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DOE OSTI2022

Discovery of two-dimensional binary nanoparticle superlattices using global Monte Carlo optimization

Binary nanoparticle (NP) superlattices exhibit distinct collective plasmonic, magnetic, optical, and electronic properties. Here, we computationally demonstrate how fluid-fluid interfaces could be used to self-assemble binary systems of NPs into 2D superlattices when the NP species exhibit different miscibility with the fluids forming the interface. We develop a basin-hopping Monte Carlo (BHMC) algorithm tailored for interface-trapped structures to rapidly determine the ground-state configuration of NPs, allowing us to explore the repertoire of binary NP architectures formed at the interface. By varying the NP size ratio, interparticle interaction strength, and difference in NP miscibility with the two fluids, we demonstrate the assembly of an array of exquisite 2D periodic architectures, including AB-, AB 2 -, and AB 3 -type monolayer superlattices as well as AB-, AB 2 -, A 3 B 5 -, and A 4 B 6 -type bilayer superlattices. Our results suggest that the interfacial assembly approach could be a versatile platform for fabricating 2D colloidal superlattices with tunable structure and properties.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Magnetic anomalies associated with domain wall freezing and coupled electron hopping in magnetite nanorods

Magnetite has fascinated researchers for decades, due to its wide range of applications from spintronics to biomedicine. Despite a large body of works aimed at its magnetic properties, no consensus has been reached on the physical origin of the low temperature magnetic anomalies observed in magnetite. Although, a lot of work has been done in studying magnetite nanoparticles, but studies on the low temperature anomalies in those nanoparticles still remains unresearched. We report on the observation of the low temperature magnetic anomalies in highly crystalline, stoichiometric Fe 3 O 4 nanorods and relate them to the coupled electron hopping relaxation process and domain wall motion. Both DC and AC susceptibility show the presence of a hump around 35 K, which is associated with the relaxation of Fe +2 extra electrons. Radiofrequency transverse susceptibility (TS) measurements indicated a noticeable increase in anisotropy field below ~ 25 K, which is attributed to the rearrangement of Fe +2 electrons in the octahedral sites. TS experiments also revealed the domain wall freezing below ~35 K. Our combined DC, AC and TS susceptibility studies shed light on the complex nature of the lowtemperature magnetic behavior in nanostructured magnetite.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Scanning SQUID study of ferromagnetism and superconductivity in infinite-layer nickelates

Infinite-layer nickelates R 1-x Sr x NiO 2 (R = La, Pr, Nd) are a class of superconductors with structural similarities to cuprates. Although long-range antiferromagnetic order has not been observed for these materials, magnetic effects such as antiferromagnetic spin fluctuations and spin-glass behavior have been reported. Different experiments have drawn different conclusions about whether the pairing symmetry is s or d wave. In this paper, we applied a scanning superconducting quantum interference device (SQUID) to probe the magnetic behavior of film samples of three infinite-layer nickelates (La 0.85 Sr 0.15 NiO 2 , Pr 0.8 Sr 0.2 NiO 2 , and Nd 0.775 Sr 0.225 NiO 2 ) grown on SrTiO 3 (STO), each with a nominal thickness of 20 unit cells. In all three films, we observed a ferromagnetic background. We also measured the magnetic susceptibility above the superconducting critical temperature in Pr 0.8 Sr 0.2 NiO 2 and La 0.85 Sr 0.15 NiO 2 and identified a non-Curie-Weiss dynamic susceptibility. Both magnetic features are likely due to NiO x nanoparticles. We investigated superconductivity in Pr 0.8 Sr 0.2 NiO 2 and Nd 0.775 Sr 0.225 NiO 2 , which exhibited inhomogeneous diamagnetic screening. The superfluid density inferred from the diamagnetic susceptibility in relatively homogeneous regions shows T-linear behavior in both samples. Finally, we observed superconducting vortices in Nd 0.775 Sr 0.225 NiO 2 . We determined a Pearl length of 330 µm for Nd 0.775 Sr 0.225 NiO 2 at 300 mK, both from the strength of the diamagnetism and from the size and shape of the vortices. These results highlight the importance of considering NiO x particles when interpreting experimental results for these films.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

Templated Mesoporous Silica Outer Shell for Controlled Silver Release of a Magnetically Recoverable and Reusable Nanocomposite for Water Disinfection

Here, we encapsulated Fe 3 O 4 @SiO 2 @Ag (MS-Ag), a bifunctional magnetic silver core–shell structure, with an outer mesoporous silica (mS) shell to form an Fe 3 O 4 @SiO 2 @ 2 Ag@mSiO 2 (MS-Ag-mS) nanocomposite using a cationic CTAB (cetyltrimethylammonium bromide) micelle templating strategy. The mS shell acts as protection to slow down the oxidation and detachment of the AgNPs and incorporates channels to control the release of antimicrobial Ag + ions. Results of TEM, STEM, HRSEM, EDS, BET, and FTIR showed the successful formation of the mS shells on MS-Ag aggregates 50–400 nm in size with highly uniform pores ~4 nm in diameter that were separated by silica walls ~2 nm thick. Additionally, the mS shell thickness was tuned to demonstrate controlled Ag + release; an increase in shell thickness resulted in an increased path length required for Ag + ions to travel out of the shell, reducing MS-Ag-mS’ ability to inhibit E. coli growth as illustrated by the inhibition zone results. Through a shaking test, the MS-Ag-mS nanocomposite was shown to eradicate 99.99+% of a suspension of E. coli at 1 × 10 6 CFU/mL with a silver release of less than 0.1 ppb, well under the EPA recommendation of 0.1 ppm. This high biocidal efficiency with minimal silver leach is ascribed to the nanocomposite’s mS shell surface characteristics, including having hydroxyl groups and possessing a high degree of structural periodicity at the nanoscale or “smoothness” that encourages association with bacteria and retains high Ag + concentration on its surface and in its close proximity. Furthermore, the nanocomposite demonstrated consistent antimicrobial performance and silver release levels over multiple repeated uses (after being recovered magnetically because of the oxidation-resistant silica-coated magnetic Fe 3 O 4 core). It also proved effective at killing all microbes from Long Island Sound surface water. The described MS-Ag-mS nanocomposite is highly synergistic, easy to prepare, and readily recoverable and reusable and offers structural tunability affecting the bioavailability of Ag + , making it excellent for water disinfection that will find wide applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2025

Field-Driven Out-of-Equilibrium Collective Patterns for Swarm Micro-Robotics

Soft robotics has been rapidly advancing, offering significant improvements over traditional rigid robotic systems through the use of compliant materials that enhance adaptability and interaction with the environment. However, current approaches face critical challenges, including the reliance on complex “top-down” fabrication techniques and the difficulty of wireless powering and control at the microscale. Swarm robotics introduces a paradigm shift, leveraging collective dynamics to achieve cooperative and adaptable behaviors among multiple robotic units. Inspired by nature, this “bottom-up” approach enables swarm robots to execute task-specific reconfigurations, enhancing flexibility and robustness. Field-driven active colloids emerge as a promising platform for swarm microrobotics, capable of self-propulsion and self-organization into dynamic collective patterns under external field excitation and manipulation. These systems mimic biologically inspired swarm behaviors, such as flocking and vortex formation, providing a versatile foundation for designing innovative swarm microrobots. Here, this review discusses the principles of electric and magnetic field-driven collective self-organization, focusing on the particle dynamics, the emergence of collective swarm patterns, and illustrative examples of functional swarm microrobots. It concludes with future perspectives on harnessing these systems for adaptive, scalable, and multifunctional microrobotic applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2024

Improved Methods for Modeling Functional Transition Metal Compounds in Complex Environments: Ground States, Excited States, and Spectroscopies

Rapid advances in energy applications require new theory and computational models to provide guidance for interpretation of experimental results and mechanistic understanding. New theory development is necessary to treat systems of increasing complexity, size, and relevance to real applications. Functional transition metal compounds, including molecules, clusters, nanoparticles, surfaces, and solids, provide particular promise for magnetic, optical, and catalytic applications. However, such systems can be exceptionally challenging to model. To make progress in understanding and designing transition metal compounds for energy applications, theory must be able to simulate such systems in complex environments, as well as simulate the spectra of such complex systems to provide direct connections with experiment. Leveraging the independent expertise of the team’s members, this project aimed to make inroads to the theoretical and computational challenges associated with studying transition metal compounds, their reaction chemistry, photophysics and photochemistry, and response to spectroscopic interrogation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

Size Dependence of Lattice Parameter and Electronic Structure in CeO2 Nanoparticles

Intrinsic properties of a compound (e.g. electronic structure, crystallographic structure, optical and magnetic properties) define notably its chemical and physical behavior. In the case of nanomaterials, these fundamental properties depend on the occurrence of quantum mechanical size effects and on the considerable increase of the surface to bulk ratio. However, the literature on this size-dependence and on the involved mechanisms is quite elusive and scarce. Here, we explore the size-dependence of both crystal and electronic properties of CeO2 nanoparticles (NPs) with different sizes by state-of-the art spectroscopic techniques. XRD, XPS and HERFD-XANES demonstrate that the as-synthesized NPs crystallize in the fluorite structure and they are predominantly composed of CeIV ions. The strong dependence of the lattice parameter with the NPs size was attributed to the presence of adsorbed species at the NPs surface thanks to FTIR and TGA measurements. In addition, the size-dependence of the eg level in the Ce LIII XANES spectra was experimentally observed by HERFD-XANES and confirmed by theoretical calculations.

Lanthanide, CeO2, HEFRD-XANES, Electronic structur↗

DOE OSTI2020

Erratum to: Soft- and reactive landing of ions onto surfaces: concepts and applications

Soft- and reactive landing of mass-selected ions is gaining attention as a promising approach for the precisely-controlled preparation of materials on surfaces that are not amenable to deposition using conventional methods. A broad range of ionization sources and mass filters are available that make ion soft-landing a versatile tool for surface modification using beams of hyperthermal (<100?eV) ions. The ability to select the mass-to-charge ratio of the ion, its kinetic energy and charge state, along with precise control of the size, shape, and position of the ion beam on the deposition target distinguishes ion soft landing from other surface modification techniques. Soft- and reactive landing have been used to prepare interfaces for practical applications as well as precisely-defined model surfaces for fundamental investigations in chemistry, physics, and materials science. For instance, soft- and reactive landing have been applied to study the surface chemistry of ions isolated in the gas-phase, prepare arrays of proteins for high-throughput biological screening, produce novel carbon-based and polymer materials, enrich the secondary structure of peptides and the chirality of organic molecules, immobilize electrochemically-active proteins and organometallics on electrodes, create thin films of complex molecules, and immobilize catalytically active organometallics as well as ligated metal clusters. In addition, soft landing has enabled investigation of the size-dependent behavior of bare metal clusters in the critical subnanometer size regime where chemical and physical properties do not scale predictably with size. The morphology, aggregation, and immobilization of larger bare metal nanoparticles, which are directly relevant to the design of catalysts as well as improved memory and electronic devices, have also been studied using ion soft landing. This review article begins in section 1 with a brief introduction to the existing applications of ion soft- and reactive landing. Section 2 provides an overview of the ionization sources and mass filters that have been used to date for soft landing of mass-selected ions. A discussion of the competing processes that occur during ion deposition as well as the types of ions and surfaces that have been investigated follows in section 3. Section 4 discusses the physical phenomena that occur during and after ion soft landing, including retention and reduction of ionic charge along with factors that impact the efficiency of ion deposition. The influence of soft landing on the secondary structure and biological activity of complex ions is addressed in section 5. Lastly, an overview of the structure and mobility as well as the catalytic, optical, magnetic, and redox properties of bare ionic clusters and nanoparticles deposited onto surfaces is presented in section 6. © 2015 Wiley Periodicals, Inc. Mass Spec Rev 35:439–479, 2016.

Johnson, Grant E.↗

DOE OSTI2023

Development of molecular cluster models to probe pyrite surface reactivity

Abstract The recent discovery that anaerobic methanogens can reductively dissolve pyrite and utilize dissolution products as a source of iron and sulfur to meet their biosynthetic demands for these elements prompted the development of atomic‐scale nanoparticle models, as maquettes of reactive surface sites, for describing the fundamental redox steps that take place at the mineral surface during reduction. The given report describes our computational approach for modeling n (FeS 2 ) nanoparticles originated from mineral bulk structure. These maquettes contain a comprehensive set of coordinatively unsaturated Fe (II) sites that are connected via a range of persulfide (S 2 2− ) ligation. In addition to the specific maquettes with n = 8, 18, and 32 FeS 2 units, we established guidelines for obtaining low‐energy structures by considering the pattern of ionic, covalent, and magnetic interactions among the metal and ligand sites. The developed models serve as computational nano‐reactors that can be used to describe the reductive dissolution mechanism of pyrite to better understand the reactive sites on the mineral, where microbial extracellular electron‐transfer reactions can occur.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Iron-based nanoparticles and grains

Example nanoparticles may include an iron-based core, and a shell. The shell may include a non-magnetic, anti-ferromagnetic, or ferrimagnetic material. Example alloy compositions may include an iron-based grain, and a grain boundary. The grain boundary may include a non-magnetic, anti-ferromagnetic, or ferrimagnetic material. Example techniques for forming iron-based core-shell nanoparticles may include depositing a shell on an iron-based core. The depositing may include immersing the iron-based core in a salt composition for a predetermined period of time. The depositing may include milling the iron-based core with a salt composition for a predetermined period of time. Example techniques for treating a composition comprising core-shell nanoparticles may include nitriding the composition.

Wang, Jian-Ping↗

DOE OSTI2023

Iron-based nanoparticles and grains

Wang, Jian-Ping↗

DOE OSTI2020

Shell-mediated control of surface chemistry of highly stoichiometric magnetite nanoparticles

Magnetite (Fe 3 O 4 ) nanoparticles are one of the most studied nanomaterials for different nanotechnological and biomedical applications. However, Fe 3 O 4 nanomaterials gradually oxidize to maghemite (γ-Fe 2 O 3 ) under conventional environmental conditions leading to changes in their functional properties that determine their performance in many applications. Here we propose a novel strategy to control the surface chemistry of monodisperse 12 nm magnetite nanoparticles by means of a 3 nm-thick Zn-ferrite epitaxial coating in core/shell nanostructures. We have carried out a combined Mössbauer spectroscopy, dc magnetometry, X-ray photoelectron spectroscopy and spatially resolved electron energy loss spectroscopy study on iron oxide and Fe 3 O 4 /Zn 0.6 Fe 2.4 O 4 core/shell nanoparticles aged under ambient conditions for 6 months. Our results reveal that while the aged iron oxide nanoparticles consist of a mixture of γ-Fe 2 O 3 and Fe 3 O 4 , the Zn-ferrite-coating preserves a highly stoichiometric Fe 3 O 4 core. Therefore, the aged core/shell nanoparticles present a sharp Verwey transition, an increased saturation magnetization and the possibility of tuning the effective anisotropy through exchange-coupling at the core/shell interface. The inhibition of the oxidation of the Fe 3 O 4 cores can be accounted for in terms of the chemical nature of the shell layer and an epitaxial crystal symmetry matching between the core and the shell.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2025

In Situ MOF Pyrolysis Construction of Hierarchical Porous Co‐Nanoparticles/Carbon Cloth Composites for Enhanced Electromagnetic Wave Shielding and Absorption

The development of high-performance electromagnetic protection materials integrating broadband absorption and effective shielding capabilities is hindered by challenges in simultaneously optimizing multiple electromagnetic properties through conventional material designs. This study pioneers a hierarchical porous Co nanoparticle/carbon cloth (Co/CC) composite via controlled annealing of a Co-MOF precursor on carbon cloth. The Co-MOF served a dual role as both magnetic source and pore-forming agent, enabling in situ generation of uniformly dispersed Co nanoparticles and creation of abundant pores/interfaces on the CC fibers during pyrolysis. This unique architecture synergistically enhanced dielectric loss (via interfacial/dipolar polarization) and magnetic loss (via natural resonance, exchange interactions, and eddy currents), significantly improving impedance matching. The hierarchical pores further functioned as integrated “absorption–reflection” units for efficient electromagnetic energy attenuation. Consequently, the Co/CC composite annealed at 800°C (Co/CC-800) achieves minimum reflection loss (−40.69 dB) and 120% effective absorption bandwidth extension (6.16 GHz) as a filler, and exhibits superior electromagnetic interference shielding effectiveness (46.66 dB) as an integrated component. Significantly, Co/CC-800 demonstrated robust photothermal and electrothermal conversion capabilities, ensuring operational stability in ice-covered and humid harsh environments. This work pioneers a pore-structure-mediated strategy to harmonize dielectric–magnetic synergy, providing a new paradigm for designing advanced multifunctional electromagnetic protection materials.

dielectric‐magnetic synergy↗

DOE OSTI2023

A Telomerase-Activated Magnetic Resonance Imaging Probe for Consecutively Monitoring Tumor Growth Kinetics and In Situ Screening Inhibitors

Telomerase has long been considered as a biomarker for cancer diagnosis and a therapeutic target for drug discovery. Detecting telomerase activity in vivo could provide more direct information of tumor progression and response to drug treatment, which, however, is hampered by the lack of an effective probe that can generate an output signal without a tissue penetration depth limit. Here in this study, using the principle of distance-dependent magnetic resonance tuning, we constructed a telomerase-activated magnetic resonance imaging probe (TAMP) by connecting superparamagnetic ferroferric oxide nanoparticles (SPFONs) and paramagnetic Gd-DOTA (Gd(III) 1,4,7,10- tetraazacyclododecane-1,4,7,10-tetraazacyclododecane-1,4,7,10-tet-raacetic acid) complexes via telomerase-responsive DNA motifs. Upon telomerase-catalyzed extension of the primer in TAMP, Gd-DOTA-conjugated oligonucleotides can be liberated from the surface of SPFONs through a DNA strand displacement reaction, restoring the T 1 signal of the Gd-DOTA for a direct readout of the telomerase activity. Here we show that, by tracking telomerase activity, this probe provides consistent monitoring of tumor growth kinetics during progression and in response to drug treatment and enables in situ screening of telomerase inhibitors in whole-animal models. This study provides an alternative toolkit for cancer diagnosis, treatment response assessment, and anticancer drug screening.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Impact of Surface Chemistry of Ultrasmall Superparamagnetic Iron Oxide Nanoparticles on Protein Corona Formation and Endothelial Cell Uptake, Toxicity, and Barrier Function

Ultrasmall superparamagnetic iron oxide nanoparticles (USPIONs) have been investigated for biomedical applications, including novel contrast agents, magnetic tracers for tumor imaging, targeted drug delivery vehicles, and magneto-mechanical actuators for hyperthermia and thrombolysis. Despite significant progress, recent clinical reports have raised concerns regarding USPION safety related to endothelial cell dysfunction; however, there is limited information on factors contributing to these clinical responses. The influence of USPION surface chemistry on nanoparticle interactions with proteins may impact endothelial cell function leading to adverse responses. Therefore, the goal of this study was to assess the effects of carboxyl-functionalized USPION (CU) or amine-functionalized USPION (AU) (approximately 30 nm diameter) on biological responses in human coronary artery endothelial cells. Increased protein adsorption was observed for AU compared with CU after exposure to serum proteins. Exposure to CU, but not AU, resulted in a concentration-dependent decrease in cell viability and perinuclear accumulation inside cytoplasmic vesicles. Internalization of CU was correlated with endothelial cell functional changes under non-cytotoxic conditions, as evidenced by a marked decreased expression of endothelial-specific adhesion proteins (eg, vascular endothelial-cadherin and platelet endothelial cell adhesion molecule-1) and increased endothelial permeability. Evaluation of downstream signaling indicated endothelial permeability is associated with actin cytoskeleton remodeling, possibly elicited by intracellular events involving reactive oxygen species, calcium ions, and the nanoparticle cellular uptake pathway. This study demonstrated that USPION surface chemistry significantly impacts protein adsorption and endothelial cell uptake, viability, and barrier function. This information will advance the current toxicological profile of USPION and improve development, safety assessment, and clinical outcomes of USPION-enabled medical products.

Toxicology↗

DOE OSTI2024

Emergent Properties from Three-Dimensional Assemblies of (Nano)particles in Confined Spaces

The assembly of (nano)particles into compact hierarchical structures yields emergent properties not found in the individual constituents. The formation of these structures relies on a profound knowledge of the nanoscale interactions between (nano)particles, which are often designed by researchers aided by computational studies. These interactions have an effect when the (nano)particles are brought into close proximity, yet relying only on diffusion to reach these closer distances may be inefficient. Recently, physical confinement has emerged as an efficient methodology to increase the volume fraction of (nano)particles, rapidly accelerating the time scale of assembly. Specifically, the high surface area of droplets of one immiscible fluid into another facilitates the controlled removal of the dispersed phase, resulting in spherical, often ordered, (nano)particle assemblies. In this review, we discuss the design strategies, computational approaches, and assembly methods for (nano)particles in confined spaces and the emergent properties therein, such as trigger-directed assembly, lasing behavior, and structural photonic color. Finally, we provide a brief outlook on the current challenges, both experimental and computational, and farther afield application possibilities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Shape-induced superstructure formation in concentrated ferrofluids under applied magnetic fields

The field-induced ordering of concentrated ferrofluids based on spherical and cuboidal maghemite nanoparticles is studied using small-angle neutron scattering, revealing a qualitative effect of the faceted shape on the interparticle interactions as shown in the structure factor and correlation lengths. Whereas a spatially disordered hard-sphere interaction potential with a short correlation length is found for ~9 nm spherical nanoparticles, nanocubes of a comparable particle size exhibit a more pronounced interparticle interaction and the formation of linear arrangements. Analysis of the anisotropic two-dimensional pair distance correlation function gives insight into the real-space arrangement of the nanoparticles. On the basis of the short interparticle distances found here, oriented attachment, i.e. a face-to-face arrangement of the nanocubes, is likely. The unusual field dependence of the interparticle correlations suggests a field-induced structural rearrangement.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Evidence of Cooperative Effects for the Fe(phen) 2 (NCS) 2 Spin Crossover Molecular Complex in Polyaniline Plus Iron Magnetite

The spin crossover complex Fe(phen) 2 (NCS) 2 and its composite, Fe(phen) 2 (NCS) 2 , combined with the conducting polymer polyaniline (PANI) plus varying concentrations of iron magnetite (Fe 3 O 4 ) nanoparticles were studied. A cooperative effect is evident from the hysteresis width in the plot of magnetic susceptibility multiplied by temperature versus temperature (χ m T versus T) for Fe(phen) 2 (NCS) 2 with PANI plus varying concentrations of Fe 3 O 4 nanoparticles. The hysteresis width in the composites vary no more than 2 K with respect to the pristine Fe(phen) 2 (NCS) 2 spin crossover crystallites despite the fact that there exists a high degree of miscibility of the Fe(phen) 2 (NCS) 2 spin crossover complex with the PANI. The Fe 3 O 4 nanoparticles in the Fe(phen) 2 (NCS) 2 plus PANI composite tend to agglomerate at higher concentrations regardless of the spin state of Fe(phen) 2 (NCS) 2 . Of note is that the Fe 3 O 4 nanoparticles are shown to be antiferromagnetically coupled with the Fe(phen) 2 (NCS) 2 when Fe(phen) 2 (NCS) 2 is in the high spin state.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗