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Results for “Nanoparticle Formation Mechanisms”

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 127 records · Page 7

Automated processing of environmental transmission electron microscopy images for quantification of thin film dewetting and carbon nanotube nucleation dynamics

We report scalable production of carbon nanotubes (CNTs) requires catalysts and reaction conditions that provide high nucleation efficiency. In situ characterization methods such as environmental transmission electron microscopy (ETEM) can reveal fundamental mechanisms of synthesis, but to date have primarily provided qualitative observations on small sample sizes. Here, quantitative analysis is performed using high-resolution, high-rate video capture of ETEM experimentation coupled with automated image processing, involving computer vision algorithms and convolutional neural networks. By this approach, we detect distinct nanoparticle formation from an alumina-supported iron thin film and subsequent CNT nucleation from the nanoparticles. The statistical summary of particles in each video shows that, compared to a H 2 -only atmosphere, pretreatment of the catalyst with carbon added to the H 2 atmosphere results in a smaller average particle diameter, a 2-fold increase in particle density (to 5300 particles/μm 2 ), a 3-fold increase in CNT nucleation efficiency (to 92%), and more than a 5-fold increase in CNT density (to 4800/μm 2 ). Addition of carbon during exposure to H 2 is also more effective than NH 3 at dewetting the catalyst film and increasing the CNT nucleation efficiency, in spite of NH 3 being a stronger reducing agent for iron. Insights from this study are applicable to improving CNT yield and productivity in both batch-style and continuous processes.

25 ENERGY STORAGE↗

Unravelling Magnetic Nanochain Formation in Dispersion for In Vivo Applications

Self-assembly of iron oxide nanoparticles (IONPs) into 1D chains is appealing, because of their biocompatibility and higher mobility compared to 2D/3D assemblies while traversing the circulatory passages and blood vessels for in vivo biomedical applications. In this work, parameters such as size, concentration, composition, and magnetic field, responsible for chain formation of IONPs in a dispersion as opposed to spatially confining substrates, are examined. In particular, the monodisperse 27 nm IONPs synthesized by an extended LaMer mechanism are shown to form chains at 4 mT, which are lengthened with applied field reaching 270 nm at 2.2 T. The chain lengths are completely reversible in field. Using a combination of scattering methods and reverse Monte Carlo simulations the formation of chains is directly visualized. The visualization of real-space IONPs assemblies formed in dispersions presents a novel tool for biomedical researchers. This allows for rapid exploration of the behavior of IONPs in solution in a broad parameter space and unambiguous extraction of the parameters of the equilibrium structures. Additionally, it can be extended to study novel assemblies formed by more complex geometries of IONPs.

36 MATERIALS SCIENCE↗

Microstructural and physicochemical origins of electroless copper deposition on graphite enhanced by acid pretreatment

We report Acid treatment is the most widely used surface modification method for enhancing the electroless metal deposition (EMD) on carbon reinforcement materials (CRMs) for metal matrix nanocomposites. However, specific microstructural and physicochemical origins of the enhanced EMD on carbon surfaces by acid treatments have been rarely studied. Here, we investigated the effects of the nitric acid treatment on graphite, a prototypical combination of acid treatment and CRM, on the fidelity of Cu EMD and their structural and chemical origins. Complementary materials characterizations and density functional theory calculations revealed the acid-induced formation of broken C–C/C=C graphitic bonds and resulting surface micropores on graphite; this enabled a uniform dispersion of catalytic Sn/Pd nanoparticles during pre-EMD sensitization/activation processes via spontaneous binding of Sn and Pd ions and, consequently, a much more uniform Cu layer EMD compared to the untreated graphite. We proposed a general mechanism illustrating how the acid-induced microstructural and chemical modifications of carbon surface affected the spatial uniformity of catalytic metal reduction during EMD and, finally, the quality of deposited metal layer. The results clearly reveal the origins of the enhanced EMD on carbon materials by acid treatments, providing guidelines for optimizing EMD on general CRMs for high-performance metal matrix nanocomposites.

36 MATERIALS SCIENCE↗

Reduction-Controlled Atomic Migration for Single Atom Alloy Library

Here, picturing the atomic migration pathways of catalysts in a reactive atmosphere is of central significance for uncovering the underlying catalytic mechanisms and directing the design of high-performance catalysts. Here, we describe a reduction-controlled atomic migration pathway that converts nanoparticles to single atom alloys (SAAs), which has remained synthetically challenging in prior attempts due to the elusive mechanism. We achieved this by thermally treating the noble-metal nanoparticles M (M = Ru, Rh, Pd, Ag, Ir, Pt, and Au) on metal oxide (CuO) supports with H2/Ar. Atomic-level characterization revealed such conversion as the synergistic consequence of noble metal-promoted H2 dissociation and concomitant CuO reduction. The observed atomic migration pathway offers an understanding of the dynamic mechanisms study of nanomaterials formation and catalyst design.

36 MATERIALS SCIENCE↗

Theoretical studies of chemical reactions related to the formation and growth of polycyclic aromatic hydrocarbons (PAH) and molecular properties of their key intermediates (Final Progress Report)

The formation mechanisms of polycyclic aromatic hydrocarbons, (PAHs) – organic molecules carrying fused benzene rings – are of great interest to scientists and engineers due to their importance in combustion chemistry and astrochemistry. On Earth, PAHs are largely produced in incomplete combustion of fossil fuel and are considered as critical precursors to unwanted soot particles leading to combustion inefficiency and causing air pollution along with detrimental health effects. Simple PAH molecules initially formed in the gas phase, are further involved in a build-up process in combustion flames leading to larger PAH, bowl-shaped nanostructures, fullerenes, and solid-phase species including carbonaceous dust, graphene particles, and soot. In deep space, PAH and their derivatives are potential key intermediates and nucleation sites leading eventually to carbonaceous nanoparticles (“interstellar grains”). Therefore, the understanding of the key processes in the synthesis of PAHs along with their precursors and their degradation mechanisms in combustion systems and in interstellar, circumstellar, and planetary atmospheric environments will provide critical insights into how complex aromatic structures, carbonaceous nanoparticles, and fullerenes are formed and destroyed. Achieving this understanding is an important step in the development of the efficient combustion processes and of the ecofriendly devices with reduced environmental pollution as well as technological strategies for the production of hydrogen and solid carbon through thermal or plasma-assisted pyrolysis of natural gas and biomass. Also, the understanding of the key processes of PAH and soot growth will help in our comprehension of chemical evolution in the universe. Detailed information on the mechanisms and reliable rate constants of the key elementary chemical reactions involved in PAH formation and destruction processes and in inception of soot particles is often missing, with the main deficiencies being the absence of temperature- and pressure-dependent rate constants for the broad range of conditions occurring in various terrestrial and interstellar processes and the lack of data on the reaction products and their branching ratios. Complementary to experimental studies, these gaps in knowledge can be filled by using quantum chemical calculations of reaction potential energy surfaces providing us with accurate energies of reaction products, intermediates, and transition states, revealing the reaction mechanism, and giving the molecular properties required to compute rate constants for relevant reaction steps and product branching ratios using the RRKM-Master Equation (ME) method. Molecular dynamics (MD) simulations can be used in cases when a reaction rate cannot be properly described by statistical theories. During the terminal renewal project period we employed these ab initio/RRKM-ME and MD approaches to complete our studies on several key reactions relevant to the formation/growth of PAH and inception of soot particles including (1) the reaction mechanism and kinetics of the resonance stabilized fulvenallenyl radical with propargyl and C 3 H 4 isomers; (2) the reaction mechanism and kinetics for the C + indene and C 2 + styrene reactions producing naphthyl or azulenyl radicals in low-temperature environments; (3) the MD study of non-equilibrium dimerization of acepyrene and coronene and its radical. The information derived from our theoretical calculations contributed to a better fundamental understanding of the reaction mechanisms and provide missing critical kinetic data to improve combustion models of hydrocarbon fuels and astrochemical models of the growth of carbonaceous molecules and particles in cold molecular clouds, circumstellar envelopes, and planetary atmospheres.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Controlling process instability for defect lean metal additive manufacturing

The process instabilities intrinsic to the localized laser-powder bed interaction cause the formation of various defects in laser powder bed fusion (LPBF) additive manufacturing process. Particularly, the stochastic formation of large spatters leads to unpredictable defects in the as-printed parts. Here we report the elimination of large spatters through controlling laser-powder bed interaction instabilities by using nanoparticles. The elimination of large spatters results in 3D printing of defect lean sample with good consistency and enhanced properties. We reveal that two mechanisms work synergistically to eliminate all types of large spatters: (1) nanoparticle-enabled control of molten pool fluctuation eliminates the liquid breakup induced large spatters; (2) nanoparticle-enabled control of the liquid droplet coalescence eliminates liquid droplet colliding induced large spatters. The nanoparticle-enabled simultaneous stabilization of molten pool fluctuation and prevention of liquid droplet coalescence discovered here provide a potential way to achieve defect lean metal additive manufacturing.

36 MATERIALS SCIENCE↗

Two Mesoporous Domains Are Better Than One for Catalytic Deconstruction of Polyolefins

Catalytic hydrogenolysis of polyolefins into valuable liquid, oil, or wax-like hydrocarbon chains for second-life applications is typically accompanied by the hydrogen-wasting co-formation of low value volatiles, notably methane, that increase greenhouse gas emissions. Catalytic sites confined at the bottom of mesoporous wells, under conditions in which the pore exerts the greatest influence over the mechanism, are capable of producing less gases than unconfined sites. A new architecture was designed to emphasize this pore effect, with the active platinum nanoparticles embedded between linear, hexagonal mesoporous silica and gyroidal cubic MCM-48 silica (mSiO 2 /Pt/MCM-48). This catalyst deconstructs polyolefins selectively into ~C 20 –C 40 paraffins and cleaves C–C bonds at a rate (TOF = 4.2 ± 0.3 s –1 ) exceeding that of materials lacking these combined features while generating negligible volatile side products including methane. The time-independent product distribution is consistent with a processive mechanism for polymer deconstruction. In contrast to time- and polymer length-dependent products obtained from non-porous catalysts, mSiO 2 /Pt/MCM-48 yields a C 28 -centered Gaussian distribution of waxy hydrocarbons from polyolefins of varying molecular weight, composition, and physical properties, including low-density polyethylene, isotactic polypropylene, ultrahigh-molecular-weight polyethylene, and mixtures of multiple, post-industrial polyolefins. Here, coarse-grained simulation reveals that the porous-core architecture enables the paraffins to diffuse away from the active platinum site, preventing secondary reactions that produce gases.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Tuscaloosa Marine Shale Laboratory

The Tuscaloosa Marine Shale (TMS) in Louisiana and Mississippi is an Upper Cretaceous source rock formation sandwiched between the sands of the upper and lower Tuscaloosa sections. The TMS is believed to be the source rock for underlying prolific Tuscaloosa sand formation. The TMS has an unproven estimate of 7,000,000,000 bbls of recoverable oil while its current total average production is about 3,000 bbls of oil per day in 2017. In 2013 and 2014, more than 80 wells were drilled horizontally into the TMS that were fractured using multi-stage fracturing technology. The results from this have been mixed, but recent production for several wells show an appealing initial oil production rate of more than 1000 bbl/day. The preliminary core analysis by industry partners and a few literature studies shows that the TMS is one of the most clay-rich and sensitive shales to water. Due to these and other technical problems, there is high risk for the economic development of TMS compared to other shale plays. The experiences of major industrial players in the TMS show the necessity of open and collaborative efforts to better understand the critical gaps in the development of this challenging and potentially highly economic shale play to enable more cost-efficient and environmentally-sound recovery from this unconventional liquid-rich shale play. The overall objective of this project is to form a consortium of science and industry partners to address the following six major objectives using scientific and technical approaches: 1. To improve wellbore integrity by better understanding the sources of the wellbore instability issues, proposing innovative mud and cement design for the TMS. 2. To improve formation evaluation using laboratory techniques for the evaluation of mineralogical composition, organic content, and produced-water chemistry as well as well log and geophysical analysis. 3. To determine the role of geologic discontinuities on fracture growth and shale creep behavior using digital image correlation technique. 4. To investigate the application of stable CO 2 foam and super-hydrophobic proppants for improved reservoir stimulation. 5. To better understand the nature of water/hydrocarbon/CO 2 flow in clay and organic-rich formation and the role of water/fluid interaction on recovery. 6. To prepare better socio-economic environment for TMS development by community engagement. Subsequently, the TMS virtual laboratory conducted testing and analysis of various properties of rock and formation fluids from the TMS, including but not limited to the following: Analyzing reports and logs to better understand the source of wellbore instability in TMS wells; Experiments to design a customized cement based on TMS requirements; Experiments to obtain the mineralogical and geochemical composition of TMS samples; Seismic analysis of TMS geophysical data to better predict total organic carbon (TOC) content and brittleness in TMS; Well log analysis to better estimate the TOC and geo-mechanical properties of TMS; Experiments on formation water to understand the chemistry of produced water; Experiments to determine the role of lamination and natural fractures on fracture propagation or rock deformation using digital image correlation technique in in-direct tensile tests, semi-circular bend test and creep tests Experiments to determine the stability and rheological properties of nanoparticle-stabilized CO 2 foam in TMS rock samples; Experiments to determine fluid dynamics in un-propped TMS fractures and the role of nano-coating of proppants on fluid dynamics in fractures with proppants; Micro-fluidics experiments to enhance the understanding of fluid dynamics in tight liquidrich pores with high clay content; Socio-economic studies to better engage communities in TMS development.

58 GEOSCIENCES↗

X-ray linear dichroic ptychography

Biominerals such as seashells, coral skeletons, bone, and tooth enamel are optically anisotropic crystalline materials with unique nanoscale and microscale organization that translates into exceptional macroscopic mechanical properties, providing inspiration for engineering new and superior biomimetic structures. Using Seriatopora aculeata coral skeleton as a model, here, we experimentally demonstrate X-ray linear dichroic ptychography and map the c-axis orientations of the aragonite (CaCO 3 ) crystals. Linear dichroic phase imaging at the oxygen K-edge energy shows strong polarization-dependent contrast and reveals the presence of both narrow (<35°) and wide (>35°) c-axis angular spread in the coral samples. These X-ray ptychography results are corroborated by four-dimensional (4D) scanning transmission electron microscopy (STEM) on the same samples. Evidence of co-oriented, but disconnected, corallite subdomains indicates jagged crystal boundaries consistent with formation by amorphous nanoparticle attachment. We expect that the combination of X-ray linear dichroic ptychography and 4D STEM could be an important multimodal tool to study nano-crystallites, interfaces, nucleation, and mineral growth of optically anisotropic materials at multiple length scales.

4D scanning transmission electron microscopy↗

Recent developments in catalyst-related PEM fuel cell durability

Cost and durability remain the two major barriers to the widespread commercialization of polymer electrolyte membrane fuel cell (PEMFC)-based power systems, especially for the most impactful but challenging fuel cell electric vehicle (FCEV) application. Commercial FCEVs are now on the road; however, their PEMFC systems do not meet the cost targets established by the U.S. Department of Energy, primarily due to the high platinum loading needed on the cathode to achieve the requisite performance and lifetime. Furthermore, while the activities of a number of commercial Pt-based alloy cathode catalysts exceed the beginning-of-life (BOL) targets, these activities, and the overall cathode performance, degrade via a variety of mechanisms described herein. Degradation is mitigated in current FCEVs by utilizing a cathode catalyst with a lower BOL activity (e.g., much lower transition metal alloy content and larger BOL nanoparticle size), necessitating higher catalyst loadings, and through the utilization of system controls that avoid conditions known to exacerbate degradation processes, such as limiting the fuel cell stack voltage range. The design and development of active and robust materials and eliminating the need for vehicle mitigation strategies would greatly simplify the operating system, allowing for greater transient operation, avoiding large hybridization, and curtailing of fuel cell power. Although system mitigation strategies have provided the near-term pathway for FCEV commercialization, material-specific solutions are required to further reduce costs and improve operability and efficiency. Future material developments should focus on stabilization of the electrode structure and minimization of the catalyst particle susceptibility to dissolution caused by oxide formation and reduction over PEMFC cathode-relevant operating potentials plus minimization of support corrosion. Ex situ accelerated stress tests have provided insight into the processes responsible for material and performance degradation and will continue to provide useful information on the relative stability of materials and benchmarks for robust and stable materials-based solutions not requiring system mitigation strategies to achieve adequate lifetime.

25 ENERGY STORAGE↗

Exosomes secreted from mesenchymal stem cells mediate the regeneration of endothelial cells treated with rapamycin by delivering pro-angiogenic microRNAs

Highlights: • MSC-derived exosomes play an important role in promoting endothelial regeneration treated with rapamycin in vitro. • A distinct class of exosomal miRNAs is identified to be tightly related to endothelial regeneration. • The therapeutic effects of MSC-exosomes may be ascribed to the delivery of pro-angiogenic miRNAs to endothelial cells. • MSC-exosomes may serve as a cell-free therapy for clinical treatment of delayed endothelial healing after DES implantation. Delayed endothelial healing after drug eluting stent (DES) implantation is a critical clinical problem in treatment of coronary artery diseases. Exosomes exhibit proangiogenic potential in a variety of ischemic diseases. However, the association of exosomes with endothelial regeneration after DES implantation has been rarely reported. In this study, we aimed to investigate the therapeutic effects of mesenchymal stem cell (MSC)-derived exosomes on endothelial cells treated with rapamycin and explore the potential mechanisms of MSC-derived exosomes in promoting endothelial regeneration. Exosomes were isolated from MSCs by ultracentrifugation and identified by transmission electron microscopy, nanoparticle tracking analysis, and Western blot assay. The in vitro effects of MSC-derived exosomes on the proliferation and migration of endothelial cells treated with rapamycin were evaluated by integrated experiment, cell counting kit-8, scratch, tube formation, and transwell assays. And the apoptosis of rapamycin-induced endothelial cells loaded with MSC-derived exosomes was detected using TUNEL and Annexin-V FITC and PI double-staining assays. The microRNA (miRNA) cargo of MSC-derived exosomes was identified by high-throughput RNA sequencing. Pro-angiogenic miRNAs and key pathways were further characterized. Our results indicated that MSC-derived exosomes could be ingested into umbilical vein endothelial cells (HUVECs) and significantly enhanced cell proliferation rate, migratory and tube-forming capabilities in vitro. MSC-derived exosomes also inhibited the apoptosis of HUVECs induced by rapamycin. A distinct class of exosomal miRNAs was further identified, including six miRNAs tightly related to neovasculogenesis. Silencing the expression of exosomal miRNA-21–5p and let-7c-5p attenuated the pro-proliferative and pro-migratory capacity of MSC-derived exosomes. Moreover, functional enrichment analysis indicated that metabolic pathways might contribute to reendothelialization. This study highlights a proregenerative effect of MSC-derived exosomes in vitro, which may be partly explained by the delivery of pro-angiogenic miRNAs to endothelial cells.

60 APPLIED LIFE SCIENCES↗

Quantifying multipoint ordering in alloys

A central problem in multicomponent lattice systems is to systematically quantify multipoint ordering. Ordering in such systems is often described in terms of pairs, even though this is not sufficient when three-point and higher-order interactions are included in the Hamiltonian. Current models and parameters for multipoint ordering are often only applicable for very specific cases or require approximating a subset of correlated occupational variables on a lattice as being uncorrelated. In this paper, cluster order parameters are introduced to systematically quantify arbitrary multipoint ordering motifs in substitutional systems through direct calculations of normalized cluster probabilities. These parameters can describe multipoint chemical ordering in crystal systems with multiple sublattices, multiple components, and systems with reduced symmetry. These are defined in this paper and applied to quantify four-point chemical ordering motifs in platinum/palladium alloy nanoparticles that are of practical interest to the synthesis of catalytic nanocages. Impacts of chemical ordering on nanocage stability are discussed. It is demonstrated that approximating four-point probabilities from superpositions of lower-order pair probabilities is not sufficient in cases where three- and four-body terms are included in the energy expression. Furthermore, conclusions about the formation mechanisms of nanocages may change significantly when using common pair approximations.

36 MATERIALS SCIENCE↗

Shape Control of Colloidal Semiconductor Nanocrystals through Thermodynamically Driven Aggregative Growth

The optoelectronic properties of colloidal semiconductor nanocrystals (NCs) can be manipulated by changing their geometric shapes. The precise synthetic control over particle morphologies, however, has remained elusive. Conventional growth techniques rely on the kinetic assembly of atomic units, where supersaturation and precipitation processes can lead to a broad distribution of particle shapes. In this paper, we demonstrate that replacing atomic precursors with small-size nanocrystals as building blocks for larger colloids offers an easier, more predictive control over nanoparticle shape evolution. The reported growth strategy is illustrated via shape-selective syntheses of CdSe and CdS NC cubes, spheres, rods, as well as unprecedented “donut” and ring-like structures. Growth of desired particle morphologies was achieved by choosing an appropriate reaction solvent that minimizes the surface free energy through a unique shape formation. This so-called "aggregative growth mechanism" is explained using a thermodynamic model for interacting viscous colloids. We expect that this novel growth strategy will offer a viable platform for shape–selective synthesis of many inorganic colloids, providing pathways to optimizable optoelectronic materials.

36 MATERIALS SCIENCE↗

Covalently Linked, Two-Dimensional Quantum Dot Assemblies

Using nanoscale building blocks to construct hierarchical materials is a radical new branch point in materials discovery that promises new structures and emergent functionality. Understanding the design principles that govern nanoparticle assembly is critical to moving this field forward. By exploiting mixed ligand environments to target patchy nanoparticle surfaces, we have demonstrated a novel method of colloidal quantum dot (QD) assembly that gives rise to 2D structures. The equilibration of solutions of spherical and quasispherical QDs, including CdS, CdSe, and InP, with 2,2'-bipyridine-5,5'-diacrylic acid resulted in the preferential formation of 2D assemblies over the course of days as determined by transmission electron microscopy analysis. Small-angle X-ray scattering confirms the existence of the QD assemblies in solution. The dependence of the assembly on linker properties (length and rigidity), linker concentration, and total concentration was investigated, together with the data point to a mechanism involving ligand redistribution to create a patchy surface that maximizes the steric repulsion of neighboring QDs. By operating in an underexchanged regime, the arising patchiness results in enthalpically preferred directions of cross-linking that can be accessed by thermal equilibration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Methane Activation on Metal-Doped (111) and (100) Ceria Surfaces with Charge-Compensating Oxygen Vacancies

Reducing the temperature for methane activation is an important objective that would benefit many technological applications. In this work we explore the possibility to achieve this goal using single atom catalysts (SACs) on ceria surfaces. In particular, we focus on Ag SACs, which have recently been suggested to be promising catalysts for both the oxidation of molecular hydrogen and CH 4 activation. The rate limiting step of methane activation on ceria is the breaking of the first C-H bond. Using first principles calculations, we investigate this reaction on CeO 2 (111) and (100) surfaces, which are both frequently exposed on ceria nanoparticles. For undoped ceria, our results show that the dissociation of CH 4 to CH 3 + H has a lower barrier on the (001) surface than on the (111) one. On both surfaces, the presence of Ag enhances the binding of CH 4 to the surface and reduces the activation energy for its dissociation. Interestingly, the formation of methanol via the Mars-van Krevelen mechanism has a slightly lower energy barrier than the dissociation of CH 4 to CH 3 + H on Ag-doped CeO 2 (111), suggesting that methanol is a likely product of methane activation on this surface. Here, a novel aspect of our work relative to previous studies on CH 4 activation over transition metal doped ceria is that we mainly focus on stable surface structures where each Ag dopant substituting a Ce atom forms a complex with a surface oxygen vacancy (VO). Our results show that these Ag-VO complexes play a critical role and accounting for their presence is essential for a proper description of the surface reactivity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In situ multimodal imaging for nanoscale visualization of tribofilm formation

A third of the energy from fuel combustion in passenger car gasoline engines is lost due to friction. Carefully designed engine lubricants can recover some of these losses by reducing friction and wear by forming a nanometer-scale chemico-physico tribofilm between surfaces. Accordingly, attention has focused on developing oil formulations that form low-friction tribofilms. However, analyses of resultant tribofilms are typically conducted after tribo-tests with conventional characterization tools and do not offer insights into tribofilm formation and evolution, precluding information critical to tuning tribofilm properties. In this work, we developed a unique multimodal methodology based on Atomic Force Microscopy (AFM) with local probe heating for in situ tribological studies that activates friction modifiers and simultaneously captures the evolution of friction and surface roughness, with nanometer resolution. As a platform to demonstrate the ability of this methodology to visualize dynamics of tribofilm formation in situ, we apply it to molybdenum-based friction modifiers to distinguish key factors in their functionality and correlate nanoscale AFM and Friction Force Microscopy data to bench tribo-tests used in the industry. To decode the formation mechanisms observed in situ and underlying chemistry of tribofilms, we performed ab initio Molecular Dynamics (AIMD) simulations at comparable conditions. AIMD simulations confirmed both nanoscale and bench tribo-test results and showed deviations in molecular organization in tribofilms that are formed from different molybdenum-based friction modifiers that corroborates with surface functionality. With this innovative methodology, we demonstrate proof-of-principle in situ formation of molybdenum-based tribofilms directly on steel surfaces that could be applied generally to studying tribofilm formation.

36 MATERIALS SCIENCE↗

Strain-Induced Nanocavitation in Block Copolymer Thin Films for High Performance Filtration Membranes

A new pore formation process was investigated for the manufacture of composite ultrafiltration membranes. Phase-separated block copolymer (BCP) thin films supported on a compliant macroporous poly(ether sulfone) (PES) support craze under tensile strain, leaving behind pores of predictable size based on the self-assembled nanoscopic domains. The high aspect ratio pores formed in this process were used to create membranes that were highly permeable (959 L/(m 2 h bar) with near complete rejection of 40 nm diameter gold nanoparticles (AuNP). By use of BCP’s inherent ability to cavitate under strain, tedious block removal steps are avoided. Membranes can thus be prepared in a simple, roll-to-roll ready, one-step process. In this initial study, BCP craze formation and filtration performance were characterized for various polymer types, molecular weights, and thicknesses. Furthermore, all these factors influenced the BCP’s thin film morphology, mechanical performance, deformation mechanism, and ultimately filtration performance. This work demonstrates a possible new path toward achieving scalable, BCP-based ultrafiltration membranes.

36 MATERIALS SCIENCE↗

Three-dimensional strain dynamics govern the hysteresis in heterogeneous catalysis

Understanding catalysts strain dynamic behaviours is crucial for the development of cost-effective, efficient, stable and long-lasting catalysts. Here, we reveal in situ three-dimensional strain evolution of single gold nanocrystals during a catalytic CO oxidation reaction under operando conditions with coherent X-ray diffractive imaging. We report direct observation of anisotropic strain dynamics at the nanoscale, where identically crystallographically-oriented facets are qualitatively differently affected by strain leading to preferential active sites formation. Interestingly, the single nanoparticle elastic energy landscape, which we map with attojoule precision, depends on heating versus cooling cycles. The hysteresis observed at the single particle level is following the normal/inverse hysteresis loops of the catalytic performances. This approach opens a powerful avenue for studying, at the single particle level, catalytic nanomaterials and deactivation processes under operando conditions that will enable profound insights into nanoscale catalytic mechanisms.

36 MATERIALS SCIENCE↗