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At least 505 records · Page 28

Dynamics of PDMS- g -PDMS Bottlebrush Polymers by Broadband Dielectric Spectroscopy

Poly(dimethylsiloxane) (PDMS)-based bottlebrush polymers, PDMS-g-PDMS, have been synthesized by anionic polymerization in combination with a condensation-based grafting reaction. Bottlebrush polymers show intriguing features, e.g., extremely low viscosities. Hereby, studies of their dynamics are rare. Therefore, we focus on the segmental relaxation by broadband dielectric spectroscopy. An increasing cross-sectional radius proportional to the increasing side chain length has been observed by small-angle neutron scattering over three samples. Here, a comparison of the segmental relaxation times of the bottlebrushes with the respective linear chains reveals slower dynamics in the former. For longer chains, this effect vanishes.

36 MATERIALS SCIENCE↗

Solvent Processing and Ionic Liquid-Enabled Long-Range Vertical Ordering in Block Copolymer Films with Enhanced Film Stability

Rapid and reliable processing methods for forming ordered block copolymer (BCP) materials with low defect density in a thin film geometry are required for many nanotechnology applications. Vertically aligned BCP structures, in particular, have applications ranging from nanolithography for electronics and photonics to nanoporous membranes for water remediation and novel batteries for flexible electronics. However, the attainment of nearly complete vertical orientational order of the BCP ordered phase remains challenging. Solvent-based techniques, such as direct immersion annealing (DIA) and solvent vapor annealing (SVA), have immense potential for these applications of BCP films, as it allows for tuning of their thermodynamic, structural, and chain mobility driven kinetic properties. We first demonstrate that DIA, using a judicious choice of binary solvent mixtures along with a relatively hydrophobic ionic liquid (IL), induces the rapid vertical ordering in polystyrene-b-polymethylmethacrylate (PS-PMMA) block copolymer in lamellar films. The IL establishes synergy to the binary solvent mixture of toluene and heptane to 1 create a near-neutral solvent environment for attaining the vertical microstructure of the BCP. Next, we show that IL can suppress the de-wetting of the PS-PMMA films to achieve long-range order using SVA in cylindrical films for long annealing times. Both vertical and horizontal morphology is attained in these films by selecting different solvent environments. Furthermore, attaining enhanced vertical and horizontal BCP structure with long-range defect-free order by tuning solvent quality and using additives like IL can render them useful for many nanotech applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dynamics of Bottlebrush Polymers in Solution by Neutron Spin Echo Spectroscopy

In this work, we present dynamical and morphological studies on poly(dimethylsiloxane) (PDMS)-based bottlebrush polymers in solution. A combination of small-angle neutron scattering (SANS), pulsed field gradient nuclear magnetic resonance (PFG NMR), and neutron spin echo (NSE) spectroscopy was used to identify structural changes inherent in changing the side-chain length while keeping the backbone constant. These morphological changes are mirrored in the diffusion coefficient determined by PFG NMR, resulting in two coefficients for the elongated and one for the more spherical sample. Faster motions are tracked by NSE using the advantage of time- and length-scale resolutions with the diffusion coefficient predetermined by PFG NMR. Hereby, the sample with short side chains relaxes like wormlike micelles considering the longitudinal direction, whereas the dynamics along the radial extension shows a much stronger Q-dependence as known from any theory. The dynamical behavior within the blob region, covered with the more spherical sample, follows the predictions of Zimm as well as of Zilman and Granek (ZG).

36 MATERIALS SCIENCE↗

Understanding Interfacial Block Copolymer Structure and Dynamics

Here, block copolymer (BCP) structure and dynamics were studied using small-angle neutron scattering (SANS), neutron spin echo (NSE) spectroscopy, and molecular dynamics (MD) simulations to obtain a fundamental understanding of the impact of an interfacial block on chain dynamics. A glassy block acted as the interface, and the dynamics of a rubbery block was studied. The rubbery block was protonated near the interface in one sample and near the chain end in another sample to observe the interfacial effect on the rubbery polymer. Analysis of the structure and dynamics revealed that the interfacial rubbery block was confined in layered morphologies and exhibited much slower dynamics than the chain-end rubbery block that was dispersed in the rubbery matrix. The interfacial rubbery block showed weaker dynamical relaxation than that at the chain end, and it also had critically important length scale dependence. Dynamical slowing was only observed at length scales significantly larger than the characteristic segmental length, and the disparity between interfacial and chain-end dynamics increased with increasing length.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Gelation and Re-entrance in Mixtures of Soft Colloids and Linear Polymers of Equal Size

Liquid mixtures composed of colloidal particles and much smaller non-adsorbing linear homopolymers can undergo a gelation transition due to polymer-mediated depletion forces. We now show that the addition of linear polymers to suspensions of soft colloids having the same hydrodynamic size yields a liquid-togel-to-re-entrant liquid transition. In particular, the dynamic state diagram of 1,4-polybutadiene star-linear polymer mixtures was determined with the help of linear viscoelastic and small-angle Xray scattering experiments. While keeping the star polymers below their nominal overlap concentration, a gel was formed upon increasing the linear polymer content. Further addition of linear chains yielded a re-entrant liquid. This unexpected behavior was rationalized by the interplay of three possible phenomena: (i) depletion interactions, driven by the size disparity between the stars and the polymer length scale which is the mesh size of its entanglement network; (ii) colloidal deswelling due to the increased osmotic pressure exerted onto the stars; and (iii) a concomitant progressive suppression of the depletion efficiency on increasing the polymer concentration due to reduced mesh size, hence a smaller range of attraction. Our results unveil an exciting new way to tailor the flow of soft colloids and highlight a largely unexplored path to engineer soft colloidal mixtures.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Comprehensive Dynamics in a Polyelectrolyte Complex Coacervate

The linear viscoelastic response, LVR, of a hydrated polyelectrolyte complex coacervate, PEC, was evaluated over a range of frequencies, temperatures, and salt concentrations. The PEC was a nearly stoichiometric blend of a quaternary ammonium poly([3-(methacrylamido)propyl]trimethylammonium chloride), PMAPTAC, and poly(2-acrylamido-2-methyl-1-propanesulfonic acid sodium salt), PAMPS, an aliphatic sulfonate, selected because they remain fully charged over the conditions of use. Narrow molecular weight distribution polyelectrolytes were prepared using fractionation techniques. A partially deuterated version of PMAPTAC was incorporated to determine its coil radius of gyration, R g , within PECs using small-angle neutron scattering. Chain dimensions were determined to be Gaussian with a Kuhn length of 2.37 nm, which remained constant from 25 to 65 °C. The LVR for a series of matched molecular weight PECs, mostly above the entanglement threshold, exhibited crossovers of modulus versus frequency classically attributed to the reptation time, relaxation between entanglements, and the relaxation of a Kuhn length of units (the “monomer” time). The scaling for zero shear viscosity, η 0 , versus chain length, N, was η 0 ~ N 3.1 , in agreement with “sticky reptation” theory. The lifetime and activation energy, E p , of a pair between polyanion and polycation repeat units, Pol + Pol – , were determined from diffusion coefficients of salt ions within the PEC. The activation energy for LVR of salt-free PECs was 2E p , showing that the key mechanism limiting the dynamics of undoped PECs is pair exchange. An FTIR technique was used to distinguish whether SCN– acts as a counterion or a co-ion within PECs. Doping of PECs with NaSCN breaks Pol + Pol – pairing efficiently, which decreases effective cross-linking and decreases viscosity. Finally, an equation was derived that quantitatively predicts this effect.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Clustering Effects on the Structure of Ionomer Solutions: A Combined SANS and Simulations Study

Ionic assemblies, or clusters, determine the structure and dynamics of ionizable polymers and enable their many applications. Fundamental to attaining well-defined materials is controlling the balance between van der Waals interactions that govern the backbone behavior and the forces that drive the formation of ionic clusters. Here, using small angle neutron scattering and fully atomistic molecular dynamics simulations, the structure of a model ionomer, sulfonated polystyrene in toluene solutions, was investigated as the cluster cohesion was tweaked by the addition of ethanol. The static structure factor was measured by both techniques and correlated with the size of the ionic clusters as the polymer concentration was varied. The conjunction of SANS results and molecular insight from MD simulations enabled the determination of the structure in these inhomogeneous networks on multiple length scales. Additionally, we find that across the entire concentration range studied, a network driven by the formation of ionic clusters was formed, where the size of the clusters drives the inhomogeneity of these systems. Tweaking the ionic clusters through the addition of ethanol impacts the packing of the sulfonated groups, their shape, and their size distribution, which in turn, affects the structure of these networks.

36 MATERIALS SCIENCE↗

Chain Conformations of TEMPO-Based Organic Radical Polymers with Varying Radical Loading and Temperature in Battery-Relevant Solvents

Poly(2,2,6,6-tetramethylpiperidinyloxy-4-yl methacrylate) (PTMA) is an organic radical polymer that is a promising active material in organic batteries. The proximity of the radical groups impacts the nature of charge transfer, in which closer packing promotes electron exchange; however, the chain conformation of PTMA is not well understood. Here, the conformation of PTMA in, and its thermodynamic interactions with, battery-relevant solvents is determined using small-angle neutron scattering (SANS). N-methyl-2-pyrrolidone (NMP) and 50:50 (wt %) ethylene carbonate/dimethyl carbonate (EC/DMC) mixtures with PTMA of varying radical content (68 vs 98%) and temperature (25 and 60 °C) are examined. Both solvents are theta solvents for PTMA irrespective of radical loading and temperature. PTMA attains an expanded chain conformation in NMP and a more compact polymer chain conformation in EC/DMC. Lastly, the electrochemical performance of PTMA films formed from EC/DMC shows improved performance relative to those cast from NMP, which is interpreted to indicate that the compact conformation of PTMA in EC/DMC enables improved inter- and intrachain charge transfer.

25 ENERGY STORAGE↗

In Situ Polymerization of Polypyrrole and Polyaniline on the Surface of Magnetic Molybdenum Trioxide Nanoparticles: Implications for Water Treatment

Photocatalyst dissolution greatly diminishes the usability of photocatalysts in water treatments. Coating conductive polymers on the surface of photocatalysts can reduce dissolution without compromising the photocatalytic properties of the material. In this investigation, polypyrrole (PPy) and polyaniline (PANI) were used to coat two magnetic MoO 3 nanoparticles with different surface chemistries. The polymer-coated MoO 3 @Fe 3 O 4 nanoparticles were synthesized by optimizing the mole fractions of PPy or PANI, MoO 3 , and Fe 3 O 4 . The optimized PPy@ MoO 3 @Fe 3 O 4 (PMF1) and PANI@MoO 3 @Fe 3 O 4 (PMF2) resulted in 95.39 and 75.98% methylene blue dye removal, respectively. MoO 3 dissolutions of 4.12 and 5.6% were obtained for PMF1 and PMF2, respectively, demonstrating the reduced solubility of the coated nanoparticles as compared to their uncoated counterparts (7.87% for MF1 and 18.1% for MF2). In situ small-angle neutron scattering (SANS) was utilized to investigate the polymerization kinetics of PPy and PANI on nanoparticles. The results revealed that an increase in base material oxygen vacancies resulted in the reduction of both the polymer size and the polymerization rate. Furthermore, this study demonstrated that SANS provides valuable insights into the polymer growth mechanisms on nanoparticle surfaces.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Structure and Dynamics of Water Confined in Transition Metal Carbide MXenes: Implications for Electrochemical Applications

Two-dimensional transition metal carbides and nitrides (MXenes) are an important family of electrochemically active 2D materials. MXenes combine high conductivity with hydrophilicity, making them attractive materials for many applications, including electrochemical energy storage, sensing, desalination, and others. In order to better understand the role of structure on MXene properties, here, we investigated the vibrational properties and diffusion of water in MXenes with differing layer thicknesses and transition metal compositions using inelastic, quasi-elastic, and small-angle neutron scattering. We found that all of the Mo-containing MXenes studied here exhibited comparable vibrational dynamics and diffusion coefficients to each other and to previously studied Ti 3 C 2 T x . However, Ti 2 CT x was distinguished by its faster diffusion and more hydroxyl groups compared to the other MXenes studied. These results can help guide the selection of appropriate MXenes for energy storage and electrochemical water purification applications.

MXenes↗

Warpage-Resistant, Under-Extrusion-Free, High-Surface-Quality Additive Manufacturing Process for Polyethylene-Based Composite Radiation Shielding Material

Polyethylene (PE) is one of the best shielding materials for primary space radiation due to its high hydrogen content. For effective secondary neutron shielding, boron-rich fillers are incorporated to enhance performance. The semicrystalline nature and high thermal expansion coefficient of PE impede its adoption for in situ additive manufacture in space via the fused deposition modeling (FDM) 3D printing. Here, we developed an optimized PE blend to mitigate the effects of under-extrusion and warpage. Guided by studies on extrusion and warpage, we developed an optimal set of printing parameters for the proposed PE blend. The optimum PE blend─both in its pure form and when doped with fillers─has been tested on different FDM printers. The printed structures exhibit high and uniform density, smooth surfaces, no warpage, and competitive mechanical properties. The FDM-printed plates demonstrate efficient shielding from thermal neutrons, predicted via modeling and confirmed experimentally using extended Q-range small-angle neutron scattering.

additive manufacturing↗

How Does the Rate of Chain Exchange Relate to Stress Relaxation in Triblock Copolymer Networks?

The relationship between macroscopic stress relaxation and molecular-level chain exchange in triblock copolymer micelles has been explored using rheology and time-resolved small-angle neutron scattering (TR-SANS), marking the first measurements of chain exchange in concentrated triblock networks. It has long been assumed in models of transient or thermoreversible networks that the time scales for these two processes are equal. Experimentally, we find that stress relaxation occurs many orders-of-magnitude faster than chain exchange. This difference is quantitatively explained by modest dispersity in the core block that results in a slight asymmetry within any given nominally symmetric triblock. For stress relaxation to occur, only the shorter chain must pull out, while chain exchange is slowed due to the requirement of the eventual pullout of the longer block. The pullout time is extremely sensitive to the length of the core block. This mechanism is supported by measurements with an intentionally asymmetric triblock copolymer, which displays an even larger difference between the stress relaxation and chain exchange rates. These results establish a quantitative molecular-level picture of the chain dynamics associated with stress relaxation in triblock copolymer networks.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Melatonin-Induced Modulation of Cholesterol-Enriched Model Neuronal Membranes

Melatonin, a hormone primarily produced by the brain’s pineal gland, not only regulates circadian rhythms, but also influences the structural and biophysical properties of neuronal membranes. Its amphiphilic nature enables direct incorporation into lipid bilayers and preferential interactions with cholesterol-rich lipid rafts, critical hubs for cellular signaling and membrane organization. Despite increasing recognition of its membrane activity, the molecular basis of melatonin’s interactions with coexisting liquid-ordered (L o ) and liquid-disordered (L d ) phases remains unclear. Here, in this study, we combine small-angle neutron scattering (SANS) and all-atom molecular dynamics simulations to examine model neuronal membranes composed of DSPC, DOPC, POPC, and cholesterol. Our results show that melatonin preserves domain morphology while adopting distinct orientations within the bilayer and at the membrane interface, allowing both lateral and transmembrane bridging across lipid phases. These findings establish the molecular underpinnings of melatonin’s modulation of membrane heterogeneity and provide strong support for its receptor-independent actions.

atomistic simulations↗

Threading–Unthreading Transition of Linear-Ring Polymer Blends in Extensional Flow

Adding small amounts of ring polymers to a matrix of their linear counterparts is known to increase the zero-shear-rate viscosity because of linear-ring threading. Uniaxial extensional rheology measurements show that, unlike its pure linear and ring constituents, the blend exhibits an overshoot in the stress growth coefficient. By combining these measurements with ex-situ small-angle neutron scattering and nonequilibrium molecular dynamics simulations, this overshoot is shown here to be driven by a transient threading–unthreading transition of rings embedded within the linear entanglement network. Prior to unthreading, embedded rings deform affinely with the linear entanglement network and produce a measurably stronger elongation of the linear chains in the blend compared to the pure linear melt. Thus, rings uniquely alter the mechanisms of transient elongation in linear polymers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Colloidal Nafion Particles: Are Cylinders Ubiquitous?

Colloidal Nafion morphology plays a critical role in determining the performance of fuel cells and electrolyzers. While small-angle neutron scattering (SANS) studies previously described Nafion in liquid media as dispersed cylinders, the analysis remains nonunique with multiple possible morphological descriptions of the data. Here, using SANS and all-atomistic molecular dynamics, we confirm that Nafion morphology in liquid media differs substantially depending on dispersing agent and dispersion method. H + Nafion dispersed in N-methyl pyrrolidone forms swollen cluster particles with physically cross-linked ionic groups. Scattering profiles from dispersed Nafion membrane have a large structure factor feature not observed for redispersed Nafion D-521. H + Nafion dispersed in water has a highly elongated cylindrical morphology (radius = 10 ± 1.5 Å, height = 358 ± 4.7 Å) with fully dissociated and solvated sulfonic acid groups on the particle wall. In conclusion, these results highlight an important discrepancy between the methods of preparing Nafion dispersions and the use of simplified analysis techniques to describe Nafion morphology.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dynamic Implications of Noncovalent Interactions in Amphiphilic Single-Chain Polymer Nanoparticles

Single-chain polymer nanoparticles (SCNPs) combine the chemical diversity of synthetic polymers with the intricate structure of biopolymers, generating versatile biomimetic materials. The mobility of polymer chain segments at length scales similar to secondary structural elements in proteins is critical to SCNP structure and thus function. However, the influence of noncovalent interactions used to form SCNPs (e.g., hydrogen-bonding and biomimetic secondary-like structure) on these conformational dynamics is challenging to quantitatively assess. To isolate the effects of noncovalent interactions on SCNP structure and conformational dynamics, we synthesized a series of amphiphilic copolymers containing dimethylacrylamide and monomers capable of forming these different interactions: (1) di(phenylalanine) acrylamide that forms intramolecular β-sheet-like cross-links, (2) phenylalanine acrylamide that forms hydrogen-bonds but lacks a defined local structure, and (3) benzyl acrylamide that has the lowest propensity for hydrogen-bonding. Each SCNP formed folded structures comparable to those of intrinsically disordered proteins, as observed by size exclusion chromatography and small angle neutron scattering. The dynamics of these polymers, as characterized by a combination of dynamic light scattering and neutron spin echo spectroscopy, was well described using the Zimm with internal friction (ZIF) model, highlighting the role of each noncovalent interaction to additively restrict the internal relaxations of SCNPs. These results demonstrate the utility of local scale interactions to control SCNP polymer dynamics, guiding the design of functional biomimetic materials with refined binding sites and tunable kinetics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dynamical Signatures of Thermotoga maritima Maltose-Binding Proteins Affected by Ligand Binding

Functional segregation among protein isoforms depends on the interplay of their overall structures and the molecular dynamics of these structures. Thermotoga maritima maltose-binding protein (tmMBP) isoforms show size-dependent differential binding of maltose and malto-oligomers while maintaining remarkable fold conservation. This differential behavior needs detailed characterization in native-like aqueous conditions to understand the effects of protein dynamics on ligand binding and recognition. Small-angle neutron scattering (SANS), neutron spin echo (NSE) spectroscopy, and dynamic light scattering (DLS) were used in conjunction with previously published computational molecular dynamics (MD) simulations to understand the dynamic behavior of tmMBPs experimentally. SANS provided information on the overall structure of the molecules, while NSE was used to determine the dynamics in the nanosecond time scale. Both tmMBP2 and tmMBP3 have a bidomain architecture linked with a flexible hinge, with the binding pocket sitting in the cleft between the two domains. tmMBP2 and tmMBP3 showed different solution dynamics, with the translational and rotational components dominating the dynamics of both systems, resulting in a clear differentiation of their diffusion pattern. A faster dynamics component was also observed and was attributed to segmental dynamics. Differences observed between the ligand-free (apo) and ligand-bound (holo) states of the two proteins are attributed to conformational entropy. Our results highlight the intricacies of how structure and dynamics can together shape binding to a repertoire of substrates in structurally similar proteins.

Diffusion↗

Controlled Deuteration of Phosphatidylcholine Biosynthetically Produced from Engineered Escherichia coli for SANS Studies

Deuterated phosphatidylcholine (PC) was produced from engineered Escherichia coli (E. coli) BL21 cells grown in deuterated media. The levels of deuteration could be controlled by growing cells in different combinations of deuterated and nondeuterated water, glycerol, and choline, which were analyzed by NMR, mass spectrometric analysis, and small-angle neutron scattering (SANS). By growing cells in deuterium oxide (D2O) in the presence of fully deuterated glycerol and choline, perdeuterated PC (PC-DDD) was produced via this method. The average neutron contrast match points of isolated PC were experimentally determined using SANS. For partially deuterated PC lipids, SANS showed match points of 92 ± 8% D2O for lipids with deuterated fatty acyl chains and glycerol (PC-DDH) and 81 ± 2% D2O for lipids with only deuterated fatty acyl chains (PC-DHH). Our results will benefit SANS studies that utilize deuterated PC lipids as mimetics of lipid bilayers or membrane-like models for structural studies of biomolecular systems.

Zhang, Qiu [ORNL] (ORCID:0000000255064955)↗