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At least 1,009 records · Page 56
All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

Rapid synthesis of ordered hexagonal mesoporous silica and their incorporation with Ag nanoparticles by solution plasma

Graphical abstract: Overall reactions of mesoporous silica and AgNPs-incorporated mesoporous silica syntheses by solution plasma process (SPP). Highlights: ► SPP for rapid synthesis of mesoporous silica. ► SPP for rapid synthesis of mesoporous silica and AgNPs incorporation. ► Higher surface area and larger pore diameter of mesoporous silica synthesized by SPP. -- Abstract: Rapid synthesis of silica with ordered hexagonal mesopore arrangement was obtained using solution plasma process (SPP) by discharging the mixture of P123 triblock copolymer/TEOS in acid solution. SPP, moreover, was utilized for Ag nanoparticles (AgNPs) incorporation in silica framework as one-batch process using silver nitrate (AgNO{sub 3}) solution as precursor. The turbid silicate gel was clearly observed after discharge for 1 min and the white precipitate formed at 3 min. The mesopore with hexagonal arrangement and AgNPs were observed in mesoporous silica. Two regions of X-ray diffraction patterns (2θ < 2° and 2θ = 35–90°) corresponded to the mesoporous silica and Ag nanocrystal characteristics. Comparing with mesoporous silica prepared by a conventional sol–gel route, surface area and pore diameter of mesoporous silica prepared by solution plasma were observed to be larger. In addition, the increase in Ag loading resulted in the decrease in surface area with insignificant variation in the pore diameter of mesoporous silica. SPP could be successfully utilized not only to enhance gelation time but also to increase surface area and pore diameter of mesoporous silica.

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

Synthesis and structural transformations of the “glaserite” type zirconosilicate Na{sub 3−x}H{sub 1+x}ZrSi{sub 2}O{sub 8}·yH{sub 2}O

Highlights: ► Hydrothermal synthesis of hydrous zirconosilicate Na{sub 3}HZrSi{sub 2}O{sub 8}·0.5H{sub 2}O is reported. ► Gradual symmetry lowering is observed upon synthesis treatment. ► This compound's modifications possess “glaserite”-type structure. ► This is a rare case of water-containing material with “glaserite”-type structure. -- Abstract: A hydrous sodium zirconosilicate material with “glaserite” type structure and generalized formula Na{sub 3−x}H{sub 1+x}ZrSi{sub 2}O{sub 8}·yH2O, 0 < x < 3, 0 < y < 1 is synthesized in the system Na{sub 2}O:ZrO{sub 2}:SiO{sub 2}:H{sub 2}O at 200 °C. Its crystal structure is composed of zirconium and silicon polyhedra connected to build layers additionally stacked to form 3D zipper-like network. Within the network there are cavities interconnected to channels with irregular shapes where the sodium atoms and water molecules reside. It is found that with synthesis duration the crystal structure gradually transforms from higher symmetrical into triclinic one. The structure of the triclinic form – Na{sub 3}HZrSi{sub 2}O{sub 8}·0.4H{sub 2}O was refined from powder diffraction data. It crystallizes in the space group P-1 with lattice parameters a = 9.05234, b = 5.56121, c = 6.96219 Å, α = 92.178, β = 90.839, γ = 90.288°. To the best of our knowledge the studied compound is the only water-containing material with “glaserite” type structure.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Study on the formation of Co{sub x}Fe{sub 3−x}O{sub 4} system using two low temperature synthesis methods

Graphical abstract: Display Omitted Highlights: ► Co{sub x}Fe{sub 3−x}O{sub 4} nanopowders are synthesized by two synthesis methods. ► The thermal decomposition of mixed Fe(III), Co(II) carboxylates method is original. ► For x = 1.0, CoFe{sub 2}O{sub 4} crystallizes as single phase at low temperatures by both methods. ► The presence of secondary phases for x ≠ 1 influences the magnetic properties. ► The particles are nanosized (<50 nm) leading to sintering at lower temperatures. -- Abstract: This paper presents a study regarding the cobalt ferrite obtaining in the Co{sub x}Fe{sub 3−x}O{sub 4} system, where x = 0.5; 1.0; 1.5 by two different synthesis methods. The Co(II) and Fe(III) complexes method leads to the thermal decomposition at 300 °C for this precursor with the pure cobalt ferrite (CoFe{sub 2}O{sub 4}) formation for x = 1 or mixed with γ-Fe{sub 2}O{sub 3} for x = 0.5 and Co{sub 3}O{sub 4} for x = 1.5. By co-precipitation followed by ultrasonic milling synthesis method the pure cobalt ferrite is obtained at 90 °C for x = 1 or mixed with Fe{sub 3}O{sub 4} for x = 0.5 and Co{sub 3}O{sub 4} for x = 1.5. When the initial samples are heated at 400 °C, the identified oxide phase is identical for the same value of x. The obtained powders were investigated by X-ray diffraction (XRD), FTIR spectrometry and scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDX). The final product has nanometric size and has a strong tendency to agglomerated, thus influencing the saturation magnetization value. The shape of the magnetization curves is influenced by the presence of the secondary phases for x ≠ 1.

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

Synthesis and characterization of iron orthophosphate by solution combustion method

Graphical abstract: Display Omitted Highlights: ► Solution combustion synthesis was firstly employed to prepare FePO{sub 4}. ► Pure, well-crystallized and porous FePO{sub 4} was obtained and characterized. ► The results proved SCS a time saving and practically applicable method. -- Abstract: The present work applies solution combustion synthesis (SCS) by employing glycine as organic fuel to stimulate the synthesis of pure iron orthophosphate with well-defined reaction parameters. The structural and morphological properties of the products were characterized and confirmed by powder X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and surface analyzer, respectively. Thermal behaviors were also investigated by TG/DT analyses. The optimal condition was set at 500 °C in a few minutes, giving pure iron orthophosphate with a good level of crystallinity and 11,769 m{sup 2}/g surface area. The results proved SCS a time saving and practically applicable method.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Ultrasonic synthesis and photocatalytic performance of metal-ions doped TiO{sub 2} catalysts under solar light irradiation

Graphical abstract: Display Omitted Highlights: ► We synthesized eight metal-ions doped TiO{sub 2} catalysts by a unique ultrasonic method. ► Mg-doped TiO{sub 2} showed the highest photocatalytic performance under solar light. ► Surface area of catalyst dominates the photocatalytic efficiency under solar light. ► Crystal property and visible light activity are less important than surface area. -- Abstract: Eight metal-ions doped TiO{sub 2} (M-TiO{sub 2}) were successfully synthesized by an ultrasonic method, including Fe, Co, Ce, Cr, Mn, Mg, Ni and Ag ions. Among them, the 1% Mg–TiO{sub 2} shows the highest photocatalytic efficiency under solar light, which was determined by degrading rhodamine B (RhB) molecules in an aqueous solution. The synthesized M-TiO{sub 2} samples were characterized by XRD, BET Surface area, TEM, XPS and diffuse reflectance spectrum. Effects of synthesis conditions and characterized properties on photocatalytic efficiency of the M-TiO{sub 2} were investigated comprehensively. A positive correlation between specific surface area and photocatalytic efficiency of the M-TiO{sub 2} was found across different synthesis conditions. However, no clear correlation with photocatalytic efficiency was observed for crystal structure and radii of doping ions of the M-TiO{sub 2}. XPS study indicates the change of oxidation states of Mn ions in Mn–TiO{sub 2} during synthesis procedure from the initial Mn{sup 2+} to a mixture of Mn{sup 3+} and Mn{sup 4+} ions. Dye sensitization mechanism was observed during the photocatalytic procedure of the Mg–TiO{sub 2}, which enhanced the degradation efficiency of the Mg–TiO{sub 2} under solar light. Finally, no obvious loss of photocatalytic activity was observed for the Mg–TiO{sub 2} after five cycles of RhB degradation.

36 MATERIALS SCIENCE↗
DOE OSTI2013

NiO nanowall array prepared by a hydrothermal synthesis method and its enhanced electrochemical performance for lithium ion batteries

Graphical abstract: Self-supported NiO nanowall array is fabricated by a facile hydrothermal synthesis method and exhibits noticeable Li ion battery performance with good cycle life and high capacity. Highlights: ► NiO nanowall array is prepared by a hydrothermal synthesis method. ► NiO nanowall array with high capacity as anode material for Li ion battery. ► Nanowall array structure is favorable for fast ion/electron transfer. - Abstract: Free-standing quasi-single-crystalline NiO nanowall array is successfully fabricated via a simple hydrothermal synthesis method. The as-prepared NiO film exhibits a highly porous nanowall structure composed of many interconnected nanoflakes with thicknesses of ∼20 nm. The NiO nanowalls arrange vertically to the substrate resulting in the formation of extended porous net-like structure with pores of 30–300 nm. As anode material for lithium ion batteries, the quasi-single-crystalline NiO nanowall array exhibits pretty good electrochemical performances with high capacity, weaker polarization, higher coulombic efficiency and better cycling performance as compared to the dense polycrystalline NiO film. The quasi-single-crystalline NiO nanowall array presents an initial coulombic efficiency of 76% and good cycling life with a capacity of 564 mAh g{sup −1} at 0.5 A g{sup −1} after 50 cycles, higher than that of the dense polycrystalline NiO film (358 mAh g{sup −1}). The enhanced performance is due to the unique nanowall array structure providing faster ion/electron transport and better morphological stability.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Synthesis and characterization of LTA nanozeolite using barley husk silica: Mercury removal from standard and real solutions

Highlights: ► Silica extraction from barley husk with high purity for the synthesis of A nanozeolite. ► Free template A nanozeolite synthesized via new source of silica at low temperature. ► Optimization of SiO{sub 2}/Al{sub 2}O{sub 3}, Na{sub 2}O/SiO{sub 2} ratios, temperature and time of the synthesis. ► Utilizing of synthesized A nanozeolite for mercury removal from aqueous solutions. ► Mercury removal at optimized pH, contact time and adsorbent dose from real solution. - Abstract: In this study, synthesized Lined Type A (LTA) nanozeolite from barley husk silica (BHS) was used for mercury removal from standard and real aqueous solutions. The BHS in amorphous phase with 80% purity was extracted from barley husk ash (BHA), and used effectively as a new source of silica for the synthesis of NaA nanozeolite. The NaA nanocrystal in pure phase has been synthesized at low temperature, without adding any organic additives. The effects of heating time, reaction temperature, SiO{sub 2}/Al{sub 2}O{sub 3}, and Na{sub 2}O/SiO{sub 2} mole ratios on the crystallization of NaA nanozeolite were studied. The adsorption capacity of mercury (II) was studied as a function of pH, contact time, and amount of adsorbent. The crystallization of NaA nanozeolite from BHS was characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), Brunauer–Emmett–Teller (BET), and FTIR techniques. Moreover, concentration of Hg{sup 2+} ions in the aqueous solutions was analyzed by hydride generation atomic absorption spectroscopy method (HG-AAS). The standard and real samples analysis showed that NaA nanozeolite is capable of Hg{sup 2+} ions removal from the aqueous solutions. Efficiency of mercury (II) adsorption from real solutions onto the nano-sized NaA zeolite was 98%.

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

In situ synthesis of TiH{sub 2} layer on metallic titanium foil through gaseous hydrogen free acid-hydrothermal method

Graphical abstract: The reaction mechanism for in situ synthesizing TiH{sub 2} layer on titanium foil by a gaseous hydrogen free acid-hydrothermal methodology. - Highlights: • A dense TiH{sub 2} layer is synthesized by a hydrogen free acid-hydrothermal method. • Hydrogen in a TiH{sub 2} layer synthesized can release at low temperature. • During the dehydrogenation process, there is no any intermediate phase forming. • We report a method of low-cost, low-risk and convenience toward productive TiH{sub 2}. - Abstract: A novel strategy for synthesis of TiH{sub 2} layer on surface of metallic titanium by using an acid-hydrothermal method was proposed. During the synthesis process, no any elemental hydrogen was involved. X-ray powder diffraction, energy-dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy and scanning electron microscopy results confirmed that a TiH{sub 2} layer of 20 μm thickness on a Ti foil surface can be formed in situ by an interface reaction of metallic titanium with sulfuric acid solution, hydrochloric acid, or phosphoric acid, which is a hydrogen self-storage process. By tuning reaction parameters, for example, concentration of acid, composition and morphology of TiH{sub 2}-Ti hybrid materials can be adjusted. The TiH{sub 2} layer on a metallic titanium surface can be decompounded completely heated below 400 °C. This convenient, safe and low-cost method is a promising gaseous hydrogen free approach for the synthesis of hydride-based hydrogen storage materials.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Low-temperature hydrothermal synthesis of the three-layered sodium cobaltite P3-Na{sub x}CoO{sub 2} (x ∼ 0.60)

Highlights: • We report direct synthesis of the high temperature stable phase, P3-Na{sub 0.6}CoO{sub 2}. • The hydrothermal synthesis of P3-Na{sub 0.6}CoO{sub 2} involves one step and low temperature. • The yield diagram for Na–Co–H{sub 2}O system has been builded up to 250 °C. • We propose a formation mechanism of P3-Na{sub 0.6}CoO{sub 2} phase using the unit cell theory. • The thermal stability of P3-Na{sub 0.6}CoO{sub 2} has been investigated by means of HT-XRD. - Abstract: In order to obtain the layered sodium cobalt oxide materials by hydrothermal synthesis, the yield diagram for Na–Co–H{sub 2}O system has been built and studied. In the same time, the well-known data of Co–H{sub 2}O system have been extended at 250 °C in basic solution. We had first synthesized directly the high temperature stable phase, P3-Na{sub 0.6}CoO{sub 2} by a one-step low-temperature hydrothermal method. The rhombohedral structure of P3-Na{sub 0.6}CoO{sub 2} has been determined by X-ray diffraction (XRD) and the purity of phases has been confirmed by XPS. The thermal stability of P3-Na{sub 0.6}CoO{sub 2} has been investigated by means of high temperature X-ray diffraction in 298–873 K range and when the temperature has reached 723 K, the completely transformation of P3-Na{sub 0.6}CoO{sub 2} in the rhombohedral stable phase α-NaCoO{sub 2} (space group R-3m) was observed. Also, a formation mechanism of P3-Na{sub 0.6}CoO{sub 2} phase using the unit cell theory in the hydrothermal process was proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Influence of starting precursors and synthesis methods on the physiochemical properties of zirconia

Graphical abstract: Crystallite size of tetragonal phase of the zirconia samples prepared using different synthesis parameters and precursors as a function of calcination temperature. Surface area values of the zirconia samples calcined at 500 and 700 °C are in given brackets. - Highlights: • Zirconia prepared with modified sol–gel method is less stable compared with zirconia prepared by precipitation method. • Optimized synthesis conditions shifted the glow exotherm to higher temperature range indicating better thermal stability. • Tetragonal-zirconia could be synthesized in cost-effective manner using zirconium oxy-nitrate. • In our studies no co-relation between the surface area and crystallite size was observed. - Abstract: Under identical and judiciously pre-optimized synthesis conditions, the influence of different combinations of zirconium sources and/or post treatment conditions on structural properties, thermal stability, phase composition and morphology of zirconia has been investigated. High surface area tetragonal zirconia could be synthesized in a cost-effective manner from 1 M solution of zirconium oxy-nitrate at pH 11 using aqueous ammonia solution as a precipitant when calcined at 400 °C for 3 h. Irrespective of the preparation method, pH and starting precursor, zirconia samples prepared without digestion contained dominant monoclinic phase with some traces of tetragonal phase when calcined at 700 °C. Even though there is linear decrease in surface area with increase in the crystallite size for each sample as a function of calcination temperature, no co-relation between the surface area and crystallite size could be achieved. SEM images show agglomerated and irregular shape particles between 10 to 20 μm.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Synthesis of magnesium aluminate spinel by periclase and alumina chlorination

Highlights: • Use of chlorination for the synthesis of magnesium aluminate spinel. • The reagents used were alumina, periclase and chlorine. • Isothermal and non-isothermal assays were performed in air and Cl{sub 2}–N{sub 2} flows. • The chlorination produced magnesium aluminate spinel at 700 °C. • Selectivity of the chlorination reaction to obtain spinel is very high. - Abstract: A pyrometallurgical route for the synthesis of magnesium aluminate spinel by thermal treatment of a mechanical mixture containing 29 wt% MgO (periclase) and 71 wt% Al{sub 2}O{sub 3} (alumina) in chlorine atmosphere was developed and the results were compared with those obtained by calcining the same mixture of oxides in air atmosphere. Isothermal and non-isothermal assays were performed in an experimental piece of equipment adapted to work in corrosive atmospheres. Both reagents and products were analyzed by differential thermal analysis (DTA), X-ray diffraction (XRD) and X-ray fluorescence (XRF). Thermal treatment in Cl{sub 2} atmosphere of the MgO–Al{sub 2}O{sub 3} mixture produces magnesium aluminate spinel at 700 °C, while in air, magnesium spinel is generated at 930 °C. The synthesis reaction of magnesium aluminate spinel was complete at 800 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Facile synthesis of efficient visible active C-doped TiO{sub 2} nanomaterials with high surface area for the simultaneous removal of phenol and Cr(VI)

Highlights: • Facile synthesis of C-doped TiO{sub 2} nanomaterials with high surface area. • Utilization of citric acid and ascorbic acid as fuels based on evolution of gases. • Enhanced visible activity for the oxidation of phenol and reduction of Cr(VI). • Study of simultaneous oxidation of phenol and reduction of Cr(VI) for the first time. • Proposed plausible mechanism for the simultaneous removal of phenol and Cr(VI). - Abstract: A single step synthesis of carbon doped TiO{sub 2} (anatase) nanomaterials have been reported by using combustion synthesis using ascorbic acid and citric acid fuels. X-ray diffraction studies indicated the formation of nanosized anatase titania, whereas, transmission electron microscopy confirmed the formation of nanosized TiO{sub 2} anatase. The carbon doping into TiO{sub 2} matrix was identified by X-ray photoelectron spectroscopy, whereas, thermogravimetric study quantified the carbon doping. Diffuse reflectance UV–vis spectra indicated the band gap of less than 3 eV, a prerequisite for the photocatalytic activity under visible light irradiation. The N{sub 2} adsorption studies revealed the high surface area (upto 290 m{sup 2}/g) of the synthesized photocatalysts. Typical photocatalytic activity data indicated that the simultaneous removal of Cr(VI) and phenol is advantageous than degradation of the individual pollutants.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Synthesis of water soluble glycine capped silver nanoparticles and their surface selective interaction

Highlights: • Synthesis of water soluble silver nanoparticles at ambient reaction conditions. • Glycine as stabilizing agent for silver nanoparticles. • Surface selective interaction of glycine with silver nanoparticles. • Glycine concentration influences crystalinity and optical property of silver nanoparticles. - Abstract: Synthesis of biocompatible metal nanoparticles has been an area of significant interest because of their wide range of applications. In the present study, we have successfully synthesized water soluble silver nanoparticles assisted by small amino acid glycine. The method is primarily based on reduction of AgNO{sub 3} with NaBH{sub 4} in aqueous solution under atmospheric air in the presence of glycine. UV–vis spectroscopy, transmission electron microscopy (TEM), X–ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, thermogravimetry (TG) and differential thermal analysis (DTA) techniques used for characterization of resulting silver nanoparticles demonstrated that, glycine is an effective capping agent to stabilize silver nanoparticles. Surface selective interaction of glycine on (1 1 1) face of silver nanoparticles has been investigated. The optical property and crystalline behavior of silver nanoparticles were found to be sensitive to concentration of glycine. X–ray diffraction studies ascertained the phase specific interaction of glycine on silver nanoparticles. Silver nanoparticles synthesized were of diameter 60 nm. We thus demonstrated an efficient synthetic method for synthesis of water soluble silver nanoparticles capped by amino acid under mild reaction conditions with excellent reproducibility.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Amorphous RE–Fe–B–Na colloidal nanoparticles: High temperature solution synthesis and magnetic properties

Graphical abstract: RE–Fe–B–Na (RE = Nd–Er) colloidal nanoparticles by high-temperature solution synthesis are ultra-small monodisperse and air-stable amorphous, whose size and magnetic dependence are studied. - Highlights: • RE–Fe–B–Na nanoparticles are obtained by high-temperature solution synthesis. • These colloidal nanoparticles are monodisperse and size controlled. • The magnetism dependence and possible magnetic coupling mechanism are studied. - Abstract: RE–Fe–B–Na (RE = Nd–Er) colloidal nanoparticles are prepared by high-temperature solution synthesis. These nanoparticles are ultra-small monodisperse, air-stable and amorphous, whose particle size and magnetic property are characterized by transmission electron microscope and superconducting quantum interference device. Taking Nd–Fe–B–Na nanoparticle as an example, it is found that the particle size can be controlled in less than 7 nm. Besides, the magnetic properties of RE–Fe–B–Na colloidal nanoparticles can be compared for different rare earth elements. Based on the bulk ferromagnetic coupling, other possible magnetic coupling mechanism is discussed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Photon up-conversion production in Tb{sup 3+}–Yb{sup 3+} co-doped CaF{sub 2} phosphors prepared by combustion synthesis

Graphical abstract: Up-conversion luminescence from Tb{sup 3+} obtained by energy transfer from Yb{sup 3+} pairs in CaF{sub 2} powder prepared by combustion synthesis. - Highlights: • Calcium fluoride (CaF{sub 2}) powders were prepared by combustion synthesis. • Rare-earth ions doped in this material were found in interstitial sites. • Cooperative up-conversion was observed in Tb{sup 3+}:Yb{sup 3+}:CaF{sub 2} powder. • Energy transfer between Tb{sup 3+} and pairs of Yb{sup 3+} was analyzed using rate equations. - Abstract: Calcium fluoride (CaF{sub 2}) crystalline powders were successfully prepared by the combustion synthesis method. The powder material containing luminescent rare-earth ions, more specifically terbium (Tb{sup 3+}) and ytterbium (Yb{sup 3+}), was studied by X-ray diffraction, scanning electronic microscopy and optical spectroscopy. These ions are allocated in charge compensated interstitial positions of tetragonal (C{sub 4v}) and trigonal (C{sub 3v}) symmetry sites of the cubic (O{sub h}) CaF{sub 2} lattice. Up-conversion (UC) luminescence in Tb{sup 3+} was achieved using a low power diode laser operating at 975 nm. Tb{sup 3+} is insensitive to near-infrared radiation but UC can be achieved via energy transfer from pairs of Yb{sup 3+} ions to Tb{sup 3+} ions. The UC luminescence dynamics of Tb{sup 3+} was used to study the energy transfer mechanism.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Low-temperature hydrothermal synthesis of ZnO nanorods: Effects of zinc salt concentration, various solvents and alkaline mineralizers

Highlights: • We synthesized ZnO nanorods by a simple hydrothermal process at 60 °C. • Effects of zinc salt concentration, solvent and alkaline mineralizer was studied. • Increasing concentration of zinc salt changed ZnO nucleation system. • NaOH yielded better results in the production of nanorods in both solvents. • Methanol performed better in the formation of nanorods using the two mineralizers. - Abstract: ZnO has been produced using various methods in the solid, gaseous, and liquid states, and the hydrothermal synthesis at low temperatures has been shown to be an environmentally-friendly one. The current work utilizes a low reaction temperature (60 °C) for the simple hydrothermal synthesis of ZnO nanorod morphologies. Furthermore, the effects of zinc salt concentration, solvent type and alkaline mineralizer type on ZnO nanorods synthesis at a low reaction temperature by hydrothermal processing was studied. Obtained samples were analyzed using X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). Increasing the concentration of the starting zinc salt from 0.02 to 0.2 M changed ZnO nucleation system from the homogeneous to the heterogeneous state. The XRD results confirmed the production hexagonal ZnO nanostructures of with a crystallite size of 40.4 nm. Varying the experimental parameters (mineralizer and solvent) yielded ZnO nanorods with diameters ranging from 90–250 nm and lengths of 1–2 μm.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Irradiation route to aqueous synthesis of highly luminescent ZnSe quantum dots and its function as a copper ion fluorescence sensor

Highlights: • Radiation chemical technique can provide a useful route for synthesis of ZnSe QDs. • Chelating nature of ethylene diamine is exploited for capping nanoparticles. • ZnSe QDs can be a suitable sensitive alternative to toxic cadmium-based system. • Cu(II) ion is probed by QDs in the presence of other physiologically relevant ions. - Abstract: Size-controlled synthesis of stable ZnSe QDs with narrow distribution in aqueous environment through conventional soft chemical method still poses a challenge. The proposed radiation assisted strategy demonstrates aqueous synthesis of stable, monodisperse and luminescent ZnSe QDs capped with chelating ethylene diamine under ambient conditions and at room temperature. Radiation chemical method facilitates in slow and in-situ release of selenium ion from sodium selenosulfate. The concentrations of precursors, such as zinc salt, selenium source, ethylene diamine and absorbed radiation (7–90 kGy) dose were optimized for obtaining good quality particles. Selective quenching of luminescence of as-synthesized quantum dots (QDs) by Cu{sup 2+} ions vis-à-vis other physiologically important cations provide evidence for use of ZnSe quantum dots as alternative to toxic Cd-based quantum dots to probe Cu{sup 2+} ions. The linear relation of ratio of loss in emission intensity as a function of concentration of Cu(II) indicates detection limit in nano-molar range.

36 MATERIALS SCIENCE↗