selective transport of lactic acid in our membrane is governed mainly by differences in solubility; lactic acid is 18 times more soluble in the membrane than water.
Jana, Rounak↗
Tuning Copolymer Microstructure Using Ring-Opening Cross-Metathesis Polymerization
The capability of ring-opening cross-metathesis (RO/CM) polymerization to produce alternating copolymers was studied. By treating commercial polybutadiene (PB) with bulky oxanorbornene monomers and Ru-based olefin metathesis catalysts, alternating copolymers were produced under mild conditions with high sequence fidelities. Here, we found that alternating copolymers could be produced starting from a variety of butadiene sources including PB, cyclooctadiene (COD), or t,t,t-1,5,9-cyclododecatriene (CDT), highlighting for the first time the kinetic pathway independence of this process. Kinetic copolymerization analysis of an oxanorbonene monomer with CDT revealed that much higher monomer conversions were obtained compared with the analogous homopolymerizations and showed evidence of alternating monomer incorporation. Copolymerization of these monomers also enabled good control when targeting different molecular weights. Copolymer thermal analysis revealed a strong correlation between thermal behavior and alternating sequence fidelity, providing a second lever beyond composition to tune thermal behavior. These data demonstrate that a broad variety of polymer microstructures can be accessed via RO/CM polymerization and highlight the potential of CDT in alternating copolymer synthesis.
Foster, Jeffrey C. [Oak Ridge National Laboratory ↗
How Topological Polymer Loops on the Nanoparticle Surface Control the Mechanical Properties of Nanocomposites
Carbon black (CB) and silica (SiO 2 ) filled elastomers are known to be the most successful polymer nanocomposites (PNCs) in industry, where “bound rubber (BR)” (i.e., polymer chains that are physically or chemically adsorbed on the nanofiller surface) plays a critical role in their reinforcement. Here, we report a molecular-scale mechanism underlying the “BR-induced reinforcement” by integrating neutron scattering experiments and molecular dynamics simulations. Simplified non-cross-linked SiO 2 -filled polybutadiene (PB) and CB-filled PB reveal the critical role of topological polymer loops in the BR for the enhanced mechanical performance. The average loop size on the SiO 2 surface modified with a silane coupling agent is much smaller than that on the CB surface and the loops on the SiO 2 surface are densely formed, preventing interdigitation with the matrix chains. On the other hand, the larger, uncrowded loops formed on the CB surface facilitate the interdigitation with the matrix polymer chains even near the filler surface. In this way, a strong connectivity is established between a matrix and a nanofiller, resulting in an adhesive filler–polymer interface. Furthermore, our findings shed light on rich and complex physics and materials design problems in PNCs, where the topological polymer structure on the nanofiller surface directly controls the macroscopic mechanical properties.
36 MATERIALS SCIENCE↗
One Step Block-like Copolymers from an Upcycled Monomer Using Ring-Opening Metathesis Polymerization
Block-like copolymers can be readily synthesized in one step using monomers with widely separated reactivity ratios. Here, we show that trans,trans,trans-1,5,9-cyclododecatriene (CDT), produced from polybutadiene via cyclodepolymerization (CDP), undergoes gradient copolymerization via ring-opening metathesis polymerization (ROMP) with a selected norbornene monomer to produce a block-like copolymer that exhibits bulk nanophase separation and excellent thermomechanical performance. These data highlight a new ROMP copolymerization system with a sharp compositional drift and introduce a simple pathway to convert waste plastic into a valuable building block for high-value thermoplastic materials.
block copolymer↗
Scalable, biologically sourced depolymerizable polydienes with intrinsically weakened carbon–carbon bonds
Currently, there are few examples of circularly recyclable polymers with all-carbon backbones, probably owing to the challenge of using selective C–C bond cleavage to efficiently produce monomers in recycling processes. Furthermore, here we demonstrate a series of biologically sourced polymuconate polymers synthesized via simple free-radical polymerization that exhibit intrinsically weakened C–C bonds and controlled chemical recycling to monomers. Modifying the side chains and copolymerization ratios allows a wide range of mechanical property tuning, achieving performances comparable to those of commercial plastics such as polystyrene, polymethyl methacrylate and polybutadiene. Techno-economic analysis and life cycle assessment for production at a scale of 100 kilotons per year show that the materials are currently slightly more expensive and environmentally intensive compared with conventional rubbers. However, use of recycled materials via depolymerization can greatly decrease the cost and environmental impacts of polymuconate production (for example, down to US$1.59 per kilogram) to outperform its commercial counterparts.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Study of solution properties of block copolymers Final report
Solution properties of polybutadiene and polystyrene block copolymers
Simha, R.↗
Photochemistry of unsaturated polymers
Radiation induced photochemical reactions in polyisoprene and polybutadiene thin films including microstructural changes
Golub, M. A.↗
Influence of chemical nature on flow behavior of polymers. I - Shear rate and temperature dependence
Low molecular weight liquid polybutadiene polymer flow behavior as function of shear rate, temperature, molecular structure and hydrogen bonding
Bauer, W. H.↗
HTPB propellants for large booster applications
Solid propellants based on low cost hydroxyl terminated polybutadiene binders meeting burning rate, mechanical properties and processing requirements for large booster motors
Bankaitis, H.↗
Effects of normal acceleration on transient burning rate augmentation of an aluminized solid propellant
Instantaneous burning rate data for a polybutadiene acrylic acid propellant, containing 16 weight percent aluminum, were calculated from the pressure histories of a test motor with 96.77 sq cm of burning area and a 5.08-cm-thick propellant web. Additional acceleration tests were conducted with reduced propellant web thicknesses of 3.81, 2.54, and 1.27 cm. The metallic residue collected from the various web thickness tests was characterized by weight and shape and correlated with the instantaneous burning rate measurements. Rapid depressurization extinction tests were conducted in order that surface pitting characteristics due to localized increased burning rate could be correlated with the residue analysis and the instantaneous burning rate data. The acceleration-induced burning rate augmentation was strongly dependent on propellant distance burned, or burning time, and thus was transient in nature. The results from the extinction tests and the residue analyses indicate that the transient rate augmentation was highly dependent on local enhancement of the combustion zone heat feedback to the surface by the growth of molten residue particles on or just above the burning surface. The size, shape, and number density of molten residue particles, rather than the total residue weight, determined the acceleration-induced burning rate augmentation.
Northam, G. B.↗
Development of the Algol III solid rocket motor for SCOUT.
The design and performance of a motor developed for the first stage of the NASA SCOUT-D and E launch vehicles are discussed. The motor delivers a 30% higher total impulse and a 35 to 45% higher payload mass capability than its predecessor, the Algol IIB. The motor is 45 in. in diameter, has a length-to-diameter ratio of 8:1 and delivers an average 100,000-lb thrust for an action time of 72 sec. The motor design features a very high volumetrically loaded internal-burning charge of 17% aluminized polybutadiene propellant, a plasma-welded and heat-treated steel alloy case, and an all-ablative plastic nose liner enclosed in a steel shell. The only significant development problem was the grain design tailoring to account for erosive burning effects which occurred in the high-subsonic-Mach-number port. The tests performed on the motor are described.
Felix, B. R.↗
Effects of the acceleration vector on transient burning rate of an aluminized solid propellant.
Experimental results concerning the transient burning-rate augmentation of a 16% aluminum polybutadiene acrylic acid (PBAA) propellant burned in a 2-in. web motor at pressure levels from 300 to 1200 psia with centrifugal accelerations from 0 to 140 g. The orientation of the acceleration vector was varied to determine its effect on the transient burning rate. The burning-rate augmentation was strongly dependent on (1) acceleration level, (2) propellant distance burned (or burn time), and (3) orientation of the acceleration vector with respect to the burning surface. This transient rate augmentation resulted from the retention of molten metallic residue on the burning surface by the normal acceleration loading. The presence of the residue altered the combustion zone heat transfer and caused increased localized burning rates, as evidenced by the pitted propellant surfaces that were observed from extinction tests conducted at various acceleration levels.
Northam, G. B.↗
Lipid-absorbing Polymers
The removal of bile acids and cholesterol by polymeric absorption is discussed in terms of micelle-polymer interaction. The results obtained with a polymer composed of 75 parts PEO and 25 parts PB plus curing ingredients show an absorption of 305 to 309%, based on original polymer weight. Particle size effects on absorption rate are analyzed. It is concluded that crosslinked polyethylene oxide polymers will absorb water, crosslinked polybutadiene polymers will absorb lipids; neither polymer will absorb appreciable amounts of lipids from micellar solutions of lipids in water.
Marsh, H. E., Jr.↗
New polymer systems: Chain extension by dianhydrides
Three anhydrides provide effective chain extension of hydroxy-terminated polyalkylene oxides and polybutadienes. Novel feature of these anhydride reactants is that they are difunctional as anhydrides, but they are tetrafunctional if conditions are selected that lead to total esterification or reaction of all carboxyl groups.
Rhein, R. A.↗
A study of the effects of solid phase reactions on the thermal degradation and ballistic properties of solid propellants
The thermal stability of perchlorate composite propellants was studied at 135 and 170 C. The experimental efforts were concentrated on determining the importance of heterogeneous oxidizer-fuel reactions in the thermal degradation process. The experimental approach used to elucidate the mechanisms by which the oxidizer fuel composites thermally degrade was divided into two parts: (1) keeping the fuel constant and varying the nature of the oxidizers, and (2) holding the oxidizer constant and varying the fuel components. The fuel component primarily utilized in the first phase was polyethylene. Oxidizers included KClO4, KClO3, NH4ClO4 and NH4ClO4 doped with materials such as chlorate, phosphate and arsenate. In the second phase the oxidizer used was primarily NH4ClO4 while the fuels included saturated and unsaturated polybutadiene prepolymers and a series of bonding agents. Techniques employed in the current study include thermogravimetric measurements, differential thermal analysis, infrared, mass spectrometry, electron microscopy, and appropriate wet chemical analysis.
Schmidt, W. G.↗
Development of procedures for calculating stiffness and damping properties of elastomers in engineering applications. Part 2: Elastomer characteristics at constant temperature
Dynamic properties of a commerical polybutadiene compound were determined at a constant temperature of 32 C by a forced-vibration resonant mass type of apparatus. The constant thermal state of the elastomer was ensured by keeping the ambient temperature constant and by limiting the power dissipation in the specimen. Experiments were performed with both compression and shear specimens at several preloads (nominal strain varying from 0 to 5 percent), and the results are reported in terms of a complex stiffness as a function of frequency. Very weak frequency dependence is observed and a simple power law type of correlation is shown to represent the data well. Variations in the complex stiffness as a function of preload are also found to be small for both compression and shear specimens.
Gupta, P. K.↗