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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Rigid-Rod Sulfonated Polyamide as an Aqueous-Processable Binder for Li-Ion Battery Electrodes

Polymer binders are important components of most battery electrodes, ensuring high performance and long-term durability. Increasing demand for lithium-ion batteries in the automotive, stationary power, and portable electronics industries calls for a greener binder to replace poly(vinylidene difluoride) (PVDF). We evaluate the performance of aqueous solution-processed electrodes prepared with a rigid-rod polymer binder, poly(2,2'-disulfonyl-4,4'-benzidine terephthalamide) (PBDT). The polyamide backbone and double-helical configuration of PBDT give rise to its mechanical strength and rigidity, and its functional nature (H-bonding amides and sulfonates) can provide specific binding with electrode particles. LiFePO 4 electrodes prepared with 3 wt% PBDT show mechanical integrity and cycling stability, achieving over 1000 cycles at 4C rate with negligible capacity decay. These electrodes demonstrate comparable rate performance with their PVDF counterparts while eliminating fluorine from the electrode as well as the organic solvents needed for processing. Furthermore, this study reveals that PBDT holds great potential as a binder for advanced sustainable batteries.

25 ENERGY STORAGE↗
DOE OSTI2023

Orientation matters: Measuring the correct surface of polyamide membranes with quartz crystal microbalance

The surface of polyamide reverse osmosis (RO) membranes which regulates interface-dominated phenomena, such as partitioning and fouling, is the one facing the feed during operation. However, the opposite surface of the polyamide selective layer, the one facing the permeate and in contact with the polysulfone porous support, is commonly analyzed in quartz crystal microbalance (QCM) measurements due to limitations of state-of-the-art transfer methodologies. Such measurements on the back surface cannot be generalized because the polyamide layer is chemically and morphologically asymmetric. Herein, we introduce a simple method to coat QCM sensors with polyamide active layers in the correct orientation (i.e., exposing their front surface) and show that interface-dominated phenomena differ significantly between orientations. We start by describing a transfer protocol to coat any surface with a polyamide layer on its front surface orientation. We then systematically analyze the chemical and morphological differences between the two surfaces of the polyamide layer of a commercial RO membrane. Finally, we demonstrate that interface-dominated phenomena depend on the orientation by showing that NaCl partitioning at pH 6 was 1.3 to 2.3-fold higher on the front surface and that organic fouling with humic acid occurred at a lower rate on this surface. The new method presented herein enables measurements on the front surface of polyamide RO membranes, which should be the standard in any future QCM studies.

Fouling behavior↗
NASA NTRS1985

Determination of the viscosity number of thermoplastics in dilute solution; polyamides (PA)

This West German Standard presents a test used to determine the viscosity number of polyamides and copolyamides which are easily diluted in sulfuric acid, and for other polyamides which are less easily diluted in sulfuric acid, and which are diluted in m-cresol. As formic acid is often used in industry instead of sulfuric acid, this solvent is also presented as an alternative, however, sulfuric acid is preferred because of the thermodynamic solubility characteristics of the polyamides and the handling safety. In addition, it is shown which solvent should be used for each polyamide. Finally, determinations concerning the preparation of the samples are presented. Using the viscosity number, a determination of the molar mass of the polyamides is possible.

Source record↗
DOE OSTI2024

Structural Effects on Solubility and Crystallinity in Polyamide Ionomers

Although polyamides have been an industrial staple for decades, their solubility and processability remain limited due to the strong hydrogen bonding between amide groups. Here, we report a family of polyamides in which aryl rings, alkyl spacers, sulfonate groups, and amide linkages are regularly spaced along the polymer backbone, allowing us to probe the structural elements that affect processability. We accessed these polymers through a synthetic route based on an expanded diamine monomer and characterized them through a range of physical and spectroscopic techniques. Our results show that the combination of sulfonate groups with increased amide content results in highly soluble polymers, which can dissolve in polar solvents such as water, methanol, and N,N-dimethylformamide. Infrared spectroscopy on the solid polymers shows that the aliphatic amides engage in hydrogen bonding with the sulfonate groups, thus inhibiting ion aggregation, crystallization, and microphase separation. These findings expand the avenue to sulfonate-containing polyamide chemistry and provide design rules for the synthesis of more processable ionic polyamides.

amides↗
NASA NTRS1983

Thermoset/Thermoplastic Aromatic Polyamides for Composites

Aromatic polyamides are processed at relatively low temperature, then heat-treated to attain high softening temperature required when polyamides are used as matrix resins in structural composites. New polyamides are compatable with organic fibers often used as reinforcing agents in such composites Pendent propargyl groups serve as latent cross-linking agents in new series of polyamide resins.

St. Clair, T. L.↗
NASA NTRS1986

Syntheses and thermal stabilities of polyamides from 2,2'-bithiophene-5,5'-dicarbonyl dichloride and diamines

The properties of 12 polymers derived from 2,2'-bithiophene-5,5'-dicarbonyl dichloride are analyzed. The solution and interfacial polymerizations of 2,2'-bithiophene-5,5'-dicarbonyl dichloride are described. It is observed that due to high glass transition temperatures and the lack of flexibility of the polyamide of 2,2'-bithiophene-5,5'-dicarbonyl dichloride most of the polymers failed to fabricate into fibers or films. The data reveal that the polyamides formed from terphenyl ether form a tough, heat-pressed film; the polyamides made from aromatic diamides show great thermal stability; and the polyamides derived from aliphatic or benzylic diamides display no thermal stability.

Barber, Patrick G.↗
DOE OSTI2023

Unveiling the microstructural evolution of carbon fibers derived from polyamide-6

Polyacrylonitrile-based carbon fibers have dominated the industry for decades, but the high cost of polyacrylonitrile has prevented the widespread adoption of carbon fiber in high-volume structural applications. As such, a significant amount of research has been dedicated to finding an alternative, low-cost carbon fiber precursor. In this work, carbon fibers were produced from polyamide-6 using metal salt impregnation and a thermo-oxidative stabilization step. To gain further insight into the carbonization process and microstructural transformation, the morphologies, crystallinities, elemental compositions, and thermal stabilities of the fibers were characterized at various stages of processing. The stabilization step resulted in a significant increase in carbon yield, indicating a dramatic increase in thermal stability. This is due to the crosslinking of polyamide-6 chains, which was confirmed by functional group analysis. The crystallinity of the fibers was also significantly altered during processing, as the produced carbon fibers consisted of pseudo-amorphous carbon with two distinct regions of metal salt impregnation. Finally, the findings and microstructural evolution mechanisms provide guidelines for further research into carbon fiber produced from polyamide-6.

36 MATERIALS SCIENCE↗
NASA NTRS2015

Synthesis and Properties of Cross-Linked Polyamide Aerogels

We report the first synthesis of cross-linked polyamide aerogels through step growth polymerization using a combination of diamines, diacid chloride and triacid chloride. Polyamide oligomers endcapped with amines are prepared as stable solutions in N-methylpyrrolidinone from several different diamine precursors and 1,3-benzenedicarbonyl dichloride. Addition of 1,3,5-benzenetricarbonyl trichloride yields gels which form in under five minutes according to the scheme shown. Solvent exchange of the gels into ethanol, followed by drying using supercritical CO2 extraction gives colorless aerogels with densities around 0.1 to 0.2 gcm3. Thicker monolithes of the polyamide aerogels are stiff and strong, while thin films of certain formulations are highly flexible, durable, and even translucent. These materials may have use as insulation for deployable space structures, rovers, habitats or extravehicular activity suits as well as in many terrestrial applications. Strucure property relationships of the aerogels, including surface area, mechanical properties, and thermal conductivity will be discussed.

Aerogel↗
NASA NTRS2024

Synthesis of Flexible Polyamide Aerogels Cross-Linked with a Tri-Isocyanate

A new series of flexible polyamide (PA) aerogels was synthesized using terephthaloyl chloride (TPC), 2,2′-dimethylbenzidine (DMBZ) and cross-linked with an inexpensive, commercially available tri-isocyanate (Desmodur N3300A) at polymer concentrations of 6–8 wt.% total solids and repeating units, n, from 30 to 60. The cross-linked DMBZ-based polyamide aerogels obtained, after supercritically drying using liquid CO 2 , had shrinkages of 19–27% with densities ranging from 0.12 g/cm 3 to 0.22 g/cm 3 , porosity and surface areas up to 91% and 309 m 2 /g, respectively, and modulus values ranging from 20.6 to 109 MPa. Evidence suggests that a higher flexibility could be achieved using DMBZ in the polyamide backbone with N3300A as a cross-linker, when compared to previously reported TPC-mPDA-BTC PA aerogels, N3300A-polyimide aerogels, and N3300-reinforced silica aerogels.

aerogels↗
DOE OSTI2026

Universal Approach for the Depolymerization of Polyamides via Photothermal Conversion

Polyamides (PAs) exhibit excellent chemical stability and mechanical resistance, yet these same characteristics lead to their widespread accumulation in the environment as pollution. In this work, we developed an inclusive and operationally simple photothermal strategy to recycle PAs, overcoming the high energy barriers necessary to break down these materials. PAs can be depolymerized using photothermally mediated ring-closing depolymerization and acidic hydrolysis to afford cyclic and linear monomers using carbon black as a photothermal agent (PTA) under visible light irradiation. We showed that polyamide 6 is efficiently depolymerized to ε-caprolactam with 74% yield in 10 min. Similarly, in 1 h, the photothermal acidic hydrolysis of polyamide 6,6 afforded hexamethylene diamine and adipic acid with 97 and 96% yields, respectively. This method was further applied to a variety of aliphatic and aromatic PAs and mixed PA waste. Both photothermally promoted processes effectively depolymerize pigment-containing postconsumer waste by leveraging existing black pigments as PTAs. Here, photothermal conversion provided a general and rapid route for PA depolymerization under visible light irradiation, enabling high monomer yields with inexpensive reagents and a general tolerance to additives, demonstrating this approach’s potential for a circular plastic economy.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1973

Heat-resistant polymers containing bipyridyl units. II Polyamide-imides

Polyamide-amic acids containing bipyridyl units were prepared by polymerization of various bipyridyl diamines with trimellitic anhydride acid chloride. These polymers were converted to polyamide-imides by thermal cyclization. The resulting polyamide-imides exhibited very good solubility in organic solvents.

Kurita, K.↗
NASA NTRS1976

New aromatic silicon-containing polyamides

The experiments described were aimed at studying systematically the effect of silyl linkages on the thermogravimetric and thermomechanical properties of aromatic polyamides. Specifically, 18 aromatic silicon-containing polyamides were synthesized via interfacial polymerization of six silicon-containing diacid chlorides with 3,3-prime-diaminodiphenylmethane, 3,3-prime-diaminobenzophenone, and 1-(3-prime-aminobenzyl)-4-(3-double prime-aminobenzoyl)benzene. All polyamides were soluble in m-cresol and N,N-dimethylacetamide, and had glass transition temperatures between 178 and 254 C. Thermogravimetric analysis conducted in static air on film specimens showed 5 and 10 percent weight losses between 331 and 400 C and 354 and 440 C, respectively. The potential gain in processability engendered by incorporation of silane substituents was offset in most cases by substantial losses in thermo-oxidative stability.

Pratt, J. R.↗
NASA NTRS1984

Thermoset-thermoplastic aromatic polyamide containing N-propargyl groups

The compounds of the class of aromatic polyamides useful as matrix resins in the manufacture of composites or laminate fabrication were developed. The process for preparing this thermoplastic-thermoset polyamide system involves incorporating a latent crosslinking moiety along the backbone of the polyamide to improve the temperature range of fabrication thereof wherein the resin softens at a relatively low temperature (approx. 154 C) and subsequently sets-up or undergoes crosslinking when subjected to higher temperature (approx. 280 C).

St.clair, T. L.↗
NASA NTRS1984

Synthesis and characterization of phosphorus-containing polyamides and copolyamides based on 1methyl]-2,4- and -2,6-diaminobenzenes

Phosphorus containing polyamides and copolyamides were prepared from 1-(dialkoxyphosphinyl)methyl-2,4- and -2,6-diaminobenzenes. The polymers produced were characterized by infrared and proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. Their thermal properties were compared with those of the corresponding common polyamides. In addition, by determining the limiting oxygen index value of some of these polyamides, their fire resistance was evaluated.

Mikroyannidis, J. A.↗
NASA NTRS1984

Synthesis and characterization of phosphorus-containing polyamides and copolyamides based on 1-(dialkoxyphosphinyl)methyl-2,4- and -2,6-diaminobenzenes

Phosphorus containing polyamides and copolyamides were prepared from 1-(dialkoxyphosphinyl)methyl-2,4- and -2,6-diaminobenzenes. The polymers produced were characterized by infrared and proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. Their thermal properties were compared with those of the corresponding common polyamides. In addition, by determining the limiting oxygen index value of some of these polyamides, their fire resistance was evaluated.

Mikroyannidis, J. A.↗
NASA NTRS2018

Process for Preparing Aerogels from Polyamides

Polyamide aerogels and methods of making the same are discussed. One example method can include the act of creating a mixture of at least one diamine with at least one diacid chloride in a first solvent. The mixture can comprise a plurality of amine capped polyamide oligomers. Such a method can also include the acts of adding a cross-linking agent to the mixture to create a gel and performing one or more solvent exchanges to remove the first solvent. Additionally, such a method can include the act of subjecting the gel to supercritical drying to polyamide aerogel.

Meador, Mary Ann B.↗