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DOE OSTI2026

Tuning Thermal Stability through Dopant Size in Chemically Doped DPP–Thiophene Polymers

Molecular doping of conjugated polymers (CPs) is a key strategy for improving the performance of organic electronics devices, particularly thermoelectrics. Doped donor–acceptor (D–A) conjugated polymers, characterized by a tunable energy gap between the Fermi level and the transport band, show great promise in achieving high electrical conductivity (σ) while preserving a favorable Seebeck coefficient (S). Despite the promising performance enhancement of chemically doped D–A polymers, their thermal stability remains largely underexplored, a crucial consideration for the long-term operation of organic thermoelectric devices. In this study, we investigated the dopant size-dependent thermal stability of a diketopyrrolopyrrole-thiophene (DPP-T) D–A copolymer, utilizing two p-dopants: 2,3,5,6-tetrafluoro-7,7,8,8-tetracyanoquinodimethane (F 4 TCNQ) and Mo(tfd-CO 2 Me) 3 . Temperature-dependent UV–vis–NIR spectroscopy revealed that DPP-T/F 4 TCNQ is more prone to dedoping under a high temperature thermal stress than DPP-T/Mo(tfd-CO 2 Me) 3 . Although the F 4 TCNQ doped polymer shows higher initial in-plane conductivity than its Mo(tfd-CO 2 Me) 3 counterpart, it undergoes a conductivity loss of more than an order of magnitude after annealing at 120 °C for 30 min. In contrast, the in-plane conductivity of DPP-T/Mo(tfd-CO 2 Me) 3 remains stable under the same thermal conditions. Thermogravimetric analysis ruled out dopant sublimation as a primary contributor to dedoping, leading us to attribute the conductivity loss in F 4 TCNQ-doped DPP-T to dopant phase separation and migration. This observation was further confirmed by X-ray scattering studies and nanoscale infrared microscopy and spectroscopy studies. This work could provide further insights into the thermal stability of doped conjugated polymers and suggests that incorporating bulkier dopants is an effective strategy to enhance the thermal robustness of doped DPP-type systems.

Conjugated polymers↗

DOE OSTI2020

Influence of Metal-Alkyls on Early-Stage Ethylene Polymerization over a Cr/SiO 2 Phillips Catalyst: A Bulk Characterization and X-ray Chemical Imaging Study

The Cr/SiO 2 Phillips catalyst has taken a central role in ethylene polymerization since its invention in 1953. The uniqueness of this catalyst is related to its ability to produce broad molecular weight distribution (MWD) PE materials as well as that no co-catalysts are required to attain activity. Nonetheless, co-catalysts in the form of metal-alkyls can be added for scavenging poisons, enhancing catalyst activity, reducing the induction period, and tailoring polymer characteristics. The activation mechanism and related polymerization mechanism remain elusive, despite extensive industrial and academic research. Here, we show that by varying the type and amount of metal-alkyl co-catalyst, we can tailor polymer properties around a single Cr/SiO 2 Phillips catalyst formulation. Furthermore, we show that these different polymer properties exist in the early stages of polymerization. We have used conventional polymer characterization techniques, such as size exclusion chromatography (SEC) and 13 C NMR, for studying the metal-alkyl co-catalyst effect on short-chain branching (SCB), long-chain branching (LCB) and molecular weight distribution (MWD) at the bulk scale. In addition, scanning transmission X-ray microscopy (STXM) was used as a synchrotron technique to study the PE formation in the early stages: allowing us to investigate the produced type of early-stage PE within one particle cross-section with high energy resolution and nanometer scale spatial resolution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Tandem pyrolysis evolved gas–gas chromatography–mass spectrometry

Analysis of byproducts from thermal degradation of polymer materials provides a wealth of information about a materials’ composition, thermal stability, degradation mechanisms, and kinetics. However, regardless of the instrumentation used, only limited information is obtainable from a single experiment. Microfurnace technology, when interfaced to a gas chromatography-mass spectrometry (GC-MS), can be used to obtain both thermal and chemical information via evolved gas analysis-MS (EGA-MS) and GC-MS analysis modes. While both EGA-MS and Py-GC-MS are valuable when characterizing polymer materials, at least two experiments on distinct samples are required, which can be a liability for clear interpretation of results from inhomogeneous samples. Here, we seek to overcome this limitation by combining EGA-MS and Py-GC-MS modes in a single experimental setup. Further, this was done by developing new gas line modifications to allow for tandem Pyrolysis Evolved Gas-Gas Chromatography-Mass Spectrometry (Py/EG-GC-MS) analysis. Verification of Py/EG-GC-MS analysis was performed using a polystyrene standard. Results demonstrate successful Py/EG-GC-MS analysis for the first-time showing the potential of these modifications for application in areas where sample is limited or direct correlation of products to the thermal profile is desirable such as in forensics or product-specific kinetics.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Surface-Functionalized Cellulose Nanocrystals as Nanofillers for Crosslinking Processes: Implications for Thermosetting Resins

Understanding the response of fillers in the epoxy resin crosslinking process and characterizing polymer–filler dynamics are the key features that guide the engineering of new thermosetting resin composites. Here, in this work, X-ray photon correlation spectroscopy (XPCS) is used as a thermal analysis tool to track the microscopic changes occurring during the cure of a functionalized cellulose nanocrystal (mCNC)–epoxy composite. In contrast, traditional methods such as differential scanning calorimetry (DSC) and curing rheology are used to understand the kinetics and properties on macroscopic length scales. Of interest is the influence of the mCNC on the curing kinetics and properties of the thermosetting resin. Two levels of modification (increasing hydrophobicity) were chosen to observe the effect of functionalization. Before cure, the highly functionalized CNC (mCNC3) shows a 44% increase in complex viscosity (η*), while the less functionalized CNC (mCNC2) shows a η* value similar to that of the neat resin. As the cure cycle progresses, results from DSC, rheology, and XPCS further show the enhancement in dispersion for mCNC3. The results show a clear difference in the maximum drift velocity, maximum heat flow, and complex viscosity during the ramp to the isothermal cure temperature (T cure ). Such results suggest that mCNC3 contains a well-dispersed network of particles due to the higher level of functionalization. During T cure , a transition in elastic modulus (G') occurs only for the highly functionalized CNC particle system. We believe that heat-induced aggregation occurs, and the crosslinked resin ultimately dominates the macroscopic properties of the final cured system for all samples. The results from the three techniques are in good agreement and showcase XPCS as a beneficial experimental tool for characterizing the microscopic dynamics of particulate-filled thermosetting resins. Hence, we envision this to be a fundamental curing study for the design of thermosetting resin composites.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Measurement of moisture-dependent ion diffusion constants in wood cell wall layers using time-lapse micro X-ray fluorescence microscopy

Our future bioeconomy depends on increased utilization of renewable lignocellulosic biomass. Controlling the diffusion of chemicals, such as inorganic ions, within secondary plant cell walls is central to many biomass applications. However, insufficient understanding of intra-cell-wall diffusion within secondary plant cell walls is hindering the advancement of many lignocellulosic biomass applications. In this work, X-ray fluorescence microscopy was used to measure diffusion constants of K + , Cu 2+ , and Cl - diffusing through loblolly pine (Pinus taeda) cell wall layers under 70%, 75%, or 80% relative humidity (RH). Results revealed that diffusion constants increased with RH, the larger Cu 2+ diffused more slowly than the K + , and the Cl - diffusion constant was the same as that for the counter cation, indicating cations and anions diffused together to maintain charge neutrality. Comparison with electrical conductivity measurements showed that conductivity is being controlled by ion mobility over these RH. The results further support that intra-cell-wall diffusion of inorganic ions is a Fickian diffusion process occurring through rubbery amorphous polysaccharides, which contradicts previous assertions that intra-cell-wall diffusion is an aqueous process occurring through water pathways. Researchers can now utilize polymer science approaches to engineer the molecular architecture of lignocellulosic biomass to optimize properties for specific end uses.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2023

Electronic properties and optical spectra of donor–acceptor conjugated organic polymers

Organic semiconductors based on conjugated donor-acceptor (D–A) polymers are a unique platform for electronic, spintronic, and energy-harvesting devices. Understanding the electronic structure of D–A polymers with a small band gap is essential for developing next-generation technologies. Here, we investigate the electronic structure and optical spectra of cyclopentadithiophene-based closed/open-shell D–A polymers using density functional theory and the Bethe–Salpeter equation based on G 0 W 0 approximation. We explored the role of different acceptor units and chemical substitutions on the structural changes and, more importantly, electronic, optical, and dielectric behavior. We found that the computed first exciton peak of the polymers agreed well with the available experimentally measured optical gap. Furthermore, D–A polymers with open-shell character display higher dielectric constant than the closed-shell polymers. We show that the exceptional performance of polycyclopentadithiophene-thiophenylthiadiazoloquinoxaline (PCPDT-TTQ) as a scalable n-type material for Faradaic supercapacitors can be partly ascribed to its elevated dielectric constant. Consequently, these D–A polymers, characterized by their high dielectric constants, exhibit significant potential for various applications, including energy storage, organic electronics, and the production of dielectric films.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Sustainable Polymer for Polyolefin Replacement (CRADA Final Report)

Sustainable Chemicals, LLC (Participant, Sust-Chem) develops renewable, biodegradable bioplastics for the replacement of large-volume petrochemical plastics such as polyethylene (PE) and polypropylene (PP). Participant’s patented bioplastics will find use in everyday items such as plastic bags, flexible containers, packaging, and toys and will address customers' ask for goods that are sustainable but don't cost a premium. Participants’ plastic comes from plant biomass and at the end of its lifecycle, is compostable or chemically recyclable. During the CRADA, Participant and Contractor will jointly refine the polymerization process used to make our bioplastic. Participant and Contractor will focus on technologies that are economically and industrially feasible, complete with full polymer characterization.

36 MATERIALS SCIENCE↗

NASA NTRS1979

Space radiation effects on composite matrix materials - Analytical approaches

In-vacuo ultraviolet and gamma radiation exposure tests are utilized in a study aimed at the identification of radiation damage mechanisms in composite materials, with the objective of predicting the long-term behavior of composite structures in a space environment at geosynchronous orbit. Physical and chemical methods of polymer characterization are utilized for the study of composite matrix degradation, in conjunction with GC/MS techniques for the analysis of volatile by-products.

Giori, C.↗

NASA NTRS1999

Experimental and Analytical Studies for a Computational Materials Program

The studies supported by Grant NAG1-1780 were directed at providing physical data on polymer behavior that would form the basis for computationally modeling these types of materials. Because of ongoing work in polymer characterization this grant supported part of a larger picture in this regard. Efforts went into two combined areas of their time dependent mechanical response characteristics: Creep properties on the one hand, subject to different volumetric changes (nonlinearly viscoelastic behavior) and time or frequency dependence of dilatational material behavior. The details of these endeavors are outlined sufficiently in the two appended publications, so that no further description of the effort is necessary.

Knauss, W. G.↗

NASA NTRS2003

Structural Evolution and Mechanical Properties of PMR-15/Layered Silicate Nanocomposites

In the first year of this research, we successfully synthesized and characterized Polymer/ Layered Silicate nanocomposite using the polyimide PMR-15 as the polymer and several layered silicate nanoparticles. We have scaled up the process to allow fabrication of monoliths using these nanocomposites. The morphology of these systems was found to evolve during processing to an exfoliated structure for one system and intercalated for the rest. Correlation with Transmission Electron Microscopy studies is underway. Dynamic mechanical analysis (DMA) results showed a significant increase in the thermomechanical properties (E' and E'') of 2.5 wt.% clay loaded nanocomposites in comparison to the neat polyimide. Increasing the clay loading to 5 wt.% decreased these properties. Higher glass transition temperatures were observed for 2.5 wt.% nanocomposites compared to the neat polyimide. A lower coefficient of thermal expansion was observed only for the PGV/PMR-15 nanocomposite. An improvement in the flexural properties (modulus, strength and elongation) was observed for the 2.5 wt.% nanocomposite but not for the 5 wt.% nanocomposites. The improved barrier properties polymer/ silicate nanocomposites suggest that moisture uptake should be decreased for PMR-15 nanocomposites. The results of some recent experiments to examine delineate the ability of the silicate nanoparticles in improving the hydrolytic degradation of PMR-15 will be discussed.

Campbell, Sandi↗

NASA NTRS1987

Dynamic characterization of viscoelastic polymer solutions in a lubricated cylinder - Plate apparatus

The characterization of several viscoelastic lubricants which are oil or water based has been studied in an apparatus consisting of a lubricated cylinder-plate contact. The friction loads were measured as a function of speed. The experimental results show the influence of the molecular weight and of the concentration of the polymeric additive as well as the influence of the viscosity of the oil-base on the load and friction coefficient. Also a test for mechanical degradation was performed on the polymer solutions. Several additives can favor a viscoelastic lubrication.

Doremus, P.↗

NASA NTRS2010

Physical and Electrical Characterization of Aluminum Polymer Capacitors

Polymer aluminum capacitors from several manufacturers with various combinations of capacitance, rated voltage, and ESR values were physically examined and electrically characterized. The physical construction analysis of the capacitors revealed three different capacitor structures, i.e., traditional wound, stacked, and laminated. Electrical characterization results of polymer aluminum capacitors are reported for frequency-domain dielectric response at various temperatures, surge breakdown voltage, and other dielectric properties. The structure-property relations in polymer aluminum capacitors are discussed.

Liu, David↗

DOE OSTI2026

Comprehensive structural characterization of charged polymers involved in moisture-driven direct air capture

This study provides a comprehensive structural characterization of commercially available alkaline anion-exchange polymers (Fumasep FAA-3 and IRA 900) used in moisture-driven direct air capture (DAC) of carbon dioxide. Using X-ray diffraction, SAXS/WAXS, atomic force microscopy, FIB-SEM, and transmission electron microscopy, the authors identify nanoscale clustering, porosity, swelling behavior, and humidity-dependent structural changes that influence CO₂ adsorption and release. These findings establish structure–function relationships critical for designing more durable and energy-efficient DAC polymer materials.

36 MATERIALS SCIENCE↗

NASA NTRS1995

Polarization and Characterization of Piezoelectric Polymers

Piezoelectric materials exhibit an electrical response, such as voltage or charge, in reaction to a mechanical stimuli. The mechanical stimuli can be force, pressure, light, or heat. Therefore, these materials are excellent sensors for various properties. The major disadvantage of state of the art piezoelectric polymers is their lack of utility at elevated temperatures. The objective of this research is to study the feasibility of inducing piezoelectricity in high performance polymer systems. The three aspects of the research include experimental poling, characterization of the capacitance, and demonstration of the use of a piezoelectric polymer as a speaker.

Bodiford, Hollie N.↗

NASA NTRS1982

Characterization and degradation studies on synthetic polymers for aerospace application

The anti-misting additive for jet fuels known as FM-9 (proprietary polymer) was characterized by elemental analysis, solubility studies and molecular weight determination. Physical properties of surface tension, viscosity, specific gravity and other physical parameters were determined. These results are compared with properties of polyisobutylene and fuels modified with the same; the misting characteristics of polyisobutylene and FM-9 in Jet A fuel are included. Characterization and degradation of phthalocyanine and its derivatives were accomplished by use of a mass spectrometer and a pyroprobe solid pyrolyzer. Metal phthalocyanine tetracarboxylic acids and phthalocyanine-tetraamine cured epoxies were studied. Epoxy/graphite composite panels were exposed to a NASA-Ames radiant panel fire simulator in the flaming and non-flaming modes; toxic gases of HCN and HZS were measured along with oxygen, Co2, Co, and organic gases.

Hsu, M. T. S.↗

NASA NTRS1991

Characterization of selected LDEF polymer matrix resin composite materials

The characterization of selected graphite fiber reinforced epoxy (934 and 5208) and polysulfone (P1700) matrix resin composite materials which received 5 years and 10 months of exposure to the LEO environment on the Long Duration Exposure Facility is reported. Resin loss and a decrease in mechanical performance as well as dramatic visual effects were observed. However, chemical characterization including infrared, thermal, and selected solution property measurements showed that the molecular structure of the polymeric matrix had not changed significantly in response to this exposure. The potential effect of a silicon-containing molecular contamination of these specimens is addressed.

Young, Philip R.↗

NASA NTRS2005

Characterization of Polymer-Coated MEMS Humidity Sensors for Flight Applications

Under NASA's Aviation Safety Program (AvSP), in addition to wind velocity and temperature, water vapor is considered one key factor in determining aviation weather, which is a substantial contributor to many general aviation (GA) accidents. The conventional and reliable humidity measuring methods such as radiation reflection or absorption have relatively high cost in addition to highly specialized operating and maintenance characteristics. This paper presents characterizations of inexpensive MEMS and capacitance type humidity sensors for their potential use on aircraft. If installed, these sensors are subjected to ambient environmental conditions as well as to different chemicals and deicing fluids used on aircraft. This paper reports the effect of different deicing fluids and chemicals on these inexpensive humidity sensors.

Shams, Qamar A.↗

NASA NTRS2015

Additive Manufacturing and Characterization of Ultem Polymers and Composites

The objective of this project was to conduct additive manufacturing to produce aircraft engine components by Fused Deposition Modeling (FDM), using commercially available polyetherimides - Ultem 9085 and experimental Ultem 1000 mixed with 10 percent chopped carbon fiber. A property comparison between FDM-printed and injection-molded coupons for Ultem 9085, Ultem 1000 resin and the fiber-filled composite Ultem 1000 was carried out. Furthermore, an acoustic liner was printed from Ultem 9085 simulating conventional honeycomb structured liners and tested in a wind tunnel. Composite compressor inlet guide vanes were also printed using fiber-filled Ultem 1000 filaments and tested in a cascade rig. The fiber-filled Ultem 1000 filaments and composite vanes were characterized by scanning electron microscope (SEM) and acid digestion to determine the porosity of FDM-printed articles which ranged from 25-31 percent. Coupons of Ultem 9085 and experimental Ultem 1000 composites were tested at room temperature and 400 degrees Fahrenheit to evaluate their corresponding mechanical properties.

Polymers↗