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At least 829 records · Page 46
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

On the state of Mn in Mn{sub x}Zn{sub 1−x}O nanoparticles and their surface modification with isonipecotic acid

Mn-doped ZnO (Mn{sub x}Zn{sub 1−x}O) nanoparticles were synthesized by the co-precipitation method and coated with isonipecotic acid as capping ligand. The structure, composition and morphology of the resulting nanomaterial were investigated by energy disperse X-ray analysis, X-ray diffraction, and transmission electron microscopy data. Such measurements showed that the solid obtained contains 6 at% of Mn and it is formed by a highly crystalline material with 3–5 nm range of crystallite size, and only a small elongation of its cell parameter with respect to undoped ZnO wurtzite unit cell. Information on the state of manganese atom in the Mn{sub x}Zn{sub 1−x}O nanostructures formed was obtained from X-ray photoelectron (XPS) and electron energy loss (EELS) spectroscopies. XPS and EELS spectra are composed of four peaks, corresponding to two species of Mn(II) and signals from Mn(III) and Mn(IV). Such spectral data on the state of Mn in the material studied is consistent with the mapping of Mn distribution observed in recorded transmission electron microscopy images, which reveal presence of clusters of Mn atoms. Only a fraction of doping Mn atoms were found forming a solid solution with the host ZnO structure. The functionalization of the nanoparticles system with Isonipecotic acid shows that this molecule remains anchored to the nanoparticles surface mainly through its N basic site. The availability of free carboxylate groups in the capping molecule was tested by conjugation to type IV horseradish peroxidase. - Graphical abstract: State of Mn atoms in Mn-doped ZnO nanostructures prepared by the precipitation method, their capping with isonipecotic acid and subsequent conjugation to peroxidase. - Highlights: • State of manganese in manganese-doped zinc oxide nanoparticles. • Isonipecotic acid as surface modifier of ZnO nanoparticles. • Peroxidase conjugation to ZnO nanoparticles modified with isonipecotic acid.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2015

Preparation of the egg membrane bandage contained the antibacterial Ag nanoparticles

Silver nanoparticles were synthesized using a rapid, single step, and completely green biosynthetic method employing aqueous aloe leaf extracts as both the reducing and capping agent. Transmission electron microscopy analysis revealed the average size of silver nanoparticles approximately 18.05 nm. Fourier transform infrared spectroscopy observation showed the estimation of two kinds of binding sites between aqueous aloe leaf and aqueous aloe leaf with silver nanoparticles. In addition, the critical roles of the concentration of silver nitrate, temperature, and reaction time in the formation of silver nanoparticles had been illustrated. Furthermore, silver nanoparticles were deposited on egg membrane bandage, forming a new egg membrane bandage that contained silver nanoparticles that exhibiting excellent antibacterial effects against Gram-negative Escherichia coli and Gram-positive Staphylococcus aureus, which was 2.5 times stronger than the commercially available bandage. - Graphical Abstract: Display Omitted.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Exothermic low temperature sintering of Cu nanoparticles

Sintering of the Cu nanoparticle at low temperatures resulted in exothermic behavior after its initiation. The calorimetry study of the heating of a 20 nm copper nanoparticles agglomerate revealed the evolution of 41.17 J/g of heat between 170 °C and 270 °C. High resolution transmission electron microscopy (HRTEM) images indicated that the heat generation was accompanied by sintering. The surface energy of the 20 nm copper nanoparticles was estimated to be 1.23 × 10{sup 3} erg/cm{sup 2} based on the heat released during sintering. The in situ high resolution transmission electron microscope (HRTEM) investigation showed that vigorous sintering occurred between 217 and 234 °C, which took place through the dislocation sintering mechanism. - Highlights: • Calorimetry showed exothermic behavior during heating of Cu nanoparticles between 170 and 270 °C. • Heat released due to the sintering of Cu nanoparticles was demonstrated by HRTEM. • Surface energy of 20 nm copper nanoparticles was estimated to be 1.23 × 10{sup 3} erg/cm{sup 2} during sintering. • Growth in crystallite sizes during sintering is disclosed by X-ray diffraction. • In situ HRTEM heating study showed occurrence of sintering through dislocation mechanism.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure, texture and tensile behavior of pulsed electrodeposited Ni–Al composites produced using organic additive-free sulfamate bath loaded with Al nanoparticles

Highlights: • Foils of fine grained Ni with Al nanoparticles reinforcement are produced by pulsed electro-codeposition. • Ni–Al composite foils exhibit increased compressive residual stresses with increasing Al content. • Well-dispersed Al nanoparticles refine Ni matrix microstructure and induces significant texture changes. • Ultrafine grained Ni-Al composites exhibit improved hardness and tensile strength. - Abstract: Nickel and Ni–Al composites with varying Al nanoparticle content were produced by pulsed electrodeposition using an organic additive-free sulfamate bath. The as-deposited Ni–Al composites exhibited increased compressive residual stresses with increasing Al nanoparticles. Detailed microstructural investigation revealed that Al codeposition led to significant refinement of the columnar morphology and grain structure of Ni matrix along with a texture change from strong <001> to <011> fiber texture parallel to the growth direction. The as-deposited Ni with bimodal grain structure displayed good tensile strength and ductility. The microhardness and tensile strength of the Ni deposits were increased initially with Al content and then decreased at higher particle content. Particle induced grain refinement and texture changes could be related to change in the growth of upcoming Ni nuclei on to the surface of well-dispersed Al nanoparticles. Significant grain refinement and lesser internal stresses along with good particle distribution and relatively harder <011> fiber texture at lower particles concentration collectively contributed to the observed higher strengths in Ni–Al composites as compared to Ni deposits. There was substantial change in fracture morphology from spherical dimples to flat regions with increasing Al content due to agglomeration of nanoparticles at higher particle loading.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2018

Information depth in backscattered electron microscopy of nanoparticles within a solid matrix

Highlights: • Backscattered electron microscopy was used for reliable determination of nanoparticle density and sizes within Al alloys • Backscattered electron information depth was determined as a function of nanoparticle size from Monte Carlo simulations • Unlike transmission electron microscopy, the method is non-destructive and allows analyzing large sample areas • Good agreement with transmission electron microscopy data shows that our method is suitable for nanocomposite materials - Abstract: Measuring the dimensions and number density of nanoparticles dispersed in a solid matrix is usually accomplished via transmission electron microscopy (TEM) which suffers from high cost, low throughput, and small analytical volume. In comparison, scanning backscattered electron microscopy is inexpensive, requires little sample preparation, and allows for the analysis of large sample areas. However, the information depth is usually not known precisely and depends on several factors such as the composition of the nanoparticles and the matrix as well as the size of the nanoparticles, hindering the reconstruction of the actual size distribution and three-dimensional number density. Here we present a method to estimate the information depth for spherical nanoparticles of different sizes in order to accurately determine size distribution and number density. The approach is based on Monte Carlo simulation of electron trajectories in the material and analysis of the obtained backscattered electron signal-to-noise-ratio. Our experimental results are compared to those obtained via TEM and good agreement is demonstrated; this shows that TEM can be replaced by scanning electron microscopy for studying nanocomposites in many cases.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2013

Investigation on the structural and nonlinear optical properties of Pt doped TiO{sub 2} nanoparticles

Graphical abstract: The open aperture Z-scan traces of Pt doped TiO{sub 2} nanoparticles at different Pt concentrations were carried out at an irradiation wavelength of 532 nm. It was numerically found that, two photon absorption (TPA) type process gives the best fit to the obtained open aperture Z-scan data. The nonlinear transmission was found to be of third order as it fits to a two-photon absorption. The optical limiting performances of nanoparticles were greatly enhanced with increased volume ratio of Pt. Increasing particle size reduced the limiting threshold and enhanced the optical limiting performance. - Highlights: • Pt doped TiO{sub 2} nanoparticles with different concentrations of Pt have been synthesized by sol–gel method. • The average fluorescence lifetime decreases as the volume fraction of Pt dopant increases. • The effects of Pt content on the optical limiting property were investigated by open aperture Z-scan measurements done at 532 nm using 5 ns laser pulses. • The values of the third-order nonlinearities of nanoparticles are interesting from the application point of view which could be used as a potential candidate for the application of nonlinear optical device. - Abstract: Pt doped TiO{sub 2} nanoparticles with different concentrations of Pt were prepared by sol–gel method. X-ray diffraction (XRD) study reveals that the samples have a homogeneous anatase phase tetragonal system and the lattice parameter analysis indicates that Pt ions substitute into the lattice of TiO{sub 2}. The addition of dopant increases the growth of TiO{sub 2} grains, agglomerates them and shifts the absorption band of TiO{sub 2} from ultraviolet to visible region. The incorporation of Pt in TiO{sub 2} is also confirmed by fluorescence quenching and the fluorescence lifetime decreases as the volume fraction of Pt dopant increases. Open aperture Z-scan measurements done at 532 nm using 7 ns laser pulses show nonlinear absorption which arises from an effective two photon absorption process. The nonlinear optical properties are characterized by using fluence dependent transmittance measurements in order to reveal the optical limiting effects. It is found that the optical limiting performances of nanoparticles were greatly enhanced with increased concentration of Pt.

36 MATERIALS SCIENCE↗
DOE OSTI2013

One-step room temperature synthesis of very small γ-Fe{sub 2}O{sub 3} nanoparticles

Graphical abstract: - Highlights: • One-step synthesis of 3 nm maghemite nanoparticles is reported. • Maghemite nanoparticles can be synthesized from a ferric solution. • γ-Fe{sub 2}O{sub 3} NPs can be obtained if the precursor has Fe(III) in tetrahedral interstices. • HR-TEM, Mössbauer, XAFS and magnetometry analysis proved the maghemite existence - Abstract: Very small maghemite nanoparticles (∼3 nm) are obtained through a one-step synthesis at room temperature. The fast neutralization reaction of a ferric solution in a basic medium produces an intermediate phase, presumably two-line ferrihydrite, which in oxidizing conditions is transformed to maghemite nanoparticles. The synthesis of maghemite, as final product of the reaction, was characterized by High-Resolution Transmission Electron Microscopy (HR-TEM), X-ray Absorption Fine Structure (XAFS), Mössbauer spectroscopy, and magnetometry. The XAFS technique allowed the analysis of the crystallographic variations into maghemite nanoparticles as a result of modification in its surface/volume ratio. Mössbauer spectroscopy at low temperature (4.2 K) confirms the presence of Fe(III) in tetrahedral and octahedral interstices, in the stoichiometry corresponding to maghemite. The specific magnetization, M vs H (3 K and 300 K, up to 7 T) and temperature dependence of the magnetization (50 Oe by ZFC mode, 2 K ≤ T ≤ 300 K) indicate that maghemite nanoparticles of 3 nm are in superparamagnetic state with a blocking temperature close to 36 K.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Gd{sup 3+} incorporated ZnO nanoparticles: A versatile material

Graphical abstract: - Highlights: • Chemically synthesized Gd{sup 3+} doped ZnO nanoparticles. • The broad visible emission of the ZnO is dependent on the surface defects and can be tailored by Gd{sup 3+} doing. • PL and magnetic properties are modified by Gd{sup 3+} doping. • Photocatalysis experiment reveals that the ZnO: Gd{sup 3+} degrades the Rh B dye faster than the undoped ZnO. - Abstract: Gd{sup 3+} doped ZnO nanoparticles are synthesized by wet chemical route method and investigated through structural, optical, magnetic and photocatalytic properties. Transmission Electron Microscopy technique has been performed on undoped and Gd{sup 3+} doped ZnO nanoparticles. X-ray diffraction, X-ray photoelectron spectroscopy and Raman analyses are carried out in order to examine the desired phase formation and substitution of Gd{sup 3+} in the ZnO matrix. Gd{sup 3+} doped ZnO nanoparticles show enhanced photoluminescent and ferromagnetic properties as compared to undoped ZnO. The broad visible emission of ZnO is found to be largely dependent on the surface defects and these surface defects can be tailored by Gd{sup 3+} doping concentration. Furthermore, Gd{sup 3+} doped ZnO nanoparticles also show improved photocatalytic properties as compared with undoped ZnO nanoparticles under ultraviolet irradiation.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Synthesis and peferentially loading of nickel nanoparticle on CdS surface and its photocatalytic performance for hydrogen evolution under visible light

Graphical abstract: Ni nanoparticles were prepared via chemical reduction of aqueous NiCl{sub 2} by borohydride reducing agent in the presence of polyvinlylpyrolidone as a modifier to prevent fast growth of Ni crystals and their aggregation, and then preferentially deposited on (1 0 0), (0 0 2), and (1 0 1) crystal planes of CdS by photo-induced electrons while water splitting reaction occurred simultaneously. Resultant nickel nanoparticles have a size of about 3 nm, and contributes to decreasing the photoluminescence peak intensity of CdS, which means that nickel functions as the trapper of photo-generated electrons thereby quenching the photoluminescence of CdS. Therefore, nano-Ni/CdS photocatalyst with a Ni loading of 2.5% possesses the best visible-light catalytic activity for water splitting-hydrogen evolution and provides a hydrogen production rate of up to 9050 μmol h{sup −1} g{sup −1}, while it exhibits stabilized activity towards H{sub 2} evolution as well. - Highlights: • Ni nanoparticles are prepared by chemical reduction and then loaded on CdS surface by photo-reduction. • Non-noble metal Ni nanoparticles (size: about 3 nm) act as co-catalyst for photocatalytic H{sub 2} evolution. • Nano-Ni/CdS exhibits high activity (9050 μmol h{sup −1} g{sup −1}) and perfect stability. - Abstract: Ni nanoparticles were prepared via chemical reduction of NiCl{sub 2} by NaBH{sub 4} in the presence of polyvinlylpyrolidone (PVP), and loaded on the surface of CdS by photo-induced electrons while water splitting reaction occurred simultaneously. Resultant Ni/CdS was characterized by high-resolution transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, ultraviolet–visible light diffuse reflectance spectrometry, and photoluminescence spectrometry. It was found that as-prepared Ni nanoparticles are about 3 nm, and preferentially deposited on (1 0 0), (0 0 2), and (1 0 1) crystal planes of CdS. Meanwhile, loading nickel decreases the photoluminescence intensity of CdS, which means nickel functions as the trapper of photo-generated electrons. Therefore, nano-Ni/CdS photocatalyst with a Ni loading of 2.5% possesses the best visible-light catalytic activity for water splitting-hydrogen evolution and provides a hydrogen production rate of up to 9050 μmol h{sup −1} g{sup −1}, while it exhibits stabilized activity towards H{sub 2} evolution as well.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Luminescence properties of LaF{sub 3}:Ce nanoparticles encapsulated by oleic acid

Highlights: • In-situ hydrophobization of water dispersible LaF{sub 3}:Ce nanoparticles was achieved. • Oleic acid surface modification of the nanoparticles was verified by IR spectra. • Quantum yields of LaF{sub 3}:Ce and OA-LaF{sub 3}:Ce nanoparticles were evaluated. • Quantum yields of LaF{sub 3}:Ce are strongly dependent on OA surface modification. - Abstract: Cerium ions doped lanthanum fluoride (LaF{sub 3}:Ce) nanopowder as well as LaF{sub 3}:Ce nanopowder whose surfaces was modified by oleic acid (OA) were synthesized by using an in-situ hydrothermal process under the various doping concentrations. Based on the XRD spectra and TEM images, it was confirmed that the crystalline structured hexagonal LaF{sub 3}:Ce nanopowder was synthesized. Oleic acid was efficient for conversion of the water dispersible LaF{sub 3}:Ce nanoparticles to hydrophobic ones. Surface modification was verified by FTIR absorption spectrum as well as TEM images, showing no agglomeration between 5 and 10 nm scaled particles. Photoluminescence based on 5d ⟶ 4f electronic transition of cerium ions excited at λ{sub ex} ∼256 nm for both neat and OA encapsulated LaF{sub 3}:Ce nanoparticles decreases as the cerium concentration increases, while the quantum yields of OA encapsulated nanoparticles were much lower than the neat particles due to low photon transmittance of OA at the range longer than ∼350 nm.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Surfactant-assisted synthesis of mono-dispersed cubic BaTiO{sub 3} nanoparticles

Mono-dispersed BaTiO{sub 3} nanoparticles have been prepared via the assistance of capping agent poly(vinylpyrrolidone) (PVP). - Highlights: • BaTiO{sub 3} nanoparticles with single cubic crystal structure. • Poor dispersibility of nanoparticles has been overcome by in situ modification way. • Growth competition between BaTiO3 core and polymer shell. - Abstract: In this study, poly(vinylpyrrolidone)-assisted synthesis of mono-dispersed BaTiO{sub 3} nanoparticles have been reported. The various processing parameters, namely, refluxing temperature, KOH concentration, and poly(vinylpyrrolidone) concentration, have been varied, and the effects on the growth of BaTiO{sub 3} particles have been analyzed systematically. X-ray diffraction studies indicated that poly(vinylpyrrolidone) did not affect the crystal structure, but rather influenced the crystal lattice structure. In addition, the use of surfactant poly(vinylpyrrolidone) hindered the agglomeration of the nanoparticles, and facilitated the formation of mono-dispersed core–shell organic/inorganic hybrid nanocomposite. Furthermore, the mineralizer KOH promoted the dissolution of reactants and promoted the crystallization of BaTiO{sub 3} particles. Accordingly, the dissolution-precipitation scheme was believed to be the mechanism underlying the formation of BaTiO{sub 3} particles. This was further substantiated by the experimental observations, which indicated that the nucleation and crystallization of the particles was affected by the KOH concentration in the reaction system. Finally, the formation of mono-dispersed core–shell nanocomposites proceeded via reaction limited cluster aggregation. We believe that the method proposed in this study could be extended for the synthesis of mono-dispersed nanoparticles for industrial applications.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Synthesis, characterization, and hydrogen uptake studies of magnesium nanoparticles by solution reduction method

Graphical abstract: X-ray diffraction (XRD) pattern of magnesium nanoparticles synthesized by solution reduction method with and without TOPO. - Highlights: • Simple and convenient method of preparing Mg nanoparticles. • Characterized by XRD, SEM, FESEM and TEM. • Trioctylphosphine oxide offers a greater control over the size of the particles. • Hydrogen uptake of samples at different temperatures and pressure of 4.5 MPa. - Abstract: Facile and simple, surfactant-mediated solution reduction method was used to synthesize monodisperse magnesium nanoparticles. Little amount of magnesium oxide nanoparticles were also formed due to the presence of TOPO and easy oxidation of magnesium, eventhough, all precautions were taken to avoid oxidation of the sample. Precise size control of particles was achieved by carefully varying the concentration ratio of two different types of surfactants, – trioctylphosphine oxide and hexadecylamine. Recrystallized magnesium nanoparticle samples with and without TOPO were analyzed by X-ray diffraction, scanning electron microscope, field emission scanning electron microscope, and transmission electron microscope. The peak diameters of particles were estimated from size distribution analysis of the morphological data. The particles synthesized in the presence and absence of TOPO found to have diameters 46.5 and 34.8 nm, respectively. This observed dependence of particle size on the presence of TOPO offers a convenient method to control the particle size by simply using appropriate surfactant concentrations. Exceptional enhancement in hydrogen uptake and kinetics in synthesized magnesium nanoparticles as compared to commercial magnesium sample was due to the smaller particle size and improved morphology. Overall hydrogen uptake not affected by the little variation in particle size with and without TOPO.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Morphology and structure features of ZnAl{sub 2}O{sub 4} spinel nanoparticles prepared by matrix-isolation-assisted calcination

Graphical abstract: The substrate ZnO as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. High purity, well-dispersed, and single-crystal ZnAl{sub 2}O{sub 4} nanoparticles with 3.72 eV band gap were obtained. - Abstract: Well-dispersed ZnAl{sub 2}O{sub 4} spinel nanoparticles with an average crystalline size of 25.7 nm were synthesized successfully and easily by polymer-network and matrix-isolation-assisted calcination. The product microstructure and features were investigated by X-ray diffractometry, thermogravimetric and differential thermal analysis, Fourier transform-infrared spectroscopy, N{sub 2} adsorption–desorption isotherms, and energy dispersive X-ray spectra. The morphology and optical performance of the as-prepared ZnAl{sub 2}O{sub 4} nanoparticles were characterized by scanning electron microscope, transmission electron microscopy, and photoluminescence spectrometer. Experimental results indicate that excess ZnO acted as the isolation medium is effective in preventing the sintering and agglomeration of ZnAl{sub 2}O{sub 4} nanoparticles, and it also prevents their contamination. Then, high purity and well-dispersed ZnAl{sub 2}O{sub 4} nanoparticles with single-crystal structure were obtained.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Structural, magnetic and electronic structure properties of Co doped ZnO nanoparticles

Highlights: • XRD and HR-TEM results show the single phase nature of Co doped ZnO nanoparticles. • XMCD and dc magnetization results indicate the RT-FM in Co doped ZnO nanoparticles. • Co L{sub 3,2} NEXAFS spectra infer that Co ions are in 2+ valence state. • O K edge NEXAFS spectra show that O vacancy increases with Co doping in ZnO. - Abstract: We reported structural, magnetic and electronic structure studies of Co doped ZnO nanoparticles. Doping of Co ions in ZnO host matrix has been studied and confirmed using various methods; such as X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), energy dispersed X-ray (EDX), high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, magnetic hysteresis loop measurements and X-ray magnetic circular dichroism (XMCD). From the XRD and HR-TEM results, it is observed that Co doped ZnO nanoparticles have single phase nature with wurtzite structure and exclude the possibility of secondary phase formation. FE-SEM and TEM micrographs show that pure and Co doped nanoparticles are nearly spherical in shape. O K edge NEXAFS spectra indicate that O vacancies increase with Co doping. The Co L{sub 3,2} edge NEXAFS spectra revealed that Co ions are in 2+ valence state. DC magnetization hysteresis loops and XMCD results clearly showed the intrinsic origin of temperature ferromagnetism in Co doped ZnO nanoparticles.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Solution combustion synthesis and enhanced electrochemical performance Li{sub 1.2}Ni{sub 0.2}Mn{sub 0.6}O{sub 2} nanoparticles by controlling NO{sub 3}{sup –}/CH{sub 3}COO{sup –} ratio of the precursors

Highlights: • The size of Li{sub 1.2}Ni{sub 0.2}Mn{sub 0.6}O{sub 2} nanoparticles can be controlled by NO{sub 3}{sup −}/CH{sub 3}COO{sup −} ratio. • 35 nm Li{sub 1.2}Ni{sub 0.2}Mn{sub 0.6}O{sub 2} nanoparticles can be obtained with 3:1 NO{sub 3}{sup –}/CH{sub 3}COO{sup –} ratio. • 35 nm Li{sub 1.2}Ni{sub 0.2}Mn{sub 0.6}O{sub 2} nanoparticles shows excellent electrochemical performance. - Abstract: Lithium-rich layer oxide Li{sub 1.2}Ni{sub 0.2}Mn{sub 0.6}O{sub 2} nanoparticles were fabricated through solution combustion synthesis by controlling NO{sub 3}{sup –}/CH{sub 3}COO{sup –} ratio of the precursors. The relationships between the NO{sub 3}{sup –}/CH{sub 3}COO{sup –} ratio and structure as well as electrochemical performance of Li{sub 1.2}Ni{sub 0.2}Mn{sub 0.6}O{sub 2} nanoparticles are investigated. XRD reveals that Li{sub 1.2}Ni{sub 0.2}Mn{sub 0.6}O{sub 2} nanoparticles obtained with a suitable NO{sub 3}{sup –}/CH{sub 3}COO{sup –} ratio of 3:1 (LLO-3N1A) is composed of the smallest nanocrystallite of 18 nm. SEM reflects that the average primary particles of LLO-3N1A are the smallest with a size of 35 nm. Those unique characteristic guarantee the excellent electrochemical performance of LLO-3N1A. LLO-3N1A exhibits a specific capacity of 252.3 mA h g{sup −1} at 0.1 C. In addition, LLO-3N1A also shows best rate capability among the four prepared Li{sub 1.2}Ni{sub 0.2}Mn{sub 0.6}O{sub 2} samples.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2015

Highly Al-doped TiO{sub 2} nanoparticles produced by Ball Mill Method: structural and electronic characterization

Highlights: • Highly Al-doped TiO{sub 2} nanoparticles were synthesized using a Ball Mill Method. • Al doping delayed anatase to rutile phase transformation. • Al doping allow controlling the structural and electronic properties of nanoparticles. - Abstract: This study presents an easy method for synthesizing highly doped TiO{sub 2} nanoparticles. The Ball Mill method was used to synthesize pure and Al-doped titanium dioxide, with an atomic percentage up to 15.7 at.% Al/(Al + Ti). The samples were annealed at 773 K, 973 K and 1173 K, and characterized using ICP-AES, XRD, Raman spectroscopy, FT-IR, TG, STEM, XPS, and UV–vis spectroscopy. The effect of doping and the calcination temperature on the structure and properties of the nanoparticles were studied. The results show high levels of internal doping due to the substitution of Ti{sup 4+} ions by Al{sup 3+} in the TiO{sub 2} lattice. Furthermore, anatase to rutile transformation occurs at higher temperatures when the percentage of doping increases. Therefore, Al doping allows us to control the structural and electronic properties of the nanoparticle synthesized. So, it is possible to obtain nanoparticles with anatase as predominant phase in a higher range of temperature.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Photocatalytic activity of SnO{sub 2} nanoparticles in methylene blue degradation

Highlights: • Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method. • SnO{sub 2} nanoparticles displayed high photocatalytic activities for the MB degradation. • OH radicals are the main active species in photocatalysis on the SnO{sub 2} nanoparticles. - Abstract: Nanosized SnO{sub 2} photocatalysts were prepared with a precipitation method and were characterized by performing transmission electron microscopy (TEM), powder X-ray diffraction (XRD), and X-ray absorption spectroscopy (XAS). The powder XRD results revealed that the SnO{sub 2} nanoparticles have a typical tetragonal rutile (cassiterite) structure and the average crystallite size was found to be approximately 4.5 nm by using the Debye–Scherrer equation. The prepared SnO{sub 2} nanoparticles consist of agglomerated particles with a mean diameter of around 4–5 nm according to the analysis of TEM images. The XAS data confirmed that the prepared samples have cassiterite structures with tin oxidation state of +4. The prepared SnO{sub 2} nanoparticles were found to exhibit approximately 3.8 times higher activity than bulk SnO{sub 2} in the photodegradation of methylene blue. On the basis of a trapping experiment, we developed a possible mechanism for the photodegradation on SnO{sub 2} nanoparticles.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Preparation of gold nanoparticles and determination of their particles size via different methods

Graphical abstract: Preparation of gold nanoparticles via NaBH{sub 4} reduction method, and determination of their particle size, size distribution and morphology by using different techniques. - Highlights: • Gold nanoparticles were synthesized by NaBH{sub 4} reduction method. • Excess of reducing agent leads to tendency of aggregation. • The particle size, size distribution and morphology were investigated. • Particle size was determined both experimentally as well as theoretically. - Abstract: Gold nanoparticles have been used in various applications covering both electronics, biosensors, in vivo biomedical imaging and in vitro biomedical diagnosis. As a general requirement, gold nanoparticles should be prepared in large scale, easy to be functionalized by chemical compound of by specific ligands or biomolecules. In this study, gold nanoparticles were prepared by using different concentrations of reducing agent (NaBH{sub 4}) in various formulations and their effect on the particle size, size distribution and morphology was investigated. Moreover, special attention has been dedicated to comparison of particles size measured by various techniques, such as, light scattering, transmission electron microscopy, UV spectrum using standard curve and particles size calculated by using Mie theory and UV spectrum of gold nanoparticles dispersion. Particle size determined by various techniques can be correlated for monodispersed particles and excess of reducing agent leads to increase in the particle size.

36 MATERIALS SCIENCE↗