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At least 397 records · Page 22

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DOE OSTI2019

Interference Provides Clarity: Direct Observation of 2D Materials at Fluid–Fluid Interfaces

Monolayer particles of two-dimensional (2D) materials represent a scientifically and technologically interesting class of anisotropic particles with colloidal-scale lateral sizes but sub-nanometer thicknesses. This atomic-scale thickness leads to interesting phenomena that can be exploited in next-generation thin-film technologies, and fluid-fluid interfaces provide a potentially scalable platform to confine, assemble, and deposit functional thin films of 2D materials. However, directly observing how these materials interact and assemble into a given film morphology is experimentally challenging because of their sub-nanometer thicknesses. Here, we demonstrate the ability to directly observe graphene, molybdenum disulfide (MoS2), and hexagonal boron nitride (h-BN) particles at fluid-fluid interfaces using interference reflection microscopy (IRM). Monolayer MoS2 and graphene particles demonstrated >10% optical contrast at an air-water interface, which allowed us to quantitatively analyze in situ images of self-assembled MoS2 particles and to map trajectories of interacting graphene particles. Additionally, the Brownian motion of a graphene particle was tracked and analyzed in the context of passive microrheology theory for 2D particle probes. Our results demonstrate how IRM can be used to obtain quantitative spatiotemporal information regarding the self-assembly and dynamics of 2D materials at fluid-fluid interfaces. It will have a significant impact on our ability to investigate systems of atomically thin particles at fluid-fluid interfaces, an area that has fundamental scientific importance and materials science applications but has suffered from a lack of direct, in situ observation techniques.

2D material↗

DOE OSTI2012

Improved rubber nanofillers

During this task, Silane functionalized TiO2 and HK3Ti4O4(SiO4)3 were sent to Goodyear (GY) for testing. These materials were characterized based on their interaction with the model elastomer, squalene. The Van der Waals interactions and Hamaker Constants for ZnO particles in squalene and rubber materials were characterized and it was determined that a 10-20 nm spacing was necessary between primary filler particles to maintain a stable nanocomposite. Contact angle measurements on the ZnO and ZnO-silane materials indicated that the solvent should wet the particles, and solvophobic attractions should not be present. These studies showed that the surface modification with sulfosilane coupling agents was successful, and high levels of dispersion of the particles remained possible. Further, a novel surface charging phenomenon where negative surface charging is developed in the squalene environment was observed and corroborated by measurements of particle size and of the surface modified materials in squalene. This impacts the dispersion of the particles according to the traditional colloidal interpretation of electrostatic repulsive forces between particles. Additionally, thin nanocomposite fibers were developed using electrospinning. The size and shape of the oxides did not change during the electrospinning process, although the shape of the fiber and the distribution of the particles, particularly for ZnO, was not ideal. There was an obvious increase in elastic modulus and hardness from the addition of the oxides, but differentiating the oxides, and particularly the surfactants, was difficult. The A-1289 lead to the greatest dispersion of the filler particles, while the A-1589 and the NXT produced clustered particle aggregates. This agrees with previous study of these materials in low molecular weight squalene solvent studies reported earlier. The behavior of the nanoparticle ZnO and the microparticle silica is different as well, with the ZnO being contained within the elastomer, and the SiO2 forming monolayers at the surface of the elastomer. The dynamic mechanical analysis did not show clear trends between the surface modification and the aggregate structure. In the silica particles, the NXT led to the least particle interaction, followed by the A-1289 and highest particle interaction found for the A-1589. For the nanosized ZnO, the best dispersion was found for the A-1589, with both the A-1289 and NXT exhibiting frequency dependent responses.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2014

The rheology and processing of “edge sheared” colloidal polymer opals

This paper is concerned with the rheology and processing of solvent-free core shell “polymer opals” that consist of a soft outer shell grafted to hard colloidal polymer core particles. Strong iridescent colors can be produced by shearing the material in a certain way that causes the initially disordered spheres to rearrange into ordered crystalline structures and produce colors by diffraction and interference of multiple light scattering, similar to gemstone opals. The basic linear viscoelastic rheology of a polymer opal sample was determined as a function of temperature, and the material was found to be highly viscoelastic at all tested temperatures. A Cambridge multipass rheometer was specifically modified in order to make controlled mechanical measurements of initially disordered polymer opal tapes that were sandwiched between protective polyethylene terephthalate sheets. Axial extension, simple shear, and a novel “edge shearing” geometry were all evaluated, and multiple successive experiments of the edge shearing test were carried out at different temperatures. The optical development of colloidal ordering, measured as optical opalescence, was quantified by spectroscopy using visible backscattered light. The development of opalescence was found to be sensitive to the geometry of deformation and a number of process variables suggesting a complex interaction of parameters that caused the opalescence. In order to identify aspects of the deformation mechanism of the edge shearing experiment, a separate series of in situ optical experiments were carried out and this helped indicate the extent of simple shear generated with each edge shear deformation. The results show that strong ordering can be induced by successive edge shearing deformation. The results are relevant to polymer opal rheology, processing, and mechanisms relating to ordering within complex viscoelastic fluids.

36 MATERIALS SCIENCE↗

DOE OSTI2013

A robust ligand exchange approach for preparing hydrophilic, biocompatible photoluminescent quantum dots

Graphical abstract: - Highlights: • Aqueous CdSe/ZnS QDs were prepared using polymaleic anhydrides as capping ligand. • Effect of reaction temperature and time were systematically studied in the synthesis process. • Water-soluble QDs exhibited a good stability in physiological relevant environment. • The aqueous QDs were applied as biological probe to detect human embryonic stem cell. - Abstract: This paper describes a robust ligand exchange approach for preparing biocompatible CdSe/ZnS quantum dots (QDs) to make bioprobe for effective cell imaging. In this method, polymaleic anhydride (PMA) ligand are first used to replace original hydrophobic ligand (oleic acid) and form a protection shell with multiple hydrophilic groups to coat and protect CdSe/ZnS QDs. The as-prepared aqueous QDs exhibit small particle size, good colloidal stability in aqueous solutions with a wide range of pH, salt concentrations and under thermal treatment, which are necessary for biological applications. The use of this new class of aqueous QDs for effective cell imaging shows strong fluorescence signal to human embryonic stem cell, which demonstrate that PMA coated QDs are fully satisfied with the requirements of preparing high quality biological probe.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Local elasticity in nonlinear rheology of interacting colloidal glasses revealed by neutron scattering and rheometry

The flow of colloidal suspensions is ubiquitous in nature and industry. Colloidal suspensions showcase a wide range of rheological behavior, which should be closely related to the microscopic structure of the systems. With in situ small-angle neutron scattering complemented by rheological measurements, we investigated the deformation behavior of a charge-stabilized colloidal glass at particle level undergoing steady shear. A short-lived, localized elastic response at particle level, termed as the transient elasticity zone (TEZ), was identified from the neutron spectra. The existence of the TEZ, which could be promoted by the electrostatic interparticle potential, is a signature of deformation heterogeneity: the body of fluids under shear behaves like an elastic solid within the spatial range of the TEZ but like fluid outside the TEZ. The size of the TEZ shrinks as the shear rate increases in the shear thinning region, which shows that the shear thinning is accompanied by a diminishing deformation heterogeneity. More interestingly, the TEZ is found to be the structural unit that provides the resistance to the imposed shear, as evidenced by the quantitative agreement between the local elastic stress sustained by the TEZ and the macroscopic stress from rheological measurements at low and moderate shear rates. Our findings indicate an understanding on the nonlinear rheology of interacting colloidal glasses from a micro-mechanical view.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Quincke Oscillations of Colloids at Planar Electrodes

Dielectric particles in weakly conducting fluids rotate spontaneously when subject to strong electric fields. Such Quincke rotation near a plane electrode leads to particle translation that enables physical models of active matter. In this Letter, we show that Quincke rollers can also exhibit oscillatory dynamics, whereby particles move back and forth about a fixed location. We explain how oscillations arise for micron-scale particles commensurate with the thickness of a field-induced boundary layer in the nonpolar electrolyte. This work enables the design of colloidal oscillators.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2019

Colloidal Gelation in Liquid Metals Enables Functional Nanocomposites of 2D Metal Carbides (MXenes) and Lightweight Metals

Nanomaterials dispersed in different media, such as liquids or polymers, generate a variety of functional composites with synergistic properties. In this work, we discuss liquid metals as the nanomaterials' dispersion media. For example, 2D transition-metal carbides and nitrides (MXenes) can be efficiently dispersed in liquid Ga and lightweight alloys of Al, Mg, and Li. We show that the Lifshitz theory predicts strong van der Waals attraction between nanoscale objects interacting through liquid metals. However, a uniform distribution of MXenes in liquid metals can be achieved through colloidal gelation, where particles form self-supporting networks stable against macroscopic phase segregation. This network acts as a reinforcement boosting mechanical properties of the resulting metal-matrix composite. By choosing Mg-Li alloy as an example of ultralightweight metal matrix and Ti 3 C 2 T x MXene as a nanoscale reinforcement, we apply a liquid metal gelation technique to fabricate functional nanocomposites with an up to 57% increase in the specific yield strength without compromising the matrix alloy's plasticity. MXenes largely retain their phase and 2D morphology after processing in liquid Mg-Li alloy at 700 degrees C. The 2D morphology enables formation of a strong semicoherent interface between MXene and metal matrix, manifested by biaxial strain of the MXene lattice inside the metal matrix. Finally, this work expands applications for MXenes and shows the potential for developing MXene-reinforced metal matrix composites for structural alloys and other emerging applications with metal-MXene interfaces, such as batteries and supercapacitors.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Distinctive rheological and temporal viscoelastic behaviour of alkali-activated fly ash/slag pastes: A comparative study with cement paste

This paper presents the results of the investigation on the fundamental differences in the viscoelasticity between alkali-activated fly ash/slag materials (AAMs) and cement pastes. The effects of the precursor and the activator on the rheological behaviour of AAM pastes were studied. Given the specific precursor, the activator viscosity significantly affected the AAM paste viscosity. The high viscous activator increased the plastic viscosity of AAM pastes by 4–8 times higher than that of cement paste and drastically decreased the yield stress due to viscous effects and weak colloidal interactions. Temporal changes in viscoelasticity showed that the negligible colloidal interactions between particles in AAM paste made the system non-percolated until the initial setting. This resulted in very different viscoelastic behaviour compared to the one from the well-percolated network in cement paste. Considering all results obtained in this study, the paper describes the short-term evolution of the AAM paste from the fresh condition to the initial setting.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Octo-diamond crystal of nanoscale tetrahedra with interchanging chiral motifs

Despite their simplicity, tetrahedra can assemble into diverse high- and low-density structures. Here we report a low-density ‘octo-diamond’ structure formed by nanoscale solid tetrahedra with a 64-tetrahedron unit cell containing 8 cubic-diamond subcells. The formed crystal is achiral, but is composed of chiral bilayers with alternating handedness. The left- and right-handed chirality of the bilayers, combined with the plasmonic nature of the gold tetrahedra, produces chiroptical responses at the crystal surface. We uncover that the hydrophobic substrate facilitates the arrangement of tetrahedra into irregular ring-like patterns, creating a critical, uneven topography to stabilize the observed octo-diamond structure. This study reveals a potent way to affect colloidal crystallization through particle–substrate interactions, expanding the nanoparticle self-assembly toolbox.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Solid-state synthesis of UV-plasmonic Cr2N nanoparticles

Materials that exhibit plasmonic response in the UV region can be advantageous for many applications, such as biological photodegradation, photocatalysis, disinfection, and bioimaging. Transition metal nitrides have recently emerged as chemically and thermally stable alternatives to metal-based plasmonic materials. However, most free-standing nitride nanostructures explored so far have plasmonic responses in the visible and near-IR regions. Herein, we report the synthesis of UV-plasmonic Cr2N nanoparticles using a solid-state nitridation reaction. The nanoparticles had an average diameter of 9 ± 5 nm and a positively charged surface that yields stable colloidal suspension. The particles were composed of a crystalline nitride core and an amorphous oxide/oxynitride shell whose thickness varied between 1 and 7 nm. Calculations performed using the finite element method predicted the localized surface plasmon resonance (LSPR) for these nanoparticles to be in the UV-C region (100–280 nm). While a distinctive LSPR peak could not be observed using absorbance measurements, low-loss electron energy loss spectroscopy showed the presence of surface plasmons between 80 and 250 nm (or ∼5 to 15 eV) and bulk plasmons centered around 50–62 nm (or ∼20 to 25 eV). Plasmonic coupling was also observed between the nanoparticles, resulting in resonances between 250 and 400 nm (or ∼2.5 to 5 eV).

Chemistry↗

DOE OSTI2023

Using small angle x-ray scattering to examine the aggregation mechanism in silica nanoparticle-based ambigels for improved optical clarity

Silica-based aerogels are a promising low-cost solution for improving the insulation efficiency of single-pane windows and reducing the energy consumption required for space heating and cooling. Two key material properties required are high porosity and small pore sizes, which lead to low thermal conductivity and high optical transparency, respectively. However, porosity and pore size are generally directly linked, where high porosity materials also have large pore sizes. This is unfavorable as large pores scatter light, resulting in reduced transmittance in the visible regime. In this work, we utilized preformed silica colloids to explore methods for reducing pore size while maintaining high porosity. Further, the use of preformed colloids allows us to isolate the effect of solution conditions on porous gel network formation by eliminating simultaneous nanoparticle growth and aggregation found when using typical sol–gel molecular-based silica precursors. Specifically, we used in situ synchrotron-based small-angle x-ray scattering during gel formation to better understand how pH, concentration, and colloid size affect particle aggregation and pore structure. Ex situ characterization of dried gels demonstrates that peak pore widths can be reduced from 15 to 13 nm, accompanied by a narrowing of the overall pore size distribution, while maintaining porosities of 70%–80%. Optical transparency is found to increase with decreasing pore sizes while low thermal conductivities ranging from 95 +/− 13 mW/m K are maintained. Mechanical performance was found to depend primarily on effective density and did not show a significant dependence on solution conditions. Overall, our results provide insights into methods to preserve high porosity in nanoparticle-based aerogels while improving optical transparency.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2019

Angular X-ray Cross-Correlation Analysis (AXCCA): Basic Concepts and Recent Applications to Soft Matter and Nanomaterials

Angular X-ray cross-correlation analysis (AXCCA) is a technique which allows quantitative measurement of the angular anisotropy of X-ray diffraction patterns and provides insights into the orientational order in the system under investigation. This method is based on the evaluation of the angular cross-correlation function of the scattered intensity distribution on a two-dimensional (2D) detector and further averaging over many diffraction patterns for enhancement of the anisotropic signal. Over the last decade, AXCCA was successfully used to study the anisotropy in various soft matter systems, such as solutions of anisotropic particles, liquid crystals, colloidal crystals, superlattices composed by nanoparticles, etc. This review provides an introduction to the technique and gives a survey of the recent experimental work in which AXCCA in combination with micro- or nanofocused X-ray microscopy was used to study the orientational order in various soft matter systems.

36 MATERIALS SCIENCE↗

NASA NTRS2009

Method for one-to-one polishing of silicon nitride and silicon oxide

The present invention provides a method of removing silicon nitride at about the same removal rate as silicon dioxide by CMP. The method utilizes a polishing slurry that includes colloidal silica abrasive particles dispersed in water and additives that modulate the silicon dioxide and silicon nitride removal rates such that they are about the same. In one embodiment of the invention, the additive is lysine or lysine mono hydrochloride in combination with picolinic acid, which is effective at a pH of about 8. In another embodiment of the invention, the additive is arginine in combination with picolinic acid, which is effective at a pH of about 10.

Babu, Suryadevara V.↗

NASA NTRS2004

Pumping Liquid Oxygen by Use of Pulsed Magnetic Fields

An effort is underway to develop a method of pumping small amounts of liquid oxygen by use of pulsed magnetic fields. This development is motivated by a desire to reduce corrosion and hazards of explosion and combustion by eliminating all moving pump parts in contact with the pumped oxygen. The method exploits the known paramagnetism of liquid oxygen. Since they both behave similarly, the existing theory of ferrofluids (liquids with colloidally suspended magnetic particles) is directly applicable to paramagnetic liquid oxygen. In general, the force density of the paramagnetic interaction is proportional to the magnetic susceptibility multiplied by the gradient of the square of the magnitude of the magnetic field. The local force is in the direction of intensifying magnetic field. In the case of liquid oxygen, the magnetic susceptibility is large enough that a strong magnetic-field gradient can lift the liquid in normal Earth gravitation.

Youngquist, Robert↗

DOE OSTI2018

Magnetic Field-Driven Convection for Directed Surface Patterning of Colloids

Drying sessile droplets is a promising route to transform colloidal dispersions into surface coatings, which are widely used in material design and biochemical detection. However, directing the assembly of the particles within drying droplets and achieving surface patterns beyond the well-known coffee-ring formation remain a challenge. Here, we present a new principle of directing the assembly of nonmagnetic colloidal particles dispersed in a magnetic fluid and generating unusual surface patterns. We use the ability of ferrofluids to change phases with the application of magnetic fields to program the assembly of nonmagnetic microparticles present in drying sessile droplets. We show that in the absence of external magnetic field, the superparamagnetic nanoparticles in the magnetic fluid are spontaneously transported to the droplet edge because of solvent evaporation. This nanoparticle transport leads to the formation of nanoparticle-rich edge and nanoparticle-depleted center of the drying droplet. Upon the application of a uniform external magnetic field, the asymmetry in the magnetic nanoparticle distribution drives a magnetostatic convection and finger-like instability from the droplet edge to the center. This magnetic microconvection from droplet edge-to-center reverses the particle transport from center-to-edge, well-known for drying droplets in the absence of external field. We use this magnetostatic microconvection to assemble secondary nonmagnetic microspheres in droplets, overwriting ring formation and direct their assembly into four distinct kinetically stable states. As a result, the method presented here offers an active control over the colloidal assembly achieved by drying sessile droplets and thus enables a new route for fabricating complex patterns and functional surface coating.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2021

Metallization of colloidal crystals

Colloidal crystals formed by size-asymmetric binary particles coassemble into a wide variety of colloidal compounds with lattices akin to ionic crystals. Recently, a transition from a compound phase with a sublattice of small particles to a metal-like phase in which the small particles are delocalized has been predicted computationally and observed experimentally. In this colloidal metallic phase, the small particles roam the crystal maintaining the integrity of the lattice of large particles, as electrons do in metals. A similar transition also occurs in superionic crystals, termed sublattice melting. Here, we use energetic principles and a generalized molecular dynamics model of a binary system of functionalized nanoparticles to analyze the transition to sublattice delocalization in different coassembled crystal phases as a function of temperature (T), number of grafted chains on the small particles, and number ratio between the small and large particles n s : n l . Here we find that n s : n l is the primary determinant of crystal type due to energetic interactions and interstitial site filling, while the number of grafted chains per small particle determines the stability of these crystals. We observe first-order sublattice delocalization transitions as T increases, in which the host lattice transforms from low- to high-symmetry crystal structures, including A20 → bct → bcc, A d → bct → bcc, and bcc → bcc/fcc → fcc transitions and lattices. Analogous sublattice transitions driven primarily by lattice vibrations have been seen in some atomic materials exhibiting an insulator-metal transition also referred to as metallization. We also find minima in the lattice vibrations and diffusion coefficient of small particles as a function of n s : n l , indicating enhanced stability of certain crystal structures for n s : n l values that form compounds.

36 MATERIALS SCIENCE↗

DOE OSTI2023

Microscopic activated dynamics theory of the shear rheology and stress overshoot in ultradense glass-forming fluids and colloidal suspensions

We formulate a particle and force level, activated dynamics-based statistical mechanical theory for the continuous startup nonlinear shear rheology of ultradense glass-forming hard sphere fluids and colloidal suspensions in the context of the elastically collective nonlinear Langevin equation approach and a generalized Maxwell model constitutive equation. Activated structural relaxation is described as a coupled local-nonlocal event involving caging and longer range collective elasticity which controls the characteristic stress relaxation time. Theoretical predictions for the deformation-induced enhancement of mobility, the onset of relaxation acceleration at remarkably low values of stress, strain, or shear rate, apparent power law thinning of the steady-state structural relaxation time and viscosity, a nonvanishing activation barrier in the shear thinning regime, an apparent Herschel–Buckley form of the shear rate dependence of the steady-state shear stress, exponential growth of different measures of a yield or flow stress with packing fraction, and reduced fragility and dynamic heterogeneity under deformation were previously shown to be in good agreement with experiments. The central new question we address here is the defining feature of the transient response—the stress overshoot. In contrast to the steady-state flow regime, understanding the transient response requires an explicit treatment of the coupled nonequilibrium evolution of structure, elastic modulus, and stress relaxation time. We formulate a new quantitative model for this aspect in a physically motivated and computationally tractable manner. Theoretical predictions for the stress overshoot are shown to be in good agreement with experimental observations in the metastable ultradense regime of hard sphere colloidal suspensions as a function of shear rate and packing fraction, and accounting for deformation-assisted activated motion appears to be crucial for both the transient and steady-state responses.

Mechanics↗

DOE OSTI2012

Optical Manipulation of Shape-Morphing Elastomeric Liquid Crystal Microparticles Doped with Gold Nanocrystals

We demonstrate facile optical manipulation of shape of birefringent colloidal microparticles made from liquid crystal elastomers. Using soft lithography and polymerization, we fabricate elastomeric microcylinders with weakly undulating director oriented on average along their long axes. These particles are infiltrated with gold nanospheres acting as heat transducers that allow for an efficient localized transfer of heat from a focused infrared laser beam to a submicrometer region within a microparticle. Photothermal control of ordering in the liquid crystal elastomer using scanned beams allows for a robust control of colloidal particles, enabling both reversible and irreversible changes of shape. Possible applications include optomechanics, microfluidics, and reconfigurable colloidal composites with shape-dependent self-assembly.

36 MATERIALS SCIENCE↗