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DOE OSTI2014

Synthesis and Characterization of Supported Cobalt-Manganese Nanoparticles as Model Catalysts for Fischer-Tropsch Synthesis

Supported Co is an effective catalyst for the Fischer-Tropsch synthesis of various hydrocarbon products that can be converted to diesel. Recent studies have shown that the formation of methane can be suppressed and the formation of C 5+ products enhanced by promoting Co with Mn. Because the activity and product selectivity of Co-based catalysts are dependent on the size of Co nanoparticles and the extent of Co promotion by Mn, it is desirable to understand these effects by investigating the performance of Co nanoparticles with well-defined size and elemental composition. The present study was undertaken with the aim of producing well-defined nanoparticles of Co and Co-Mn and then supporting them on silica. Co and Co-Mn particles were synthesized through the polyol reduction of Co and Mn acetylacetonates. By controlling synthesis conditions, Co particles with diameters of 7-10 nm and similarly sized Co-Mn (Mn/Co=0.1) particles were prepared. XRD and elemental mapping with scanning TEM-energy-dispersive X-ray spectroscopy and scanning TEM-electron energy loss spectroscopy studies suggested that most of the Mn species was associated with the Co particles. Ex situ prepared Co and Co-Mn nanoparticles were first supported on silica and then investigated for the catalytic activity for the Fischer-Tropsch synthesis. The turnover frequencies and product distributions obtained with silica-supported Co and Co-Mn nanoparticles were similar to those obtained with catalysts prepared by using the conventional incipient wetness impregnation method. However, the rate of CO consumption per mass of Co was much lower for the catalysts produced by supporting ex situ prepared nanoparticles. This effect was attributed to the sintering of the nanoparticles during their calcination and reduction. Magnetic interactions among nanoparticles during their immobilization and thermal pretreatment were identified as the primary cause of sintering. Balancing yin and yang energy: The immobilization of well-defined cobalt-manganese nanoparticles on porous supports leads to the formation of Fischer-Tropsch catalysts with turnover frequencies and product selectivities comparable to those of conventionally prepared catalysts. The catalytic activity per cobalt mass is found to be significantly lower owing to sintering. Finally, magnetic interactions among nanoparticles during immobilization and thermal pretreatment are identified as the primary cause of this phenomenon.

cobalt↗

DOE OSTI2017

The Role of Gas in Determining Image Quality and Resolution During In Situ Scanning Transmission Electron Microscopy Experiments

As gas-solid heterogeneous catalytic reactions are molecular in nature, a full mechanistic understanding of the process requires atomic scale characterization under realistic operating conditions. While atomic resolution imaging has become a routine in modern high-vacuum (scanning) transmission electron microscopy ((S)TEM), both image quality and resolution nominally degrade when reaction gases are introduced. In this work, we systematically assess the effects of different gases at various pressures on the quality and resolution of images obtained at room temperature in the annular dark field STEM imaging mode using a differentially pumped (DP) gas cell. This imaging mode is largely free from inelastic scattering effects induced by the presence of gases and retains good imaging properties over a wide range of gas mass/pressures. We demonstrate the application of the ESTEM with atomic resolution images of a complex oxide alkane oxidation catalyst MoVNbTeOx (M1) immersed in light and heavy gas environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Surface and Structural Investigation of a MnO x Birnessite‐Type Water Oxidation Catalyst Formed under Photocatalytic Conditions

Abstract Catalytically active MnO x species have been reported to form in situ from various Mn‐complexes during electrocatalytic and solution‐based water oxidation when employing cerium(IV) ammonium ammonium nitrate (CAN) oxidant as a sacrificial reagent. The full structural characterization of these oxides may be complicated by the presence of support material and lack of a pure bulk phase. For the first time, we show that highly active MnO x catalysts form without supports in situ under photocatalytic conditions. Our most active 4 MnO x catalyst (∼0.84 mmol O 2 mol Mn −1 s −1 ) forms from a Mn 4 O 4 bearing a metal–organic framework. 4 MnO x is characterized by pair distribution function analysis (PDF), Raman spectroscopy, and HR‐TEM as a disordered, layered Mn‐oxide with high surface area (216 m 2 g −1 ) and small regions of crystallinity and layer flexibility. In contrast, the S MnO x formed from Mn 2+ salt gives an amorphous species of lower surface area (80 m 2 g −1 ) and lower activity (∼0.15 mmol O 2 mol Mn −1 s −1 ). We compare these catalysts to crystalline hexagonal birnessite, which activates under the same conditions. Full deconvolution of the XPS Mn2p 3/2 core levels detects enriched Mn 3+ and Mn 2+ content on the surfaces, which indicates possible disproportionation/comproportionation surface equilibria.

Deibert, Benjamin J.↗

DOE OSTI2017

Stimulation of synaptoneurosome glutamate release by monomeric and fibrillated α-synuclein

The α-synuclein protein exists in vivo in a variety of covalently modified and aggregated forms associated with Parkinson's disease (PD) pathology. However, the specific proteoform structures involved with neuropathological disease mechanisms are not clearly defined. Since α-synuclein plays a role in presynaptic neurotransmitter release, an in vitro enzyme-based assay was developed to measure glutamate release from mouse forebrain synaptoneurosomes (SNs) enriched in synaptic endings. Glutamate measurements utilizing SNs from various mouse genotypes (WT, over-expressers, knock-outs) suggested a concentration dependence of α-synuclein on calcium/depolarization-dependent presynaptic glutamate release from forebrain terminals. In vitro reconstitution experiments with recombinant human α-synuclein proteoforms including monomers and aggregated forms (fibrils, oligomers) produced further evidence of this functional impact. Notably, brief exogenous applications of fibrillated forms of α-synuclein enhanced SN glutamate release but monomeric forms did not, suggesting preferential membrane penetration and toxicity by the aggregated forms. However, when applied to brain tissue sections just prior to homogenization, both monomeric and fibrillated forms stimulated glutamate release. Immuno-gold and transmission electron microscopy (TEM) detected exogenous fibrillated α-synuclein associated with numerous SN membranous structures including synaptic terminals. Western blots and immuno-gold TEM were consistent with SN internalization of α-synuclein. Additional studies revealed no evidence of gross disruption of SN membrane integrity or glutamate transporter function by exogenous α-synuclein. Finally, overall excitotoxicity, due to enhanced glutamate release in the face of either overexpressed monomeric α-synuclein or extrasynaptic exposure to fibrillated α-synuclein, should be considered as a potential neuropathological pathway during the progression of PD and other synucleinopathies.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2016

Enamel ribbons, surface nodules, and octacalcium phosphate in C57BL/6 Amelx -/- mice and Amelx +/- lyonization

Amelogenin is required for normal enamel formation and is the most abundant protein in developing enamel. Methods. Amelx +/+ , Amelx +/- and Amelx -/- molars and incisors from C57BL/6 mice were characterized using RT-PCR, Western blotting, dissecting and light microscopy, immunohistochemistry (IHC), transmission electron microscopy (TEM), scanning electron microscopy (SEM), backscattered SEM (bSEM), nanohardness testing, and X-ray diffraction. No amelogenin protein was detected by Western blot analyses of enamel extracts from Amelx -/- mice. Amelx -/- incisor enamel averaged 20.3±3.3 μm in thickness, or only 1/6th that of the wild-type (122.3±7.9 μm). Amelx -/- incisor enamel nanohardness was 1.6 Gpa, less than half that of wild-type enamel (3.6 Gpa). Amelx +/- incisors and molars showed vertical banding patterns unique to each tooth. IHC detected no amelogenin in Amelx -/- enamel and varied levels of amelogenin in Amelx +/- incisors, which correlated positively with enamel thickness, strongly supporting lyonization as the cause of the variations in enamel thickness. TEM analyses showed characteristic mineral ribbons in Amelx +/+ and Amelx -/- enamel extending from mineralized dentin collagen to the ameloblast. The Amelx -/- enamel ribbons were not well-separated by matrix and appeared to fuse together, forming plates. Furthermore, x-ray diffraction determined that the predominant mineral in Amelx -/- enamel is octacalcium phosphate (not calcium hydroxyapatite). Amelx -/- ameloblasts were similar to wild-type ameloblasts except no Tomes’ processes extended into the thin enamel. Amelx -/- and Amelx +/- molars both showed calcified nodules on their occlusal surfaces. Histology of D5 and D11 developing molars showed nodules forming during the maturation stage. Amelogenin forms a resorbable matrix that separates and supports, but does not shape early secretory stage enamel ribbons. Amelogenin may facilitate the conversion of enamel ribbons into hydroxyapatite by inhibiting the formation of octacalcium phosphate. Finally, amelogenin is necessary for thickening the enamel layer, which helps maintain ribbon organization and development and maintenance of the Tomes process.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2023

Structure and properties of bottlebrush polyelectrolyte complexes

Abstract Structural variation of polyelectrolytes has been shown to play an important role in altering polyelectrolyte complex (PEC) properties in recent years. However, molecular‐level details such as polyelectrolyte architecture remain underdeveloped. Here, we use a combination of ring‐opening metathesis polymerization (ROMP), atom‐transfer radical polymerization (ATRP), and postpolymerization reactions to create densely branched bottlebrushes of poly(dimethylamino ethyl methcacrylate) and poly(tert‐butyl methacrylate) with high molecular weights (MDa), which we then convert into fully charged and densely branched bottlebrushes of poly(trimethylaminoethyl methacrylate) (PTMAEMA) and poly(methacrylic acid) (PAA). We investigate the structure and properties of bottlebrush polyelectrolyte complexes (BPECs) using optical microscopy, rheology, cryogenic transmission electron microscopy (Cryo‐TEM), and small‐angle X‐ray scattering (SAXS). Bottlebrush polyelectrolyte complexes are white solids, which exhibit gel‐like mechanical properties, which we attribute to sidechain interpenetration. Using a combination of Cryo‐TEM and SAXS, we are able to outline the structural development of BPECs, detailing how the network topology, sidechain conformation, and interdigitation spacing changes as a function of salt. Our results provide a foundation for further exploration of branched architectures within polyelectrolyte complexation.

Polymer Science↗

DOE OSTI2017

Ion transport properties of mechanically stable symmetric ABCBA pentablock copolymers with quaternary ammonium functionalized midblock

Anion exchange membranes (AEMs) are a promising class of materials for applications that require selective ion transport, such as fuel cells, water purification, and electrolysis devices. Studies of structure–morphology–property relationships of ion-exchange membranes revealed that block copolymers exhibit improved ion conductivity and mechanical properties due to their microphase-separated morphologies with well-defined ionic domains. While most studies focused on symmetric diblock or triblock copolymers, here, the first example of a midblock quaternized pentablock AEM is presented. A symmetric ABCBA pentablock copolymer was functionalized to obtain a midblock brominated polymer. Solution cast films were then quaternized to obtain AEMs with resulting ion exchange capacities (IEC) ranging from 0.4 to 0.9 mmol/g. Despite the relatively low IEC, the polymers were highly conductive (up to 60 mS/cm Br- at 90 °C and 95%RH) with low water absorption (<25 wt %) and maintained adequate mechanical properties in both dry and hydrated conditions. X-ray scattering and transmission electron microscopy (TEM) revealed formation of cylindrical non-ionic domains in a connected ionic phase.

Ertem, SP↗

DOE OSTI2014

Laser-Induced Self-Assembled Nanostructures on Electron-Transparent Substrates

Currently, one of the challenges in high-resolution transmission electron microscopy (TEM) studies of nanomaterials is to make contamination-free materials in a simple and time-efficient way. We demonstrate a method that combines nanosecond-pulsed laser dewetting of thin films with a film float-off technique to realize nanostructures (NSs) on electron-transparent substrates in a robust and rapid manner. NSs of metal (Ag) and bimetals (AgCo, AuCo) ranging from 20 to 150 nm are synthesized on thin carbon film deposited on mica substrates. The NS/carbon system is subsequently transferred onto TEM grids by a float-off process resulting from debonding of the carbon from mica due to their contrasting hydrophobic nature. Our process enables the fabrication of different NSs on flexible and electron-transparent substrates.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Quantized Grain Boundary States Promote Nanoparticle Alignment During Imperfect Oriented Attachment

Oriented attachment (OA) has become a well-recognized mechanism for the growth of metal, ceramic, and biomineral crystals. While many computational and experimental studies of OA have shown that particles can attach with some misorientation then rotate to remove adjoining grain boundaries, the underlying atomistic pathways for this “Imperfect OA” process remain the subject of debate. In this paper, molecular dynamics and in situ TEM were used to probe the crystallographic evolution of up to 30 gold and copper nanoparticles during aggregation. It was found that Imperfect OA occurs because (1) grain boundaries become quantized when their size is comparable to the separation between constituent dislocations and (2) kinetic barriers associated with the glide of grain boundary dislocations are small. In support of these findings, TEM experiments show the formation of a single crystal aggregate after annealing 9 initially misoriented, agglomerated particles with evidence of dislocation slip and twin formation during particle/grain alignment. These observations motivate future work on assembled nanocrystals with tailored defects and call for a revision of Read-Shockley models for grain boundary energies in nanocrystalline materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Uncovering the Size-dependent Thermal Solid Transformation of Akaganéite

Investigating the structural evolution and phase transformation of iron oxides is crucial for gaining a deeper understanding of geological changes on diverse planets and preparing oxide materials suitable for industrial applications. In this study, we employed in-situ heating techniques in conjunction with transmission electron microscopy (TEM) observations and ex-situ characterization to thoroughly analyze the thermal solid-phase transformation of akaganéite one-dimensional (1D) nanostructures with varying diameters. Our findings offer compelling evidence for a size-dependent morphology evolution in akaganéite 1D nanostructures, which can be attributed to the transformation from akaganéite to maghemite (?-Fe2O3) and subsequent crystal growth. Specifically, we observed that akaganéite nanorods with a diameter of around 50 nm transformed into hollow polycrystalline maghemite nanorods, which demonstrated remarkable stability without arresting crystal growth under continuous heating. In contrast, smaller akaganéite nanoneedles or nanowires with a diameter ranging from 20 to 8 nm displayed a propensity for forming single-crystal nanoneedles or nanowires through phase transformation and densification. By manipulating the size of the precursors, we have developed a straightforward method for the synthesis of single-crystal and polycrystalline maghemite nanowires through solid-phase transformation. These significant findings provide new insights into the size-dependent structural evolution and phase transformation of iron oxides at the nanoscale.

Wang, Xiang↗

DOE OSTI2019

Imaging of Unstained DNA Origami Triangles with Electron Microscopy

Imaging of scaffolded DNA and DNA origami nanostructures has been dominated by atomic force microscopy of samples immobilized on bulk substrates. Less commonly used are electron microscopy techniques, typically carried out after negative staining of DNA structures or by using cryo-transmission electron microscopy (TEM). In this work, direct imaging of unstained DNA origami on common electron-transparent substrates with utilizing high angular annular dark field scanning transmission electron microscopy (HAADF-STEM) is reported. This approach establishes a method for depositing and imaging intact DNA triangles with mass-thickness contrast sufficient to measure the scaffold-to-scaffold distances and the length of the triangle's seam. The signal-to-noise ratio (SNR) of the DNA supported on amorphous carbon as a function of the carbon thickness is measured on three types of commercially available TEM grids. This allows for edge detection of ≈1 nm height DNA triangles on carbon substrates as thick as ≈25 nm. Observations on the effect on SNR with the imaging modes are discussed. The effect of cation concentration used for pretreating the grid on the image resolution is also explored. Finally, this work presents proof-of-concept results demonstrating that electron microscopy can be used to resolve key elements of the DNA origami triangle without the use of staining protocols.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Electron Microscopy Approaches to Unraveling the Structure of Amorphous Materials

Determining atomic structures in crystalline materials—where atoms are arranged in rigid, periodic lattices—has been highly successful using probes such as electrons, X-rays, and neutrons. In contrast, amorphous materials, despite their ubiquity and technological importance, remain far more challenging to characterize with comparable accuracy and precision. This review highlights existing, emerging, and potential (scanning) transmission electron microscopy ((S)TEM) techniques for probing short- and medium-range order in amorphous materials. Approaches ranging from high-resolution (S)TEM imaging and selected electron diffraction pattern to four-dimensional STEM (4D-STEM) based pair distribution function, fluctuation electron microscopy, tomography, ptychography, and spectroscopic methods are discussed, emphasizing their ability to provide complementary insights across multiple length scales—from sub-angstrom local environments to nanometer-scale correlations. Here, we further explore the promise of multimodal and correlative strategies, as well as the growing role of machine learning and physics-informed AI in enabling real-time, quantitative interpretation of complex structural signatures. Together, these advances point toward a future where electron microscopy not only reveals the hidden order in amorphous systems but also establishes robust structure–property relationships, paving the way for materials innovation in disordered matter.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Comparison of the Microstructure and Flux Pinning Properties of Polycrystalline YBa{sub 2}Cu{sub 3}O{sub 7-d} Containing Zn{sub 0.95}Mn{sub 0.05}O or Al{sub 2}O{sub 3} Nanoparticles

Here we compare the microstructure and flux pinning properties of polycrystalline YBa{sub 2}Cu{sub 3}O{sub 7-d} (Y-123 or YBCO) containing either Al{sub 2}O{sub 3} or Zn{sub 0.95}Mn{sub 0.05}O nanoparticles. Samples were prepared using a standard solid-state reaction process, and nanoparticles were added up to a concentration of 0.1 wt%. The crystal structure, microstructure, electrical and magnetic properties were analyzed using X-ray diffraction, scanning electron microscopy and transmission electron microscopy (TEM), and electrical resistivity and DC magnetization measurements, respectively. TEM observations showed that the addition of Zn{sub 0.95}Mn{sub 0.05}O resulted in a high density of fine twins and a variety of interacting microstructures, while Al{sub 2}O{sub 3} addition resulted in a high density of Al-rich nanoscale inhomogeneities embedded in the Y-123 matrix. Flux pinning forces were determined, and predominant pinning mechanisms in the prepared samples were proposed. We evaluated the superconducting properties of YBCO considering the effects of adding insulating or magnetic nanoparticles.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Investigation of Polypropylene-Montmorillonite Clay Nanocomposite Films Containing a Pro-degradant Additive

This paper investigates the performance of polypropylene (PP) incorporated with montmorillonite (MMT) nanoclay, maleic anhydride grafted PP (PP-g-MAH), and pro-degradant additive (TDPA®), which provides additional benefits of increasing biodegradability. A twin-screw extruder was used to compound PP, MMT, PP-g-MAH, and TDPA, and the extruded nanocomposite films were collected for testing, and their mechanical, thermal, barrier, oxo-biodegradability, and morphological properties were evaluated. Tensile test, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), oxygen permeability test, soil burial test, X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscope (SEM) analysis were used to investigate these properties. Increasing MMT content from 1 to 3 phr increases tensile strength and Young’s modulus of the neat PP samples up to ca.45% and 27% respectively. Improvement of thermal properties for neat PP samples was observed by increasing MMT content from 1 to 3 phr. However, at 4 phr MMT content, both mechanical and thermal properties of nanocomposites dropped slightly. For soil buried samples, DSC and TGA results revealed significant changes in the thermal properties for PP samples containing TDPE additive compared to neat PP, clearly confirming the effectiveness of this TDPA additive in promoting oxo-biodegradation process of PP. Similarly weight loss evaluation result shows that about 4% weight loss for sample (PP/TD), which is PP and TDPA blend only, compared to neat PP. However, increasing MMT content from 1 to 4 phr slightly reduced weight loss of PP from 3.5 to 1.5%, respectively, for 6 month soil exposure period, which indicates that increasing MMT content was detrimental to the degradation process. For higher MMT content, the oxygen permeability of PP nanocomposites was decreased by 46% of the corresponding values for neat PP. The XRD and TEM results confirmed the exfoliation structure of the nanocomposites. The morphological change after soil burial test was studied using scanning electron microscopy (SEM).

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Utilization of a Novel Chitosan/Clay/Biochar Nanobiocomposite for Immobilization of Heavy Metals in Acid Soil Environment

An organic–inorganic composite of chitosan, nanoclay, and biochar (named as MTCB) was chosen to develop a bionanocomposite to simultaneously immobilize Cu, Pb, and Zn metal ions within the contaminated soil and water environments. The composite material was structurally and chemically characterized with the XRD, TEM, SEM, BET, and FT-IR techniques. XRD and TEM results revealed that a mixed exfoliated/intercalated morphology was formed upon addition of small amounts of nanoclay (5% by weight). Batch adsorption experiments showed that the adsorption capacity of MTCB for Cu{sup 2+}, Pb{sup 2+}, and Zn{sup 2+} were much higher than that of the pristine biochar sample (121.5, 336, and 134.6 mg g{sup −1} for Cu{sup 2+}, Pb{sup 2+}, and Zn{sup 2+}, respectively). The adsorption isotherm for Cu{sup 2+} and Zn{sup 2+} fitted satisfactorily to a Freundlich model while the isotherm of Pb{sup 2+} was best represented by a Temkin model. That the adsorption capacity increased with increasing temperature is indicative of the endothermic nature of the adsorption process. According to the FTIR analysis, the main mechanism involved in immobilization of metals is binding with –NH{sub 2} groups. Results from this study indicated that modification of biochar by chitosan/clay nanocomposite enhances its potential capacity for immobilization of heavy metals, rendering the bionanocomposite into an efficient heavy metal sorbent in mine-impacted acidic waters and soils.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Green Synthesis and Antioxidant Study of Silver Nanoparticles of Root Extract of Sageretia thea and Its Role in Oxidation Protection Technology

Development of environmentally friendly synthesis of nanoparticles is one of the important areas of research in nanotechnology. In present study silver naopartticles (AgNPs) of root extract of Sageretia thea (S. thea) were synthesized at room temperature. The synthesized AgNPs were characterized by UV. Visible spectroscopy (UV), scanning electron microscopy (SEM), X-ray diffraction (XRD), energy dispersive spectroscopy (EDX), transmission electron microscopy (TEM), dynamic light scattering (DLS) and Fourier transform infrared (FT-IR) spectroscopy. Formation of AgNPs was confirmed by visual examination the colour change from yellow to brick red due to surface Plasmon resonance band at 435 nm. SEM and TEM analysis of synthesized AgNPs revealed spherical morphology with average particle size 25 nm. Crystalline nature of the AgNPs in face centered cubic structure is evident from the selected area electron diffraction (SAED) and XRD pattern. The presence of elemental Ag was confirmed by EDX analysis at 3kv. Different functional groups which responsible for reduction and stabilization of reaction medium was confirmed by FTIR spectroscopy. The biosynthesized AgNPs showed strong DPPH and dye protection radical scavenging assay while modest hydrogen peroxide radical scavenging assay as compare to crude extract. The present investigations suggest that biosynthesized nanoparticles have a high potential for use in the preparation of drugs used against various diseases and also a promising candidate for many medical applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Effect of Silver Doped Zinc Oxide as Nanofiller for the Development of Biopolymer Nanocomposites from Chitin and Cashew Gum

Nanocomposites based on chitin (CT) and cashew gum (CG) with different concentrations of silver doped zinc oxide nanoparticles (Ag–ZnO) were prepared and characterized by FTIR, UV, XRD, TEM, SEM, DSC, TGA, electrical conductivity measurements. FTIR spectra showed that the characteristic absorption band of the blend was shifted to a higher frequency in nanocomposites, indicating the intermolecular interaction between the blend and nanoparticles. The change in the UV absorption of nanocomposites relative to that of pure blend indicated the successful encapsulation of crystalline metal oxide nanoparticles in the blend matrix. XRD patterns showed that the diffraction peak of the composites were shifted near to the metal oxide peak which indicated that the surface of Ag–ZnO was perpendicular to CT/CG and changed from a semi-crystalline nature to a crystalline structure. The morphological analysis using SEM and TEM showed a uniform attachment of nanoparticles within the CT/CG blend. DSC analysis showed the increased glass transition temperature by the addition of nanoparticles. Thermal stability of nanocomposites was higher than the blend and thermal stability increased with an increase in the content of nanoparticles. The different electrical properties such as AC conductivity and dielectric behaviour of the composites were increased with an increased loading of nanoparticles.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2018

Fabrication of Engineered Silica-Functionalized-Polyanilines Nanocomposites for Water Decontamination of Cadmium and Lead

In this study, two novel functionalized silica nanocomposites were synthesized via covalent bonding with nanopolyaniline (NPANI) and crosslinked nanopolyaniline (CrossNPANI) to produce [NSi-NPANI] and [NSi-CrossNPANI], respectively. The two nanocomposites were portrayed by SEM, FT-IR, HR-TEM, BET-surface and TGA. The HR-TEM images of [NSi-NPANI] and [NSi-CrossNPANI] confirmed the particle size in the range 14.28–21.43 and 26.19–35.71 nm, respectively and these two nanocomposites were successfully applied to remove divalent cadmium and lead from solutions. As compared to nanosilica [NSi] sorbent, the maximum capacity values of the two nanocomposites for divalent cadmium and lead were identified to increase from 100–250 µmole g{sup −1} (pH 1.0) to 750–800 µmole g{sup −1} (pH 7.0) and from 400–1050 µmole g{sup −1} (pH 1.0) to 650–1350 µmole g{sup −1} (pH 6.0), at the optimum conditions. The adsorption data were compared using two and three parameter equations based on Langmuir, Freundlich, Temkin, Dubinin-Radushkevich, Redlish-Peterson and sips models. The kinetic study of [NSi-NPANI] and [NSi-CrossNPANI] revealed that the pseudo-second order kinetic was the best model to explain the kinetic data for cadmium(II) and lead(II). The free energy of sorption (ΔG{sup o}), enthalpy (ΔH{sup o}), and entropy (ΔS{sup o}) changes were calculated to portend the nature of adsorption. Adsorptive extraction of toxic lead and cadmium from tap water and wastewater was successfully accomplished with the range of percentage recovery values 98.5–100.0 and 91.9–93.0%, respectively.

77 NANOSCIENCE AND NANOTECHNOLOGY↗