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At least 379 records · Page 21

Macroscale Control of Reactivity using 3D Printed Materials with Intrinsic Catalytic Properties

The morphology of heterogeneous catalysts can impact their performance. However, standard manufacturing methods like extrusion or pelleting offer little options for tailoring catalyst shape. Herein, stereolithographic 3D printing is used to produce catalysts with controlled topologies to enhance their performance. A series of magnetic stir-bar compartments (SBC) were 3D printed and tested as catalysts for sucrose hydrolysis. The SBC were printed using acrylic acid (AA) and 1,6-hexanediol diacrylate (HDDA) as acid sites and hydrophobic crosslinking domains, respectively. Variations in the number and tilt direction of the SBC blades produced significant changes in their apparent catalytic activities. These changes resulted from differences in the fraction of active surface effectively interacting with the reactants in solution, as revealed by computational fluid dynamics simulations. Moreover, varying HDDA:AA ratios in SBC regulated reactant-surface interactions to control catalytic activity. Overall, 3D printing catalysts enables quick performance optimization by simultaneously controlling macroscopic structure and molecular composition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Tuning Organic Semiconductor Packing and Morphology through Non-equilibrium Solution Processing (Final Report)

Organic semiconductors (OSCs) are a promising candidate to produce low-cost, large area, and flexible electronics. There has previously been successful development of organic field effect transistors (OFETs), photovoltaics (OPV), and bioelectronics using OSCs. Solution processing of these materials allows for the fabrication of large-area devices in the kinetic crystallization regime. The charge transport capabilities have been shown to depend on the morphology and molecular packing of the OSC within thin films. Our hypothesis is that solution processing conditions may significantly impact OSC morphology and as a result the charge transport. Therefore, this work has focused on obtaining a fundamental understanding of the morphology and molecular packing of OSCs for optimal device performance. Through our work, we have gained a better understanding of how these structural conditions were influenced by the solution processing conditions. Our studies have led to a more systematic understanding of the various parameters that impact OSC morphology. Solution processing leads to non-equilibrium films, thus allowing for the formation of diverse morphologies that are inaccessible by other fabrication methods. Previously, our group has focused on tuning the morphology of small-molecular OSCs [53, 55-57]. However, little work had been devoted to polymer OSCs. There was a lack of detailed studies characterizing the solution-state of polymer OSCs in terms of their conformation, degree of entanglement, polymer aggregation, and chain relaxation dynamics. The solution state properties are also likely to be influenced by the rigidity and molecular weight of the polymer OSCs investigated. Thus, we have focused our attention on gaining a better insight of polymer OSC films and solution processing methods. Through this proposal, our approach is to investigate the correlation between solution-state properties and the morphology of the resulting polymer OSC films. We worked three specific aims: investigate the effects of 1) polymer OSC solution-state properties on final film morphology; 2) molecular additives on the solution-state and final film properties; 3) controlled pre-aggregation in the solution-state in the final film morphology. More rigid and planar polymer backbones should promote interchain charge transport and more efficient interchain hopping between polymer chains. Through tailoring the polymer backbone, polymer sidechains, and molecular weight, we expected the altered solution-state properties to affect the final film morphology. In addition, reducing the entanglements and promoting chain alignment will likely prevent charge carrier trapping through conformation disorders. We thus studied different mechanisms, such as molecular additives, to reduce entanglements in solution. Devices fabricated from these solutions were expected to have improved charge transport abilities. In addition to tailoring the solution-state characteristics of the polymer OSCs, we investigated the effect of solution processing methods on the molecular packing and morphology of polymer OSC films. Two main solution processing techniques, e.g., spin-coating and solution shearing, were employed to fabricate OFETs. Spin coating was employed to prepare OSC films, which produce isotropic films. This technique creates several parameters to tune such as spin coating speed, acceleration, and time. Additionally, our research group developed the solution shearing method, which consists of the solution initially sandwiched between two plates. By sliding the top plate, the solution front is exposed and drying begins. This technique allows for the creation of aligned large crystalline domains. Solution shearing consists of different processing parameters which can affect the final morphology, such as shearing speed, substrate temperature and temperature gradient, distance between both plates, and the tilt angle of the top plate. Due to the complexity of the polymer systems investigated, numerous techniques were employed to characterize the polymer OSC solution state and films. All the materials were characterized using the DOE supported synchrotron X-ray scattering facilities at the Stanford Synchrotron Radiation Lightsource (SSRL). Using grazing incidence X-ray scattering (GIXS) and Near Edge X-ray Absorption Fine Structure (NEXAFS) techniques, the crystalline structure and molecular orientations of the thin films were measured. Optical absorption (UV-Vis) spectroscopy was employed to determine the aggregation state in solution and films of the polymer systems. Polarized UV-Vis also allowed for the determination of the relative degree of polymer chain alignment for solution sheared films. Additionally, various other techniques were used to investigate other properties within the film, such as atomic force microscopy (AFM) and solution rheology. Finally, the device performance is quantified through the fabrication and characterization of OFETs, which will highlight the effects of morphology on charge transport.

36 MATERIALS SCIENCE↗

Architected mesoporous crystalline magnesium silicates with ordered pore structures

Novel approaches to harness earth abundant silicates as building blocks for carbon dioxide removal, capture, utilization, and storage are gaining increasing attention in the context of sustainable and low carbon energy and resource recovery. Advancing a calibrated understanding of these fluid-silicate interactions is essential for developing scalable processes. One of the challenges in developing predictive controls over these interactions is the compositional and morphological heterogeneity of naturally occurring, heterogeneous magnesium silicate minerals. To address this challenge, the synthesis of architected mesoporous crystalline magnesium silicate (Mg 2 SiO 4 ) is proposed. While synthesis routes for producing amorphous mesoporous magnesium silicates have been developed via sol-gel methods, approaches to synthesize crystalline magnesium silicates with well-controlled pore size distributions have not been explored. The conventional approaches of converting matter that is amorphous to crystalline states at elevated temperatures results in a heterogeneous pore size distribution. To develop controls on pore size distribution, amorphous mesoporous magnesium silicates are coated with carbon. This approach preserves the pore size distributions during the amorphous to crystalline transformations of Mg-silicates at elevated temperatures. The carbon coating is removed on heating. Magnesium silicate particles produced using this approach have highly ordered pores around 2.58 nm and a specific surface area of 124.25 m 2 /g. In this study, we report the chemical compositions, morphologies, phase transitions, and pore structures of the intermediate materials produced during the synthesis of crystalline mesoporous magnesium silicates. The transitions, and pore structures of the intermediate materials produced during the synthesis of crystalline mesoporous magnesium silicates. Furthermore, the synthesis routes discussed in this study can be applied translationally to produce metal silicates with ordered mesoporous structures.

36 MATERIALS SCIENCE↗

Development of a Printable Prill Formulation Technique and Demonstration of Monomodal Prill Size on Compaction Density and Compressive Strength

Polymer-bonded explosive molding powder, or “prills,” are relied on for the fabrication of pressed high explosives since the 1950's. The wet granulation technique, also known as “slurry coating,” that is used to formulate prills, is a complex process that results in polydisperse and variable yields. This makes it difficult to study the mesoscale effect that prills have on the microstructure of a pressed article. The following study introduces a novel approach to energetic granulation that leverages techniques used in the additive manufacturing of paste-like energetic materials. This extrusion granulation, or prill printing technique, makes it possible to tailor the sizes and shapes of prills, allowing for their morphological influences to be studied in a controlled manner. The following work details the fabrication and characterization of four monomodal size lots of prills using an inert formulation (95 wt.% melamine, 5 wt.% polymer binder). Prills from each size lot were die-pressed using a fixed recipe to investigate how prill size impacts compaction density and therefore compressive strength. It was found that larger prills influence the pressing density by creating larger defects within the microstructure of a pressed article, resulting in a decrease in compressive strength.

direct ink write↗

High Speed In-situ X-ray Imaging of 3D Freeze Printing of Aerogels

3D freeze printing (3DFP) combines drop-on-demand (DOD) inkjet printing with freeze casting to fabricate lightweight and multifunctional aerogels with customized geometries. Freeze casting is an efficient and easily implemented method capable of fabricating porous, sponge-like structures for many different applications. This process enables tailoring the microstructure of the final product (i.e., pore morphology, alignment, average size distribution, etc.) by controlling the fabrication conditions and freezing kinetics. Furthermore, its combination with DOD printing provides the capability of engineering the macrostructure without relying on a mold as reported for 3D freeze-printed aerogels made from graphene, silver nanowires, and other nanocomposites. In this paper, we performed in-situ X-ray imaging to understand the inside process dynamics in 3DFP using a commercially available colloidal silica ink. We investigated the 3DFP process with the following hierarchy: first, single droplets; then, uniform lines obtained from coalescence of droplets; and finally, three consecutive lines deposited layer by layer. With the help of X-ray imaging, the importance of the balance between material deposition and freezing rates was shown in-situ by the observation inside of the freeze front following the tip of the printed line. The effects of the substrate temperature on the elimination of undesired interfacial boundaries were also shown by the observed ice crystals penetrating from lower to upper layer.

36 MATERIALS SCIENCE↗

Texture evolution as a function of scan strategy and build height in electron beam melted Ti-6Al-4V

Metal additive manufacturing (AM) enables customizable, on-demand parts, allowing for new designs and improved engineering performance. Yet, the ability to control AM metal alloy microstructures (i.e., grain morphology, crystallographic texture, and phase content) is lacking. Furthermore, this work performs corroborative neutron diffraction and large-scale electron backscatter diffraction (EBSD) measurements to assess crystallographic texture in electron beam melted (EBM) Ti-6Al-4V as a function of scan strategy and build height. Texture components for one raster and two spot melt scan strategies were evaluated using a triclinic specimen symmetry to capture all possible texture components, which were found to be considerably different than previously reported values from studies employing orthotropic specimen symmetry. This finding highlights the importance of a standard method and best practice for assessing textures produced by AM.

36 MATERIALS SCIENCE↗

Stimuli-responsive petroleum cement composite with giant expansion and enhanced mechanical properties

Shrinkage, as an inherent property of cement during the curing process, has been a concern in the oil & gas industry for centuries. Therefore, expansive cement has been studied for many decades, primarily through incorporation of expansive additives. Nevertheless, traditional expansive additives are not able to achieve the required expansive ratio or maintain a good mechanical property for the cement composite at extreme underground condition. Accordingly, a new generation of expansive additive, which not only has the required expansion, but also work at the downhole high temperature and high pressure environment, and maintain or even enhance the mechanical property, is highly desired. In this work, a high enthalpy storage shape memory polymer (SMP) as a new class of expansive additive is investigated. It is found that the cement composite achieves 1.4% circumferential expansion by only 6% by weight of SMP additives. The compressive strength and flexural strength are also enhanced at the same time, which is hardly achievable by other expansive additives with the same concertation. Good pumpability is also proved by rheological study. The mechanism controlling the enhanced properties is reveled through morphological study and element mapping analysis at the SMP/cement interface.

36 MATERIALS SCIENCE↗

Growth mechanism of glucose-based hydrochar under the effects of acid and temperature regulation

Improving the tailorability of hydrochar synthesis is an effective way to enhance its performance and utilization efficiency. In this study, the growth rate, morphology, and molecular structure of hydrochar were controlled by regulating the pH and temperature of the hydrothermal carbonization process. Growth process analysis indicates that hydrochar has three growth periods: induction, rapid, and stable growth periods. It is mainly controlled by 5-hydroxymethylfurfural (HMF), which is formed by converting glucose and its transformation products. Further, the regulation of acid can significantly shorten the induction period of hydrochar, even under low-temperature conditions (<180 °C), and increase the growth rate of hydrochar. However, the degree of hydrochar adhesion varies: the lower the temperature, the greater the degree of its adhesion. Molecular structural analysis demonstrates that hydrochar mainly consists of furan structural domains and aromatic clusters, and its surface is rich in oxygen-containing functional groups. The degree at which hydrochar was aromatized was improved by increasing the reaction temperature (160–220 °C); whereas the regulation of acid reduced it and increased the content of oxygen-containing functional groups on the hydrochar surface. Based on these results, it is proposed that hydrochar formation has five stages and three growth periods with or without acid regulation.

59 BASIC BIOLOGICAL SCIENCES↗

Predicting Morphological Evolution during Coprecipitation of MnCO 3 Battery Cathode Precursors Using Multiscale Simulations Aided by Targeted Synthesis

The performance of lithium-ion batteries is intimately linked to both the structure and the morphology of the cathode material, which in turn is critically linked to the synthesis conditions. However, few studies focus on understanding synthesis, especially during the coprecipitation of metal oxide precursors, a process that largely determines the final morphology of the material. In this paper, we go beyond the typical equilibrium particle shape analysis conducted in the literature and incorporate kinetic aspects of morphology evolution. We perform these studies using controlled synthesis on a well-defined metal salt system (MnCO 3 ) combined with multiscale simulations and high-resolution microscopy. Results show that with increasing metal concentration, the particles transition from rhombohedral to cubic to spherical shapes. Computational analysis using density functional theory (DFT) reveals that rhombohedral shaped particles evolve under equilibrium conditions. Phase field techniques indicate that at higher metal concentrations, fast growth kinetics of the precipitates result in the transition to cubic and, subsequently, spherical shapes, accompanied by a decrease in particle size. This study, while limited to the one metal salt system, provides an approach to shed light on the synthesis process of mixed transition metal salts, gradient materials, and other cathode materials of interest to the battery community.

25 ENERGY STORAGE↗

Modulating the Contact Angle between Nonpolar Polymers and SiO 2 Nanoparticles

Polymer–nanoparticle interactions play an important role in determining the morphology and properties of polymer nanocomposites and controlling the polymeric reactions involving heterogeneous catalysts. Here, in this study, we modulate the interactions between nonpolar polymers and nanoparticles by modifying the nanoparticle surface chemistry and quantify the interaction strength through direct contact angle measurements. We investigate the interactions of three nonpolar polymers, polystyrene, polyethylene, and polycyclooctene, with silica nanoparticles whose surface chemistry has been modified by atomic layer deposition of titania and calcium carbonate and by alkyl silanization. Significant differences in polymer–nanoparticle interactions are observed, which can be attributed to differences in the polarizability of the polymers and oxide surface composition. Compared to fully hydrogenated polycyclooctene, polycyclooctene is shown to have stronger interactions with most metal oxides; however, this trend is reversed following alkyl silanization of the silica nanoparticles, which makes the surface of the particles less polar. These differences in interactions can be leveraged to make polymer nanocomposites with unique properties and enable the selective conversion of polymers without the need for separations.

36 MATERIALS SCIENCE↗

The effect of blue and infrared laser melting frequency on oxide morphology in 304L

Continuous Wave Laser Beam (LB) melting offers control over the localised heating and cooling of melt pools for welding, brazing, additive manufacturing and solidification. Research into laserliquid metal interactions has primarily focused on the heat and mass transport under large thermal gradients imposed by the localised melting conditions. Recent commercial availability of blue (450 nm) wavelength lasers has enabled the printing of material with poor IR (1064) nm attenuation like Cu. However, little research has been conducted into varying input laser frequency and scan rate at fixed absorption to understand the effects of laser light on surface oxide formation and the underlying liquid metal thermodynamic response. Here, this article conducts laser melting of 304L under Blue (450 nm) and Infrared (IR, 1064 nm) laser frequencies and examines their impact on laser oxide thickness, chemistry and coloration. We find that laser frequencies induce changes in the oxide layer thickness and chemistry that cannot be explained using conventional thermal absorption shifts and fluid dynamics. We suggest that light coupling may have thermodynamic implications for the chemical potential of the liquid metal, which may drive the observed phase behaviour. Identifying mechanisms for the tuning of the chemical potential via laser frequency control could enable the ability to control solidification microstructure and atomic ordering in laser welding and additive manufacturing processes.

304L↗

Efficient Organic Solar Cell with 16.88% Efficiency Enabled by Refined Acceptor Crystallization and Morphology with Improved Charge Transfer and Transport Properties

Abstract Single‐layered organic solar cells (OSCs) using nonfullerene acceptors have reached 16% efficiency. Such a breakthrough has inspired new sparks for the development of the next generation of OSC materials. In addition to the optimization of electronic structure, it is important to investigate the essential solid‐state structure that guides the high efficiency of bulk heterojunction blends, which provides insight in understanding how to pair an efficient donor–acceptor mixture and refine film morphology. In this study, a thorough analysis is executed to reveal morphology details, and the results demonstrate that Y6 can form a unique 2D packing with a polymer‐like conjugated backbone oriented normal to the substrate, controlled by the processing solvent and thermal annealing conditions. Such morphology provides improved carrier transport and ultrafast hole and electron transfer, leading to improved device performance, and the best optimized device shows a power conversion efficiency of 16.88% (16.4% certified). This work reveals the importance of film morphology and the mechanism by which it affects device performance. A full set of analytical methods and processing conditions are executed to achieve high efficiency solar cells from materials design to device optimization, which will be useful in future OSC technology development.

Zhu, Lei↗

Effect of layer thickness on structural, morphological and superconducting properties of Nb 3 Sn films fabricated by multilayer sequential sputtering

Superconducting Nb3Sn films can be synthesized by controlling atomic concentration of Sn. Multilayer sequential sputtering of Nb and Sn thin films followed by high temperature annealing is considered as a method to fabricate Nb3Sn films where Sn composition of deposited films can be controlled by controlling the thickness of alternating Nb and Sn layers. We report on the structural, morphological and superconducting properties of Nb3Sn films fabricated by multilayer sequential sputtering of Nb and Sn films on sapphire substrates with ex-situ annealing at 950 °C for 3 h. We have investigated the effect of Nb and Sn layer thickness on the properties of Nb3Sn films. The thicknesses of Nb and Sn layers were varied in two ways: (1) varied Nb:Sn thickness ratio (1:1, 2:1, 3:1, 4:1), and (2) varied layer thickness of both Nb and Sn layers, while keeping constant Nb:Sn thickness ratio of 2:1. The crystal structure, surface morphology, topography, and film composition were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM), and energy dispersive X-ray spectroscopy (EDS) respectively. The results showed Sn loss from the surface due to evaporation during annealing. Superconducting Nb3Sn films of critical temperature up to 17.93 K have been achieved.

Sayeed, M. N.↗

Amphiphile conformation impacts aggregate morphology and solution structure across multiple lengthscales

Although the self-assembly of amphiphiles is well-studied in aqueous solutions, much less is understood about the fundamental driving forces and structure property relationships in non-polar media. In recent work [Journal of Physical Chemistry B, 2020, 124, 10822.] the authors have studied a series of malonomide-based amphiphiles that are relevant to liquid-liquid extraction. That work demonstrated that aggregation is largely driven by local dipole-dipole interactions between molecules. Here, we build upon this observation to develop a more detailed understanding of how the balance of dipole-dipole interactions (controlled by conformation) and molecular architecture influences the morphology of the aggregates across lengthscales. Using constrained molecular dynamics about key degrees of freedom, we demonstrate that the conformation of N,N-dimethyl,N,N-dioctylhexylethoxy malonamide (DMDOHEMA) and N,N-dimethyl,N,N-dibutyltetradecyl malonamide (DMDBTDMA) has a significant impact upon self-association - where appropriate conformational sampling is essential. To quantify the aggregate morphology, several graph theoretic and persistent homology based properties are determined. The former examines the patterns of intermolecular interactions within clusters, while the latter examines the 3-dimensional spatial distribution. Based upon these analyses, we find that the morphology of aggregates, particularly at higher malonamide concentration, depends on a balance of dipole alignment and alkyl tail sterics. Dipole alignment encourages linear patterns of the intermolecular interactions within aggregates, while the alkyl tail steric interactions between the malonamide result in noticeably less linear aggregates for DMDOHEMA than DMDBTDMA. This is reflected in the spatial distribution, where more holes or voids exist between extractants within the DMDOHEMA that distribute within the solution in more of a "swiss cheese" arrangement as opposed to the more filamentous distribution of DMBDTDMA. This study links conformation and molecular structure to the morphology of amphiphile assemblies, and serves as a basis for ongoing study of multicomponent amphiphile solutions with polar and other solutes, and how these impact aggregation phenomena.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Chemomechanical origin of morphological disparity in lithium metal electrodeposition

The morphology of electrochemically deposited lithium (Li) critically governs the cycling stability and safety of Li metal batteries, yet the underlying controlling factors remain poorly understood. Even within the same coin cell, Li deposits can exhibit strikingly different morphologies, for example, sparse whiskers coexisting with particle-like deposits, indicting strong local variations in growth conditions. By combining cryogenic transmission electron microscopy with phase-field modeling, we here identify the root cause of this disparity. We reveal that the morphological divergence originates from the variations in structure and chemical composition of the initial SEI layer formed on the copper (Cu) substrate. These variations arise from substrate defects that induce localized electrochemical fields, driving selective dissociation of either solvent or salt, producing SEI layers with distinct chemomechanical properties. Solvent-derived organic SEI favors whisker growth, whereas salt-derived SEI promotes particle formation. This study establishes a direct mechanistic link between SEI chemomechanical properties and Li morphology, providing design principles for tailoring SEI layers to control Li deposition

energy storage↗

Conservative solute transport processes and associated transient storage mechanisms: Comparing streams with contrasting channel morphologies, land use and land cover

Abstract Land use within a watershed impacts stream channel morphology and hydrology and, therefore, in‐stream solute transport processes and associated transient storage mechanisms. This study evaluated transport processes in two contrasting stream sites where channel morphology was influenced by the surrounding land use, land cover, climate and geologic controls: Como Creek, CO, a relatively undisturbed, high gradient, forested stream with a gravel bed and complex channel morphology, and Clear Creek, IA, an incised, low‐gradient stream with low‐permeability substrate draining an agricultural landscape. We performed conservative stream tracer injections at these sites to address the following questions: (1) How does solute transport vary between streams with differing morphologies? and (2) How does solute transport at each stream site change as a function of discharge? We analysed in‐stream tracer time series data and compared results quantifying solute attenuation in surface and subsurface transient storage zones. Significant trends were observed in these metrics with varying discharge conditions at the forested site but not at the agricultural site. There was a broad range of transport mechanisms and evidence of substantial exchange with both surface and hyporheic transient storage in the relatively undisturbed, forested stream. Changing discharge conditions activated or deactivated different solute transport mechanisms in the forested site and greatly impacted advective travel time. Conversely in the simplified agricultural stream, there was a narrow range of solute transport behaviour across flows and predominantly surface transient storage at all measured discharge conditions. These results demonstrate how channel simplification inhibits available solute transport mechanisms across varying discharge conditions.

54 ENVIRONMENTAL SCIENCES↗

Enabling Bipolar Membrane Manufacturing Using Microscopy

Bipolar membranes (BPMs) used for water treatment suffer from interface instabilities, causing premature failure and decreased performance. Recent research has highlighted the impacts of membrane morphology on mechanical behavior and performance. Improved material performance of thin film membranes requires enhanced transport properties coupled with better control of the mechanical characteristics to avoid premature failure of the film. Thus, morphology is a key parameter when developing and evaluating novel membrane materials. Microscopy offers unique advantages for nano-scale characterization of thin film membrane interfaces and morphologies. In this study, the interface junction of BPMs was evaluated using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX). BPMs were fabricated using (1) hot pressing lamination, (2) bench-scale solution casting, and (3) roll-to-roll sequential casting (R2R). Both commercial and in-house fabricated ion exchange membranes were used in the BPMs. The BPMs were comprised of a cation exchange membrane and an anion exchange membrane with a catalyst layer sandwiched in between. Cross sectional SEM and EDX images of the membrane interface junction were compared among the different fabrication techniques and materials. The bench cast catalyst layers were nonuniform compared to the R2R and hot pressed membranes, demonstrating the importance of precise catalyst application conditions. Different thicknesses of the BPMs and individual membrane layers revealed that polymer solution concentration needs to be optimized during manufacturing. This work shows that microscopy can identify key processing parameters that affect BPM interface junction quality at the microscale to enable manufacturing of high performance BPMs.

36 MATERIALS SCIENCE↗