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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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At least 163 records · Page 9
All sourcesNASA NTRSDOE OSTI
NASA NTRS2004

Lightweight Stacks of Direct Methanol Fuel Cells

An improved design concept for direct methanol fuel cells makes it possible to construct fuel-cell stacks that can weigh as little as one-third as much as do conventional bipolar fuel-cell stacks of equal power. The structural-support components of the improved cells and stacks can be made of relatively inexpensive plastics. Moreover, in comparison with conventional bipolar fuel-cell stacks, the improved fuel-cell stacks can be assembled, disassembled, and diagnosed for malfunctions more easily. These improvements are expected to bring portable direct methanol fuel cells and stacks closer to commercialization. In a conventional bipolar fuel-cell stack, the cells are interspersed with bipolar plates (also called biplates), which are structural components that serve to interconnect the cells and distribute the reactants (methanol and air). The cells and biplates are sandwiched between metal end plates. Usually, the stack is held together under pressure by tie rods that clamp the end plates. The bipolar stack configuration offers the advantage of very low internal electrical resistance. However, when the power output of a stack is only a few watts, the very low internal resistance of a bipolar stack is not absolutely necessary for keeping the internal power loss acceptably low.

Narayanan, Sekharipuram↗
DOE OSTI2022

IER 555: Godiva Benchmark Update CED-2 (Final Design Report)

The International Criticality Safety Benchmark Evaluation Project (ICSBEP) evaluation of the Godiva IV critical assembly, HEU-MET-FAST-086: GODIVA-IV DELAYED-CRITICAL EXPERIMENTS (HMF-086), was completed by Russ Mosteller. Five critical experiment configurations performed at the Los Alamos National Laboratory (LANL) Technical Area (TA)-18 were evaluated as acceptable benchmark cases. The five cases consist of four delayed critical configurations which differ in control rod positions and one prompt critical configuration. All cases calculated a lower $k_{eff}$ than measured by experiment. This data is referred to as the TA-18 Godiva IV benchmark in this report. In 2005, Godiva IV was disassembled for relocation to the Nevada Test Site (NTS), now Nevada National Security Site (NNSS), at the National Criticality Experiments Research Center (NCERC). Following the disassembly and subsequent reassembly and startup of Godiva IV at NCERC, additional information about the Godiva IV components was obtained. An errata note was added to the HMF-086 evaluation in the ICSBEP handbook to provide this new information until a revision to the benchmark evaluation could be performed. In addition to those corrections, there are differences between the Godiva IV assembly at TA-18 and the Godiva IV assembly at NCERC. These differences include both assembly-specific differences (differences in the safety block gap, differences in the control rod positions, a new NCERC Top Hat and contamination shield) as well as environmental differences, such as the size and shape of the experimental building where the assembly is located. An additional model with similar cases, referred to as the NCERC Godiva IV benchmark in this report, will be added to the revised HMF-086 to capture these additional differences. This will provide the best benchmark model of Godiva for use by those performing experiments at NCERC. The IER 555 CED-2 report documents the information that will be updated in the HMF-086 revision, both the corrections to the TA-18 Godiva IV benchmark and the subsequent changes to create a NCERC Godiva IV benchmark. It describes the measurements that will be performed for cases similar to those performed at TA-18. It also describes measurements that will be included in the evaluation as additional data.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
NASA NTRS1984

The Design and Use of Subtasks in Part Training and Their Relationship to the Whole Task

The part versus whole training is discussed. Common sense dictates that a massive body of knowledge should not be taught as a whole. For the same reason, if a part of the task is very difficult, one should not go over the task in its entirety. Repetitive training on the difficult part should lead to better results. Several part training methods were developed, including: pure part, progressive part, repetitive part, retrogressive and isolated parts. The question was posited whether training on parts of a task is a beneficial enterprise. The way the task will be disassembled for the part training needs to be determined. It is argued that the effectiveness of part training depends on the degree to which a task is decomposable.

Mane, A. M.↗
NASA NTRS2001

Space Shuttle Main Engine Joint Data List Applying Today's Desktop Technologies to Facilitate Engine Processing

Boeing-Rocketdyne's Space Shuttle Main Engine (SSME) is the world's first large reusable liquid rocket engine. The space shuttle propulsion system has three SSMEs, each weighing 7,400 lbs and providing 470,000 lbs of thrust at 100% rated power level. To ensure required safety and reliability levels are achieved with the reusable engines, each SSME is partially disassembled, inspected, reassembled, and retested at Kennedy Space Center between each flight. Maintenance processing must be performed very carefully to replace any suspect components, maintain proper engine configuration, and avoid introduction of contaminants that could affect performance and safety. The long service life, and number, complexity, and pedigree of SSME components makes logistics functions extremely critical. One SSME logistics challenge is documenting the assembly and disassembly of the complex joint configurations. This data (joint nomenclature, seal and fastener identification and orientation, assembly sequence, fastener torques, etc.) must be available to technicians and engineers during processing. Various assembly drawings and procedures contain this information, but in this format the required (practical) joint data can be hard to find, due to the continued use of archaic engineering drawings and microfilm for field site use. Additionally, the release system must traverse 2,500 miles between design center and field site, across three time zones, which adds communication challenges and time lags for critical engine configuration data. To aid in information accessibility, a Joint Data List (JDL) was developed that allows efficient access to practical joint data. The published JDL has been a very useful logistics product, providing illustrations and information on the latest SSME configuration. The JDL identifies over 3,350 unique parts across seven fluid systems, over 300 joints, times two distinct engine configurations. The JDL system was recently converted to a web-based, navigable electronic manual that contains all the required data and illustrations in expanded view format using standard PC products (Word, Excel, PDF, Photoshop). The logistics of accurately releasing this information to field personnel was greatly enhanced via the utilization of common office products to produce a more user-friendly format than was originally developed under contract to NASA. This was done without reinventing the system, which would be cost prohibitive on a program of this maturity. The brunt of the joint part tracking is done within the logistics organization and disseminated to all field sites, without duplicating effort at each site. The JDL is easily accessible across the country via the NASA intranet directly at the SSME workstand. The advent of this logistics data product has greatly enhanced the reliability of tracking dynamic changes to the SSME and greatly reduces engineering change turnaround time and potential for errors. Since the inception of the JDL system in 1997, no discrepant parts have propagated to engine assembly operations. This presentation focuses on the challenges overcome and the techniques used to apply today's desktop technologies to an existing logistics data source.

Jacobs, Kenneth↗
NASA NTRS1989

Using multiple sensors for printed circuit board insertion

As more and more activities are performed in space, there will be a greater demand placed on the information handling capacity of people who are to direct and accomplish these tasks. A promising alternative to full-time human involvement is the use of semi-autonomous, intelligent robot systems. To automate tasks such as assembly, disassembly, repair and maintenance, the issues presented by environmental uncertainties need to be addressed. These uncertainties are introduced by variations in the computed position of the robot at different locations in its work envelope, variations in part positioning, and tolerances of part dimensions. As a result, the robot system may not be able to accomplish the desired task without the help of sensor feedback. Measurements on the environment allow real time corrections to be made to the process. A design and implementation of an intelligent robot system which inserts printed circuit boards into a card cage are presented. Intelligent behavior is accomplished by coupling the task execution sequence with information derived from three different sensors: an overhead three-dimensional vision system, a fingertip infrared sensor, and a six degree of freedom wrist-mounted force/torque sensor.

Sood, Deepak↗
NASA NTRSDate not supplied

Experimental and CFD Investigation of the Titled Jet Behavior in the Zero Boil-Off Tank (ZBOT) Experiment

Screens are used in cryogenic storage tanks to diffuse the incoming gas or liquid injection/flow into the tank. Meshed screens were also used in the jet mixing pressure control tests of the Zero Boil-Off Tank (ZBOT) Experiment which was recently performed aboard the International Space Station (ISS). The ZBOT pressure control studies used a liquid jet that was intended to be aligned with the longitudinal axis of the tank. A cartridge consisting of a honeycomb flow straightener and two screen diffusers, one upstream of the honeycomb, and one downstream, were designed to obtain the desired velocity profile in a manner that would be consistent in all the tests and could also be used as an input to the CFD simulations. Unfortunately, during the flight operations, the Digital Particle Image Velocimetry (DPIV) measurements indicated that the jet actually exited the nozzle at an angle to the main axis. This unexpected tilt affected the motion and deformation of the ullage during the pressure control tests, influencing the initial pressure drops. Upon disassembling the experiment hardware, it was discovered that the screen diffuser upstream of the honeycomb was clogged with debris. Since this behavior is important, not only to the follow-on ZBOT-NC experiment, but also to the operation of cryogenics storage tanks in general, a series of ground-based experiments and parametric CFD model simulations were performed to understand and characterize the tilted flow in terms of the clogged area of the upstream screen and the jet velocity. The experimental and CFD results surprisingly and non-intuitively showed that although the modification of the flow originated from the clogging of the upstream screen, the presence of the downstream unclogged screen was also necessary to produce the tilted jet. Two different CFD models were used for the numerical simulations, and only the one using a porous media formulation to capture the screen pressure drop was able to produce the correct tilting behavior. Parametric runs with the porous media CFD model were used to characterize the jet tilt in terms of the blockage area and jet velocity for both the future ZBOT-NC Experiment and other propellant tank applications. Supported by NASA Biological & Physical Sciences (BPS) Division, Physical Sciences Research Program, NASA HQ, USA.

Cryogenic Fluid Management↗
NASA NTRS1985

Nickel-hydrogen Cell Test Program Summary

Three prototype 50 ampere-hour (Ah) nickel-hydrogen cells of the Air Force Wright Aeronautical Laboratories (AWFAL) design were cycled to failure. A summary of the life cycling tests and failure analyses of the cells are presented. The cells were cycled in a simulated low earth orbit regime at depths of discharge ranging from 25 to 80 percent. Trend data, such as end of discharge voltage and cell capacity, was recorded during test. Cells 1, 2, and 3 completed 17167, 2473, and 10080 charge/discharge cycles, respectively, prior to failure. All failed due to internal shorts, and were disassembled to determine cause of failure.

Mueller, V. C.↗
NASA NTRS2023

The Assembly, Test, and Integration of LOFTID (Low-Earth Orbit Flight Test of an Inflatable Decelera-tor)

R.J. Bodkin Biography Mr. Bodkin worked in industry for a rapid prototype company focusing on UAVs and manned experimental aircraft. Later he served as the Inflation System Lead on IRVE-II and 3 and the Re-Entry Vehicle Lead for LOFTID at NASA Langley Research Center. Introduction: The Low-Earth Orbit Flight Test of an Inflatable Decelerator (LOFTID), developed in partnership with United Launch Alliance (ULA) and flown in conjunction with the National Oceanic and Atmospheric Administration (NOAA) Joint Polar Satellite System-2 (JPSS-2) satellite, demonstrated Hypersonic Inflatable Aerodynamic Decelerator (HIAD) technology has progressed and is ready for mission infusion. LOFTID’s success demonstrates that aeroshells are not limited to the internal diame-ter of the launch vehicle payload fairing, allowing larger payloads to be deployed to the surfaces of planetary bodies with atmospheres. The challenges of assembling, integrating, and testing this revolutionary spacecraft will be dis-cussed as well as issues associated with doing this with a fixed launch date the project did not control. Assembly: Because LOFTID flew as a rideshare partner with JPSS-2, it was constrained with addi-tional schedule, milestone, and technical require-ments that were beyond the project’s control. As-sembly of the LOFTID hardware was challenged with the normal mechanical fit issues while also having to navigate the SARS-COVID-II pandemic. Challenges ranged from availability of team per-sonnel required on-site for vehicle assembly to dif-ficulties associated with team collaboration while working remotely and increased costs and lead times of components due to supply chain con-straints. Numerous additional challenges cascaded from the additional time required. Integration: LOFTID flew as a secondary pay-load to JPSS-2 in a mission-unique configuration, directly under JPSS-2 primary payload, inside the Payload Adapter that integrated JPSS-2 to the Atlas V launch vehicle. A mission unique Payload Adapt-er Separation System (PASS) was required to sepa-rate the Payload Adapter from the Launch Vehicle prior to the start of the LOFTID flight demonstra-tion. Development of this system was challenging due to a shortened development schedule resulting from the iterative nature of Payload Adapter devel-opment with the partners at ULA. Preparations to integrate the main segments of the LOFTID vehicle posed unique challenges of having to accommodate issues with a fixed launch date that led to some cre-ative solutions to the integration. The partnership agreement with ULA and JPSS-2 resulted in a mass simulator designed to be installed late in the inte-gration in the event the LOFTID vehicle was not ready in time.. Test: LOFTID testing was carried out in several phases. Some components were tested at the com-ponent level, others at the sub-system levels and then finally the integrated vehicle level. This culmi-nated with the Complete Systems Test (CST) per-formed in a vacuum chamber as one of the final checkouts prior to disassembly for re-packing of the aeroshell. CST challenges will be discussed as well as obstacles encountered post-CST. After CST, the vehicle was disassembled so the HIAD could be repacked, and the vehicle was reassembled for ac-ceptance vibration testing. Testing concluded with the fully assembled vehicle being shipped to the launch site for final testing and integrations with the Payload Adapter to JPSS-2 for launch and opera-tions. Conclusion: The challenges posed by the AI&T for LOFTID could inform the planetary community of some of the opportunities and challenges of de-veloping technologies on a rideshare with a rela-tively small budget.

R.J. Bodkin↗
NASA NTRS2014

End-of-Test Performance and Wear Characterization of NASA's Evolutionary Xenon Thruster (NEXT) Long-Duration Test

The NASA's Evolutionary Xenon Thruster (NEXT) program is developing the next-generation solar electric ion propulsion system with significant enhancements beyond the state-of-the-art NASA Solar Electric Propulsion Technology Application Readiness (NSTAR) ion propulsion system to provide future NASA science missions with enhanced capabilities. A Long-Duration Test (LDT) was initiated in June 2005 to validate the thruster service life modeling and to quantify the thruster propellant throughput capability. Testing was recently completed in February 2014, with the thruster accumulating 51,184 hours of operation, processing 918 kg of xenon propellant, and delivering 35.5 MN-s of total impulse.As part of the test termination procedure, a comprehensive performance characterization was performed across the entire NEXT throttle table. This was performed prior to planned repairs of numerous diagnostics that had become inoperable over the course of the test. After completion of these diagnostic repairs in November 2013, a comprehensive end-of-test performance and wear characterization was performed on the test article prior to exposure to atmosphere. These data have confirmed steady thruster performance with minimal degradation as well as mitigation of numerous life limiting mechanisms encountered in the NSTAR design. Component erosion rates compare favorably to pretest predictions based on semi-empirical models used for the thruster service life assessment. Additional data relating to ion beam density profiles, facility backsputter rates, facility backpressure effects on thruster telemetry, and modulation of the neutralizer keeper current are presented as part of the end-of-test characterization. Presently the test article for the NEXT LDT has been exposed to atmosphere and placed within a clean room environment, with post-test disassembly and inspection underway.

wear tests↗
NASA NTRS2001

MPLM On-Orbit Interface Dynamic Flexibility Modal Test

Now that the International Space Station (ISS) is being constructed, payload developers have to not only verify the Shuttle-to-payload interface, but also the interfaces their payload will have with the ISS. The Multi Purpose Logistic Module (MPLM) being designed and built by Alenia Spazio in Torino, Italy is one such payload. The MPLM is the primary carrier for the ISS Payload Racks, Re-supply Stowage Racks, and the Resupply Stowage Platforms to re-supply the ISS with food, water, experiments, maintenance equipment and etc. During the development of the MPLM there was no requirement for verification of the on-orbit interfaces with the ISS. When this oversight was discovered, all the dynamic test stands had already been disassembled. A method was needed that would not require an extensive testing stand and could be completed in a short amount of time. The residual flexibility testing technique was chosen. The residual flexibility modal testing method consists of measuring the free-free natural frequencies and mode shapes along with the interface frequency response functions (FRF's). Analytically, the residual flexibility method has been investigated in detail by, MacNeal, Martinez, Carne, and Miller, and Rubin, but has not been implemented extensively for model correlation due to difficulties in data acquisition. In recent years improvement of data acquisition equipment has made possible the implementation of the residual flexibility method as in Admire, Tinker, and Ivey, and Klosterman and Lemon. The residual flexibility modal testing technique is applicable to a structure with distinct points (DOF) of contact with its environment, such as the MPLM-to-Station interface through the Common Berthing Mechanism (CBM). The CBM is bolted to a flange on the forward cone of the MPLM. During the fixed base test (to verify Shuttle interfaces) some data was gathered on the forward cone panels. Even though there was some data on the forward cones, an additional modal test was performed to better characterize its behavior. The CBM mounting flange is the only remaining structure of the MPLM that no test data was available. This paper discusses the implementation of the residual flexibility modal testing technique on the CBM flange and the modal test of the forward cone panels.

Bookout, Paul S.↗
NASA NTRS1990

Single launch lunar habitat derived from an NSTS external tank

A concept for using the spent external tank from a National Space Transportation System (NSTS) to derive a lunar habitat is described. The external tank is carried into low Earth orbit where the oxygen tank-intertank subassembly is separated from the hydrogen tank, berthed to Space Station Freedom and the subassembly outfitted as a 12-person lunar habitat using extravehicular activity (EVA) and intravehicular activity (IVA). A single launch of the NSTS orbiter can place the external tank in LEO, provide orbiter astronauts for disassembly of the external tank, and transport the required subsystem hardware for outfitting the lunar habitat. An estimate of the astronauts' EVA and IVA is provided. The liquid oxygen intertank modifications utilize existing structures and openings for man access without compromising the structural integrity of the tank. The modifications include installation of living quarters, instrumentation, and an airlock. Feasibility studies of the following additional systems include micrometeoroid and radiation protection, thermal control, environmental control and life support, and propulsion. The converted lunar habitat is designed for unmanned transport and autonomous soft landing on the lunar surface without need for site preparation. Lunar regolith is used to fill the micrometeoroid shield volume for radiation protection using a conveyer. The lunar habitat concept is considered to be feasible by the year 2000 with the concurrent development of a space transfer vehicle and a lunar lander for crew changeover and resupply.

King, Charles B.↗
DOE OSTI2020

Dilute and Dispose Cost Estimate for Equipment Installation per the LCCE

As directed in the Consolidation Appropriations Act, 2016, the National Nuclear Security Administration (NNSA) initiated the preconceptual design and development of a Lifecycle Cost Estimate for the Surplus Plutonium Disposition (SPD) Dilute and Dispose Program. Based on August 2016 Program Requirements Document and subsequent supplemental guidance, LANL prepared the Lifecycle Cost Estimate under key assumptions that meet the program’s requirements. For Dilute and Dispose, the program would disposition surplus Pu by diluting oxide produced at LANL with inhibitor materials, packaging the materials in containers, and shipping the containers to a deep geologic repository for permanent disposal. The base assumption is that LANL would disassemble pits, convert the Pu metal to oxide, and characterize and package the material for shipment to SRS, where it would be diluted prior to geologic disposal at the WIPP site in New Mexico. Another major assumption for the Dilute and Dispose option is that LANL would increase the current oxide production rate (or throughput) to 1500 kg/year, 5 times higher than the maximum annual production of ~300 Kgs executed by the ARIES Oxide Production Program at LANL. Analysis based on the ARIES program’s throughput model revealed that 15 pieces of equipment would need to be installed within PF-4 and certain facility improvements would need to be accomplished in order to meet the desired throughput levels. The additional equipment would be essentially identical to equipment already used within PF-4 for existing operations.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1984

Reusable rocket engine turbopump condition monitoring

Significant improvements in engine readiness with reductions in maintenance costs and turn-around times can be achieved with an engine condition monitoring systems (CMS). The CMS provides health status of critical engine components, without disassembly, through monitoring with advanced sensors. Engine failure reports over 35 years were categorized into 20 different modes of failure. Rotor bearings and turbine blades were determined to be the most critical in limiting turbopump life. Measurement technologies were matched to each of the failure modes identified. Three were selected to monitor the rotor bearings and turbine blades: the isotope wear detector and fiberoptic deflectometer (bearings), and the fiberoptic pyrometer (blades). Signal processing algorithms were evaluated for their ability to provide useful health data to maintenance personnel. Design modifications to the Space Shuttle Main Engine (SSME) high pressure turbopumps were developed to incorporate the sensors. Laboratory test fixtures have been designed for monitoring the rotor bearings and turbine blades in simulated turbopump operating conditions.

Hampson, M. E.↗
NASA NTRS2016

Wire Rope Failure on the Guppy Winch

On January 6, 2016 at El Paso, the Guppy winch motor was changed. After completion of the operational checks, the load bar was being reinstalled on the cargo pallet when the motor control FORWARD relay failed in the energized position. The pallet was pinned at all locations (each pin has a load capacity of 16,000 lbs.) while the winch was running. The wire rope snapped before aircraft power could be removed. After disassembly, the fractured wire rope was shipped to ES4 lab for further characterization of the wire rope portion of the failure. The system was being operated without a clear understanding of the system capability and function. The proximate cause was the failure of the K48 -Forward Winch Control Relay in the energized position, which allowed the motor to continuously run without command from the hand controller, and operation of the winch system with both controllers connected to the system. This prevented the emergency stop feature on the hand controller from functioning as designed. An electrical checkout engineering work instruction was completed and identified the failed relay and confirmed the emergency stop only paused the system when the STOP button on both connected hand controllers were depressed simultaneously. The winch system incorporates a torque limiting clutch. It is suspected that the clutch did not slip and the motor did not stall or overload the current limiter. Aircraft Engineering is looking at how to change the procedures to provide a checkout of the clutch and set to a slip torque limit appropriate to support operations.

Figert, John↗
DOE OSTI2023

Carbon Scaffold Architectures for Stable Lithium Metal Anodes

In light of the skyrocketing demand for electric vehicles and consequent need for high-performing lithium-ion batteries, there has been significant research into the creation of a battery with a lithium metal anode due to its high theoretical capacity and energy density. Unfortunately, nonuniform lithium deposition and consequent dendrite growth diminish performance and pose a safety risk. To combat this, lightweight carbon scaffolds are being developed to stabilize the electric field of these batteries and induce uniform deposition through rational design at the nano-, micro-, and meso- scales. However, there is a paucity of research on the impacts of macroscale scaffold topology on lithium cycling performance. Here, we report the creation of two graphite-based scaffolds with distinct 3D topologies: one a series of triangular prisms and one a series of rectangular prisms. Coin cells were made using these scaffolds and cycled at a current of 1mA/cm2 for 50 cycles to test the performance. The triangular topology was found to outperform the rectangular topology in terms of both potential magnitude and stability during cycling. Disassembling the cells revealed more even lithium deposition on the rectangular scaffold; however, some of the rectangular prisms were broken while all the triangular prisms remained intact. Last, future experiments are proposed regarding the scaffold spacing and mass of the cells in order to isolate the topological impact.

25 ENERGY STORAGE↗
NASA NTRS1991

The application of statistically designed experiments to resistance spot welding

State-of-the-art Resistance Spot Welding (RSW) equipment has the potential to permit realtime monitoring of operations through advances in computerized process control. In order to realize adaptive feedback capabilities, it is necessary to establish correlations among process variables, welder outputs, and weldment properties. The initial step toward achieving this goal must involve assessment of the effect of specific process inputs and the interactions among these variables on spot weld characteristics. This investigation evaluated these effects through the application of a statistically designed experiment to the RSW process. A half-factorial, Taguchi L sub 16 design was used to understand and refine a RSW schedule developed for welding dissimilar aluminum-lithium alloys of different thickness. The baseline schedule had been established previously by traditional trial and error methods based on engineering judgment and one-factor-at-a-time studies. A hierarchy of inputs with respect to each other was established, and the significance of these inputs with respect to experimental noise was determined. Useful insight was gained into the effect of interactions among process variables, particularly with respect to weldment defects. The effects of equipment related changes associated with disassembly and recalibration were also identified. In spite of an apparent decrease in equipment performance, a significant improvement in the maximum strength for defect-free welds compared to the baseline schedule was achieved.

Hafley, Robert A.↗
DOE OSTI2021

Kinetically Controlled Formation of Semi-crystalline Conjugated Polymer Nanostructures

Conjugated polymer (CP) materials that are considered as an attractive choice for various electronic and optoelectronic applications possess highly heterogeneous complex structures that can span several orders of magnitude in length scale. This is due to the intricate coupling effects of weak secondary interactions and entropic forces that determine molecular organization in bulk polymer materials. Understanding the influence of molecular interactions on the emergence and evolution of nano- and microscale structures is of paramount importance to the guided design and development of condensed CP materials. Such understanding is even more critical for the rational design of hierarchical systems away from equilibrium, where weak molecular interactions can guide the system along competing kinetic pathways toward local energy minima and metastable architectures. In this work, we studied a promising concept for accessing various kinetically stabilized semi-crystalline CP nanostructures that are formed in the process of controlled chain-growth Kumada catalyst-transfer polymerization initiated by a small-molecule catalytic species which can exist in equilibrium between free and aggregated states. Specifically, we chose a small-molecule perylenedicarboximide (PDCI) polymerization catalytic initiator which has a strong tendency toward reversible supramolecular assembly–disassembly that can be controlled by temperature. Addition of a thiophene monomer to a solution of the PDCI initiator starts the chain-growth polymerization process, which produces distinct nanoscale semi-crystalline polythiophene structures formed under predominant kinetic control. Furthermore, we demonstrated that, depending on the reaction temperature (which affects the fine balance between the position of PDCI assembly–disassembly equilibrium, rate of polymerization, and solvent–solute interactions for the growing polythiophene chains), a range of kinetically trapped hierarchically organized semi-crystalline CP systems with substantially varying optoelectronic properties could be obtained. In addition to spectroscopic and electron microscopic studies, in order to better reveal the structural aspects of the generated polymer nanoscale systems, we carried out a series of X-ray diffraction and neutron scattering experiments which indicated complex hierarchical organization in these kinetically stabilized CP assembled materials. We expect that this in situ polymerization-based approach can lead to a general way to expand access to various semi-crystalline CP nanostructured materials with broadly tunable electronic and optical properties.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗