Synthesis and Characterization of Monodisperse Core-shell Lanthanide Upconversion Nanoparticles NaYF4: Yb,Tm/SiO2

NASA Astrophysics Data System (ADS)

Manurung, R. V.; Wiranto, G.; Hermida, I. D. P.

2018-05-01

Lanthanide up-converting luminescent nanoparticles (UCNPs) are exciting and promising materials for optical bioimaging, biosensor and theranostic due to their unique and advantageous optical and chemical properties. The UCNPs absorb low energy near-infrared (NIR) light and emit high-energy shorter wavelength photons (visible light). Their unique features allow them to overcome various problems associated with conventional imaging probes such as photostability, lack of toxicity, and to provide versatility for creating nanoplatforms with both imaging and therapeutic modalities. This paper reports synthesis and characterization of core-shell structured of NaYF4:Yb,Tm/SiO2 microspheres. The synthesis of lanthanide upconversion nanoparticles NaYF4:Yb,Tm was prepared by thermal decomposition process which involves dissolving organic precursors in high-boiling-point solvents oleic acid (OA) and octadecene (ODE). After that, the NaYF4:Yb,Tm phosphors was coated by silica via reverse microemulsion process to obtain core-shell structured NaYF4:Yb,Tm/SiO2. Scanning electron microscopy, transmission electron microscopy, specific area electron diffraction, and photoluminescence were applied to characterize these samples. The obtained core-shell structured NaYF4:Yb,Tm/SiO2 phosphors exhibit a perfect cubic morphology with narrow size distribution and smooth surface. Upon IR excitation at 980 nm, the NaYF4:Yb,Tm/SiO2 samples exhibit whitish blue upconversion (UC) luminescence, respectively. These phosphors show potential applications in the displaying on biological fields and biosensing.

Synthesis and characterization of RuO(2)/poly(3,4-ethylenedioxythiophene) composite nanotubes for supercapacitors.

PubMed

Liu, Ran; Duay, Jonathon; Lane, Timothy; Bok Lee, Sang

2010-05-07

We report the synthesis of composite RuO(2)/poly(3,4-ethylenedioxythiophene) (PEDOT) nanotubes with high specific capacitance and fast charging/discharging capability as well as their potential application as electrode materials for a high-energy and high-power supercapacitor. RuO(2)/PEDOT nanotubes were synthesized in a porous alumina membrane by a step-wise electrochemical deposition method, and their structures were characterized using electron microscopy. Cyclic voltammetry was used to qualitatively characterize the capacitive properties of the composite RuO(2)/PEDOT nanotubes. Their specific capacitance, energy density and power density were evaluated by galvanostatic charge/discharge cycles at various current densities. The pseudocapacitance behavior of these composite nanotubes originates from ion diffusion during the simultaneous and parallel redox processes of RuO(2) and PEDOT. We show that the energy density (specific capacitance) of PEDOT nanotubes can be remarkably enhanced by electrodepositing RuO(2) into their porous walls and onto their rough internal surfaces. The flexible PEDOT prevents the RuO(2) from breaking and detaching from the current collector while the rigid RuO(2) keeps the PEDOT nanotubes from collapsing and aggregating. The composite RuO(2)/PEDOT nanotube can reach a high power density of 20 kW kg(-1) while maintaining 80% energy density (28 Wh kg(-1)) of its maximum value. This high power capability is attributed to the fast charge/discharge of nanotubular structures: hollow nanotubes allow counter-ions to readily penetrate into the composite material and access their internal surfaces, while a thin wall provides a short diffusion distance to facilitate ion transport. The high energy density originates from the RuO(2), which can store high electrical/electrochemical energy intrinsically. The high specific capacitance (1217 F g(-1)) which is contributed by the RuO(2) in the composite RuO(2)/PEDOT nanotube is realized because of the high

Development and characterization of Mn{sup 2+}-doped MgO nanoparticles by solution combustion synthesis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Basha, Md. Hussain; Gopal, N. O., E-mail: nogopal@yahoo.com; Rao, J. L.

2015-06-24

Mn doped MgO Nanoparticles have been prepared by Solution Combustion Synthesis. The synthesized sample is characterized by X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Electron Paramagnetic Resonance (EPR). The prepared MgO:Mn (1 mol%) nano crystals appear to be of simple cubic crystalline phase with lattice parameters a = 4.218(2) Å and cell volume = 74.98 (7) Å{sup 3}. SEM micrograph of powders show highly porous, many agglomerates with irregular morphology, large voids, cracks and pores. EPR spectrum of the sample at room temperature exhibit an isotropic sextet hyperfine pattern, centered at g=1.99, characteristic if Mn{sup 2+} ions with S=I=5/2.The observedmore » g value and the hyperfine value reveal the ionic bonding between Mn{sup 2+} and its surroundings.« less

Synthesis, characterization and multifunctional properties of plasmonic Ag-TiO2 nanocomposites

NASA Astrophysics Data System (ADS)

Prakash, Jai; Kumar, Promod; Harris, R. A.; Swart, Chantel; Neethling, J. H.; Janse van Vuuren, A.; Swart, H. C.

2016-09-01

We report on the synthesis of multifunctional Ag-TiO2 nanocomposites and their optical, physio-chemical, surface enhanced Raman scattering (SERS) and antibacterial properties. A series of Ag-TiO2 nanocomposites were synthesized by sol-gel technique and characterized by x-ray diffraction, scanning and transmission electron microscopy, energy-dispersed x-ray analysis, photoluminescence, UV-vis, x-ray photoelectron and Raman spectroscopy and Brunauer-Emmett-Teller method. The Ag nanoparticles (NPs) (7-20 nm) were found to be uniformly distributed around and strongly attached to TiO2 NPs. The novel optical responses of the nanocomposites are due to the strong electric field from the localized surface plasmon (LSP) excitation of the Ag NPs and decreased recombination of photo-induced electrons and holes at Ag-TiO2 interface providing potential materials for photocatalysis. The nanocomposites show enhancement in the SERS signals of methyl orange (MO) molecules with increasing Ag content attributed to the long-range electromagnetic enhancement from the excited LSP of the Ag NPs. To further understand the SERS activity, molecular mechanics and molecular dynamics simulations were used to study the geometries and SERS enhancement of MO adsorbed onto Ag-TiO2 respectively. Simulation results indicate that number of ligands (MO) that adsorb onto the Ag NPs as well as binding energy per ligand increases with increasing NP density and molecule-to-surface orientation is mainly flat resulting in strong bond strength between MO and Ag NP surface and enhanced SERS signals. The antimicrobial activity of the Ag-TiO2 nanocomposites was tested against the bacterium Staphylococcus aureus and enhanced antibacterial effect was observed with increasing Ag content explained by contact killing action mechanism. These results foresee promising applications of the plasmonic metal-semiconductor based nano-biocomposites for both chemical and biological samples.

Synthesis and characterization of fluorapatite-titania (FAp-TiO 2) nanocomposite via mechanochemical process

NASA Astrophysics Data System (ADS)

Ebrahimi-Kahrizsangi, Reza; Nasiri-Tabrizi, Bahman; Chami, Akbar

2010-09-01

In this paper, synthesis of bionanocomposite of fluorapatite-titania (FAp-TiO 2) was studied by using one step mechanochemical process. Characterization of the products was accomplished by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. Based on XRD patterns and FT-IR spectroscopy, correlation between the structural features of the nanostructured FAp-TiO 2 and the process conditions was discussed. Variations in crystallite size, lattice strain, and volume fraction of grain boundary were investigated during milling and the following heat treatment. Crystallization of the nanocomposite occurred after thermal treatment at 650 °C. Morphological features of powders were influenced by the milling time. The resulting FAp-20 wt.%TiO 2 nanocomposite powder exhibited an average particle size of 15 nm after 20 h of milling. The results show that the one step mechanosynthesis technique is an effective route to prepare FAp-based nanocomposites with excellent morphological and structural features.

Synthesis and characterization of Ni doped ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Tamgadge, Y. S.; Gedam, P. P.; Ganorkar, R. P.; Mahure, M. A.; Pahurkar, V. G.; Muley, G. G.

2018-05-01

In this paper, we present synthesis of L-valine assisted surface modification of Ni doped ZnO nanoparticles (NPs) using chemical precipitation method. Samples were calcined at 500oC for 2h. Uncalcined and calcined samples were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and ultraviolet-visible (UV-vis) spectroscopy. Ni doped ZnO NPs with average particle size of 8 nm have been successfully obtained using L-valine as surface modifying agent. Increase in the particle size was observed after the calcination. XRD and TEM studies confirmed the purity, surface morphology and hexagonal wurtzite crystal structure of ZnO NPs. UV-vis spectroscopy indicated the blue shift of excitons absorption wavelength and surface modification by L-valine.

Synthesis of Nanoscale CaO-Al2O3-SiO2-H2O and Na2O-Al2O3-SiO2-H2O Using the Hydrothermal Method and Their Characterization

PubMed Central

Yang, Jingbin; Li, Dongxu; Fang, Yuan

2017-01-01

C-A-S-H (CaO-Al2O3-SiO2-H2O) and N-A-S-H (Na2O-Al2O3-SiO2-H2O) have a wide range of chemical compositions and structures and are difficult to separate from alkali-activated materials. Therefore, it is difficult to analyze their microscopic properties directly. This paper reports research on the synthesis of C-A-S-H and N-A-S-H particles with an average particle size smaller than 300 nm by applying the hydrothermal method. The composition and microstructure of the products with different CaO(Na2O)/SiO2 ratios and curing conditions were characterized using XRD, the RIR method, FTIR, SEM, TEM, and laser particle size analysis. The results showed that the C-A-S-H system products with a low CaO/SiO2 ratio were mainly amorphous C-A-S-H gels. With an increase in the CaO/SiO2 ratio, an excess of Ca(OH)2 was observed at room temperature, while in a high-temperature reaction system, katoite, C4AcH11, and other crystallized products were observed. The katoite content was related to the curing temperature and the content of Ca(OH)2 and it tended to form at a high-temperature and high-calcium environment, and an increase in the temperature renders the C-A-S-H gels more compact. The main products of the N-A-S-H system at room temperature were amorphous N-A-S-H gels and a small amount of sodalite. An increase in the curing temperature promoted the formation of the crystalline products faujasite and zeolite-P. The crystallization products consisted of only zeolite-P in the high-temperature N-A-S-H system and its content were stable above 70%. An increase in the Na2O/SiO2 ratio resulted in more non-bridging oxygen and the TO4 was more isolated in the N-A-S-H structure. The composition and microstructure of the C-A-S-H and N-A-S-H system products synthesized by the hydrothermal method were closely related to the ratio of the raw materials and the curing conditions. The results of this study increase our understanding of the hydration products of alkali-activated materials. PMID

Synthesis, characterization, and thermal stability of SiO2/TiO2/CR-Ag multilayered nanostructures

NASA Astrophysics Data System (ADS)

Díaz, Gabriela; Chang, Yao-Jen; Philipossian, Ara

2018-06-01

The controllable synthesis and characterization of novel thermally stable silver-based particles are described. The experimental approach involves the design of thermally stable nanostructures by the deposition of an interfacial thick, active titania layer between the primary substrate (SiO2 particles) and the metal nanoparticles (Ag NPs), as well as the doping of Ag nanoparticles with an organic molecule (Congo Red, CR). The nanostructured particles were composed of a 330-nm silica core capped by a granular titania layer (10 to 13 nm in thickness), along with monodisperse 5 to 30 nm CR-Ag NPs deposited on top. The titania-coated support (SiO2/TiO2 particles) was shown to be chemically and thermally stable and promoted the nucleation and anchoring of CR-Ag NPs, which prevented the sintering of CR-Ag NPs when the structure was exposed to high temperatures. The thermal stability of the silver composites was examined by scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HRTEM). Larger than 10 nm CR-Ag NPs were thermally stable up to 300 °C. Such temperature was high enough to destabilize the CR-Ag NPs due to the melting point of the CR. On the other hand, smaller than 10 nm Ag NPs were stable at temperatures up to 500 °C because of the strong metal-metal oxide binding energy. Energy dispersion X-ray spectroscopy (EDS) was carried out to qualitatively analyze the chemical stability of the structure at different temperatures which confirmed the stability of the structure and the existence of silver NPs at temperatures up to 500 °C.

Sb:SnO2 thin films-synthesis and characterization

NASA Astrophysics Data System (ADS)

Bhadrapriya B., C.; Varghese, Anitta Rose; Amarendra, G.; Hussain, Shamima

2018-04-01

Transparent thin films of antimony doped SnO2 have been synthesized and characterized using optical spectroscopy, XRD, RAMAN and FESEM. The band gap of Sb doped tin oxide thin film samples were found to vary from 3.26 eV to 3.7 eV. The XRD peaks showed prominent rutile SnO2 peaks with diminished intensity due to antimony doping. A wide band in the range 550-580 cm-1 was observed in raman spectra and is a feature of nano-sized SnO2. SEM images showed flower-like structures on thin film surface, a characteristic feature of antimony.

Cobalt–iron nano catalysts supported on TiO{sub 2}–SiO{sub 2}: Characterization and catalytic performance in Fischer–Tropsch synthesis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Feyzi, Mostafa, E-mail: Dalahoo2011@yahoo.com; Yaghobi, Nakisa; Eslamimanesh, Vahid

2015-12-15

Graphical abstract: The Co–Fe/TiO{sub 2}–SiO{sub 2} catalysts were prepared. The prepared catalysts were tested for light olefins and C{sub 5}–C{sub 12} production. The best operational conditions are 250 °C, H{sub 2}/CO = 1/1 under 5 bar pressure. - Highlights: • The TiO{sub 2}–SiO{sub 2} supported cobalt–iron catalysts were prepared via sol–gel method. • The best operational conditions were 250 °C, GHSV = 2000 h{sup −1}, H{sub 2}/CO = 1/1 and 5 bar. • The (Co/Fe)/TiO{sub 2}–SiO{sub 2} is efficient catalyst for light olefins and C{sub 5}–C{sub 12} production. - Abstract: A series of Co–Fe catalysts supported on TiO{sub 2}–SiO{sub 2}more » were prepared by the sol–gel method. This research investigated the effects of (Co/Fe) wt.%, the solution pH, different Co/Fe molar ratio, calcination conditions and different promoters on the catalytic performance of cobalt–iron catalysts for the Fisher–Tropsch synthesis (FTS). It was found that the catalyst containing 35 wt.% (Co–Fe)/TiO{sub 2}–SiO{sub 2} (Co/Fe molar ratio is 80/20) promoted with 1.5 wt.% Cu and calcined in air atmosphere at 600 °C for 7 h with a heating rate of 3 °C min{sup −1} is an optimal nano catalyst for converting synthesis gas to light olefins and C{sub 5}–C{sub 12} hydrocarbons. The effects of operational conditions such as the H{sub 2}/CO ratio, gas hourly space velocity (GHSV), different reaction temperature, and reaction pressure were investigated. The results showed that the best operational conditions for optimal nano catalyst are 250 °C, GHSV = 2000 h{sup −1}, H{sub 2}/CO molar ratio 1/1 under 5 bar total pressure. Catalysts and precursors were characterized by, X-ray diffraction (XRD), scanning electron microcopy (SEM), thermal gravimetric analysis (TGA), differential scanning calorimetry (DSC), temperature program reduction (TPR) and N{sub 2} adsorption–desorption measurements.« less

Synthesis and Structural Characterization of a Novel Indium Mercapto Derivative [clln(sch2(co)o)2]2-[(4-mepyh)2]2+

NASA Technical Reports Server (NTRS)

Banger, Kulbinder K.; Duraj, Stan A.; Fanwick, Philip E.; Hepp, Aloysius F.; Martock, Robert A.

2004-01-01

The synthesis and structural characterization of a novel In(III) complex is described. The reaction between InCl3 with sodium mercapto-acetic acid, (NaSCH2(CO)OH) in 4-methylpyridine, (CH3(C5H5N), (4-Mepy)) at 25 C affords [ClIn(SCH2(CO)O)2]2- [(4-MepyH)2]2+. X-ray diffraction studies show it to have a distorted square pyramidal geometry, with the [(-SCH2(CO)CO-)] ligands in a trans conformation. The compound crystallizes in the P(raised dash) 1 (No. 2) space group with a = 7.8624 Angstrom, b = 9.950 Angstrom, c = 13.793 Angstrom, alpha = 107.60 degrees, beta= 90.336 degrees, gamma = 98.983 degrees, V = 1014.3 Angstroms (sup 3), R(F(raised circle)) = 0.037, and R(sub w) = 0.048.

Self-standing crystalline TiO2 nanotubes/CNTs heterojunction membrane: synthesis and characterization.

PubMed

Hesabi, Zohreh R; Allam, Nageh K; Dahmen, Klaus; Garmestani, Hamid; A El-Sayed, Mostafa

2011-04-01

In the present study, we report for the first time synthesis of TiO(2) nanotubes/CNTs heterojunction membrane. Chemical vapor deposition (CVD) of CNTs at 650 °C in a mixture of H(2)/He atmosphere led to in situ detachment of the anodically fabricated TiO(2) nanotube layers from the Ti substrate underneath. Morphological and structural evolution of TiO(2) nanotubes after CNTs deposition were investigated by field- emission scanning electron microscopy (FESEM), glancing angle X-ray diffraction (GAXRD), and X-ray photoelectron spectroscopy (XPS) analyses. © 2011 American Chemical Society

Synthesis and Characterization of A2Mo3O 12 Materials

NASA Astrophysics Data System (ADS)

Young, Lindsay Kay

Negative thermal expansion (NTE) materials have attracted considerable research interest in recent decades. These unique materials shrink when heated, offering a potential means to control the overall thermal expansion of composites. Several families of materials display this behavior, the largest of which is the A2Mo3O12 family (also called the scandium tungstate family), in which A is a trivalent cation and M is molybdenum or tungsten. These materials show NTE in an orthorhombic structure, but many members transform to a monoclinic structure with positive expansion at low temperatures. Many properties of these materials are dependent on their elemental composition, especially the identity of the A3+ cation. This includes the magnitude of NTE, as well as the phase transition behavior as a function of temperature and pressure. It is also possible to create "mixed site" cation A2Mo3O12 materials, in which the A site is occupied by two different cations. These are described as AxA'2-xM3O12 materials, as the composition A:A' can vary. Creating these new compositions may result in different phase transition properties or the ability to tune the NTE properties of these materials. In this work, the focus was on synthesis and characterization of indium gallium molybdate (InxGa2-xM3O12). The non-hydrolytic sol-gel (NHSG) method was used to synthesize indium gallium molybdate while exploring a variety of reaction parameters. While the goal was to create stoichiometric, homogenous materials, it was found that this could not be accomplished using easily accessible parameters during NHSG reactions. However, it was discovered that certain conditions allowed unusually low temperature (230 °C) crystallization of these materials. Similar conditions were explored for single cation A2Mo3O12 materials, and it was determined that crystallization of indium molybdate, iron molybdate, and scandium molybdate was possible at temperatures of 230 or 300 °C. This extremely low temperature

Synthesis, characterization and electrocatalytic properties of delafossite CuGaO{sub 2}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ahmed, Jahangeer; Department of Chemistry, College of Science, King Saud University, Riyadh 11451; Mao, Yuanbing, E-mail: yuanbing.mao@utrgv.edu

2016-10-15

Delafossite CuGaO{sub 2} has been employed as photocatalysts for solar cells, but their electrocatalytic properties have not been extensively studied, especially no comparison among samples made by different synthesis routes. Herein, we first reported the successful synthesis of delafossite CuGaO{sub 2} particles with three different morphologies, i.e. nanocrystalline hexagons, sub-micron sized plates and micron–sized particles by a modified hydrothermal method at 190 °C for 60 h [1–3], a sono-chemical method followed by firing at 850 °C for 48 h, and a solid state route at 1150 °C, respectively. Morphology, composition and phase purity of the synthesized samples was confirmed bymore » powder X-ray diffraction and Raman spectroscopic studies, and then their electrocatalytic performance as active and cost effective electrode materials to the oxygen and hydrogen evolution reactions in 0.5 M KOH electrolyte versus Ag/AgCl was investigated and compared under the same conditions for the first time. The nanocrystalline CuGaO{sub 2} hexagons show enhanced electrocatalytic activity than the counterpart sub-micron sized plates and micron-sized particles. - Graphical abstract: Representative delafossite CuGaO2 samples with sub-micron sized plate and nanocrystalline hexagon morphologies accompanying with chronoamperometric voltammograms for oxygen evolution reaction and hydrogen evolution reaction in 0.5 M KOH electrolyte after purged with N{sub 2} gas. - Highlights: • Delafossite CuGaO{sub 2} with three morphologies has been synthesized. • Phase purity of the synthesized samples was confirmed. • Comparison on their electrocatalytic properties was made for the first time. • Their use as electrodes for oxygen and hydrogen evolution reactions was evaluated. • Nanocrystalline CuGaO{sub 2} hexagons show highest electrocatalytic activity.« less

Effect of TiO2, ZrO2, and TiO2-ZrO2 on the performance of CuO-ZnO catalyst for CO2 hydrogenation to methanol

NASA Astrophysics Data System (ADS)

Xiao, Jie; Mao, Dongsen; Guo, Xiaoming; Yu, Jun

2015-05-01

The influence of TiO2, ZrO2, and TiO2-ZrO2 mixed oxide on the catalytic performance of CuO-ZnO catalyst in the methanol synthesis from CO2 hydrogenation was studied. The catalysts were prepared by oxalate co-precipitation method and characterized by TGA, N2 adsorption, XRD, reactive N2O adsorption, XPS, H2-TPR, H2-TPD, and CO2-TPD techniques. Characterization results reveal that all the additives improve the CuO dispersion in the catalyst body and increase the Cu surface area and adsorption capacities of CO2 and H2. The results of catalytic test reveal that the additives increase both the CO2 conversion and methanol selectivity, and TiO2-ZrO2 mixed oxide is more effective than single components of TiO2 or ZrO2. Moreover, the activity of methanol synthesis is correlated directly with CO2 adsorption capacity over the catalysts.

Synthesis and White-Light Emission of ZnO/HfO2: Eu Nanocables

PubMed Central

2010-01-01

ZnO/HfO2:Eu nanocables were prepared by radio frequency sputtering with electrospun ZnO nanofibers as cores. The well-crystallized ZnO/HfO2:Eu nanocables showed a uniform intact core–shell structure, which consisted of a hexagonal ZnO core and a monoclinic HfO2 shell. The photoluminescence properties of the samples were characterized. A white-light band emission consisted of blue, green, and red emissions was observed in the nanocables. The blue and green emissions can be attributed to the zinc vacancy and oxygen vacancy defects in ZnO/HfO2:Eu nanocables, and the yellow–red emissions are derived from the inner 4f-shell transitions of corresponding Eu3+ ions in HfO2:Eu shells. Enhanced white-light emission was observed in the nanocables. The enhancement of the emission is ascribed to the structural changes after coaxial synthesis. PMID:20730130

Single step synthesis and characterization of ZnAl2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Jain, Megha; Manju, Singh, Kulwinder; Kumar, Akshay; Sharma, Jeewan; Chae, K. H.; Vij, Ankush; Thakur, Anup

2018-05-01

Zinc aluminate (ZnAl2O4) has proved to be a potential candidate in many areas such as catalysis, display panels, pigments in paints, radiation dosimetry, luminescence etc. Here, we report the solution combustion synthesis & spectroscopic studies of ZnAl2O4 nanoparticles. Urea (fuel) and metal nitrates (oxidizer) were taken in stoichiometric ratio at 1:1. The X-ray diffraction analysis of the as-prepared and annealed samples showed all reflection planes pertaining to ZnAl2O4. However, a weak intensity peak of secondary phase was also observed at 2θ value of 34.5°, which correspond to the diffraction plane (002) of ZnO. This phase was found to disappear after annealing the sample at 1000 °C for 1 hour. Fourier transform infrared spectroscopy (FTIR) also inferred the formation of ZnAl2O4. Photoluminescence measurements carried out on samples at excitation wavelength of 345 nm showed that ZnAl2O4 is an efficient luminescent material with emission in violet region of visible spectra.

Microwave-assisted synthesis of C-doped TiO2 and ZnO hybrid nanostructured materials as quantum-dots sensitized solar cells

NASA Astrophysics Data System (ADS)

Rangel-Mendez, Jose R.; Matos, Juan; Cházaro-Ruiz, Luis F.; González-Castillo, Ana C.; Barrios-Yáñez, Guillermo

2018-03-01

The microwave-assisted solvothermal synthesis of C-doped TiO2 and ZnO hybrid materials was performed. Saccharose, titanium isopropoxide and zinc acetate were used as organic and inorganic sources for the synthesis. The influence of temperature and reaction time on the textural and optoelectronic properties of the hybrid materials was verified. Carbon quantum-dots of TiO2 and ZnO nanostructured spheres were obtained in a second pot by controlled calcination steps of the precursor hybrid materials. A carefully characterization by adsorption-desorption N2 isotherms, XRD, XPS, SEM, UV-vis/DR and electro- and photo-electrochemistry properties of the carbon quantum-dots TiO2 and ZnO spheres was performed. The photoelectrochemical activity of TiO2-C and ZnO-C films proved to be dependent on the conditions of synthesis. It was found a red-shift in the energy band gap of the semiconductors with values of 3.02 eV and 3.13 eV for the TiO2-C and ZnO-C, respectively, clearly lower than those on bare semiconductors, which is associated with the C-doping effect. From the photo-electrochemistry characterization of C-doped TiO2 and ZnO films can be concluded that the present materials have potential applications as photoelectrodes for quantum-dots sensitized solar cells.

Low-Cost and Facile Synthesis of the Vanadium Oxides V2O3, VO2, and V2O5 and Their Magnetic, Thermochromic and Electrochromic Properties.

PubMed

Mjejri, Issam; Rougier, Aline; Gaudon, Manuel

2017-02-06

In this study, vanadium sesquioxide (V 2 O 3 ), dioxide (VO 2 ), and pentoxide (V 2 O 5 ) were all synthesized from a single polyol route through the precipitation of an intermediate precursor: vanadium ethylene glycolate (VEG). Various annealing treatments of the VEG precursor, under controlled atmosphere and temperature, led to the successful synthesis of the three pure oxides, with sub-micrometer crystallite size. To the best of our knowledge, the synthesis of the three oxides V 2 O 5 , VO 2 , and V 2 O 3 from a single polyol batch has never been reported in the literature. In a second part of the study, the potentialities brought about by the successful preparation of sub-micrometer V 2 O 5 , VO 2 , and V 2 O 3 are illustrated by the characterization of the electrochromic properties of V 2 O 5 films, a discussion about the metal to insulator transition of VO 2 on the basis of in situ measurements versus temperature of its electrical and optical properties, and the characterization of the magnetic transition of V 2 O 3 powder from SQUID measurements. For the latter compound, the influence of the crystallite size on the magnetic properties is discussed.

Copolymers of polyaniline and poly-o-toluidine: Electrochemical synthesis and characterization

NASA Astrophysics Data System (ADS)

Yadav, Pooja C.; Deshmukh, Megha A.; Patil, Harshada K.; Bodkhe, Gajanan A.; Sayyad, Pasha W.; Ingle, Nikesh N.; Shirsat, Mahendra D.

2018-05-01

In the present study we have reported Electrochemical polymerization of poly(Aniline) (PANI), Poly(O-Toluidine) (POT) and poly(Aniline-co-O-Toluidine) (PAOT) copolymers. Electrochemical Synthesis of PANI, POT and Poly(Aniline-co-O-Toluidine) was done by using Cyclic Voltammetry technique. The morphological study done by Atomic Force Microscopy (AFM) which shows that formation of uniform granular structure and topographic changes in each respective thin film. Spectroscopic characterization was done by FTIR spectroscopy. The FT-IR study revealed the formation of PANI/POT/Poly(Aniline co O-Toluidine) with a absorption band are reported. For structural information done by X-ray diffraction(XRD) Characterization.

Characterization and optimization of cathodic conditions for H2O2 synthesis in microbial electrochemical cells.

PubMed

Sim, Junyoung; An, Junyeong; Elbeshbishy, Elsayed; Ryu, Hodon; Lee, Hyung-Sool

2015-11-01

Cathode potential and O2 supply methods were investigated to improve H2O2 synthesis in an electrochemical cell, and optimal cathode conditions were applied for microbial electrochemical cells (MECs). Using aqueous O2 for the cathode significantly improved current density, but H2O2 conversion efficiency was negligible at 0.3-12%. Current density decreased for passive O2 diffusion to the cathode, but H2O2 conversion efficiency increased by 65%. An MEC equipped with a gas diffusion cathode was operated with acetate medium and domestic wastewater, which presented relatively high H2O2 conversion efficiency from 36% to 47%, although cathode overpotential was fluctuated. Due to different current densities, the maximum H2O2 production rate was 141 mg H2O2/L-h in the MEC fed with acetate medium, but it became low at 6 mg H2O2/L-h in the MEC fed with the wastewater. Our study clearly indicates that improving anodic current density and mitigating membrane fouling would be key parameters for large-scale H2O2-MECs. Copyright © 2015 Elsevier Ltd. All rights reserved.

Synthesis, Characterization and Comparative Luminescence Studies of Rare-Earth-Doped Gd2O3 Nanoparticles

NASA Astrophysics Data System (ADS)

Pyngrope, D.; Singh, L. R.; Prasad, A. I.; Bora, A.

2018-04-01

A facile direct precipitation method was used for the synthesis of luminescence nanomaterial. Gd2O3 doped with rare earth element Eu3+ is synthesized by polyol route. The synthesized nanoparticles show their characteristic red emission. The nanoparticles are characterized by x-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM) and photoluminescence (PL) study. The synthesized nanoparticles are spherical particles with 30 nm size. The photoluminescence studies show the characteristic Eu3+ red emission. The PL study shows the intensity of the magnetic dipole transition ( 5 D0 \\to 7 F1 ) at 592 nm compared to that of the electronic dipole transition ( 5 D0 \\to 7 F2 ) at 615 nm. The nanomaterials can show significant application in various display devices and biomedical applications for tracking.

Polysilicic acid gel method derived V2O5/SiO2 composite materials: Synthesis and characterization

NASA Astrophysics Data System (ADS)

Wang, Dawei; Zhou, Linzong; Feng, Xiaofei; Zhao, Ning; Yang, Bin

2017-01-01

The V2O5/SiO2 composite was prepared by a sol-gel method followed a sintering procedure. The low-cost Na2SiO3•9H2O was used as silicon source, while NH4VO3 was used as vanadium source. By adding NH4VO3 to Na2SiO3 solution and adjusting the mixture's pH with saturated (NH4)2SO4 solution the polysilicic acid gel was formed to give a homogeneous gel composite with VO3-well-distributed in it. The gel composite was dried at 100 °C to give the xerogel, then the xerogel was calcined in air to obtain the V2O5/SiO2 composite. The V2O5/SiO2 composites were characterized by SEM analysis, FT-IR spectroscopy and powder X-ray diffractions.

Effect of solvent on the synthesis of SnO{sub 2} nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Virender; Singh, Karamjit; Singh, Kulwinder

Tin oxide (SnO{sub 2}) nanoparticles have been synthesized by co-precipitation method. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD) and Ultraviolet-Visible spectroscopy (UV-VIS). XRD analysis confirmed the formation of single phase of SnO{sub 2} nanoparticles. It has been found that solvents played important role in controlling the crystallite size of SnO{sub 2} nanoparticles. The XRD analysis showed well crystallized tetragonal SnO{sub 2} nanoparticles. The crystallite size of SnO{sub 2} nanoparticles varies with the solvent. Tauc plot showed that optical band gap was also tailored by controlling the solvent during synthesis.

Synthesis, structure and magnetic properties ofβ-MnO2nanorods

PubMed Central

Kim, HaeJin; Lee, JinBae; Kim, Young-Min; Jung, Myung-Hwa; Jagličić, Z; Umek, P

2007-01-01

We present synthesis, structure and magnetic properties of structurally well-ordered single-crystalline β-MnO2nanorods of 50–100 nm diameter and several µm length. Thorough structural characterization shows that the basic β-MnO2material is covered by a thin surface layer (∼2.5 nm) of α-Mn2O3phase with a reduced Mn valence that adds its own magnetic signal to the total magnetization of the β-MnO2nanorods. The relatively complicated temperature-dependent magnetism of the nanorods can be explained in terms of a superposition of bulk magnetic properties of spatially segregated β-MnO2and α-Mn2O3constituent phases and the soft ferromagnetism of the thin interface layer between these two phases.

Visible-light-driven N-TiO2@SiO2@Fe3O4 magnetic nanophotocatalysts: Synthesis, characterization, and photocatalytic degradation of PPCPs.

PubMed

Kumar, Ashutosh; Khan, Musharib; Fang, Liping; Lo, Irene M C

2017-07-24

TiO 2 -based photocatalysis offers certain advantages like rapid degradation and mineralization of organic compounds. However, the practical applicability of photocatalysts in degradation of pharmaceuticals and personal care products (PPCPs) is still restricted by challenges including their limited photocatalytic activity under visible light and difficulty in their separation from suspension. To overcome these challenges, a visible-light-driven magnetic N-TiO 2 @SiO 2 @Fe 3 O 4 nanophotocatalyst was developed through fine-tuning the pertinent factors (calcination temperature, Fe 3 O 4 loading, and nitrogen doping) involved during synthesis process, on the basis of degradation of ibuprofen (a typical PPCP). The TEM-EDX, XRD and XPS analyses confirmed the successful synthesis of nanophotocatalyst. By comparing nanophotocatalyst's performance on ibuprofen under two visible light sources, i.e., compact fluorescent lamps (CFLs) and light emitting diodes (LEDs) of similar irradiance, CFLs of irradiance 320μWcm -2 and peak emissive wavelength 543nm served as a better source, resulting in 94% degradation. Furthermore, 93% of benzophenone-3 within 5h and 71% of carbamazepine within 9h was degraded under visible light emitted by CFLs. The superparamagnetic behavior of the nanophotocatalyst enabled its successful magnetic separation (95% efficiency) from the suspension within 20-25min under an electromagnetic field of ∼200mT. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis, Characterization, and Theoretical Considerations of 1,2-bis(oxyamino)ethane Salts

NASA Technical Reports Server (NTRS)

Crake, Greg; Hawkins, Tom; Hall, Leslie; Tollison, Kerri; Brand, Adam

2003-01-01

The synthesis, characterization, theoretical calculations, and safety studies of energetic salts of 1,2- bis(oxyamino) ethane, (H2N-O-CH2-CH2-O-NH2), were carried out. The salts were characterized by vibrational (infrared, Raman), multinuclear nmr studies (1H, 13C), differential scanning calorimetry (DSC); elemental analysis; and initial safety testing (impact and friction sensitivity) . Theoretical calculations on the neutral, monoprotonated, and doubly protonated species of ethylene bisoxyamine were carried out using xxxx level of theory for the lowest energy structure and these theoretical results compared with the experimentally observed bond distances and vibrational (ir, Raman) frequency values. The single crystal X-ray diffraction study was carried out on the mono-perchlorate salt revealing a high degree of hydrogen bonding with an unexpected structure.

Synthesis and structural characterization of ZnO and CuO nanoparticles supported mesoporous silica SBA-15

NASA Astrophysics Data System (ADS)

El-Nahhal, Issa M.; Salem, Jamil K.; Selmane, Mohamed; Kodeh, Fawzi S.; Ebtihan, Heba A.

2017-01-01

Zinc oxide (ZnO) and copper oxide (CuO) nanoparticles were loaded into mesoporous silica SBA-15 by post-synthesis and direct methods. The structural properties were characterized using wide and small angle X-ray diffraction (WXRD & SXRD), X-ray photoelectron spectroscopy (XPS) and N2-adsorption desorption (BET). The WXRD showed that, the loaded zinc and copper oxides were present in crystalline forms (impregnation). The mesoporosity properties of SBA-15 silica were well maintained even after the introduction of metal oxide nanoparticles. BET analysis indicate that the impregnated and condensed ZnO and CuO supported SBA-15 nanocomposites have a lower surface area than that of its parent SBA-15.

Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

NASA Technical Reports Server (NTRS)

Nanjundaswamy, K. S.; Standlee, D.; Kelly, C. O.; Whiteley, R. V., Jr.

1997-01-01

A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

Synthesis and characterization of sodium vanadium oxide gels: the effects of water (n) and sodium (x) content on the electrochemistry of Na(x)V2O5·nH2O.

PubMed

Lee, Chia-Ying; Marschilok, Amy C; Subramanian, Aditya; Takeuchi, Kenneth J; Takeuchi, Esther S

2011-10-28

Sodium vanadium oxide gels, Na(x)V(2)O(5)·nH(2)O, of varying sodium content (0.12 < x < 0.32) were prepared by careful control of an ion exchange process. The water content (0.23 > n > 0.01) and interlayer spacing were found to be inversely proportional to the sodium level (x), thus control of sodium (x) content provided a direct, chimie douce approach for control of hydration level (n) and interlayer spacing, without the need for high temperature treatment to affect dehydration. Notably, the use of high temperatures to modify hydration levels can result in crystallization and collapse of the interlayer structure, highlighting the distinct advantage of our novel chimie douce synthesis strategy. Subsequent to synthesis and characterization, results from an electrochemical study of a series of Na(x)V(2)O(5)·nH(2)O samples highlight the significant impact of interlayer water on delivered capacity of the layered materials. Specifically, the sodium vanadium oxide gels with higher sodium content and lower water content provided higher capacities in lithium based cells, where capacity delivered to 2.0 V under C/20 discharge ranged from 170 mAh/g for Na(0.12)V(2)O(5)·0.23H(2)O to 300 mAh/g for Na(0.32)V(2)O(5)·0.01H(2)O. The capacity differences were maintained as the cells were cycled. This journal is © the Owner Societies 2011

Facile synthesis of layered V2O5/ZnV2O6 heterostructures with enhanced sensing performance

NASA Astrophysics Data System (ADS)

Xiao, Bingxin; Huang, Hao; Yu, Xiantong; Song, Jun; Qu, Junle

2018-07-01

A low-cost and environment-friendly hydrothermal approach was used for the synthesis of layered V2O5/ZnV2O6 hybrid nanobelts. Characterization results indicate that the V2O5/ZnV2O6 nanobelts are composed of several thin layers. Additionally, it is illustrated that the chemical formation process of V2O5/ZnV2O6 occurred in the solution. The synthesized V2O5/ZnV2O6 heterostructures were subjected to detailed ethanol sensing tests. Results demonstrate that V2O5/ZnV2O6 based sensor shows about 4.3 of response to 100 ppm of ethanol gases, reveals relatively high sensitivity at relatively low optimal operating temperature of 240 °C, as well as relatively good selectivity and stability. The performance of the sensor is better than most of reported vanadium based sensing devices. Thus this work offers a new insight into the rational regulation of vanadium based sensing devices.

One-Pot Polyol Synthesis of Pt/CeO2 and Au/CeO2 Nanopowders as Catalysts for CO Oxidation.

PubMed

Pilger, Frank; Testino, Andrea; Lucchini, Mattia Alberto; Kambolis, Anastasios; Tarik, Mohammed; El Kazzi, Mario; Arroyo, Yadira; Rossell, Marta D; Ludwig, Christian

2015-05-01

The facile one-pot synthesis of CeO2-based catalysts has been developed to prepare a relatively large amount of nanopowders with relevant catalytic activity towards CO oxidation. The method consists of a two-steps process carried out in ethylene glycol: in the first step, 5 nm well-crystallized pure CeO2 is prepared. In a subsequent second step, a salt of a noble metal is added to the CeO2 suspension and the deposition of the noble metal on the nanocrystalline CeO2 is induced by heating. Two catalysts were prepared: Pt/CeO2 and Au/CeO2. The as-prepared catalysts, the thermally treated catalysts, as well as the pure CeO2, are characterized by XRD, TGA, XPS, FTIR, HR-TEM, STEM, particle size distribution, and N2-physisorption. In spite of the identical preparation protocol, Au and Pt behave in a completely different way: Au forms rather large particles, most of them with triangular shape, easily identifiable and dispersed in the CeO2 matrix. In contrast, Pt was not identified as isolated particles. The high resolution X-ray diffraction carried out on the Pt/CeO2 thermally treated sample (500 degrees C for 1 h) shows a significant CeO2 lattice shrinkage, which can be interpreted as an at least partial incorporation of Pt into the CeO2 crystal lattice. Moreover, only Pt2+ and Pt4+ species were identified by XPS. In literature, the incorporation of Pt into the CeO2 lattice is supported by first-principle calculations and experimentally demonstrated only by combustion synthesis methods. To the best of our knowledge this is the first report where ionically dispersed Pt into the CeO2 lattice is obtained via a liquid synthesis method. The thermally treated Pt/CeO2 sample revealed good activity with 50% CO conversion at almost room temperature.

Synthesis and characterization of luminescent materials for thermal sensing and proton dosimetry

NASA Astrophysics Data System (ADS)

Doull, Brandon Arthur

The work presented in this thesis is the materials synthesis, investigation of synthesis parameters, and basic luminescent characterizations of MgB 4O7, Li2B4O7, and MgO for the applications of thermal sensing using thermoluminescence (TL) and proton dosimetry using optically stimulated luminescence (OSL). The materials were synthesized using solution combustion synthesis and characterized by x-ray diffraction, radioluminescence, thermoluminescence, and optically stimulated luminescence. Based upon the basic characterizations MgB 4O7:Li,Dy and Li2B4O7:Cu,Ag were selected for their potential for use as TL materials for thermal sensing while MgB4O7:Li,Ce and MgO:Li were chosen for use as OSL materials in proton dosimetry. Furthermore, MgB4O7:Li,Ce and MgO:Li were fabricated into detector assemblies and exposed to a clinical proton beam for analysis.

Synthesis and characterization of ZnS@Fe3O4 fluorescent-magnetic bifunctional nanospheres

NASA Astrophysics Data System (ADS)

Koc, Kenan; Karakus, Baris; Rajar, Kausar; Alveroglu, Esra

2017-10-01

Herein, we synthesized and characterized fluorescent and super paramagnetic ZnS@Fe3O4 nanospheres. First, (3-mercaptopropyl) trimethoxysilane (MPS) capped ZnS quantum dots (QDs) and SiO2 coated Fe3O4 nanoparticles were synthesized separately by using solution growth and co-precipitation techniques. After synthesis and characterization of these two nanoparticles, they were conglutinated together in a nano sized sphere. The QDs were attached to the surface of the Fe3O4 nanoparticles by Sisbnd Osbnd Si bonds and so Sisbnd Osbnd Si bonds created a SiO2 network around the nanoparticles during the formation of the ZnS@Fe3O4 nanospheres. The synthesized MPS capped ZnS fluorescent QDs, SiO2 coated magnetite super paramagnetic nanoparticles and ZnS@Fe3O4 fluorescent-magnetic bifunctional nanospheres were characterized by using UV-Vis Absorption Spectroscopy, Fluorescence Spectroscopy, X-ray analysis, Vibrating Sample Magnetometer analysis, Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy, Scanning Electron Microscope and Energy-dispersive X-ray spectroscopy. ZnS@Fe3O4 bifunctional nanospheres were shown to retain the magnetic properties of magnetite, while exhibiting the luminescent optical properties of ZnS nanoparticles. The combination of fluorescent and magnetic behaviors of nano composites make them useful for potential applications in the field of bio-medical and environmental.

Synthesis and characterization of anionic/nonionic surfactant-interceded iron-doped TiO{sub 2} to enhance sorbent/photo-catalytic properties

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sharma, Ajit; Lee, Byeong-Kyu, E-mail: bklee@ulsan.ac.kr

2015-09-15

We investigated the synthesis, characterization, and application of surfactant-interceded Fe nanoparticle-doped TiO{sub 2} (TiO{sub 2}/Fe-S1 and TiO{sub 2}/Fe-S2) that were used as adsorbents and photo-catalysts for the removal of As(V) ions from aqueous media. Two types of surfactant (anionic (sodium dodecyl sulfate), S1 and non-ionic (Triton X-100), S2) were used to obtain the separation and mono-dispersion of Fe(III) ions in the reaction solution. The nanocomposites were characterized by Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), UV–vis, scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX) and elemental mapping analysis before and after As(V) removal. The Langmuir capacities (q{submore » e}, mg/g) of the sodium dodecyl sulfate (SDS) and Triton X-100 interceded nanocomposites (TiO{sub 2}/Fe-S1 and TiO{sub 2}/Fe-S2, respectively) for arsenic removal were determined to be 65.79 and 50.76 mg/g, respectively, in aqueous media with As(V) concentration ranges of 0–10 mg/L at pH 6.5. - Highlights: • Fe(III) doped TiO{sub 2} nanocomposite was prepared with surfactant. • Anionic surfactant SDS enhanced the transfer of Fe(III) ions to TiO{sub 2}. • Surfactant-interceded nanocomposite enhanced As(V) removal. • Arsenic removal efficiency was as follows: dark phase>visible phase>UV region.« less

Hydrothermal synthesis, characterization, and thermal properties of alumino silicate azide sodalite, Na8[AlSiO4]6(N3)2

NASA Astrophysics Data System (ADS)

Borhade, A. V.; Wakchaure, S. G.; Dholi, A. G.; Kshirsagar, T. A.

2017-07-01

First time we report the synthesis, structural characterization and thermal behavior of an unusual N3 - containing alumino-silicate sodalite mineral. Azide sodalite, Na8[AlSiO4]6(N3)2 has been synthesized under hydrothermal conditions at 433 K in steel lined Teflon autoclave. The structural and microstructural properties of azide sodalite mineral was characterized by various methods including FT-IR, XRD, SEM, TGA, and MAS NMR. Crystal structure have been refined by Rietveld method in P\\bar 43n space group, indicating that the N3 - sodalite has cubic in lattice. High temperature study was carried out to see the effect of thermal expansion on cell dimension ( a o) of azide sodalite. Thermal behavior of sodalite was also assessed by thermogravimetric method.

Synthesis and characterization of Cu2O/TiO2 photocatalysts for H2 evolution from aqueous solution with different scavengers

NASA Astrophysics Data System (ADS)

Li, Yanping; Wang, Baowei; Liu, Sihan; Duan, Xiaofei; Hu, Zongyuan

2015-01-01

A series of Cu2O/TiO2 photocatalysts with different molar fraction of Cu2O were prepared by a facile modified ethanol-induced approach followed by a calcination process. The chemical state of copper compound was proved to be cuprous oxide by the characterization of X-ray photoelectron spectra (XPS). Furthermore, these composite oxides were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), N2 adsorption desorption and UV-vis techniques to study the morphologies, structures, and optical properties of the as-prepared samples. The results indicated that the photocatalytic activity of n-type TiO2 was significantly enhanced by combined with p-type Cu2O, due to the efficient p-n heterojunction. The p-n heterojunction between Cu2O and TiO2 can enhance visible-light adsorption, efficiently suppress charge recombination, improve interfacial charge transfer, and especially provide plentiful reaction active sites on the surface of photocatalyst. As a consequence, the prepared 2.5-Cu2O/TiO2 photocatalyst exhibited the highest photocatalytic activity for H2 evolution rate and reached 2048.25 μmol/(g h), which is 14.48 times larger than that of pure P25. The apparent quantum yield (AQY) of the 2.5-Cu2O/TiO2 sample at 365 nm was estimated to be 4.32%. In addition, the influence of different scavengers, namely methanol, anhydrous ethanol, ethylene glycol and glycerol, on the photocatalytic activity for H2 evolution rate was discussed.

Microfluidic reactor synthesis and photocatalytic behavior of Cu@Cu2O nanocomposite

NASA Astrophysics Data System (ADS)

Xu, Lei; Srinivasakannan, C.; Peng, Jinhui; Yan, Mi; Zhang, Di; Zhang, Libo

2015-03-01

The Cu@Cu2O nanocomposites were synthesized by solution-phase synthesis of Cu nanoparticles in microfluidic reactor at room temperature, followed by controlling the oxidation process. The size, morphology, elemental compositions, and the chemical composition on the surface of Cu@Cu2O nanocomposite were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). Experimental results demonstrated that the surface of the Cu nanoparticles was oxidized to Cu2O which serves as the shell of nanoparticle. The amount of Cu2O can be controlled by varying the drying temperature. Additionally the binary Cu@Cu2O nanocomposite along with H2O2 exhibited its potential as an excellent photocatalyst for degradation of methylene blue (MB) under UV irradiation.

Designed synthesis of multi-functional PEGylated Yb2O3:Gd@SiO2@CeO2 islands core@shell nanostructure.

PubMed

Li, Junqi; Yao, Shuang; Song, Shuyan; Wang, Xiao; Wang, Yinghui; Ding, Xing; Wang, Fan; Zhang, Hongjie

2016-07-28

Nanomaterials that can restrain or reduce the production of excessive reactive oxygen species such as H2O2 to defend and treat against Alzheimer's disease (AD) have attracted much attention. In this paper, we adopt the strategy of layer-by-layer deposition; namely, first synthesizing available gadolinium-doped ytterbia nanoparticles (Yb2O3:Gd NPs) as cores, and then coating them with silica via the classical Stöber method to prevent leakage and act as a carrier for subsequent ceria deposition and PEGylation, and finally obtain the expected core@shell-structured nanocomposite of PEGylated Yb2O3:Gd@SiO2@CeO2 islands. The nanomaterial has proved not only to be a high-performance dual-modal contrast agent for use in MRI and CT, but also to exhibit excellent catalase mimetic activity, which may help the prognosis, diagnosis and treatment of AD in the future. In addition, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared (FTIR) spectroscopy characterization have revealed the successful design and synthesis of the cores with remarkable size uniformity, with well-distributed CeO2 islands decorated on the surface of SiO2 shells, and tightly immobilized PEG.

Synthesis and characterization of novel Cu(II) complex coated Fe3O4@SiO2 nanoparticles for catalytic performance

NASA Astrophysics Data System (ADS)

Nasrollahzadeh, Mahmoud; Sajjadi, Mohaddeseh; Khonakdar, Hossein Ali

2018-06-01

In this study, a convenient method for the synthesis of arylaminotetrazoles has been developed using a copper (II)-aminotetrazole complex immobilized on silica-coated Fe3O4 (Fe3O4@SiO2) nanoparticles (Fe3O4@SiO2-aminotet-Cu(II)) as a novel and efficient magnetically catalyst. The constructed superparamagnetic core-shell nanoparticles were successfully prepared, as proven using different spectroscopic techniques such as fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), transmission electron microscope (TEM), field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDS), thermogravimetry and differential thermogravimetry (TG-DTG) and vibrating sample magnetometer (VSM) analysis. The applicability of Fe3O4@SiO2-aminotet-Cu(II) magnetic catalyst allows the efficient synthesis of a variety of arylaminotetrazoles from the reaction between various arylcyanamides with sodium azide in high yields. The effect of catalyst loading was investigated. In addition, the reaction mechanism for the synthesis of arylaminotetrazoles was reasonably proposed. Results show that the 1-aryl-5-amino-1H-tetrazole (B isomer) and 5-arylamino-1H-tetrazole (A isomer) can be obtained from the arylcyanamides carrying electron-donating and electron-withdrawing substituents, respectively. This procedure offers a simple methodology, relatively short reaction times, easy work-up, high yields of the products and a cleaner reaction with elimination of hydrazoic acid (HN3). Moreover, catalyst can be conveniently recovered through the use of external magnet and reused for at least 6 times without any significant loss of its activity.

Magnetic zeolite NaA: synthesis, characterization based on metakaolin and its application for the removal of Cu2+, Pb2+.

PubMed

Liu, Haibo; Peng, Shuchuan; Shu, Lin; Chen, Tianhu; Bao, Teng; Frost, Ray L

2013-06-01

The optimum parameters for synthesis of zeolite NaA based on metakaolin were investigated according to results of cation exchange capacity and static water adsorption of all synthesis products and selected X-ray diffraction (XRD). Magnetic zeolite NaA was synthesized by adding Fe3O4 in the precursor of zeolite. Zeolite NaA and magnetic zeolite NaA were characterized with scanning electron microscopy (SEM) and XRD. Magnetic zeolite NaA with different Fe3O4 loadings was prepared and used for removal of heavy metals (Cu(2+), Pb(2+)). The results show the optimum parameters for synthesis zeolite NaA are SiO2/Al2O3=2.3, Na2O/SiO2=1.4, H2O/Na2O=50, crystallization time 8h, crystallization temperature 95 °C. The addition of Fe3O4 makes the NaA zeolite with good magnetic susceptibility and good magnetic stability regardless of the Fe3O4 loading, confirming the considerable separation efficiency. Additionally, Fe3O4 loading had a little effect on removal of heavy metal by magnetic zeolite, however, the adsorption capacity still reaches 2.3 mmol g(-1) for Cu(2+), Pb(2+) with a removal efficiency of over 95% in spite of 4.7% Fe3O4 loading. This indicates magnetic zeolite can be used to remove metal heavy at least Cu(2+), Pb(2+) from water with metallic contaminants and can be separated easily after a magnetic process. Copyright © 2013 Elsevier Ltd. All rights reserved.

Low temperature synthesis and characterization of Na–M–(O)–F phases with M=Ti, V

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nava-Avendaño, Jessica; Ayllón, José A.; Frontera, Carlos

2015-03-15

Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} was prepared by the microwave assisted method, and presents a chiolite related structure with cell parameters a=10.5016(5), b=10.4025(5), and c=10.2911(5) Å and Cmca (no. 64) space group. From solvothermal synthesis at 100 °C the cryolite Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} was prepared, which crystallizes in the monoclinic system with a=5.5403(2), b=5.6804(2), c=7.9523(2) Å, β=90.032(7)° cell parameters and P2{sub 1}/n (no. 14) space group. Under similar synthesis conditions but with higher HF concentration the chiolite-type phase Na{sub 5−δ}V{sub 3}F{sub 14} was achieved, which exhibits a=10.5482(2), b=10.4887(1) and c=10.3243(1) Å cell parameters and Cmc2{sub 1} (no. 36) spacemore » group. A single crystal also having the chiolite structure was synthesized at 200 °C which exhibits tetragonal symmetry (a=7.380(3) and c=10.381(11) Å and space group P4{sub 2}2{sub 1}2 (no. 94)). Bond valence sum indicates that it contains V{sup 4+} and therefore can be formulated as Na{sub 5}V{sub 3}O{sub 3}F{sub 11}. - Graphical abstract: Na{sub 5}M{sub 3}(O,F){sub 14} with M=Ti and V having chiolite structure and Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} cryolite were prepared by means of microwave-assisted and solvothermal synthesis. - Highlights: • Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} chiolite was prepared by a microwave assisted method and characterized. • Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} and Na{sub 5−δ}V{sub 3}F{sub 14} were prepared by solvothermal synthesis. • The compounds were structurally characterized by diffraction techniques. • O/F distribution was estimated by applying Pauling’s second rule.« less

Precipitation method for barium metaborate (BaB2O4) synthesis from borax solution

NASA Astrophysics Data System (ADS)

Akşener, Eymen; Figen, Aysel Kantürk; Pişkin, Sabriye

2013-12-01

In this study, barium metaborate (BaB2O4, BMB) synthesis from the borax solution was carried out. BMB currently is used in production of ceramic glazes, luminophors, oxide cathodes as well as additives to pigments for aqueous emulsion paints and also β-BaB2O4 single crystals are the best candidate for fabrication of solid-state UV lasers operating at a wavelength of 200 nm due to excellent nonlinear optical properties. In the present study, synthesis was carried out from the borax solution (Na2B4O7ṡ10H2O, BDH) and barium chloride (BaCI2ṡ2H2O, Ba) in the glass-batch reactor with stirring. The effect of, times (5-15 min), molar ratio [stoich.ration (1.0:2.0), 1.25:2.0, 1.5:2.0, 2.5:2:0, 3.0:2.0, 3.5:2.0,4.0:2.0, 5.0:2.0] and also crystallization time (2-6 hour) on the BMB yield (%) was investigated at 80 °C reaction temperature. It is found that, BMB precipitation synthesis with 90 % yield can be performed from 0.50 molar ration (BDH:Ba), under 80 °C, 15 minute, and 6 hours crystallization time. The structural properties of BMB powders were characterized by using XRD, FT-IR and DTA-TG instrumental analysis technique.

An alternative gas sensor material: Synthesis and electrical characterization of SmCoO{sub 3}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Michel, Carlos Rafael; Delgado, Emilio; Santillan, Gloria

2007-01-18

Single-phase perovskite SmCoO{sub 3} was prepared by a wet-chemical synthesis technique using metal-nitrates and citric acid; after its characterization by thermal analyses and X-ray diffraction, sintering at 900 deg. C in air, gave single phase and well crystallized powders. The powders were mixed with an organic solvent to prepare a slurry, which was deposited on alumina substrates as thick films, using the screen-printing technique. Electrical and gas sensing properties of sintered SmCoO{sub 3} films were investigated in air, O{sub 2} and CO{sub 2}, the results show that sensitivity reached a maximum value at 420 deg. C, for both gases. Dynamicmore » tests revealed a better behavior of SmCoO{sub 3} in CO{sub 2} than O{sub 2}, due to a fast response and a larger electrical resistance change to this gas. X-ray diffraction made on powders after electrical characterization in gases, showed that perovskite-type structure was preserved.« less

Towards the development of a novel bioinspired functional material: synthesis and characterization of hybrid TiO2/DHICA-melanin nanoparticles.

PubMed

Pezzella, Alessandro; Capelli, Luigia; Costantini, Aniello; Luciani, Giuseppina; Tescione, Fabiana; Silvestri, Brigida; Vitiello, Giuseppe; Branda, Francesco

2013-01-01

A large number of recent literature data focus on modification/modulation of surface chemistry of inorganic materials in order to improve their functional properties. Melanins, a wide class of natural pigments, are recently emerging as a powerful organic component for developing bioinspired active material for a large number of applications from organoelectronics to bioactive compounds. Here we report the use of the approach referred as "chimie douce", involving in situ formation of the hybrids through reactions of precursors under mild conditions, to prepare novel hybrid functional architectures based on eumelanin like 5,6 dihydroxyindole-2-carboxylic acid (DHICA) polymer and TiO2. Two synthesis procedures were carried out to get DHICA-melanin coated TiO2 nanoparticles as well as mixed DHICA/TiO2 hybrid nanostructures. Such systems were characterized through EPR, FT-IR and fluorescence spectroscopy, thermogravimetric analysis (TGA), X-ray diffraction (XRD), and TEM microscopy in order to assess the effect of synthesis path as well as of DHICA content on structural, morphological and optical properties of TiO2 nanostructures. In particular, EPR, FT-IR spectra and TGA analysis confirmed the presence of DHICA-melanin in these samples. TEM measurements indicated the formation of the nanoparticles having relatively narrow size distribution with average particle size of about 10nm. DHICA-melanin does act as a morphological agent affecting morphology of hybrid nanostructures. XRD analysis proved that TiO2 hybrid nanoparticles kept anatase structures for DHICA-melanin contents within the range of investigated compositions, i.e. up to 50% wt/wt. Copyright © 2012 Elsevier B.V. All rights reserved.

CdS-sensitized TiO2 nanocorals: hydrothermal synthesis, characterization, application.

PubMed

Mali, S S; Desai, S K; Dalavi, D S; Betty, C A; Bhosale, P N; Patil, P S

2011-10-01

Cadmium sulfide (CdS) nanoparticle-sensitized titanium oxide nanocorals (TNC) were synthesized using a two-step deposition process. The TiO(2) nanocorals were grown on the conducting glass substrates (FTO) using A hydrothermal process and CdS nanoparticles were loaded on TNC using successive ionic layer adsorption and reaction (SILAR) method. The TiO(2), CdS and TiO(2)-CdS samples were characterized by optical absorption, X-ray diffraction (XRD), FT-Raman, FT-IR, scanning electron microscopy (SEM) and contact angle. Further, their photoelectrochemical (PEC) performance was tested in NaOH, Na(2)S-NaOH-S and Na(2)S electrolytes, respectively. When CdS nanoparticles are coated on TNCs, the optical absorption is found to be enhanced and band edge is red-shifted towards visible region. The TiO(2)-CdS sample exhibits improved photoelectrochemical (PEC) performance with maximum short circuit current of (J(sc)) 1.04 mA cm(-2). After applying these TiO(2)-CdS electrodes in photovoltaic cells, the photocurrent was found to be enhanced by 2.7 and 32.5 times, as compared with those of bare CdS and TiO(2) nanocorals films electrodes respectively. Also, the power conversion efficiency of TiO(2)-CdS electrodes is 0.72%, which is enhanced by about 16 and 29 times for TiO(2), CdS samples. This journal is © The Royal Society of Chemistry and Owner Societies 2011

Synthesis of TiO2 nanoparticles by hydrolysis and peptization of titanium isopropoxide solution

NASA Astrophysics Data System (ADS)

Mahata, S.; Mahato, S. S.; Nandi, M. M.; Mondal, B.

2012-07-01

Here we report the synthesis and characterization of a stable suspension of modified titania nanoparticles. Phase-pure TiO2 nanocrystallites with narrow particle-size distributions were selectively prepared by hydrolysis-peptization of modified alkoxide followed by hydrothermal treatment. Autoclaving modified TiO2 in the presence of HNO3 as cooperative catalysts led to the formation of crystalline TiO2 with narrow-sized distribution. Following the hydrothermal treatment at 150°C, X-ray diffraction shows the particles to be exclusively anatase. Synthesized powder is characterized by FT-IR, scanning electron microscopy (FESEM) and transmission electron microscopy (HRTEM). The photocatalytic activity in the degradation of orange-II is quite comparable to good anatase and rutile nanocrystallites.

Green synthesis, characterization and catalytic activity of the Pd/TiO2 nanoparticles for the ligand-free Suzuki-Miyaura coupling reaction.

PubMed

Nasrollahzadeh, Mahmoud; Sajadi, S Mohammad

2016-03-01

A green synthesis process was developed for production of the Pd/TiO2 nanoparticles (NPs) without using toxic, hazardous and dangerous materials. Myrtus communis L. leaf extract serves as a mild, renewable and non-toxic reducing agent. The advantages of this biosynthesis method include use of cheap, clean, nontoxic and environmentally benign precursors and simple procedures without time-consuming polymerization and problems with treatment of a highly viscous polymeric resin. More importantly, the synthesized Pd/TiO2 NPs presented excellent catalytic activity for ligand-free Suzuki-Miyaura coupling which could be easily separated from the reaction mixture and reused many times with no loss of activity. Therefore, these properties indicate demonstrative benefits of the catalyst. The Pd/TiO2 NPs was characterized by FESEM, TEM, FT-IR, UV-vis spectroscopy and EDS. Copyright © 2015 Elsevier Inc. All rights reserved.

Activation of Nrf2 by H2O2: de novo synthesis versus nuclear translocation.

PubMed

Covas, Gonçalo; Marinho, H Susana; Cyrne, Luísa; Antunes, Fernando

2013-01-01

The most common mechanism described for the activation of the transcription factor Nrf2 is based on the inhibition of its degradation in the cytosol followed by its translocation to the nucleus. Recently, Nrf2 de novo synthesis was proposed as an additional mechanism for the rapid upregulation of Nrf2 by hydrogen peroxide (H2O2). Here, we describe a detailed protocol, including solutions, pilot experiments, and experimental setups, which allows exploring the role of H2O2, delivered either as a bolus or as a steady state, in endogenous Nrf2 translocation and synthesis. We also show experimental data, illustrating that H2O2 effects on Nrf2 activation in HeLa cells are strongly dependent both on the H2O2 concentration and on the method of H2O2 delivery. The de novo synthesis of Nrf2 is triggered within 5min of exposure to low concentrations of H2O2, preceding Nrf2 translocation to the nucleus which is slower. Evidence of de novo synthesis of Nrf2 is observed only for low H2O2 steady-state concentrations, a condition that is prevalent in vivo. This study illustrates the applicability of the steady-state delivery of H2O2 to uncover subtle regulatory effects elicited by H2O2 in narrow concentration and time ranges. Copyright © 2013 Elsevier Inc. All rights reserved.

Synthesis and characterization of polycrystalline brownmillerite cobalt doped Ca2Fe2O5

NASA Astrophysics Data System (ADS)

Dhankhar, Suchita; Bhalerao, Gopal; Baskar, K.; Singh, Shubra

2016-05-01

Brownmillerite compounds with general formula A2BB'O5 (BB' = Mn, Al, Fe, Co) have attracted attention in wide range of applications such as in solid oxide fuel cell, oxygen separation membrane and photocatalysis. Brownmillerite compounds have unique structure with alternate layers of BO6 octahedral layers and BO4 tetrahedral layers. Presence of dopants like Co in place of Fe increases oxygen vacancies. In the present work we have synthesized polycrystalline Ca2Fe2O5 and Ca2Fe1-xCoxO5 (x = 0.01, 0.03) by citrate combustion route. The as prepared samples were characterized by XRD using PANalytical X'Pert System, DRS (Diffuse reflectance spectroscopy) and SEM (Scanning electron microscopy).

Synthesis of LiNiO2 cathode materials with homogeneous Al doping at the atomic level

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Zengcai; Zhen, Honghe; Kim, Yoongu

2011-01-01

Aluminum doped LiNiO2 cathode materials are synthesized by using Raney nickel as the starting material. The structure and composition are characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) coupled with elemental mapping. The lithium deficiency is analyzed by Rieveld refinement. The initial capacity and retention of capacity are correlated to the lithium deficiency of the resulting cathode material. Using strong oxidant of Li2O2 in the synthesis results in materials with improved electrochemical cyclability. The improvement is related to the diminishing of lithium deficiency in strong oxidizing synthesis conditions.

Novel synthesis approach for stable sodium superoxide (NaO2) nanoparticles for LPG sensing application

NASA Astrophysics Data System (ADS)

Nemade, Kailash; Waghuley, Sandeep

2017-05-01

The synthesis of stable superoxide is still great challenge for the researchers working in the field of materials science. Through this letter, we report the novel and simple synthesis approach for the preparation of stable sodium superoxide (NaO2) nanoparticles. NaO2 nanoparticles were prepared by a spray pyrolysis technique, under oxygen rich environment for gas sensing application. The texture characterizations show that as-obtained NaO2 nanoparticles have high structural purity. Most importantly, NaO2 nanoparticles exhibits higher sensing response, shorter response time and recovery time, low operating temperature and good stability during sensing of liquefied petroleum gas (LPG). The main accomplishment of present work is that as-fabricated sensor has low operating temperature (423 K), which is below auto-ignition temperature of LPG. The gas sensing mechanism of NaO2 nanoparticles was discussed without the conventional oxygen bridging mechanism. Through this short communication, LPG sensing application of stable sodium superoxide nanoparticle is explored.

Synthesis, structural and magnetic characterization of polycrystalline Yb{sub 2}Ti{sub 2}O{sub 7}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Juyal, Abhishek, E-mail: abijuyal@iitk.ac.in; Mukhopadhyay, Soumik; Barman, Kalyani

2015-06-24

The discovery of the Yb{sub 2}Ti{sub 2}O{sub 7} is among the most significant findings in magnetic materials in over a decade. The spin-ice model is based on an ingenious analogy to Pauling’s model of geometrical frustration in water ice, which is confirmed by various experiments. Here we present the characteristics of Yb2Ti2O7 studied by X-ray diffraction and magnetic measurements. Polycrystalline sample of Yb{sub 2}Ti{sub 2}O{sub 7} was prepared by sol-gel synthesis followed by thermal annealing at 1400 ° C for 36 hours. We calculated the change in the magnetic entropy from isothermal magnetization curves. We find no evidence of plateaumore » at Pauling residual entropy. Temperature dependence of the inverse magnetic susceptibility reveals Curie-Wiess temperature Θ{sub cw} = 156mK and paramagnetic moment μ{sub eff} ≈ 3.58 µ{sub B}, indicating weak ferromagnetic interaction. Using Arrott plot we conclude that Yb{sub 2}Ti{sub 2}O{sub 7} possibly enters a magnetic ground state below Tc~140 mK.« less

Synthesis and characterization of NaCo(1-x)MnxO2 solid electrolyte using sol-gel method: the effect of milling speed variations

NASA Astrophysics Data System (ADS)

Suyati, L.; Widyayanti, O. A.; Qushoyyi, M.; Darmawan, A.; Nuryanto, R.

2018-04-01

Battery is a device that converts chemical energy into electrical energy through electrochemical process. Further research on the synthesis of cathode of Na-ion battery that has good conductivity to maximize the battery performance needs to be conducted. One of the production steps of the NaCo(1-x)NaCo cathode synthesis in the Na-Ion battery was a ball-milling process, in which by the ball-milling process, the crystal size of NaCo(1-x)MnxO2 cathode can be minimized. The purpose of this study was to determine the effect of variation of ball-milling speed to the characteristics of resulting product including the oxide types composing NaCo(1-x)MnxO2 cathode, surface morphology, and conductivity. The main ingredients used were sodium acetate, manganese acetate, cobalt acetate with molar ratio of 0.7: 0.66: 0.22, respectively and citric acid as chelating agent with the M/CA ratio of 1: 1. The variations of milling speed were 0, 300, 400, 500, 600 and 700 rpm. Characterization of the product was conducted using XRD, SEM-EDS, and conductivity meter (LCR-meter). The result showed that a solid electrolyte of NaCo(1-x)MnxO2 consisting of NaMnO2, NaO2, CoO, Co2O3, MnO2 components was successfully synthesized. The observation on the milling speed at 400 rpm showed that the solid electrolyte produced had the highest conductivity i.e. 4.08 x 10-6 Scm-1 with a homogeneous surface morphology and had a spinel formula NaCo0,65Mn0,35O2.

Auto-combustion synthesis and characterization of Mg doped CuAlO2 nanoparticles

NASA Astrophysics Data System (ADS)

Agrawal, Shraddha; Parveen, Azra; Naqvi, A. H.

2015-06-01

The synthesis of pure and Mg doped Copper aluminumoxide CuAlO2nanoparticles, a promising p-type TCO (transparent conducting oxide) have been done bysol gel auto combustion method using NaOH as a fuel, calcinated at 600°C. The structural properties were examined by XRD and SEM techniques. The optical absorption spectra of CuAlO2 sample recorded by UV-VIS spectrophotometer in the range of 200 to 800 nm have been presented. The crystallite size was determined by powder X-ray diffraction technique. The electrical behavior of pure and Mg doped CuAlO2 has been studied over a wide range of frequencies by using complex impedance spectroscopy.The variation of a.c. conductivity has been studied as function of frequency and temperature. The data taken together conclude that doping causes decreases in the ac conductivity of the nanoparticles as compared with the pure nanoparticles. Mg doping affects the optical properties and band gap.

Incorporation of TiO2 nanotubes in a polycrystalline zirconia: Synthesis of nanotubes, surface characterization, and bond strength.

PubMed

Dos Santos, Angélica Feltrin; Sandes de Lucena, Fernanda; Sanches Borges, Ana Flávia; Lisboa-Filho, Paulo Noronha; Furuse, Adilson Yoshio

2018-04-05

Despite numerous advantages such as high strength, the bond of yttria-stabilized zirconia polycrystal (Y-TZP) to tooth structure requires improvement. The purpose of this in vitro study was to evaluate the incorporation of TiO 2 nanotubes into zirconia surfaces and the bond strength of resin cement to the modified ceramic. TiO 2 nanotubes were produced by alkaline synthesis, mixed with isopropyl alcohol (50 wt%) and applied on presintered zirconia disks. The ceramics were sintered, and the surfaces were characterized by confocal laser microscopy, scanning electron microscopy (SEM), and energy-dispersive x-ray spectroscopy (EDS) analysis. For bond strength, the following 6 groups (n=16) were evaluated: without TiO 2 and Single Bond Universal; with TiO 2 nanotubes and Single Bond Universal; without TiO 2 nanotubes and Z-prime; with TiO 2 nanotubes and Z-prime; without TiO 2 and Signum Zirconia Bond; with TiO 2 and Signum Zirconia Bond. After sintering, resin cement cylinders, diameter of 1.40 mm and 1 mm in height, were prepared and polymerized for 20 seconds. Specimens were stored in water at 37°C for 30 days and submitted to a shear test. Data were analyzed by 2-way ANOVA and Tukey honest significant difference (α=.05) tests. EDS analysis confirmed that nanoagglomerates were composed of TiO 2 . The shear bond strength showed statistically significant differences among bonding agents (P<.001). No significant differences were found with the application of nanotubes, regardless of the group analyzed (P=.682). The interaction among the bonding agent factors and addition of nanotubes was significant (P=.025). Nanotubes can be incorporated into zirconia surfaces. However, this incorporation did not improve bond strength. Copyright © 2017 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

The result of synthesis analysis of the powder TiO{sub 2}/ZnO as a layer of electrodes for dye sensitized solar cell applications

DOE Office of Scientific and Technical Information (OSTI.GOV)

Retnaningsih, Lilis, E-mail: lilisretna@gmail.com; Muliani, Lia

2016-04-19

This study has been conducted synthesis of TiO{sub 2} nanoparticle powders and ZnO nanoparticle powder into a paste to be in this research, dye-sensitive solar cells (DSSC) was produced by TiO{sub 2} nanopowder and ZnO nanopowder synthesis to make paste that is applied as electrode. This electrode works based on photon absorbed by dye and transferred to different composition of TiO{sub 2}/ ZnO particle. Properties of DSSC are affected by fabrication method, parameter and dimension of TiO{sub 2} / ZnO nanoparticles, technique and composition of TiO{sub 2} / ZnO paste preparation is important to get the higher performance of DSSC.more » Doctor blade is a method for electrode coating on glass substrate. The electrode was immersed into dye solution of Z907 and ethanol. From the experiment, the effect of TiO{sub 2} and ZnO nanopowder mixture for electrode was investigated. XRD characterization show anatase and rutile phase, which sintered TiO{sub 2}/ZnO has intensity more than 11,000. SEM characterization shows the composition of 20% TiO{sub 2} / 80% ZnO has better porosity. Higher efficiency that is investigated by I-V measurement using Sun Simulator.« less

Chemicals from ethanol: the acetone synthesis from ethanol employing Ce0.75Zr0.25O2, ZrO2 and Cu/ZnO/Al2O3.

PubMed

Rodrigues, Clarissa Perdomo; Zonetti, Priscila da Costa; Appel, Lucia Gorenstin

2017-04-04

Acetone is an important solvent and widely used in the synthesis of drugs and polymers. Currently, acetone is mainly generated by the Cumene Process, which employs benzene and propylene as fossil raw materials. Phenol is a co-product of this synthesis. However, this ketone can be generated from ethanol (a renewable feedstock) in one-step. The aim of this work is to describe the influence of physical-chemical properties of three different catalysts on each step of this reaction. Furthermore, contribute to improve the description of the mechanism of this synthesis. The acetone synthesis from ethanol was studied employing Cu/ZnO/Al 2 O 3 , Ce 0.75 Zr 0.25 O 2 and ZrO 2 . It was verified that the acidity of the catalysts needs fine-tuning in order to promote the oxygenate species adsorption and avoid the dehydration of ethanol. The higher the reducibility and the H 2 O dissociation activity of the catalysts are, the higher the selectivity to acetone is. In relation to the oxides, these properties are associated with the presence of O vacancies. The H 2 generation, which occurs during the TPSR, indicates the redox character of this synthesis. The main steps of the acetone synthesis from ethanol are the generation of acetaldehyde, the oxidation of this aldehyde to acetate species (which reduces the catalyst), the H 2 O dissociation, the oxidation of the catalyst producing H 2 , and, finally, the ketonization reaction. These pieces of information will support the development of active catalysts for not only the acetone synthesis from ethanol, but also the isobutene and propylene syntheses in which this ketone is an intermediate. Graphical abstract Acetone from ethanol.

Synthesis and Characterization of TiO2/SiO2 Thin Film via Sol-Gel Method

NASA Astrophysics Data System (ADS)

Halin, D. S. C.; Abdullah, M. M. A. B.; Mahmed, N.; Malek, S. N. A. Abdul; Vizureanu, P.; Azhari, A. W.

2017-06-01

TiO2/SiO2 thin films were prepared by sol-gel spin coating method. Structural, surface morphology and optical properties were investigated for different annealing temperatures at 300°C, 400°C and 500°C. X-ray diffraction pattern show that brookite TiO2 crystalline phase with SiO2 phase presence at 300°C. At higher temperatures of 400-500°C, the only phase presence was brookite. The surface morphology of film was characterized by scanning electron microscopy (SEM). The films annealed at 300°C shows an agglomeration of small flaky with crack free. When the temperature of annealing increase to 400-500°C, the films with large flaky and large cracks film were formed which was due to surface tension between the film and the air during the drying process. The UV-Vis spectroscopy shows that the film exhibits a low transmittance around 30% which was due to the substrate is inhomogeneously covered by the films. In order to improve the coverage of the film on the substrate, it has to repeatable the spin coating to ensure the substrate is fully covered by the films.

Synthesis and characterization of molybdenum catalysts supported on {gamma}-Al{sub 2}O{sub 3}-CeO{sub 2} composite oxides

DOE Office of Scientific and Technical Information (OSTI.GOV)

Farooq, Muhammad; Ramli, Anita; Subbarao, Duvvuri

2012-09-26

The physical and chemical properties of a catalyst play a vital role in various industrial applications. Molybdenum catalysts supported on {gamma}-Al{sub 2}O{sub 3} and {gamma}-Al{sub 2}O{sub 3}-CeO{sub 2} mixed oxides with varying loading of CeO{sub 2} (5, 10, 15, 20 wt% with respect to {gamma}-Al{sub 2}O{sub 3}) were prepared by wet impregnation method. The physiochemical properties of these synthesized Mo catalysts were studied with various characterization techniques such as X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), temperature-programmed reduction (TPR), field emission scanning electron microscopy-energy dispersive analysis (FESEM-EDX) and X-ray fluorescence spectrometer (XRF). The results showed that the addition of CeO{submore » 2} into the support affected the binding energies of the elements and reducibility of the metal oxides formed after calcination of catalyst samples due to the change in metal-support interaction. Further, the characterization techniques showed that the active metal was well dispersed on the surface of support material.« less

Synthesis, characterization and wound healing imitation of Fe3O4 magnetic nanoparticle grafted by natural products

NASA Astrophysics Data System (ADS)

Pala, Sravan Kumar

This research focused on the study of the core-shelled magnetic nanomaterials derived from a colloidal chemistry. The goals are four-fold: (1) synthesis of Fe3O4MNMs using colloidal chemistry. The Fe 3O4 MNMs were then grafted with extracts derived from natural products, namely Olecraceavar italica (broccoli), Boletus edulis (mushroom)and Solanum lycopersicum (tomato);(2)characterization of natural products by chromatography and mass spectrometry;(3) characterization of MNMs to determine their crystallinity, morphological and elemental composition by the state-of-the-art instruments; and (4) biological evaluation using Gram-negative and Gram-positive bacteria. The approach provides advantages to precisely control the composition and homogeneity. The second advantage of the colloidal chemistry is its user friendliness and feasibility. Due to the nature of the natural products, the compatibility of MNM is anticipated to be enhanced.In this chapter, the nanomaterials will be discussed from four perspectives,§1.1 Nanotechnology (§1.1), §1.2 Synthesis of nanomaterials; §1.3 The natural product extract,; §1.4 Characterization of nanomaterials; and §1.5Biological application of nanomaterials.Fig. 1 summarized the overarching goals of this study.

Synthesis, characterization and photocatalysis enhancement of Eu2O3-ZnO mixed oxide nanoparticles

NASA Astrophysics Data System (ADS)

Mohamed, W. S.; Abu-Dief, Ahmed M.

2018-05-01

Pure ZnO nanoparticles (NPs) and mixed Eu2O3 and ZnO NPs with different Eu2O3 ratios (5%, 10%, and 15%) were synthesized by a precipitation method under optimum conditions. The synthesized samples were characterized by means of X-ray diffraction, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy, transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, Raman spectroscopy, and UV-vis diffuse reflectance spectroscopy. The as-synthesized ZnO NPs exhibit high phase purity and a highly crystalline wurtzite ZnO structure. The mixed Eu2O3 and ZnO NPs exhibit a Eu2O3 zinc blend phase in addition to the wurtzite phase of pure ZnO, confirming the high purity and good crystallinity of the as-synthesized samples. The high-purity formation of ZnO and Eu2O3 phases was confirmed by FTIR and Raman spectra. Microstructural analysis by SEM and TEM confirmed the sphere-like morphology with different particle sizes (29-40 nm) of the as-synthesized samples. The photocatalytic activities of pure ZnO NPs and mixed Eu2O3 and ZnO NPs for the degradation of methylene blue were evaluated under ultraviolet (UV) irradiation. The results show that Eu2O3 plays an important role in the enhancement of the photocatalytic properties of ZnO NPs. We found that mixed 5% Eu2O3 and ZnO NPs exhibit the highest photocatalytic activity (degradation efficiency of 96.5% after 180 min of UV irradiation) as compared with pure ZnO NPs (degradation efficiency of 80.3% after 180 min of UV irradiation). The increased photocatalytic activity of the optimum mixed Eu2O3 and ZnO NPs is due to the high crystallinity, high surface area with small particle size, and narrow energy gap.

Synthesis and Characterization of 2-D Materials

NASA Astrophysics Data System (ADS)

Pazos, S.; Sahoo, P.; Afaneh, T.; Rodriguez Gutierrez, H.

Atomically thin transition-metal dichacogenides (TMD), graphene, and boron nitride (BN) are two-dimensional materials where the charge carriers (electrons and holes) are confined to move in a plane. They exhibit distinctive optoelectronic properties compared to their bulk layered counterparts. When combined into heterostructures, these materials open more possibilities in terms of new properties and device functionality. In this work, WSe2 and graphene were grown using Chemical Vapor Deposition (CVD) and Physical Vapor Deposition (PVD) techniques. The quality and morphology of each material was checked using Raman, Photoluminescence Spectroscopy, and Scanning Electron Microscopy. Graphene had been successfully grown homogenously, characterized, and transferred from copper to silicon dioxide substrates; these films will be used in future studies to build 2-D devices. Different morphologies of WSe2 2-D islands were successfully grown on SiO2 substrates. Depending on the synthesis conditions, the material on each sample had single layer, double layer, and multi-layer areas. A variety of 2-D morphologies were also observed in the 2-D islands. This project is supported by the NSF REU Grant #1560090 and NSF Grant #DMR-1557434.

Co-Precipitation Synthesis and Characterization of SrBi2Ta2O9 Ceramic

NASA Astrophysics Data System (ADS)

Afqir, Mohamed; Tachafine, Amina; Fasquelle, Didier; Elaatmani, Mohamed; Carru, Jean-Claude; Zegzouti, Abdelouahad; Daoud, Mohamed

2018-04-01

Strontium bismuth tantalate (SrBi2Ta2O9) was synthesized by a co-precipitation method. The sample was characterized by x-ray powder diffraction patterns (XRD), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The results of the dielectric properties are reported at room temperature. No secondary phases were found while heating the powder at 850°C and the pure SrBi2Ta2O9 phase was formed, as revealed by XRD. The characteristic bands for SrBi2Ta2O9 were observed by FTIR at approximately 619 cm-1 and 810 cm-1. SEM micrographs for the sample displayed thin plate-like grains. The grain size was less than 1 μm and the crystallite size of about 24 nm. Dielectric response at room temperature shows that the SrBi2Ta2O9 ceramic has low loss values, and the flattening of the dielectric constant at higher frequencies. The observed Curie temperature is comparable with those reported in the literature.

Synthesis and characterization of titanium dioxide (TiO2) nanopowder

NASA Astrophysics Data System (ADS)

Munirah, S.; Nadzirah, Sh.; Khusaimi, Z.; Fazlena, H.; Rusop, M.

2018-05-01

Titanium dioxide (TiO2) powder was synthesized via sol-gel technique using Titanium tetraisopropoxide (TTIP) and ethanol as precursors. Acetylacetone, distilled water, polyethylene glycol (PEG) and stabilizers (glacial acetic acid and nitric acid) were then added to the solution. The solution was left for ageing for 24 hours and then dried into powder. The synthesized powders were characterized by X-ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Thermogravimetric Analysis (TGA).

V-doped TiO2 supported Pt as a promising oxygen reduction reaction catalyst: Synthesis, characterization and in-situ evaluation in proton exchange membrane fuel cell

NASA Astrophysics Data System (ADS)

Bharti, Abha; Cheruvally, Gouri

2017-09-01

This study deals with the synthesis and characterization of V-doped, TiO2 supported Pt catalyst (Pt/V-TiO2) for oxygen reduction reaction (ORR) and its in-situ performance investigation in proton exchange membrane (PEM) fuel cell. Pt/V-TiO2 nanocomposite catalyst is prepared via a facile sol-gel and microwave assisted, modified chemical reduction route and its performance is compared with the undoped TiO2 supported catalyst, Pt/TiO2 prepared in an identical way. The prepared Pt/V-TiO2 and Pt/TiO2 catalysts are employed as cathode catalyst in PEM fuel cell and compared with standard Pt/C catalyst. Their comparative studies are conducted with physical and electrochemical techniques. In-situ electrochemical characterization studies show improved ORR catalytic activity of Pt/V-TiO2 compared to Pt/TiO2. Furthermore, both Pt/TiO2 and Pt/V-TiO2 are more stable than Pt/C when subjected to 6000 voltammetric cycles in the range of 0.2-1.2 V vs. standard hydrogen electrode in operating fuel cell conditions, losing only <20% of its electrochemical surface area as compared to 50% loss exhibited by Pt/C. This study thus demonstrates Pt/V-TiO2 nanocomposite material as a potential cathode catalyst for PEM fuel cell with immense scope for further investigation.

Synthesis and Characterization of N-Doped Porous TiO2 Hollow Spheres and Their Photocatalytic and Optical Properties

PubMed Central

Li, Hongliang; Liu, Hui; Fu, Aiping; Wu, Guanglei; Xu, Man; Pang, Guangsheng; Guo, Peizhi; Liu, Jingquan; Zhao, Xiu Song

2016-01-01

Three kinds of N-doped mesoporous TiO2 hollow spheres with different N-doping contents, surface area, and pore size distributions were prepared based on a sol–gel synthesis and combined with a calcination process. Melamine formaldehyde (MF) microspheres have been used as sacrificial template and cetyltrimethyl ammonium bromide (CTAB) or polyvinylpyrrolidone (PVP) was selected as pore-directing agent. Core–shell intermediate spheres of titania-coated MF with diameters of 1.2–1.6 μm were fabricated by varying the volume concentration of TiO2 precursor from 1 to 3 vol %. By calcining the core–shell composite spheres at 500 °C for 3 h in air, an in situ N-doping process occurred upon the decomposition of the MF template and CTAB or PVP pore-directing surfactant. N-doped mesoporous TiO2 hollow spheres with sizes in the range of 0.4–1.2 μm and shell thickness from 40 to 110 nm were obtained. The composition and N-doping content, thermal stability, morphology, surface area and pore size distribution, wall thickness, photocatalytic activities, and optical properties of the mesoporous TiO2 hollow spheres derived from different conditions were investigated and compared based on Fourier-transformation infrared (FTIR), SEM, TEM, thermogravimetric analysis (TGA), nitrogen adsorption–desorption, and UV–vis spectrophotoscopy techniques. The influences of particle size, N-doping, porous, and hollow characteristics of the TiO2 hollow spheres on their photocatalytic activities and optical properties have been studied and discussed based on the composition analysis, structure characterization, and optical property investigation of these hollow spherical TiO2 matrices. PMID:28773967

One-pot synthesis and optical properties of Eu3+-doped nanocrystalline TiO2 and ZrO2

NASA Astrophysics Data System (ADS)

Julián, Beatriz; Corberán, Rosa; Cordoncillo, Eloisa; Escribano, Purificación; Viana, Bruno; Sanchez, Clément

2005-11-01

A simple and versatile one-pot sol-gel synthesis of Eu3+-doped nanocrystalline TiO2 and ZrO2 nanomaterials is reported in this paper. It consists of the controlled crystallization of Eu3+-doped TiO2 or ZrO2 nanoparticles from an initial solution containing the metal alkoxide, the lanthanide precursor, a complexing agent and a non-complexing acid. The main interest is that it could be extended to different lanthanide ions and inorganic metal oxides to prepare other multifunctional nanomaterials. The characterization by XRD, HRTEM and SAED techniques showed that the TiO2 and ZrO2 crystallization takes place at very low temperatures (60 °C) and that the crystallite size can be tailored by modifying the synthetic conditions. The optical properties of the resulting materials were studied by emission spectra and decay measurements. Both Eu3+:TiO2 and Eu3+:ZrO2 samples exhibited long lifetime values after removing organic components (τ = 0.7 and 1.3 ms, respectively), but the Eu3+:ZrO2 system is specially promising for photonic applications since its τ value is longer than some reported for other inorganic or hybrid matrices in which Eu3+ ions are complexed. This behaviour has been explained through an effective dispersion of the lanthanide ions within the ZrO2 nanocrystals.

Enzymatic Synthesis of Acylphloroglucinol 3-C-Glucosides from 2-O-Glucosides using a C-Glycosyltransferase from Mangifera indica.

PubMed

Chen, Dawei; Sun, Lili; Chen, Ridao; Xie, Kebo; Yang, Lin; Dai, Jungui

2016-04-18

A green and cost-effective process for the convenient synthesis of acylphloroglucinol 3-C-glucosides from 2-O-glucosides was exploited using a novel C-glycosyltransferase (MiCGTb) from Mangifera indica. Compared with previously characterized CGTs, MiCGTb exhibited unique de-O-glucosylation promiscuity and high regioselectivity toward structurally diverse 2-O-glucosides of acylphloroglucinol and achieved high yields of C-glucosides even with a catalytic amount of uridine 5'-diphosphate (UDP). These findings demonstrate for the first time the significant potential of a single-enzyme approach to the synthesis of bioactive C-glucosides from both natural and unnatural acylphloroglucinol 2-O-glucosides. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis and electrochemical characterization of mesoporous Li2FeSiO4/C composite cathode material for Li-ion batteries

NASA Astrophysics Data System (ADS)

Kumar, Ajay; Jayakumar, O. D.; Bazzi, Khadije; Nazri, Gholam-Abbas; Naik, Vaman M.; Naik, Ratna

2015-03-01

Lithium iron silicate (Li2FeSiO4) has the potential as cathode for Li ion batteries due to its high theoretical capacity (~ 330 mAh/g) and improved safety. The application of Li2FeSiO4 as cathode material has been challenged by its poor electronic conductivity and slow lithium ion diffusion in the solid phase. In order to solve these problems, we have synthesized mesoporous Li2FeSiO4/C composites by sol-gel method using the tri-block copolymer (P123) as carbon source. The phase purity and morphology of the composite materials were characterized by x-ray diffraction, SEM and TEM. The XRD pattern confirmed the formation of ~ 12 nm size Li2FeSiO4 crystallites in composites annealed at 600 °C for 6 h under argon atmosphere. The electrochemical properties are measured using the composite material as positive electrode in a standard coin cell configuration with lithium as the active anode and the cells were tested using AC impedance spectroscopy, cyclic voltammetry, and galvanostatic charge/discharge cycling. The Li2FeSiO4/C composites showed a discharge capacity of ~ 240 mAh/g at a rate of C/30 at room temperature. The effect of different annealing temperature and synthesis time on the electrochemical performance of Li2FeSiO4/C will be presented.

Low‐Temperature Combustion Synthesis of a Spinel NiCo2O4 Hole Transport Layer for Perovskite Photovoltaics

PubMed Central

Papadas, Ioannis T.; Ioakeimidis, Apostolos; Armatas, Gerasimos S.

2018-01-01

Abstract The synthesis and characterization of low‐temperature solution‐processable monodispersed nickel cobaltite (NiCo2O4) nanoparticles (NPs) via a combustion synthesis is reported using tartaric acid as fuel and the performance as a hole transport layer (HTL) for perovskite solar cells (PVSCs) is demonstrated. NiCo2O4 is a p‐type semiconductor consisting of environmentally friendly, abundant elements and higher conductivity compared to NiO. It is shown that the combustion synthesis of spinel NiCo2O4 using tartaric acid as fuel can be used to control the NPs size and provide smooth, compact, and homogeneous functional HTLs processed by blade coating. Study of PVSCs with different NiCo2O4 thickness as HTL reveals a difference on hole extraction efficiency, and for 15 nm, optimized thickness enhanced hole carrier collection is achieved. As a result, p‐i‐n structure of PVSCs with 15 nm NiCo2O4 HTLs shows reliable performance and power conversion efficiency values in the range of 15.5% with negligible hysteresis. PMID:29876223

Structural and magnetic characterizations of Co2FeGa/SiO2 nanoparticles prepared via chemical route

NASA Astrophysics Data System (ADS)

Priyanka, Dhaka, Rajendra S.

2018-04-01

We report the synthesis of Co2FeGa/SiO2 nanoparticles by sol-gel method and characterization usingx-ray diffraction (XRD), transmission electron microscopy (TEM) and magnetic measurements. The Rietveld refinementsof XRD data with space group Fm-3m clearly show the formation of A2 disordersingle phase and the lattice constant isfound to be 5.738 Å. The energy-dispersive x-ray spectroscopy (EDX) confirm the elemental composition close the desired values. The value of coercivity is found to be around 283 Oe and 126 Oe, measured at 10 K and 300 K, respectively. We observed the saturation magnetization significantly lower than expected from Slater-Pauling rule. This decrease in the magnetic moment might be due to the presence of amorphous SiO2 during the synthesis process. A large content of small size SiO2 particles along with Co2FeGa nanoparticles are also found in TEM study.

Solvothermal synthesis of nanocrystalline TiO 2 in toluene with surfactant

NASA Astrophysics Data System (ADS)

Kim, Chung-Sik; Moon, Byung Kee; Park, Jong-Ho; Choi, Byung-Chun; Seo, Hyo-Jin

2003-10-01

Synthesis of narrow-dispersed nanocrystalline TiO 2 was investigated by surfactant-aided solvothermal synthetic method in toluene solutions. Titanium isopropoxide (TIP) was used as precursor, which was decomposed at high temperature in the surfactant-dissolved solution. After the solution was thermally treated at 250°C for 20 h in an autoclave, low-dispersed TiO 2 nanocrystalline particles with average size of <6 nm were synthesized. When sufficient amount of TIP or surfactant was added in the solution, long dumbbell-shaped nanorods were formed, which may be due to the oriented growth of particles along [0 0 1] axis. Characterization of products was investigated by X-ray diffraction and transmission electron microscopy.

Synthesis of TiO{sub 2} nanoparticles by hydrolysis and peptization of titanium isopropoxide solution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahata, S.; Mahato, S. S.; Nandi, M. M.

2012-07-23

Here we report the synthesis and characterization of a stable suspension of modified titania nanoparticles. Phase-pure TiO{sub 2} nanocrystallites with narrow particle-size distributions were selectively prepared by hydrolysis-peptization of modified alkoxide followed by hydrothermal treatment. Autoclaving modified TiO{sub 2} in the presence of HNO3 as cooperative catalysts led to the formation of crystalline TiO{sub 2} with narrow-sized distribution. Following the hydrothermal treatment at 150 Degree-Sign C, X-ray diffraction shows the particles to be exclusively anatase. Synthesized powder is characterized by FT-IR, scanning electron microscopy (FESEM) and transmission electron microscopy (HRTEM). The photocatalytic activity in the degradation of orange-II is quitemore » comparable to good anatase and rutile nanocrystallites.« less

Synthesis and characterization of Zn(O,OH)S and AgInS2 layers to be used in thin film solar cells

NASA Astrophysics Data System (ADS)

Vallejo, W.; Arredondo, C. A.; Gordillo, G.

2010-11-01

In this paper AgInS2 and Zn(O,OH)S thin films were synthesized and characterized. AgInS2 layers were grown by co-evaporation from metal precursors in a two-step process, and, Zn(O,OH)S thin films were deposited from chemical bath containing thiourea, zinc acetate, sodium citrate and ammonia. X-ray diffraction measurements indicated that AgInS2 thin films grown with chalcopyrite structure, and the as-grown Zn(O,OH)S thin films were polycrystalline. It was also found that the AgInS2 films presented p-type conductivity, a high absorption coefficient (greater than 104 cm-1) and energy band-gap Eg of about 1.95 eV, Zn(O,OH),S thin films presented Eg of about 3.89 eV. Morphological analysis showed that under this synthesis conditions Zn(O,OH),S thin films coated uniformly the absorber layer. Additionally, the Zn(O,OH)S kinetic growth on AgInS2 layer was studied also. Finally, the results suggest that these layers possibly could be used in one-junction solar cells and/or as top cell in a tandem solar cell.

Defective TiO2 with oxygen vacancies: synthesis, properties and photocatalytic applications

NASA Astrophysics Data System (ADS)

Pan, Xiaoyang; Yang, Min-Quan; Fu, Xianzhi; Zhang, Nan; Xu, Yi-Jun

2013-04-01

Titanium dioxide (TiO2), as an important semiconductor metal oxide, has been widely investigated in the field of photocatalysis. The properties of TiO2, including its light absorption, charge transport and surface adsorption, are closely related to its defect disorder, which in turn plays a significant role in the photocatalytic performance of TiO2. Among all the defects identified in TiO2, oxygen vacancy is one of the most important and is supposed to be the prevalent defect in many metal oxides, which has been widely investigated both by theoretical calculations and experimental characterizations. Here, we give a short review on the existing strategies for the synthesis of defective TiO2 with oxygen vacancies, and the defect related properties of TiO2 including structural, electronic, optical, dissociative adsorption and reductive properties, which are intimately related to the photocatalytic performance of TiO2. In particular, photocatalytic applications with regard to defective TiO2 are outlined. In addition, we offer some perspectives on the challenge and new direction for future research in this field. We hope that this tutorial minireview would provide some useful contribution to the future design and fabrication of defective semiconductor-based nanomaterials for diverse photocatalytic applications.Titanium dioxide (TiO2), as an important semiconductor metal oxide, has been widely investigated in the field of photocatalysis. The properties of TiO2, including its light absorption, charge transport and surface adsorption, are closely related to its defect disorder, which in turn plays a significant role in the photocatalytic performance of TiO2. Among all the defects identified in TiO2, oxygen vacancy is one of the most important and is supposed to be the prevalent defect in many metal oxides, which has been widely investigated both by theoretical calculations and experimental characterizations. Here, we give a short review on the existing strategies for the

Sustainable synthesis of magnetically separable SiO2/Co@Fe2O4 nanocomposite and its catalytic applications for the benzimidazole synthesis

NASA Astrophysics Data System (ADS)

Jithendra Kumara, K. S.; Krishnamurthy, G.; Sunil Kumar, N.; Naik, Nagaraja; Praveen, T. M.

2018-04-01

The Co(II) and Fe(III) centres magnetically separable two new mesoporous nanocatalyst were synthesised via chemical synthesis method. The transmission electron microscopic studies (TEM) show that, the particles are spherical shape with mean size of 20 nm. The Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) reveals that SiO2 is coating on the surface of the cobalt ferrate nanoparticle (CoFe2O4). The SiO2 coating is efficiently preventing the aggregated collision of nanoparticles. Magnetic measurements show that diamagnetic character of the SiO2 is unaffected to the coercivity of SiO2 coated CoFe2O4 particles. In addition, these nanoparticles are used as nanocatalyst for high yielding, facile and expeditious synthesis of various functionalized 2-arylbenzimidazoles via one-pot condensation. The cascade including imine formation, cyclization, condensation, and aromatization occurs, without addition of any reducing or oxidizing agents. In all situations, the desired product was synthesised with excellent yield. The shorter reaction time, mild reaction condition, simplicity, non-toxicity, safe reaction and easy workup are the impotent merits of this protocol.

Synthesis, characterization and antibacterial property of ZnO:Mg nanoparticles

NASA Astrophysics Data System (ADS)

Kompany, A.; Madahi, P.; Shahtahmasbi, N.; Mashreghi, M.

2012-09-01

Sol-gel method was successfully used for the synthesis of ZnO nanoparticles (NPs) doped with different concentrations of Mg and the structural, optical and antibacterial properties of the nanoparticles were studied. The synthesized ZnO:Mg powders were characterized using x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transformation Infrared (FTIR) and UV-Vis spectroscopy. It was revealed that the samples have hexagonal Wurtzite structure, and the phase segregation takes place for 15% Mg content. TEM images show that the average size of the particles is about 50 nm. Also, the antibacterial activities of the nanoparticles were tested against Escherichia coli (Gram negative) cultures. ZnO:Mg nanofluid showed good antibacterial activity which increases with the increase of NPs concentration, and decreases slightly with the amount of Mg.

Synthesis, characterization, electrical conductivity and luminescence properties of two copper(II) complexes with tridentate N2O chelating ligands containing imine bond

NASA Astrophysics Data System (ADS)

Gönül, İlyas; Ay, Burak; Karaca, Serkan; Şahin, Onur; Serin, Selahattin

2018-03-01

In the present study, we describe the synthesis and characterization of two tridentate N2O donor ligands, namely, (E)-2-(((2-(diethylamino)ethyl)imino)methyl)-6-methoxyphenol (HL1) and (E)-2-(((2-(diethylamino)ethyl)imino)methyl)-6-ethoxyphenol (HL2), and their copper(II) complexes, [Cu(L1)(CH3COO)] (1), [Cu(L2)(CH3COO)] (2). They have been synthesized under conventional methods and characterized by elemental analysis, FTIR, 1H and 13C NMR, ICP-OES, TGA and GC/MS analysis. For the morphological analysis field emission scanning electron microscopy (FESEM) was used. The geometry of the copper(II) complexes was determined by single crystal X-ray diffraction analysis. The copper(II) ions are in distorted square-pyramidal coordination environments. Complexes crystallize in monoclinic space group, P21/c. The electrical conductivity and luminescence properties of 1-2 have been investigated.

Lanthanum cerate (La2Ce2O7): hydrothermal synthesis, characterization and optical properties

NASA Astrophysics Data System (ADS)

Khademinia, Shahin; Behzad, Mahdi

2015-03-01

La2Ce2O7 nano-powders were synthesized via a hydrothermal reaction in a deionized water (S 1) and in a 2 M NaOH aqueous solution (S 2) at 180 °C for 48 h. La(NO3)3·H2O and (NH4)2Ce(NO3)6 were used in the stoichiometric 1:1 La:Ce molar ratio as raw materials. The obtained materials were crystallized in a cubic crystal structure with space group. The synthesized materials were characterized by powder X-ray diffraction technique and Fourier-transform infrared spectroscopy. To investigate the effect of the basic solution on the morphology of the obtained materials, the morphologies of the synthesized materials were studied by field emission scanning electron microscopy technique. The technique showed that the morphology of La2Ce2O7 samples changed from grain to rod-like structure in presence of the basic solution. Cell parameter refinements showed that these parameters were larger for S2 than those for S 1. Photoluminescence and ultraviolet visible spectra of the synthesized nanomaterials were also investigated.

Molten Salt Synthesis and Structural Characterization of BaTiO3 Nanocrystal Ceramics

NASA Astrophysics Data System (ADS)

Ahda, S.; Misfadhila, S.; Parikin, P.; Putra, T. Y. S. P.

2017-02-01

A new synthesis route to obtain high-purity barium titanate powder, BaTiO3, using the molten salt method by reacting the raw materials (BaCO3 and TiO2) in an atmosphere of molten NaCl and KCl, has been developed. The synthesized BaTiO3 ceramic particles have been successfully carried out at the sintering temperature 950°C for 4 hours. The Rietveld refinement of the XRD diffraction patterns was employed to characterize the structural information of the nanocrystalline BaTiO3 ceramics. The lattice parameters (a=4.0043 Å, b=4.0308Å with space group P4mm) of tetragonal perovskite structure, as an indication of piezoelectric characteristics, have been successfully determined by the Rietveld refinement. While the crystallitte particle size and strains have been obtained for the values of 110.6 nm and 0.74 % respectively

Synthesis and characterization of metal oxide-polyaniline emeraldine salt based nanocomposite

NASA Astrophysics Data System (ADS)

Kumar, K. Siva; Kavitha, B.; Prabakar, K.; Srinivasu, D.; Srinivas, Ch.; Narsimlu, N.

2013-02-01

This paper describes the synthesis of TiO2 (core)/Polyaniline (shell) core-shell structured nanocomposites and characterization of the synthesized material. The morphological characterization is performed with XRD, SEM, DLS and SANS. Spectroscopic characterization is performed with FTIR, UV/Visible and ESR techniques.

Combustion synthesized TiO{sub 2} for enhanced photocatalytic activity under the direct sunlight-optimization of titanylnitrate synthesis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daya Mani, A.; Laporte, V.; Ghosal, P.

2012-09-15

Graphical abstract: Effect of oxidant on the combustion synthesis of TiO{sub 2} has been studied by preparing titanylnitrate in four different ways from Ti(IV) iso-propoxide. It is observed that oxidant preparation method has a significant effect on physico-chemical as well as photocatalytic properties of TiO{sub 2}. All the catalysts showed excellent photocatalytic activity than Degussa P-25 under direct sunlight for the degradation of a textile dye (methylene blue), without the need of external light sources, oxygen supply and reactor systems. Highlights: ► Optimized synthesis of titanylnitrate. ► Influence of titanylnitrate synthesis on the physico-chemical properties of TiO{sub 2} prepared bymore » combustion synthesis. ► Development of highly efficient TiO{sub 2} photocatalysts those are active under the direct sunlight in open atmosphere. ► Degradation of the textile dye (methylene blue) under direct sunlight. -- Abstract: Optimized synthesis of Ti-precursor ‘titanylnitrate’ for one step combustion synthesis of N- and C-doped TiO{sub 2} catalysts were reported and characterized by using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), diffused reflectance UV–vis spectroscopy, N{sub 2} adsorption and X-ray photoelectron spectroscopy (XPS). XRD confirmed the formation of TiO{sub 2} anatase and nano-crystallite size which was further confirmed by TEM. UV-DRS confirmed the decrease in the band gap to less than 3.0 eV, which was assigned due to the presence of C and N in the framework of TiO{sub 2} as confirmed by X-ray photoelectron spectroscopy. Degradation of methylene blue in aqueous solution under the direct sunlight was carried out and typical results indicated the better performance of the synthesized catalysts than Degussa P-25.« less

High-pressure synthesis and characterizations of the R2Pt2O7 pyrochlores.

NASA Astrophysics Data System (ADS)

Cai, Yunqi; Cui, Qi; Cheng, Jinguang; Dun, Zhiling; Zhou, Haidong; Ma, Jie; Cruz, C. Dela; Yan, Jiaqiang; Li, Xiang; Zhou, Jianshi

Pyrochlore R2B2O7 where R3 + stands for rear-earth ion and B4 + for a nonmagnetic cation such as Sn4 +or Ti4 +consist of an important family of geometrically frustrated magnets, which have been the focus of extensive investigations over last decades. To further enlarge the R2B2O7, we have chosen to stabilize the Pt-based cubic pyrochlores under HPHT conditions for two reasons: (1) Pt4 + is in a low-spin state which ionic radius is located in between Ti4 + (0.605\\x85) and Sn4 + (0.69\\x85), and (2) Pt4 + has a spatially much more extended 5d orbitals and thus enhanced Pt 5d-O 2p hybridizations that might modify the local anisotropic exchange interactions. Such an effect has never been taken into account in the previous studies. In this work, we will present the detailed characterizations on the pyrochlores R2Pt2O7 obtained under HPHT conditions. This work is supported by the National Science Foundation of China (Grant Nos.11304371, 11574377), part of the work was supported by the CEM, and NSF MRSEC, under Grant DMR-1420451, and Grant No. NSF-DMR-1350002.

Synthesis of Fe3O4@SiO2@OSi(CH2)3NHRN(CH2PPh2)2PdCl2 type nanocomposite complexes: Highly efficient and magnetically-recoverable catalysts in vitamin K3 synthesis.

PubMed

Uruş, Serhan

2016-12-15

The synthesis of aminomethylphosphine-metal complexes have opened a new perspective to the catalytic applications of organic compounds. Magnetic Fe3O4 nano-core was synthesized using the closed quartz tube with Teflon cover and microwaved 200°C for 1h with power controlled instrument set to max. 600W. Novel nano-composite supported; Fe3O4@SiO2(CH2)3NHArN(CH2PPh2)2 and Fe3O4@SiO2(CH2)3N(CH2PPh2)2 type bis(diphenylphosphinomethyl)amino ligands and their Pd(II) complexes have been synthesized and characterized with FT-IR, SEM, EDX, TEM, UV-Visible, XRD and TG/DTA techniques. All the complexes were used as heterogeneous catalysts in the oxidation of 2-methyl naphthalene (2MN) to 2-methyl-1, 4-naphthoquinone (vitamin K3, menadione, 2MNQ) in the presence of hydrogen peroxide and acetic acid. Selectivity reached about 55-60% with a conversion of 90-96% using the nano-magnetite supported aminomethylphosphine-Pd(II) complexes. The complexes were very active in three times in the catalytic recycling experiments in five catalytic cycles. Copyright © 2016 Elsevier Ltd. All rights reserved.

Sol-gel synthesis of fine Gd{sub 2}CuO{sub 4} particles: Influence of synthesis variables

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mahia, J.; Vazquez-Vazquez, C.; Basadre-Pampin, M.I.

1996-02-01

Fine particles of Gd{sub 2}CuO{sub 4} were prepared by a sol-gel reaction of an aqueous solution of metal nitrates in the presence of urea, which leads to high-homogeneity polycrystalline powders of Gd{sub 2}CuO{sub 4}. The authors have studied the synthesis conditions, demonstrating the existence of a relationship between the calcination temperature and the heating time needed to attain the pure phase. Gd{sub 2}CuO{sub 4} was obtained at temperatures of the order of 650 C, lower than temperatures employed in the conventional ceramic technique. The influence of the [urea]/[salts] ratio and an excess of Cu(II) in the starting solution was alsomore » studied and discussed. X-ray powder diffraction inductively coupled plasma atomic emission spectroscopy (ICPAES), photon correlation spectroscopy (PCS), and transmission electron microscopy (TEM) were used to characterize the Gd{sub 2}CuO{sub 4} samples obtained.« less

Synthesis and physicochemical characterizations and antimicrobial activity of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Sharma, Bhumika K.; Patel, Kinjal; Roy, Debesh R.

2018-05-01

Nanoparticles exhibit very interesting and useful physicochemical properties when they interact with substrates and goes through some physicochemical and/or biological processes. ZnO is known to be a highly demanding nanomaterial due to its discreet properties, shapes and sizes. A detail experimental study on the synthesis, characterization and antibacterial activity of ZnO nanoparticles (NPs) is performed. ZnO NPs are synthesized using chemical precipitation method. The understanding of crystal structure, morphology and elemental compositions are explained using Powder X-Ray Diffraction (XRD) and Field Emission Scanning Electron Microscope (FE-SEM) respectively. Fourier transform infrared spectroscopy (FTIR) is performed to achieve the information on the presence of various functional groups. The antibacterial activity of these ZnO NPs is investigated in terms of Zone of Inhibition (ZOI) against Escherichia coli (Gram negative) microorganisms.

Hydrothermal synthesis of MnO2/CNT nanocomposite with a CNT core/porous MnO2 sheath hierarchy architecture for supercapacitors.

PubMed

Xia, Hui; Wang, Yu; Lin, Jianyi; Lu, Li

2012-01-05

MnO2/carbon nanotube [CNT] nanocomposites with a CNT core/porous MnO2 sheath hierarchy architecture are synthesized by a simple hydrothermal treatment. X-ray diffraction and Raman spectroscopy analyses reveal that birnessite-type MnO2 is produced through the hydrothermal synthesis. Morphological characterization reveals that three-dimensional hierarchy architecture is built with a highly porous layer consisting of interconnected MnO2 nanoflakes uniformly coated on the CNT surface. The nanocomposite with a composition of 72 wt.% (K0.2MnO2·0.33 H2O)/28 wt.% CNT has a large specific surface area of 237.8 m2/g. Electrochemical properties of the CNT, the pure MnO2, and the MnO2/CNT nanocomposite electrodes are investigated by cyclic voltammetry and electrochemical impedance spectroscopy measurements. The MnO2/CNT nanocomposite electrode exhibits much larger specific capacitance compared with both the CNT electrode and the pure MnO2 electrode and significantly improves rate capability compared to the pure MnO2 electrode. The superior supercapacitive performance of the MnO2/CNT nancomposite electrode is due to its high specific surface area and unique hierarchy architecture which facilitate fast electron and ion transport.

Hydrothermal synthesis of MnO2/CNT nanocomposite with a CNT core/porous MnO2 sheath hierarchy architecture for supercapacitors

PubMed Central

2012-01-01

MnO2/carbon nanotube [CNT] nanocomposites with a CNT core/porous MnO2 sheath hierarchy architecture are synthesized by a simple hydrothermal treatment. X-ray diffraction and Raman spectroscopy analyses reveal that birnessite-type MnO2 is produced through the hydrothermal synthesis. Morphological characterization reveals that three-dimensional hierarchy architecture is built with a highly porous layer consisting of interconnected MnO2 nanoflakes uniformly coated on the CNT surface. The nanocomposite with a composition of 72 wt.% (K0.2MnO2·0.33 H2O)/28 wt.% CNT has a large specific surface area of 237.8 m2/g. Electrochemical properties of the CNT, the pure MnO2, and the MnO2/CNT nanocomposite electrodes are investigated by cyclic voltammetry and electrochemical impedance spectroscopy measurements. The MnO2/CNT nanocomposite electrode exhibits much larger specific capacitance compared with both the CNT electrode and the pure MnO2 electrode and significantly improves rate capability compared to the pure MnO2 electrode. The superior supercapacitive performance of the MnO2/CNT nancomposite electrode is due to its high specific surface area and unique hierarchy architecture which facilitate fast electron and ion transport. PMID:24576342

Hydrothermal synthesis of MnO2/CNT nanocomposite with a CNT core/porous MnO2 sheath hierarchy architecture for supercapacitors

NASA Astrophysics Data System (ADS)

Xia, Hui; Wang, Yu; Lin, Jianyi; Lu, Li

2012-01-01

MnO2/carbon nanotube [CNT] nanocomposites with a CNT core/porous MnO2 sheath hierarchy architecture are synthesized by a simple hydrothermal treatment. X-ray diffraction and Raman spectroscopy analyses reveal that birnessite-type MnO2 is produced through the hydrothermal synthesis. Morphological characterization reveals that three-dimensional hierarchy architecture is built with a highly porous layer consisting of interconnected MnO2 nanoflakes uniformly coated on the CNT surface. The nanocomposite with a composition of 72 wt.% (K0.2MnO2·0.33 H2O)/28 wt.% CNT has a large specific surface area of 237.8 m2/g. Electrochemical properties of the CNT, the pure MnO2, and the MnO2/CNT nanocomposite electrodes are investigated by cyclic voltammetry and electrochemical impedance spectroscopy measurements. The MnO2/CNT nanocomposite electrode exhibits much larger specific capacitance compared with both the CNT electrode and the pure MnO2 electrode and significantly improves rate capability compared to the pure MnO2 electrode. The superior supercapacitive performance of the MnO2/CNT nancomposite electrode is due to its high specific surface area and unique hierarchy architecture which facilitate fast electron and ion transport.

Synthesis and Characterization of Mg-doped ZnO Nanorods for Biomedical Applications

NASA Astrophysics Data System (ADS)

Gemar, H.; Das, N. C.; Wanekaya, A.; Delong, R.; Ghosh, K.

2013-03-01

Nanomaterials research has become a major attraction in the field of advanced materials research in the area of Physics, Chemistry, and Materials Science. Bio-compatible and chemically stable metal nanoparticles have biomedical applications that includes drug delivery, cell and DNA separation, gene cloning, magnetic resonance imaging (MRI). This research is aimed at the fabrication and characterization of Mg-doped ZnO nanorods. Hydrothermal synthesis of undoped ZnO and Mg-doped ZnO nanorods is carried out using aqueous solutions of Zn(NO3)2 .6H2O, MgSO4, and using NH4OH as hydrolytic catalyst. Nanomaterials of different sizes and shapes were synthesized by varying the process parameters such as molarity (0.15M, 0.3M, 0.5M) and pH (8-11) of the precursors, growth temperature (130°C), and annealing time during the hydrothermal Process. Structural, morphological, and optical properties are studied using various techniques such as XRD, SEM, UV-vis and PL spectroscopy. Detailed structural, and optical properties will be discussed in this presentation. This work is partially supported by National Cancer Institute (1 R15 CA139390-01).

Reverse Micelle Synthesis and Characterization of Supported Pt/Ni Bimetallic Catalysts on gamma-Al2O3

DOE Office of Scientific and Technical Information (OSTI.GOV)

B Cheney; J Lauterbach; J Chen

2011-12-31

Reverse micelle synthesis was used to improve the nanoparticle size uniformity of bimetallic Pt/Ni nanoparticles supported on {gamma}-Al{sub 2}O{sub 3}. Two impregnation methods were investigated to optimize the use of the micelle method: (1) step-impregnation, where Ni nanoparticles were chemically reduced in microemulsion and then supported, followed by Pt deposition using incipient wetness impregnation, and (2) co-impregnation, where Ni and Pt were chemically reduced simultaneously in microemulsion and then supported. Transmission electron microscopy (TEM) was used to characterize the particle size distribution. Atomic absorption spectroscopy (AAS) was used to perform elemental analysis of bimetallic catalysts. Extended X-ray absorption fine structuremore » (EXAFS) measurements were utilized to confirm the formation of the Pt-Ni bimetallic bond in the step-impregnated catalyst. CO pulse chemisorption and Fourier transform infrared spectroscopy (FTIR) studies of 1,3-butadiene hydrogenation in a batch reactor were performed to determine the catalytic activity. Step-impregnated Pt/Ni catalyst demonstrated enhanced hydrogenation activity over the parent monometallic Pt and Ni catalysts due to bimetallic bond formation. The catalyst synthesized using co-impregnation showed no enhanced activity, behaving similarly to monometallic Ni. Overall, our results indicate that reverse micelle synthesis combined with incipient wetness impregnation produced small, uniform nanoparticles with bimetallic bonds that enhanced hydrogenation activity.« less

Combustion synthesis and characterization of blue long lasting phosphor CaAl2O4: Eu2+, Dy3+ and its novel application in latent fingerprint and lip mark detection

NASA Astrophysics Data System (ADS)

Sharma, Vishal; Das, Amrita; Kumar, Vijay; Kumar, Vinay; Verma, Kartikey; Swart, H. C.

2018-04-01

This work investigates the structural, optical and photometric characterization of a Eu2+/Dy3+ doped calcium aluminates phosphor (CaAl2O4: Eu2+/Dy3+) for finger and lip print detections. Synthesis of CaAl2O4: Eu2+/Dy3+ (CAED) phosphors were carried out via a combustion synthesis method with urea as a fuel. Eu2+/Dy3+ doped CaAl2O4 phosphors have been studied with X-ray diffraction (XRD, Energy Dispersive X-Ray Spectroscopy Selected Area Diffraction (SAED) and High resolution Transmission Electron Microscope (HR-TEM). The XRD pattern shows that the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphor have a single monoclinic structure and show that the addition of the dopant/co-dopants didn't change the crystal structure. The formation of monoclinic phase was confirmed by the selected area diffraction pattern. The TEM micrograph displays the morphology of the synthesized Eu2+/Dy3+ doped CaAl2O4 phosphors as spherical particles with an average particle size of 33 nm. The optical band gap was calculated using the diffuse reflectance for the synthesized nanophosphor powders. The photoluminescence emission spectra was recorded for the synthesized powder, with an excitation wavelength of 326 nm and the major bands was recorded at 447 nm corresponding to the blue color and two minor bands were recorded at 577 nm and 616 nm. To the best of our knowledge, this work is the first to show the use of CaAl2O4: Eu2+/Dy3+ nanophosphor in developing latent fingerprint and lip print effectively.

Precipitation method for barium metaborate (BaB{sub 2}O{sub 4}) synthesis from borax solution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Akşener, Eymen; Figen, Aysel Kantürk; Pişkin, Sabriye

2013-12-16

In this study, barium metaborate (BaB{sub 2}O{sub 4}, BMB) synthesis from the borax solution was carried out. BMB currently is used in production of ceramic glazes, luminophors, oxide cathodes as well as additives to pigments for aqueous emulsion paints and also β−BaB{sub 2}O{sub 4} single crystals are the best candidate for fabrication of solid-state UV lasers operating at a wavelength of 200 nm due to excellent nonlinear optical properties. In the present study, synthesis was carried out from the borax solution (Na{sub 2}B{sub 4}O{sub 7⋅}10H{sub 2}O, BDH) and barium chloride (BaCI{sub 2⋅}2H{sub 2}O, Ba) in the glass-batch reactor with stirring.more » The effect of, times (5-15 min), molar ratio [stoich.ration (1.0:2.0), 1.25:2.0, 1.5:2.0, 2.5:2:0, 3.0:2.0, 3.5:2.0,4.0:2.0, 5.0:2.0] and also crystallization time (2-6 hour) on the BMB yield (%) was investigated at 80 °C reaction temperature. It is found that, BMB precipitation synthesis with 90 % yield can be performed from 0.50 molar ration (BDH:Ba), under 80 °C, 15 minute, and 6 hours crystallization time. The structural properties of BMB powders were characterized by using XRD, FT-IR and DTA-TG instrumental analysis technique.« less

Synthesis and characterization of reduced graphene oxide decorated with CeO2-doped MnO2 nanorods for supercapacitor applications.

PubMed

Ojha, Gunendra Prasad; Pant, Bishweshwar; Park, Soo-Jin; Park, Mira; Kim, Hak-Yong

2017-05-15

A novel and efficient CeO 2 -doped MnO 2 nanorods decorated reduced graphene oxide (CeO 2 -MnO 2 /RGO) nanocomposite was successfully synthesized via hydrothermal method. The growth of the CeO 2 doped MnO 2 nanorods over GO sheets and reduction of GO were simultaneously carried out under hydrothermal treatment. The morphology and structure of as-synthesized nanocomposite were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and Raman spectroscopy, which revealed the formation of CeO 2 -MnO 2 decorated RGO nanocomposites. The electrochemical performance of as-prepared CeO 2 -MnO 2 /RGO nanocomposites as an active electrode material for supercapacitor was evaluated by cyclic voltammetry, charge-discharge, and electrochemical impedance spectroscopy (EIS) methods in 2M alkaline medium. The obtained results revealed that as-synthesized CeO 2 -MnO 2 /RGO nanocomposite exhibited higher specific capacitance (648F/g) as compared to other formulations (MnO 2 /RGO nanocomposites: 315.13 F/g and MnO 2 nanorods: 228.5 F/g) at the scan rate of 5mV/s. After 1000 cycles, it retained ∼90.4%, exhibiting a good stability. The high surface area, enhanced electrical conductivity, and good stability possess by the nanocomposite make this material a promising candidate to be applied as a supercapacitor electrode. Copyright © 2017 Elsevier Inc. All rights reserved.

Synthesis and characterization of polycrystalline CdSiP2

NASA Astrophysics Data System (ADS)

Bereznaya, S. A.; Korotchenko, Z. V.; Sarkisov, S. Yu; Korolkov, I. V.; Kuchumov, B. M.; Saprykin, A. I.; Atuchin, V. V.

2018-05-01

A modified method is proposed for the CdSiP2 compound synthesis from elemental starting components. The developed technique allows completing the synthesis process within 30 h. The phase and chemical composition of the synthesized material were confirmed by the x-ray diffraction analysis and scanning electron microscopy with energy-dispersive spectroscopy. The transparent crystal block sized 3 × 3 × 2 mm3 was cut from the polycrystalline ingot and characterized by optical methods.

Synthesis, characterization and solid-state properties of [Zn(Hdmmthiol)2]\\cdot2H2O complex

NASA Astrophysics Data System (ADS)

Dagdelen, Fethi; Aydogdu, Yildirim; Dey, Kamalendu; Biswas, Susobhan

2016-05-01

The zinc(II) complex with tridentate thiohydrazone ligand have been prepared by metal template reaction. The metal template reaction was used to prepare the zinc (II) complex with tridentate thiohydrazone ligand. The reaction of diacetylmonoxime and, morpholine N-thiohydrazidewith Zn(OAc)2 \\cdot2H2O under reflux yielded the formation of the [Zn(Hdmmthiol )2]\\cdot2H2O complex. The complex was characterized by a combination of protocols including elemental analysis, UV+vis, FT-IR, TG and PXRD. The temperature dependence of the electrical conductivity and the optical property of the [Zn(Hdmmthiol )2] \\cdot2H2O complex is called H2dammthiol was studied. Powder X-ray diffraction (PXRD) method was used to investigate the crystal structure of the sample. The zinc complex was shown to be a member of the triclinic system. The zinc complex was determined to have n-type conductivity as demonstrated in the hot probe measurements. The complex was determined to display direct optical transition with band gaps of 2.52eV as determined by the optical absorption analysis.

Synthesis of ZnFe2O4/SiO2 composites derived from a diatomite template.

PubMed

Liu, Zhaoting; Fan, Tongxiang; Zhou, Han; Zhang, Di; Gong, Xiaolu; Guo, Qixin; Ogawa, Hiroshi

2007-03-01

A novel porous ZnFe2O4/SiO2 composite product has been generated with a template-directed assembly method from porous diatomite under different synthesis conditions, such as precursor concentrations (metallic nitrates), calcination temperature and diatomite type. The phase composition and morphology of all the materials were examined by x-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). The results indicated that an inherited hierarchical porous structure from the diatomite template can be obtained, and the synthesis conditions were found to have clear effects on the formation of the ZnFe2O4/SiO2 composite. The ideal composite of ZnFe2O4/SiO2 can be obtained through optimization of diatomite template type, precursor solution and calcination temperature. Furthermore, the adsorption abilities of two types of diatomites were analyzed in detail using FTIR spectra and nitrogen adsorption measurements etc, which proved that A-diatomite (Shengzhou-diatomite) is better than B-diatomite (Changbai-diatomite) on the aspect of adsorbing Zn and Fe ions, and of forming the ZnFe2O4.

Synthesis and characterization of magnesium aluminate (MgAl2O4) spinel (MAS) thin films

NASA Astrophysics Data System (ADS)

Ahmad, Syed Muhammad; Hussain, Tousif; Ahmad, Riaz; Siddiqui, Jamil; Ali, Dilawar

2018-01-01

In a quest to identify more economic routes for synthesis of magnesium aluminate (MgAl2O4) spinel (MAS) thin films, dense plasma focus device was used with multiple plasma focus shots. Structural, bonding between composite films, surface morphological, compositional and hardness properties of MAS thin films were investigated by using x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive x-rays (EDX) analysis and Vickers micro hardness test respectively. In XRD graph, the presence of MgAl2O4 diffraction peaks in crystallographic orientations (222), (400) and (622) pointed out the successful formation of polycrystalline thin films of MgAl2O4 with face centered cubic structure. The FTIR spectrums showed a major common transmittance band at 697.95 cm-1 which belongs to MgAl2O4. SEM micrographs illustrated a mesh type, granular and multi layers microstructures with significant melting effects. EDX spectrum confirmed the existence of magnesium, oxygen and aluminum in MAS films. A common increasing behavior in micro-hardness of composite MgAl2O4 films by increasing number of plasma focus shots was found.

Auto-combustion synthesis and characterization of Mg doped CuAlO{sub 2} nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Agrawal, Shraddha, E-mail: shraddhaa32@gmail.com; Parveen, Azra; Naqvi, A. H.

2015-06-24

The synthesis of pure and Mg doped Copper aluminumoxide CuAlO{sub 2}nanoparticles, a promising p-type TCO (transparent conducting oxide) have been done bysol gel auto combustion method using NaOH as a fuel, calcinated at 600°C. The structural properties were examined by XRD and SEM techniques. The optical absorption spectra of CuAlO{sub 2} sample recorded by UV-VIS spectrophotometer in the range of 200 to 800 nm have been presented. The crystallite size was determined by powder X-ray diffraction technique. The electrical behavior of pure and Mg doped CuAlO{sub 2} has been studied over a wide range of frequencies by using complex impedance spectroscopy.Themore » variation of a.c. conductivity has been studied as function of frequency and temperature. The data taken together conclude that doping causes decreases in the ac conductivity of the nanoparticles as compared with the pure nanoparticles. Mg doping affects the optical properties and band gap.« less

Synthesis and optical characterization of LiKB4O7, Li2B6O10, and LiCsB6O10 glasses.

PubMed

Adamiv, V; Teslyuk, I; Dyachok, Ya; Romanyuk, G; Krupych, O; Mys, O; Martynyuk-Lototska, I; Burak, Ya; Vlokh, R

2010-10-01

In the current work we report on the synthesis of LiKB(4)O(7), Li(2)B(6)O(10), and LiCsB(6)O(10) borate glasses. The results for their piezo-optic, acousto-optic, acoustic, elastic, refractive, optical transmission, and optical resistance properties are also presented. It is shown that some of these glasses represent efficient acousto-optic materials that are transparent down to the vacuum ultraviolet range and highly resistant to laser radiation.

Synthesis, structure, and characterization of a new sandwich-type arsenotungstocerate, [As 2W 18Ce 3O 71(H 2O) 3] 12-

NASA Astrophysics Data System (ADS)

Alizadeh, M. H.; Eshtiagh-Hosseini, H.; Khoshnavazi, R.

2004-01-01

The rational synthesis of the new sandwich-type arsenotungstocerate [As 2W 18Ce 3O 71(H 2O) 3] 12- is reported for the first time by reaction of the trivacant lacunary species A-α-[AsW 9O 34] 9- with appropriate Ce IV. The single crystal structure analysis was carried out on K 7(H 3O) 5[As 2W 18Ce 3O 71(H 2O) 3]·9H 2O; H 39As 2Ce 3K 7O 88W 18; ( 2) which crystallizes in triclinic system, space group P overline1 with a=11.615(5) Å, b=17.638(7) Å, c=19.448(8) Å, α=73.643(7)°, β=88.799(7)°, γ=88.078(7)° and Z=2. The anion consists on two lacunary A-α-[AsW 9O 34] 9- Keggin moieties linked via a (H 2OCeO) 3 belt leading to a sandwich-type structure. Each cerium atom adopts tri-capped trigonal-prismatic coordination achieved by two terminal oxygen of an edge shared paired of WO 6 octahedra to each A-α-AsW 9O 349- moiety and two oxygen from the belt and the cap by one μ 3-O (As, W 2) to each A-α-AsW 9O 349- moiety and one external water ligand. The Ce-O bond lengths average in CeO 6 group, Ce-O(As, W 2) and Ce-O(nW) are 2.300(9), 2.887(3) and 2.682(5) Å, respectively. The acid/base titration curve reveals that the anion has two different titrable protons.

Caged Naloxone: Synthesis, Characterization, and Stability of 3- O-(4,5-Dimethoxy-2-nitrophenyl)carboxymethyl Naloxone (CNV-NLX).

PubMed

Lewin, Anita H; Fix, Scott E; Zhong, Desong; Mayer, Louise D; Burgess, Jason P; Mascarella, S Wayne; Reddy, P Anantha; Seltzman, Herbert H; Carroll, F Ivy

2018-03-21

The photolabile analogue of the broad-spectrum opioid antagonist naloxone, 3- O-(4,5-dimethoxy-2-nitrophenyl)carboxymethyl naloxone (also referred to as "caged naloxone", 3- O-(α-carboxy-6-nitroveratryl)naloxone, CNV-NLX), has been found to be a valuable biochemical probe. While the synthesis of CNV-NLX is simple, its characterization is complicated by the fact that it is produced as a mixture of α R,5 R,9 R,13 S,14 S and α S,5 R,9 R,13 S,14 S diastereomers. Using long-range and heteronuclear NMR correlations, the 1 H NMR and 13 C NMR resonances of both diastereomers have been fully assigned, confirming the structures. Monitoring of solutions of CNV-NLX in saline buffer, in methanol, and in DMSO has shown CNV-NLX to be stable for over a week under fluorescent laboratory lights at room temperature. Exposure of such solutions to λ 365 nm from a hand-held UV lamp led to the formation of naloxone and CNV-related breakdown products.

Synthesis and properties of 2'-O-methyl-4'-thioRNA.

PubMed

Takahashi, Mayumi; Inoue, Naonori; Minakawa, Noriaki; Matsuda, Akira

2005-01-01

In this presentation, we will discuss the synthesis and properties of 2'-O-methyl-4'-thioRNA, an RNA molecule consisting of 2'-O-methyl-4'-thionucleosides. We first synthesized 2'-O-methyl-4'-thiouridine and -cytidine derivatives via 2,2'-O-anhydro-4'-thiouridine. The RNA consisting of 2'-O-methyl-4'-thiopyrimidine nucleosides and 2'-O-methylpurine nucleosides, 2'-OMe-4'-thioRNA, was synthesized on a DNA synthesizer according to the standard phosphoramidite protocol.

Synthesis and characterization of physical properties of Gd2O2S:Pr3+ semi-nanoflower phosphor

NASA Astrophysics Data System (ADS)

Bagheri, A.; Rezaee Ebrahim Saraee, Kh.; Shakur, H. R.; Zamani Zeinali, H.

2016-05-01

Pure gadolinium oxysulfide phosphor (Gd2O2S) and trivalent praseodymium-doped gadolinium oxysulfide phosphor (Gd2O2S:Pr3+) scintillators with semi-nanoflower crystalline structures were successfully synthesized through a precipitation method and subsequent calcination treatment as a converter for X-ray imaging detectors. The characterization such as the crystal structures and nanostructure of Gd2O2S:Pr3+ scintillator measured by XRD and FeE-SEM experiment. The optical properties of Gd2O2S:Pr3+ scintillator were studied. Luminescence spectra of Gd2O2S:Pr3+ under 320 nm UV excitation show a green emission at near 511 nm corresponding to the 3P0-3H4 of Pr ions. After scintillation properties of synthesized Gd2O2S:Pr3+ scintillator investigated, Gd2O2S:Pr3+ scintillating film fabricated on a glass substrate by a sedimentation method. X-ray imaging of the fabricated scintillators confirmed that the Gd2O2S:Pr3+ scintillator could be used for radiography applications in which good spatial resolution is needed.

Synthesis, characterization and electrochemical performance of graphene decorated with 1D NiMoO4.nH2O nanorods

NASA Astrophysics Data System (ADS)

Ghosh, Debasis; Giri, Soumen; Das, Chapal Kumar

2013-10-01

One-dimensional NiMoO4.nH2O nanorods and their graphene based hybrid composite with good electrochemical properties have been synthesized by a cost effective hydrothermal procedure. The formation of the mixed metal oxide and the composite was confirmed by XRD, XPS and Raman analyses. The morphological characterizations were carried out using FESEM and TEM analyses. The materials were subjected to electrochemical characterization through cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) studies with 6 M KOH as the supporting electrolyte. For NiMoO4.nH2O, a maximum specific capacitance of 161 F g-1 was obtained at 5 A g-1 current density, accompanied with an energy density of 4.53 W h kg-1 at a steady power delivery rate of 1125 W kg-1. The high utility of the pseudocapacitive NiMoO4.nH2O was achieved in its graphene based composite, which exhibited a high specific capacitance of 367 F g-1 at 5 A g-1 current density and a high energy density of 10.32 W h kg-1 at a power density of 1125 W kg-1 accompanied with long term cyclic stability.One-dimensional NiMoO4.nH2O nanorods and their graphene based hybrid composite with good electrochemical properties have been synthesized by a cost effective hydrothermal procedure. The formation of the mixed metal oxide and the composite was confirmed by XRD, XPS and Raman analyses. The morphological characterizations were carried out using FESEM and TEM analyses. The materials were subjected to electrochemical characterization through cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) studies with 6 M KOH as the supporting electrolyte. For NiMoO4.nH2O, a maximum specific capacitance of 161 F g-1 was obtained at 5 A g-1 current density, accompanied with an energy density of 4.53 W h kg-1 at a steady power delivery rate of 1125 W kg-1. The high utility of the pseudocapacitive NiMoO4.nH2O was achieved in its graphene

Synthesis and characterization of nanostructured CaSiO3 biomaterial

NASA Astrophysics Data System (ADS)

Jagadale, Pramod N.; Kulal, Shivaji R.; Joshi, Meghanath G.; Jagtap, Pramod P.; Khetre, Sanjay M.; Bamane, Sambhaji R.

2013-04-01

Here we report a successful preparation of nanostructured calcium silicate by wet chemical approach. The synthesized sample was characterized by various physico-chemical methods. Thermal stability was investigated using thermo-gravimetric and differential thermal analysis (TG-DTA). Structural characterization of the sample was carried out by the X-ray diffraction technique (XRD) which confirmed its single phase hexagonal structure. Transmission electron microscopy (TEM) was used to study the nanostructure of the ceramics while homogeneous grain distribution was revealed by scanning electron microscopy studies (SEM). The elemental analysis data obtained from energy dispersive X-ray spectroscopy (EDAX) were in close agreement with the starting composition used for the synthesis. Superhydrophilic nature of CaSiO3 was investigated at room temperature by sessile drop technique. Effect of porous nanosized CaSiO3 on early adhesion and proliferation of human bone marrow mesenchymal stem cells (BMMSCs) and cord blood mesenchymal stem (CBMSCs) cells was measured in vitro. MTT cytotoxicity test and cell adhesion test showed that the material had good biocompatibility and promoted cell viability and cell proliferation. It has been stated that the cell viability and proliferation are significantly affected by time and concentration of CaSiO3. These findings indicate that the CaSiO3 ceramics has good biocompatibility and that it is promising as a biomaterial.

Protocol for the Solid-phase Synthesis of Oligomers of RNA Containing a 2'-O-thiophenylmethyl Modification and Characterization via Circular Dichroism.

PubMed

Francis, Andrew J; Resendiz, Marino J E

2017-07-28

Solid-phase synthesis has been used to obtain canonical and modified polymers of nucleic acids, specifically of DNA or RNA, which has made it a popular methodology for applications in various fields and for different research purposes. The procedure described herein focuses on the synthesis, purification, and characterization of dodecamers of RNA 5'-[CUA CGG AAU CAU]-3' containing zero, one, or two modifications located at the C2'-O-position. The probes are based on 2-thiophenylmethyl groups, incorporated into RNA nucleotides via standard organic synthesis and introduced into the corresponding oligonucleotides via their respective phosphoramidites. This report makes use of phosphoramidite chemistry via the four canonical nucleobases (Uridine (U), Cytosine (C), Guanosine (G), Adenosine (A)), as well as 2-thiophenylmethyl functionalized nucleotides modified at the 2'-O-position; however, the methodology is amenable for a large variety of modifications that have been developed over the years. The oligonucleotides were synthesized on a controlled-pore glass (CPG) support followed by cleavage from the resin and deprotection under standard conditions, i.e., a mixture of ammonia and methylamine (AMA) followed by hydrogen fluoride/triethylamine/N-methylpyrrolidinone. The corresponding oligonucleotides were purified via polyacrylamide electrophoresis (20% denaturing) followed by elution, desalting, and isolation via reversed-phase chromatography (Sep-pak, C18-column). Quantification and structural parameters were assessed via ultraviolet-visible (UV-vis) and circular dichroism (CD) photometric analysis, respectively. This report aims to serve as a resource and guide for beginner and expert researchers interested in embarking in this field. It is expected to serve as a work-in-progress as new technologies and methodologies are developed. The description of the methodologies and techniques within this document correspond to a DNA/RNA synthesizer (refurbished and purchased in

Electrodeposition synthesis and electrochemical properties of nanostructured γ-MnO 2 films

NASA Astrophysics Data System (ADS)

Chou, Shulei; Cheng, Fangyi; Chen, Jun

The thin films of carambola-like γ-MnO 2 nanoflakes with about 20 nm in thickness and at least 200 nm in width were prepared on nickel sheets by combination of potentiostatic and cyclic voltammetric electrodeposition techniques. The as-prepared MnO 2 nanomaterials, which were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), were used as the active material of the positive electrode for primary alkaline Zn/MnO 2 batteries and electrochemical supercapacitors. Electrochemical measurements showed that the MnO 2 nanoflake films displayed high potential plateau (around 1.0 V versus Zn) in primary Zn/MnO 2 batteries at the discharge current density of 500 mA g -1 and high specific capacitance of 240 F g -1 at the current density of 1 mA cm -2. This indicated the potential application of carambola-like γ-MnO 2 nanoflakes in high-power batteries and electrochemical supercapacitors. The growth process for the one- and three-dimensional nanostructured MnO 2 was discussed on the basis of potentiostatic and cyclic voltammetric techniques. The present synthesis method can be extended to the preparation of other nanostructured metal-oxide films.

Synthesis of polycarbonate-r-polyethylene glycol copolymer for templated synthesis of mesoporous TiO2 films.

PubMed

Patel, Rajkumar; Kim, Jinkyu; Lee, Chang Soo; Kim, Jong Hak

2014-12-01

We synthesized a novel polycarbonate Z-r-polyethylene glycol (PCZ-r-PEG) copolymer by solution polycondensation. Successful synthesis of PCZ-r-PEG copolymer was confirmed by Fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (1H-NMR), gel permeation chromatography (GPC), and transmission electron microscopy (TEM). PCZ-r-PEG copolymer was used as a structure-directing agent for fabrication of mesoporous thin film containing a titanium dioxide (TiO2) layer. To control the porosity of the resultant inorganic layer, the ratio of titanium(IV) isopropoxide (TTIP) to PCZ-r-PEG copolymer was varied. The structure and porosity of the resulting mesoporous films were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) analyses. Mesoporous TiO2 films fabricated on an F-doped tin oxide (FTO) surface were used as photoanodes for quasi-solid-state dye-sensitized solar cells (qssDSSCs). The highest efficiency achieved was 3.3% at 100 mW/cm2 for a film thickness of 750 nm, which is high considering the thickness of TiO2 film, indicating the importance of the structure-directing agent.

Synthesis of reduced graphene oxide-anatase TiO2 nanocomposite and its improved photo-induced charge transfer properties.

PubMed

Wang, Ping; Zhai, Yueming; Wang, Dejun; Dong, Shaojun

2011-04-01

The construction of reduced graphene oxide or graphene oxide with semiconductor has gained more and more attention due to its unexpected optoelectronic and electronic properties. The synthesis of reduced graphene oxide (RGO) or graphene oxide-semiconductor nanocomposite with well-dispersed decorated particles is still a challenge now. Herein, we demonstrate a facile method for the synthesis of graphene oxide-amorphous TiO(2) and reduced graphene oxide-anatase TiO(2) nanocomposites with well-dispersed particles. The as-synthesized samples were characterized by transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, UV-Vis absorption spectroscopy, Fourier transform infrared spectrometry, and thermogravimetric analysis. The photovoltaic properties of RGO-anatase TiO(2) were also compared with that of similar sized anatase TiO(2) by transient photovoltage technique, and it was interesting to find that the combination of reduced graphene oxide with anatase TiO(2) will significantly increase the photovoltaic response and retard the recombination of electron-hole pairs in the excited anatase TiO(2).

Synthesis, characterization, and antibacterial activities of ZnLaFe2O4/NiTiO3 nanocomposite

NASA Astrophysics Data System (ADS)

Sobhani-Nasab, Ali; Zahraei, Zohreh; Akbari, Maryam; Maddahfar, Mahnaz; Hosseinpour-Mashkani, S. Mostafa

2017-07-01

In this research, for the first time, ZnLaFe2O4/NiTiO3 nanocomposites have been synthesized through a polyol assistant sol-gel method. To investigate the effect of different surfactants on the morphology and particle size of ZnLaFe2O4 nanostructure, cetrimonium bromide, sodium dodecyl sulfate, polyvinylpyrrolidone, polyvinyl alcohol, and oleic acid were used as surfactant agents. Based on the SEM results, it was found that morphology and particle size of the products could be affected by these surfactants. Furthermore, study on antibacterial effect of ZnLaFe2O4/NiTiO3 nanocomposites by colony forming unit (CFU) reduction assay showed that ZnLaFe2O4/NiTiO3 nanocomposites have antibacterial activity against Gram-negative Escherchia coli (ATCC 10536) and Gram-positive Staphylococcus aureus (ATCC 29737). Antibacterial results demonstrate that nanocomposite significantly reduced the growth rate of E. coli bacteria and S. aureus after 120 min. The structure and morphology of the resulting particles were characterized by XRD, FT-IR, EDX, and SEM analysis.

Synthesis, characterization and adsorptive performance of MgFe2O4 nanospheres for SO2 removal.

PubMed

Zhao, Ling; Li, Xinyong; Zhao, Qidong; Qu, Zhenping; Yuan, Deling; Liu, Shaomin; Hu, Xijun; Chen, Guohua

2010-12-15

A type of uniform Mg ferrite nanospheres with excellent SO(2) adsorption capacity could be selectively synthesized via a facile solvothermal method. The size of the MgFe(2)O(4) nanospheres was controlled to be 300-400 nm in diameter. The structural, textural, and surface properties of the adsorbent have been fully characterized by a variety of techniques (Brunauer-Emmett-Teller, BET; X-ray diffraction analysis, XRD; scanning electron microscopy, SEM; and energy-dispersive X-ray spectroscopy, EDS). The valence states and the surface chemical compositions of MgFe(2)O(4) nanospheres were further identified by X-ray photoelectron spectroscopy (XPS). The behaviors of SO(2) oxidative adsorption on MgFe(2)O(4) nanospheres were studied using Fourier transform infrared spectroscopy (FTIR). Both the sulfite and sulfate species could be formed on the surface of MgFe(2)O(4). The adsorption equilibrium isotherm of SO(2) was analyzed using a volumetric method at 298 K and 473 K. The results indicate that MgFe(2)O(4) nanospheres possess a good potential as the solid-state SO(2) adsorbent for applications in hot fuel gas desulfurization. Copyright © 2010 Elsevier B.V. All rights reserved.

Synthesis and atomic scale characterization of Er2O3 nanoparticles: enhancement of magnetic properties and changes in the local structure

NASA Astrophysics Data System (ADS)

Corrêa, Eduardo L.; Bosch-Santos, Brianna; Freitas, Rafael S.; Potiens, Maria da Penha A.; Saiki, Mitiko; Carbonari, Artur W.

2018-05-01

In the investigation reported in this paper a modified thermal decomposition method was developed to produce very small Er2O3 nanoparticles (NPs). Particles structure, shape and size were characterized by x-ray diffraction and transmission electron microscopy which showed that the synthesis by thermal decomposition under O2 atmosphere produced very small and monodisperse NPs, allowing the investigation of finite-size and surface effects. Results of magnetization measurements showed that the smallest particles present the highest values of susceptibility that decrease as particle size increases. Specific heat measurements indicate that the sample with the smallest NPs (diameter ∼5 nm) has a Néel temperature of 0.54 K. The local structure of particles was investigated by measurements of hyperfine interactions with perturbed angular correlation spectroscopy using 111Cd as probe nuclei replacing the cationic sites. Results showed that the relative population of sites 8b increases in both the core and surface layer of particles.

Synthesis and atomic scale characterization of Er2O3 nanoparticles: enhancement of magnetic properties and changes in the local structure.

PubMed

Corrêa, Eduardo L; Bosch-Santos, Brianna; Freitas, Rafael S; da Penha A Potiens, Maria; Saiki, Mitiko; Carbonari, Artur W

2018-05-18

In the investigation reported in this paper a modified thermal decomposition method was developed to produce very small Er 2 O 3 nanoparticles (NPs). Particles structure, shape and size were characterized by x-ray diffraction and transmission electron microscopy which showed that the synthesis by thermal decomposition under O 2 atmosphere produced very small and monodisperse NPs, allowing the investigation of finite-size and surface effects. Results of magnetization measurements showed that the smallest particles present the highest values of susceptibility that decrease as particle size increases. Specific heat measurements indicate that the sample with the smallest NPs (diameter ∼5 nm) has a Néel temperature of 0.54 K. The local structure of particles was investigated by measurements of hyperfine interactions with perturbed angular correlation spectroscopy using 111 Cd as probe nuclei replacing the cationic sites. Results showed that the relative population of sites 8b increases in both the core and surface layer of particles.

Uniform TiO2-SiO2 hollow nanospheres: Synthesis, characterization and enhanced adsorption-photodegradation of azo dyes and phenol

NASA Astrophysics Data System (ADS)

Guo, Na; Liang, Yimai; Lan, Shi; Liu, Lu; Ji, Guijuan; Gan, Shucai; Zou, Haifeng; Xu, Xuechun

2014-06-01

TiO2-SiO2 hollow nanospheres with remarkable enhanced photocatalytic performance have been fabricated by sol-gel method. The hollow sphere possesses both high phototcatalytic activity and adsorption capability. The as-prepared samples were characterized by XRD, SEM, TEM, FTIR, XPS, BJH and TGA/DSC. The experiment results show that, the photocatalyst calcined at 500 °C with Ti/Si ratio of 5:1 (denoted as 5T/S-500) displayed superiorities in both textural and functional properties with the enhanced degradation efficiency on azo dyes (methylene blue, methyl orange) and phenol. The high adsorption capability of organic poisonous contaminants onto 5T/S-500 in aqueous solution demonstrated that the photocatalyst can remove the contaminants from water effectively even without illumination. The TEM and SEM morphologies demonstrated unique hollow and coarse structure of 5T/S-500. Structural analysis showed that Si was doped into the lattice of TiO2 and SiO2 nanoparticles can work as a surface modifier on TiO2. The surface area of 5T/S-500 is 1105 m2/g, 14.5 times as great as that of the pure hollow TiO2 nanosphere, confirms the effect of SiO2 on the improvement of specific surface area. The high photocatalytic activities and high adsorption ability for organic poisonous contaminants demonstrate that the nanocomposite of TiO2-SiO2 is a promising candidate material for future treatment of contaminated water.

Synthesis of In2O3nanoparticles by thermal decomposition of a citrate gel precursor

NASA Astrophysics Data System (ADS)

Rey, J. F. Q.; Plivelic, T. S.; Rocha, R. A.; Tadokoro, S. K.; Torriani, I.; Muccillo, E. N. S.

2005-06-01

This paper describes the synthesis of indium oxide by a modified sol-gel method, and the study of thermal decomposition of the metal complex in air. The characterization of the intermediate as well as the final compounds was carried out by thermogravimetry, differential thermal analysis, Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and small angle X-ray scattering. The results show that the indium complex decomposes to In2O3 with the formation of an intermediate compound. Nanoparticles of cubic In2O3 with crystallite sizes in the nanosize range were formed after calcination at temperatures up to 900°C. Calcined materials are characterized by a polydisperse distribution of spherical particles with sharp and smooth surfaces.

Phosphorous-doped TiO2 nanoparticles: synthesis, characterization, and visible photocatalytic evaluation on sulfamethazine degradation.

PubMed

Mendiola-Alvarez, Sandra Yadira; Hernández-Ramírez, Ma Aracely; Guzmán-Mar, Jorge Luis; Garza-Tovar, Lorena Leticia; Hinojosa-Reyes, Laura

2018-05-24

Mesoporous phosphorous-doped TiO 2 (TP) with different wt% of P (0.5, 1.0, and 1.5) was synthetized by microwave-assisted sol-gel method. The obtained materials were characterized by XRD with cell parameters refinement approach, Raman, BET-specific surface area analysis, SEM, ICP-OES, UV-Vis with diffuse reflectance, photoluminescence, FTIR, and XPS. The photocatalytic activity under visible light was evaluated on the degradation of sulfamethazine (SMTZ) at pH 8. The characterization of the phosphorous materials (TP) showed that incorporation of P in the lattice of TiO 2 stabilizes the anatase crystalline phase, even increasing the annealing temperature. The mesoporous P-doped materials showed higher surface area and lower average crystallite size, band gap, and particle size; besides, more intense bands attributed to O-H bond were observed by FTIR analysis compared with bare TiO 2 . The P was substitutionally incorporated in the TiO 2 lattice network as P 5+ replacing Ti 4+ to form Ti-O-P bonds and additionally present as PO 4 3-  on the TiO 2 surface. All these characteristics explain the observed superior photocatalytic activity on degradation (100%) and mineralization (32%) of SMTZ under visible radiation by TP catalysts, especially for P-doped TiO 2 1.0 wt% calcined at 450 °C (TP1.0-450). Ammonium, nitrate, and sulfate ions released during the photocatalytic degradation were quantified by ion chromatography; the nitrogen and sulfur mass balance evidenced the partial mineralization of this recalcitrant molecule.

Synthesis of MnFe2O4 magnetic nano hollow spheres by a facile solvothermal route and its characterization

NASA Astrophysics Data System (ADS)

Dey, Chaitali; Chaudhuri, Arka; Goswami, Madhuri Mandal

2018-04-01

Herein, we report the synthesis of manganese ferrite (MnFe2O4) magnetic nano hollow sphere (NHS) by a solvothermal route. Crystalline phase was confirmed by X-ray diffraction (XRD), energy dispersive x-ray (EDX). Magnetic measurements were done in vibrating sample magnetometer (VSM) and morphological structure was analyzed by field emission high resolution scanning electron microscope (FESEM) and structural characterization was confirmed by Fourier transform infrared spectroscopy (FTIR), thermal analysis was performed by thermo-gravimetric analysis-differential thermal analysis (TGA-DTA). The size of the NHS was around 470 nm, this large size may show a potential applicability in industrial application, like dye adsorption, catalysis etc. In addition, because of its ferromagnetic character at room temperature, it can be easily separated by external magnetic field after the application is done.

Synthesis and characterization of TiO2 loaded cashew nut shell activated carbon and photocatalytic activity on BG and MB dyes under sunlight radiation

NASA Astrophysics Data System (ADS)

Ragupathy, S.; Raghu, K.; Prabu, P.

2015-03-01

Synthesis of titanium dioxide (TiO2) nanoparticles and TiO2 loaded cashew nut shell activated carbon (TiO2/CNSAC) had been undertaken using sol-gel method and their application in BG and MB dyes removal under sunlight radiation has been investigated. The synthesized photocatalysts were characterized by X-ray diffraction analysis (XRD), Fourier infra-red spectroscopy (FT-IR), UV-Vis-diffuse reflectance spectroscopy (DRS) and scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX). The various experimental parameters like amount of catalyst, contact time for efficient dyes degradation of BG and MB were concerned in this study. Activity measurements performed under solar irradiation has shown good results for the photodegradation of BG and MB in aqueous solution. It was concluded that the higher photocatalytic activity in TiO2/CNSAC was due to parameters like band-gap, number of hydroxyl groups, surface area and porosity of the catalyst. The kinetic data were also described by the pseudo-first-order and pseudo-second-order kinetic models.

Synthesis and characterization of TiO2 loaded cashew nut shell activated carbon and photocatalytic activity on BG and MB dyes under sunlight radiation.

PubMed

Ragupathy, S; Raghu, K; Prabu, P

2015-03-05

Synthesis of titanium dioxide (TiO2) nanoparticles and TiO2 loaded cashew nut shell activated carbon (TiO2/CNSAC) had been undertaken using sol-gel method and their application in BG and MB dyes removal under sunlight radiation has been investigated. The synthesized photocatalysts were characterized by X-ray diffraction analysis (XRD), Fourier infra-red spectroscopy (FT-IR), UV-Vis-diffuse reflectance spectroscopy (DRS) and scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX). The various experimental parameters like amount of catalyst, contact time for efficient dyes degradation of BG and MB were concerned in this study. Activity measurements performed under solar irradiation has shown good results for the photodegradation of BG and MB in aqueous solution. It was concluded that the higher photocatalytic activity in TiO2/CNSAC was due to parameters like band-gap, number of hydroxyl groups, surface area and porosity of the catalyst. The kinetic data were also described by the pseudo-first-order and pseudo-second-order kinetic models. Copyright © 2014 Elsevier B.V. All rights reserved.

Synthesis and characterization of nano TiO2-SiO2: PVA composite - a novel route

NASA Astrophysics Data System (ADS)

Venckatesh, Rajendran; Balachandaran, Kartha; Sivaraj, Rajeshwari

2012-07-01

A novel, simple, less time consuming and cost-effective sol-gel method has been developed to synthesize nano titania-silica with polyvinyl alcohol (PVA) composite relatively at low temperature in acidic pH. Titania sol is prepared by hydrolysis of titanium tetrachloride and was mixed with silicic acid and tetrahydrofuran mixture. The reaction was carried out under vigorous stirring for 6 h and dried at room temperature with the addition of PVA solution. The resulting powders were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared (FT-IR), UV-visible spectroscopy and thermal techniques. The grain size of the particles was calculated by X-ray diffraction; surface morphology and chemical composition were determined from scanning electron microscopy-energy dispersive spectroscopy; metal oxide stretching was confirmed from FT-IR spectroscopy; bandgap was calculated using UV-visible spectroscopy, and thermal stability of the prepared composite was determined by thermogravimetric/differential thermal analysis. Since TiO2 got agglomerated on the surface of SiO2, effective absorptive sites increase which in turn increase the photocatalytic efficiency of the resulting composite.

Micelle-Assisted Synthesis of Al2O3 ·CaO Nanocatalyst: Optical Properties and Their Applications in Photodegradation of 2,4,6-Trinitrophenol

PubMed Central

Imtiaz, Ayesha; Khaleeq-ur-rahman, Muhammad; Adnan, Rohana

2013-01-01

Calcium oxide (CaO) nanoparticles are known to exhibit unique property due to their high adsorption capacity and good catalytic activity. In this work the CaO nanocatalysts were prepared by hydrothermal method using anionic surfactant, sodium dodecyl sulphate (SDS), as a templating agent. The as-synthesized nanocatalysts were further used as substrate for the synthesis of alumina doped calcium oxide (Al2O3 ·CaO) nanocatalysts via deposition-precipitation method at the isoelectric point of CaO. The Al2O3 ·CaO nanocatalysts were characterized by FTIR, XRD, TGA, TEM, and FESEM techniques. The catalytic efficiencies of these nanocatalysts were studied for the photodegradation of 2,4,6-trinitrophenol (2,4,6-TNP), which is an industrial pollutant, spectrophotometrically. The effect of surfactant and temperature on size of nanocatalysts was also studied. The smallest particle size and highest percentage of degradation were observed at critical micelle concentration of the surfactant. The direct optical band gap of the Al2O3 ·CaO nanocatalyst was found as 3.3 eV. PMID:24311980

Synthesis and characterization of maleimide-functionalized polystyrene-SiO2/TiO2 hybrid nanocomposites by sol-gel process

NASA Astrophysics Data System (ADS)

Ramesh, Sivalingam; Sivasamy, Arumugam; Kim, Joo-Hyung

2012-06-01

Maleimide-functionalized polystyrene (PSMA-SiO2/TiO2) hybrid nanocomposites were prepared by sol-gel reaction starting from tratraethoxysilane (TEOS) and titanium isopropoxide in the solution of polystyrene maleimide in 1,4-dioxane. The hybrid films were obtained by the hydrolysis and polycondensation of TEOS and titanium isopropoxide in maleimide-functionalized polystyrene solution followed by the Michael addition reaction. The transparency of polymer (PSMA-SiO2/TiO2) hybrid was prepared from polystyrene titanium isopropoxide using the γ-aminopropyltriethoxy silane as crosslinking agent by in situ sol-gel process via covalent bonding between the organic-inorganic hybrid nanocomposites. The maleimide-functionalized polystyrene was synthesized by Friedel-Crafts reaction from N-choloromethyl maleimide. The FTIR spectroscopy data conformed the occurrence of Michael addition reaction between the pendant maleimide moieties of the styrene and γ-aminopropyltriethoxysilane. The chemical structure and morphology of PSMA-SiO2/TiO2 hybrid nanocomposites were characterized by FTIR, nuclear magnetic resonance (NMR), 13 C NMR, SEM, XRD, and TEM analyses. The results also indicate that the inorganic particles are much smaller in the ternary systems than in the binary systems; the shape of the inorganic particles and compatibility for maleimide-functionalized polystrene and inorganic moieties are varied with the ratio of the inorganic moieties in the hybrids. Furthermore, TGA and DSC results indicate that the thermal stability of maleimide-functionalized polystyrene was enhanced through the incorporation of the inorganic moieties in the hybrid materials.

2D SnO2 Nanosheets: Synthesis, Characterization, Structures, and Excellent Sensing Performance to Ethylene Glycol

PubMed Central

Wan, Wenjin; Li, Yuehua; Ren, Xingping; Zhao, Yinping; Gao, Fan; Zhao, Heyun

2018-01-01

Two dimensional (2D)SnO2 nanosheets were synthesized by a substrate-free hydrothermal route using sodium stannate and sodium hydroxide in a mixed solvent of absolute ethanol and deionized water at a lower temperature of 130 °C. The characterization results of the morphology, microstructure, and surface properties of the as-prepared products demonstrated that SnO2 nanosheets with a tetragonal rutile structure, were composed of oriented SnO2 nanoparticles with a diameter of 6–12 nm. The X-ray diffraction (XRD) and high-resolution transmission electron microscope (FETEM) results demonstrated that the dominant exposed surface of the SnO2 nanoparticles was (101), but not (110). The growth and formation was supposed to follow the oriented attachment mechanism. The SnO2 nanosheets exhibited an excellent sensing response toward ethylene glycol at a lower optimal operating voltage of 3.4 V. The response to 400 ppm ethylene glycol reaches 395 at 3.4 V. Even under the low concentration of 5, 10, and 20 ppm, the sensor exhibited a high response of 6.9, 7.8, and 12.0 to ethylene glycol, respectively. The response of the SnO2 nanosheets exhibited a linear dependence on the ethylene glycol concentration from 5 to 1000 ppm. The excellent sensing performance was attributed to the present SnO2 nanoparticles with small size close to the Debye length, the larger specific surface, the high-energy exposed facets of the (101) surface, and the synergistic effects of the SnO2 nanoparticles of the nanosheets. PMID:29462938

Synthesis of hectorite-TiO2 and kaolinite-TiO2 nanocomposites with photocatalytic activity for the degradation of model air pollutants

DOE Office of Scientific and Technical Information (OSTI.GOV)

Destaillats, Hugo; Kibanova, D.; Trejo, M.

2008-03-01

We studied the synthesis and photocatalytic activity of small-sized TiO{sub 2} supported on hectorite and kaolinite. Deposition of TiO{sub 2} on the clay mineral surface was conducted by using a sol-gel method with titanium isopropoxide as precursor. Anatase TiO{sub 2} particles formation was achieved by hydrothermal treatment at 180 C. Material characterization was conducted using XRD, SEM, XPS, ICP-OES, BET and porosimetry analysis. Efficiency in synthesizing clay-TiO{sub 2} composites depended strongly on the clay mineral structure. Incorporation of anatase in hectorite, an expandable clay mineral, was found to be very significant (> 36 wt.% Ti) and to be followed bymore » important structural changes at the clay mineral surface. Instead, no major structural modifications of the clay were observed for kaolinite-TiO{sub 2}, as compared with the untreated material. Photocatalytic performance of clay-TiO{sub 2} composites was evaluated with ATR-FTIR following the oxidation of adsorbed toluene and d-limonene, two model air pollutants. In either case, the photocatalytic removal efficiency of these hydrophobic substrates by the synthesized clay-TiO{sub 2} composites was comparable to that observed using pure commercial TiO{sub 2} (Degussa P25).« less

Synthesis and characterization of a pH-sensitive conjugate of isoniazid with Fe3O4@SiO2 magnetic nanoparticles.

PubMed

Sedlák, Miloš; Bhosale, Dattatry Shivajirao; Beneš, Ludvík; Palarčík, Jiří; Kalendová, Andrea; Královec, Karel; Imramovský, Aleš

2013-08-15

The Letter describes the preparation and characterization of a conjugate of isoniazid (INH) with magnetic nanoparticles Fe3O4@SiO2 115±60 nm in size. The INH molecules were attached to the surface of nanoparticles by a covalent pH-sensitive amidine bond. The conjugate was characterized by X-ray diffraction, SEM, dynamic light scattering, IR spectroscopy and microanalysis. The conjugate released isoniazid under in vitro conditions (pH=4; 37 °C; t1/2≈115 s). In addition, the cytotoxicity of the Fe3O4@SiO2-INH conjugate was evaluated in SK-BR-3 cells using the xCELLigence system. Copyright © 2013 Elsevier Ltd. All rights reserved.

A Green Protocol for Synthesis of MAl2O4, [M=Cu and Co] Spinels Under Microwave Irradiation Method

NASA Astrophysics Data System (ADS)

Yuvasravana, R.; George, P. P.

Nanosized metal aluminates MAl2O4, [M=Cu and Co] are synthesized from their nitrates solution by using pomegranate peel extract as fuel in microwave combustion. MAl2O4 [M=Cu and Co] nanoparticles are grown in microwave assisted synthesis followed by annealing at 700∘C. The nanoparticles have been characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), UV-VIS spectroscopy and photoluminescence (PL) spectroscopy. The PXRD analysis has confirmed their spinel composition. The green protocol and microwave combustion route for spinel synthesis are rapid, simple, without any hazardous chemicals as reducing or stabilizing agents and economical.

Synthesis, characterization, and photocatalytic application of Pd/ZrO2 and Pt/ZrO2

NASA Astrophysics Data System (ADS)

Saeed, Khalid; Sadiq, Mohammad; Khan, Idrees; Ullah, Saleem; Ali, Nauman; Khan, Adnan

2018-05-01

Zirconia-supported palladium (Pd/ZrO2) and Zirconia-supported platinum (Pt/ZrO2) nanoparticles (NPs) are synthesized from their precursors via impregnation technique. The Pd/ZrO2 and Pt/ZrO2 NPs were analyzed via SEM and EDX, while the study of indigo disulfonate dye degradation was carried out by UV/VIS spectrophotometer. The SEM micrographs illustrated that the Pd and Pt NPs were well placed on ZrO2 surface. The Pd/ZrO2 and Pt/ZrO2 NPs were also employed as photocatalysts for the photodegradation of indigo disulfonate in an aqueous medium under UV-light irradiation. The photodegradation study presented that Pd/ZrO2 and Pt/ZrO2 NPs degraded 96 and 94% of indigo disulfonate in 14 h, respectively. The effect of pH of medium and catalyst dosage and efficiency of recovered Pd/ZrO2 and Pt/ZrO2 NPs on the photocatalytic degradation were also studied. It was also found that the maximum degradation of dye was found at pH 10 (95-97%) and at 0.02 g weight (40.28%).

Synthesis of Ordered Mesoporous CuO/CeO2 Composite Frameworks as Anode Catalysts for Water Oxidation

PubMed Central

Markoulaki, Vassiliki Ι.; Papadas, Ioannis T.; Kornarakis, Ioannis; Armatas, Gerasimos S.

2015-01-01

Cerium-rich metal oxide materials have recently emerged as promising candidates for the photocatalytic oxygen evolution reaction (OER). In this article, we report the synthesis of ordered mesoporous CuO/CeO2 composite frameworks with different contents of copper(II) oxide and demonstrate their activity for photocatalytic O2 production via UV-Vis light-driven oxidation of water. Mesoporous CuO/CeO2 materials have been successfully prepared by a nanocasting route, using mesoporous silica as a rigid template. X-ray diffraction, electron transmission microscopy and N2 porosimetry characterization of the as-prepared products reveal a mesoporous structure composed of parallel arranged nanorods, with a large surface area and a narrow pore size distribution. The molecular structure and optical properties of the composite materials were investigated with Raman and UV-Vis/NIR diffuse reflectance spectroscopy. Catalytic results indicated that incorporation of CuO clusters in the CeO2 lattice improved the photochemical properties. As a result, the CuO/CeO2 composite catalyst containing ~38 wt % CuO reaches a high O2 evolution rate of ~19.6 µmol·h−1 (or 392 µmol·h−1·g−1) with an apparent quantum efficiency of 17.6% at λ = 365 ± 10 nm. This OER activity compares favorably with that obtained from the non-porous CuO/CeO2 counterpart (~1.3 µmol·h−1) and pure mesoporous CeO2 (~1 µmol·h−1). PMID:28347106

Synthesis and characterization of Nafion/TiO2 nanocomposite membrane for proton exchange membrane fuel cell.

PubMed

Kim, Tae Young; Cho, Sung Yong

2011-08-01

In this study, the syntheses and characterizations of Nafion/TiO2 membranes for a proton exchange membrane fuel cell (PEMFC) were investigated. Porous TiO2 powders were synthesized using the sol-gel method; with Nafion/TiO2 nanocomposite membranes prepared using the casting method. An X-ray diffraction analysis demonstrated that the synthesized TiO2 had an anatase structure. The specific surface areas of the TiO2 and Nafion/TiO2 nanocomposite membrane were found to be 115.97 and 33.91 m2/g using a nitrogen adsorption analyzer. The energy dispersive spectra analysis indicated that the TiO2 particles were uniformly distributed in the nanocomposite membrane. The membrane electrode assembly prepared from the Nafion/TiO2 nanocomposite membrane gave the best PEMFC performance compared to the Nafion/P-25 and Nafion membranes.

One pot synthesis of CdS/TiO{sub 2} hetero-nanostructures for enhanced H{sub 2} production from water and removal of pollutants from aqueous streams

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mani, A. Daya; Subrahmanyam, Ch., E-mail: csubbu@iith.ac.in

2016-01-15

Highlights: • Novel one pot synthesis of CdS/TiO{sub 2} hetero nanostructures by combustion synthesis. • Excellent visible light photocatalytic activity for H{sub 2} production from water. • Enhanced activity for the removal of Cr(VI) from aqueous streams. - Abstract: To achieve more effective coupling of cadmium sulfide (CdS) to the TiO{sub 2}, single step synthesis of CdS/TiO{sub 2} composites is advantageous. In the present study a novel one pot synthesis of several CdS/TiO{sub 2} hetero-nanostructures was explored through combustion technique. As the process involves the simultaneous nucleation of CdS and TiO{sub 2} it leads to the proper connectivity between themore » constituent materials. All the catalysts were characterized by using several techniques and the excellent visible light activity of the composites has been asserted by the H{sub 2} production from water containing sacrificial reagents, removal of methylene blue and Cr(VI) from aqueous streams. Therefore the present synthetic strategy which is devoid of using molecular linker at interface is more suitable for solar applications, which require faster rates of electron transfer at the hetero junctions.« less

Synthesis and characterization of (Sn,Zn)O alloys

DOE PAGES

Bikowski, Andre; Holder, Aaron; Peng, Haowei; ...

2016-09-29

SnO exhibits electrical properties that render it promising for solar energy conversion applications, but it also has a strongly indirect band gap. Recent theoretical calculations predict that this disadvantage can be mitigated by isovalent alloying with other group-II oxides such as ZnO. Here, we synthesized new metastable isovalent (Sn,Zn)O alloy thin films by combinatorial reactive co-sputtering and characterized their structural, optical and electrical properties. The alloying of ZnO into SnO leads to a change of the valence state of the tin from Sn 0 via Sn 2+ to Sn 4+, which can be counteracted by reducing the oxygen partial pressuremore » during the deposition. The optical characterization of the smooth <10 at. % Sn 1-xZn xO thin films showed an increase in the absorption coefficient in the range from 1 to 2 eV, which is consistent with the theoretical predictions for the isovalent alloying. However, the experimentally observed alloying effect may be convoluted with the effect of local variations of the Sn oxidation state. As a result, this effect would have to be minimized to improve the (Sn,Zn)O optical and electrical properties for their use as absorbers in solar energy conversion applications.« less

Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

NASA Astrophysics Data System (ADS)

Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

2011-11-01

The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO2) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO2). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO2/TiO2) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO2-Degussa P25 catalyst is detected.

Synthesis and Characterization of Thin Film Lithium-Ion Batteries Using Polymer Electrolytes

NASA Technical Reports Server (NTRS)

Maranchi, Jeffrey P.; Kumta, Prashant N.; Hepp, Aloysius F.; Raffaelle, Ryne P.

2002-01-01

The present paper describes the integration of thin film electrodes with polymer electrolytes to form a complete thin film lithium-ion battery. Thin film batteries of the type, LiCoO2 [PAN, EC, PC, LiN(CF3SO2)2] SnO2 have been fabricated. The results of the synthesis and characterization studies will be presented and discussed.

Synthesis and Characterization of Highly Intercalated Graphite Bisulfate.

PubMed

Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

2017-12-01

Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy (μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO 4 , K 2 Cr 2 O 7 ) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO 4 and NaClO 3 .

Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

NASA Astrophysics Data System (ADS)

Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

2017-03-01

Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.

Synthesis, characterization, and magnetic properties of ZnO-ZnFe2O4 nanoparticles with high photocatalytic activity

NASA Astrophysics Data System (ADS)

Falak, P.; Hassanzadeh-Tabrizi, S. A.; Saffar-Teluri, A.

2017-11-01

In the present research, a magnetic ZnO-ZnFe2O4 binary nanocomposite was synthesized by a one-step microemulsion method. The characteristics of the synthesized powders were characterized using various analytical instruments including X-ray diffraction, scanning electron microscope, transmission electron microscope, thermogravimetric and differential thermal analysis, vibrating sample magnetometer, and ultraviolet-visible spectroscopy. The results of transmission electron microscope proved that the synthesized nanoparticles have irregular morphologies and the average particle size is about 20 nm. The photocatalytic investigation of ZnO-ZnFe2O4 nanoparticles was carried out using methylene blue solution under UV light. The synthesized nanoparticles showed enhanced photocatalytic performance in comparison with the ZnO nanoparticles more than 40%. The magnetization saturation value of ZnO-ZnFe2O4 nanoparticles was about 5.8 emu/g, which was high enough to be magnetically removed by applying a magnetic field. The results showed that the magnetization and coercivity of the samples reduced by increasing calcination temperature.

Size-Selective Synthesis and Stabilization of Small Silver Nanoparticles on TiO 2 Partially Masked by SiO 2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bo, Zhenyu; Eaton, Todd R.; Gallagher, James R.

Controlling metal nanoparticle size is one of the principle challenges in developing new supported catalysts. Typical methods where a metal salt is deposited and reduced can result in a polydisperse mixture of metal nanoparticles, especially at higher loading. Polydispersity can exacerbate the already significant challenge of controlling sintering at high temperatures, which decreases catalytic surface area. Here, we demonstrate the size-selective photoreduction of Ag nanoparticles on TiO2 whose surface has been partially masked with a thin SiO2 layer. To synthesize this layered oxide material, TiO2 particles are grafted with tert-butylcalix[4]arene molecular templates (~2 nm in diameter) at surface densities ofmore » 0.05–0.17 templates.nm–2, overcoated with ~2 nm of SiO2 through repeated condensation cycles of limiting amounts of tetraethoxysilane (TEOS), and the templates are removed oxidatively. Ag photodeposition results in uniform nanoparticle diameters ≤ 3.5 nm (by transmission electron microscopy (TEM)) on the partially masked TiO2, whereas Ag nanoparticles deposited on the unmodified TiO2 are larger and more polydisperse (4.7 ± 2.7 nm by TEM). Furthermore, Ag nanoparticles on the partially masked TiO2 do not sinter after heating at 450 °C for 3 h, while nanoparticles on the control surfaces sinter and grow by at least 30%, as is typical. Overall, this new synthesis approach controls metal nanoparticle dispersion and enhances thermal stability, and this facile synthesis procedure is generalizable to other TiO2-supported nanoparticles and sizes and may find use in the synthesis of new catalytic materials.« less

Synthesis and Characterization Hierarchical Three-Dimensional TiO2 Structure via Hydrothermal Method

NASA Astrophysics Data System (ADS)

Syuhada, N.; Yuliarto, B.; Nugraha

2018-05-01

TiO2 is one of the most potential candidates due to its fascinating properties for multi-discipline fields. One dimensional nanostructure TiO2 such as nanotube and nanorods has been widely used for many devices technology. Compare with one-dimensional nanostructure TiO2; the hierarchical TiO2 has not been widely applied. Three dimensional TiO2 play a promising role for application in many different fields such as photovoltaics, photocatalytic and a gas sensor. Herein, we report that the hierarchically structures TiO2 have been successfully obtained by the one-pot Hydrothermal process. The growth mechanism of Titania was controlled by Titanium (IV) isopropoxide (TTIP). Ethylene glycol (EG). Hydrochloric acid (HCl). Hexadecyltrimethylammonium bromide (CTAB) molar ratio. TTIP was used as titanium source and CTAB as a soft template. The molar ratio of TTIP. EG. HCl. CTAB was 0.1:0.2:0.4:0.001. Those samples were synthesized using the hydrothermal method at 180 °C for 20 h. The purpose of this work was focused on investigating morphology, crystallite size, crystalline phase, and particle size. The properties of these materials were characterized by XRay Diffraction, Energy Dispersive Spectroscopy and Scanning Electron Microscope. It was found all particles exhibited unique spherical morphology which arranged by nanorods and good distribution nanoparticle. The Average size of the sphere has range 1 µm to 3 µm with diameter nanorods 60 nm to 100 nm. The TiO2 spheres were constructed of interconnected nanorods and formed a three dimensional (3D) porous framework. XRD analysis confirmed that sample consisted of pure rutile crystal structure with crystallite size was 50 nm, and EDS revealed an elemental content of Ti 61.03 % and O 38.97 %.

Synthesis of zinc sulfide nanoparticles during zinc oxidization by H2S and H2S/H2O supercritical fluids

NASA Astrophysics Data System (ADS)

Vostrikov, A. A.; Fedyaeva, O. N.; Sokol, M. Ya.; Shatrova, A. V.

2014-12-01

Formation of zinc sulfide nanoparticles was detected during interaction of bulk samples with hydrogen sulfide at supercritical parameters. Synthesis proceeds with liberation of H2 by the reaction nZn + nH2S = (ZnS) n + nH2. It has been found by the X-ray diffraction method, scanning electron microscopy, and mass spectrometry that the addition of water stimulates coupled reactions of nanoparticle synthesis nZn + nH2O = (ZnO) n + nH2 and (ZnO) n + nH2S = (ZnS) n + nH2O and brings about an increase in the synthesis rate and morphological changes of (ZnS) n nanoparticles.

Copper-catalyzed formic acid synthesis from CO2 with hydrosilanes and H2O.

PubMed

Motokura, Ken; Kashiwame, Daiki; Miyaji, Akimitsu; Baba, Toshihide

2012-05-18

A copper-catalyzed formic acid synthesis from CO2 with hydrosilanes has been accomplished. The Cu(OAc)2·H2O-1,2-bis(diphenylphosphino)benzene system is highly effective for the formic acid synthesis under 1 atm of CO2. The TON value approached 8100 in 6 h. The reaction pathway was revealed by in situ NMR analysis and isotopic experiments.

Preparation, characterization and properties of ZnO nanomaterials

NASA Astrophysics Data System (ADS)

Luo, Jiaolian; Zhang, Xiaoming; Chen, Ruxue; Wang, Xiaohui; Zhu, Ji; Wang, Xiaomin

2017-06-01

In this paper, using the hydrothermal synthesis method, NaOH, Zn(NO3)2, anhydrous ethanol, deionized water as raw material to prepare ZnO nanomaterial, and by X ray diffraction (XRD), scanning electron microscopy (SEM) and photoluminescence spectroscopy (PL) on the synthesis of nano materials, surface morphology and phase luminescence characterization. The results show that the nano materials synthesized for single-phase ZnO, belonging to the six wurtzite structure; material surface shaped, arranged evenly distributed, and were the top six party structure; ZnO nano materials synthesized with strong emission spectra, emission peak is located at 394nm.

Hydrothermal synthesis of CuO micro-/nanostructures and their applications in the oxidative degradation of methylene blue and non-enzymatic sensing of glucose/H2O2.

PubMed

Prathap, M U Anu; Kaur, Balwinder; Srivastava, Rajendra

2012-03-15

In this paper, we report on the amino acids-/citric acid-/tartaric acid-assisted morphologically controlled hydrothermal synthesis of micro-/nanostructured crystalline copper oxides (CuO). These oxides were characterized by means of X-ray diffraction, nitrogen sorption, scanning electron microscopy, Fourier transform infrared, and UV-visible spectroscopy. The surface area of metal oxides depends on the amino acid used in the synthesis. The formation mechanisms were proposed based on the experimental results, which show that amino acid/citric acid/tartaric acid and hydrothermal time play an important role in tuning the morphology and structure of CuO. The catalytic activity of as-synthesized CuO was demonstrated by catalytic oxidation of methylene blue in the presence of hydrogen peroxide (H(2)O(2)). CuO synthesized using tyrosine was found to be the best catalyst compared to a variety of CuO synthesized in this study. CuO (synthesized in this study)-modified electrodes were used for the construction of non-enzymatic sensors, which displayed excellent electrocatalytic response for the detection of H(2)O(2) and glucose compared to conventional CuO. The high electrocatalytic response observed for the CuO synthesized using tyrosine can be correlated with the large surface area, which enhances the accessibility of H(2)O(2)/glucose molecule to the active site that results in high observed current. The methodology adopted in the present study provides a new platform for the fabrication of CuO-based high-performance glucose and other biosensors. Copyright © 2012 Elsevier Inc. All rights reserved.

Surfactant-assisted hydrothermal crystallization of nanostructured lithium metasilicate (Li{sub 2}SiO{sub 3}) hollow spheres: (I) Synthesis, structural and microstructural characterization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Ortiz-Landeros, J.; Departamento de Ingenieria Metalurgica, Escuela Superior de Ingenieria Quimica e Industrias Extractivas, IPN, UPALM, Av. Instituto Politecnico Nacional s/n, CP 07738, Mexico DF; Contreras-Garcia, M.E.

Lithium metasilicate (Li{sub 2}SiO{sub 3}) was successfully synthesized using a hydrothermal process in the presence of different surfactants with cationic, non-ionic and anionic characters. The samples obtained were compared to a sample prepared by the conventional solid-state reaction method. The structural and microstructural characterizations of different Li{sub 2}SiO{sub 3} powders were performed using various techniques. Diffraction analyses revealed the successful crystallization of pure Li{sub 2}SiO{sub 3} single phase by hydrothermal technique, even without further heat-treatments and independent of the surfactant used. Electron microscopy analyses revealed that Li{sub 2}SiO{sub 3} powders were composed of uniform micrometric particles with a hollow spheremore » morphology and nanostructured walls. Finally, different thermal analyses showed that Li{sub 2}SiO{sub 3} samples preserved their structure and microstructure after further thermal treatments. Specific aspects regarding the formation mechanism of the spherical aggregates under hydrothermal conditions are discussed, and there is a special emphasis on the effect of the synthesis pathway on the morphological characteristics. -- Graphical abstract: Li{sub 2}SiO{sub 3} was synthesized using a hydrothermal process in the presence of different surfactants. Li{sub 2}SiO{sub 3} powders were composed of uniform micrometric particles with a hollow sphere morphology and nanostructured walls. Display Omitted Highlights: {yields} Pure Li{sub 2}SiO{sub 3} was synthesized by the hydrothermal method. {yields} Surfactant addition produced microstructural and morphological variations. {yields} TEM reveled the generation of nanostructured hollow spheres.« less

One-pot synthesis of monodisperse CoFe2O4@Ag core-shell nanoparticles and their characterization.

PubMed

Hara, Shuta; Aisu, Jumpei; Kato, Masahiro; Aono, Takashige; Sugawa, Kosuke; Takase, Kouichi; Otsuki, Joe; Shimizu, Shigeru; Ikake, Hiroki

2018-06-08

In recent years, monodispersed magnetic nanoparticles with a core/shell structure are expected for their wide applications including magnetic fluid, recoverable catalysts, and biological analysis. However, their synthesis method needs numerous processes such as solvent substitution, exchange of protective agents, and centrifugation. A simple and rapid method for the synthesis of monodispersed core-shell nanoparticles makes it possible to accelerate their further applications. This paper describes a simple and rapid one-pot synthesis of core (CoFe 2 O 4 )-shell (Ag) nanoparticles with high monodispersity. The synthesized nanoparticles showed plasmonic light absorption owing to the Ag shell. Moreover, the magnetic property of the nanoparticles had a soft magnetic behavior at room temperature and a hard magnetic behavior at 5 K. In addition, the nanoparticles showed high monodispersity with a low polydispersity index (PDI) value of 0.083 in hexane.

One-pot synthesis of monodisperse CoFe2O4@Ag core-shell nanoparticles and their characterization

NASA Astrophysics Data System (ADS)

Hara, Shuta; Aisu, Jumpei; Kato, Masahiro; Aono, Takashige; Sugawa, Kosuke; Takase, Kouichi; Otsuki, Joe; Shimizu, Shigeru; Ikake, Hiroki

2018-06-01

In recent years, monodispersed magnetic nanoparticles with a core/shell structure are expected for their wide applications including magnetic fluid, recoverable catalysts, and biological analysis. However, their synthesis method needs numerous processes such as solvent substitution, exchange of protective agents, and centrifugation. A simple and rapid method for the synthesis of monodispersed core-shell nanoparticles makes it possible to accelerate their further applications. This paper describes a simple and rapid one-pot synthesis of core (CoFe2O4)-shell (Ag) nanoparticles with high monodispersity. The synthesized nanoparticles showed plasmonic light absorption owing to the Ag shell. Moreover, the magnetic property of the nanoparticles had a soft magnetic behavior at room temperature and a hard magnetic behavior at 5 K. In addition, the nanoparticles showed high monodispersity with a low polydispersity index (PDI) value of 0.083 in hexane.

Preparation and characterization of V/TiO{sub 2} nanocatalyst with magnetic nucleus of iron

DOE Office of Scientific and Technical Information (OSTI.GOV)

Feyzi, Mostafa; Rafiee, Hamid Reza, E-mail: rafieehr@yahoo.com; Ranjbar, Shahram

2013-11-15

Graphical abstract: - Highlights: • Fe-V/TiO{sub 2} nanocatalyst is prepared. • Combination of sol–gel and wetness impregnation methods. • Facile separation of catalyst from medium by magnet. - Abstract: A magnetic composite containing V/TiO{sub 2} was prepared by combination of sol–gel and wetness impregnation methods. The effects of synthesis temperature, different weight percents of Fe supported on TiO{sub 2}, vanadium loading and the heating rate of calcination on the structure and morphology of nanocatalyst were investigated. The optimum conditions for synthesized catalyst were 40 wt.% of Fe, 15 wt.% of V and synthesis temperature equal to 30 °C. Characterization ofmore » catalyst is carried out using XRD, TGA, DSC, SEM, FTIR and N{sub 2} physisorption measurements. The magnetic character of nanocatalyst was measured using VSM, which showed the typical paramagnetic behavior of sample at room temperature with a saturation magnetization value equal to 8.283 emu/g. The nanocatalyst has a particle size about 56 nm and can easily be separated from medium by a magnet.« less

Cr:SnO2 thin films-synthesis and characterization

NASA Astrophysics Data System (ADS)

Varghese, Anitta Rose; B. Bhadrapriya, C.; Amarendra, G.; Hussain, Shamima

2018-04-01

Thin films of pure and Chromium doped SnO2 were synthesized using sol-gel method by spin coating technique. XRD studies confirmed the formation of tetragonal structure for SnO2 thin films. Variations in peak width and position were identified with doping. The optical band gap of the undoped films was found to be 3.8eV and varied with doping. Raman spectrum gave signature peaks of Sn-O and Cr-O bonds for undoped and doped films. The uniformity of the samples and formation of aggregates were observed from FESEM analysis.

A comparative synthesis and physicochemical characterizations of Ni/Al2O3-MgO nanocatalyst via sequential impregnation and sol-gel methods used for CO2 reforming of methane.

PubMed

Aghamohammadi, Sogand; Haghighi, Mohammad; Karimipour, Samira

2013-07-01

Carbon dioxide reforming of methane is an interesting route for synthesis gas production especially over nano-sized catalysts. The present research deals with catalyst development for dry reforming of methane with the aim of reaching the most stable catalyst. Effect of preparation method, one of the most significant variables, on the properties of the catalysts was taken in to account. The Ni/Al2O3-MgO catalysts were prepared via sol-gel and sequential impregnation methods and characterized with XRD, FESEM, EDAX, BET and FTIR techniques. The reforming reactions were carried out using different feed ratios, gas hourly space velocities (GHSV) and reaction temperatures to identify the influence of operational variables. FESEM images indicate uniform particle size distribution for the sample synthesized with sol-gel method. It has been found that the sol-gel method has the potential to improve catalyst desired properties especially metal surface enrichment resulting in catalytic performance enhancement. The highest yield of products was obtained at 850 degrees C for both of the catalysts. During the 10 h stability test, CH4 and CO2 conversions gained higher values in the case of sol-gel made catalyst compared to impregnated one.

One-pot synthesis of MnO2-chitin hybrids for effective removal of methylene blue.

PubMed

Dassanayake, Rohan S; Rajakaruna, Erandathi; Moussa, Hanna; Abidi, Noureddine

2016-12-01

Manganese dioxide (MnO 2 )-chitin-hybrid material was prepared by a facile "one-pot" synthesis method. MnO 2 -chitin hybrid was used for the effective removal of methylene blue (MB) from liquid solution as model for wastewater treatment. The hybrid obtained was characterized by field emission scanning electron microscopy and energy dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction and thermogravimetric analysis. The effect of pH and temperature were studied. MnO 2 -chitin hybrid showed high performance for oxidative decolorization and removal of MB. Typically, 25mL of MB (20mg/L) can be completely decolorized in 2.5min with 8.5mg of the MnO 2 -chitin hybrid. The hybrid material exhibited excellent recyclability and durability with the degradation value of 99% for MB after ten consecutive cycles. Copyright © 2016 Elsevier B.V. All rights reserved.

High-yield sol-gel synthesis of well-dispersed, colorless ZrO(2) nanocrystals.

PubMed

Mizuno, Mikihisa; Sasaki, Yuichi; Lee, Sungkil; Katakura, Hitoshi

2006-08-15

A 93% high-yield synthesis of well-dispersed, colorless zirconium dioxide (ZrO(2)) nanocrystals is reported. In this synthesis, hydrolysis and condensation reactions of zirconium(IV) tert-butoxide in the presence of oleic acid (100 degrees C) formed ZrO(2) precursors. The ZrO(2) precursors were made of -Zr-O-Zr- networks surrounded by oleic acid molecules. Annealing (280 degrees C) the precursors dispersed in dioctyl ether caused crystallization of the -Zr-O-Zr- networks, thereby generating 4 nm ZrO(2) nanocrystals stabilized with oleic acid. The particles were highly crystalline and tetragonal phase. A dense ZrO(2) nanocrystal dispersion in toluene (280 mg/mL) showed a transmittance of about 90% (3 mm optical path length) in the whole visible region.

Synthesis and characterization of heteroleptic titanium MOCVD precursors for TiO2 thin films.

PubMed

Kim, Euk Hyun; Lim, Min Hyuk; Lah, Myoung Soo; Koo, Sang Man

2018-02-13

Heteroleptic titanium alkoxides with three different ligands, i.e., [Ti(O i Pr)(X)(Y)] (X = tridentate, Y = bidentate ligands), were synthesized to find efficient metal organic chemical vapor deposition (MOCVD) precursors for TiO 2 thin films. Acetylacetone (acacH) or 2,2,6,6-tetramethyl-3,5-heptanedione (thdH) was employed as a bidentate ligand, while N-methyldiethanolamine (MDEA) was employed as a tridentate ligand. It was expected that the oxygen and moisture susceptibility of titanium alkoxides, as well as their tendency to form oligomers, would be greatly reduced by placing multidentate and bulky ligands around the center Ti atom. The synthesized heteroleptic titanium alkoxides were characterized both physicochemically and crystallographically, and their thermal behaviors were also investigated. [Ti(O i Pr)(MDEA)(thd)] was found to be monomeric and stable against moisture; it also showed good volatility in the temperature window between volatilization and decomposition. This material was used as a single-source precursor during MOCVD to generate TiO 2 thin films on silicon wafers. The high thermal stability of [Ti(O i Pr)(MDEA)(thd)] enabled the fabrication of TiO 2 films over a wide temperature range, with steady growth rates between 500 and 800 °C.

Synthesis and characterization of breast-phantom-based gelatine-glutaraldehyde-TiO2 as a test material for the application of breast cancer diagnosis

NASA Astrophysics Data System (ADS)

Ukhrowiyah, Nuril; Setyaningsih, Novi; Hikmawati, Dyah; Yasin, Moh

2017-05-01

Synthesis of breast-phantom-based on gelatine-glutaraldehyde-TiO2 as testing material of breast cancer diagnosis using Near Infrared-Diffuse Optical Tomography (NIR-DOT) is presented. Glutaraldehyde (GA) is added to obtain optimum breast phantom which has same elasticity modulus with mammae. First, synthesis is conducted by mixing gelatine with various amounts of 1 g, 2 g and 3 g with saline solution on 40° C temperature for 30 minutes until they become homogenous. Next, GA with concentration of 0.5 and 1.0% is added. The characterization includes FTIR test, physical test, and mechanical test used to identify group of gelatine’s functions. Elasticity modulus of breast phantom of gelatine composition 2 g and 0.5% GA is obtained at 53.46 kPA which is the approximation of mammae culture elasticity. This composition is chosen to synthesise the next step. In the second step, TiO2 is added with variation of 0.01 g, 0.015 g, 0.02 g, 0.025 g, and 0,03 g. With this variation, it is aimed to get a breast phantom providing image with optimum absorption. The test of this material uses Differential Scanning Calorimetry (DSC), homogeneity test, and analysis of coefficient absorption. The result shows the sample has a good thermal property in the range of 40 - 70° C with a good homogeneity and absorption coefficient of 0.4 mm-1.

Synthesis and characterization of binary ZnO-SnO2 (ZTO) thin films by e-beam evaporation technique

NASA Astrophysics Data System (ADS)

Bibi, Shagufta; Shah, A.; Mahmood, Arshad; Ali, Zahid; Raza, Qaisar; Aziz, Uzma; Haneef; Waheed, Abdul; Shah, Ziaullah

2018-04-01

The binary ZnO-SnO2 (ZTO) thin films with varying SnO2 concentrations (5, 10, 15, and 20 wt%) were grown on glass substrate by e-beam evaporation technique. The prepared ZTO films were annealed at 400 °C in air. These films were then characterized to investigate their structural, optical, and electrical properties as a function of SnO2 concentration. XRD analysis reveals that the crystallinity of the film decreases with the addition of SnO2 and it transforms to an amorphous structure at a composition of 40% SnO2 and 60% ZnO. Morphology of the films was examined by atomic force microscopy which points out that surface roughness of the films decreases with the increasing of SnO2 in the film. Optical properties such as optical transparency, band-gap energy, and optical constants of these films were examined by spectrophotometer and spectroscopic Ellipsometer. It was observed that the average optical transmission of mixed films improves with incorporation of SnO2. In addition, the band-gap energy of the films was determined to be in the range of 3.37-3.7 eV. Furthermore, it was found that the optical constants (n and k) decrease with the addition of SnO2. Similarly, it is observed that the electrical resistivity increases nonlinearly with the increase in SnO2 in ZnO-SnO2 thin films. However, it is noteworthy that the highest figure of merit (FOM) value, i.e., 55.87 × 10-5 Ω-1, is obtained for ZnO-SnO2 (ZTO) thin film with 40 wt% of SnO2 composition. Here, we suggest that ZnO-SnO2 (ZTO) thin film with composition of 60:40 wt% can be used as an efficient TCO film due to the improved transmission, and reduced RMS value and highest FOM value.

Synthesis and Characterization of Fe3O4 Nanoparticles using Polyvinyl Alcohol (PVA) as Capping Agent and Glutaraldehyde (GA) as Crosslinker

NASA Astrophysics Data System (ADS)

Budi Hutami Rahayu, Lale; Oktavia Wulandari, Ika; Herry Santjojo, Djoko; Sabarudin, Akhmad

2018-01-01

The use of polyvinyl alcohol (PVA) as a capping agent and glutaraldehyde (GA) as a crosslinker for a synthesis of magnetite (Fe3O4) nanoparticles is able to reduce agglomeration of produced Fe3O4. Additionally, oxidation of Fe3O4 by air could be avoided. The synthesis is carried out in two steps: first step, magnetite (Fe3O4) nanoparticles were prepared by dissolving the FeCl3.6H2O and FeCl2.4H2O in alkaline media (NH3.H2O). The second step, magnetite nanoparticles were coated with polyvinyl alcohol (PVA) and glutaraldehyde (GA) to obtain Fe3O4-PVA-GA. The latter material was then characterized by FTIR to determine the typical functional groups of magnetite coated with PVA-GA. X-ray Diffraction analysis was used to determine structure and size of crystal as well as the percentage of magnetite produced. It was found that the produced nanoparticles have crystal sizes around 4-9 nm with the cubic crystal structure. The percentage of magnetite phase increases when the amount of glutaraldehyde increased. SEM-EDX was employed to assess the surface morphology and elemental composition of the resulted nanoparticles. The magnetic character of the magnetite and Fe3O4- PVA-GA were studied using Electron Spin Resonance.

Synthesis of TiO2 by solution combustion technique by mixed fuel approach for wLED applications

NASA Astrophysics Data System (ADS)

Venkatesha Babu K., R.; Renuka C., G.

2018-05-01

Synthesis of Ce3+ (0.25-0.75 mol %) doped TiO2 nanophosphors was done by solution combustion route using combination of fuels. The structural characterization of the nanophosphor was performed by PXRD, SEM and TEM. The estimated crystallite sizes are in the nano meter scale range. The Eg of pure and doped TiO2 were 3.10 and 3.23 eV respectively were estimated from DRS data. The CIE and CCT data reveals that the nanophosphor emits pale green and is useful for wLED at a temperature 4474K.

Synthesis and characterization of polycrystalline brownmillerite cobalt doped Ca{sub 2}Fe{sub 2}O{sub 5}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dhankhar, Suchita; Baskar, K.; Singh, Shubra, E-mail: shubra6@gmail.com

2016-05-23

Brownmillerite compounds with general formula A{sub 2}BB’O{sub 5} (BB’ = Mn, Al, Fe, Co) have attracted attention in wide range of applications such as in solid oxide fuel cell, oxygen separation membrane and photocatalysis. Brownmillerite compounds have unique structure with alternate layers of BO{sub 6} octahedral layers and BO{sub 4} tetrahedral layers. Presence of dopants like Co in place of Fe increases oxygen vacancies. In the present work we have synthesized polycrystalline Ca{sub 2}Fe{sub 2}O{sub 5} and Ca{sub 2}Fe{sub 1-x}Co{sub x}O{sub 5} (x = 0.01, 0.03) by citrate combustion route. The as prepared samples were characterized by XRD using PANalyticalmore » X’Pert System, DRS (Diffuse reflectance spectroscopy) and SEM (Scanning electron microscopy).« less

Synthesis and characterization of ZnO nanoparticles: effect of solvent and antifungal capacity of NPs obtained in ethylene glycol

NASA Astrophysics Data System (ADS)

López, Cenayda; Rodríguez-Páez, Jorge E.

2017-12-01

In this work, nanoparticles of zinc oxide (ZnO-NPs) were synthesized using acetic acid, ethanol and ethylene glycol as solvents. To determine the physicochemical and structural characteristics of the synthesized nanoparticles, IR spectroscopy, X-ray diffraction, UV-Vis spectroscopy and transmission electron microscopy were used. The characterization results indicated that the particles obtained were of nanometers size (< 100 nm) with different morphologies: needle-type when using acetic acid, nanoribbons using ethanol, and spheroidal using ethylene glycol. The results of this work show that on using solvents with a lower dielectric constant value a preferential direction of nanoparticle growth would be favored, leading to the formation of nanoribbons, in ethanol ( ɛ r = 24.3), and needles in acetic acid ( ɛ r = 6.2). The band gap of ZnO-Nps depends of synthesis solvent used: 3.37 eV for acetic acid, 3.3 eV to ethanol and 3.28 eV to ethylene glycol, indicating that the optical properties of these nanoparticles are affected by the synthesis medium. Based on the information from the characterization of the ZnO-NPs synthesized, the spheroidal nanoparticles were selected, to determine their antifungal capacity on cultures of Aspergillus niger strains. The concentrations of ZnO-NPs that showed the greatest antifungal effect were those from 9 mmol L-1.

Catalytic activity of bimetallic Zn/TiO2 catalyst for degradation of herbicide paraquat: synthesis and characterization

NASA Astrophysics Data System (ADS)

Sakee, Uthai; Wanchanthuek, Ratchaneekorn

2017-11-01

The preparation and characterization of Zn/TiO2 catalysts were performed and the photocatalytic properties of the resulting catalysts were tested using the paraquat degradation reaction under UV and solar light irradiation. The effect of the preparation method, amount of Zn loading, the calcination temperature and the thermal annealing during the autoclave aging were studied as well as the light irradiation during the testing reaction. The initial concentration of paraquat was 400 ppm, the pH during the catalytic testing was seven and the reaction temperature was 30 °C. The characterization information were obtained from XRD, XPS, UV-vis diffuse reflectance, FTIR, TEM and BET techniques. They were used to explain the expressed catalytic activity of Zn/TiO2. The results showed that the Zn/TiO2 catalyst from the hydrothermal method could remove about 80% of the paraquat from the solution (using 4 g l-1 of catalyst). The characterization data showed that the surface area, porous structure and dispersion of Zn species could affect the ability of the paraquat removal rather than the crystallnity of the TiO2 in the catalyst. The XPS spectra suggested that the preparation method, between the sol gel and hydrothermal, could not affect the state of the Zn and Ti, which presented in the Zn2+ and Ti4+ forms. This primary result will lead us to further study to elucidate the main active site by the XPS technique. Moreover, it clearly showed that the lowering of the band gap energy in the Zn/TiO2 was achieved (compared to bare TiO2), and this phenomena was one of the factors that gave the higher photocatalytic activity of the Zn/TiO2 catalyst.

Synthesis and modification of nano-sized TiO{sub 2} for photo-degradation process under visible light irradiation; a Placket–Burman experimental design

DOE Office of Scientific and Technical Information (OSTI.GOV)

Izadyar, Soheila; Fatemi, Shohreh, E-mail: shfatemi@ut.ac.ir; Mousavand, Tahereh

2013-09-01

Graphical abstract: - Highlights: • Nanosized TiO{sub 2} doped with nitrogen and iron was produced by sol-gel method. • Linear models were derived to relate the phase and particle size to synthesis factors. • High photocatalytic activity was observed for acetaldehyde degradation. - Abstract: In this research, nitrogen and iron (III) co-doped nano TiO{sub 2} (N-Fe-TiO{sub 2}) was prepared by sol-gel method using ammonium chloride and iron chloride solutions as nitrogen and iron sources, respectively. The effect of synthesis parameters (weight ratios of N/TiO{sub 2} and Fe/TiO{sub 2}, synthesis temperature, calcination time and temperature) was simultaneously investigated on the qualitymore » of the N-Fe-TiO{sub 2} product by a two-level Placket–Burman experimental design. The synthesized powders were characterized by XRD, XPS and UV–Vis spectroscopy techniques. The mean crystal size and anatase content were determined and evaluated as the linear functions of so-called synthesis parameters by the statistical analysis and regression. The 2%N-1%Fe-TiO{sub 2} product by 11 nm mean crystal size and 78% anatase content, synthesized at 35 °C and calcined at 500 °C during 2 h, exhibited the most significant activity during the photo-degradation of acetaldehyde under visible light irradiation and its efficiency was obtained about four times more than photocatalytic activity of Degussa TiO{sub 2}-P25.« less

High-throughput continuous hydrothermal synthesis of nanomaterials (part II): unveiling the as-prepared CexZryYzO2-δ phase diagram.

PubMed

Quesada-Cabrera, Raul; Weng, Xiaole; Hyett, Geoff; Clark, Robin J H; Wang, Xue Z; Darr, Jawwad A

2013-09-09

High-throughput continuous hydrothermal flow synthesis was used to manufacture 66 unique nanostructured oxide samples in the Ce-Zr-Y-O system. This synthesis approach resulted in a significant increase in throughput compared to that of conventional batch or continuous hydrothermal synthesis methods. The as-prepared library samples were placed into a wellplate for both automated high-throughput powder X-ray diffraction and Raman spectroscopy data collection, which allowed comprehensive structural characterization and phase mapping. The data suggested that a continuous cubic-like phase field connects all three Ce-Zr-O, Ce-Y-O, and Y-Zr-O binary systems together with a smooth and steady transition between the structures of neighboring compositions. The continuous hydrothermal process led to as-prepared crystallite sizes in the range of 2-7 nm (as determined by using the Scherrer equation).

In-situ synthesis of MoSi{sub 2}-Al{sub 2}O{sub 3} composite by a thermite reaction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Deevi, S.C.; Deevi, S.

1995-08-01

In this paper, the authors discuss the reaction mechanism involved in the thermite reaction leading to the synthesis of a composite since in an actual combustion synthesis, the reaction propagates at a velocity of 10 to 20 mm/sec. Reaction mechanism was determined by using a differential thermal analysis (DTA) and X-ray diffraction (XRD). During the combustion synthesis of MoSi{sub 2}-{alpha}Al{sub 2}O{sub 3}, reaction of MoO{sub 3}, Al and Si occurs rapidly and the reactants and products are expected to be in the liquid state at the combustion temperature. MoO{sub 3} is first reduced to MoO{sub 2}, and the reaction betweenmore » MoO{sub 2}, Al and Si leads to a composite of MoSi{sub 2}-{alpha}Al{sub 2}O{sub 3}. Differential thermal analysis reveals that the onset of exothermic reactions is preceded by melting indicating the necessity of molten Al for the synthesis of the composite. The reaction between MoO{sub 2} + 2Al +2Si can be moderated with Mo-Si mixtures such that the ratio of MoSi{sub 2} to Al{sub 2}O{sub 3} can be increased in the composite of MoSi{sub 2}-{alpha}Al{sub 2}O{sub 3}.« less

Synthesis and characterization of Cu-Zn/TiO2 for the photocatalytic conversion of CO2 to methane.

PubMed

Rana, Adeem Ghaffar; Ahmad, Waqar; Al-Matar, Ali; Shawabkeh, Reyad; Aslam, Zaheer

2017-05-01

Different Cu-Zn/TiO 2 catalysts were synthesized by using the wet impregnation method. The prepared catalysts were used for the conversion of CO 2 into methane by photocatalysis. Various characterization techniques were used to observe the surface morphology, crystalline phase, Brunauer-Emmett-Teller (BET) surface area, presence of impregnated Cu and Zn, and functional group. Scanning electron microscope analysis showed spherical morphology, and slight agglomeration of catalyst particles was observed. BET analysis revealed that the surface area of the catalyst was decreased from 10 to 8.5 m 2 /g after impregnation of Cu and Zn over TiO 2 support. Synergetic effect of Cu and Zn over TiO 2 support (Cu 2.6 /TiO 2 , Zn 0.5 /TiO 2 and Cu 2.6 -Zn 0.5 /TiO 2 ) and the effects of Cu loading (0, 1.8, 2.1, 2.6 and 2.9 wt%) were also investigated at different feed molar ratios of H 2 /CO 2 (2:1 and 4:1). The Cu 2.6 -Zn 0.5 /TiO 2 catalyst showed a maximum conversion of 14.3% at a feed molar ratio of 4. The addition of Zn over the catalyst surface increased the conversion of CO 2 from 10% to 14.3% which might be due to synergy of Cu and Zn over TiO 2 support.

Synthesis, characterization and biological study on Cr(3+), ZrO(2+), HfO(2+) and UO(2)(2+) complexes of oxalohydrazide and bis(3-hydroxyimino)butan-2-ylidene)-oxalohydrazide.

PubMed

El-Asmy, A A; El-Gammal, O A; Radwan, H A

2010-09-01

Cr(3+), ZrO(2+), HfO(2+) and UO(2)(2+) complexes of oxalohydrazide (H(2)L(1)) and oxalyl bis(diacetylmonoxime hydrazone) [its IUPAC name is oxalyl bis(3-hydroxyimino)butan-2-ylidene)oxalohydrazide] (H(4)L(2)) have been synthesized and characterized by partial elemental analysis, spectral (IR; electronic), thermal and magnetic measurements. [Cr(L(1))(H(2)O)(3)(Cl)].H(2)O, [ZrO(HL(1))(2)].C(2)H(5)OH, [UO(2)(L(1))(H(2)O)(2)] [ZrO(H(3)L(2))(Cl)](2).2H(2)O, [HfO(H(3)L(2))(Cl)](2).2H(2)O and [UO(2)(H(2)L(2))].2H(2)O have been suggested. H(2)L(1) behaves as a monobasic or dibasic bidentate ligand while H(4)L(2) acts as a tetrabasic octadentate with the two metal centers. The molecular modeling of the two ligands have been drawn and their molecular parameters were calculated. Examination of the DNA degradation of H(2)L(1) and H(4)L(2) as well as their complexes revealed that direct contact of [ZrO(H(3)L(2))(Cl)](2).2H(2)O or [HfO(H(3)L(2))(Cl)](2).2H(2)O degrading the DNA of Eukaryotic subject. The ligands and their metal complexes were tested against Gram's positive Bacillus thuringiensis (BT) and Gram's negative (Escherichia coli) bacteria. All compounds have small inhibitory effects. Copyright 2010 Elsevier B.V. All rights reserved.

Synthesis, characterization and catalytic performance of ZnO-CeO2 nanoparticles in wet oxidation of wastewater containing chlorinated compounds

NASA Astrophysics Data System (ADS)

Anushree; Kumar, S.; Sharma, C.

2017-11-01

Here we report the catalytic property of ZnO-CeO2 nanoparticles towards oxidative degradation of organic pollutants present in industrial wastewater. The catalysts were prepared by co-precipitation method without using any surfactant. The physicochemical properties of catalysts were studied by XRD, Raman, XPS, N2-sorption, FE-SEM, TEM and EDX techniques. The characterization results confirmed the formation of porous ZnO-CeO2 nanocatalysts with high surface area, pore volume and oxygen vacancies. ZnO-CeO2 nanocatalysts exhibited appreciable efficiency in CWAO of industrial wastewater under mild conditions. The Ce40Zn60 catalyst was found to be most efficient with 72% color, 64% chemical oxygen demand (COD) and 63% total organic carbon (TOC) removal. Efficient removal of chlorophenolics (CHPs, 59%) and adsorbable organic halides (AOX, 54%) indicated the feasibility of using ZnO-CeO2 nanocatalysts in degradation of non-biodegradable and toxic chlorinated compounds.

Eco-friendly synthesis of TiO2, Au and Pt doped TiO2 nanoparticles for dye sensitized solar cell applications and evaluation of toxicity

NASA Astrophysics Data System (ADS)

Gopinath, K.; Kumaraguru, S.; Bhakyaraj, K.; Thirumal, S.; Arumugam, A.

2016-04-01

Driven by the demand of pure TiO2, Au and Pt doped TiO2 NPs were successfully synthesized using Terminalia arjuna bark extract. The eco-friendly synthesized NPs were characterized by UV-Vis-DRS, ATR-FT-IR, PL, XRD, Raman, SEM with EDX and TEM analysis. The synthesized NPs were investigation for dye sensitized solar cell applications. UV-Vis-Diffused Reflectance Spectra clearly showed that the expected TiO2 inter band absorption below 306 nm, incorporation of gold shows surface plasma resonant (SPR) near 555 nm and platinum incorporated TiO2 NPs shows absorbance at 460 nm. The energy conversion efficiency for Au doped TiO2 NPs when compared to pure and Pt doped TiO2 NPs. In addition to that, Au noble metal present TiO2 matrix and an improve open-circuit voltage (Voc) of DSSC. Synthesized NPs was evaluated into antibacterial and antifungal activities by disk diffusion method. It is observed that NPs have not shown any activities in all tested bacterial and fungal strains. In this eco-friendly synthesis method to provide non toxic and environmental friendly nanomaterials can be used for solar energy device application.

Synthesis and characterization of a NaSICON series with general formula Na 2.8Zr 2-ySi 1.8-4yP 1.2+4yO 12 (0⩽ y⩽0.45)

NASA Astrophysics Data System (ADS)

Essoumhi, A.; Favotto, C.; Mansori, M.; Satre, P.

2004-12-01

In this work, we present the synthesis and the characterization of ionic conducting ceramics of NaSICON-type (Natrium super ionic conductor). The properties of this ceramic make it suitable for use in electrochemical devices. These solid electrolytes can be used as sensors for application in the manufacturing of potentiometric gas sensors, for the detection of pollutant emissions and for environment control. The family of NaSICON that we studied has as a general formula Na 2.8Zr 2-ySi 1.8-4yP 1.2+4yO 12 with 0⩽ y⩽0.45. The various compositions were synthesized by produced using the sol-gel method. The electric properties of these compositions were carried out by impedance spectroscopy. The results highlight the good conductivity of the Na 2.8Zr 1.775Si 0.9P 2.1O 12 composition.

CdO nanorods and Cd(OH)2/Ag core/satellite nanorods: Rapid and efficient sonochemical synthesis, characterization and their magnetic properties.

PubMed

Abbas, Mohamed; Tawfik, Wael; Chen, Jiangang

2018-01-01

We have designed an efficient and direct sonochemical method for the facile synthesis of Cd(OH) 2 , CdO, and Cd(OH) 2 /Ag core/satellite nanorods. A Cd(OH) 2 nanorod was synthesized with a one-pot, environmentally-friendly aqueous sonochemical reaction, followed by calcination at 500°C to produce CdO nanorods. Thirty minutes of re-ultrasonicated CdO nanorods in the presence of the Ag precursor was sufficient for phase transformation from the cubic structure of CdO to the monoclinic crystalline structure of Cd(OH) 2 , accompanied by deposition of Ag nanodots on the surface to form Cd(OH) 2 /Ag core/satellite nanorods. X-ray diffraction, transmission electron microscopy, high-resolution transmission electron microscopy, energy-dispersive spectroscopy, N 2 Brunauer-Emmett-Teller adsorption-desorption, and Fourier-transform infrared spectroscopy measurements confirmed the successful formation of the various phases and the unique morphology of the nanorods/satellites. We also measured the magnetic properties using a vibrating sample magnetometer at room temperature, and the produced nanorods showed weak unsaturated ferromagnetic properties with a magnetic moment values of 0.105 and 0.076emu/g for CdO and Cd(OH) 2 /Ag NRs, respectively. In conclusion, our one-pot, cost-effective, sonochemical approach holds promise for the synthesis of various oxides and core/satellite nanoparticles. Copyright © 2017 Elsevier B.V. All rights reserved.

Sol-Gel Synthesis of Fe-Doped TiO2 Nanocrystals

NASA Astrophysics Data System (ADS)

Marami, Mohammad Bagher; Farahmandjou, Majid; Khoshnevisan, Bahram

2018-03-01

Fe-doped TiO2 powders were synthesized by the sol-gel method using titanium (IV) isopropoxide (TTIP) as the starting material, ethanol as solvent, and ethylene glycol (EG) as stabilizer. These prepared samples were characterized by x-ray diffractometer (XRD), field emission scanning electron microscope (FESEM), Fourier-transform infrared (FTIR) spectroscopy, diffuse reflection spectroscopy (DRS), energy-dispersive x-ray spectroscopy (EDX), and photoluminescence (PL) analyses to study their structure, morphology, and optical properties. The particle size of Fe-doped TiO2 was in the range of 18-39 nm and the minimum crystallite size was achieved for 4 mol.% of Fe. The XRD result of the samples that were doped with Fe showed a tetragonal structure. It also revealed the coexistence of the anatase and rutile phases, and showed that their ratio changed with various molar concentrations of Fe dopant. FTIR spectroscopy showed the presence of the Ti-O vibration band in the samples. PL analysis revealed the PL property in the UV region. Visible irradiation and the intensity of PL spectra were both reduced by doping TiO2 with 3 mol.% of Fe as compared to the pure variety. The spectra from the DRS showed a red shift and a reduction of 2.6 eV in the band gap energy for 4 mol.% Fe-doped TiO2. The optimum level of impurity (4 mol.%) for Fe-doped TiO2 nanoparticles (NPs), which improve the optical and electrical properties by using new precursors and can be used in solar cells and electronic devices, was determined. The novelty of this work consists of: the Fe/TiO2 NPs are synthesized by new precursors from sol-gel synthesis of iron and TTIP using acetic acid-catalyzed solvolysis (original idea) and the optical properties optimized with a mixture of phases (anatase/rutile) of Fe-doped TiO2 by this facile method.

Sol-Gel Synthesis of Fe-Doped TiO2 Nanocrystals

NASA Astrophysics Data System (ADS)

Marami, Mohammad Bagher; Farahmandjou, Majid; Khoshnevisan, Bahram

2018-07-01

Fe-doped TiO2 powders were synthesized by the sol-gel method using titanium (IV) isopropoxide (TTIP) as the starting material, ethanol as solvent, and ethylene glycol (EG) as stabilizer. These prepared samples were characterized by x-ray diffractometer (XRD), field emission scanning electron microscope (FESEM), Fourier-transform infrared (FTIR) spectroscopy, diffuse reflection spectroscopy (DRS), energy-dispersive x-ray spectroscopy (EDX), and photoluminescence (PL) analyses to study their structure, morphology, and optical properties. The particle size of Fe-doped TiO2 was in the range of 18-39 nm and the minimum crystallite size was achieved for 4 mol.% of Fe. The XRD result of the samples that were doped with Fe showed a tetragonal structure. It also revealed the coexistence of the anatase and rutile phases, and showed that their ratio changed with various molar concentrations of Fe dopant. FTIR spectroscopy showed the presence of the Ti-O vibration band in the samples. PL analysis revealed the PL property in the UV region. Visible irradiation and the intensity of PL spectra were both reduced by doping TiO2 with 3 mol.% of Fe as compared to the pure variety. The spectra from the DRS showed a red shift and a reduction of 2.6 eV in the band gap energy for 4 mol.% Fe-doped TiO2. The optimum level of impurity (4 mol.%) for Fe-doped TiO2 nanoparticles (NPs), which improve the optical and electrical properties by using new precursors and can be used in solar cells and electronic devices, was determined. The novelty of this work consists of: the Fe/TiO2 NPs are synthesized by new precursors from sol-gel synthesis of iron and TTIP using acetic acid-catalyzed solvolysis (original idea) and the optical properties optimized with a mixture of phases (anatase /rutile) of Fe-doped TiO2 by this facile method.

Highly reactive {001} facets of TiO2-based composites: synthesis, formation mechanism and characterization

NASA Astrophysics Data System (ADS)

Ong, Wee-Jun; Tan, Lling-Lling; Chai, Siang-Piao; Yong, Siek-Ting; Mohamed, Abdul Rahman

2014-01-01

Titanium dioxide (TiO2) is one of the most widely investigated metal oxides due to its extraordinary surface, electronic and catalytic properties. However, the large band gap of TiO2 and massive recombination of photogenerated electron-hole pairs limit its photocatalytic and photovoltaic efficiency. Therefore, increasing research attention is now being directed towards engineering the surface structure of TiO2 at the most fundamental and atomic level namely morphological control of {001} facets in the range of microscale and nanoscale to fine-tune its physicochemical properties, which could ultimately lead to the optimization of its selectivity and reactivity. The synthesis of {001}-faceted TiO2 is currently one of the most active interdisciplinary research areas and demonstrations of catalytic enhancement are abundant. Modifications such as metal and non-metal doping have also been extensively studied to extend its band gap to the visible light region. This steady progress has demonstrated that TiO2-based composites with {001} facets are playing and will continue to play an indispensable role in the environmental remediation and in the search for clean and renewable energy technologies. This review encompasses the state-of-the-art research activities and latest advancements in the design of highly reactive {001} facet-dominated TiO2via various strategies, including hydrothermal/solvothermal, high temperature gas phase reactions and non-hydrolytic alcoholysis methods. The stabilization of {001} facets using fluorine-containing species and fluorine-free capping agents is also critically discussed in this review. To overcome the large band gap of TiO2 and rapid recombination of photogenerated charge carriers, modifications are carried out to manipulate its electronic band structure, including transition metal doping, noble metal doping, non-metal doping and incorporating graphene as a two-dimensional (2D) catalyst support. The advancements made in these aspects are

Highly reactive {001} facets of TiO2-based composites: synthesis, formation mechanism and characterization.

PubMed

Ong, Wee-Jun; Tan, Lling-Lling; Chai, Siang-Piao; Yong, Siek-Ting; Mohamed, Abdul Rahman

2014-02-21

Titanium dioxide (TiO2) is one of the most widely investigated metal oxides due to its extraordinary surface, electronic and catalytic properties. However, the large band gap of TiO2 and massive recombination of photogenerated electron-hole pairs limit its photocatalytic and photovoltaic efficiency. Therefore, increasing research attention is now being directed towards engineering the surface structure of TiO2 at the most fundamental and atomic level namely morphological control of {001} facets in the range of microscale and nanoscale to fine-tune its physicochemical properties, which could ultimately lead to the optimization of its selectivity and reactivity. The synthesis of {001}-faceted TiO2 is currently one of the most active interdisciplinary research areas and demonstrations of catalytic enhancement are abundant. Modifications such as metal and non-metal doping have also been extensively studied to extend its band gap to the visible light region. This steady progress has demonstrated that TiO2-based composites with {001} facets are playing and will continue to play an indispensable role in the environmental remediation and in the search for clean and renewable energy technologies. This review encompasses the state-of-the-art research activities and latest advancements in the design of highly reactive {001} facet-dominated TiO2via various strategies, including hydrothermal/solvothermal, high temperature gas phase reactions and non-hydrolytic alcoholysis methods. The stabilization of {001} facets using fluorine-containing species and fluorine-free capping agents is also critically discussed in this review. To overcome the large band gap of TiO2 and rapid recombination of photogenerated charge carriers, modifications are carried out to manipulate its electronic band structure, including transition metal doping, noble metal doping, non-metal doping and incorporating graphene as a two-dimensional (2D) catalyst support. The advancements made in these aspects are

High-Throughput Synthesis and Characterization of Eu Doped Ba xSr2- xSiO4 Thin Film Phosphors.

PubMed

Frost, Sara; Guérin, Samuel; Hayden, Brian E; Soulié, Jean-Philippe; Vian, Chris

2018-06-20

High-throughput techniques have been employed for the synthesis and characterization of thin film phosphors of Eu-doped Ba x Sr 2- x SiO 4 . Direct synthesis from evaporation of the constituent elements under a flux of atomic oxygen on a sapphire substrate at 850 °C was used to directly produce thin film libraries (415 nm thickness) of the crystalline orthosilicate phase with the desired compositional variation (0.24 > x > 1.86). The orthosilicate phase could be synthesized as a pure, or predominantly pure, phase. Annealing the as synthesized library in a reducing atmosphere resulted in the reduction of the Eu while retaining the orthosilicate phase, and resulted in a materials thin film library where fluorescence excited by blue light (450 nm) was observable by the naked eye. Parallel screening of the fluorescence from the combinatorial libraries of Eu doped Ba x Sr 2- x SiO 4 has been implemented by imaging the fluorescent radiation over the library using a monochrome digital camera using a series of color filters. Informatics tools have been developed to allow the 1931 CIE color coordinates and the relative quantum efficiencies of the materials library to be rapidly assessed and mapped against composition, crystal structure and phase purity. The range of compositions gave values of CIE x between 0.17 and 0.52 and CIE y between 0.48 and 0.69 with relative efficiencies in the range 2.0 × 10 -4 -7.6 × 10 -4 . Good agreement was obtained between the thin film phosphors and the fluorescence characteristics of a number of corresponding bulk phosphor powders. The thermal quenching of fluorescence in the thin film libraries was also measured in the temperature range 25-130 °C: The phase purity of the thin film was found to significantly influence both the relative quantum efficiency and the thermal quenching of the fluorescence.

Citrate gel-combustion synthesis and sintering of nanocrystalline ThO2 powders

NASA Astrophysics Data System (ADS)

Sanjay Kumar, D.; Ananthasivan, K.; Amirthapandian, S.; Dasgupta, Arup; Jogeswara Rao, G.

2017-12-01

A systematic study of the influence of citric acid to nitrate mole (R) ratio (R = 0 to 0.50) on the citrate gel-combustion synthesis of nanocrystalline (nc) ThO2 in bulk quantities (30 g) by using citrate gel-combustion was carried out. The nc-ThO2 powders were characterized for their bulk density, size distribution of particles, specific surface area, carbon residue and X-ray crystallite size. All these powders were compacted at pressures varying from 60 to 353 MPa and sintered by using the "two-step sintering" method. Powders prepared from a mixture with an "R" value of 0.125 compacted at 243 MPa yielded a maximum sintered density of 98.8 ± 0.3% T.D. For nc-ThO2, this is the highest sintered density reported so far. The microstructural investigations on nc-ThO2 powders were carried out by using both scanning electron microscopy (SEM) and transmission electron microscopy (TEM). SEM images of the sintered thoria monoliths revealed faceted grains with well defined grain boundaries. Shrinkage anisotropy factor (α) revealed that the compacts prepared from the powders obtained from starting mixtures with R values of 0.125-0.50 had undergone uniform sintering (near isotropic shrinkage).

One-step green synthesis and characterization of plant protein-coated mercuric oxide (HgO) nanoparticles: antimicrobial studies

NASA Astrophysics Data System (ADS)

Das, Amlan Kumar; Marwal, Avinash; Sain, Divya; Pareek, Vikram

2015-03-01

The present study demonstrates the bioreductive green synthesis of nanosized HgO using flower extracts of an ornamental plant Callistemon viminalis. The flower extracts of Callistemon viminalis seem to be environmentally friendly, so this protocol could be used for rapid production of HgO. Till date, there is no report of synthesis of nanoparticles using flower extract of Callistemon viminalis. Mercuric acetate was taken as the metal precursor in the present experiment. The flower extract was found to act as a reducing as well as a stabilizing agent. The phytochemicals present in the flower extract act as reducing agent which include proteins, saponins, phenolic compounds, phytosterols, and flavonoids. FT-IR spectroscopy confirmed that the extract had the ability to act as a reducing agent and stabilizer for HgO nanoparticles. The formation of the plant protein-coated HgO nanoparticles was first monitored using UV-Vis absorption spectroscopy. The UV-Vis spectroscopy revealed the formation of HgO nanoparticles by exhibiting the typical surface plasmon absorption maxima at 243 nm. The average particle size formed ranges from 2 to 4 nm. The dried form of synthesized nanoparticles was further characterized using TGA, XRD, TEM, and FTIR spectroscopy. FT-IR spectra of synthesized HgO nanoparticles were performed to identify the possible bio-molecules responsible for capping and stabilization of nanoparticles, which confirm the formation of plant protein-coated HgO nanoparticles that is further corroborated by TGA study. The optical band gap of HgO nanoparticle was measured to be 2.48 eV using cutoff wavelength which indicates that HgO nanoparticles can be used in metal oxide semiconductor-based photovoltaic cells. A possible core-shell structure of the HgO nanobiocomposite has been proposed.

Synthesis of anatase TiO2 nanoparticles with beta-cyclodextrin as a supramolecular shell.

PubMed

Li, Landong; Sun, Xiaohong; Yang, Yali; Guan, Naijia; Zhang, Fuxiang

2006-11-20

We report a novel, green hydrothermal-synthesis route to well-dispersed anatase TiO2 nanoparticles with particle sizes of 9-16 nm in the presence of beta-CD (beta-cyclodextrin). During the synthesis process, the CD-containing synthesis mixture assembled in both longitudinal and latitudinal directions. Driven by the interaction between molecules, the beta-CDs assembled in the longitudinal direction to form long-chain compounds, whereas in the latitudinal direction, they tended to form regular aggregates through coordination with the Ti species from the hydrolysis of tetrabutyl titanate. In view of the effect of the coordination and the steric hindrance of beta-CDs as a supramolecular shell, homogeneous nuclei and slow growth of TiO2 crystals during the synthesis process was observed, which was responsible for the formation of uniform TiO2 nanoparticles. The low beta-CD dosage and the high product yield (>90%) demonstrated well the potential of this synthesis route in the large-scale industrial production of anatase nanoparticles.

Sol–gel synthesis of SnO{sub 2}–MgO nanoparticles and their photocatalytic activity towards methylene blue degradation

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bayal, Nisha; Jeevanandam, P., E-mail: jeevafcy@iitr.ernet.in

2013-10-15

Graphical abstract: - Highlights: • A simple sol–gel method for the synthesis of SnO{sub 2}–MgO nanoparticles is reported. • Band gap of SnO{sub 2} can be tuned by varying the magnesium content in SnO{sub 2}–MgO. • SnO{sub 2}–MgO shows good photocatalytic activity towards degradation of methylene blue. - Abstract: SnO{sub 2}–MgO mixed metal oxide nanoparticles were prepared by a simple sol–gel method. The nanoparticles were characterized by power X-ray diffraction, scanning electron microscopy coupled with energy dispersive X-ray analysis, transmission electron microscopy and UV–vis diffuse reflectance spectroscopy. The XRD results indicate the formation of mixed metal oxide nanoparticles and alsomore » a decrease of SnO{sub 2} crystallite size in the mixed metal oxide nanoparticles with increasing magnesium oxide content. The reflectance spectroscopy results show a blue shift of the band gap of SnO{sub 2} in the mixed metal oxide nanoparticles. The photocatalytic activity of the SnO{sub 2}–MgO nanoparticles was tested using the photodegradation of aqueous methylene blue in the presence of sunlight. The results indicate that the mixed metal oxide nanoparticles possess higher efficiency for the photodegradation of methylene blue compared to pure SnO{sub 2} nanoparticles.« less

Synthesis and Characterization of SiO2@Y2MoO6:Eu3+ Core-Shell Structured Spherical Phosphors by Sol-Gel Process.

PubMed

Li, G Z; Liu, F H; Chu, Z S; Wu, D M; Yang, L B; Li, J L; Wang, M N; Wang, Z L

2016-04-01

SiO2@Y2MoO6:Eu3+ core-shell phosphors were prepared by the sol-gel process. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectra (EDS), transmission electron microscopy (TEM), photoluminescence (PL) spectra as well as kinetic decays were used to characterize the resulting SiO2@Y2MoO6:Eu3+ core-shell phosphors. The XRD results demonstrated that the Y2MoO6:Eu3+ layers on the SiO2 spheres crystallized after being annealed at 700 °C and the crystallinity increased with raising the annealing temperature. The obtained core-shell phosphors have spherical shape with narrow size distribution (average size ca. 640 nm), non-agglomeration, and smooth surface. The thickness of the Y2MoO6:Eu3+ shells on the SiO2 cores could be easily tailored by varying the number of deposition cycles (70 nm for four deposition cycles). The Eul+ shows a strong PL emission (dominated by 5D0-7F2 red emission at 614 nm) under the excitation of 347 nm UV light. The PL intensity of Eu3+ increases with increasing the annealing temperature and the number of coating cycles.

Unconventional Synthesis of γ-Fe2O3: Excellent Low-Concentration Ethanol Sensing Performance

NASA Astrophysics Data System (ADS)

Naskar, Atanu; Narjinary, Mousumi; Kundu, Susmita

2017-01-01

This study reports on a simple unconventional procedure for synthesis of γ-Fe2O3 nanopowder and its fabrication as a resistive ethanol sensor. γ-Fe2O3 powder having an average particle size of ˜15 nm was prepared by thermal decomposition of iron(III) acetylacetonate. Platinum incorporation (0.5-1.5 wt.%) was also carried out for enhancing sensing performance. The powders were characterized using an x-ray diffractometer, x-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area, field area scanning electron microscopy, transmission electron microscopy along with energy dispersion x-ray analyses. Sensor fabricated from pure γ-Fe2O3 exhibited excellent ethanol sensing performance at concentrations down to 1 ppm, having a great demand in medical diagnosis and food-processing industries. The response observed for pure γ-Fe2O3 (˜75% for 1 ppm ethanol) was enhanced ˜10% after 1 wt.% Pt impregnation. Sensors were quite stable and selective towards ethanol vapour detection. A possible mechanism for high sensing performance has been discussed.

Synthesis and evaluation of optical and antimicrobial properties of Ag-SnO2 nanocomposites

NASA Astrophysics Data System (ADS)

Kumar Nair, Kishore; Kumar, Promod; Kumar, Vinod; Harris, R. A.; Kroon, R. E.; Viljoen, Bennie; Shumbula, P. M.; Mlambo, M.; Swart, H. C.

2018-04-01

We report on the sol-gel based room temperature synthesis of undoped SnO2 and Ag-SnO2 nanostructures. The synthesized nanostructures were characterized by Fourier transform infrared spectroscopy, X-ray diffraction (XRD), Raman spectroscopy, High-resolution transmission electron microscopy (HR-TEM) and UV-visible spectroscopy. The XRD pattern confirmed that the obtained nanostructures have a tetragonally rutile structure. No extra phase changes were observed after Ag doping. UV-visible spectroscopy measurements indicated that the band gap of 3.59 eV for pure SnO2 nanostructures, decreased to 3.39 eV after doping. TEM analysis showed that no regular shape morphology existed and some rod-shaped particles were also detected in the nanostructures. The antibacterial activity of the nanostructures against E. coli was evaluated and a continuous decrease of microbial count was observed. The microbial population decreased from 6 × 105 cfu/ml to 7 × 104 cfu/ml and 5 × 104 cfu/ml on SnO2 and Ag-SnO2 treatments, respectively. Thus, the nanostructures can be used for the biorational management of E. coli for waste water treatment before discharge.

Synthesis and characterization of Y2O3 nano-material: An experimental and theoretical study

NASA Astrophysics Data System (ADS)

Ahmad, Sheeraz; Faizan, Mohd; Ahmad, Shabbir; Ikram, Mohd

2018-04-01

We made an attempt to synthesize pure Y2O3 nanomaterial by using the sol-gel method followed by annealing at 600°C and 900°C. The synthesized Y2O3 nanoparticle was characterized by using XRD, FTIR, and UV-Vis spectroscopy. The structural refinement was performed using FULLPROF software by the Rietveld method. The refinement parameters such as lattice constant, atomic position, occupancy, R-factor and goodness of fit (χ2) were calculated. The nanoparticle has a single phase cubic structure with Ia -3 space group. The main absorption band in FTIR spectra centered at 560 cm-1 is attributed to Y-O vibration while the broadband at 3450 cm-1 arises due to O-H vibration. The band gap was obtained from the reflectance spectra using the K-M function F(R∞). The optimized structural parameters and UV-Vis spectrum were calculated using DFT and TD-DFT/B3LYP methods in bulk phase of Y2O3 and compared with experimental UV-Vis spectra in nanophase.

Synthesis of nanocrystalline TiO 2 in toluene by a solvothermal route

NASA Astrophysics Data System (ADS)

Kim, Chung-Sik; Moon, Byung Kee; Park, Jong-Ho; Tae Chung, Su; Son, Se-Mo

2003-07-01

A solvothermal synthetic method to TiO 2 nanoparticles has been investigated in toluene solutions with titanium isopropoxide (TIP) as precursor. Weight ratios of precursor to solvent prepared in the mixture are 5/100, 10/100, 20/100, 30/100 and 40/100. At the weight ratio of 10/100, 20/100 and 30/100, TiO 2 nanocrystalline particles were obtained after synthesis at 250°C for 3 h in an autoclave. X-ray diffraction and tranmission electron microscopy shows that the product has uniform anatase structure with average particle size below 20 nm. As the composition of TIP in the solution increases, the particle size of TiO 2 powder tends to increase. At 5/100 and 40/100, however, pale yellow colloidal solution is obtained after synthesis and crystalline phase of TiO 2 is not produced. The specific surface area of the TiO 2 nanocrystalline powder was also investigated using BET surface area analyzer.

Subsurface synthesis and characterization of Ag nanoparticles embedded in MgO

NASA Astrophysics Data System (ADS)

Vilayurganapathy, S.; Devaraj, A.; Colby, R.; Pandey, A.; Varga, T.; Shutthanandan, V.; Manandhar, S.; El-Khoury, P. Z.; Kayani, Asghar; Hess, W. P.; Thevuthasan, S.

2013-03-01

Metal nanoparticles exhibit a localized surface plasmon resonance (LSPR) which is very sensitive to the size and shape of the nanoparticle and the surrounding dielectric medium. The coupling between the electromagnetic radiation and the localized surface plasmon in metallic nanoparticles results in a sizable enhancement of the incident fields, making them possible candidates for plasmonic applications. In particular, partially exposed metallic nanoparticles distributed in a dielectric matrix can provide prime locations for LSPR spectroscopy and sensing. We report the synthesis and characterization of a plasmonic substrate consisting of Ag nanoparticles partially buried in MgO. Ag nanoparticles of different shapes and size distributions were synthesized below the surface of MgO by implanting 200 keV Ag+ ions followed by annealing at 1000 °C for 10 and 30 h. A detailed optical and structural characterization was carried out to understand the evolution of the Ag nanoparticle and size distribution inside the MgO matrix. Micro x-ray diffraction (Micro-XRD) was employed to investigate the structural properties and estimate the crystallite size. The nanoparticles evolved from a spherical to a faceted morphology with annealing time, assuming an octahedral shape truncated at the (001) planes, as visualized from aberration-corrected transmission electron microscopy (TEM) images. The nanoparticles embedded in MgO were shown to be pure metallic Ag using atom probe tomography (APT). The nanoparticles were partially exposed to the surface by employing plasma etch techniques to remove the overlaying MgO. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were employed to study the surface morphology and obtain a height distribution for the partially exposed nanoparticles.

Facile synthesis of SnO2/α-Fe2O3 nanocomposite for supercapacitor capacitor applications

NASA Astrophysics Data System (ADS)

Rani, B. Jansi; Saravanakumar, B.; Ravi, G.; Yuvakkumar, R.

2018-05-01

Facile and economically viable one step hydrothermal route was adapted to synthesis SnO2/α-Fe2O3 nanocomposite with and without hexamine (HMT) as surfactant successfully. The formation of SnO2/α-Fe2O3 nanocomposite was confirmed through XRD, Raman, PL and FTIR studies. The presence of well defined XRD diffraction peaks of both SnO2 and α-Fe2O3 revealed the formation SnO2/α-Fe2O3 nanocomposite. The obtained characteristic Raman active (Eg+Eg+Eu+A2u) mode of vibrations confirmed the formation of SnO2/α-Fe2O3 nanocomposite. Photoluminescence study revealed the emission behavior of the product. Metal oxygen vibrations of Fe-O in both octahedral, tetrahedral sites and Sn-O were confirmed by the bands located at 466, 580 and 673 cm-1 respectively through FTIR. The spherical morphology of the product synthesized with and without the surfactant HMT has been revealed by SEM images. The electrochemical behavior of the product was investigated through CV and EIS studies in 1M Na2SO4 electrolyte solution and obtained the highest specific capacitance of 211.25 F/g at 5 mV for the surfactant assisted product.

Synthesis of Hollow Nanotubes of Zn2SiO4 or SiO2: Mechanistic Understanding and Uranium Adsorption Behavior.

PubMed

Tripathi, Shalini; Bose, Roopa; Roy, Ahin; Nair, Sajitha; Ravishankar, N

2015-12-09

We report a facile synthesis of Zn2SiO4 nanotubes using a two-step process consisting of a wet-chemical synthesis of core-shell ZnO@SiO2 nanorods followed by thermal annealing. While annealing in air leads to the formation of hollow Zn2SiO4, annealing under reducing atmosphere leads to the formation of SiO2 nanotubes. We rationalize the formation of the silicate phase at temperatures much lower than the temperatures reported in the literature based on the porous nature of the silica shell on the ZnO nanorods. We present results from in situ transmission electron microscopy experiments to clearly show void nucleation at the interface between ZnO and the silica shell and the growth of the silicate phase by the Kirkendall effect. The porous nature of the silica shell is also responsible for the etching of the ZnO leading to the formation of silica nanotubes under reducing conditions. Both the hollow silica and silicate nanotubes exhibit good uranium sorption at different ranges of pH making them possible candidates for nuclear waste management.

Facile synthesis and characterization of N-doped TiO2/C nanocomposites with enhanced visible-light photocatalytic performance

NASA Astrophysics Data System (ADS)

Jia, Tiekun; Fu, Fang; Yu, Dongsheng; Cao, Jianliang; Sun, Guang

2018-02-01

Ultrafine anatase N-doped TiO2 nanocrystals modified with carbon (denoted as N-doped TiO2/C) were successfully prepared via a facile and low-cost approach, using titanium tetrachloride, aqueous ammonia and urea as starting materials. The phase composition, surface chemical composition, morphological structure, electronic and optical properties of the as-prepared photocatalysts were well characterized and analyzed. On the basis of Raman spectral characterization combining with the results of X-ray photoelectron spectroscopy (XPS) and high resolution transmission electron microscopy (HRTEM), it could be concluded that N dopant ions were successfully introduced into TiO2 crystal lattice and carbon species were modified on the surface or between the nanoparticles to form N-doped TiO2/C nanocomposites. Compared with that of bare TiO2, the adsorption band edge of N-doped TiO2/C nanocomposites were found to have an evident red-shift toward visible light region, implying that the bandgap of N-doped TiO2/C nanocomposites is narrowed and the visible light absorption capacity is significantly enhanced due to N doping and carbon modification. The photoactivity of the as-prepared photocatalytsts was tested by the degradation of Rhodamine B (RhB) under visible light (λ > 420 nm), and the results showed that the N-doped TiO2/C nanocomposites exhibited much higher photodegradation rate than pure TiO2 and N-doped TiO2, which was mainly attributed to the synergistic effect of the enhanced light harvesting, augmented catalytic active sites and efficient separation of photogenerated electron-hole pairs.

Chemoenzymatic synthesis and structural characterization of 2-O-sulfated glucuronic acid-containing heparan sulfate hexasaccharides

PubMed Central

Hsieh, Po-Hung; Xu, Yongmei; Keire, David A; Liu, Jian

2014-01-01

Heparan sulfate and heparin are highly sulfated polysaccharides that consist of a repeating disaccharide unit of glucosamine and glucuronic or iduronic acid. The 2-O-sulfated iduronic acid (IdoA2S) residue is commonly found in heparan sulfate and heparin; however, 2-O-sulfated glucuronic acid (GlcA2S) is a less abundant monosaccharide (∼<5% of total saccharides). Here, we report the synthesis of three GlcA2S-containing hexasaccharides using a chemoenzymatic approach. For comparison purposes, additional IdoA2S-containing hexasaccharides were synthesized. Nuclear magnetic resonance analyses were performed to obtain full chemical shift assignments for the GlcA2S- and IdoA2S-hexasaccharides. These data show that GlcA2S is a more structurally rigid saccharide residue than IdoA2S. The antithrombin (AT) binding affinities of a GlcA2S- and an IdoA2S-hexasaccharide were determined by affinity co-electrophoresis. In contrast to IdoA2S-hexasaccharides, the GlcA2S-hexasaccharide does not bind to AT, confirming that the presence of IdoA2S is critically important for the anticoagulant activity. The availability of pure synthetic GlcA2S-containing oligosaccharides will allow the investigation of the structure and activity relationships of individual sites in heparin or heparan sulfate. PMID:24770491

Microwave Synthesis of BCNO/SiO2 Nanocomposite Material

NASA Astrophysics Data System (ADS)

Faryuni, I. D.; Ramdhani, F.; Sampurno, J.; Nuryadin, B. W.; Noor, F. A.; Iskandar, F.

2017-07-01

In the present work, we report the preparation of BCNO/SiO2 phosphor synthesized using a microwave-assisted method. This method allows a lower temperature and a shorter reaction time than simple heating (furnace). The phosphors were prepared from precursors containing, boric acid, urea, citric acid and SiO2 nanoparticles. To These precursors, silica nanoparticles were added at various concentrations from 0 to 5 %wt. The emission wavelength produced by the phosphor was varied by varying the fraction mass of the silica that were added to the precursors. The results showed that higher photoluminescence (PL) intensity was produced by the BCNO/SiO2 with 3 %wt silica addition. The novelty of this research is using microwave heating for BCNO/SiO2 synthesis, which is usually conducted using a simple heating method.

Spectroscopic characterization approach to study surfactants effect on ZnO 2 nanoparticles synthesis by laser ablation process

NASA Astrophysics Data System (ADS)

Drmosh, Q. A.; Gondal, M. A.; Yamani, Z. H.; Saleh, T. A.

2010-05-01

Zinc peroxide nanoparticles having grain size less than 5 nm were synthesized using pulsed laser ablation in aqueous solution in the presence of different surfactants and solid zinc target in 3% H 2O 2. The effect of surfactants on the optical and structure of ZnO 2 was studied by applying different spectroscopic techniques. Structural properties and grain size of the synthesized nanoparticles were studied using XRD method. The presence of the cubic phase of zinc peroxide in all samples was confirmed with XRD, and the grain sizes were 4.7, 3.7, 3.3 and 2.8 nm in pure H 2O 2, and H 2O 2 mixed with SDS, CTAB and OGM respectively. For optical characterization, FTIR transmittance spectra of ZnO 2 nanoparticles prepared with and without surfactants show a characteristic ZnO 2 absorption at 435-445 cm -1. FTIR spectrum revealed that the adsorbed surfactants on zinc peroxide disappeared in case of CTAB and OGM while it appears in case of SDS. This could be due to high critical micelles SDS concentration comparing with others which is attributed to the adsorption anionic nature of this surfactant. Both FTIR and UV-vis spectra show a red shift in the presence of SDS and blue shift in the presence of CTAB and OGM. The blue shift in the absorption edge indicates the quantum confinement property of nanoparticles. The zinc peroxide nanoparticles prepared in additives-free media was also characterized by Raman spectra which show the characteristic peaks at 830-840 and 420-440 cm -1.

Characterization and properties of TiO2-SnO2 nanocomposites, obtained by hydrolysis method

NASA Astrophysics Data System (ADS)

Kutuzova, Anastasiya S.; Dontsova, Tetiana A.

2018-04-01

The paper deals with the process of TiO2-SnO2 nanocomposites synthesis utilizing simple hydrolysis method with further calcination for photocatalytic applications. The obtained nanopowders contain 100, 90, 75, 65 and 25 wt% of TiO2. The synthesized nanocomposite samples were analyzed by X-ray diffraction method, scanning electron microscopy, transmission electron microscopy, Fourier transform infrared spectroscopy and N2 adsorption-desorption method. The correlation between structure and morphology of the obtained nanocrystalline composite powders and their sorption and photocatalytic activity towards methylene blue degradation was established. It was found that the presence of SnO2 in the nanocomposites stabilizes the anatase phase of TiO2. Furthermore, sorption and photocatalytic properties of the obtained composites are significantly influenced not only by specific surface area, but also by pore size distribution and mesopore volume of the samples. In our opinion, the results obtained in this study have shown that the TiO2-SnO2 composites with SnO2 content that does not exceed 10% are promising for photocatalytic applications.

Tin-Assisted Synthesis of ɛ -Ga2O3 by Molecular Beam Epitaxy

NASA Astrophysics Data System (ADS)

Kracht, M.; Karg, A.; Schörmann, J.; Weinhold, M.; Zink, D.; Michel, F.; Rohnke, M.; Schowalter, M.; Gerken, B.; Rosenauer, A.; Klar, P. J.; Janek, J.; Eickhoff, M.

2017-11-01

The synthesis of ɛ -Ga2O3 and β -Ga2O3 by plasma-assisted molecular beam epitaxy on (001 )Al2O3 substrates is studied. The growth window of β -Ga2O3 in the Ga-rich regime, usually limited by the formation of volatile gallium suboxide, is expanded due to the presence of tin during the growth process, which stabilizes the formation of gallium oxides. X-ray diffraction, transmission electron microscopy, time-of-flight secondary-ion mass spectrometry, Raman spectroscopy, and atomic force microscopy are used to analyze the influence of tin on the layer formation. We demonstrate that it allows the synthesis of phase-pure ɛ -Ga2O3 . A growth model based on the oxidation of gallium suboxide by reduction of an intermediate sacrificial tin oxide is suggested.

Synthesis, characterization and antibacterial activity of colloidal NiO nanoparticles.

PubMed

Khashan, Khawlah Salah; Sulaiman, Ghassan Mohammad; Abdul Ameer, Farah Abdul Kareem; Napolitano, Giuliana

2016-03-01

The Colloidal solutions of nickel oxide (NiO) nanoparticles synthesized via Nd-Yag pulse ablation of nickel immersed in H2O were studied. The created nanoparticles were characterized by UV-VIS absorption, Fourier transform infrared spectroscopy (FTIR) and transmission electron microscope (TEM). FTIR characterization confirms the formation of nickel oxide nanoparticles. The optical band gap values, determined by UV-VIS absorption measurements, are found to be (4.5 ev). TEM shows that nanoparticles size ranged from 2-21 nm. The antimicrobial activity was carried out against pseudomonas aurogenisa, Escherichia coli (gram negative bacteria), Staphylococcus aureus and Streptococcus pneumonia (gram positive bacteria). The NiO nanoparticles showed inhibitory activity in both strains of bacteria with best selectivity against gram-positive bacteria. The findings of present study indicate that NiO nanoparticles could potentiate the permeability of bacterial cell wall, and remarkably increase the accumulation of amoxicillin in bacteria, suggesting that NiO nanoparticles together with amoxicillin would facilitate the synergistic impact on growth inhibition of bacterial strains.

Synthesis and characterization of mangan oxide coated sand from Capkala kaolin

NASA Astrophysics Data System (ADS)

Destiarti, Lia; Wahyuni, Nelly; Prawatya, Yopa Eka; Sasri, Risya

2017-03-01

Synthesis and characterization of mangan oxide coated sand from quartz sand fraction of Capkala kaolin has been conducted. There were two methods on synthesis of Mangan Oxide Coated Sand (MOCS) from Capkala Kaolin compared in this research. Characterization of MOCS was done by using Scanning Electron Microscope/Energy Dispersive X-Ray Spectrometer (SEM/EDX) and X-Ray Diffraction (XRD). The MOCS was tested to reduce phosphate in laundry waste. The result showed that the natural sand had bigger agregates and a relatively uniform structural orientation while both MOCS had heterogen structural orientation and manganese oxide formed in cluster. Manganese in first and second methods were 1,93% and 2,63%, respectively. The XRD spectrum showed clear reflections at 22,80°, 36,04°, 37,60° and a broad band at 26,62° (SiO2). Based on XRD spectrum, it can be concluded that mineral constituents of MOCS was verified corresponding to pyrolusite (MnO2). The former MOCS could reduce almost 60% while the later could reduce 70% phosphate in laundry waste.

Role of alkali carbonate and salt in topochemical synthesis of K1/2Na1/2NbO3 and NaNbO3 templates

NASA Astrophysics Data System (ADS)

Lee, Jae-Seok; Jeon, Jae-Ho; Choi, Si-Young

2013-11-01

Since the properties of lead-free piezoelectric materials have thus far failed to meet those of lead-based materials, either chemical doping or morphological texturing should be employed to improve the piezoelectric properties of lead-free piezoelectric ceramics. The goal of this study was to synthesize plate-like K1/2Na1/2NbO3 and NaNbO3 particles, which are the most favorable templates for morphological texturing of K1/2Na1/2NbO3 ceramics. To achieve this goal, Bi2.5Na3.5Nb5O18 precursors in a plate-like shape were first synthesized and subsequently converted into K1/2Na1/2NbO3 or NaNbO3 particles that retain the morphology of Bi2.5Na3.5Nb5O18. In this study, we found that sodium or potassium carbonate does not play a major role in converting the Bi2.5Na3.5Nb5O18 precursor to K1/2Na1/2NbO3 or NaNbO3, on the contrary to previous reports; however, the salt contributes to the conversion reaction. All synthesis processes have been performed via a molten salt method, and scanning electron microscopy, scanning probe microscopy, and inductively coupled plasma mass spectroscopy were used to characterize the synthesized K1/2Na1/2NbO3 or NaNbO3 templates.

Ga2O3 and GaN nanocrystalline film: reverse micelle assisted solvothermal synthesis and characterization.

PubMed

Sinha, Godhuli; Ganguli, Dibyendu; Chaudhuri, Subhadra

2008-03-01

Gallium oxide (beta-Ga2O3) nanoparticles were successfully deposited on quartz glass substrates using sodium bis(2-ethylhexyl) sulfosuccinate (AOT)/n-hexane/ethylene glycol monomethyl ether (EGME) reverse micelle-mediated solvothermal process with different omega values. The mean diameter of Ga2O3 particles was approximately 2-3 nm and found to be approximately independent of omega values of the reverse micelles. However, when the Ga2O3 nanocrystalline films were nitrided at 900 degrees C under flowing NH3 atmosphere for 1 h, the mean diameter of the resulted gallium nitride (wurtzite-GaN) nanoparticles varied from 3-9 nm. Both nanocrystalline films of Ga2O3 and GaN were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR) spectroscopy, UV-vis spectroscopy and photoluminescence in order to study their chemical and physical properties explicitly.

Synthesis and optical properties modulation of ZnO/Eu2O3 nanocable arrays

NASA Astrophysics Data System (ADS)

Yang, Lei; She, Yajuan; Zhao, Shihua; Yue, Shihai; Wang, Qian; Hu, Aiping; Zhang, Wei

2010-11-01

White-light-emitting materials have attracted considerable attention because of their applications, such as large-surface emitting devices and displays. However, simply mixing nanoparticles would result in uneven color. Nanocables are expected to improve the chemical stability and color uniformity. Herein we demonstrate the synthesis of Eu2O3/ZnO nanocable arrays embedded in anodic alumina template via a versatile, simple, and cheap method. In order to control the composition of the cable with low cost, a two-step synthesis including an electric field deposition and a sol-gel template approach is used to fabricate the nanocable. The product is investigated by x-ray powder diffraction, transmission electron microscopy, selected area electron diffraction, and photoluminescence (PL) spectrum. The results show that ordered Eu2O3/ZnO nanocable arrays with an average inside diameter of 20-40 nm and wall thickness of 20-40 nm were prepared. By adjusting the excitation wavelength, change of the emitting color of the cables from blue to white could be obtained. Energy and charge transfer were found by investigating the electronic transition and recombination in the PL process. These arrays are promising for applications in display, white phosphors, and ultraviolet detectors owing to the special optical properties. And this method may be of much significance in the synthesis of nanocables with the controllable composition.

Synthesis, characterization and low temperature electrical conductivity of Polyaniline/NiFe2O4 nanocomposites

NASA Astrophysics Data System (ADS)

Prasanna, G. D.; Prasad, V. B.; Jayanna, H. S.

2015-02-01

Conducting polymer/ferrite nanocomposites with an organized structure provide a new functional hybrid between organic and inorganic materials. The most popular among the conductive polymers is the polyaniline (PANI) due to its wide application in different fields. In the present work nickel ferrite (NiFe2O4) nanoparticles were prepared by sol-gel citrate-nitrate method with an average size of 21.6nm. PANI/NiFe2O4 nanoparticles were synthesized by a simple general and inexpensive in-situ polymerization in the presence of NiFe2O4 nanoparticles. The effects of NiFe2O4 nanoparticles on the dc-electrical properties of polyaniline were investigated. The structural components in the nanocomposites were identified from Fourier Transform Infrared (FTIR) spectroscopy. The crystalline phase of nanocomposites was characterized by X-Ray Diffraction (XRD). The Scanning Electron Micrograph (SEM) reveals that there was some interaction between the NiFe2O4 particles and polyaniline and the nanocomposites are composed of polycrystalline ferrite nanoparticles and PANI. The dc conductivity of polyaniline/NiFe2O4 nanocomposites have been measured as a function of temperature in the range of 80K to 300K. It is observed that the room temperature conductivity cRT decreases with increase in the relative content of NiFe2O4. The experimental data reveals that the resistivity increases for all composites with decrease of temperature exhibiting semiconductor behaviour.

Theoretical study of the promotional effect of ZrO2 on In2O3 catalyzed methanol synthesis from CO2 hydrogenation

NASA Astrophysics Data System (ADS)

Zhang, Minhua; Dou, Maobin; Yu, Yingzhe

2018-03-01

Methanol synthesis from CO2 hydrogenation on the ZrO2 doped In2O3(110) surface (Zr-In2O3(110)) with oxygen vacancy has been studied using the density functional theory calculations. The calculated results show that the doped ZrO2 species prohibits the excessive formation of oxygen vacancies and dissociation of H2 on In2O3 surface slightly, but enhances the adsorption of CO2 on both perfect and defective Zr-In2O3(110) surface. Methanol is formed via the HCOO route. The hydrogenation of CO2 to HCOO is both energetically and kinetically facile. The HCOO hydrogenates to polydentate H2CO (p-H2CO) species with an activation barrier of 0.75 eV. H3CO is produced from the hydrogenation of monodentate H2CO (mono-H2CO), transformation from p-H2CO with 0.82 eV reaction energy, with no barrier whether there is hydroxyl group between the mono-H2CO and the neighboring hydride or not. Methanol is the product of H3CO protonation with 0.75 eV barrier. The dissociation and protonation of CO2 are both energetically and kinetically prohibited on Zr-In2O3(110) surface. The doped ZrO2 species can further enhance the adsorption of all the intermediates involved in CO2 hydrogenation to methanol, activate the adsorbed CO2 and H2CO, and stabilize the HCOO, H2CO and H3CO, especially prohibit the dissociation of H2CO or the reaction of H2CO with neighboring hydride to form HCOO and gas phase H2. All these effects make the ZrO2 supported In2O3 catalyst exhibit higher activity and selectivity on methanol synthesis from CO2 hydrogenation.

Fe3O4 nanocubes assembled on RGO nanosheets: Ultrasound induced in-situ and eco-friendly synthesis, characterization and their excellent catalytic performance for the production of liquid fuel in Fischer-tropsch synthesis.

PubMed

Abbas, Mohamed; Zhang, Juan; Lin, Ke; Chen, Jiangang

2018-04-01

In this study, Fe 3 O 4 nanocubes (NCs) decorated on RGO nanosheets (NSs) structures were successfully synthesized through an innovative and environmentally-friendly rapid sonochemical method. More importantly, iron(II) sulfate heptahydrate and GO were employed as precursors and water as reaction medium, meanwhile, NaOH within the generated free radicals from the high intensity ultrasound were sufficient as reducing and base agent in our clean synthesis. Moreover, the hydrothermal method as a conventional approach was employed to synthesize the same catalysts for the comparison with the ultrasonocation technique. The as-synthesized Fe 3 O 4 and RGO/Fe 3 O 4 NSs catalysts were exposed to industrially relevant Fischer-tropsch synthesis (FTS) conditions at various reaction temperatures (250-290 °C), and they subjected to fully characterization before and after FTS reaction using XRD, TEM, HRTEM, EDS mapping, XPS, FTIR, BET, H 2 -TPR, H 2 -TPD and CO-TPD to understand the structure-performance relationships. Notably, the catalysts produced using the sonochemical method had a better CO conversion rate [Fe 3 O 4 (80%), RGO/Fe 3 O 4 (82%)] than the hydrothermally synthesized catalysts. However, compared to the naked-Fe 3 O 4 catalysts, the sonochemically and hydrothermally synthesized RGO-supported Fe 3 O 4 catalysts had higher long chain hydrocarbon (C5+) selectivity values (72% and 67%) and C 2 -C 4 olefin/paraffin selectivity ratio (3.2 and 2) and low CH4 selectivity values (6% and 8.5%), respectively. This can be attributed to their high surface area, the degree of reducibility, and content of Hägg iron carbide (χ-Fe 5 C 2 ) as the most active phase of the FTS reaction. Proposed reaction mechanisms for the sonochemical and hydrothermal reaction synthesis of Fe 3 O 4 and RGO/Fe 3 O 4 nanoparticles are discussed. In conclusion, our developed surfactantless-sonochemical method holds promise for the eco-friendly synthesis of highly efficient catalysts materials for

Chemoenzymatic convergent synthesis of 2'-O,4'-C-methyleneribonucleosides.

PubMed

Sharma, Vivek K; Kumar, Manish; Olsen, Carl E; Prasad, Ashok K

2014-07-03

Novozyme-435-catalyzed efficient regioselective acetylation of one of the two diastereotopic hydroxymethyl functions in 3-O-benzyl-4-C-hydroxymethyl-1,2-O-isopropylidene-α-d-ribofuranose has been achieved. The enzymatic methodology has been successfully utilized for convergent synthesis of bicyclic nucleosides (LNA monomers) T, U, A, and C. Further, it has been demonstrated that Novozyme-435 can be used for 10 cycles of the acylation reaction without losing selectivity and efficiency.

Synthesis and characterization of YBaCu2O5-δ compound

NASA Astrophysics Data System (ADS)

Ehsandoust, A.; Sandoghchi, M.; Mokhtari, P.; Akhavan, M.

2018-05-01

YBaCu2O5 compound as one of the possible microstructures of Y3Ba5Cu8O19 has been synthesized. The X-ray diffraction analysis of this compound indicates that its formation is accompanied with the formation of YBa2Cu3O7-δ. The observed superconductivity around ∼92 K supports this. So, it seems that YBa2Cu3O7-δ is responsible for the observed superconductivity in YBaCu2O5, and this phase is not an independent superconducting phase. Consequently, the overall effect of the YBaCu2O5 formation during the Y3Ba5Cu8O19 fabrication process could be a reduction in Tc.

Synthesis, structural properties and catalytic activity of MgO-SnO2 nanocatalysts

NASA Astrophysics Data System (ADS)

Perveen, Hina; Farrukh, Muhammad Akhyar; Khaleeq-ur-Rahman, Muhammad; Munir, Badar; Tahir, Muhammad Ashraf

2015-01-01

Surfactant controlled synthesis of magnesium oxide-tin oxide (MgO-SnO2) nanocatalysts was carried out via the hydrothermal method. Concentration of sodium dodecyl sulfate (SDS) was varied while all other reaction conditions were kept constant same for this purpose. Furthermore, MgO-SnO2 nanocatalysts were also prepared by changing the precursor's concentration. These precursors are magnesium nitrate Mg(NO3)2 · 6H2O and tin chloride (SnCl4 · 5H2O). The influence of these reaction parameters on the sizes and morphology of the nanocatalysts were studied by using Fourier transform infrared (FTIR) spectroscopy, Scanning electron microscopy-Energy dispersive X-ray (SEM-EDX), Powder X-ray diffraction (XRD), Transmission electron microscopy and Thermo gravimetric analysis (TGA). The catalytic efficiency of MgO-SnO2 was checked against 2,4-dinitrophenylhydrazine (DNPH), which is an explosive compound. The nanocatalysts were found as a good catalyst to degrade the DNPH. Catalytic activity of nanocatalysts was observed up to 19.13% for the degradation DNPH by using UV-spectrophotometer.

Preparation and characterization of [H2-DABCO][ClO4]2 as a new member of DABCO-based ionic liquids for the synthesis of pyrimido[4,5-b]-quinoline and pyrimido[4,5-d]pyrimidine derivatives

NASA Astrophysics Data System (ADS)

Shirini, Farhad; Langarudi, Mohaddeseh Safarpoor Nikoo; Daneshvar, Nader; Jamasbi, Negar; Irankhah-Khanghah, Mahsa

2018-06-01

[H2-DABCO][ClO4]2, as a novel DABCO-based ionic liquid, has been synthesized, characterized, and used as an affordable and recyclable catalyst in the synthesis of pyrimido [4,5-b]-quinoline and pyrimido [4,5-d]pyrimidine derivatives. The procedure shows several advantages over the previous methods such as simplicity, high yields, short reaction times, easy work-up, and use of a non-metal catalyst. Moreover, this paper virtually debates the impact of anions and cations on moisture-resistant property and catalytic activity in DABCO-based ionic liquids through the comparison of [DABCO](SO3H)2(Cl)2, [DABCO](SO3H)2(HSO4)2, [H2-DABCO][H2PO4]2, [H2-DABCO][HSO4]2, and [H2-DABCO][ClO4]2.

Organic-Free, ZnO-Assisted Synthesis of Zeolite FAU with Tunable SiO2 /Al2 O3 Molar Ratio.

PubMed

Guo, Ya; Sun, Tianjun; Gu, Yiming; Liu, Xiaowei; Ke, Quanli; Wang, Shudong

2018-05-04

Zeolite FAU with tunable SiO 2 /Al 2 O 3 molar ratio has been successfully synthesized in the absence of organic structure-directing agents (OSDA). Specifically, the addition of zinc species contributes to the feasible and effective adjustment of the framework SiO 2 /Al 2 O 3 molar ratio between about 4 and 6 depending on the amount of zinc species added in the batch composition. In contrast, a typical OSDA such as tetramethylammonium hydroxide (TMAOH) has a limited effect on the SiO 2 /Al 2 O 3 molar ratio of the zeolite. The role of zinc species is essential for the crystallization of zeolite FAU with a higher SiO 2 /Al 2 O 3 molar ratio under the particular synthesis conditions. It is speculated that zinc species may suppress the incorporation of aluminum into the aluminosilicate framework, which is due to the Coulombic repulsive interaction. A higher SiO 2 /Al 2 O 3 molar ratio is also found to be accompanied by a lower CO 2 adsorption heat for CO 2 /CH 4 separation. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrasound-assisted sol-gel synthesis of ZrO2.

PubMed

Guel, Marlene Lariza Andrade; Jiménez, Lourdes Díaz; Hernández, Dora Alicia Cortés

2017-03-01

Synthesis of tetragonal ZrO 2 by both conventional sol-gel and ultrasound-assisted sol-gel methods and using a non-ionic surfactant Tween-20, was performed. A porous microstructure composed of nanometric particles was observed. Tetragonal ZrO 2 was obtained using a low heat treatment temperature of powders, 500°C by both methods. A higher crystallinity and a shorter reaction time were observed when ultrasound was used in the sol-gel method due to the cavitation phenomenon. Copyright © 2016 Elsevier B.V. All rights reserved.

[Zn(phen)(O,N,O)(H2O)] and [Zn(phen)(O,N)(H2O)] with O,N,O is 2,6-dipicolinate and N,O is L-threoninate: synthesis, characterization, and biomedical properties.

PubMed

Chin, Lee-Fang; Kong, Siew-Ming; Seng, Hoi-Ling; Tiong, Yee-Lian; Neo, Kian-Eang; Maah, Mohd Jamil; Khoo, Alan Soo-Beng; Ahmad, Munirah; Hor, Tzi-Sum Andy; Lee, Hong-Boon; San, Swee-Lan; Chye, Soi-Moi; Ng, Chew-Hee

2012-10-01

Two ternary Zn(II) complexes, with 1,10-phenanthroline (phen) as the main ligand and a carboxylate-containing ligand [dipicolinate (dipico) or L-threoninate (L-Thr)] as the subsidiary ligand, were prepared and characterized by elemental analysis, Fourier transform IR, UV, and fluorescence spectroscopy, X-ray diffraction, molar conductivity, and electrospray ionization mass spectrometry. X-ray structure analysis shows that both [Zn(phen)(dipico)(H(2)O)]·H(2)O (1) and [Zn(phen)(L-Thr)(H(2)O)Cl]·2H(2)O (2) have octahedral geometry about the Zn(II) atom. Both complexes can inhibit topoisomerase I, and have better anticancer activity than cisplatin against nasopharyngeal cancer cell lines, HK1 and HONE-1, with concentrations causing 50 % inhibition of cell proliferation (IC(50)) in the low micromolar range. Complex 2 has the highest therapeutic index for HK1. Both Zn(II) complexes can induce cell death by apoptosis. Changing the subsidiary ligand in the Zn(II) complexes affects the UV-fluorescence spectral properties of the coordinated phen ligand, the binding affinity for some DNA sequences, nucleobase sequence-selective binding, the phase at which cell cycle progression was arrested for treated cancer cells, and their therapeutic index.

Synthesis, structure, optical, photoluminescence and magnetic properties of K2[Co(C2O4)2(H2O)2]·4H2O

NASA Astrophysics Data System (ADS)

Narsimhulu, M.; Hussain, K. A.

2018-06-01

The synthesis, crystal structure, optical, photoluminescence and magnetic behaviour of potassium bis(oxalato)cobaltate(II)tertrahydrate{K2[Co(C2O4)2(H2O)2]·4H2O} are described. The compound was grown at room temperature from mixture of aqueous solutions by slow evaporation method. The X-ray crystallographic data showed that the compound belongs to the monoclinic crystal system with P21/n space group and Z = 4. The UV-visible diffuse absorbance spectra exhibited bands at 253, 285 and 541 nm in the visible and ultraviolet regions. The optical band gap of the compound was estimated as 3.4 eV. At room temperature, an intense photoluminescence was observed from this material around 392 nm when it excited at 254 nm. The variable temperature dc magnetic susceptibility measurements exposed paramagnetic behaviour at high temperatures and antiferromagnetic ordering at low temperatures.

Synthesis and characterization of Ag+ ion conducting glassy electrolytes

NASA Astrophysics Data System (ADS)

Chandra, Angesh; Bhatt, Alok; Chandra, Archana

2013-07-01

Synthesis and characterization of new Ag+ ion conducting glassy systems: x[0.75AgI:0.25AgC1]: (1 - x)[Ag2O:P2O5], where 0.1 < x < 1 in molar weight fraction, are reported. The present glassy electrolytes have been synthesized by melt-quench technique using a high-speed twin roller-quencher. An alternate host salt: "quenched [0.75AgI:0.25AgC1] mixed system/solid solution", has been used in place of the traditional host AgI. The compositional dependence conductivity studies on the glassy systems: x[0.75AgI:0.25AgC1]:(1 - x)[Ag2O:P2O5] as well as xAgI:(1 - x)[Ag2O:P2O5] prepared identically, indicated that the composition at x = 0.75 exhibited the highest room temperature conductivity (σ ~ 5.5 x 10-3 S cm-1). The composition: 0.75[0.75AgI:0.25AgC1]:0.25[Ag2O:P2O5] has been referred to as optimum conducting composition (OCC). The some basic ion transport parameters viz. ionic conductivity (σ), ionic mobility (μ), mobile ion concentration (n), ionic drift velocity (vd), ion transference number (tion) and activation energy (Ea) values have been characterized with the help of various experimental techniques. A solid state battery was fabricated and its basic cell parameters calculated.

Synthesis and Characterization of Thermoelectric Oxides at Macro- and Nano-scales

NASA Astrophysics Data System (ADS)

Ma, Feiyue

Thermoelectric materials can directly convert a temperature difference into electrical voltage and vice versa. Due to this unique property, thermoelectric materials are widely used in industry and scientific laboratories for temperature sensing and thermal management applications. Waste heat harvesting, another potential application of thermoelectric materials, has long been limited by the low conversion efficiency of the materials. Potential high temperature applications, such as power plant waste heat harvesting and combustion engine exhaust heat recovery, make thermoelectric oxides a very promising class of thermoelectric materials. In this thesis, the synthesis and characterization of thermoelectric oxide materials are explored. In the first part of this thesis, the measurement methodologies and instrumentation processes employed to investigate different thermoelectric properties, such as the Seebeck coefficient and carrier concentration at the bulk scale and the thermal conductivity at the nanoscale, are detailed. Existing scientific and engineering challenges associated with these measurements are also reviewed. To overcome such problems, original parts and methodologies have been designed. Three fully functional systems were ultimately developed for the characterization of macroscale thermoelectric properties as well as localized thermal conductivity. In the second part of the thesis, the synthesis of NaxCo 2O4, a thermoelectric oxide material, is discussed. Modification of both composition and structure were carried out so as to optimize the thermoelectric performance of NaxCo2O4. Nanostructuring methods, such as ball milling, electrospinning, auto-combustion synthesis, and core-shell structure fabrication, have been developed to refine the grain size of NaxCo2O4 in order to reduce its thermal conductivity. However, the structure of the nanostructured materials is very unstable at high temperature and limited improvement on thermoelectric performance is

Green synthesis of nanocrystalline α-Al2O3 powders by both wet-chemical and mechanochemical methods

NASA Astrophysics Data System (ADS)

Gao, Huiying; Li, Zhiyong; Zhao, Peng

2018-03-01

Nanosized α-Al2O3 powders were prepared with AlCl3ṡ6H2O and NH4HCO3 as raw materials by both wet-chemical and mechanochemical methods, through the synthesis of the ammonium aluminum carbonate hydroxide (AACH) precursor followed by calcination. The environmentally benign starch was used as an effective dispersant during the preparation of nanocrystalline α-Al2O3 powders. X-ray diffraction (XRD), thermogravimetric differential thermal analysis (TG-DTA), transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were employed to characterize the precursor AACH and products. The results show that nanosized spherical α-Al2O3 powders without hard agglomeration and with particle size in the range of 20-40 nm can be obtained by the two methods. Comparing the two “green” processes, the mechanochemical method has better prospects for commercial production.

Obtaining and characterization of La0.8Sr0.2CrO3 perovskite by the combustion method

NASA Astrophysics Data System (ADS)

Morales Rivera, A. M.; Gómez Cuaspud, J. A.; López, E. Vera

2017-01-01

This research is focused on the synthesis and characterization of a perovskite oxide based on La0.8Sr0.2CrO3 system by the combustion method. The material was obtained in order to contribute to analyse the effect of synthesis route in the obtaining of advanced anodic materials for solid oxide fuel cells (SOFC). The obtaining of solid was achieved starting from corresponding nitrate dissolutions, which were polymerized by temperature effect in presence of citric acid. The solid precursor as a foam citrate was characterized by infrared (FTIR) and ultraviolet (UV) spectroscopy, confirming the effectiveness in synthesis process. The solid was calcined in oxygen atmosphere at 800°C and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive of X-ray spectroscopy (EDX) and solid state impedance spectroscopy (IS). Results confirm the obtaining of an orthorhombic solid with space group Pnma (62) and cell parameters a=5.4590Å, b=7.7310Å and c=5.5050Å. At morphological level the solid showed a heterogeneous distribution with an optimal correspondence with proposed and obtained stoichiometry. The electrical characterization, confirm a semiconductor behaviour with a value of 2.14eV Band-gap according with previous works.

Ultrasound with low intensity assisted the synthesis of nanocrystalline TiO2 without calcination.

PubMed

Ghows, Narjes; Entezari, Mohamad H

2010-06-01

A novel method has been developed for the preparation of nano-sized TiO(2) with anatase phase. Nanoparticles with diameter about 6 nm were prepared at a relatively low temperature (75 degrees C) and short time. The synthesis was carried out by the hydrolysis of titanium tetra-isopropoxide (TTIP) in the presence of water, ethanol, and dispersant under ultrasonic irradiation (500 kHz) at low intensity. The results show that variables such as water/ethanol ratio, irradiation time, and temperature have a great influence on the particle size and crystalline phases of TiO(2) nanoparticles. Characterization of the product was carried out by different techniques such as powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HRTEM) and UV-vis spectroscopy. (c) 2010 Elsevier B.V. All rights reserved.

Lipoic acid functionalized SiO2@Ag nanoparticles. Synthesis, characterization and evaluation of biological activity.

PubMed

Tudose, Madalina; Culita, Daniela Cristina; Musuc, Adina Magdalena; Somacescu, Simona; Ghica, Cornel; Chifiriuc, Mariana Carmen; Bleotu, Coralia

2017-10-01

A novel nanocomposite was obtained through the covalent immobilization of lipoic acid on the surface of silver nanoparticles-decorated silica nanoparticles (SiO 2 @Ag). The hybrid organic - inorganic material obtained was characterized by Fourier transform infrared spectroscopy, thermal analysis, scanning and transmision electron microscopy, X-ray photoelectron spectroscopy and UV-Visible spectroscopy. Its antioxidant, cytotoxic, antimicrobial activity and influence on mammalian cells cycle were evaluated. The results of this study have shown that the functionalization of SiO 2 @Ag with lipoic acid resulted in a composite with increased specificity of interaction with different mammalian cell lines and antioxidant activity, but with decreased cytotoxicity and antimicrobial properties. Therefore, the SiO 2 @Ag functionalized with lipoic acid could be successfully used in certain concentrations to modulate the cell cycle, in order to obtain the desired anti-proliferative or stimulatory therapeutic effect. Copyright © 2017 Elsevier B.V. All rights reserved.

Theoretical study of methanol synthesis from CO2 and CO hydrogenation on the surface of ZrO2 supported In2O3 catalyst

NASA Astrophysics Data System (ADS)

Dou, Maobin; Zhang, Minhua; Chen, Yifei; Yu, Yingzhe

2018-06-01

The interactions between ZrO2 support and In2O3 catalyst play pivotal role in the catalytic conversion of CO2 to methanol. Herein, a density functional theory study has been conducted to research the mechanism of methanol synthesis from CO2 and CO hydrogenation on the defective ZrO2 supported In2O3(110) surface (D surface). The calculations reveal that methanol is produced mainly via the HCOO reaction pathway from CO2 hydrogenation on D surface, and the hydrogenation of HCOO to form H2COO species with an activation barrier of 1.21 eV plays the rate determining step for the HCOO reaction pathway. The direct dissociation of CO2 to CO on D surface is kinetically and energetically prohibited. Methanol synthesis from CO hydrogenation on D surface is much facile comparing with the elementary steps involved in CO2 hydrogenation. The rate determining step of CO hydrogenation to methanol is the formation of H3CO species on the vacancy site with a barrier of 0.51 eV. ZrO2 support has significant effect on the suppressing of the dissociation of CO2 and stabilization of H2COO species on the surface of In2O3 catalyst.

High temperature hydrothermal synthesis of rare-earth titanates: synthesis and structure of RE5Ti4O15(OH) (RE = La, Er), Sm3TiO5(OH)3, RE5Ti2O11(OH) (RE = Tm-Lu) and Ce2Ti4O11.

PubMed

Fulle, Kyle; Sanjeewa, Liurukara D; McMillen, Colin D; Kolis, Joseph W

2018-05-15

Reactions of rare-earth oxides with TiO2 were performed in high temperature (650-700 °C) hydrothermal fluids. Two different mineralizer fluids were examined, 20 M KOH and 30 M CsF, and their respective products analyzed. When concentrated KOH fluids were used, single crystals of a variety of new OH- containing species were isolated and structurally characterized: RE5Ti4O15(OH) (RE = La, Er) I, Sm3TiO5(OH)3II and RE5Ti2O11(OH) (RE = Tm-Lu) III. La5Ti4O15(OH) I crystallizes in the orthorhombic space group Pnnm with unit cell dimensions of a = 30.5152(12) Å, b = 5.5832(2) Å, c = 7.7590(3) Å and V = 1321.92(9) Å3, Z = 4. Sm3TiO5(OH)3II crystallizes in the monoclinic space group P21/m with unit cell parameters of a = 5.6066(2) Å, b = 10.4622(4) Å, c = 6.1258(2) Å and β = 104.7390(10)°, V = 347.50(2) Å3, Z = 2. Lu5Ti2O11(OH) III crystallizes in the monoclinic space group C2/m with unit cell dimensions of a = 12.1252(9) Å, b = 5.8243(4) Å, c = 7.0407(5) Å, β = 106.939(3)° and V = 475.65(6) Å3, Z = 2. When concentrated fluoride solutions are used, mostly RE2Ti2O7 type compounds were isolated in either cubic or monoclinic phases. In the case of cerium, Ce2Ti4O11IV was isolated that crystallizes in the monoclinic space group C2/c with unit cell parameters of a = 13.6875(7) Å, b = 5.0955(3) Å, c = 12.8592(7) Å, β = 108.964(2)° and V = 848.18(8) Å3, Z = 4. The synthesis, structural characterization, and supporting characterization are reported for all compounds. The work highlights the complementary nature of hydroxide and fluoride fluids in studying the reactivity of refractory oxides.

The Effects of Leaching Process to the TiO2 Synthesis from Bangka Ilmenite

NASA Astrophysics Data System (ADS)

Wahyuningsih, S.; Ramelan, A. H.; Pramono, E.; Argawan, P.; Djatisulistya, A.; Firdiyono, F.; Sulistiyono, E.; Sari, P. P.

2018-03-01

Ilmenite mineral is a naturally occurring iron titanate (FeTiO3) and is abundant in nature. The separation of components into TiO2 and Fe2O3 must be expand. The purpose of this research is to synthesis TiO2 nanoparticles from the filtrate of Bangka ilmenite leaching process. Leaching of ilmenite was done with H2SO4 and HCl at various concentrations. The formation of TiO2 crystal determined by hydrolysis conditions and condensation reaction. TiO2 synthesized from the filtrate of sulfuric acid leaching that produced from TiO2 anatase phase when hydrolyzed in an aquaregia solvent and low concentrations of HCl (0.1M). Hydrolysis conditions at higher concentrations of HCl (1M) was produced TiO2 anatase-rutile phase. The synthesis of TiO2 from the filtrate of hydrochloric acid leaching was produced anatase phase. While the condition under the alcoholic solvent (2-propanol: H2O (v/v) = 9: 1) anatase phase crystallites grow in the temperature range up to 550 °C, above this temperature, TiO2 transform into rutile phase.

Synthesis of methyl 2-O- and 3-O-alpha-D-talopyranosyl-alpha-D-mannopyranoside.

PubMed

Rana, S S; Matta, K L

1986-09-01

Methyl 3,4,6-tri-O-benzyl-2-O-[6-O-(tert-butyldiphenylsilyl)-alpha-D- mannopyranosyl]-alpha-D-mannopyranoside (2) was synthesized by treatment of methyl 3,4,6-tri-O-benzyl-2-O-alpha-D-mannopyranosyl-alpha-D-mannopyranoside with tert-butylchlorodiphenylsilane in the presence of imidazole. Isopropylidenation, followed by oxidation with pyridinium chlorochromate, and stereoselective reduction with sodium borohydride, converted 2 into methyl 3,4,6-tri-O-benzyl-2-O-[6-O-(tert-butyldiphenylsilyl)-2,3-O-isopro pylidene- alpha-D-talopyranosyl]-alpha-D-mannopyranoside (5). Treatment of 5 with a molar solution of tetrabutylammonium fluoride in dry oxolane produced a diol which, on O-de-isopropylidenation followed by catalytic hydrogenolysis, afforded the disaccharide glycoside methyl 2-O-alpha-D-talopyranosyl-alpha-D-mannopyranoside. Synthesis of methyl 3-O-alpha-D-talopyranosyl-alpha-D-mannopyranoside was accomplished by a similar reaction-sequence. The structures of the final disaccharides, and of various other intermediates, were established by 1H- and 13C-n.m.r. spectroscopy.

Synthesis and Characterization of Polyether Adducts of Barium and Strontium Carboxylates and Their Use in the Formation of MTiO(3) Films.

PubMed

Wojtczak, William A.; Atanassova, Paolina; Hampden-Smith, Mark J.; Duesler, Eileen

1996-11-20

The synthesis, characterization, and reactivity of new polyether adducts of strontium and barium carboxylates of general composition M(O(2)CCF(3))(n)()(L) (M = Ba, L = 15-crown-5, (1); M = Ba (2), Sr (3), respectively, with L = tetraglyme are reported. The compounds were synthesized by reaction of BaCO(3) or MH(2) (M = Sr or Ba) with organic acids in the presence of the polyether ligands. These compounds have been characterized by IR and (13)C and (1)H NMR spectroscopies, elemental analyses, and thermogravimetric analysis. The species Ba(2)(O(2)CCF(3))(4)(15-crown-5)(2) (1) and [Ba(2)(O(2)CCF(3))(4)(tetraglyme)](infinity) (2), were also characterized by single-crystal X-ray diffraction. Ba(2)(O(2)CCF(3))(4)(15-crown-5)(2) (1) crystallizes in the orthorhombic space group Cccm with cell dimensions of a = 13.949(1) Å, b = 19.376(2) Å, c = 16.029(1) Å, and Z = 8. [Ba(2)(O(2)CCF(3))(4)(tetraglyme)](infinity) (2) crystallizes in the monoclinic space group C2/c with cell dimensions of a = 12.8673(12) Å, b = 16.6981(13) Å, c = 15.1191(12) Å, beta = 99.049(8) degrees, and Z = 4. Compounds 1-3 thermally decompose at high temperatures in the solid state to give MF(2). However, solutions of compounds 1-3 dissolved in ethanol with Ti(O-i-Pr)(4) give crystalline perovskite phase MTiO(3) films, or in the case of mixtures of 2 and 3, Ba(1)(-)(x)()Sr(x)()TiO(3) films below 600 degrees C when spin coated onto silicon substrates and thermally treated. The crystallinity, purity, and elemental composition of the films was determined by glancing angle X-ray diffraction and Auger electron spectroscopy.

Characterization of pulsed laser deposition grown V2O3 converted VO2

NASA Astrophysics Data System (ADS)

Majid, Suhail; Shukla, D. K.; Rahman, F.; Gautam, Kamini; Sathe, V. G.; Choudhary, R. J.; Phase, D. M.

2016-10-01

Controllable tuning of Metal-insulator transition in VxOy thin film has been a field of extensive research. However controlled synthesis of desired Vanadium oxide phase is a challenging task. We have successfully achieved VO2 phase on Silicon substrate after post deposition annealing treatment to the PLD grown as deposited V2O3 thin films. The annealed thin film was characterized by x-ray diffraction (XRD), resistivity, Raman spectroscopy, X-ray absorption spectroscopy (XAS) and X-ray photoelectron spectroscopy (XPS) measurements. XRD confirms the crystalline nature and growth of VO2 phase in thin film. The characteristic MIT was observed from resistivity measurements and transition temperature appeared at lower value around 336 K, compared to bulk VO2. The structural transition accompanied with MIT from lower temperature monoclinic phase to higher temperature Rutile phase became evident from temperature dependent Raman measurements. Chemical state of vanadium was examined using XAS and XPS measurements which confirm the presence of +4 oxidation state of vanadium in thin film.

Synthesis and characterization of Chitosan-CuO-MgO polymer nanocomposites

NASA Astrophysics Data System (ADS)

Praffulla, S. R.; Bubbly, S. G.

2018-05-01

In the present work, we have synthesized Chitosan-CuO-MgO nanocomposites by incorporating CuO and MgO nanoparticles in chitosan matrix. Copper oxide and magnesium oxide nanoparticles synthesized by precipitation method were characterized by X-ray diffraction and the diffraction patterns confirmed the monoclinic and cubic crystalline structures of CuO and MgO nanoparticles respectively. Chitosan-CuO-MgO composite films were prepared using solution- cast method with different concentrations of CuO and MgO nanoparticles (15 - 50 wt % with respect to chitosan) and characterized by XRD, FTIR and UV-Vis spectroscopy. The X-ray diffraction pattern shows that the crystallinity of the chitosan composite increases with increase in nanoparticle concentration. FTIR spectra confirm the chemical interaction between chitosan and metal oxide nanoparticles (CuO and MgO). UV absorbance of chitosan nanocomposites were up to 17% better than pure chitosan, thus confirming its UV shielding properties. The mechanical and electrical properties of the prepared composites are in progress.

Green approach for the synthesis and characterization of ZrSnO4 nanopowder

NASA Astrophysics Data System (ADS)

Athar, Taimur; Vishwakarma, Sandeep Kumar; Bardia, Avinash; Alabass, Razzaq; Alqarlosy, Ahmed; Khan, Aleem Ahmed

2016-06-01

Well-defined structural framework of ZrSnO4 nanopowder has been synthesized for the fabrications of cost-effective and sensitive devices which give final reproducible result with reliability under ideal conditions. The synthesis was carried out at moderate temperature and then finally dried in the laboratory oven and then followed with calcination at 1000 °C for 4 h to get phase selective product. It was observed that gelation time depends on the concentration of reactants and temperature. The characterization of ZrSnO4 was carried out with XRD, SEM, TEM, UV, thermal analysis, DLS and FT-IR techniques. With adjustment of reaction parameters, the systematic tuning of the particle size, shape and functional properties can be controlled. It was concluded that self-assembly is an integral part for the synthesis and opens a new exciting opportunity for better understanding the formation of nanostructure framework from micro- to nanoscale along with mechanistic via wet chemical approach. ZrSnO4 has vital role in identifying its potential cytotoxicity in the biological systems. The cytotoxicity effects of ZrSnO4 nanopowder in vitro were evaluated in three different human cell types (hepatocytes, mesenchymal stem cells and neuronal cells). Acute exposure of nanoparticles was found to have greater cytotoxic effect at higher concentration (30 µg/ml). However, partial detoxification was observed during nanoparticles exposure at day 6. The study concluded that an initial stress from nanoparticles incorporates sealing or detoxification of nanoparticles which may help to recover cell viability.

Facile synthesis of CuFe2O4-Fe2O3 composite for high-performance supercapacitor electrode applications

NASA Astrophysics Data System (ADS)

Khan, Rashid; Habib, Muhammad; Gondal, Mohammed A.; Khalil, Adnan; Rehman, Zia Ur; Muhammad, Zahir; Haleem, Yasir A.; Wang, Changda; Wu, Chuan Qiang; Song, Li

2017-10-01

We report the synthesis of CuFe2O4-Fe2O3 composite material for efficient and highly stable supercapacitor electrode by using eco-friendly low-temperature co-precipitation method. The CuFe2O4-Fe2O3 composite demonstrated the highest specific capacitance of 638.24 F g-1 and excellent stability up to 2000 charge/discharge cycles. The achieved capacitance value is 16 times higher than that of pure CuFe2O4. The results revealed the extraordinary performance of CuFe2O4-Fe2O3 composite as supercapacitor electrode with excellent retention in comparison to CuFe2O4. The enhanced electrochemical activity of CuFe2O4-Fe2O3 composite is attributed to the synergistic effect which is responsible for redox coupling between Cu2+ and Fe3+ that has never been achieved by single component before.

Structural and surface properties of CuO-ZnO-Cr{sub 2}O{sub 3} catalysts and their relationship with selectivity to higher alcohol synthesis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Campos-Martin, J.M.; Fierro, J.L.G.; Guerrero-Ruiz, A.

1995-10-01

A series of copper-zinc-chromium catalysts of different compositions and calcination temperatures has been prepared, characterized by several techniques (BET specific surface area, XRD, gravimetric TPR, TPD-CO, and XPS), and tested under high alcohol synthesis (HAS) conditions. CO hydrogenation was carried out at reaction temperatures of 523-598 K and 50 bar total pressure. The influence of catalyst composition, calcination temperature, and surface characteristics on the HAS selectivity was studied. The optimum HAS yields were found in the low Cr content region, but chromium was needed. Although chromium oxide does not seem to be involved in the catalytic site, its presence inmore » the catalyst composition is essential, owing to the larger specific surfaces and catalyst stability obtained at the highest reaction temperatures. For low Cr content composition, the temperature-programmed reduction (TPR) profiles were shifted to higher temperatures and simultaneously larger CO{sub 2} amounts were found in the temperature-programmed desorption profiles of adsorbed CO (TPD-CO). Photoelectron spectra (XPS) revealed that the oxidation state of copper is Cu{sup 2+} in the calcined catalysts and Cu{sup O} in the reduced ones; Cu{sup +} was only stabilized in a CuCr{sub 2}O{sub 4} spinel in the Cr-rich catalysts. These features derived from catalyst characterization are discussed in the framework of the catalytic behaviour for HAS synthesis. 53 refs., 7 figs., 4 tabs.« less

Synthesis and Characterization of Yttria-Stabilized Zirconia Nanoparticles Doped with Ytterbium and Gadolinium: ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3

NASA Astrophysics Data System (ADS)

Bahamirian, M.; Hadavi, S. M. M.; Rahimipour, M. R.; Farvizi, M.; Keyvani, A.

2018-03-01

Defect cluster thermal barrier coatings (TBCs) are attractive alternatives to Yttria-stabilized zirconia (YSZ) in advanced applications. In this study, YSZ nanoparticles doped with ytterbium and gadolinium (ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3 (ZGYbY)) were synthesized through a chemical co-precipitation and calcination method, and characterized by in situ high-temperature X-ray diffraction analysis in the temperature range of 25 °C to 1000 °C (HTK-XRD), thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, and field emission scanning electron microscopy (FE-SEM). Precise cell parameters of t-prime phase and the best zirconia phase for TBC applications were calculated by Cohen's and Rietveld refinement methods. Optimum crystallization temperature of the precursor powder was found to be 1000 °C. Furthermore, FE-SEM results for the calcined ZGYbY powders indicated orderly particles of uniform shape and size with a small tendency toward agglomeration. Average lattice thermal expansion coefficient in the temperature range of 25 °C to 1000 °C was determined to be 31.71 × 10-6 K-1.

Synthesis and Characterization of Yttria-Stabilized Zirconia Nanoparticles Doped with Ytterbium and Gadolinium: ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3

NASA Astrophysics Data System (ADS)

Bahamirian, M.; Hadavi, S. M. M.; Rahimipour, M. R.; Farvizi, M.; Keyvani, A.

2018-06-01

Defect cluster thermal barrier coatings (TBCs) are attractive alternatives to Yttria-stabilized zirconia (YSZ) in advanced applications. In this study, YSZ nanoparticles doped with ytterbium and gadolinium (ZrO2 9.5Y2O3 5.6Yb2O3 5.2Gd2O3 (ZGYbY)) were synthesized through a chemical co-precipitation and calcination method, and characterized by in situ high-temperature X-ray diffraction analysis in the temperature range of 25 °C to 1000 °C (HTK-XRD), thermogravimetric analysis, differential thermal analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, and field emission scanning electron microscopy (FE-SEM). Precise cell parameters of t-prime phase and the best zirconia phase for TBC applications were calculated by Cohen's and Rietveld refinement methods. Optimum crystallization temperature of the precursor powder was found to be 1000 °C. Furthermore, FE-SEM results for the calcined ZGYbY powders indicated orderly particles of uniform shape and size with a small tendency toward agglomeration. Average lattice thermal expansion coefficient in the temperature range of 25 °C to 1000 °C was determined to be 31.71 × 10-6 K-1.

Sol-Gel Synthesis, Electrochemical Characterization, and Stability Testing of Ti0.7W0.3O2 Nanoparticles for Catalyst Support Applications in Proton-Exchange Membrane Fuel Cells

DOE Office of Scientific and Technical Information (OSTI.GOV)

Subban, Chinmayee V.; Zhou, Qin; Hu, Anthony

2010-11-19

The materials currently used in proton-exchange membrane fuel cells (PEMFCs) require complex control of operating conditions to make them sufficiently durable to permit commercial deployment. One of the major materials challenges to allow simplification of fuel cell operating strategies is the discovery of catalyst supports that are much more stable to oxidative decomposition than currently used carbon blacks. Here we report the synthesis and characterization of Ti 0.7W 0.3O 2 nanoparticles (approximately 50 nm diameter), a promising doped metal oxide that is a candidate for such a durable catalyst support. The synthesized nanoparticles were platinized, characterized by electrochemical testing, andmore » evaluated for stability under PEMFC and other oxidizing acidic conditions. Ti 0.7W 0.3O 2 nanoparticles show no evidence of decomposition when heated in a Nafion solution for 3 weeks at 80 °C. In contrast, when heated in sulfuric, nitric, perchloric, or hydrochloric acid, the oxide reacts to form salts such as titanylsulfatehydrate from sulfuric acid. Electrochemical tests show that rates of hydrogen oxidation and oxygen reduction by platinum nanoparticles supported on Ti 0.7W 0.3O 2 are comparable to those of commercial Pt on carbon black.« less

H2O2_COD_EPA; MEC_acclimation

EPA Pesticide Factsheets

H2O2_COD_EPA: Measurements of hydrogen peroxide and COD concentrations for water samples from the MEC reactors.MEC_acclimation: raw data for current and voltage of the anode in the MEC reactor.This dataset is associated with the following publication:Sim, J., J. An, E. Elbeshbishy, R. Hodon, and H. Lee. Characterization and optimization of cathodic conditions for H2O2 synthesis in microbial electrochemical cells. Bioresource Technology. Elsevier Online, New York, NY, USA, 195: 31-36, (2015).

Double enzymatic cascade reactions within FeSe-Pt@SiO2 nanospheres: synthesis and application toward colorimetric biosensing of H2O2 and glucose.

PubMed

Qiao, Fengmin; Wang, Zhenzhen; Xu, Ke; Ai, Shiyun

2015-10-07

A facile process was developed for the synthesis of FeSe-Pt@SiO2 nanospheres based on the hydrothermal treatment of FeCl3·6H2O, selenium and NaBH4 in ethanolamine solvent, followed by reducing HPtCl4 with NaBH4 in the presence of FeSe particles to obtain FeSe coated with Pt NPs (FeSe-Pt), ending with a surfactant assembled sol-gel process to obtain FeSe-Pt@SiO2. The morphology and composition of FeSe-Pt@SiO2 were characterized by transmission electron microscopy, high resolution TEM, X-ray diffraction and Fourier transform infrared spectroscopy. Structural analyses revealed that FeSe-Pt@SiO2 nanospheres were of regular spherical shape with smooth surfaces due to the SiO2 shells, compared with FeSe particles with 150 nm lateral diameter. The prepared FeSe-Pt@SiO2 nanospheres possessed both intrinsic glucose oxidase (GOx-) and peroxidase-mimic activities, and we engineered an artificial enzymatic cascade system with high activity and stability based on this nanostructure. The good catalytic performance of the composites could be attributed to the synergy between the functions of FeSe particles and Pt NPs. Significantly, the FeSe-Pt@SiO2 nanospheres as robust nanoreactors can catalyze a self-organized cascade reaction, which includes oxidation of glucose by oxygen to yield gluconic acid and H2O2, and then oxidation of 3,3,5,5-tetramethylbenzidine (TMB) by H2O2 to produce a colour change. Colorimetric detection of H2O2 and glucose using the FeSe-Pt@SiO2 nanospheres was conducted with high detection sensitivities, 0.227 nM and 1.136 nM, respectively, demonstrating the feasibility of practical sensing applications. It is therefore believed that our findings in this study could open up the possibility of utilizing FeSe-Pt@SiO2 nanospheres as enzymatic mimics in diagnostic and biotechnology fields.

Synthesis and magnetic properties of single-crystalline Na2-xMn8O16 nanorods

PubMed Central

2011-01-01

The synthesis of single-crystalline hollandite-type manganese oxides Na2-xMn8O16 nanorods by a simple molten salt method is reported for the first time. The nanorods were characterized by powder X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and a superconducting quantum interference device magnetometer. The magnetic measurements indicated that the nanorods showed spin glass behavior and exchange bias effect at low temperatures. The low-temperature magnetic behaviors can be explained by the uncompensated spins on the surface of the nanorods. PMID:21711626

XPS and EELS characterization of Mn2SiO4, MnSiO3 and MnAl2O4

NASA Astrophysics Data System (ADS)

Grosvenor, A. P.; Bellhouse, E. M.; Korinek, A.; Bugnet, M.; McDermid, J. R.

2016-08-01

X-ray Photoelectron Spectroscopy (XPS) and Electron Energy Loss Spectroscopy (EELS) are strong candidate techniques for characterizing steel surfaces and substrate-coating interfaces when investigating the selective oxidation and reactive wetting of advanced high strength steels (AHSS) during the continuous galvanizing process. However, unambiguous identification of ternary oxides such as Mn2SiO4, MnSiO3, and MnAl2O4 by XPS or EELS, which can play a significant role in substrate reactive wetting, is difficult due to the lack of fully characterized standards in the literature. To resolve this issue, samples of Mn2SiO4, MnSiO3 and MnAl2O4 were synthesized and characterized by XPS and EELS. The unique features of the XPS and EELS spectra for the Mn2SiO4, MnSiO3 and MnAl2O4 standards were successfully derived, thereby allowing investigators to fully differentiate and identify these oxides at the surface and subsurface of Mn, Si and Al alloyed AHSS using these techniques.

Synthesis, Characterization, and Gas-Sensing Properties of Mesoporous Nanocrystalline Sn(x)Ti(1-x)O2.

PubMed

Zhong, Cheng; Lin, Zhidong; Guo, Fei; Wang, Xuehua

2015-06-01

A nanocomposite mesoporous material composed by SnO2 and TiO2 with the size of -5-9 nm were prepared via a facile wet-chemical approach combining with an annealing process. The microstructure of obtained Sn(x)Ti(1-x)O2 powders were characterized by X-ray diffraction, X-ray Photo-electronic Spectroscopy, scanning electron microscope, transmission electron microscope and nitrogen adsorption-desorption experiment. The gas sensing performances to several gases of the mesoporous material were studied. The sensors of Sn(x)Ti(1-x)O2 (ST10, with 9.1% Ti) exhibited very high responses to volatile organic compounds at 160 degrees C. The order of the responses to volatile gases based on ST10 was ethanol > formaldehyde > acetone > toluene > benzene > methane. Sensor based on ST10 displays a highest sensitivity to hydrogen at 200 degrees C. Sensor responses to H2 at 200 degrees C have been measured and analyzed in a wide concentration range from 5 to 2000 ppm. The solid solution Sn(x)Ti(1-x)O2 can be served as a potential gas-sensing material for a broad range of future sensor applications.

Synthesis, structure, and electronic structure calculation of a new centrosymmetric borate Pb{sub 2}O[BO{sub 2}(OH)] based on anion-centered OPb{sub 4} tetrahedra

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Feng; Wang, Li, E-mail: wangliresearch@163.com; Stoumpos, Constantinos C.

2016-08-15

The synthesis, structure, and characterization of a new centrosymmetric borate Pb{sub 2}O[BO{sub 2}(OH)] based on anion-centered OPb{sub 4} tetrahedra are reported. Pb{sub 2}O[BO{sub 2}(OH)] crystallizes in monoclinic space group C2/m with a=12.725(7) Å, b=5.698(3) Å, c=7.344(4) Å, β=116.277(6)°. The electronic band structure and density of states of Pb{sub 2}O[BO{sub 2}(OH)] have been calculated via the density functional theory (DFT). Electron density difference calculation indicates that lone-pair electrons of Pb{sup 2+} cation should be stereoactive. - Graphical abstract: An indirect gap compound of Pb{sub 2}O[BO{sub 2}(OH)] with 2D inorganic layers motif based on OPb{sub 4} tetrahedra has been synthesized and fullmore » characterized by crystallographic, IR, TG, UV–vis-NIR Diffuse Reflectance, and theoretical calculations. Display Omitted - Highlights: • A centrosymmetric borate Pb{sub 2}O[BO{sub 2}(OH)] was synthesized and characterized. • The crystalstructure, electronic band and density states was analyzed. • The lone-pair electrons of Pb{sup 2+} were proved to be stereoactive.« less

Laurus nobilis leaf extract mediated green synthesis of ZnO nanoparticles: Characterization and biomedical applications.

PubMed

Vijayakumar, Sekar; Vaseeharan, Baskaralingam; Malaikozhundan, Balasubramanian; Shobiya, Malaikkarasu

2016-12-01

The present study reports the green synthesis of zinc oxide nanoparticles using the aqueous leaf extract of Laurus nobilis (Ln-ZnO NPs) by co-precipitation method. The synthesized Ln-ZnO NPs were characterized by UV-Vis spectroscopy, FTIR, XRD, TEM, SEM and EDX. Ln-ZnO NPs were crystalline in nature, flower like and have hexagonal wurtzite structure with a mean particle size of 47.27nm. The antibacterial activity of Ln-ZnO NPs was greater against Gram positive (Staphylococcus aureus) bacteria than Gram negative (Pseudomonas aeruginosa) bacteria. The zone of inhibition against S. aureus was 11.4, 12.6 and 14.2mm at 25, 50 and 75μgmL -1 . The zone of inhibition against P. aeruginosa was 9.8, 10.2 and 11.3mm at 25, 50 and 75μgmL -1 . The light and confocal laser scanning microscopic images evidenced that Ln-ZnO NPs effectively inhibited the biofilm growth of S. aureus and P. aeruginosa at 75μgmL -1 . The cytotoxicity studies revealed that Ln-ZnO NPs showed no effect on normal murine RAW264.7 macrophage cells. On the other hand, Ln-ZnO NPs were effective in inhibiting the viability of human A549 lung cancer cells at higher concentrations of 80μgmL -1 . The morphological changes in the Ln-ZnO NPs treated A549 lung cancer cells were observed under phase contrast microscope. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

Synthesis and characterization of Cr doped CoFe2O4

NASA Astrophysics Data System (ADS)

Verma, Kavita; Patel, K. R.; Ram, Sahi; Barbar, S. K.

2016-05-01

Polycrystalline samples of pure and Cr-doped cobalt ferrite (CoFe2O4 and CoCrFeO4) were prepared by solid state reaction route method. X-ray diffraction pattern infers that both the samples are in single phase with Fd3m space group. Slight reduction in the lattice parameter of CoCrFeO4 has been observed as compared to CoFe2O4. The dielectric dispersion has been explained on the basis of Fe2+ ↔ Fe3+ hopping mechanism. The polarizations at lower frequencies are mainly attributed to electronic exchange between Fe2+ ↔ Fe3+ ions on the octahedral site in the ferrite lattice. In the present system a part from n-type charge carrier (Fe3+/Fe2+), the presence of (Co3+/Co2+) ions give rise to p-type charge carrier. Therefore in addition to n-type charge carrier, the local displacement of p-type charge carrier in direction of external electric field also contributes to net polarization. However, the dielectric constant and loss tangent of CoCrFeO4 are found to be lower than CoFe2O4 and is attributed to the availability of ferrous ion. CoCrFeO4 have less amount of ferrous ion available for polarization as compared to that of CoFe2O4. The impedance spectra reveal a grain interior contribution to the conduction process.

Shape-Controlled Synthesis of NiCo2 O4 Microstructures and Their Application in Supercapacitors.

PubMed

Xiang, Nannan; Ni, Yonghong; Ma, Xiang

2015-09-01

The shape-controlled synthesis of NiCo2 O4 microstructures through a facile hydrothermal method and subsequent calcinations was explored. By employing CoSO4 , NiSO4 , and urea as the starting reactants, flower-like NiCo2 O4 microstructures were obtained at 100 °C after 5 h without the assistance of any additive and subsequent calcination at 300 °C for 2 h; dumbbell-like NiCo2 O4 microstructures were prepared at 150 °C after 5 h in the presence of trisodium citrate and subsequent calcination at 300 °C for 2 h. The as-prepared NiCo2 O4 microstructures were characterized by X-ray powder diffraction, field-emission scanning electron microscopy, energy-dispersive X-ray spectroscopy, and (high-resolution) transmission electron microscopy. Both the flower-like and dumbbell-like NiCo2 O4 microstructures could be used as electrode materials for supercapacitors, and they exhibited excellent electrochemical performance, including high specific capacitance, good rate capability, and excellent long-term cycle stability. Simultaneously, the shape-dependent electrochemical properties of the product were investigated. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of synthesis method on structure, band gap and surface morphology of delafossite oxides, CuAlO2 and CuFeO2

NASA Astrophysics Data System (ADS)

Shah, Aadil Abass; Azam, Ameer

2018-04-01

In this research work we have reported the synthesis of two different delafossites, CuAlO2 and CuFeO2 by two different synthesis methods viz hydrothermal method and the combustion method. The effect of synthesis on structure, band gap and morphology of the synthesized delafossites was carried out using various techniques. The phase and structure of the synthesized delafossites were studied and confirmed using X-ray diffraction and the crystallite size was calculated. FTIR measurements showed the presence of different stretching modes and functional groups in the synthesized oxides. The surface morphology was studied using the scanning electron microscopy. The band gap of the synthesized delafossite oxides was found to be in the range of 2.8 and 3.3 eV.

Synthesis and characterization of oxyanion (phosphate, sulphate) doped Ba{sub 2}Sc{sub 2-y}Ga{sub y}O{sub 5}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, A.D.; Shin, J.F.; Slater, P.R., E-mail: p.r.slater@bham.ac.uk

2013-02-15

In this paper we examine the effect of partial substitution of Ga for Sc in the oxyanion (phosphate, sulphate) containing perovskites, Ba{sub 2}Sc{sub 2-x}P{sub x}O{sub 5+x} and Ba{sub 2}Sc{sub 2-x}S{sub x}O{sub 5+3x/2} with the samples analysed through a combination of X-ray diffraction, TGA, Raman spectroscopy and conductivity measurements. The results demonstrate that in both cases, Ga can be incorporated in place of Sc up to 40%. In order to accommodate the increasing Ga content, a reduction in the oxyanion content is required. Thus for the highest Ga content sample achieved, only 10% oxyanion incorporation was achieved giving endmember compositions ofmore » Ba{sub 2}ScGa{sub 0.8}P{sub 0.2}O{sub 5.2} and Ba{sub 2}ScGa{sub 0.8}S{sub 0.2}O{sub 5.3} for phosphate and sulphate doping respectively. While the Ga doping was shown to significantly improve the stability of the systems towards CO{sub 2} containing atmospheres, conductivity measurements showed a reduction in the conductivity with increasing Ga content. - Graphical abstract: Phosphate and sulphate doped Ba{sub 2}Sc{sub 2-x}Ga{sub x}O{sub 5} perovskites have been successfully prepared, with the highest conductivities observed for samples with the lowest Ga content. Highlights: Black-Right-Pointing-Pointer The successful synthesis of phosphate and sulphate doped Ba{sub 2}Sc{sub 2-x}Ga{sub x}O{sub 5} perovskites. Black-Right-Pointing-Pointer The demonstration of significant oxide ion and proton conduction in these perovskites. Black-Right-Pointing-Pointer The demonstration of improved CO{sub 2} stability with increasing Ga content.« less

Preparation and characterization of TiO2 coated Fe nanofibers for electromagnetic wave absorber.

PubMed

Jang, Dae-Hwan; Song, Hanbok; Lee, Young-In; Lee, Kun-Jae; Kim, Ki Hyeon; Oh, Sung-Tag; Lee, Sang-Kwan; Choa, Yong-Ho

2011-01-01

Recently, electromagnetic interference (EMI) and electromagnetic compatibility (EMC) have become serious problems due to the growth of electronic device and next generation telecommunication. It is necessary to develop new electromagnetic wave absorbing material to overcome the limitation of electromagnetic wave shielding materials. The EMI attenuation is normally related to magnetic loss and dielectric loss. Therefore, magnetic material coating dielectric materials are required in this reason. In this study, TiO2 coated Fe nanofibers were prepared to improve their properties for electromagnetic wave absorption. Poly(vinylpyrrolidone) (PVP) and Iron (III) nitrate nonahydrate (Fe(NO3)3 x 9H2O) were used as starting materials for the synthesis of Fe oxide nanofibers. Fe oxide nanofibers were prepared by electrospinning in an electric field and heat treatment. TiO2 layer was coated on the surface of Fe oxide nanofibers using sol-gel process. After the reduction of TiO2 coated Fe oxide nanofibers, Fe nanofibers with a TiO2 coating layer of about 10 nm were successfully obtained. The morphology and structure of fibers were characterized by SEM, TEM, and XRD. In addition, the absorption properties of TiO2 coated Fe nanofibers were measured by network analyzer.

Template free synthesis of ZnO/Ag2O nanocomposites as a highly efficient visible active photocatalyst for detoxification of methyl orange.

PubMed

Kadam, Abhijit; Dhabbe, Rohant; Gophane, Anna; Sathe, Tukaram; Garadkar, Kalyanrao

2016-01-01

A simple and effective route for the synthesis of ZnO/Ag2O nanocomposites with different weight ratios (4:1 to 4:4) have been successfully obtained by combination of thermal decomposition and precipitation technique. The structure, composition, morphology and optical properties of the as-prepared ZnO/Ag2O composites were characterized by XRD, FT-IR, EDS, SEM, TEM, UV-Vis DRS and PL, respectively. The photocatalytic performance of the photocatalysts was evaluated towards the degradation of a methyl orange (MO) under UV and visible light. More specifically, the results showed that the photocatalytic activity with highest rate constant of MO degradation over ZnO/Ag2O (4:2) nanocomposites is more than 22 and 4 times than those of pure ZnO and Ag2O under visible light irradiation, respectively. An improved photocatalytic activity was attributed to the formation of heterostructure between Ag2O and ZnO, the strong visible light absorption and more separation efficiency of photoinduced electron-hole pairs. Moreover, the ZnO/Ag2O (4:2) nanocomposite showed excellent stability towards the photodegradation of MO under visible light. Finally, a possible mechanism for enhanced charge separation and photodegrdation is proposed. Genotoxicity of MO before and after photodegradation was also evaluated by simple comet assay technique. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis and characterization of polymeric V2O5/AlO(OH) with nanopores on alumina support.

PubMed

Ahmad, A L; Abd Shukor, S R; Leo, C P

2006-12-01

Polymeric vanadium pentoxide gel was formed via the reaction of V2O5 powder with hydrogen peroxide. The polymeric vanadium pentoxide gel was then dispersed in alumina gel. Different vanadium loading composites were coated on alumina support and calcined at 500 degrees C for 1 hr. These composite layers were characterized using TGA, FT-IR, XRD, SEM, and Autosorb. It was found that the lamellar structure of polymerized vanadium pentoxide was retained in the inorganic matrix. Crystalline alumina in gamma phase was formed after calcinations. However, the vanadium-alumina mixed oxides are lack of the well defined PXRD peaks for polycrystalline V2O5. This is possibly because the vanadia species are highly dispersed in the alumina matrix or the vanadia species are dispersed as crystalline which is smaller than 4 nm. In addition, the imbedded polymeric vanadium oxide improved the specific area and average pore diameter of the composite layer.

Synthesis and characterization of ultra-fine Y2O3:Eu3+ nanophosphors for luminescent security ink applications.

PubMed

Gupta, Bipin Kumar; Haranath, D; Saini, Shikha; Singh, V N; Shanker, V

2010-02-05

We report a simple method for the synthesis of ultra-fine Eu(3+)-doped yttria (Y(2)O(3)) nanophosphors with an average diameter of approximately 5 nm for development of a transparent colloid that could be used as a luminescent security ink. This has been achieved by suitably substituting Eu(3+) ions at the favorable C(2) symmetry sites of Y(3+) ions and quantum mechanically confining the growth of the nanophosphor using a novel acid-catalyzed sol-gel technique. This is one of the few reports that depict the development of a transparent aqueous-stable Y(2)O(3):Eu(3+) colloidal solution for strategic applications related to security codes. High resolution transmission electron microscopy images showed excellent lattice fringes that in turn support the presence of better crystal quality and enhanced photoluminescence (PL) emission from the Y(1.9)O(3)Eu(0.1)(3+) nanophosphor system. Time resolved emission spectroscopy measurement indicated a PL decay time in the range of a few milliseconds, suitable for making luminescent security ink and other advanced applications in optoelectronic devices and bio-labeling.

Effect of synthesis conditions on the nanopowder properties of Ce{sub 0.9}Zr{sub 0.1}O{sub 2}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zimicz, M.G.; Fabregas, I.O.; Lamas, D.G.

Graphical abstract: . The synthesis of nanocrystalline Ce{sub 0.9}Zr{sub 0.1}O{sub 2} powders via the gel-combustion method, using different fuels, and following either stoichiometric or non-stoichiometric pH-controlled routes is investigated. Research highlights: {yields} All samples exhibited the fluorite-type crystal structure, nanometric average crystallite size and negligible carbon content. {yields} Synthesis conditions strongly affect the average crystallite size, the degree of agglomeration, the specific surface area and the pore volume. {yields} Our results indicate that, by controlling the synthesis conditions it is possible to obtain solids with custom-made morphological properties. -- Abstract: In this work, the synthesis of nanocrystalline Ce{sub 0.9}Zr{sub 0.1}O{submore » 2} powders via the gel-combustion method, using different fuels, and following either stoichiometric or non-stoichiometric pH-controlled routes is investigated. The objective is to evaluate the effect of synthesis conditions on the textural and morphological properties, and the crystal structure of the synthesized materials. The solids were characterized by nitrogen physisorption, Scanning Electron Microscopy (SEM), X-ray powder diffraction (XPD), and Carbon-Hydrogen-Nitrogen Elemental Analysis (CHN). All the powders exhibited nanometric crystallite size, fluorite-type structure and negligible carbon content. Synthesis conditions strongly affect the average crystallite size, the degree of agglomeration, the specific surface area and the pore volume. Our results indicate that, by controlling the synthesis conditions it is possible to obtain solids with custom-made morphological properties.« less

Novel porous Al2O3-SiO2-TiO2 bone grafting materials: formation and characterization.

PubMed

Naga, Salma M; El-Kady, Abeer M; El-Maghraby, Hesham F; Awaad, Mohamed; Detsch, Rainer; Boccaccini, Aldo R

2014-02-01

The present article deals with the development of 3D porous scaffolds for bone grafting. They were prepared based on rapid fluid infiltration of Al2O3-SiO2 sol into a polyethylene non-woven fabric template structure. Titanium dioxide in concentration equal to 5 wt% was added to the Al2O3-SiO2 mixture to produce Al2O3-SiO2-TiO2 composite scaffolds. The prepared scaffolds are characterized by means of X-ray diffraction, scanning electron microscopy and three-point bending test techniques. The bioactivity of the produced bodies is discussed, including the in vitro and in vivo assessments. The produced scaffolds exhibit mean total porosity of 66.0% and three-point bending strength of 7.1 MPa. In vitro studies showed that MG-63 osteoblast-like cells attach and spread on the scaffolds surfaces. Furthermore, cells grew through the scaffolds and start to produce extra-cellular matrix. Additionally, in vivo studies revealed the ability of the porous scaffolds to regenerate bone tissue in femur defects of albino rats 5 months post surgery. Histological analysis showed that the defect is almost entirely filled with new bone. The formed bone is characterized as a mature bone. The produced bone grafts are intended to be used as bone substitute or bone filler as their degradation products caused no inflammatory effects.

Synthesis and Characterization of Molybdenum Based Colloidal Particles.

PubMed

Moreno; Vidoni; Ovalles; Chaudret; Urbina; Krentzein

1998-11-15

The synthesis and characterization of molybdenum colloidal particles were evaluated using thermal and sonochemical methods and starting from different metal precursors, Mo(CO)6 and (NH4)2MoS4. The products were characterized by elemental analysis, spectroscopic (UV, FTIR), and surface analysis (XPS) techniques, as well as by transmission electron microscopy (TEM) for determining the particle sizes. Using Mo(CO)6 as metal source, particle sizes with an average diameter of 1.5 nm can be obtained using tert-amyl alcohol as solvent and tetrahydrothiophene as sulfurating ligand. The characterization of these particles showed that they are composed of molybdenum oxide MoO3. Using (NH4)2MoS4 as metal precursor, particles with average diameters of 4.7 and 2.5 nm were synthesized using thermal and sonochemical methods, respectively. The characterization of these particles showed them to be composed of molybdenum sulfide, MoS2. The sonochemical method proved to be the fastest and most convenient synthetic pathway of obtaining small colloidal particles at low temperatures and with control of the average size. Copyright 1998 Academic Press.

Plasma Spray Synthesis Of Nanostructured V2O5 Films For Electrical Energy Storage

DOE Office of Scientific and Technical Information (OSTI.GOV)

Nanda, Jagjit

We demonstrate for the first time, the synthesis of nanostructured vanadium pentoxide (V2O5) films and coatings using plasma spray technique. V2O5 has been used in several applications such as catalysts, super-capacitors and also as an electrode material in lithium ion batteries. In the present studies, V2O5 films were synthesized using liquid precursors (vanadium oxychloride and ammonium metavanadate) and powder suspension. In our approach, the precursors were atomized and injected radially into the plasma gun for deposition on the substrates. During the flight towards the substrate, the high temperature of the plasma plume pyrolyzes the precursor particles resulting into the desiredmore » film coatings. These coatings were then characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Differential Scanning Calorimetry (DSC). Among the precursors, vanadium oxychloride gave the best results in terms of nanocrystalline and monophasic films. Spraying of commercial powder suspension yielded multi-phasic mixture in the films. Our approach enables deposition of large area coatings of high quality nanocrystalline films of V2O5 with controllable particle morphology. This has been optimized by means of control over precursor composition and plasma spray conditions. Initial electrochemical studies of V2O5 film electrodes show potential for energy storage studies.« less

Synthesis and characterization of beta-Ga2O3 nanorod array clumps by chemical vapor deposition.

PubMed

Shi, Feng; Wei, Xiaofeng

2012-11-01

beta-Ga2O3 nanorod array clumps were successfully synthesized on Si (111) substrates by chemical vapor deposition. The composition, microstructure, morphology, and light-emitting property of these clumps were characterized by X-ray diffraction, Fourier transform infrared spectrophotometry, X-ray photoelectron spectroscopy, scanning electron microscopy, high-resolution transmission electron microscopy, Raman spectroscopy, and photoluminescence. The results demonstrate that the sample synthesized at 1050 degrees C for 15 min was composed of monoclinic beta-Ga2O3 nanorod array clumps, where each single nanorod was about 300 nm in diameter with some nano-droplets on its tip. These results reveal that the growth mechanism agrees with the vapor-liquid-solid (VLS) process. The photoluminescence spectrum shows that the Ga2O3 nanorods have a blue emission at 438 nm, which may be attributed to defects, such as oxygen vacancies and gallium-oxygen vacancy pairs. Defect-energy aggregation confinement growth theory was proposed to explain the growth mechanism of Ga2O3 nanorod array clumps collaborated with the VLS mechanism.