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At least 775 records · Page 43
All sourcesNASA NTRSDOE OSTI
DOE OSTI2014

Detection and quantification of solute clusters in a nanostructured ferritic alloy

A series of simulated atom probe datasets were examined with a friends-of-friends method to establish the detection efficiency required to resolve solute clusters in the ferrite phase of a 14YWT nanostructured ferritic alloy. The size and number densities of solute clusters in the ferrite of the as-milled mechanically-alloyed condition and the stir zone of a friction stir weld were estimated with a prototype high-detection-efficiency (~80%) local electrode atom probe. High number densities, 1.8 × 10 24 m –3 and 1.2 × 10 24 m –3 , respectively of solute clusters containing between 2 and 9 solute atoms of Ti, Y and O and were detected for these two conditions. Furthermore, these results support first principle calculations that predicted that vacancies stabilize these Ti–Y–O– clusters, which retard diffusion and contribute to the excellent high temperature stability of the microstructure and radiation tolerance of nanostructured ferritic alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Modern nanostructured ferritic alloys: A compelling and viable choice for sodium fast reactor fuel cladding applications

Sodium fast reactor cores present a truly challenging environment for the fuel cladding and core structural materials that limit achievable fuel burnup in these systems. Modern nanostructured ferritic alloys have the potential to deliver the desired high performance characteristics where historic austenitic and ferritic/martensitic alloys fall short. Herein, a new nanostructured ferritic alloy, OFRAC ( O ak Ridge F ast R eactor A dvanced Fuel C ladding), is developed and demonstrated in cladding geometry with a length > 1 m. The alloy composition and microstructure are tailored to deliver dramatically improved strength and creep resistance. At 600 °C the ultimate tensile strength is ~600 MPa and the stress to induce a steady state strain rate of 10 -6 s -1 is 500 MPa vs. 200 MPa for traditional ferritic/martensitic alloys. A very high defect sink density was engineered in these alloys that is expected to further enhance the traditional good swelling and irradiation creep resistance of ferritic/martensitic steels. These significant improvements along with the demonstrated viability for seamless cladding production indicate that this alloy is a compelling and viable choice for sodium fast reactor fuel cladding applications.

36 MATERIALS SCIENCE↗
DOE OSTI2019

High-Performance Thermoelectrics from Cellular Nanostructured Sb 2 Si 2 Te 6

We introduce Sb 2 Si 2 Te 6 as a high-performance thermoelectric material. Single-crystal X-ray diffraction analysis indicates that Sb 2 Si 2 Te 6 has a layered twodimensional structure with Sb 3+ cations and [Si 2 Te 6 ] 6- units as building blocks adopting the Fe 2 P 2 Se 6 structure type. Sb 2 Si 2 Te 6 is a direct-band-gap semiconductor with valence-band maximum and conduction-band minimum at the Z point in the Brillouin zone, where the band is doubly degenerate. Polycrystalline bulk pellets of Sb 2 Si 2 Te 6 with randomly packed grains exhibit an intrinsically high thermoelectric figure of merit ZT of ~1.08 at 823 K. We then create a cellular nanostructure with ultrathin Si 2 Te 3 nanosheets covering the Sb 2 Si 2 Te 6 grains, which act as a hole-transmitting electron-blocking filter and at the same time cause extra phonon scattering. Lastly, this dual function of the cellular nanostructure achieves an ultralow thermal conductivity value of ~0.29 Wm -1 K -1 and a high ZT value of ~1.65 at 823 K for Sb 2 Si 2 Te 6 , along with a high average ZT value of ~0.98.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2010

Synthesis of porous and nonporous ZnO nanobelt, multipod, and hierarchical nanostructure from Zn-HDS

Zn based hydroxide double salts (Zn-HDS) with an interlayer spacing of 20 A was produced by dissolving dumbbell-like ZnO crystal. The resulting Zn-HDS with a ribbon-like shape has a suitable morphology to explore the remarkably mild procedure for synthesis of ZnO nanobelts. We found that the intercalated water molecules into the Zn-HDS could play a key role in the ZnO nanobelts porosity. The nonporous ZnO nanobelts were successfully synthesized from the Zn-HDS by soft-solution process at 95 {sup o}C through mild dehydration agent as Na{sub 2}CO{sub 3}. As-synthesized ZnO nanobelts were grown along not only the [0 1 -1 0], but also the [2 -1 -1 0]. On the other hand, the porous ZnO nanobelts were obtained from the Zn-HDS by calcinations at 200 and 400 {sup o}C. In addition, flower-like ZnO multipod and hierarchical nanostructures were produced from the Zn-HDS by using of strong dehydration agent (NaOH) through hydrothermal reaction at 150 and 230 {sup o}C. - Graphical abstract: Porous and nonporous ZnO nanobelts, multipod, and hierarchical nanostructure were successfully synthesized from Zn based hydroxyl double salts by hydrothermal reaction.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2011

Formation of titanate nanostructures under different NaOH concentration and their application in wastewater treatment

The effects of the concentration of NaOH on the formation and transformation of various titanate nanostructures were studied. With increasing NaOH concentration, three different formation mechanisms were proposed. Nanotubes can only be obtained under moderate NaOH conditions, and should transform into nanowires with prolonged hydrothermal treatment, and their formation rate is accelerated by increasing NaOH concentration. Low concentration of NaOH results in the direct formation of nanowires, while extra high concentration of NaOH leads to the formation of amorphous nanoparticles. Adsorption and photocatalysis studies show that titanate nanowires and nanotubes might be potential adsorbents for the removal of both heavy metal ions and dyes and photocatalysts for the removal of dyes from wastewater. -- Graphical abstract: The morphologies of the titanates depend deeply on the concentration of NaOH. With increasing NaOH concentration, three different formation mechanisms were proposed. The application of these titanate nanostructures in the wastewater treatment was studied. Display Omitted Research highlights: {yields} Effect of NaOH concentration on the structures of various titanates was reported. {yields} Three different formation mechanisms were presented with increasing NaOH concentration. {yields} Various titanates were used as adsorbents/photocatalysts in wastewater treatment.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2011

One-step growth of Si{sub 3}N{sub 4} stem-branch featured nanostructures: Morphology control by VS and VLS mode

We report here one-step synthesis of Si{sub 3}N{sub 4} nanodendrites by selectively applying a vapor-solid (VS) and vapor-liquid-solid (VLS) strategy via direct current arc discharge method. The resultant nanodendrites were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy and X-ray powder diffraction. The spine-shaped nanodendrites were generated by a noncatalytic growth following a VS mode. The uniform secondary nanowire branches were epitaxial grown from two side surfaces of the nanowire stems. The pine-shaped nanodendrites were obtained through a catalytic growth in a VLS process. These branch nanowires were unsystematically grown from the nanocone-like stems. The photoluminescence spectra of the nanodendrites show a strong white light emission around 400-750 nm, suggesting their potential applications in light and electron emission devices. - Graphical abstract: Spine-shaped and pine-shaped Si{sub 3}N{sub 4} hierarchical nanostructures were synthesized by VS and VLS mode with plasma-assisted dc arc discharge method. Highlights: > Si{sub 3}N{sub 4} stem-branch featured nanostructures have been prepared. > Spine-shaped nanodendrites were generated by a noncatalytic growth following a VS mode. > Pine-shaped nanodendrites were obtained through a catalytic growth in a VLS process.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Facile synthesis of {alpha}-MnO{sub 2} one-dimensional (1D) nanostructure and energy storage ability studies

The dense manganese oxide nanorods with an extremely narrow distribution are synthesized at a low temperature using first cathodic electrodeposition subsequently heat treatment. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images show that the nanorods have bar shapes, and their average diameter is less than 50 nm. The Fourier transform infrared (FT-IR) study, the selected area electron diffraction (SAED) pattern in TEM images and the X-ray diffraction (XRD) result show that the nanorods are {alpha}-MnO{sub 2} single crystal. The results of N{sub 2} adsorption-desorption analysis indicate that the BET surface area of the {alpha}-MnO{sub 2} nanorods is 93 m{sup 2} g{sup -1}. By recording the potential-time curve during the electrodeposition process, it is revealed that water reduction reaction has a major role in the electrogeneration of base at the cathode surface under the applied electrochemical conditions. Finally, based on the H{sub 2} bubbling on the cathode surface, the mechanism of the formation and the growth of {alpha}-MnO{sub 2} nanorods are proposed and discussed. For the electrochemical supercapacitor application, electrochemically prepared {alpha}-MnO{sub 2} is found to be stable for a large number of cycles with high specific capacitance, 338 F g{sup -1} at a scan rate of 10 mV s{sup -1}. Finally, the charge-discharge mechanism is discussed. - Graphical abstract: Highlights: Black-Right-Pointing-Pointer New nanostructures of MnO{sub 2} is synthesized by simple method of cathodicelectrodeposition. Black-Right-Pointing-Pointer The product has unique one-dimensional morphology with average diameter size of 50 nm. Black-Right-Pointing-Pointer The experiment conditions (temperature, current density) has not been reported. Black-Right-Pointing-Pointer The one-nanostructures obtained without using of hard template or surfactant.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Influence of nanoinclusions on scattering of holes and phonons and transport coefficients in Bi{sub x}Sb{sub 1-x}Te{sub 3} bulk nanostructures

One of the possible ways to increase the thermoelectric figure of merit is the use of bulk nanostructured materials fabricated by melt spinning with subsequent hot pressing or spark plasma sintering. Among a variety of nanostructure types these materials contain regions of initial solid solution with nanometer sized inclusions of different compositions. In the present work the scattering of holes and phonons on nanoinclusions in such p-Bi{sub x}Sb{sub 1-x}Te{sub 3} based materials is considered. The change of transport coefficients due to this scattering mechanism is theoretically estimated. The estimations showed that the reduction of lattice thermal conductivity (about 12-13%) for nanoinclusions of Bi{sub 2}Te{sub 3}-Sb{sub 2}Te{sub 3} solid solution with different compositions is much greater than the change in power factor. Therefore the corresponding increase of the thermoelectric figure of merit for this case is determined mainly by phonon scattering. Also it is shown that the results of estimations depend on phonon spectrum approximation, e.g. in the case of sine-shaped instead of linear phonon spectrum the estimations give two times higher thermal conductivity reduction. - Graphical abstract: Relative phonon thermal conductivity {kappa}{sub ph} change (black line) due to nanoinclusion scattering versus nanoinclusion radius a, and relative thermoelectric power factor change (red line) due to nanoinclusion scattering versus chemical potential {mu} at nanoinclusion size a=1.5 nm and U{sub 0}=-0.146 eV. Highlights: Black-Right-Pointing-Pointer p-Bi{sub x}Sb{sub 1-x}Te{sub 3} solid solutions with nanosized inclusions were considered. Black-Right-Pointing-Pointer Selective hole scattering can increase power factor at high carrier concentrations. Black-Right-Pointing-Pointer Lattice thermal conductivity estimations depend on phonon spectrum approximation. Black-Right-Pointing-Pointer Phonon scattering can reduce lattice thermal conductivity by about 12-13%. Black-Right-Pointing-Pointer The latter factor mainly determines the increase of thermoelectric efficiency.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Magnetron sputtered nanostructured cadmium oxide films for ammonia sensing

Nanostructured cadmium oxide (CdO) films were deposited on to glass substrates by reactive dc magnetron sputtering technique. The depositions were carried out for different deposition times in order to obtain films with varying thicknesses. The CdO films were polycrystalline in nature with cubic structure showing preferred orientation in (1 1 1) direction as observed by X-ray diffraction (XRD). Field-emission scanning electron microscope (FE-SEM) micrographs showed uniform distribution of grains of 30–35 nm size and change in morphology from spherical to elliptical structures upon increasing the film thickness. The optical band gap value of the CdO films decreased from 2.67 to 2.36 eV with increase in the thickness. CdO films were deposited on to interdigitated electrodes to be employed as ammonia (NH{sub 3}) gas sensor. The fabricated CdO sensor with thickness of 294 nm has a capacity to detect NH{sub 3} as low as 50 ppm at a relatively low operating temperature of 150 °C with quick response and recovery time. - Highlights: • Nanostructured CdO films were deposited on to glass substrates using magnetron sputtering. • Deposition time was varied in order to obtain films with different thicknesses. • The CdO films were polycrystalline in nature with preferred orientation along (1 1 1) direction. • The optical bandgap values of the films decreased on increasing the thickness of the films. • CdO films with different thickness such as 122, 204, 294 nm was capable to detect NH{sub 3} down to 50 ppm at operating temperature of 150 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2014

Magnetic and structural investigations on La{sub 0.6}Sr{sub 0.4}MnO{sub 3} nanostructured manganite: Evidence of a ferrimagnetic shell

This paper presents the structural and magnetic properties of La{sub 0.6}Sr{sub 0.4}MnO{sub 3} nanoparticles with sizes from 21 to 106 nm, which have been prepared using the sol–gel method. The reduction of the nanoparticles' size tends to broaden the paramagnetic to ferromagnetic transition, as well as to promote magnetic hysteresis and a remarkable change on the magnetic saturation. In order to better understand the magnetic behavior of those nanoparticles, a simple model based on a ferromagnetic core and a ferrimagnetic shell was considered, where the magnetization was described in terms of the standard mean-field Brillouin function. This model matches the experimental data, leading to conclusion the nanoparticles with size <40nm are single magnetic domain. In addition, the output fitting parameters give information on the Landé factor of the core and shell. - Graphical abstract: Core–shell model: The core has a ferromagnetic character, while the shell is ferrimagnetic. Each one has two sub-lattices (Mn{sup 3+} and Mn{sup 4+}) that interact through a mean-field (see Eq. (6)). Interactions strength and signals are also represented in this figure. In this figure the arrows (or vectors) represent the magnetic moment of ions Mn{sup 3+} (s=2) and Mn{sup 4+} (s=3/2). βλ's describe the ferromagnetic interaction between Mn{sup 4+} ions into the core (βλ{sub co}) and into the shell (βλ{sub sh}), while αλ's represent ferromagnetic interaction between Mn{sup 3+} ions into the core (αλ{sub co}) and into the shell (αλ{sub sh}). The −λ{sub sh} and +λ{sub co}co are associated to the mean field parameter of interaction between Mn{sup 3+} and Mn{sup 4+} sub-lattices in the shell (ferrimagnetic, negative sign) and core (ferromagnetic, positive sign), respectively. - Highlights: • Evidences of ferromagnetic shell in La{sub 0.6}Sr{sub 0.4}MnO{sub 3} ferromagnetic nanoparticles. • Core(ferromagnetic)–shell(ferromagnetic) model for nanostructured manganite. • Sol–gel method was successfully used to obtain nanostructured manganite.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Ultrasound-assisted facile synthesis of a new tantalum(V) metal-organic framework nanostructure: Design, characterization, systematic study, and CO{sub 2} adsorption performance

This work presents a fast route for the preparation of a new Ta(V) metal-organic framework nanostructure with high surface area, significant porosity, and small size distribution. X-ray diffraction (XRD), scanning electron microscopy (SEM), Transition electron microscopy (TEM), energy dispersive spectrometer (EDS), thermo-gravimetric analysis (TGA), differential scanning calorimetry (DSC), fourier transform infrared spectroscopy (FTIR), CHNS/O elemental analyser, and Brunauer-Emmett-Teller (BET) surface area analysis were applied to characterize the synthesized product. Moreover, the influences of ultrasonic irradiation including temperature, time, and power on different features of the final products were systematically studied using 2{sup k-1} factorial design experiments, and the response surface optimization was used for determining the best welding parameter combination. The results obtained from analyses of variances showed that ultrasonic parameters affected the size distribution, thermal behaviour, and surface area of Ta-MOF samples. Based on response surface methodology, Ta-MOF could be obtained with mean diameter of 55 nm, thermal stability of 228 °C, and high surface area of 2100 m{sup 2}/g. The results revealed that the synthesized products could be utilized in various applications such as a novel candidate for CO{sub 2} adsorption. - Graphical abstract: A facile route was used for fabrication of a new metal -organic framework based on tantalum nanostructures that have high surface area, considerable porosity, homogenous morphology, and small size distribution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2010

Synthesis and characterization of xTiO{sub 2}{center_dot}(1 - x){alpha}-Fe{sub 2}O{sub 3} magnetic ceramic nanostructure system

Rutile-doped hematite xTiO{sub 2}{center_dot}(1 - x){alpha}-Fe{sub 2}O{sub 3} (x = 0.0-1.0) nanostructures were synthesized using mechanochemical activation by ball milling. Their complex structural, magnetic and thermal properties were characterized by X-ray diffraction, Moessbauer spectroscopy and simultaneous DSC-TGA. XRD patterns yielded the dependence of lattice parameters and grain size as a function of ball milling time. For the molar concentrations x = 0.1 and 0.3, the Moessbauer spectra were fitted with one, two, three or four sextets, corresponding to the degree of Ti ion substitution of Fe ions in hematite lattice. After 12 h of ball milling, the completion of Ti ion substitution of Fe ions in hematite lattice occurs for x = 0.1 and 0.3. For x = 0.5 and 0.7, Moessbauer spectra fitting required sextets and a quadrupole-split doublet, representing Fe ions substituting Ti ions in the rutile lattice. The completion of Fe ion substitution of Ti ions in rutile lattice was not observed, as indicated by XRD patterns and Moessbauer spectra for these two molar concentrations. Simultaneous DSC-TGA measurements revealed that the mechanochemical activation by ball milling has a strong effect on the thermal behavior of this nanostructure system. The enthalpy dropped dramatically after 2 h of milling time, indicating the strong solid-solid interactions between TiO{sub 2} and {alpha}-Fe{sub 2}O{sub 3} after ball milling. The change in weight loss of hematite was caused by the decrease of grain size and ion substitutions between Fe and Ti after mechanochemical activation.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Microstructure and mechanical properties of 7075 aluminum alloy nanostructured composites processed by mechanical milling and indirect hot extrusion

Nanostructured composites of 7075 aluminum alloy and carbon coated silver nanoparticles were produced by mechanical milling and indirect hot extrusion. The milling products were obtained in a high energy SPEX ball mill, and then were compacted by uniaxial load and pressure-less sintered under argon atmosphere. Finally, the sintered product was hot extruded. Carbon coated silver nanoparticles were well distributed in the matrix of the extruded material. Tensile tests were carried out to corroborate the hypothesis that second phase particles, well dispersed in the matrix, improve the strength of the material. High resolution transmission electron microscopy was employed to locate and make sure that the silver nanoparticles were homogeneously and finely dispersed. Highlights: Black-Right-Pointing-Pointer 7075 Al nanostructured composites can be produced by mechanical milling. Black-Right-Pointing-Pointer Carbon coated silver nanoparticles are well dispersed into aluminum matrix. Black-Right-Pointing-Pointer Ductile Ag-C NP's improve the mechanical properties of the 7075 Al-alloy. Black-Right-Pointing-Pointer Ag-C NP's content has an important effect in the particle and crystallite size. Black-Right-Pointing-Pointer Ag-C NP's keep their morphology after milling and conformation processes.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Study of various Sb{sub 2}S{sub 3} nanostructures synthesized by simple solvothermal and hydrothermal methods

Controlling the size and morphology of the antimony sulfide nanostructures is important for photocatalytic and photovoltaic applications. Herein, we report a systematic approach to synthesize various nanostructures of antimony sulfide. Based on simple solvothermal and hydrothermal routes antimony sulfide nanorods have been synthesized at different temperatures. The size of the nanorods and the morphology of the constituent nano-units, in the form of nanorods, dumbbell and sphere have been controlled by adjusting the temperature. The changes have been confirmed by scanning electron microscope and transmission electron microscope analysis. - Highlights: • We prepared dumbbell structured Sb{sub 2}Sb{sub 3} by simple solvothermal and hydrothermal method. • Investigated the importance of bath temperature on the formation of various structures. • Growth mechanism of dumbbell like structured Sb{sub 2}S{sub 3} nanorods was estimated.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Magnetic and structural properties of nanostructured Fe–20Al–2Cr powder mixtures

Nanostructured Fe–20Al–2Cr (wt.%) powders have been prepared using high energy planetary ball-mill. Changes in structural, morphological and magnetic properties of the powders during mechanical alloying (MA) and during subsequent annealing have been examined by X-ray diffraction, scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). The observed structural and microstructural changes have been related to several processes occurring during MA. After MA, the material becomes significantly disordered and refines to nanoscale grain sizes (~ 14 nm). The obtained bcc α-Fe(Al,Cr) solid solution shows a ferromagnetic behavior. Upon subsequent annealing at 400 °C, α-Fe{sub 2}O{sub 3} and spinel oxides are formed at the surface of particles, while structural defects disappeared as Fe(Al,Cr) solid solution becomes more ordered and grain growth occurs. The saturation magnetization (Ms) shows lower values after annealing, attributed to the formation of metal oxides with low magnetic moment. - Graphical abstract: Display Omitted - Highlights: • Nanostructured Fe–Al–Cr powders were prepared by MA. • Careful analysis of the XRD patterns by using the Rietveld refinement • The lattice distortion is evidenced by the increase of both the lattice parameter and the static Debye Waller parameter. • Annealing at 400 °C stabilizes the microstructure at the nanometer range and leads to the formation of Fe{sub 3}O{sub 4} and Fe{sub 2}O{sub 3} oxides. • Both the milled and annealed samples are ferromagnetic.

36 MATERIALS SCIENCE↗
DOE OSTI2011

A novel nanostructure of cadmium oxide synthesized by mechanochemical method

Highlights: {yields} A novel nanostructure of CdO was synthesized by mechanochemical reaction followed by calcination. {yields} Mechanochemical method is a simple and low-cost to synthesize nanomaterials. {yields} The obtained precursor was characterized by FT-IR, NMR techniques and elemental analysis. {yields} SEM images showed cauliflower-like shape of sample with components average diameter of 68 nm. {yields} The rods and tubes bundles with single crystalline nature were revealed by ED pattern and TEM images. -- Abstract: Cauliflower-like cadmium oxide (CdO) nanostructure was synthesized by mechanochemical reaction followed calcination procedure. Cadmium acetate dihydrate and acetamide were used as reagents and the resulting precursor was calcinated at 450 {sup o}C for 2 h in air. The structures of the precursor and resultant product of the heating treatment were characterized using Fourier transform infrared (FT-IR) spectroscopy, nuclear magnetic resonance (NMR) spectroscopy and elemental analysis, X-ray powder diffraction (XRD), energy-dispersive X-ray spectroscopy analysis (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction pattern (ED). SEM and TEM images revealed the cauliflower-like morphology of the sample. This structure includes the bundles of rods and tubes in nanoscale, which combine with each other and form the resulting morphology with the average diameter, 68 nm of the components. ED pattern indicated the single crystal nature of the formed bundles.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2011

Effect of boron doping on optical properties of sol-gel based nanostructured zinc oxide films on glass

Graphical abstract: Room temperature fine structured UV-vis PL emissions (a) as phonon replicas in 1 at.% boron doped film originated from LO phonon evidenced from Near Grazing Incidence Angle (NGIA) IR spectral study (b). Highlights: Black-Right-Pointing-Pointer Sol-gel based boron doped nanostructured ZnO thin films deposited on pure silica glass using crystalline boric acid as boron source. Black-Right-Pointing-Pointer Observed first time, room temperature fine structured PL emissions in 1 at.% doped film as phonon replicas originated from LO phonon (both IR and Raman active). Black-Right-Pointing-Pointer Boron doping controls the LO phonon energy in addition to visible reflection, band gap and grain size. Black-Right-Pointing-Pointer The films possessed mixed crystal phases with hexagonal as major phase. -- Abstract: Boron doped zinc oxide thin films ({approx}80 nm) were deposited onto pure silica glass by sol-gel dip coating technique from the precursor sol/solution of 4.0 wt.% equivalent oxide content. The boron concentration was varied from 0 to 2 at.% w.r.t. Zn using crystalline boric acid. The nanostructured feature of the films was visualized by FESEM images and the largest cluster size of ZnO was found in 1 at.% boron doped film (B1ZO). The presence of mixed crystal phases with hexagonal as major phase was identified from XRD reflections of the films. Particle size, optical band gap, visible specular reflection, room temperature photoluminescence (PL) emissions (3.24-2.28 eV), infra-red (IR) and Raman active longitudinal optical (LO) phonon vibration were found to be dependent on dopant concentration. For the first time, we report the room temperature fine structured PL emissions as phonon replicas originated from the LO phonon (both IR and Raman active) in 1 at.% boron doped zinc oxide film.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Structural and electrochemical properties of nanostructured nickel silicides by reduction and silicification of high-surface-area nickel oxide

Graphical abstract: Nanostructured nickel silicides have been synthesized by reduction and silification of high-surface-area nickel oxide, and exhibited remarkably like-noble metal property, lower electric resistivity, and ferromagnetism at room temperature. Highlights: Black-Right-Pointing-Pointer NiSi{sub x} have been prepared by reduction and silification of high-surface-area NiO. Black-Right-Pointing-Pointer The structure of nickel silicides changed with increasing reaction temperature. Black-Right-Pointing-Pointer Si doping into nickel changed the magnetic properties of metallic nickel. Black-Right-Pointing-Pointer NiSi{sub x} have remarkably lower electric resistivity and like-noble metal property. -- Abstract: Nanostructured nickel silicides have been prepared by reduction and silicification of high-surface-area nickel oxide (145 m{sup 2} g{sup -1}) produced via precipitation. The prepared materials were characterized by nitrogen adsorption, X-ray diffraction, thermal analysis, FT-IR spectroscopy, scanning electron microscopy, transmission electron microscopy, magnetic and electrochemical measurements. The nickel silicide formation involves the following sequence: NiO (cubic) {yields} Ni (cubic) {yields} Ni{sub 2}Si (orthorhombic) {yields} NiSi (orthorhombic) {yields} NiSi{sub 2} (cubic), with particles growing from 13.7 to 21.3 nm. The nickel silicides are ferromagnetic at room temperature, and their saturation magnetization values change drastically with the increase of Si content. Nickel silicides have remarkably low electrical resistivity and noble metal-like properties because of a constriction of the Ni d band and an increase of the electronic density of states. The results suggest that such silicides are promising candidates as inexpensive yet functional materials for applications in electrochemistry as well as catalysis.

36 MATERIALS SCIENCE↗