PYROLYSIS OF NEW FLUOROPOLYMERS
Volatilization and decomposition of fluoropolymers determined by pyrolysis
PYROLYSIS↗
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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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HALAR fluoropolymer: A versatile insulation material
Research directed toward developing materials for the wire and cable industry has resulted in a new product, E-CTFE copolymer, which has an outstanding combination of electrical, thermal, and mechanical properties. The properties of E-CTFE are discussed and compared with those of other commercial fluoropolymers. Particular attention is given to the utility of E-CTFE as a wire and cable insulation.
Robertson, A. B.↗
The Acute Inhalation Toxicity in Rats from the Pyrolysis Products of Four Fluoropolymers
Male Sprague-Dawley rats (225?250 g) were exposed to the thermal degradation products from four fluoropolymers. The three polymers containing vinylidene fluoride and hexafluoropropene (VF2/HFP) were pyrolyzed at 550? and 800?C, whereas polytetrafluoroethylene (PTFE) was pyrolyzed at 625 and 800?C. At the lower temperatures, the pyrolysate from the copolymer of vinylidene fluoride and hexafluoropropene (VF2/HFP) was less toxic than the pyrolysates from either the terpolymer of vinyidene fluoride, hexafluoropropene, and tetrafluoroethylene (VF2/HFP/TFE) or the copolymer of vinylidene fluoride and hexafluoropropene with ?additives? (VF2/HFP-A). However, the pyrolysates from the VF2/HFP-containing materials produced less toxic products than the pyrolysate from PTFE at 625?C. When the pyrolysis temperature was increased to 800?C, very little difference was noted between the pyrolysis toxicity for any of the VF2/HFP-containing polymers with the most toxic pyrolysate again produced by PTFE. Carbon monoxide levels were all sublethal. No correlation could be established between hydrolyzable fluoride levels and the lethality of the pyrolysates. Death following exposure occurred within 48 hr due to acute pulmonary edema and hemorrhage. Survival of this acute phase was followed by alveolar lymphocytic infiltration and peribronchial tissue proliferation.
Carter, V. L., Jr.↗
Flexible fluoropolymer filled protective coatings
Metal oxide films such as SiO2 are known to provide an effective barrier to the transport of moisture as well as gaseous species through polymeric films. Such thin film coatings have a tendency to crack upon flexure of the polymeric substrate. Sputter co-deposition of SiO2 with 4 to 15 percent fluoropolymers was demonstrated to produce thin films with glass-like barrier properties that have significant increases in strain to failure over pure glass films which improves their tolerance to flexure on polymeric substrates. Deposition techniques capable of producing these films on polymeric substrates are suitable for durable food packaging and oxidation/corrosion protection applications.
Banks, Bruce A.↗
Reactively Deposited Aluminum Oxide and Fluoropolymer Filled Aluminum Oxide Protective Coatings for Polymers
Reactive ion beam sputter deposition of aluminum simultaneous with low energy arrival of oxygen ions at the deposition surface enables the formation of highly transparent aluminum oxide films. Thick (12 200 A), adherent, low stress, reactively deposited aluminum oxide films were found to provide some abrasion resistance to polycarbonate substrates. The reactively deposited aluminum oxide films are also slightly more hydrophobic and more transmitting in the UV than aluminum oxide deposited from an aluminum oxide target. Simultaneous reactive sputter deposition of aluminum along with polytetrafluoroethylene (PTFE Teflon) produces fluoropolymer-filled aluminum oxide films which are lower in stress, about the same in transmittance, but more wetting than reactively deposited aluminum oxide films. Deposition properties, processes and potential applications for these coatings will be discussed.
Rutledge, Sharon K.↗
Fluoropolymer Films Deposited by RF Plasma Sputtering of Polytetrafluoroethylene Using Inert Gases
The FT-IR (Fourier Transform Infrared), UV (Ultraviolet) and XPS (X Ray Photoelectron Spectroscopy) spectra of fluoropolymer films (SPTFE) deposited by rf (radio frequency) plasma sputtering of polytetrafluoroethylene (PTFE), using Ne, Kr and Xe as sputtering gases, were obtained and compared with prior spectra for SPTFE formed using He and Ar. The F/C (fluorine / carbon) ratios for SPTFE films (1.44-1.55), obtained at a rf power of 10 W, were essentially the same for all five rare gases, there being no trend of decreasing fluorine content in the SPTFE product with increasing atomic weight of the sputtering gas - contrary to the momentum transfer notion advanced by M. E. Ryan, et al. Increasing rf power from 10 to 50 W resulted in successively lower F/C ratios for SPTFE (e.g., from 1.55 to 1.21 in the case of Xe plasma-sputtered PTFE), accompanied by sputtering of the glass reactor and deposition of fragments of sodium aluminum silicate occurring at 40 W and above. In order to achieve a "Teflon-like" SPTFE structure (i.e., products with as high a F/C ratio as possible) in a given plasma reactor, an optimum rf power must be found, which in the present case was approximately 10 W.
Golub, Morton A.↗
Potential SSP Perfluorooctanoic Acid Related Fluoropolymer Materials Obsolescence
The Shuttle Environmental Assurance Initiative (SEA) has identified a potential for the Space Shuttle Program (SSP) to incur materials obsolescence issues due to agreements between the fluoro-chemical industry and the United States Environmental Protection Agency (USEPA) to participate in a Global Stewardship Program for perfluorooctanoic acid (PFOA). This presentation will include discussions of the chemistry, regulatory drivers, affected types of fluoropolymer and fluoroelastomer products, timeline for reformulations, and methodology for addressing the issue. It will cover the coordination of assessment efforts with the International Space Station and Head Quarters Air Force Space Command, along with some examples of impacted materials. The presentation is directed at all members of the international aerospace community concerned with identifying potential environmentally driven materials obsolescence issues.
Segars, Matt G.↗
Giant piezoelectricity in fluoropolymer fiber mats achieved by corona poling in water
Polymer piezoelectrics hold great potential for energy harvesting and wearable electronics. Efforts have been dedicated to enhancing piezoelectric coefficients and thermostability for several decades, but most of these have not been successful. In this report, we demonstrate a straightforward way to achieve high piezoelectric coefficients and output voltages while maintaining high thermostability at temperatures over 110 °C. Poly(vinylidene fluoride-co-trifluoroethylene) [P(VDF-TrFE)] 80/20 mol.% nanofiber mats (made by electrospinning) with extremely high crystallinity and Curie temperatures were obtained via a two-step annealing process, from which large ferroelectric domains were formed in extended-chain crystals. After corona poling using water, which is a high dielectric constant medium, giant piezoelectricity (apparent d 33 = 1045 ± 20 pC/N) and high output voltages (29.9 ± 0.5 V) were achieved. It is found that the dimensional effect induced significant polarization changes, which is the key requirement for piezoelectricity. Our finding in this work paves a way to further improve high-performance polymer piezoelectrics.
36 MATERIALS SCIENCE↗
Unveiling the Reactivity of Fluoropolymers with Sodium Metal: Mechanistic Insights and Battery Implications
Poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) has broad applications across various metal-ion battery systems, such as a binder for electrodes, a supporting matrix for electrolytes, and a separator material. Due to its excellent mechanical properties, PVDF-HFP has become an excellent candidate for fabricating gel and solid-state electrolytes in sodium-based batteries. However, in this study, we noticed notable side reactions occurring at the interface of PVDF-HFP membranes and Na metal. These reactions not only alter chemical compositions but also further affect the surface morphology and adhesive properties of membranes. Similar phenomena are observed in other polyfluoroalkyl-based membranes (PVDF and PTFE). Therefore, we systematically studied the reaction mechanisms between the Na metal and these polymers. The influence of different functional groups (−F, −CF 3 , −H) and their arrangement on the reaction extent has also been discussed. Finally, we concluded with the key factors driving these side reactions and provided new perspectives for designing polymers tailored for sodium-based batteries.
Interfacial side reactions↗
Predicting the viscoplastic response of a crystallizing fluoropolymer using transient network theory
We employ a molecular theory of dynamic polymer networks to describe the viscoplastic response of rubbery FK-800, a thermoplastic copolymer of chlorotrifluoroethylene and vinylidene fluoride, over a broad range of thermal histories. The kinetics of crystallization at different annealing temperatures was modeled using a modified Avrami equation, whose parameters were found to evolve through simple relationships over the full temperature range of the rubbery state. By fitting experimental compression data, we discovered predictable trends for the physical parameters in our mechanical model over its full range of crystallinities (up to ≈20%) and provided insights based on molecular-level physics to justify them. Using this, an end-to-end model was developed to predict the yielding and post-yield behavior of rubbery FK-800 for arbitrary thermal histories. The model successfully predicted the highly nonlinear evolution of characteristic mechanical signatures (stiffness, yield point, post-yield drop) throughout the crystallization process. A statistical analysis of variance test was employed to determine that the measured variations in the mechanical behavior of rubbery FK-800 are primarily dictated by its fractional crystallinity, regardless of its exact thermal history.
36 MATERIALS SCIENCE↗
Utilization of oxygen difluoride for syntheses of fluoropolymers
The reaction oxygen difluoride, OF2, with ethylenically unsaturated fluorocarbon compounds is examined. Depending upon the fluorocarbon material and reaction conditions, OF2 can chain extend fluoropolyenes, convert functional perfluorovinyl groups to acyl fluoride and/or epoxide groups, and act as a monomer for an addition type copolymerization with diolefins.
Toy, M. S.↗
Surface texturing of fluoropolymers
A method is disclosed for improving surface texture for adhesive bonding, metal bonding, substrate plating, decal substrate preparation, and biomedical implant applications. The surface to be bonded is dusted in a controlled fashion to produce a disbursed layer of fine mesh particles which serve as masks. The surface texture is produced by impinging gas ions on the masked surface. The textured surface takes the form of pillars or cones. The bonding material, such as a liquid epoxy, flows between the pillars which results in a bond having increased strength. For bonding metals a thin film of metal is vapor or sputter deposited onto the textured surface. Electroplating or electroless plating is then used to increase the metal thickness in the desired amount.
Banks, B. A.↗
Concerning apparent similarity of structures of fluoropolymer surfaces exposed to an argon plasma or argon ion beam
No abstract available
NASA Discipline Environmental Health↗
Measurement of Fluoride Generated from Fluoropolymer Wire Insulations
No abstract available
Boddapati, Aparna↗
Cellular thermosetting fluorodiepoxide polymers
Thermosetting fluoropolymer foams are made by mixing fluid form thermosetting fluoropolymer components having a substantial fluorine content, placing the mixture in a pressure tight chamber, filling the chamber with a gas, at relatively low pressure, that is unreactive with the fluoropolymer components, allowing the mixture to gel, removing the gelled fluoropolymer from the chamber and thereafter heating the fluoropolymer at a relatively low temperature to simultaneously sure and foam the fluoropolymer. The resulting fluoropolymer product is closed celled with the cells storing the gas employed for foaming. The fluoropolymer resins employed may be any thermosetting fluoropolymer including fluoroepoxies, fluoropolyurethanes and fluoroacrylates.
Lee, Sheng Y.↗
Mixed composition materials suitable for vacuum web sputter coating
Ion beam sputter deposition techniques were used to investigate simultaneous sputter etching of two component targets so as to produce mixed composition films. Although sputter deposition has been largely confined to metals and metal oxides, at least one polymeric material, poly-tetra-fluorethylene, has been demonstrated to produce sputtered fragments which repolymerize upon deposition to produce a highly cross-linked fluoropolymer resembling that of the parent target Fluoropolymer-filled silicon dioxide and fluoropolymer-filled aluminum oxide coatings have been deposited by means of ion beam sputter coat deposition resulting in films having material properties suitable for aerospace and commercial applications. The addition of fluoropolymer to silicon dioxide films was found to increase the hydrophobicity of the resulting mixed films; however, adding fluoropolymer to aluminum oxide films resulted in a reduction in hydrophobicity, thought to be caused by aluminum fluoride formation.
Banks, Bruce A.↗
ECTFE (HALAR) as a New Material for Primary Sample Containment of Astromaterials
Fluoropolymers, such as Teflon® (PTFE, PFA, FEP) and Viton® (FKM), have been used for over 40 years in curating astromaterials at NASA JSC. In general, fluoropolymers have low outgassing and particle shedding properties that reduce cross-contamination to curated samples. Ethylene - Chlorotrifluoroethylene (ECTFE), commonly called Halar® (trademark of Solvay Solexis), is a partially fluorinated semi-crystalline copolymer in the same class of fluoropolymers with superior abrasion resistance and extremely low permeability to liquids, gases, and vapors than any other fluoropolymer (fig. 1). ECTFE coatings are becoming more popular in the nuclear, semiconductor, and biomedical industry for lining isolation containment gloveboxes and critical piping as well as other clean room applications. A study was conducted at NASA JSC to evaluate the potential use of Halar on future sample return missions as a material for primary sample containment.
Calaway, Michael J.↗