nm crystallite size: Topics by Science.gov

Sample records for nm crystallite size

Synthetic Control of Crystallite Size of Silver Vanadium Phosphorous Oxide (Ag 0.50VOPO 4·1.9H 2O): Impact on Electrochemistry

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

Huie, Matthew M.; Marschilok, Amy C.; Takeuchi, Esther S.

Here, this report describes a synthetic approach to control the crystallite size of silver vanadium phosphorous oxide, Ag 0.50VOPO 4·1.9H 2O, and the impact on electrochemistry in lithium based batteries. Ag 0.50VOPO 4·1.9H 2O was synthesized using a stirred hydrothermal method over a range of temperatures. X-ray diffraction (XRD) was used to confirm the crystalline phase and the crystallite size sizes of 11, 22, 38, 40, 49, and 120 nm. Particle shape was plate-like with edges <1 micron to >10 microns. Under galvanostatic reduction the samples with 22 nm crystallites and 880 nm particles produced the highest capacity, ~25% moremore » capacity than the 120 nm sample. Notably, the 11 nm sample resulted in reduced delivered capacity and higher resistance consistent with increased grain boundaries contributing to resistance. Under intermittent pulsing ohmic resistance decreased with increasing crystallite size from 11 nm to 120 nm implying that electrical conduction within a crystal is more facile than between crystallites and across grain boundaries. Finally, this systematic study of material dimension shows that crystallite size impacts deliverable capacity as well as cell resistance where both interparticle and intraparticle transport are important.« less
Synthetic Control of Crystallite Size of Silver Vanadium Phosphorous Oxide (Ag 0.50VOPO 4·1.9H 2O): Impact on Electrochemistry

DOE PAGES

Huie, Matthew M.; Marschilok, Amy C.; Takeuchi, Esther S.; ...

2017-04-12

Here, this report describes a synthetic approach to control the crystallite size of silver vanadium phosphorous oxide, Ag 0.50VOPO 4·1.9H 2O, and the impact on electrochemistry in lithium based batteries. Ag 0.50VOPO 4·1.9H 2O was synthesized using a stirred hydrothermal method over a range of temperatures. X-ray diffraction (XRD) was used to confirm the crystalline phase and the crystallite size sizes of 11, 22, 38, 40, 49, and 120 nm. Particle shape was plate-like with edges <1 micron to >10 microns. Under galvanostatic reduction the samples with 22 nm crystallites and 880 nm particles produced the highest capacity, ~25% moremore » capacity than the 120 nm sample. Notably, the 11 nm sample resulted in reduced delivered capacity and higher resistance consistent with increased grain boundaries contributing to resistance. Under intermittent pulsing ohmic resistance decreased with increasing crystallite size from 11 nm to 120 nm implying that electrical conduction within a crystal is more facile than between crystallites and across grain boundaries. Finally, this systematic study of material dimension shows that crystallite size impacts deliverable capacity as well as cell resistance where both interparticle and intraparticle transport are important.« less
Crystallite-size dependency of the pressure and temperature response in nanoparticles of magnesia

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

Rodenbough, Philip P.; Chan, Siu-Wai

We have carefully measured the hydrostatic compressibility and thermal expansion for a series of magnesia nanoparticles. We found a strong variance in these mechanical properties as crystallite size changed. For decreasing crystallite sizes, bulk modulus first increased, then reached a modest maximum of 165 GPa at an intermediate crystallite size of 14 nm, and then decreased thereafter to 77 GPa at 9 nm. Thermal expansion, meanwhile, decreased continuously to 70% of bulk value at 9 nm. These results are consistent to nano-ceria and together provide important insights into the thermal-mechanical structural properties of oxide nanoparticles.
Size dependent compressibility of nano-ceria: Minimum near 33 nm

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

Rodenbough, Philip P.; Chemistry Department, Columbia University, New York, New York 10027; Song, Junhua

2015-04-20

We report the crystallite-size-dependency of the compressibility of nanoceria under hydrostatic pressure for a wide variety of crystallite diameters and comment on the size-based trends indicating an extremum near 33 nm. Uniform nano-crystals of ceria were synthesized by basic precipitation from cerium (III) nitrate. Size-control was achieved by adjusting mixing time and, for larger particles, a subsequent annealing temperature. The nano-crystals were characterized by transmission electron microscopy and standard ambient x-ray diffraction (XRD). Compressibility, or its reciprocal, bulk modulus, was measured with high-pressure XRD at LBL-ALS, using helium, neon, or argon as the pressure-transmitting medium for all samples. As crystallite sizemore » decreased below 100 nm, the bulk modulus first increased, and then decreased, achieving a maximum near a crystallite diameter of 33 nm. We review earlier work and examine several possible explanations for the peaking of bulk modulus at an intermediate crystallite size.« less
Metrological characterization of X-ray diffraction methods at different acquisition geometries for determination of crystallite size in nano-scale materials

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

Uvarov, Vladimir, E-mail: vladimiru@savion.huji.ac.il; Popov, Inna

2013-11-15

Crystallite size values were determined by X-ray diffraction methods for 183 powder samples. The tested size range was from a few to about several hundred nanometers. Crystallite size was calculated with direct use of the Scherrer equation, the Williamson–Hall method and the Rietveld procedure via the application of a series of commercial and free software. The results were statistically treated to estimate the significance of the difference in size resulting from these methods. We also estimated effect of acquisition conditions (Bragg–Brentano, parallel-beam geometry, step size, counting time) and data processing on the calculated crystallite size values. On the basis ofmore » the obtained results it is possible to conclude that direct use of the Scherrer equation, Williamson–Hall method and the Rietveld refinement employed by a series of software (EVA, PCW and TOPAS respectively) yield very close results for crystallite sizes less than 60 nm for parallel beam geometry and less than 100 nm for Bragg–Brentano geometry. However, we found that despite the fact that the differences between the crystallite sizes, which were calculated by various methods, are small by absolute values, they are statistically significant in some cases. The values of crystallite size determined from XRD were compared with those obtained by imaging in a transmission (TEM) and scanning electron microscopes (SEM). It was found that there was a good correlation in size only for crystallites smaller than 50 – 60 nm. Highlights: • The crystallite sizes for 183 nanopowders were calculated using different XRD methods • Obtained results were subject to statistical treatment • Results obtained with Bragg-Brentano and parallel beam geometries were compared • Influence of conditions of XRD pattern acquisition on results was estimated • Calculated by XRD crystallite sizes were compared with same obtained by TEM and SEM.« less
Near-infrared emission from mesoporous crystalline germanium

NASA Astrophysics Data System (ADS)

Boucherif, Abderraouf; Korinek, Andreas; Aimez, Vincent; Arès, Richard

2014-10-01

Mesoporous crystalline germanium was fabricated by bipolar electrochemical etching of Ge wafer in HF-based electrolyte. It yields uniform mesoporous germanium layers composed of high density of crystallites with an average size 5-7 nm. Subsequent extended chemical etching allows tuning of crystallites size while preserving the same chemical composition. This highly controllable nanostructure exhibits photoluminescence emission above the bulk Ge bandgap, in the near-infrared range (1095-1360nm) with strong evidence of quantum confinement within the crystallites.
Effect of roll hot press temperature on crystallite size of PVDF film

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

Hartono, Ambran, E-mail: ambranhartono@yahoo.com; Sanjaya, Edi; Djamal, Mitra

2014-03-24

Fabrication PVDF films have been made using Hot Roll Press. Preparation of samples carried out for nine different temperatures. This condition is carried out to see the effect of Roll Hot Press temperature on the size of the crystallite of PVDF films. To obtain the diffraction pattern of sample characterization is performed using X-Ray Diffraction. Furthermore, from the diffraction pattern is obtained, the calculation to determine the crystallite size of the sample by using the Scherrer equation. From the experimental results and the calculation of crystallite sizes obtained for the samples with temperature 130 °C up to 170 °C respectivelymore » increased from 7.2 nm up to 20.54 nm. These results show that increasing temperatures will also increase the size of the crystallite of the sample. This happens because with the increasing temperature causes the higher the degree of crystallization of PVDF film sample is formed, so that the crystallite size also increases. This condition indicates that the specific volume or size of the crystals depends on the magnitude of the temperature as it has been studied by Nakagawa.« less
Synthesis of Copper Birnessite, Cu xMnO y·nH 2O with Crystallite Size Control: Impact of Crystallite Size on Electrochemistry

DOE PAGES

Li, Yue Ru; Marschilok, Amy C.; Takeuchi, Esther S.; ...

2015-11-24

This report describes the first detailed electrochemical examination of a series of copper birnessite samples under lithium-based battery conditions, allowing a structure/function analysis of the electrochemistry and related material properties. To obtain the series of copper birnessite samples, a novel synthetic approach for the preparation of copper birnessite, Cu xMnO y·nH 2O is reported. The copper content (x) in Cu xMnO y·nH 2O, 0.28 >= x >= 0.20, was inversely proportional to crystallite size, which ranged from 12 to 19 nm. The electrochemistry under lithium-based battery conditions showed that the higher copper content (x = 0.28) and small crystallite sizemore » (similar to 12 nm) sample delivered similar to 194 mAh/g, about 20% higher capacity than the low copper content (x = 0.22) and larger crystallite size (similar to 19 nm) material. In addition, Cu xMnO y·nH 2O displays quasi-reversible electrochemistry in magnesium based electrolytes, indicating that copper birnessite could be a candidate for future application in magnesium-ion batteries.« less
Correlations between Crystallite Size, Shape, Surface, and Infrared Spectra Using the Ti-C System

NASA Astrophysics Data System (ADS)

Kimura, Y.; Ikegami, A.; Kurumada, M.; Kamitsuji, K.; Kaito, C.

2004-06-01

TiC crystallites less than 10 nm in size showed an absorption feature at 14.3 μm. This 14.3 μm absorption was rarely seen in specimens ranging from bulk material to grains of 50 nm in size. The 14.3 μm feature was weakened as a result of the growth of TiC crystallites by heat treatment. When the carbide grains were covered with a carbon layer, the absorption peaks were considerably weakened, i.e., the absorption intensity depended on the grain surface state. A possible explanation is that the effects of size and shape on the spectra depend on the surface anisotropy.
The effect of confinement on the crystalline microstructure of polymer: fullerene bulk heterojunctions

DOE PAGES

Ashraf, A.; Dissanayake, D. M. N. M.; Eisaman, M. D.

2015-07-01

We investigate the effect of confinement on the coherence length and the crystalline microstructure of the polymer component of polymer: fullerene bulk heterojunction thin films using grazing incidence wide angle x-ray scattering. We find that the polymer crystallite size decreases and the alignment of the molecules along the surface normal increases, as the thin-film thickness is reduced from 920nm to < 20nm and approaches the thin-film confinement regime. Furthermore, we find that the polymer crystallite size near the surface (air interface) is lower than the crystallite size in the bulk or the bottom (substrate interface) of bulk heterojunction films thickermore » than the confinement regime. Variation in polymer crystallite size can cause changes in charge carrier mobility and recombination rates, which in turn affect the performance of bulk heterojunction thin film devices such as photovoltaics and photodetectors« less
Effect of calcination temperature on phase transformation and crystallite size of copper oxide (CuO) powders

NASA Astrophysics Data System (ADS)

Ratnawulan, Fauzi, Ahmad; AE, Sukma Hayati

2017-08-01

Copper oxide powder was prepared from Copper iron from South Solok, Indonesia. The samples was dried and calcined for an hour at temperatures of 145°C, 300°C,850°C, 1000°C. Phase transformation and crystallite size of the calcined powders have been investigated as a function of calcination temperature by room-temperature X-ray diffraction (XRD). It was seen that the tenorite, CuO was successfully obtained. With increasing calcining temperature, CuO transformed from malachite Cu2(CO3)(OH)2 to tenorite phase (CuO) and crystallite size of prepared samples increased from 36 nm to 76 nm.
Study of the resonant frequencies of silicon microcantilevers coated with vanadium dioxide films during the insulator-to-metal transition

NASA Astrophysics Data System (ADS)

Rúa, Armando; Fernández, Félix E.; Hines, Melissa A.; Sepúlveda, Nelson

2010-03-01

Vanadium dioxide (VO2) thin films were grown on silicon microcantilevers and companion test substrates by pulsed laser deposition followed by in situ annealing in an oxidizing atmosphere, with annealing times used to control crystallite sizes. Annealing times of 18 min produced VO2 films with average crystallite sizes of ˜10 nm or less, while those annealed for 35 min had crystallites of average size ˜90 nm, comparable to sample thickness. X-ray diffraction and x-ray photoelectron spectroscopy studies of the samples showed that films with crystallite sizes ˜40 nm or greater consisted of substoichiometric VO2 in its monoclinic phase, with preferential orientation with (011) planes parallel to the sample surface, while finer structured samples had a substantially similar composition, but showed no clear evidence of preferential orientation and were probably partially amorphous. Forced vibration experiments were performed with the cantilevers as they were thermally cycled through the VO2 insulator-to-metal transition (IMT). Very large reversible changes in the resonant frequencies of up to 5% (3.6 kHz) as well as hysteretic behavior were observed, which depend strongly on film crystallite size. The average value of Young's modulus for VO2 films with crystallite sizes of ˜90 nm was estimated from the mechanical resonance data at room temperature to be ˜120 GPa, but the large tensile stresses which develop between film and substrate through the IMT impede a similar determination for the VO2 tetragonal phase, since the commonly used relationships for cantilever frequencies derived from elasticity theory are not applicable for strongly curved composite beams. The results presented show that VO2 thin films can be useful in novel microscale and nanoscale electromechanical resonators in which effective stiffness can be tuned thermally or optically. This response can provide additional functionality to VO2—based devices which take advantage of other property changes through the IMT.
Crystallite Size-Lattice Strain Estimation and Optical Properties of Mn0.5Zn0.5Fe2O4 Nanoparticles

NASA Astrophysics Data System (ADS)

Indrayana, I. P. T.; Suharyadi, E.

2018-04-01

In the present work, we performed William-Hall plot using uniform deformation model (UDM) to estimate the crystallite size and lattice strain of Mn0.5Zn0.5Fe2O4 with various calcination temperature. The calculated crystallite sizes are 25.86 nm, 29.55 nm and 24.97 nm for nanoparticles which were calcined at a temperature of 600°C, 800°C and 1000°C, consecutively. The strain of nanoparticles has value in the order of 10-3. Controlling the calcination temperature will facilitate a change in crystallinity of nanoparticles and influence their crystallite size and strain of the crystal lattice. The optical band gap energy of samples nanoparticles is in a range of 1.09 eV – 3.30 eV. Increasing calcination temperature increased the direct and indirect band gap energy. The Urbach energy was found to increase with increased of gap energy. These results demonstrated that higher structural and optical properties of Mn0.5Zn0.5Fe2O4 can be obtained from a higher calcination temperature.
Cavitational synthesis of nanostructured inorganic materials for enhanced heterogeneous catalysis

NASA Astrophysics Data System (ADS)

Krausz, Ivo Michael

The synthesis of nanostructured inorganic materials by hydrodynamic cavitation processing was investigated. The goal of this work was to develop a general synthesis technique for nanostructured materials with a control over crystallite size in the 1--20 nm range. Materials with crystallite sizes in this range have shown enhanced catalytic activity compared to materials with larger crystallite sizes. Several supported and unsupported inorganic materials were studied to understand the effects of cavitation on crystallite size. Cavitation processing of calcium fluoride resulted in more spherical particles, attached to one another by melted necks. This work produced the first evidence of shock wave heating of nanostructured materials by hydrodynamic cavitation processing. Hydrodynamic cavitation synthesis of various catalytic support materials indicated that their phase composition and purity could be controlled by adjustment of the processing parameters. Zirconia/alumina supports synthesized using hydro-dynamic cavitation and calcined to 1368 K retained a high purity cubic zirconia phase, whereas classically prepared samples showed a phase transformation to monoclinic zirconia. Similarly, the synthesis of alumina resulted in materials with varying Bohmite and Bayerite contents as a function of the process parameters. High temperature calcination resulted in stable alumina supports with varying amounts of delta-, and theta-alumina. Synthesis studies of palladium and silver showed modest variations in crystallite size as a function of cavitation process parameters. Calcination resulted in larger grain materials, indicating a disappearance of intergrain boundaries. Based on these results, a new synthesis method was studied involving controlled agglomeration of small silver crystallites by hydrodynamic cavitation processing, followed by deposition on alumina. The optimal pH, concentration, and processing time for controlling the silver crystallite size in the cavitation equipment were determined using a statistical design of experiments approach. Three series of alumina supported silver catalysts were prepared, with silver weight loadings of 1%, 2%, and 5%. Variation of cavitation processing time between 1--64 min allowed the systematic control of silver crystallite size in the range of 3--19 nm. The preferred oxidation of CO in hydrogen (PROX) was chosen as a catalytic test reaction, because of its increasing importance for fuel cell applications. It was found that the catalytic activity was significantly increased for silver crystallite sizes below 5 nm. This work is the first experimental evidence of independent crystallite size control by hydrodynamic cavitation for alumina supported silver catalysts. The synthesis method involving controlled agglomeration and calcination is a general synthesis procedure that can be used to synthesize a wide range of novel catalysts and advanced materials.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Fitriana, Karina Nur, E-mail: nurfitriana.karina@gmail.com; Hafizah, Mas Ayu Elita, E-mail: kemasayu@yahoo.com; Manaf, Azwar, E-mail: azwar@ui.ac.id

Synthesis of single phased SrO.6Fe{sub 2-x}Mn{sub x/2}Ti{sub x/2}O{sub 3} (x = 0.0; 0.5; and 1.0) nanoparticles has been prepared through mechanical alloying, assisted with the ultrasonic destruction process. Monocrystalline particles were obtained when x = 0 treated with ultrasonic destruction at 55 μm of transducer amplitude. Average particle size and crystallite size were reduced significantly from 723 nm to ∼87 nm for x = 0. The particle size was not significantly reduced when x = 0.5 and x = 1 was changed. On the other hand, substitution of Ti elements on some of Fe elements expectedly had a major effectmore » on reducing particle size. This was proven by larger size on both particle and crystallite size at x = 1 rather than x = 0.5, with comparison respectively 2:1 (in nm). In addition, a higher transducer power was required for modifying Strontium Hexaferrite (SHF) with more Ti elements and a bigger size of pre-ultrasonic destructed sample. It is concluded that the amplitude of the transducer in ultrasonic destruction process and the element of ionic substitution affects both average particle size and crystallite size of SHF.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)

Apaydin, Ramazan Oguzhan; Ebin, Burcak; Gurmen, Sebahattin

Copper-Nickel (CuNi) nanostructured alloy particles were produced by Ultrasonic Spray Pyrolysis and Hydrogen Reduction Method (USP-HR) from high purity copper and nickel nitrate aqueous solutions. The effect of the precursor solution in the range of 0.1 and 0.5 mol/L on the morphology and crystallite size of CuNi nanoparticles were investigated under 2 h running time, 700 °C operating temperature and 0.5 L/min H{sub 2} flow rate. Particle size, morphology, composition and crystallite structure were characterized by Scanning Electron Microscopy (SEM), Energy Dispersive Spectroscopy (EDS) and X-Ray Diffraction (XRD). Particle characterization studies show that nanostructured alloy particles have cubic crystal structuremore » and they are in submicron size range with spherical morphology. The crystallite sizes of the particles calculated with Scherrer formula are 40 and 34 nm and average particles sizes observed from the SEM images are 300 and 510 nm for each experiment respectively.« less
Effect of the CTAB concentration on the upconversion emission of ZrO 2:Er 3+ nanocrystals

NASA Astrophysics Data System (ADS)

López-Luke, T.; De la Rosa, E.; Sólis, D.; Salas, P.; Angeles-Chavez, C.; Montoya, A.; Díaz-Torres, L. A.; Bribiesca, S.

2006-10-01

Upconversion emission of ZrO 2:Er 3+ (0.2 mol%) nanophosphor were studied as function of surfactant concentration after excitation at 968 nm. The strong green emission was produced by the transition 2H 11/2 + 4S 3/2 → 4I 15/2 and was explained in terms of cooperative energy transfer between neighboring ions. The upconverted signal was enhanced but the fluorescence decay time was reduced as either the surfactant concentration increases or the annealing time reduces. Experimental results show that surfactant concentration controls the particle size and morphology while annealing time control the phase composition and crystallite size. The highest intensity was obtained for a sample composed of a mixture of tetragonal (33 wt.%) and monoclinic (67 wt.%) phase with crystallite size of 31 and 59 nm, respectively. This result suggests that tetragonal crystalline structure and small crystallite size are more favorable for the upconversion emission.
Synthesis of strontium substituted barium titanate nanoparticles by mechanical alloying and high power ultrasonication destruction

NASA Astrophysics Data System (ADS)

Yustanti, Erlina; Hafizah, Mas Ayu Elita; Manaf, Azwar

2016-04-01

This paper reports the particle and crystallite size characterizations of mechanically alloyed Ba(1-x)SrxTiO3 (BST) with x = 0.3 and 0.7 prepared with the assistance of a high-power sonicator. Analytical grade BaCO3, TiO2 and SrCO3 precursors with a purity of greater than 99 wt.% were mixed and milled using a planetary ball mill to a powder weight ratio of 10:1. Powders obtained after 20 hours of milling time were then sintered at 1200°C for 4 hours to form crystalline powders.These powders were further treated ultrasonically under a fixed 6.7 gr/l particle concentration in demineralized water for 1, 3, 5, 7 hours and a fixed ultrasonic irradiation time of 1 hour to the dispersion of 6.7; 20; 33.3 gr/l concentrations. As to the results of crystallite size characterization, it is demonstrated that the mean crystallite size of BST with x = 0.3 and 0.7 undergo a slight change after the first 1 hour irradiation time and then remain almost unchanged. This was in contrary to the particle size in which the mean particle size of BST with x = 0.3 increased from 765 nm to 1405 nm after 7 hours irradiation time, while that of x = 0.7 increased from 505 nm to 1298 nm after 3 hours and then reduced back to the initial size after 7 hours ultra sonication time. The increase in particle size was due to large of cohesive forces among fine particles. It is also demonstrated that the concentration of particles in a dispersion with anionic surfactant do not effective to reduce the particle sizes ultrasonically. Nanoparticles with the mean size respectively 40 and 10 times larger than their respective crystallite size were successfully obtained respectively in x = 0.3 and x = 0.7.
Synthesis of strontium substituted barium titanate nanoparticles by mechanical alloying and high power ultrasonication destruction

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

Yustanti, Erlina, E-mail: erlina.yustanti@ui.ac.id; Department of Metallurgy, Faculty of Engineering University of Sultan AgengTirtayasa Jl. Jenderal Sudirman KM 03 Cilegon-Banten 65134; Hafizah, Mas Ayu Elita, E-mail: kemasayu@yahoo.com

2016-04-19

This paper reports the particle and crystallite size characterizations of mechanically alloyed Ba{sub (1-x)}Sr{sub x}TiO{sub 3} (BST) with x = 0.3 and 0.7 prepared with the assistance of a high-power sonicator. Analytical grade BaCO{sub 3}, TiO{sub 2} and SrCO{sub 3} precursors with a purity of greater than 99 wt.% were mixed and milled using a planetary ball mill to a powder weight ratio of 10:1. Powders obtained after 20 hours of milling time were then sintered at 1200°C for 4 hours to form crystalline powders.These powders were further treated ultrasonically under a fixed 6.7 gr/l particle concentration in demineralized watermore » for 1, 3, 5, 7 hours and a fixed ultrasonic irradiation time of 1 hour to the dispersion of 6.7; 20; 33.3 gr/l concentrations. As to the results of crystallite size characterization, it is demonstrated that the mean crystallite size of BST with x = 0.3 and 0.7 undergo a slight change after the first 1 hour irradiation time and then remain almost unchanged. This was in contrary to the particle size in which the mean particle size of BST with x = 0.3 increased from 765 nm to 1405 nm after 7 hours irradiation time, while that of x = 0.7 increased from 505 nm to 1298 nm after 3 hours and then reduced back to the initial size after 7 hours ultra sonication time. The increase in particle size was due to large of cohesive forces among fine particles. It is also demonstrated that the concentration of particles in a dispersion with anionic surfactant do not effective to reduce the particle sizes ultrasonically. Nanoparticles with the mean size respectively 40 and 10 times larger than their respective crystallite size were successfully obtained respectively in x = 0.3 and x = 0.7.« less
Hydrothermal synthesis and magnetic properties of Mn doped ZnS nanoparticles

NASA Astrophysics Data System (ADS)

Rashad, M. M.; Rayan, D. A.; El-Barawy, K.

2010-01-01

Nanocrystallite Mn doped Zn1-XS (X = 0 to 0.4) powders have been synthesized through a hydrothermal route. The effect of the hydrothermal temperature and Mn2+ ions substitution on the crystal structure, crystallite size, microstructure and magnetic properties were investigated using (XRD), (SEM) and (VSM). The results revealed that wurtzite zinc sulfide phase was formed using thiourea as a sulfur source at temperature 150- 200oC for 24 h. The crystallite size was (7.9-15.1 nm) was obtained at the same conditions. The doping of Mn2+ ions decreased the crystallite size of the formed ZnS wurtzite phase was in the range between 7.9 and 3.8 nm. SEM micrographs showed that the produced ZnS and Mn doped ZnS particles were appeared as spherical shape. The magnetic properties were improved by substitution of Mn2+ ions up to 0.2.

Efficient perovskite light-emitting diodes featuring nanometre-sized crystallites

NASA Astrophysics Data System (ADS)

Xiao, Zhengguo; Kerner, Ross A.; Zhao, Lianfeng; Tran, Nhu L.; Lee, Kyung Min; Koh, Tae-Wook; Scholes, Gregory D.; Rand, Barry P.

2017-01-01

Organic-inorganic hybrid perovskite materials are emerging as highly attractive semiconductors for use in optoelectronics. In addition to their use in photovoltaics, perovskites are promising for realizing light-emitting diodes (LEDs) due to their high colour purity, low non-radiative recombination rates and tunable bandgap. Here, we report highly efficient perovskite LEDs enabled through the formation of self-assembled, nanometre-sized crystallites. Large-group ammonium halides added to the perovskite precursor solution act as a surfactant that dramatically constrains the growth of 3D perovskite grains during film forming, producing crystallites with dimensions as small as 10 nm and film roughness of less than 1 nm. Coating these nanometre-sized perovskite grains with longer-chain organic cations yields highly efficient emitters, resulting in LEDs that operate with external quantum efficiencies of 10.4% for the methylammonium lead iodide system and 9.3% for the methylammonium lead bromide system, with significantly improved shelf and operational stability.
Synthesis of nanocrystalline Ni/Ce-YSZ powder via a polymerization route

NASA Astrophysics Data System (ADS)

Abolghasemi, Z.; Tamizifar, M.; Arzani, K.; Nemati, A.; Khanfekr, A.; Bolandi, M.

2013-08-01

Pechini process was used for preparation of three kinds of nanocrystalline powders of yttria-stabilized zirconia (YSZ): doped with 1.5 mol% nickel oxide, doped with 15 mol% ceria, and doped with 1.5 mol% nickel oxide plus 15 mol% ceria. Zirconium chloride, yttrium nitrate, cerium nitrate, nickel nitrate, citric acid and ethylene glycol were polymerized at 80 °C to produce a gel. XRD, SEM and TEM analyses were used to investigate the crystalline phases and microstructures of obtained compounds. The results of XRD revealed the formation of nanocrystalline powder at 900 °C. Morphology of the powder calcined at 900 °C, examined with a scanning electron microscope, showed that the presence of nickel and cerium inhibited the grain growth in the system. The average crystallite size of the material doped with nickel oxide (9.33 nm) was bigger than the one doped with cerium oxide (9.29 nm), while the YSZ doping with the two oxides simultaneously promoted the grain growth with crystallite size of 11.37 nm. Yttria-stabilized zirconia powder with a mean crystallite size of 9.997 nm was prepared successfully by this method.
Influence of crystallite size on the magnetic and heat generation properties of La0.77Sr0.23MnO3 nanoparticles for hyperthermia applications

NASA Astrophysics Data System (ADS)

Das, Harinarayan; Inukai, Akihiro; Debnath, Nipa; Kawaguchi, Takahiko; Sakamoto, Naonori; Hoque, Sheikh Manjura; Aono, Hiromichi; Shinozaki, Kazuo; Suzuki, Hisao; Wakiya, Naoki

2018-01-01

In this paper, we report a detailed study of magnetic properties and AC magnetic heat generation characteristics of La0.77Sr0.23MnO3 (LSMO) nanoparticles to investigate appropriate crystallite size with a view to the proper application of self-controlled magnetic hyperthermia treatments of cancer. A series of nanocrystalline LSMO manganite was synthesized through the chemical route called as "polymerized complex method" and then subsequently annealed at the different temperature from 600 to 1400 °C to obtain various crystallite size. Phase formation and crystal structure of the prepared powder were determined by the powder X-ray diffraction (XRD) using Rietveld analysis. The XRD patterns reveal that all powder samples are a single phase rhombohedral perovskite-like structure with R 3 bar c space group. The mean crystallite size of prepared particles varied from 19 to 243.8 nm with the increase of the annealing temperature starting from 600 to 1400 °C. The field emission scanning electron microscopy (FE-SEM) analysis shows the surface morphology with a strong agglomeration of fine nanoparticles. The Magnetic study reveals that these nanoparticles exhibit ferromagnetic nature with different value of magnetization, coercivity, Curie temperature which is strongly dependent on their crystallite size. The maximum saturation temperature (TS = 66 °C) under AC magnetic field (H = 1.77 kA/m, f = 370 kHz) was found for the crystallite size of 39.5 nm due to its pure single domain phase. Such LSMO nanoparticles, having the higher heating rate, can be used in magnetically induced hyperthermia cancer treatment.
Synthesis and characterization of nanocrystalline mesoporous zirconia using supercritical drying.

PubMed

Tyagi, Beena; Sidhpuria, Kalpesh; Shaik, Basha; Jasra, Raksh Vir

2006-06-01

Synthesis of nano-crystalline zirconia aerogel was done by sol-gel technique and supercritical drying using n-propanol solvent at and above supercritical temperature (235-280 degrees C) and pressure (48-52 bar) of n-propanol. Zirconia xerogel samples have also been prepared by conventional thermal drying method to compare with the super critically dried samples. Crystalline phase, crystallite size, surface area, pore volume, and pore size distribution were determined for all the samples in detail to understand the effect of gel drying methods on these properties. Supercritical drying of zirconia gel was observed to give thermally stable, nano-crystalline, tetragonal zirconia aerogels having high specific surface area and porosity with narrow and uniform pore size distribution as compared to thermally dried zirconia. With supercritical drying, zirconia samples show the formation of only mesopores whereas in thermally dried samples, substantial amount of micropores are observed along with mesopores. The samples prepared using supercritical drying yield nano-crystalline zirconia with smaller crystallite size (4-6 nm) as compared to higher crystallite size (13-20 nm) observed with thermally dried zirconia.
Influence of the crystallinity of a sputtered hydroxyapatite film on its osteocompatibility.

PubMed

Ozeki, K; Goto, T; Aoki, H; Masuzawa, T

2015-01-01

Hydroxyapatite (HA) was coated onto titanium substrates using radio frequency sputtering, and the sputtered films were crystallized using a hydrothermal treatment at 120°C and 170°C to evaluate the influence of the crystallinity of the HA film on its osteocompatibility. The crystallite size and surface morphology of the films were observed using X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The alkaline phosphatase (ALP) expression, osteocalin (OCN) expression and bone formation of osteoblast cells on the films were measured to evaluate the osteocompatibility of the film.The crystallite size increased as the hydrothermal temperature increased, and the crystallite sizes of the film treated at 120°C and 170°C were 82.2±12.3 nm and 124.7±13.3 nm, respectively. Globular particles were observed in the hydrothermally treated film using SEM. The size of the particles on the film increased as the hydrothermal temperature increased, and the width of the particles on the film treated at 120°C and 170°C were approximately 120-190 nm and 300-500 nm, respectively. In the osteoblast cell culture experiments, the ALP expression, OCN expression and bone formation area on the films treated at 120°C were higher than those treated for films treated at 170°C.
Effect of nanostructure on thermoelectric properties of La0.7Sr0.3MnO3 in 300–600 K temperature range

NASA Astrophysics Data System (ADS)

Singh, Saurabh; Srivastav, Simant Kumar; Patel, Ashutosh; Chatterjee, Ratnamala; Pandey, Sudhir K.

2018-05-01

In oxide materials, nanostructuring effect has been found a very promising approach for the enhancement of figure-of-merit, ZT. In the present work, we have synthesized La0.7Sr0.3MnO3 (LSMO) compound using sol-gel method and samples of crystallite size of ∼20, ∼41, and ∼49 nm were obtained by giving different heat treatment. Seebeck coefficient (α), electrical resistivity (ρ), and thermal conductivity (κ) measurements were carried out in 300–600 K temperature range. The systematic change in the values of α from ∼‑19 μV/K to ∼‑24 μV/K and drastic reduction in the values of κ from ∼0.88 W/mK to ∼0.23 W/mK are observed as crystallite size is reduced from 49 nm to 20 nm at ∼600 K. Also, fall in the values of ρ in the paramagnetic (PM) insulator phase (400–600 K) are effectively responsible for the increasing trend in the values of ZT at high temperature. For the crystallite size of 41 nm, the value of ZT at 600 K was found to be ∼0.017.
X-ray peak profile analysis of zinc oxide nanoparticles formed by simple precipitation method

NASA Astrophysics Data System (ADS)

Pelicano, Christian Mark; Rapadas, Nick Joaquin; Magdaluyo, Eduardo

2017-12-01

Zinc oxide (ZnO) nanoparticles were successfully synthesized by a simple precipitation method using zinc acetate and tetramethylammonium hydroxide. The synthesized ZnO nanoparticles were characterized by X-ray Diffraction analysis (XRD) and Transmission Electron Microscopy (TEM). The XRD result revealed a hexagonal wurtzite structure for the ZnO nanoparticles. The TEM image showed spherical nanoparticles with an average crystallite size of 6.70 nm. For x-ray peak analysis, Williamson-Hall (W-H) and Size-Strain Plot (SSP) methods were applied to examine the effects of crystallite size and lattice strain on the peak broadening of the ZnO nanoparticles. Based on the calculations, the estimated crystallite sizes and lattice strains obtained are in good agreement with each other.
XRD analysis of undoped and Fe doped TiO{sub 2} nanoparticles by Williamson Hall method

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

Bharti, Bandna; Barman, P. B.; Kumar, Rajesh, E-mail: rajesh.kumar@juit.ac.in

2015-08-28

Undoped and Fe doped titanium dioxide (TiO{sub 2}) nanoparticles were synthesized by sol-gel method at room temperature. The synthesized samples were annealed at 500°C. For structural analysis, the prepared samples were characterized by X-ray diffraction (XRD). The crystallite size of TiO{sub 2} and Fe doped TiO{sub 2} nanoparticles were calculated by Scherer’s formula, and was found to be 15 nm and 11 nm, respectively. Reduction in crystallite size of TiO{sub 2} with Fe doping was observed. The anatase phase of Fe-doped TiO{sub 2} nanoparticles was also confirmed by X-ray diffraction. By using Williamson-Hall method, lattice strain and crystallite size weremore » also calculated. Williamson–Hall plot indicates the presence of compressive strain for TiO{sub 2} and tensile strain for Fe-TiO{sub 2} nanoparticles annealed at 500°C.« less
The Scherrer equation and the dynamical theory of X-ray diffraction.

PubMed

Muniz, Francisco Tiago Leitão; Miranda, Marcus Aurélio Ribeiro; Morilla Dos Santos, Cássio; Sasaki, José Marcos

2016-05-01

The Scherrer equation is a widely used tool to determine the crystallite size of polycrystalline samples. However, it is not clear if one can apply it to large crystallite sizes because its derivation is based on the kinematical theory of X-ray diffraction. For large and perfect crystals, it is more appropriate to use the dynamical theory of X-ray diffraction. Because of the appearance of polycrystalline materials with a high degree of crystalline perfection and large sizes, it is the authors' belief that it is important to establish the crystallite size limit for which the Scherrer equation can be applied. In this work, the diffraction peak profiles are calculated using the dynamical theory of X-ray diffraction for several Bragg reflections and crystallite sizes for Si, LaB6 and CeO2. The full width at half-maximum is then extracted and the crystallite size is computed using the Scherrer equation. It is shown that for crystals with linear absorption coefficients below 2117.3 cm(-1) the Scherrer equation is valid for crystallites with sizes up to 600 nm. It is also shown that as the size increases only the peaks at higher 2θ angles give good results, and if one uses peaks with 2θ > 60° the limit for use of the Scherrer equation would go up to 1 µm.
Influences of Co doping on the structural and optical properties of ZnO nanostructured

NASA Astrophysics Data System (ADS)

Majeed Khan, M. A.; Wasi Khan, M.; Alhoshan, Mansour; Alsalhi, M. S.; Aldwayyan, A. S.

2010-07-01

Pure and Co-doped ZnO nanostructured samples have been synthesized by a chemical route. We have studied the structural and optical properties of the samples by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), field-emission transmission electron microscope (FETEM), energy-dispersive X-ray (EDX) analysis and UV-VIS spectroscopy. The XRD patterns show that all the samples are hexagonal wurtzite structures. Changes in crystallite size due to mechanical activation were also determined from X-ray measurements. These results were correlated with changes in particle size followed by SEM and TEM. The average crystallite sizes obtained from XRD were between 20 to 25 nm. The TEM images showed the average particle size of undoped ZnO nanostructure was about 20 nm whereas the smallest average grain size at 3% Co was about 15 nm. Optical parameters such as absorption coefficient ( α), energy band gap ( E g ), the refractive index ( n), and dielectric constants ( σ) have been determined using different methods.
Effects of solution concentration and capping agents on the properties of potassium titanyl phosphate noparticles synthesized using a co-precipitation method

NASA Astrophysics Data System (ADS)

Gharibshahian, E.; Jafar Tafershi, M.; Fazli, M.

2018-05-01

In this study, KTiOPO4 (KTP) nanoparticles were synthesized using a co-precipitation method. The effects of the solution concentration (M) and capping agents, such as PVA, oxalic acid, glycine, triethanolamine, and L-alanine, on the structural, microstructural, and optical properties of the products were investigated using X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, ultraviolet-visible spectroscopy, field emission scanning electron microscopy, and transmission electron microscopy. Decreasing the solution concentration decreased the crystallite size from 53.07 nm (for M = 2) to 39.42 nm (for M = 0.5). After applying different capping agents to the sample at the optimum concentration (M = 0.5), the crystallite size decreased again and grains as small as 10.61 nm were obtained. XRD and FTIR analyses indicated the formation of KTP nanoparticles with an orthorhombic structure in all of the samples. The optical band gap increased as the crystallite size decreased. Different morphological patterns such as spherical, needle shaped, polyhedron, and tablet forms were observed in the nanoparticles, which were correlated with the effects of the capping agents employed.
Synthesis and characterization of a mixed phase of anatase TiO2 and TiO2(B) by low pressure chemical vapour deposition (LPCVD) for high photocatalytic activity

NASA Astrophysics Data System (ADS)

Chimupala, Y.; Hyett, G.; Simpson, R.; Brydson, R.

2014-06-01

This project is concerned with enhancing photocatalytic activity by preparing a mixed phase of nano-sized TiO2. TiO2 thin films were synthesized by using Low Pressure Chemical Vapour Deposition (LPCVD). Titanium isopropoxide and N2 gas were used as the precursor and carrier gas respectively. The effects of reaction temperature, carrier gas flow rate and deposited area were studied. TiO2 thin films with nano-sized TiO2 particles were obtained under suitable conditions and SEM, TEM, powder XRD and Raman spectroscopy were employed to characterize the phase and physical appearance of synthesized materials. Preliminary results show that a dual phase (TiO2(B) and anatase) thin film nanopowder was successfully prepared by LPCVD with needle- and polygonal plate-shape crystallites respectively. This thin film deposit produced a preferred orientation of TiO2(B) needles in the [001] direction of average crystallite size 50-80 nm in length and 5-10 nm in width, whilst the crystallite size of anatase polygonal-plates was around 200 nm. The optimal LPCVD condition for preparing this mixed phase of TiO2 was 600°C with a 1 mL/s N2 flow rate.
Size-controlled synthesis of nanocrystalline CdSe thin films by inert gas condensation

NASA Astrophysics Data System (ADS)

Sharma, Jeewan; Singh, Randhir; Kumar, Akshay; Singh, Tejbir; Agrawal, Paras; Thakur, Anup

2018-02-01

Size, shape and structure are considered to have significant influence on various properties of semiconducting nanomaterials. Different properties of these materials can be tailored by controlling the size. Size-controlled CdSe crystallites ranging from ˜ 04 to 95 nm were deposited by inert gas-condensation technique (IGC). In IGC method, by controlling the inert gas pressure in the condensation chamber and the substrate temperature or both, it was possible to produce nanoparticles with desired size. Structure and crystallite size of CdSe thin films were determined from Hall-Williamson method using X-ray diffraction data. The composition of CdSe samples was estimated by X-ray microanalysis. It was confirmed that CdSe thin film with different nanometer range crystallite sizes were synthesized with this technique, depending upon the synthesis conditions. The phase of deposited CdSe thin films also depend upon deposition conditions and cubic to hexagonal phase transition was observed with increase in substrate temperature. The effect of crystallite size on optical and electrical properties of these films was also studied. The crystallite size affects the optical band gap, electrical conductivity and mobility activation of nanocrystalline CdSe thin films. Mobility activation study suggested that there is a quasi-continuous linear distribution of three different trap levels below the conduction band.
Size-dependent elastic/inelastic behavior of enamel over millimeter and nanometer length scales.

PubMed

Ang, Siang Fung; Bortel, Emely L; Swain, Michael V; Klocke, Arndt; Schneider, Gerold A

2010-03-01

The microstructure of enamel like most biological tissues has a hierarchical structure which determines their mechanical behavior. However, current studies of the mechanical behavior of enamel lack a systematic investigation of these hierarchical length scales. In this study, we performed macroscopic uni-axial compression tests and the spherical indentation with different indenter radii to probe enamel's elastic/inelastic transition over four hierarchical length scales, namely: 'bulk enamel' (mm), 'multiple-rod' (10's microm), 'intra-rod' (100's nm with multiple crystallites) and finally 'single-crystallite' (10's nm with an area of approximately one hydroxyapatite crystallite). The enamel's elastic/inelastic transitions were observed at 0.4-17 GPa depending on the length scale and were compared with the values of synthetic hydroxyapatite crystallites. The elastic limit of a material is important as it provides insights into the deformability of the material before fracture. At the smallest investigated length scale (contact radius approximately 20 nm), elastic limit is followed by plastic deformation. At the largest investigated length scale (contact size approximately 2 mm), only elastic then micro-crack induced response was observed. A map of elastic/inelastic regions of enamel from millimeter to nanometer length scale is presented. Possible underlying mechanisms are also discussed. (c) 2009 Elsevier Ltd. All rights reserved.
Magnesium-ion battery-relevant electrochemistry of MgMn 2O 4: crystallite size effects and the notable role of electrolyte water content

DOE PAGES

Yin, Jiefu; Brady, Alexander B.; Takeuchi, Esther S.; ...

2017-03-06

MgMn 2O 4 nanoparticles with crystallite sizes of 11 (MMO-1) and 31 nm (MMO-2) were synthesized and their magnesium-ion battery-relevant electrochemistry was investigated. Here, MMO-1 delivered an initial capacity of 220 mA h g –1 (678 mW h g –1). Electrolyte water content had a profound effect on cycle retention.
Controlling morphology and crystallite size of Cu(In{sub 0.7}Ga{sub 0.3})Se{sub 2} nano-crystals synthesized using a heating-up method

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

Hsu, Wei-Hsiang; Hsiang, Hsing-I, E-mail: hsingi@mail.ncku.edu.tw; Chia, Chih-Ta

2013-12-15

CuIn{sub 0.7}Ga{sub 0.3}Se{sub 2}(CIGS) nano-crystals were successfully synthesized via a heating-up process. The non-coordinating solvent (1-octadecene) and selenium/cations ratio effects on the crystalline phase and crystallite size of CIGS nano-crystallites were investigated. It was observed that the CIGS nano-crystallite morphology changed from sheet into spherical shape as the amount of 1-octadecene addition was increased. CIGS nano-crystals were obtained in 9–20 nm sizes as the selenium/cations ratio increased. These results suggest that the monomer reactivity in the solution can be adjusted by changing the solvent type and selenium/cations ratio, hence affecting the crystallite size and distribution. - Graphical abstract: CuIn{sub 0.7}Ga{submore » 0.3}Se{sub 2}(CIGS) nano-crystals were successfully synthesized via a heating-up process in this study. The super-saturation in the solution can be adjusted by changing the OLA/ODE ratio and selenium/cation ratio.« less
Structural and optical properties of ZnO thin films prepared by RF sputtering at different thicknesses

NASA Astrophysics Data System (ADS)

Hammad, Ahmed H.; Abdel-wahab, M. Sh.; Vattamkandathil, Sajith; Ansari, Akhalakur Rahman

2018-07-01

Hexagonal nanocrystallites of ZnO in the form of thin films were prepared by radio frequency sputtering technique. X-ray diffraction analysis reveals two prominent diffraction planes (002) and (103) at diffraction angles around 34.3 and 62.8°, respectively. The crystallite size increases through (103) plane from 56.1 to 64.8 Å as film thickness changed from 31 nm up to 280 nm while crystallites growth through (002) increased from 124 to 136 Å as film thickness varies from 31 to 107 nm and dropped to 115.8 Å at thickness 280 nm. The particle shape changes from spherical to longitudinal form. The particle size is 25 nm for films of thickness below 107 nm and increases at higher thicknesses (134 and 280 nm) from 30 to 40 nm, respectively. Optical band gap is deduced to be direct with values varied from 3.22 to 3.28 eV and the refractive index are evaluated based on the optical band values according to Moss, Ravindra-Srivastava, and Dimitrov-Sakka models. All refractive index models gave values around 2.3.
Effect of current density during electrodeposition on microstructure and hardness of textured Cu coating in the application of antimicrobial Al touch surface.

PubMed

Augustin, Arun; Huilgol, Prashant; Udupa, K Rajendra; Bhat K, Udaya

2016-10-01

Copper is a well proven antimicrobial material which can be used in the form of a coating on the touch surfaces. Those coating can offer a good service as touch surface for very long time if only they possess good mechanical properties like scratch resistance and microhardness. In the present work the above mentioned mechanical properties were determined on the electrodeposited copper thin film; deposited on double zincated aluminium. During deposition, current density was varied from 2Adm(-2) to 10Adm(-2), to produce crystallite size in the range of 33.5nm to 66nm. The crystallite size was calculated from the X-ray peak broadening (Scherrer׳s formula) which were later confirmed by TEM micrographs. The scratch hardness and microhardness of the coating were measured and correlated with the crystallite size in the copper coating. Both characteristic values were found to increase with the reduction in crystallite size. Reduced crystallite size (Hall-Petch effect) and preferred growth of copper films along (111) plane play a significant role on the increase in the hardness of the coating. Further, TEM analysis reveals the presence of nano-twins in the film deposited at higher current density, which contributed to a large extent to the sharp increase of coating hardness compared to the mechanism of Hall-Petch effect. The antimicrobial ability of the coated sample has been evaluated against Escherichia coli bacteria and which is compared with that of commercially available bulk copper using the colony count method. 94% of E. coli cells were died after six hours of exposure to the copper coated surface. The morphology of the copper treated cells was studied using SEM. Copyright © 2016 Elsevier Ltd. All rights reserved.
Role of SiO2 coating in multiferroic CoCr2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Kamran, M.; Ullah, Asmat; Mehmood, Y.; Nadeem, K.; Krenn, H.

2017-02-01

Effect of silica (SiO2) coating concentration on structural and magnetic properties of multiferroic cobalt chromite (CoCr2O4) nanoparticles have been studied. The nanoparticles with average crystallite size in the range 19 to 28 nm were synthesised by sol-gel method. X-ray diffraction (XRD) analysis has verified the composition of single-phase cubic normal spinel structure of CoCr2O4 nanoparticles. The average crystallite size and cell parameter decreased with increasing SiO2 concentration. TEM image revealed that the shape of nanoparticles was non-spherical. Zero field cooled/field cooled (ZFC/FC) curves revealed that nanoparticles underwent a transition from paramagnetic (PM) state to collinear short-range ferrimagnetic (FiM) state, and this PM-FiM transition temperature decreased from 101 to 95 K with increasing SiO2 concentration or decreasing crystallite size. A conical spin state at Ts = 27 K was also observed for all the samples which decreased with decreasing average crystallite size. Low temperature lock-in transition was also observed in these nanoparticles at 12 K for uncoated nanoparticles which slightly shifted towards low temperature with decreasing average crystallite size. Saturation magnetization (Ms) showed decreasing trend with increasing SiO2 concentration, which was due to decrease in average crystallite size of nanoparticles and enhanced surface disorder in smaller nanoparticles. The temperature dependent AC-susceptibility also showed the decrease in the transition temperature (Tc), broadening of the Tc peak and decrease in magnetization with increasing SiO2 concentration or decreasing average crystallite size. In summary, the concentration of SiO2 has significantly affected the structural and magnetic properties of CoCr2O4 nanoparticles.
Size-induced variations in bulk/surface structures and their impact on photoluminescence properties of GdVO4:Eu3+ nanoparticles.

PubMed

Yang, Liusai; Li, Liping; Zhao, Minglei; Li, Guangshe

2012-07-28

This work explores the size-induced lattice modification and its relevance to photoluminescence properties of tetragonal zircon-type GdVO(4):Eu(3+) nanostructures. GdVO(4):Eu(3+) nanoparticles with crystallite sizes ranging from 14.4 to 24.7 nm were synthesized by a hydrothermal method using sodium citrate as a capping agent. Regardless of the reaction temperatures, all samples retained an ellipsoidal-like morphology. Nevertheless, as the crystallite size reduces, there appears a tensile strain and lattice distortion, which is accompanied by a lattice expansion and a decreased symmetry of structural units. These lattice modifications could be associated with the changes in the interior chemical bonding due to the interactions of surface defect dipoles that have imposed an increased negative pressure with crystallite size reduction. Furthermore, crystallite size reduction also led to a significant increase in the amounts of surface hydroxyl groups and citric species, as well as the concentration of the surface Eu(3+) ions. When Eu(3+) was taken as a structural probe, it was found that the asymmetric ratio (I(02)/I(01)) of Eu(3+) gradually declined to show a remarkable decrease in color chromaticity as crystallite size reduces, which could be interpreted as due to the change of local environments of Eu(3+) ions from the interior to the surface of the nanoparticles.

Effect of Cu2+ substitution on the structural, optical and magnetic behaviour ofchemically derived manganese ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Vasuki, G.; Balu, T.

2018-06-01

Mixed spinel copper manganese ferrite (CuXMn1‑XFe2O4, X = 0, 0.25, 0.5, 0.75, 1) nanoparticles were synthesized by chemical co-precipitation technique. From the powder x-ray diffraction analysis the lattice constant, volume of unit cell, x-ray density, hopping lengths, crystallite size, surface area, dislocation density and microstrain were calculated. The substitution of Cu2+ ions shows a considerable reduction in the crystallite size of manganese ferrite from 34 nm to 22 nm. Further a linear fit of Williamson-Hall plot has been drawn to determine the microstrain and crystallite size. The crystallite size and morphology were further observed through high resolution transmission electron microscope and scanning electron microscope. The diffraction rings observed from selected area electron diffraction pattern exhibits the crystalline nature of all the samples. The energy dispersive x-ray analysis shows the composition of all the elements incorporated in the synthesized nanomaterials. FTIR studies reveal the absorption peaks that correspond to the metal-oxygen vibrations in the tetrahedral and octahedral sites. From the UV–vis absorption spectra the band gap energy, refractive index and optical dielectric constant were determined. Magnetic studies carried out using vibrating sample magnetometer shows interesting behaviour in the variation of magnetisation and coercivity. Peculiar magnetic behaviour is observed when Cu2+ ions are substituted in manganese ferrites. All the synthesized materials have very low value of squareness ratio which attributes to the superparamagnetic behaviour.
Williamson-Hall analysis and optical properties of small sized ZnO nanocrystals

NASA Astrophysics Data System (ADS)

Kalita, Amarjyoti; Kalita, Manos P. C.

2017-08-01

We apply Williamson-Hall (WH) method of X-ray diffraction (XRD) line profile analysis for lattice strain estimation of small sized ZnO nanocrystals (crystallite size≈4 nm). The ZnO nanocrystals are synthesized by room temperature chemical co-precipitation followed by heating at 40 °C. Zinc acetate, sodium hydroxide and 2-mercaptoethanol (ME) are used for the synthesis of the nanocrystals. {100}, {002}, {101} and {200}, {112}, {201} line profiles in the XRD pattern are significantly merged, therefore determination of the full width at half maximum values and peak positions of the line profiles required for WH analysis has been carried out by executing Rietveld refinement of the XRD pattern. Lattice strain of the 4 nm sized ZnO nanocrystals is found to be 5.8×10-3 which is significantly higher as compared to the literature reported values for larger ones (crystallite size≈17-47 nm). Role of ME as capping agent is confirmed by Fourier transform infrared spectroscopy. The band gap of the nanocrystals is determined from the UV-Visible absorption spectrum and is found to be 3.68 eV. The photoluminescence spectrum exhibits emissions in the visible (408 nm-violet, 467 nm-blue and 538 nm-green) regions showing presence of zinc interstitial and oxygen vacancy in the ZnO nanocrystals.
Synthesis and structural characterization of transition metal doped MgO: Mg0.95Mn0.01TM0.04O (TM = Co, Ni, Cu)

NASA Astrophysics Data System (ADS)

Islam, Ishtihadah; Khandy, Shakeel Ahmad; Hafiz, Aurangzeb Khurram

2018-05-01

In the present work, preparation and characterization of transition metal doped MgO: Zn0.94Mn0.01TM0.05O (TM = Co, Ni and Cu) nano-particles have been reported. Transition metal doped samples of MgO were synthesized by Sol gel auto combustion method. Structural characterisation from XRD and SEM show the formation of single-phase primary particles, nearly of spherical shaped nano-crystallites. The crystallite size was found to be 78.2, 67.02, 78.11 and 64 nm for pure, Co, Cu and Ni doped MgMnO nano-particles, respectively. Hence, the average crystallite size increases monotonously from Co to Cu doping.
Synthesis and characterization of nano-sized zirconia powder synthesized by single emulsion-assisted direct precipitation.

PubMed

Chandra, Navin; Singh, Deepesh Kumar; Sharma, Meenakshi; Upadhyay, Ravi Kant; Amritphale, S S; Sanghi, S K

2010-02-15

For the first time, single reverse microemulsion-assisted direct precipitation route has been successfully used to synthesize tetragonal zirconia nanoparticles in narrow size range. The synthesized powder was characterized using FT-IR, XRD and HRTEM techniques. The zirconia nanoparticles obtained were spherical in shape and has narrow particle size distribution in the range of 13-31nm and crystallite size in the range of 13-23nm. Copyright 2009 Elsevier Inc. All rights reserved.
Microstructural Evolution of Nanocrystalline ZrO2 in a Fe Matrix During High-Temperature Exposure

NASA Astrophysics Data System (ADS)

Raghavendra, K. G.; Dasgupta, Arup; Athreya, C. N.; Jayasankar, K.; Saroja, S.; Subramanya Sarma, V.

2018-06-01

The current study examines the evolution of nanocrystallites of ZrO2 with time and temperature in a Fe-ZrO2 composite. The crystallite sizes were determined through X-ray peak broadening analysis by the Williamson-Hall method together with dark field transmission electron microscopy. The ZrO2 crystallites were found to be stable and retained their sizes at 973 K and 1073 K for hold durations up to 600 minutes. On the other hand, the crystallites were seen to grow at 1173 K and reached up to 200 nm for a hold time of 600 minutes. The Ostwald ripening model was adopted to understand crystallite growth while a dislocation-driven pipe diffusion was adopted for understanding the kinetics of grain growth. The activation energy of grain growth was calculated as 379 kJ mol-1. The modeled and experimentally calculated size evolutions with time and temperature were shown to be in good agreement with each other. A detailed discussion on the kinetics and activation energy of grain growth of ZrO2 crystallites in a Fe matrix is presented in this manuscript.
Phase Composition, Crystallite Size and Physical Properties of B2O3-added Forsterite Nano-ceramics

NASA Astrophysics Data System (ADS)

Pratapa, S.; Chairunnisa, A.; Nurbaiti, U.; Handoko, W. D.

2018-05-01

This study was aimed to know the effect of B2O3 addition on the phase composition, crystallite size and dielectric properties of forsterite (Mg2SiO4) nano-ceramics. It utilized a purified silica sand from Tanah Laut, South Kalimantan as the source of (amorphous) silica and a magnesium oxide (MgO) powder. They were thoroughly mixed and milled prior to calcination. The addition of 1, 2, 3, and 4 wt% B2O3 to the calcined powder was done before uniaxial pressing and then sintering at 950 °C for 4 h. The phase composition and forsterite crystallite size, the microstructure and the dielectric constant of the sintered samples were characterized using X-ray diffractometer (XRD), Scanning Electron Microscope (SEM) and Vector Network Analyzer (VNA), respectively. Results showed that all samples contained forsterite, periclase (MgO) and proto enstatite (MgSiO3) with different weight fractions and forsterite crystallite size. In general, the weight fraction and crystallite size of forsterite increased with increasing B2O3 addition. The weight fraction and crystallite size of forsterite in the 4%-added sample reached 99% wt and 164 nm. Furthermore, the SEM images showed that the average grain size became slightly larger and the ceramics also became slightly denser as more B2O3 was added. The results are in accordance with density measurements using the Archimedes method which showed that the 4% ceramic exhibited 1.845 g/cm3 apparent density, while the 1% ceramic 1.681 g/cm3. We also found that the higher the density, the higher the average dielectric constant, i.e. it was 4.6 for the 1%-added sample and 6.4 for the 4%-added sample.
Structural properties and gas sensing behavior of sol-gel grown nanostructured zinc oxide

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

Rajyaguru, Bhargav; Gadani, Keval; Kansara, S. B.

2016-05-06

In this communication, we report the results of the studies on structural properties and gas sensing behavior of nanostructured ZnO grown using acetone precursor based modified sol-gel technique. Final product of ZnO was sintered at different temperatures to vary the crystallite size while their structural properties have been studied using X-ray diffraction (XRD) measurement performed at room temperature. XRD results suggest the single phasic nature of all the samples and crystallite size increases from 11.53 to 20.96 nm with increase in sintering temperature. Gas sensing behavior has been studied for acetone gas which indicates that lower sintered samples are moremore » capable to sense the acetone gas and related mechanism has been discussed in the light of crystallite size, crystal boundary density, defect mechanism and possible chemical reaction between gas traces and various oxygen species.« less
Structural, morphological, and optical properties of tin(IV) oxide nanoparticles synthesized using Camellia sinensis extract: a green approach

NASA Astrophysics Data System (ADS)

Selvakumari, J. Celina; Ahila, M.; Malligavathy, M.; Padiyan, D. Pathinettam

2017-09-01

Tin oxide (SnO2) nanoparticles were cost-effectively synthesized using nontoxic chemicals and green tea ( Camellia sinensis) extract via a green synthesis method. The structural properties of the obtained nanoparticles were studied using X-ray diffraction, which indicated that the crystallite size was less than 20 nm. The particle size and morphology of the nanoparticles were analyzed using scanning electron microscopy and transmission electron microscopy. The morphological analysis revealed agglomerated spherical nanoparticles with sizes varying from 5 to 30 nm. The optical properties of the nanoparticles' band gap were characterized using diffuse reflectance spectroscopy. The band gap was found to decrease with increasing annealing temperature. The O vacancy defects were analyzed using photoluminescence spectroscopy. The increase in the crystallite size, decreasing band gap, and the increasing intensities of the UV and visible emission peaks indicated that the green-synthesized SnO2 may play future important roles in catalysis and optoelectronic devices.
Synthesis, Optical and Structural Properties of Copper Sulfide Nanocrystals from Single Molecule Precursors

PubMed Central

Ajibade, Peter A.; Botha, Nandipha L.

2017-01-01

We report the synthesis and structural studies of copper sulfide nanocrystals from copper (II) dithiocarbamate single molecule precursors. The precursors were thermolysed in hexadecylamine (HDA) to prepare HDA-capped CuS nanocrystals. The optical properties of the nanocrystals studied using UV–visible and photoluminescence spectroscopy showed absorption band edges at 287 nm that are blue shifted, and the photoluminescence spectra show emission curves that are red-shifted with respect to the absorption band edges. These shifts are as a result of the small crystallite sizes of the nanoparticles leading to quantum size effects. The structural studies were carried out using powder X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and atomic force microscopy. The XRD patterns indicates that the CuS nanocrystals are in hexagonal covellite crystalline phases with estimated particles sizes of 17.3–18.6 nm. The TEM images showed particles with almost spherical or rod shapes, with average crystallite sizes of 3–9.8 nm. SEM images showed morphology with ball-like microspheres on the surfaces, and EDS spectra confirmed the presence of CuS nanoparticles. PMID:28336865
Use of scanning near-field optical microscope with an aperture probe for detection of luminescent nanodiamonds

NASA Astrophysics Data System (ADS)

Shershulin, V. A.; Samoylenko, S. R.; Shenderova, O. A.; Konov, V. I.; Vlasov, I. I.

2017-02-01

The suitability of scanning near-field optical microscopy (SNOM) to image photoluminescent diamond nanoparticles with nanoscale resolution is demonstrated. Isolated diamond nanocrystals with an average size of 100 nm, containing negatively charged nitrogen-vacancy (NV-) centers, were chosen as tested material. The NV- luminescence was stimulated by continuous 532 nm laser light. Sizes of analyzed crystallites were monitored by an atomic force microscope. The lateral resolution of the order of 100 nm was reached in SNOM imaging of diamond nanoparticles using 150 nm square aperture of the probe.
Structure of Cu/Ni Nanowires Obtained by Matrix Synthesis

NASA Astrophysics Data System (ADS)

Zhigalina, O. M.; Doludenko, I. M.; Khmelenin, D. N.; Zagorskiy, D. L.; Bedin, S. A.; Ivanov, I. M.

2018-05-01

The structure of layered Cu/Ni nanowires obtained by template synthesis in 100-nm channels of track membranes has been investigated by transmission and scanning electron microscopy. The phase composition and main structural features of individual nanowires are determined. It is shown that nanowires consist of alternating Ni ( Fm3m) and Cu ( Fm3m) layers with grains up to 100 nm in size. It is found that nanowires contain also copper oxide crystallites up to 20 nm in size. The elemental composition of individual layers and their mutual arrangement are determined.
Zinc-Containing Restorations Create Amorphous Biogenic Apatite at the Carious Dentin Interface: A X-Ray Diffraction (XRD) Crystal Lattice Analysis.

PubMed

Toledano, Manuel; Aguilera, Fátima S; López-López, Modesto T; Osorio, Estrella; Toledano-Osorio, Manuel; Osorio, Raquel

2016-10-01

The aim of this research was to assess the ability of amalgam restorations to induce amorphous mineral precipitation at the caries-affected dentin substrate. Sound and caries-affected dentin surfaces were subjected to both Zn-free and Zn-containing dental amalgam restorations. Specimens were submitted to thermocycling (100,000 cycles/5°C-55°C, 3 months). Dentin surfaces were studied by atomic force microscopy (nanoroughness), X-ray diffraction, field emission scanning electron microscopy, and energy-dispersive analysis, for physical and morphological surface characterization. Zn-containing amalgam placement reduced crystallinity, crystallite size, and grain size of calcium phosphate crystallites at the dentin surface. Both microstrain and nanoroughness were augmented in caries-affected dentin restored with Zn-containing amalgams. Caries-affected dentin showed the shortest mineral crystallites (11.04 nm), when Zn-containing amalgams were used for restorations, probably leading to a decrease of mechanical properties which might favor crack propagation and deformation. Sound dentin restored with Zn-free amalgams exhibited a substantial increase in length of grain particles (12.44 nm) embedded into dentin crystallites. Zn-containing amalgam placement creates dentin mineralization and the resultant mineral was amorphous in nature. Amorphous calcium phosphate provides a local ion-rich environment, which is considered favorable for in situ generation of prenucleation clusters, promotong further dentin remineralization.
Effect of oxidizer to fuel molar ratio on particle size and DC conductivity of CeO{sub 2} nanoparticles

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

Harish, B. M.; Rajeeva, M. P.; Naveen, C. S.

2016-05-06

Cerium oxide nanoparticles were synthesized by solution combustion method with varying the oxidizer (cerium nitrate hexa hydrate) to fuel (Glycine) molar ratio. The prepared samples were characterized by UV-visible spectrometer, X-ray diffractometer (XRD), Scanning electron microscope (SEM) and Energy dispersive X-Ray analysis (EDAX). XRD pattern reveals the formation of cubic fluorite structure of CeO{sub 2}. It was observed that finest crystallites were found at extreme fuel-deficient condition and it is good enough to produce favorable powder characteristics. The average crystallite size was found to be 14.46 nm to 21.57 nm. The temperature dependent dc conductivity was carried out using Keithleymore » source meter between the temperature range from 300 K to 573 K. From this study it was found that the conductivity increases with increase of temperature due to semiconducting behavior of CeO{sub 2} and it decreases with particle size due to increase in the energy band gap.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)

Tahir, Dahlang, E-mail: dtahir@fmipa.unhas.ac.id; Bakri, Fahrul; Liong, Syarifuddin

We have studied the molecular properties, structural properties, and chemical composition of composites by Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) spectroscopy, and X-ray fluorescence (XRF) spectroscopy, respectively. FTIR spectra shows absorption band of hydroxyl group (-OH), methyl group (-CH{sub 3}) and aromatic group (C-C). The absorption band for aromatic group (C-C) shows the formation of carbonaceous in composites. XRF shows chemical composition of composites, which the main chemicals are SO{sub 3}, Cl, and ZnO. The loss on ignition value (LOI) of activated charcoal indicates high carbonaceous matter. The crystallite size for diffraction pattern from hydrogel polymer is aboutmore » 17 nm and for activated charcoal are about 19 nm. The crystallite size of the polymer is lower than that of activated charcoal, which make possible of the particle from filler in contact with each other to form continuous conducting polymer through polymer matrix.« less
Microstructural changes in CdSe-coated ZnO nanowires evaluated by in situ annealing in transmission electron microscopy and x-ray diffraction

NASA Astrophysics Data System (ADS)

Majidi, Hasti; Winkler, Christopher R.; Taheri, Mitra L.; Baxter, Jason B.

2012-07-01

We report on the crystallite growth and phase change of electrodeposited CdSe coatings on ZnO nanowires during annealing. Both in situ transmission electron microscopy (TEM) and x-ray diffraction (XRD) reveal that the nanocrystal size increases from ˜3 to ˜10 nm upon annealing at 350 °C for 1 h and then to more than 30 nm during another 1 h at 400 °C, exhibiting two distinct growth regimes. Nanocrystal growth occurs together with a structural change from zinc blende to wurtzite. The structural transition begins at 350 °C, which results in the formation of stacking faults. Increased crystallite size, comparable to the coating thickness, can improve charge separation in extremely thin absorber solar cells. We demonstrate a nearly two-fold improvement in power conversion efficiency upon annealing.
Synthesis and Characterization of Some Alkaline-Earth-Oxide Nanoparticles

NASA Astrophysics Data System (ADS)

Singh, Jitendra Pal; Lim, Weon Cheol; Won, Sung Ok; Song, Jonghan; Chae, Keun Hwa

2018-04-01

The present work reports the synthesis of MgO and CaO nanoparticles by using the sol-gel autocombustion method. The annealing of the precursor at 1200 °C was observed to lead the formation of MgO nanoparticles having average crystallite size of 31 nm. Annealing the precursor at same temperature produced materials having a CaO phase with a minor impure phase of calcium carbonate ( 3%). The crystallite size corresponding to the CaO phase was 38 nm. A change of thermal history in the precursor was observed not to result in an improvement of the CaO phase. The change of thermal history in the precursor gave rise to mixed phases of CaCO3 and Ca(OH)2 rather than the phase of CaO. Further, annealing at 1200 °C for 12 h resulted in the formation of the CaO phase along with almost 1 - 5% of calcium hydroxide as an impurity phase. X-ray absorption spectroscopic measurements carried out on these materials revealed that the local electronic/atomic structure of these oxides was not only affected by the impurity phases but also influenced by the carbaneous impurities attached to the crystallites.
Structural and Morphological Evaluation of Nano-Sized MoSi2 Powder Produced by Mechanical Milling

NASA Astrophysics Data System (ADS)

Sameezadeh, Mahmood; Farhangi, Hassan; Emamy, Masoud

Nano-sized intermetallic powders have received great attention owing to their property advantages over conventional micro-sized counterparts. In the present study nano-sized MoSi2 powder has been produced successfully from commercially available MoSi2 (3 μm) by a mechanical milling process carried out for a period of 100 hours. The effects of milling time on size and morphology of the powders were studied by SEM and TEM and image analyzing system. The results indicate that the as-received micrometric powder with a wide size distribution of irregular shaped morphology changes to a narrow size distribution of nearly equiaxed particles with the progress of attrition milling up to 100 h, reaching an average particle size of 71 nm. Structural evolution of milled samples was characterized by XRD to determine the crystallite size and lattice microstrain using Williamson-Hall method. According to the results, the crystallite size of the powders decreases continuously down to 23 nm with increasing milling time up to 100 h and this size refinement is more rapid at the early stages of the milling process. On the other hand, the lattice strain increases considerably with milling up to 65 h and further milling causes no significant changes of lattice strain.
Structural, magnetic, dielectric, and electrical properties of NiFe2O4 spinel ferrite nanoparticles prepared by honey-mediated sol-gel combustion

NASA Astrophysics Data System (ADS)

Yadav, Raghvendra Singh; Kuřitka, Ivo; Vilcakova, Jarmila; Havlica, Jaromir; Masilko, Jiri; Kalina, Lukas; Tkacz, Jakub; Enev, Vojtěch; Hajdúchová, Miroslava

2017-08-01

In this study, NiFe2O4 nanoparticles were synthesized using a honey-mediated sol-gel combustion method. The synthesized nanoparticles and samples annealed at 800 °C and 1100 °C were characterized by X-ray diffraction (XRD), field emission-scanning electron microscopy (FE-SEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and vibrating sample magnetometry (VSM). XRD and Raman spectroscopy confirmed the formation of a cubic spinel ferrite structure. FE-SEM demonstrated the octahedral morphology of the NiFe2O4 spinel ferrite nanoparticles with sizes ranging from 10 to 70 nm. Quantitative analysis based on XPS suggested a mixed spinel structure comprising NiFe2O4 nanoparticles. XPS analysis determined occupation formulae of (Ni0.212+ Fe0.443+)[Ni0.792+ Fe1.563+]O4 and (Ni0.232+ Fe0.503+)[Ni0.772+ Fe1.503+]O4, for the as-prepared NiFe2O4 nanoparticles and those annealed at 1100 °C, respectively. Magnetic measurements showed that the saturation magnetization increased with the crystallite size from 32.3 emu/g (20 nm) to 49.9 emu/g (163 nm), whereas the coercivity decreased with the crystallite size from 162 Oe (20 nm) to 47 Oe (163 nm). Furthermore, the dielectric constant, dielectric loss tangent, and AC conductivity of the NiFe2O4 nanoparticles were dependent on the frequency (1-107 Hz) and grain size. The influence of the grain size was also observed by modulus spectroscopy based on the Cole-Cole plot.
Size dependent polaronic conduction in hematite

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

Sharma, Monika; Banday, Azeem; Murugavel, Sevi

2016-05-23

Lithium Ion Batteries have been attracted as the major renewable energy source for all portable electronic devices because of its advantages like superior energy density, high theoretical capacity, high specific energy, stable cycling and less memory effects. Recently, α-Fe{sub 2}O{sub 3} has been considered as a potential anode material due to high specific capacity, low cost, high abundance and environmental benignity. We have synthesized α-Fe{sub 2}O{sub 3} with various sizes by using the ball milling and sol-gel procedure. Here, we report the dc conductivity measurement for the crystallite size ranging from 15 nm to 50 nm. It has been observedmore » that the enhancement in the polaronic conductivity nearly two orders in magnitude while reducing the crystallite size from bulk into nano scale level. The enhancement in the conductivity is due to the augmented to compressive strain developed in the material which leads to pronounced decrease in the hopping length of polarons. Thus, nanocrystaline α-Fe{sub 2}O{sub 3} may be a better alternative anode material for lithium ion batteries than earlier reported systems.« less
Influence of the hydrothermal temperature and pH on the crystallinity of a sputtered hydroxyapatite film

NASA Astrophysics Data System (ADS)

Ozeki, K.; Aoki, H.; Masuzawa, T.

2010-09-01

Hydroxyapatite (HA) was coated onto titanium substrates using radio frequency sputtering, and the sputtered films were crystallized under hydrothermal conditions at 110-170 °C at pH values of 7.0 and 9.5. The crystallite size, the remnant film thickness, and the surface morphology of the films were observed using X-ray diffraction, energy dispersive X-ray spectroscopy, and scanning electron microscopy, respectively. The crystallite size increased with the process temperature, and reached 123.6 nm (pH 9.5 and 170 °C) after 24 h. All of the crystallite sizes of the film treated at pH 9.5 were higher than those treated at pH 7.0 at each process temperature. The film treated at pH 9.5 retained more than 90% of the initial film thickness at any process temperature. The ratio of the film treated at pH 7.0 did not reached 90% at less than 150 °C, and tended to increase with the process temperature.

Influence of Fe doping on the structural, optical and acetone sensing properties of sprayed ZnO thin films

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

Prajapati, C.S.; Kushwaha, Ajay; Sahay, P.P., E-mail: dr_ppsahay@rediffmail.com

2013-07-15

Graphical abstract: All the films are found to be polycrystalline ZnO possessing hexagonal wurtzite structure. The intensities of all the peaks are diminished strongly in the Fe-doped films, indicating their lower crystallinity as compared to the undoped ZnO film. The average crystallite size decreases from 35.21 nm (undoped sample) to 15.43 nm (1 at% Fe-doped sample). - Highlights: • Fe-doped ZnO films show smaller crystallinity with crystallite size: 15–26 nm. • Optical band gap in ZnO films decreases on Fe doping. • Fe-doped films exhibit the normal dispersion for the wavelength range 450–600 nm. • PL spectra of the Fe-dopedmore » films show quenching of the broad green-orange emission. • Acetone response of the Fe-doped films increases considerably at 300 °C. - Abstract: The ZnO thin films (undoped and Fe-doped) deposited by chemical spray pyrolysis technique have been analyzed by X-ray powder diffraction (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM). Results show that all the films possess hexagonal wurtzite structure of zinc oxide having crystallite sizes in the range 15–36 nm. On 1 at% Fe doping, the surface roughness of the film increases which favors the adsorption of atmospheric oxygen on the film surface and thereby increase in the gas response. Optical studies reveal that the band gap decreases due to creation of some defect energy states below the conduction band edge, arising out of the lattice disorder in the doped films. The refractive index of the films decreases on Fe doping and follows the Cauchy relation of normal dispersion. Among all the films examined, the 1 at% Fe-doped film exhibits the maximum response (∼72%) at 300 °C for 100 ppm concentration of acetone in air.« less
Phase composition and morphological characterization of human kidney stones using IR spectroscopy, scanning electron microscopy and X-ray Rietveld analysis.

PubMed

Chatterjee, Paramita; Chakraborty, Arup; Mukherjee, Alok K

2018-07-05

Pathological calcification in human urinary tract (kidney stones) is a common problem affecting an increasing number of people around the world. Analysis of such minerals or compounds is of fundamental importance for understanding their etiology and for the development of prophylactic measures. In the present study, structural characterization, phase quantification and morphological behaviour of thirty three (33) human kidney stones from eastern India have been carried out using IR spectroscopy (FT-IR), powder X-ray diffraction (PXRD) and scanning electron microscopy (SEM). Quantitative phase composition of kidney stones has been analyzed following the Rietveld method. Based on the quantitative estimates of constituent phases, the calculi samples have been classified into oxalate (OX), uric acid (UA), phosphate (PH) and mixed (MX) groups. Rietveld analysis of PXRD patterns showed that twelve (36%) of the renal calculi were composed exclusively of whewellite (calcium oxalate monohydrate, COM). The remaining twenty one (64%) stones were mixture of phases with oxalate as the major constituent in fourteen (67%) of these stones. The average crystallite size of whewellite in oxalate stones, as determined from the PXRD analysis, varies between 93 (1) nm and 202 (3) nm, whereas the corresponding sizes for the uric acid and struvite crystallites in UA and PH stones are 79 (1)-155 (4) nm and 69 (1)-123(1) nm, respectively. The size of hydroxyapatite crystallites, 10 (1)-21 (1) nm, is smaller by about one order of magnitude compared to other minerals in the kidney stones. A statistical analysis using fifty (50) kidney stones (33 calculi from the present study and 17 calculi reported earlier from our laboratory) revealed that the oxalate group (whewellite, weddellite or mixture of whewellite and weddellite as the major constituent) is the most prevalent (82%) kidney stone type in eastern India. Copyright © 2018 Elsevier B.V. All rights reserved.
Characterization of the enhancement effect of Na2CO3 on the sulfur capture capacity of limestones.

PubMed

Laursen, Karin; Kern, Arnt A; Grace, John R; Lim, C Jim

2003-08-15

It has been known for a long time that certain additives (e.g., NaCl, CaCl2, Na2CO3, Fe2O3) can increase the sulfur dioxide capture-capacity of limestones. In a recent study we demonstrated that very small amounts of Na2CO3 can be very beneficial for producing sorbents of very high sorption capacities. This paper explores what contributes to these significant increases. Mercury porosimetry measurements of calcined limestone samples reveal a change in the pore-size from 0.04-0.2 microm in untreated samples to 2-10 microm in samples treated with Na2CO3--a pore-size more favorable for penetration of sulfur into the particles. The change in pore-size facilitates reaction with lime grains throughout the whole particle without rapid plugging of pores, avoiding premature change from a fast chemical reaction to a slow solid-state diffusion controlled process, as seen for untreated samples. Calcination in a thermogravimetric reactor showed that Na2CO3 increased the rate of calcination of CaCO3 to CaO, an effect which was slightly larger at 825 degrees C than at 900 degrees C. Peak broadening analysis of powder X-ray diffraction data of the raw, calcined, and sulfated samples revealed an unaffected calcite size (approximately 125-170 nm) but a significant increase in the crystallite size for lime (approximately 60-90 nm to approximately 250-300 nm) and less for anhydrite (approximately 125-150 nm to approximately 225-250 nm). The increase in the crystallite and pore-size of the treated limestones is attributed to an increase in ionic mobility in the crystal lattice due to formation of vacancies in the crystals when Ca is partly replaced by Na.
Electronic and structural properties of micro-and nanometre-sized crystalline copper monoxide ceramics investigated by positron annihilation

NASA Astrophysics Data System (ADS)

Druzhkov, A. P.; Gizhevskii, B. A.; Arbuzov, V. L.; Kozlov, E. A.; Shalnov, K. V.; Naumov, S. V.; Perminov, D. A.

2002-09-01

Electronic and structural properties of copper monoxide (CuO) sintered as a common ceramic and nanoceramic are studied by positron annihilation spectroscopy. A CuO nanoceramic with crystallite size ranging from 15 to 90 nm was prepared from a common one by shock-wave loading. It is found that the momentum distribution of valence electrons in CuO is shifted, as compared with metallic copper, towards higher momentum values. This result is related to the effect of the Cu 3d-O 2p hybridization in the Cu-O ionic covalent bond formation. It is found that open volumes, identified mainly as small agglomerates of oxygen vacancies, appear at the nanoceramic crystallite interfaces. The degree of the Cu-O bond covalency decreases locally at the crystallite interfaces because of an oxygen deficit. The nanocrystalline state in CuO is shown to be thermally stable up to 700 K.
Size dependence of magnetorheological properties of cobalt ferrite ferrofluid

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

Radhika, B.; Sahoo, Rasmita; Srinath, S., E-mail: srinath@uohyd.ac.in

2015-06-24

Cobalt Ferrite nanoparticles were synthesized using co-precipitation method at reaction temperatures of 40°C and 80°C. X-Ray diffraction studies confirm cubic phase formation. The average crystallite sizes were found to be ∼30nm and ∼48nm for 40°C sample and 80°C sample respectively. Magnetic properties measured using vibrating sample magnetometer show higher coercivety and magnetization for sample prepared at 80°C. Magnetorheological properties of CoFe2O4 ferrofluids were measured and studied.
Mimosa pudica (L.) assisted green synthesis and photoluminescence studies of Y2O3:Mg2+ nanophosphor for display applications

NASA Astrophysics Data System (ADS)

Venkatachalaiah, KN; Venkataravanappa, M.; Nagabhushana, H.; Basavaraj, R. B.

2016-09-01

For the first time green route method was used to synthesize pure and Mg2+(1-11 mol %) doped Y2O3 nanophosphors by using Mimosa pudica leaves extract as a fuel. The final product was well characterized by powder x-ray diffraction (PXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), diffuse reflectance spectroscopy (DRS) and photoluminescence (PL).The PXRD result shows the formation of single phase, cubic structure of Y2O3 with crystallite sizes ∼25 nm. The SEM results showed porous and agglomerated structures, TEM images showed the crystallite size of the material and was found to be around ∼ 25 nm. PL emission spectra show the blue light emission under the excitation wavelength of 315 nm. The emission peaks of Mg2+were observed at 428 nm, 515 nm and 600 nm corresponding to the transitions of 4F9/2 → 6Hi7/2 (violet), 4F9/2 → 6Hi5/2 (blue), 4F9/2 → 6HJ3/2 (yellow) respectively. The estimated CIE chromaticity co-ordinate was very close to the national television standard committee value of blue emission. CCT was found to be ∼ 6891 K as a result the present phosphor was potential to be used for warm white light emitting display applications.
Effects of crystallite size on the structure and magnetism of ferrihydrite

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

Wang, Xiaoming; Zhu, Mengqiang; Koopal, Luuk K.

2015-12-15

The structure and magnetic properties of nano-sized (1.6 to 4.4 nm) ferrihydrite samples are systematically investigated through a combination of X-ray diffraction (XRD), X-ray pair distribution function (PDF), X-ray absorption spectroscopy (XAS) and magnetic analyses. The XRD, PDF and Fe K-edge XAS data of the ferrihydrite samples are all fitted well with the Michel ferrihydrite model, indicating similar local-, medium- and long-range ordered structures. PDF and XAS fitting results indicate that, with increasing crystallite size, the average coordination numbers of Fe–Fe and the unit cell parameter c increase, while Fe2 and Fe3 vacancies and the unit cell parameter a decrease.more » Mössbauer results indicate that the surface layer is relatively disordered, which might have been caused by the random distribution of Fe vacancies. These results support Hiemstra's surface-depletion model in terms of the location of disorder and the variations of Fe2 and Fe3 occupancies with size. Magnetic data indicate that the ferrihydrite samples show antiferromagnetism superimposed with a ferromagnetic-like moment at lower temperatures (100 K and 10 K), but ferrihydrite is paramagnetic at room temperature. In addition, both the magnetization and coercivity decrease with increasing ferrihydrite crystallite size due to strong surface effects in fine-grained ferrihydrites. Smaller ferrihydrite samples show less magnetic hyperfine splitting and a lower unblocking temperature (T B) than larger samples. The dependence of magnetic properties on grain size for nano-sized ferrihydrite provides a practical way to determine the crystallite size of ferrihydrite quantitatively in natural environments or artificial systems.« less
Structural and optical properties of hydrazine hydrate capped cadmium sulphide nanoparticles

NASA Astrophysics Data System (ADS)

Solanki, Rekha Garg; Rajaram, P.

2018-05-01

Semiconductor nanoparticles have received considerable interest due to their size-dependent optical properties. CdS is an important semiconductor material widely used in low cost photovoltaic devices, light-emitting diodes and biological imaging. The nanoparticles of CdS were prepared by a simple chemical precipitation method in aqueous medium. The reaction was carried out at room temperature. The cadmium sulphide nanoparticles were characterized using X-ray powder diffraction (XRD) and UV-visible spectroscopy. The lattice strain, crystallite size and dislocation density were calculated using the Williamson-Hall (W-H) method. The band gap was obtained from the UV-Visible spectra of CdS nanoparticles. The band gap of CdS nanoparticles is around 2.68 eV and the crystallite size is around 5.8 nm.
Effect of Annealing Temperature on Structural and Optical Properties of Sol-Gel-Derived ZnO Thin Films

NASA Astrophysics Data System (ADS)

Arif, Mohd.; Sanger, Amit; Vilarinho, Paula M.; Singh, Arun

2018-04-01

Nanocrystalline ZnO thin films were deposited on glass substrate via sol-gel dip-coating technique then annealed at 300°C, 400°C, and 500°C for 1 h. Their optical, structural, and morphological properties were studied using ultraviolet-visible (UV-Vis) spectrophotometry, x-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM). XRD diffraction revealed that the crystalline nature of the thin films increased with increasing annealing temperature. The c-axis orientation improved, and the grain size increased, as indicated by increased intensity of the (002) plane peak at 2θ = 34.42° corresponding to hexagonal ZnO crystal. The average crystallite size of the thin films ranged from 13 nm to 23 nm. Increasing the annealing temperature resulted in larger crystallite size and higher crystallinity with increased surface roughness. The grain size according to SEM analysis was in good agreement with the x-ray diffraction data. The optical bandgap of the thin films narrowed with increasing annealing temperature, lying in the range of 3.14 eV to 3.02 eV. The transmission of the thin films was as high as 94% within the visible region. The thickness of the thin films was 400 nm, as measured by ellipsometry, after annealing at the different temperatures of 300°C, 400°C, and 500°C.
Synthesis, characterization and magnetic properties of nanocrystalline FexNi80-xCo20 ternary alloys

NASA Astrophysics Data System (ADS)

Dalavi, Shankar B.; Theerthagiri, J.; Raja, M. Manivel; Panda, R. N.

2013-10-01

Fe-Ni-Co alloys of various compositions (FexNi80-xCo20,x=20-50) were synthesized by using a sodium borohydride reduction route. The phase purity and crystallite size was ascertained by using powder X-ray diffraction (XRD). The alloys crystallize in the face centered cubic (fcc) structure with lattice parameters, a=3.546-3.558 Å. The XRD line broadening indicates the fine particle nature of the materials. The estimated crystallite sizes were found to be 27.5, 27, 24, and 22.8 nm for x=20, 30, 40, and 50; alloys respectively. Scanning electron micrograph studies indicates particle sizes to be in the range of 83-60 nm for Fe-Ni-Co alloys. The values of saturation magnetization for FexNi80-xCo20 are found to be in the range of 54.3-41.2 emu/g and are significantly lower than the bulk values (175-180 emu/g). The coercivity decreases from 170 to 122 Oe with decrease in Fe content. The observed magnetic behavior has been explained on the basis of size, surface effects, spin canting and the presence of superparamagnetic fractions in the ultrafine materials.
Catalyst support of mixed cerium zirconium titanium oxide, including use and method of making

DOEpatents

Willigan, Rhonda R [Manchester, CT; Vanderspurt, Thomas Henry [Glastonbury, CT; Tulyani, Sonia [Manchester, CT; Radhakrishnan, Rakesh [Vernon, CT; Opalka, Susanne Marie [Glastonbury, CT; Emerson, Sean C [Broad Brook, CT

2011-01-18

A durable catalyst support/catalyst is capable of extended water gas shift operation under conditions of high temperature, pressure, and sulfur levels. The support is a homogeneous, nanocrystalline, mixed metal oxide of at least three metals, the first being cerium, the second being Zr, and/or Hf, and the third importantly being Ti, the three metals comprising at least 80% of the metal constituents of the mixed metal oxide and the Ti being present in a range of 5% to 45% by metals-only atomic percent of the mixed metal oxide. The mixed metal oxide has an average crystallite size less than 6 nm and forms a skeletal structure with pores whose diameters are in the range of 4-9 nm and normally greater than the average crystallite size. The surface area of the skeletal structure per volume of the material of the structure is greater than about 240 m.sup.2/cm.sup.3. The method of making and use are also described.
Control of crystallite orientation and size in Fe and FeCo nanoneedles.

PubMed

Mendoza-Reséndez, Raquel; Luna, Carlos; Barriga-Castro, Enrique Diaz; Bonville, Pierre; Serna, Carlos J

2012-06-08

Uniform magnetic nanoneedles have been prepared by hydrogen reduction of elongated nanoarchitectures. These precursors are as-prepared or cobalt-coated aggregates of highly oriented haematite nanocrystals (∼5 nm). The final materials are flattened nanoneedles formed by chains of assembled Fe or FeCo single-domain nanocrystals. The microstructural properties of such nanoneedles were tailored using renewed and improved synthetic strategies. In this fashion, the needle elongation and composition, the crystallite size (from 15 up to 30 nm), the nanocrystal orientation (with the 〈110〉 or 〈001〉 directions roughly along the long axis of the nanoneedle) and their type of arrangement (single chains, frustrated double chains and double chains) were controlled by modifying the reduction time, the axial ratio of the precursor haematite and the presence of additional coatings of aluminum or yttrium compounds. The values of the coercivity H(C) found for these nanoneedles are compared with the values predicted by the chain of spheres model assuming a symmetric fanning mechanism for magnetization reversal.
Metalorganic Chemical Vapor Deposition of Ruthenium-Doped Diamond like Carbon Films

NASA Technical Reports Server (NTRS)

Sunkara, M. K.; Ueno, M.; Lian, G.; Dickey, E. C.

2001-01-01

We investigated metalorganic precursor deposition using a Microwave Electron Cyclotron Resonance (ECR) plasma for depositing metal-doped diamondlike carbon films. Specifically, the deposition of ruthenium doped diamondlike carbon films was investigated using the decomposition of a novel ruthenium precursor, Bis(ethylcyclopentadienyl)-ruthenium (Ru(C5H4C2H5)2). The ruthenium precursor was introduced close to the substrate stage. The substrate was independently biased using an applied RF power. Films were characterized using Fourier Transform Infrared Spectroscopy (FTIR), Transmission Electron Microscopy (TEM) and Four Point Probe. The conductivity of the films deposited using ruthenium precursor showed strong dependency on the deposition parameters such as pressure. Ruthenium doped sample showed the presence of diamond crystallites with an average size of approx. 3 nm while un-doped diamondlike carbon sample showed the presence of diamond crystallites with an average size of 11 nm. TEM results showed that ruthenium was atomically dispersed within the amorphous carbon network in the films.
Titanium dioxide nanoparticles: Impact of increasing ionic strength during synthesis, reflux, and hydrothermal aging

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

Isley, Sara L.; Jordan, David S.; Penn, R. Lee

2009-01-08

This work investigates the role of ionic strength during synthesis, reflux, and hydrothermal aging of sol-gel synthesized titanium dioxide. Research presented here uses X-ray diffraction data and Rietveld refinements to quantify anatase, brookite, and rutile phases as functions of synthetic and aging variables. In addition, the Scherrer equation is used to obtain average crystallite sizes for each phase quantified. Results presented in this work demonstrate that the most control over the sol-gel products can be obtained by modifying the pH during hydrolysis. In addition, while varying the ionic strength during reflux and hydrothermal aging can result in enhanced control overmore » the crystalline phase and crystallite size, the most control can be achieved by varying the ionic strength during synthesis. Finally, sol-gel synthesis at low pH (-0.6) and high-chloride concentration (3 M NaCl) produced a heterogeneous sample composed of nanocrystalline anatase (3.8 nm) and rutile (2.9 nm)« less
Manifestation of weak ferromagnetism and photocatalytic activity in bismuth ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Sakar, M.; Balakumar, S.; Saravanan, P.; Jaisankar, S. N.

2013-02-01

Bismuth ferrite (BFO) nanoparticles were synthesized by auto-ignition technique with and without adding ignition fuel such as citric acid. The presence of citric acid in the reaction mixture yielded highly-magnetic BFO/γ-Fe2O3 nanocomposite. When this composite was annealed to 650°C, a single phase BFO was formed with average crystallite size of 50 nm and showed weak ferromagnetic behavior. Conversely, the phase pure BFO prepared without adding citric acid exhibited antiferromagnetism because of its larger crystallite size of around 70 nm. The visible-light driven photocatalytic activity of both the pure BFO and BFO/γ-Fe2O3 nanocomposite were examined by degrading methyl orange dye. The pure BFO showed a moderate photocatalytic activity; while BFO/γ-Fe2O3 nanocomposite showed enhanced activity. This could be probably due to the optimal band gap ratio between BFO and γ-Fe2O3 phases reduced the recombination of electron-hole pairs which aided in the enhancement of photocatalytic activity.
Preparation of ultrafine grained copper nanoparticles via immersion deposit method

NASA Astrophysics Data System (ADS)

Abbasi-Kesbi, Fatemeh; Rashidi, Ali Mohammad; Astinchap, Bandar

2018-03-01

Today, the exploration about synthesis of nanoparticles is much of interest to materials scientists. In this work, copper nanoparticles have been successfully synthesized by immersion deposit method in the absence of any stabilizing and reducing agents. Copper (II) sulfate pentahydrate as precursor salt and distilled water and Ethylene glycol as solvents were used. The copper nanoparticles were deposited on plates of low carbon steel. The effects of copper sulfate concentrations and solvent type were investigated. X-ray diffraction, scanning electron microscopy and UV-Visible spectroscopy were taken to investigate the crystallite size, crystal structure, and morphology and size distribution and the growth process of the nanoparticles of obtained Cu particles. The results indicated that the immersion deposit method is a particularly suitable method for synthesis of semispherical copper nanoparticles with the crystallites size in the range of 22 to 37 nm. By increasing the molar concentration of copper sulfate in distilled water solvent from 0.04 to 0.2 M, the average particles size is increased from 57 to 81 nm. The better size distribution of Cu nanoparticles was achieved using a lower concentration of copper sulfate. By increasing the molar concentration of copper sulfate in water solvent from 0.04 to 0.2, the location of the SPR peak has shifted from 600 to 630 nm. The finer Cu nanoparticles were formed using ethylene glycol instead water as a solvent. Also, the agglomeration and overlapping of nanoparticles in ethylene glycol were less than that of water solvent.
The formation of titanium dioxide crystallite nanoparticles during activation of PAN nanofibers containing titanium isopropoxide

NASA Astrophysics Data System (ADS)

Mehrpouya, Fahimeh; Tavanai, Hossein; Morshed, Mohammad; Ghiaci, Mehran

2012-08-01

Activated carbon (AC) can act as an important carrier for TiO2 nanoparticles. TiO2 nanoparticle can be fabricated by the hydrolysis and condensation of titanium alkoxides like titanium isopropoxide. This study showed that the formation of titanium dioxide crystallite nanoparticle during activation of PAN nanofibers containing titanium isopropoxide leads to the formation of mainly anatase crystal TiO2 nanoparticle in AC nanofibers, with a good dispersion in both the longitude and cross section of nanofibers. The TiO2 crystallite size lies in the range of 7.3-11.3 nm. The dispersion of TiO2 nanoparticles in the matrix of AC nanofibers is far superior to the direct mixing of TiO2 nanoparticles in the original electrospinning solution.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Pratapa, S.; Susanti, L.; Insany, Y. A. S.

Simple coprecipitation method has been used to produce nanoparticles of MgO (magnesia), MgO{center_dot}Al{sub 2}O{sub 3}(spinel), Y{sub 2}O{sub 3}(yttria) and Fe{sub 3}O{sub 4}(ferrite). The raw materials were, in respective, magnesium powder, magnesium and aluminium powders, ytrria powder, and natural sand. The coprecipitation included the use of suitable acid and base to dissolve the powders or sand and to produce precipitates, as well as the use of water to wash and purify the precipitates, and drying at relatively low temperatures, namely lower than 100 deg. C, followed by heating at 450 deg. C, 750 deg. C, 600 deg. C and 200 deg.more » C to produce magnesia, spinel, yttria and ferrite nanopowders, respectively. X-ray diffractometry was used to characterise the purity and nanocrystallinity of the final powders. It was found qualitatively that the powders were of high purity. Further line-broadening analysis using single-line and Rietveld-based softwares was performed to reveal the nanocrystallinity of the powders. Different line breadth values were found for the powders, indicating different crystallite sizes. It was also found that, particularly for spinel and yttria, the diffraction peaks exhibited 'longer' tails, indicating broader crystallite size distribution. The average crystallite size for the powders ranged from 3 to 70 nm. The results could then be used as 'fingerprints' for nanocrystallinity using x-ray diffractometry. The XRD crystallite sizes for yttria and ferrite nanocrystals are in fair agreement with their counterparts from electron microscopy observation.« less
Structure, microstructure, and size dependent catalytic properties of nanostructured ruthenium dioxide

NASA Astrophysics Data System (ADS)

Nowakowski, Pawel; Dallas, Jean-Pierre; Villain, Sylvie; Kopia, Agnieszka; Gavarri, Jean-Raymond

2008-05-01

Nanostructured powders of ruthenium dioxide RuO 2 were synthesized via a sol gel route involving acidic solutions with pH varying between 0.4 and 4.5. The RuO 2 nanopowders were characterized by X-ray diffraction, scanning and transmission electron microscopy (SEM and TEM). Rietveld refinement of mean crystal structure was performed on RuO 2 nanopowders and crystallized standard RuO 2 sample. Crystallite sizes measured from X-ray diffraction profiles and TEM analysis varied in the range of 4-10 nm, with a minimum of crystallite dimension for pH=1.5. A good agreement between crystallite sizes calculated from Williamson Hall approach of X-ray data and from direct TEM observations was obtained. The tetragonal crystal cell parameter (a) and cell volumes of nanostructured samples were characterized by values greater than the values of standard RuO 2 sample. In addition, the [Ru-O 6] oxygen octahedrons of rutile structure also depended on crystal size. Catalytic conversion of methane by these RuO 2 nanostructured catalysts was studied as a function of pH, catalytic interaction time, air methane composition, and catalysis temperature, by the way of Fourier transform infrared (FTIR) spectroscopy coupled to homemade catalytic cell. The catalytic efficiency defined as FTIR absorption band intensities I(CO 2) was maximum for sample prepared at pH=1.5, and mainly correlated to crystallite dimensions. No significant catalytic effect was observed from sintered RuO 2 samples.
Growth, characterization and estimation of lattice strain and size in CdS nanoparticles: X-ray peak profile analysis

NASA Astrophysics Data System (ADS)

Solanki, Rekha Garg; Rajaram, Poolla; Bajpai, P. K.

2018-05-01

This work is based on the growth, characterization and estimation of lattice strain and crystallite size in CdS nanoparticles by X-ray peak profile analysis. The CdS nanoparticles were synthesized by a non-aqueous solvothermal method and were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman and UV-visible spectroscopy. XRD confirms that the CdS nanoparticles have the hexagonal structure. The Williamson-Hall (W-H) method was used to study the X-ray peak profile analysis. The strain-size plot (SSP) was used to study the individual contributions of crystallite size and lattice strain from the X-rays peaks. The physical parameters such as strain, stress and energy density values were calculated using various models namely, isotropic strain model, anisotropic strain model and uniform deformation energy density model. The particle size was estimated from the TEM images to be in the range of 20-40 nm. The Raman spectrum shows the characteristic optical 1LO and 2LO vibrational modes of CdS. UV-visible absorption studies show that the band gap of the CdS nanoparticles is 2.48 eV. The results show that the crystallite size estimated from Scherrer's formula, W-H plots, SSP and the particle size calculated by TEM images are approximately similar.

Synthesis of nanometer-size inorganic materials for the examination of particle size effects on heterogeneous catalysis

NASA Astrophysics Data System (ADS)

Emerson, Sean Christian

The effect of acoustic and hydrodynamic cavitation on the precipitation of inorganic catalytic materials, specifically titania supported gold, was investigated. The overall objective was to understand the fundamental factors involved in synthesizing nanometer-size catalytic materials in the 1--10 nm range in a cavitating field. Materials with grain sizes in this range have been associated with enhanced catalytic activity compared to larger grain size materials. A new chemical approach was used to produce titania supported gold by co-precipitation with higher gold yields compared to other synthesis methods. Using this approach, it was determined that acoustic cavitation was unable to influence the gold mean crystallite size compared to non-sonicated catalysts. However, gold concentration on the catalysts was found to be very important for CO oxidation activity. By decreasing the gold concentration from a weight loading of 0.50% down to approximately 0.05%, the rate of reaction per mole of gold was found to increase by a factor of 19. Hydrodynamic cavitation at low pressures (6.9--48 bar) was determined to have no effect on gold crystallite size at a fixed gold content for the same precipitation technique used in the acoustic cavitation studies. By changing the chemistry of the precipitation system, however, it was found that a synergy existed between the dilution of the gold precursor solution, the orifice diameter, and the reducing agent addition rate. Individually, these factors were found to have little effect and only their interaction allowed gold grain size control in the range of 8--80 nm. Further modification of the system chemistry and the use of hydrodynamic cavitation at pressures in excess of 690 bar allowed the systematic control of gold crystallite size in the range of 2--9 nm for catalysts containing 2.27 +/- 0.17% gold. In addition, it was shown that the enhanced mixing due to cavitation led to larger gold yields compared to classical syntheses. The control of gold grain size was gained at the loss of CO activity, which was attributed to the formation of non-removable sodium titanate species. The increased mixing associated with cavitation contributed to the activity loss by partially burying the gold and incorporating more of the sodium titanate species into the catalysts. This work produced the first evidence of hydrodynamic cavitation influencing the gold crystallite size on titania supported gold catalysts and is the only study reporting the control of grain size by simple mechanical adjustment of the experimental parameters. Despite the low activity observed due to sodium titanate, the methodology of adjusting the chemistry of a precipitating system could be used to eliminate such species. The approach of modifying the chemical precipitation kinetics relative to the dynamics of cavitation offers a general scheme for future research on cavitational processing effects.
Surface morphology of vacuum-evaporated pentacene film on Si substrate studied by in situ grazing-incidence small-angle X-ray scattering: I. The initial stage of formation of pentacene film

NASA Astrophysics Data System (ADS)

Hirosawa, Ichiro; Watanabe, Takeshi; Koganezawa, Tomoyuki; Kikuchi, Mamoru; Yoshimoto, Noriyuki

2018-03-01

The progress of the surface morphology of a growing sub-monolayered pentacene film on a Si substrate was studied by in situ grazing-incidence small angle X-ray scattering (GISAXS). The observed GISAXS profiles did not show sizes of pentacene islands but mainly protuberances on the boundaries around pentacene film. Scattering of X-ray by residual pits in the pentacene film was also detected in the GISAXS profiles of an almost fully covered film. The average radius of pentacene protuberances increased from 13 to 24 nm as the coverage increased to 0.83 monolayer, and the most frequent radius was almost constant at approximately 9 nm. This result suggests that the population of larger protuberances increase with increasing lengths of boundaries of the pentacene film. It can also be considered that the detected protuberances were crystallites of pentacene, since the average size of protuberances was nearly equal to crystallite sizes of pentacene films. The almost constant characteristic distance of 610 nm and amplitudes of pair correlation functions at low coverages suggest that the growth of pentacene films obeyed the diffusion-limited aggregation (DLA) model, as previously reported. It is also considered that the sites of islands show a triangular distribution for small variations of estimated correlation distances.
Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods

NASA Astrophysics Data System (ADS)

Sivakami, R.; Dhanuskodi, S.; Karvembu, R.

2016-01-01

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55 eV. BET measurements show a high specific surface area (SSA) of 118-133 m2/g and pore diameter (10-25 nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM.
White random lasing in mixture of ZnSe, CdS and CdSSe micropowders

NASA Astrophysics Data System (ADS)

Alyamani, A. Y.; Leanenia, M. S.; Alanazi, L. M.; Aljohani, M. M.; Aljariwi, A. A.; Rzheutski, M. V.; Lutsenko, E. V.; Yablonskii, G. P.

2016-03-01

Room temperature random lasing with white light emission in a mixture of AIIBVI semiconductor powders was achieved for the first time. The scattering gain media was formed by the mixture of closely packed active micron sized crystallites of ZnSe, CdS, CdSSe semiconductors. The micropowders were produced by grinding bulk crystals of each compound. Optical excitation was performed by 10-nanosecond pulses of tuned Ti:Al2O3-laser at 390 nm. The lasing in the mixture of semiconductor powders was achieved simultaneously at four wavelengths in blue, green, yellow and red spectral regions after exceeding the threshold excitation power density. A drastic integral intensity increase, spectrum narrowing and appearance of mode structure accompanied the laser action. ZnSe crystallites produce the laser light at about 460 nm while CdS particles - at about 520 nm. Two types of CdSSe semiconductor micropowders with different sulfur content lase at 580 nm and 660 nm. The threshold excitation power densities for all laser lines in the emission spectrum are approximately the same of about 0.9 MW/cm2. The sum of the emission spectrum of the mixture of the micropowders forms white light with high brightness. Lasing is due to an appearance of random feedback for amplified radiation in the active medium of closely packed light scattering crystallites. The presented results may find their applications for visualization systems, lighting technology, data transmission, medicine as biosensors and in identification systems. The key feature of random lasers is low cost of its production and possibility to be deposited on any type of surface.
Dislocation, crystallite size distribution and lattice strain of magnesium oxide nanoparticles

NASA Astrophysics Data System (ADS)

Sutapa, I. W.; Wahid Wahab, Abdul; Taba, P.; Nafie, N. L.

2018-03-01

The oxide of magnesium nanoparticles synthesized using sol-gel method and analysis of the structural properties was conducted. The functional groups of nanoparticles has been analysed by Fourier Transform Infrared Spectroscopy (FT-IR). Dislocations, average size of crystal, strain, stress, the energy density of crystal, crystallite size distribution and morphologies of the crystals were determined based on X-ray diffraction profile analysis. The morphological of the crystal was analysed based on the image resulted from SEM analysis. The crystallite size distribution was calculated with the contention that the particle size has a normal logarithmic form. The most orientations of crystal were determined based on the textural crystal from diffraction data of X-ray diffraction profile analysis. FT-IR results showed the stretching vibration mode of the Mg-O-Mg in the range of 400.11-525 cm-1 as a broad band. The average size crystal of nanoparticles resulted is 9.21 mm with dislocation value of crystal is 0.012 nm-2. The strains, stress, the energy density of crystal are 1.5 x 10-4 37.31 MPa; 0.72 MPa respectively. The highest texture coefficient value of the crystal is 0.98. This result is supported by morphological analysis using SEM which shows most of the regular cubic-shaped crystals. The synthesis method is suitable for simple and cost-effective synthesis model of MgO nanoparticles.
Synthesis of nanocrystalline zirconia by amorphous citrate route: structural and thermal (HTXRD) studies

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

Bhagwat, Mahesh; Ramaswamy, Veda

Nanocrystalline zirconia powder with a fairly narrow particle size distribution has been synthesized by the amorphous citrate route. The sample obtained has a high BET surface area of 89 m{sup 2} g{sup -1}. Rietveld refinement of the powder X-ray diffraction (XRD) profile of the zirconia sample confirms stabilization of zirconia in the tetragonal phase with around 8% monoclinic impurity. The data show the presence of both anionic as well as cationic vacancies in the lattice. Crystallite size determined from XRD is 8 nm and is in close agreement with the particle size determined by TEM. The in situ high temperature-X-raymore » diffraction (HTXRD) study revealed high thermal stability of the mixture till around 1023 K after which the transformation of tetragonal phase into the monoclinic phase has been seen as a function of temperature till 1473 K. This transformation is accompanied by an increase in the crystallite size of the sample from 8 to 55 nm. The thermal expansion coefficients are 9.14 x 10{sup -6} K{sup -1} along 'a'- and 15.8 x 10{sup -6} K{sup -1} along 'c'-axis. The lattice thermal expansion coefficient in the temperature range 298-1623 K is 34.6 x 10{sup -6} K{sup -1}.« less
Rietveld analysis of the effect of annealing atmosphere on phase evolution of nanocrystalline TiO2 powders.

PubMed

Salari, M; Rezaee, M; Chidembo, A T; Konstantinov, K; Liu, H K

2012-06-01

The structural evolution of nanocrystalline TiO2 was studied by X-ray diffraction (XRD) and the Rietveld refinement method (RRM). TiO2 powders were prepared by the sol-gel technique. Post annealing of as-synthesized powders in the temperature range from 500 degrees C to 800 degrees C under air and argon atmospheres led to the formation of TiO2 nanoparticles with mean crystallite size in the range of 37-165 nm, based on the Rietveld refinement results. It was found that the phase structure, composition, and crystallite size of the resulting particles were dependent on not only the annealing temperature, but also the annealing atmosphere. Rietveld refinement of the XRD data showed that annealing the powders under argon atmosphere promoted the polymorphic phase transformation from anatase to rutile. Field emission scanning electron microscopy (FESEM) was employed to investigate the morphology and size of the annealed powders.
Gamma-radiolytic preparation of multi-component oxides

NASA Astrophysics Data System (ADS)

Procházková, Lenka; Bárta, Jan; Čuba, Václav; Ekberg, Christian; Tietze, Sabrina; Jakubec, Ivo

2016-07-01

The preparation of solid precursors to Zn1-xCdxO and (Lu,Y)3Al5O12:Ce induced by 60Co gamma-ray irradiation of aqueous solutions containing soluble metal salts and ammonium formate is presented. Due to the irradiation, crystalline zinc carbonate hydroxide Zn4(CO3)(OH)6·H2O or amorphous carbonates of Lu, Y and Al were formed in the solutions. After calcination at 500 °C, the agglomerated phase-pure Zn1-xCdxO with crystallite size about 50 nm was obtained if the Cd concentration in solutions remained below 16 M% (with respect to Zn) with x being up to 0.035. The solid precursors to garnets contained the intended concentration of all elements, according to X-ray fluorescence analysis. After calcination at 1200 °C in mild vacuum, the respective phase-pure garnets with crystallite size 100 nm or their solid solution were produced when the Ce dopation was kept below 2 M% (with respect to rare-earth metals). The Ce solubility in the garnet lattice was estimated as 1-2 M% at the calcination conditions used.
Simple synthesis of graphene nanocomposites MgO-rGO and Fe2O3-rGO for multifunctional applications

NASA Astrophysics Data System (ADS)

Abdel-Aal, Seham K.; Ionov, Andrey; Mozhchil, R. N.; Naqvi, Alim H.

2018-05-01

Hummer's method was used to prepare graphene oxide (GO) by chemical exfoliation of graphite. Simple precipitation method was used for the preparation of hybrid nanocomposites MgO-rGO and Fe2O3-rGO. A 0.3 Molar of corresponding metal nitrate solution and GO solution are used for the preparation process. XRD, FT-IR, and XPS were used to characterize the prepared nanocomposites. The reduction of GO into reduced rGO in the formed nanocomposites was confirmed. Morphological characterization showed the formation of needle-shaped nanocrystals of MgO successfully grown on graphene nanosheet with average crystallite size 8.4 nm. Hematite nanocomposite Fe2O3-rGO forms rod-shaped crystals with average crystallite size 27.5 nm. The saturation magnetization observed for Fe2O3-rGO is less than reported value for the pure Fe2O3 nanoparticles. Thermal properties of as-prepared hybrid nanocomposites MgO-rGO and Fe2O3-rGO showed thermal stability of the prepared nanocomposite over long range of temperature.
Role of substrate in the surface diffusion and kinetic roughening of nanocrystallised nickel electrodeposits

NASA Astrophysics Data System (ADS)

Nzoghe-Mendome, L.; Aloufy, A.; Ebothé, J.; El Messiry, M.; Hui, D.

2009-02-01

The surface growth and roughening of nano-crystallised Ni electrodeposits prepared at the same conditions have been studied on Cu, Au and ITO substrates. The Ni films obtained are characterised by the same face-centred cubic structure with a texture affected by the substrate chemical nature. Practically, the same small-sized grains of 83 nm mean height depicting a statistical mono-mode feature grow on Cu. A three-modal feature corresponding to the biggest and compact crystallites of 335, 368 and 400 nm mean height is obtained with Au. Two typical modes, respectively, linked to isolated big crystallites of 343 nm mean height and large zones of small grains of 170 nm height, result from the ITO effect. The surface transport properties of Ni ad-atoms on each substrate have been studied from the theoretical approach including the film global roughness measured by AFM. It is shown that the ad-atom diffusion coefficients ( D s) ranged in the interval 10 -10-10 -9 cm 2 s -1 are greatly affected by the non-equilibrium conditions of the film formation. Cu and ITO, respectively, lead to Λ s=11.92 and 14.30 nm, while the higher D s value and diffusion length Λ s=37.32 nm are obtained with Au substrate.
Structure investigations of ferromagnetic Co-Ni-Al alloys obtained by powder metallurgy.

PubMed

Maziarz, W; Dutkiewicz, J; Lityńska-Dobrzyńska, L; Santamarta, R; Cesari, E

2010-03-01

Elemental powders of Co, Ni and Al in the proper amounts to obtain Co(35)Ni(40)Al(25) and Co(40)Ni(35)Al(25) nominal compositions were ball milled in a high-energy mill for 80 h. After 40 h of milling, the formation of a Co (Ni, Al) solid solution with f.c.c. structure was verified by a change of the original lattice parameter and crystallite size. Analytical transmission electron microscopy observations and X-ray diffraction measurements of the final Co (Ni, Al) solid solution showed that the crystallite size scattered from 4 to 8 nm and lattice parameter a = 0.36086 nm. The chemical EDS point analysis of the milled powder particles allowed the calculation of the e/a ratio and revealed a high degree of chemical homogeneity of the powders. Hot pressing in vacuum of the milled powders resulted in obtaining compacts with a density of about 70% of the theoretical one. An additional heat treatment increased the density and induced the martensitic transformation in a parent phase. Selected area diffraction patterns and dark field images obtained from the heat-treated sample revealed small grains around 300 nm in diameter consisting mainly of the ordered gamma phase (gamma'), often appearing as twins, and a small amount of the L1(0) ordered martensite.
Thermal-induced structural and optical investigations of Agsbnd ZnO nanocomposite thin films

NASA Astrophysics Data System (ADS)

Singh, S. K.; Singhal, R.

2018-07-01

In the present paper, we have successfully synthesized Agsbnd ZnO nanocomposite thin films by RF-magnetron sputtering technique at room temperature. Systematic investigations of thermal-induced structural and optical modifications in Agsbnd ZnO thin films have been observed and described. The Agsbnd ZnO thin films were annealed at three different temperatures of 300 °C, 400 °C and 500 °C in vacuum to prevent the oxidation of Ag. The presence and formation of Ag nanoparticles were estimated by transmission electron microscopy. X-ray diffraction analysis revealed the structural information about the crystalline quality of ZnO. The crystallinity as well as the crystallite size of the films have been found to be improved with annealing temperatures. The estimated crystallite size was ∼15.8 nm for as-deposited film and 19.0 nm for the film at a higher temperature. The chemical composition and structural analysis of as-deposited film were carried out by X-ray photoelectron spectroscopy. A very sharp absorption band appeared at ∼540 nm for Ag NPs that is associated with the surface plasmon resonance band of Ag. A noticeable red shift of about ∼12 nm has been recorded for films annealed at 500 °C. Atomic force microscopy has been utilized to examine the surface morphology of the as-deposited and annealed films. The grain size was found to be increase with increasing annealing temperature, while no significant changes were observed in the roughness of Agsbnd ZnO thin films. Raman spectroscopy revealed lattice defects and disordering in the films after the thermal annealing.
Structural and dielectric studies of Ce doped BaSnO3 perovskite nanostructures

NASA Astrophysics Data System (ADS)

Angel, S. Lilly; Deepa, K.; Rajamanickam, N.; Jayakumar, K.; Ramachandran, K.

2018-04-01

Undoped and Cerium (Ce) doped BaSnO3(BSO) nanostructures were synthesized by co-precipitation method. The cubic structure and perovskite phase were confirmed by X-ray diffraction (XRD). The crystallite size of BSO is 41nm and when Ce ion concentration is increased, the crystallite sizesdecreased. The nanocube, nanocuboids and nanorods are observed from SEM analysis. The purity of the undoped and doped samples are confirmed by EDS spectrum. For larger defects, wide band gap was obtained from UV-Vis and PL spectrum. The dielectric constants are increased at low frequencies when Ce impurities are introduced in the BSO matrix at Sn site.
Pulsed supercritical synthesis of anatase TiO₂ nanoparticles in a water-isopropanol mixture studied by in situ powder X-ray diffraction.

PubMed

Rostgaard Eltzholtz, Jakob; Tyrsted, Christoffer; Ørnsbjerg Jensen, Kirsten Marie; Bremholm, Martin; Christensen, Mogens; Becker-Christensen, Jacob; Brummerstedt Iversen, Bo

2013-03-21

A new step in supercritical nanoparticle synthesis, the pulsed supercritical synthesis reactor, is investigated in situ using synchrotron powder X-ray diffraction (PXRD) to understand the formation of nanoparticles in real time. This eliminates the common problem of transferring information gained during in situ studies to subsequent laboratory reactor conditions. As a proof of principle, anatase titania nanoparticles were synthesized in a 50/50 mixture of water and isopropanol near and above the critical point of water (P = 250 bar, T = 300, 350, 400, 450, 500 and 550 °C). The evolution of the reaction product was followed by sequentially recording PXRD patterns with a time resolution of less than two seconds. The crystallite size of titania is found to depend on both temperature and residence time, and increasing either parameter leads to larger crystallites. A simple adjustment of either temperature or residence time provides a direct method for gram scale production of anatase nanoparticles of average crystallite sizes between 7 and 35 nm, thus giving the option of synthesizing tailor-made nanoparticles. Modeling of the in situ growth curves using an Avrami growth model gave an activation energy of 66(19) kJ mol(-1) for the initial crystallization. The in situ PXRD data also provide direct information about the size dependent macrostrain in the nanoparticles and with decreasing crystallite size the unit cell contracts, especially along the c-direction. This agrees well with previous ex situ results obtained for hydrothermal synthesis of titania nanoparticles.
Nano crystalline Bi2(VO5) phases in lithium bismuth borate glasses containing mixed vanadium-nickel oxides

NASA Astrophysics Data System (ADS)

Yadav, Arti; Khasa, S.; Dahiya, M. S.; Agarwal, A.

2016-05-01

Glass composition 7V2O5.23Li2O.20Bi2O3.50B2O3 and x(2NiO.V2O5).(30-x)Li2O.20Bi2O3.50B2O3, x=0, 2, 5, 7 and 10, were produced by conventional melt quenching technique. The quenched amorphous glass samples were annealed at temperatures 400°C and 500°C for 6 hours. The Bi2(VO5) crystallite were grown in all prepared glass matrix. Tn vanadium lithium bismuth borate glass (annealed), the some phrase of V2O5-crystal were observed along with the nano crystalline Bi2(VO5) phase. The sharp peaks in FTTR spectra of all annealed compositions were also compatible with the XRD diffraction peaks of the system under investigation. Average crystalline size (D) of the Bi2(VO5) nano-crystallite was ~30nm for samples annealed at 400°C and ~42nm for samples annealed at 500°C. Lattice parameter and the lattice strain for all the samples was also calculated corresponding to the (113) plane of Bi2(VO5) crystallite.
The effect of milling time and sintering temperature on Mn, Ti substituted barium hexaferrite nanoparticle

NASA Astrophysics Data System (ADS)

Yustanti, Erlina; Manaf, Azwar

2018-04-01

Barium hexaferrite (BaO.6Fe2O3/BaFe12O19) is a permanent magnetic material and microwave absorbing material. The value of microwave absorption can be increased through the engineering of the material structure, while the reduction of crystallite and particle size up to nanometer results device performance improvement to be superior. In this research, the structural engineering through mechanical alloying and crystallite size reduction through high power ultrasonic irradiation will be explained. Mixing and alloying of Sigma Aldrich BaCO3, Fe2O3, MnCO3, TiO2 p.a 99% precursor material used ball mill with powder ratio of vial at 1:10. Mechanical alloying for 60 hours at 160 rpm produced amorphous material. The process of the crystalline embryo nucleation for 4 hours produced multicrystalline material at a sinter temperature of 1100°C. Phase analysis of the mechanical alloying result using x-ray diffractometer was confirmed either the formation of BaO.6Fe2-xMnx/2Tix/2O3 (x=0.5) single phase. Multicrystalline powder of BaO.6Fe2-xMnx/2Tix/2O3 (x=0.5) was obtained through 20 hours hand grinding and re-milling to bulk sample. Crystallite size reduction in the analysis was conducted through particle density variation in ultrasonic reactor and variation of the increase in ultrasonic time. Increase in milling time up to 60 hours produced fragmenting so that particle size reduction from 18.8 µm to 0.9 µm was occurred. The 12-h ultrasonic irradiation at a frequency of 20 kHz amplitude of 60 µm produced a crystallite-size reduction up to 18 nm at a 10 g/L particle density.
Tunable conductivity in mesoporous germanium

NASA Astrophysics Data System (ADS)

Beattie, Meghan N.; Bioud, Youcef A.; Hobson, David G.; Boucherif, Abderraouf; Valdivia, Christopher E.; Drouin, Dominique; Arès, Richard; Hinzer, Karin

2018-05-01

Germanium-based nanostructures have attracted increasing attention due to favourable electrical and optical properties, which are tunable on the nanoscale. High densities of germanium nanocrystals are synthesized via electrochemical etching, making porous germanium an appealing nanostructured material for a variety of applications. In this work, we have demonstrated highly tunable electrical conductivity in mesoporous germanium layers by conducting a systematic study varying crystallite size using thermal annealing, with experimental conductivities ranging from 0.6 to 33 (×10‑3) Ω‑1 cm‑1. The conductivity of as-prepared mesoporous germanium with 70% porosity and crystallite size between 4 and 10 nm is shown to be ∼0.9 × 10‑3 Ω‑1 cm‑1, 5 orders of magnitude smaller than that of bulk p-type germanium. Thermal annealing for 10 min at 400 °C further reduced the conductivity; however, annealing at 450 °C caused a morphological transformation from columnar crystallites to interconnecting granular crystallites and an increase in conductivity by two orders of magnitude relative to as-prepared mesoporous germanium caused by reduced influence of surface states. We developed an electrostatic model relating the carrier concentration and mobility of p-type mesoporous germanium to the nanoscale morphology. Correlation within an order of magnitude was found between modelled and experimental conductivities, limited by variation in sample uniformity and uncertainty in void size and fraction after annealing. Furthermore, theoretical results suggest that mesoporous germanium conductivity could be tuned over four orders of magnitude, leading to optimized hybrid devices.
Solvent free tin oxide nanoparticle for gas sensing application

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

Ranjan, Pranay, E-mail: pranjan@iitp.ac.in; Thakur, Ajay D.; Centre for Energy and Environment, Indian Institute of Technology Patna, Patliputra, Patna 800013 India

2016-05-06

A new modified technique of synthesizing tin oxide nanoparticles with crystallite size of 2 nm to 6 nm has been developed. Surface area of the nanoparticle has been increased as we approached towards the Debye length. Such a techniques for approaching the Debye length is expected to bring remarkable changes in the properties of resistive based gas sensors. The technique used here is less toxic, economical and has high yield. Phase purity, size, shape and composition has been investigated using x-ray diffraction, micro Raman, scanning electron microscopy and energy dispersive x ray spectroscopy. While surface area has been calculated through Brunaur-Emmett-Teller (BET).
Microwave Synthesis, Characterization, and Photoluminescence Properties of Nanocrystalline Zirconia

PubMed Central

Singh, A. K.; Nakate, Umesh T.

2014-01-01

We report synthesis of ZrO2 nanoparticles (NPs) using microwave assisted chemical method at 80°C temperature. Synthesized ZrO2 NPs were calcinated at 400°C under air atmosphere and characterized using FTIR, XRD, SEM, TEM, BET, and EDS for their formation, structure, morphology, size, and elemental composition. XRD results revealed the formation of mixed phase monoclinic and tetragonal ZrO2 phases having crystallite size of the order 8.8 nm from most intense XRD peak as obtained using Scherrer formula. Electron microscope analysis shows that the NPs were less than 10 nm and highly uniform in size having spherical morphology. BET surface area of ZrO2 NPs was found to be 65.85 m2/g with corresponding particle size of 16 nm. The band gap of synthesized NPs was found to be 2.49 eV and PL spectra of ZrO2 synthesized NPs showed strong peak at 414 nm, which corresponds to near band edge emission (UV emission) and a relatively weak peak at 475 and 562 nm. PMID:24578628
Modeling of Amorphous Calcium Carbonate

NASA Astrophysics Data System (ADS)

Sinha, Sourabh; Rez, Peter

2011-10-01

Many species (e.g. sea urchin) form amorphous calcium carbonate (ACC) precursor phases that subsequently transform into crystalline CaCO3. It is certainly possible that ACC might have up to 10 wt% Mg and ˜3 wt% of water. The structure of ACC and mechanisms by which it transforms to crystalline phase are still unknown. Our goal here is to determine an atomic structure model that is consistent with diffraction and IR measurements of ACC. For this purpose a calcite supercell with 24 formula units (120 atoms) was constructed. Various configurations with 6 Mg atoms substituting for Ca (6 wt%) and 3-5 H2O molecules (2.25- 3.75 wt%) inserted in the spaces between Ca atoms, were relaxed using VASP. Most noticeable effects were the tilts of CO3 groups and distortion of Ca sub-lattice, especially in the case of water. The distributions of nearest Ca-Ca distance and CO3 tilts were extracted from those configurations. We also performed the same analysis starting with aragonite. Sampling from above distributions we built models for amorphous calcite/aragonite of size ˜1700 nm^3. We found that the induced distortions were not enough to generate a diffraction pattern typical of an amorphous material. Next we studied diffraction pattern of several nano-crystallites as recent studies suggest that amorphous calcite might be composed of nano- crystallites. We could then generate a diffraction pattern that appeared similar to that from ACC, for a nano-crystallite of size ˜2 nm^3.

Neodymium cobalt oxide as a chemical sensor

NASA Astrophysics Data System (ADS)

Abdel-Latif, I. A.; Rahman, Mohammed M.; Khan, Sher Bahadar

2018-03-01

Chemical sensing and electrical transport properties of neodymium coblate, NdCoO3, was investigated in this work. It was prepared by using co-precipitation method. Pure neodymium chloride and cobalt chloride were mixing in the presence of sodium hydroxide and the obtained co-precipitated powder was calcined at 850 and 1000 °C. The synthesized composites, as-grown (NdCoO3-I), calcined at 850 °C (NdCoO3-II), and calcined at 1000 °C (NdCoO3-III) were studied in details in terms of their morphological and structural properties. The X-ray analysis confirmed that the synthesized products are well crystalline possessing single phase orthorhombic crystal system of space group Pbnm(62). The crystallite size of NdCoO3-I, NdCoO3-II, and NdCoO3-III is 22, 111, and 338 nm, respectively which reflect that crystallite size is increasing with increase in firing temperature. The DC resistivity was measured as a function of temperature in the temperature range from room temperature up to 200 °C. All NdCoO3 are semiconductor in this range of temperature but showed different activation energy which strongly depends on the crystallite size of the products. The activation energy decreased with increase in crystallite size, 0.798, 0.414 and 0.371 eV for NdCoO3-I, NdCoO3-II, and NdCoO3-III, respectively. Thus resistivity increases with increase in crystallite size of NdCoO3. All NdCoO3 products were tested as chemical sensor for acetone by electrochemical approaches and showed excellent sensitivity. Among the NdCoO3 samples, NdCoO3-III showed the highest sensitivity (3.4722 μAcm-2 mM-1) compared to other compositions and gradually decreased to 3.2407 μAcm-2 mM-1 with decreasing the crystallite size of NdCoO3-II. It is also observed that the sensitivity drastically decreased to 0.76253 μAcm-2 mM-1 in the case of NdCoO3-I. It is introduced an efficient route for the detection of environmental unsafe chemicals by electrochemical approach for the safety of healthcare and environmental fields in broad scales.
The development of latent fingerprints by zinc oxide and tin oxide nanoparticles prepared by precipitation technique

NASA Astrophysics Data System (ADS)

Luthra, Deepali; Kumar, Sacheen

2018-05-01

Fingerprints are the very important evidence at the crime scene which must be developed clearly with shortest duration of time to solve the case. Metal oxide nanoparticles could be the mean to develop the latent fingerprints. Zinc oxide and Tin Oxide Nanoparticles were prepared by using chemical precipitation technique which were dried and characterized by X-ray diffraction, UV-Visible spectroscopy and FTIR. The size of zinc oxide crystallite was found to be 14.75 nm with minimum reflectance at 360 nm whereas tin oxide have the size of 90 nm and reflectance at minimum level 321 nm. By using these powdered samples on glass, plastic and glossy cardboard, latent fingerprints were developed. Zinc oxide was found to be better candidate than tin oxide for the fingerprint development on all the three types of substrates.
Effect of milling atmosphere on structural and magnetic properties of Ni-Zn ferrite nanocrystalline

NASA Astrophysics Data System (ADS)

Hajalilou, Abdollah; Hashim, Mansor; Ebrahimi-Kahrizsangi, Reza; Masoudi Mohamad, Taghi

2015-04-01

Powder mixtures of Zn, NiO, and Fe2O3 are mechanically alloyed by high energy ball milling to produce Ni-Zn ferrite with a nominal composition of Ni0.36Zn0.64Fe2O4. The effects of milling atmospheres (argon, air, and oxygen), milling time (from 0 to 30 h) and heat treatment are studied. The products are characterized using x-ray diffractometry, field emission scanning electron microscopy equipped with energy-dispersive x-ray spectroscopy, and transmitted electron microscopy. The results indicate that the desired ferrite is not produced during the milling in the samples milled under either air or oxygen atmospheres. In those samples milled under argon, however, Zn/NiO/Fe2O3 reacts with a solid-state diffusion mode to produce Ni-Zn ferrite nanocrystalline in a size of 8 nm after 30-h-milling. The average crystallite sizes decrease to 9 nm and 10 nm in 30-h-milling samples under air and oxygen atmospheres, respectively. Annealing the 30-h-milling samples at 600 °C for 2 h leads to the formation of a single phase of Ni-Zn ferrite, an increase of crystallite size, and a reduction of internal lattice strain. Finally, the effects of the milling atmosphere and heating temperature on the magnetic properties of the 30-h-milling samples are investigated. Project supported by the University Putra Malaysia Graduate Research Fellowship Section.
A bottom-up building process of nanostructured La0.75Sr0.25Cr0.5Mn0.5O3-δ electrodes for symmetrical-solid oxide fuel cell: Synthesis, characterization and electrocatalytic testing

NASA Astrophysics Data System (ADS)

Chanquía, Corina M.; Montenegro-Hernández, Alejandra; Troiani, Horacio E.; Caneiro, Alberto

2014-01-01

Pure-phase La0.75Sr0.25Cr0.5Mn0.5O3-δ (LSCM) nanocrystallites have been successfully synthesized by the combustion method, employing glycine as fuel and complexing agent, and ammonium nitrate as combustion trigger. A detailed morphological and structural characterization is performed, by using of X-ray diffraction, N2 physisorption and electron microscopy. The LSCM material consists in interconnected nanocrystallites (∼30 nm) forming a sponge-like structure with meso and macropores, being its specific surface area around 10 m2 g-1. Crystalline structural analyses show that the LSCM nanopowder has trigonal/rhombohedral symmetry in the R-3c space group. By employing the spin coating technique and quick-stuck thermal treatments of the ink-electrolyte, electrodes with different crystallite size (95, 160 and 325 nm) are built onto both sides of the La0.8Sr0.2Ga0.8Mg0.2O3-δ-disk electrolyte. To test the influence of the electrode crystallite size on the electrocatalytic behavior of the symmetrical cells, electrochemical impedance spectroscopy measurements at 800 °C were performed. When the electrode crystallite size becomes smaller, the area specific resistance decreases from 3.6 to 1.31 Ω cm2 under 0.2O2-0.8Ar atmosphere, possibly due to the enlarging of the triple-phase boundary, while this value increases from 7.04 to 13.78 Ω cm2 under 0.17H2-0.03H2O-0.8Ar atmosphere, probably due to thermodynamic instability of the LSCM nanocrystallites.
Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity.

PubMed

Wijesinghe, W P S L; Mantilaka, M M M G P G; Premalal, E V A; Herath, H M T U; Mahalingam, S; Edirisinghe, M; Rajapakse, R P V J; Rajapakse, R M G

2014-09-01

Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10°C to 95°C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3h, at 700°C. The as-prepared products, after 2h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.
Moessbauer Characterization of Magnetite/Polyaniline Magnetic Nanocomposite

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

Rodriguez, Anselmo F. R.; Faria, Fernando S. E. D. V.; Lopez, Jorge L.

2010-12-02

Aniline surface coated Fe{sub 3}O{sub 4} nanoparticles have been successfully synthesized by UV irradiation varying the time and the acid media (HCl, HNO{sub 3}, or H{sub 2}SO{sub 4}). The synthesized material represents a promising platform for application in nerve regeneration. XRD patterns are consistent with the crystalline structure of magnetite. Nevertheless, for UV irradiation times longer than 2 h, extra XRD lines reveal the presence of goethite. The mean crystallite size of uncoated particles is estimated to be 25.4 nm, meanwhile that size is reduced to 19.9 nm for the UV irradiated sample in HCl medium for 4 h. Moessbauermore » spectra of uncoated nanoparticles reveal the occurrence of thermal relaxation at room temperature, while the 77 K-Moessbauer spectrum suggests the occurrence of electron localization effects similar to that expected in bulk magnetite. The Mossbauer spectra of UV irradiated sample in HCl medium during 4 h, confirms the presence of the goethite phase. For this sample, the thermal relaxation is more evident, since the room temperature spectrum shows larger spectral area for the nonmagnetic component due to the smaller crystallite size. Meanwhile, the 77 K-Moessbauer spectrum suggests the absence of the electron localization effect above 77 K.« less
Synthesis of fluorapatite–hydroxyapatite nanoparticles and toxicity investigations

PubMed Central

Montazeri, N; Jahandideh, R; Biazar, Esmaeil

2011-01-01

In this study, calcium phosphate nanoparticles with two phases, fluorapatite (FA; Ca10(PO4)6F2) and hydroxyapatite (HA; Ca10(PO4)6(OH)2), were prepared using the solgel method. Ethyl phosphate, hydrated calcium nitrate, and ammonium fluoride were used, respectively, as P, Ca, and F precursors with a Ca:P ratio of 1:72. Powders obtained from the sol-gel process were studied after they were dried at 80°C and heat treated at 550°C. The degree of crystallinity, particle and crystallite size, powder morphology, chemical structure, and phase analysis were investigated by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and Zetasizer experiments. The results of XRD analysis and FTIR showed the presence of hydroxyapatite and fluorapatite phases. The sizes of the crystallites estimated from XRD patterns using the Scherrer equation and the crystallinity of the hydroxyapatite phase were about 20 nm and 70%, respectively. Transmission electron microscope and SEM images and Zetasizer experiments showed an average size of 100 nm. The in vitro behavior of powder was investigated with mouse fibroblast cells. The results of these experiments indicated that the powders were biocompatibile and would not cause toxic reactions. These compounds could be applied for hard-tissue engineering. PMID:21499417
Conductivity dependence of lithium diffusivity and electrochemical performance for electrospun TiO2 fibers

NASA Astrophysics Data System (ADS)

Qing, Rui; Liu, Li; Bohling, Christian; Sigmund, Wolfgang

2015-01-01

TiO2 is one of the most exciting anode candidates for safe application in lithium ion batteries. However, its low intrinsic electronic conductivity limits application. In this paper, a simple sol-gel based route is presented to produce nanosize TiO2 fibers with 119 ± 27 nm diameters via electrospinning. Subsequent calcination in various atmospheres was applied to achieve anatase and anatase-rutile mixed phase crystallites with and without carbon coating. The crystallite size was 5 nm for argon calcined fibers and 13-20 nm for air calcined fibers. Argon calcined TiO2 nanofibers exhibited electronic conductivity orders of magnitude higher than those of air-calcined samples. Lithium diffusivity was increased by one time and specific capacity by 26.9% due to the enhanced conductivity. It also had a different intercalation mechanism of lithium. Hydrogen post heat-treatment was found to benefit electronic conductivity (by 3-4.5 times), lithium diffusivity (1.5-2 times) and consequently the high rate performance of the TiO2 nanofibers (over 80%). The inner mechanism and structure-property relations among these parameters were also discussed.
Basic molten salt process-A new route for synthesis of nanocrystalline Li 4Ti 5O 12-TiO 2 anode material for Li-ion batteries using eutectic mixture of LiNO 3-LiOH-Li 2O 2

NASA Astrophysics Data System (ADS)

Rahman, M. M.; Wang, Jia-Zhao; Hassan, Mohd Faiz; Chou, Shulei; Wexler, David; Liu, Hua-Kun

A nanocrystalline Li 4Ti 5O 12-TiO 2 duplex phase has been synthesized by a simple basic molten salt process (BMSP) using an eutectic mixture of LiNO 3-LiOH-Li 2O 2 at 400-500 °C. The microstructure and morphology of the Li 4Ti 5O 12-TiO 2 product are characterized by means of X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). The sample prepared by heat-treating at 300 °C for 3 h (S-1) reveals dense agglomerates of ultra-fine nanocrystalline Li 4Ti 5O 12; with heat treatment at 400 °C for 3 h (S-2), there is a duplex crystallite size (fine < 10 nm, and coarse > 20 nm) of Li 4Ti 5O 12-TiO 2; at 500 °C for 3 h (S-3), a much coarser and less-dense distribution of lithium titanate (crystallite size ∼15-30 nm) is observed. According to the results of electrochemical testing, the S-2 sample shows initial discharge capacities of 193 mAh g -1 at 0.2 C, 168 mAh g -1 at 0.5 C, 146 mAh g -1 at 1 C, 135 mAh g -1 at 2 C, and 117 mAh g -1 at 5 C. After 100 cycles, the discharge capacity is 138 mAh g -1 at 1 C with a capacity retention of 95%. The S-2 sample yields the best electrochemical performance in terms of charge-discharge capacity and rate capability compared with other samples. Its superior electrochemical performance can be mainly attributed to the duplex crystallite structure, composed of fine (<10 nm) and coarse (>20) nm nanoparticles, where lithium ions can be stored within the grain boundary interfaces between the spinel Li 4Ti 5O 12 and the anatase TiO 2.
Nanocrystals of [Cu3(btc)2] (HKUST-1): a combined time-resolved light scattering and scanning electron microscopy study.

PubMed

Zacher, Denise; Liu, Jianing; Huber, Klaus; Fischer, Roland A

2009-03-07

The formation of [Cu(3)(btc)(2)] (HKUST-1; btc = 1,3,5-benzenetricarboxylate) nanocrystals from a super-saturated mother solution at room temperature was monitored by time-resolved light scattering (TLS); the system is characterized by a rapid growth up to a size limit of 200 nm within a few minutes, and the size and shape of the crystallites were also determined by scanning electron microscopy (SEM).
Production of Ti-C presolar carbide grain analogies and its infrared spectra

NASA Astrophysics Data System (ADS)

Kimura, Y.; Ikegami, A.; Tanigaki, T.; Ishikawa, M.; Sato, T.; Suzuki, H.; Kido, O.; Kaito, C.

The infrared emission of the circumstellar environment of carbon-rich stars and dense molecular cloud cores is believed to be dominated by the emissivity of carbon dust. The origins of absorption peaks will be identified on the basis of laboratory studies. Important factors in the determination of absorption features are size, shape and structure of the grain (Bohren and Huffman, 1983). Therefore, the production of presolar grain analogy is important for the identification of the observation spectra. Recently, we succeeded in the formation of Si-, Ti- and Zr-C grains of the order of 50 nm by advanced gas evaporation method. We have started to obtain characteristic data of carbide grains in laboratory experiments. The spectra from ultraviolet to infrared of samples embedded in KBr pellets are presented. In the present study, we will elucidate the correlation between the size of TiC grain or thickness of the carbon mantle layer and spectra of TiC core-carbon mantle grains. Because TiC is one of the candidates of 21 micron feature. The absorption peaks of TiC core (50 nm)-carbon mantle (2 nm) grains were found to be at 9.5 and 12.5 microns. When the thickness of the mantle layer increased to 15 nm, the peak at 12.5 microns disappeared and the peak at 9.5 microns was significantly weakened. These results are similar to the calculated result for SiC core-carbon mantle grains, i.e., increased thickness of the mantle layer weakens the spectrum intensity (Kozasa et al., 1996). The 20.1 micron absorption feature never appeared, even if the same size grains seen in meteorites were produced. Moreover, the infrared spectra were observed when the size of TiC grains was smaller than presolar grain. Carbon was deposited on the surface of Ti grains. Then, TiC nanocrystallites with the size of 2-3 nm were produced by the diffusion of Ti and/or carbon. The new absorption feature was appeared at 14 microns. The 12.5 micron absorption was hardly seen. If the samples are heated at 700circC for 1h, crystallites size of TiC was increased to about 5 nm. The absorption feature at 14 microns was weaken. It was concluded that the infrared absorption feature was depend on the crystallites size.
Nanophase cobalt, nickel and zinc ferrites: synchrotron XAS study on the crystallite size dependence of metal distribution.

PubMed

Nordhei, Camilla; Ramstad, Astrid Lund; Nicholson, David G

2008-02-21

Nanophase cobalt, nickel and zinc ferrites, in which the crystallites are in the size range 4-25 nm, were synthesised by coprecipitation and subsequent annealing. X-Ray absorption spectroscopy using synchrotron radiation (supported by X-ray powder diffraction) was used to study the effects of particle size on the distributions of the metal atoms over the tetrahedral and octahedral sites of the spinel structure. Deviations from the bulk structure were found which are attributed to the significant influence of the surface on very small particles. Like the bulk material, nickel ferrite is an inverse spinel in the nanoregime, although the population of metals on the octahedral sites increases with decreasing particle size. Cobalt ferrite and zinc ferrite take the inverse and normal forms of the spinel structure respectively, but within the nanoregime both systems show similar trends in being partially inverted. Further, in zinc ferrite, unlike the normal bulk structure, the nanophase system involves mixed coordinations of zinc(ii) and iron(iii) consistent with increasing partial inversion with size.
Estimation of lattice strain in nanocrystalline RuO2 by Williamson-Hall and size-strain plot methods.

PubMed

Sivakami, R; Dhanuskodi, S; Karvembu, R

2016-01-05

RuO2 nanoparticles (RuO2 NPs) have been successfully synthesized by the hydrothermal method. Structure and the particle size have been determined by X-ray diffraction (XRD), scanning electron microscopy (SEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM). UV-Vis spectra reveal that the optical band gap of RuO2 nanoparticles is red shifted from 3.95 to 3.55eV. BET measurements show a high specific surface area (SSA) of 118-133m(2)/g and pore diameter (10-25nm) has been estimated by Barret-Joyner-Halenda (BJH) method. The crystallite size and lattice strain in the samples have been investigated by Williamson-Hall (W-H) analysis assuming uniform deformation, deformation stress and deformation energy density, and the size-strain plot method. All other relevant physical parameters including stress, strain and energy density have been calculated. The average crystallite size and the lattice strain evaluated from XRD measurements are in good agreement with the results of TEM. Copyright © 2015 Elsevier B.V. All rights reserved.
Simple size control of TiO2 nanoparticles and their electrochemical performance: emphasizing the contribution of the surface area to lithium storage at high-rates

NASA Astrophysics Data System (ADS)

Lim, Joohyun; Um, Ji Hyun; Lee, Kyung Jae; Yu, Seung-Ho; Kim, Young-Jae; Sung, Yung-Eun; Lee, Jin-Kyu

2016-03-01

The particle size effects of TiO2 nanoparticles (TNPs), which are composed of small crystallites, on Li ion storage are a very fundamental and important subject. However, size control of TNPs under 200 nm using a sol-gel method has been limited due to the highly reactive precursor, titanium alkoxide. In this study, TNPs with various sizes even under 100 nm are obtained by controlling the reactant concentrations in a mixed solvent of ethanol and acetonitrile. Among them, three different sizes of TNPs are prepared to compare the Li ion storage capacity, and 60 nm TNPs are found to have the best reversible capacity of 182 mA h g-1 after 50 cycles at 1 C and a remarkable rate performance of 120 mA h g-1 at 10 C. Capacity increase upon cycling is observed in the size-controlled TNPs, and the explanation of this phenomenon is proposed to the lattice volume expansion of TiO2 upon intercalation for enabling further penetration of the electrolyte into the particles' interior. Moreover, the capacity at high rates is more closely related to the surface area from Hg porosimetry analysis than from typical N2 adsorption/desorption analysis.The particle size effects of TiO2 nanoparticles (TNPs), which are composed of small crystallites, on Li ion storage are a very fundamental and important subject. However, size control of TNPs under 200 nm using a sol-gel method has been limited due to the highly reactive precursor, titanium alkoxide. In this study, TNPs with various sizes even under 100 nm are obtained by controlling the reactant concentrations in a mixed solvent of ethanol and acetonitrile. Among them, three different sizes of TNPs are prepared to compare the Li ion storage capacity, and 60 nm TNPs are found to have the best reversible capacity of 182 mA h g-1 after 50 cycles at 1 C and a remarkable rate performance of 120 mA h g-1 at 10 C. Capacity increase upon cycling is observed in the size-controlled TNPs, and the explanation of this phenomenon is proposed to the lattice volume expansion of TiO2 upon intercalation for enabling further penetration of the electrolyte into the particles' interior. Moreover, the capacity at high rates is more closely related to the surface area from Hg porosimetry analysis than from typical N2 adsorption/desorption analysis. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr00104a
A single phase, red emissive Mg2SiO4:Sm3+ nanophosphor prepared via rapid propellant combustion route

NASA Astrophysics Data System (ADS)

Naik, Ramachandra; Prashantha, S. C.; Nagabhushana, H.; Sharma, S. C.; Nagaswarupa, H. P.; Anantharaju, K. S.; Nagabhushana, B. M.; Premkumar, H. B.; Girish, K. M.

2015-04-01

Mg2SiO4:Sm3+ (1-11 mol%) nanoparticles were prepared by a rapid low temperature solution combustion route. The powder X-ray diffraction (PXRD) patterns exhibit orthorhombic structure with α-phase. The average crystallite size estimated using Scherer's method, W-H plot and strain-size plots were found to be in the range 25-50 nm and the same was confirmed by Transmission Electron Microscopy (TEM). Scanning electron microscopy (SEM) pictures show porous structure and crystallites were agglomerated. The effect of Sm3+ cations on luminescence of Mg2SiO4 was well studied. Interestingly the samples could be effectively excited with 315 nm and emitted light in the red region, which was suitable for the demands of high efficiency WLEDs. The emission spectra consists of four main peaks which can be assigned to the intra 4-f orbital transitions of Sm3+ ions 4G5/2 → 6H5/2 (576 nm), 4G5/2 → 6H7/2 (611 nm), 4G5/2 → 6H9/2 (656 nm) and 4G5/2 → 6H11/2 (713 nm). The optimal luminescence intensity was obtained for 5 mol% Sm3+ ions. The CIE (Commission International de I'Eclairage) chromaticity co-ordinates were calculated from emission spectra, the values (0.588, 0.386) were close to the NTSC (National Television Standard Committee) standard value of red emission. Coordinated color temperature (CCT) was found to be 1756 K. Therefore optimized Mg2SiO4:Sm3+ (5 mol%) phosphor was quite useful for solid state lighting.
Deconvolution of Composition and Crystallite Size of Silver Hollandite Nanorods: Influence on Electrochemistry

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

Durham, Jessica L.; Huang, Jianping; Zhang, Bingjie

In this paper, silver hollandite (Ag 1.4Mn 8O 16) has been synthesized by an aqueous, low-temperature co-precipitation technique to afford silver hollandite with distinct crystallite sizes (10 and 15 nm, identified as S-Ag 1.4Mn 8O 16 and L-Ag 1.4Mn 8O 16, respectively) and equivalent silver content (x), allowing for the deconvolution of electrochemical effects related to crystallite size and silver content. The as-prepared silver hollandite materials were confirmed to be structurally analogous. Notably, TEM imaging reveals a high degree of bundling of S-Ag 1.4Mn 8O 16 nanorods compared to L-Ag 1.4Mn 8O 16 which facilitates more intimate connection of themore » S-Ag 1.4Mn 8O 16 material with enhanced interparticle contact. The electrochemical behavior and lithium diffusion properties were investigated by galvanostatic cycling, CV, electrochemical impedance, pulsed-discharge experiments, and ex-situ XAS analysis of cycled cathodes. Lithium based electrochemical cells containing S-Ag 1.4Mn 8O 16 delivered a capacity 15X higher than L-Ag 1.4Mn 8O 16 on cycle 1. Ex-situ XAS demonstrated structural change for S-Ag 1.4Mn 8O 16 and formation of Ag 0 on insertion of 3.8 Li + intercalation. However, the samples of L-Ag 1.4Mn 8O 16 were lithiated by a more limited 0.25 molar equivalents, where no significant structural changes were observed. Finally, the findings affirm crystallite size significantly impacts electrochemistry independent of cation occupancy of the α-MnO 2 type structure.« less
Deconvolution of Composition and Crystallite Size of Silver Hollandite Nanorods: Influence on Electrochemistry

DOE PAGES

Durham, Jessica L.; Huang, Jianping; Zhang, Bingjie; ...

2017-12-16

In this paper, silver hollandite (Ag 1.4Mn 8O 16) has been synthesized by an aqueous, low-temperature co-precipitation technique to afford silver hollandite with distinct crystallite sizes (10 and 15 nm, identified as S-Ag 1.4Mn 8O 16 and L-Ag 1.4Mn 8O 16, respectively) and equivalent silver content (x), allowing for the deconvolution of electrochemical effects related to crystallite size and silver content. The as-prepared silver hollandite materials were confirmed to be structurally analogous. Notably, TEM imaging reveals a high degree of bundling of S-Ag 1.4Mn 8O 16 nanorods compared to L-Ag 1.4Mn 8O 16 which facilitates more intimate connection of themore » S-Ag 1.4Mn 8O 16 material with enhanced interparticle contact. The electrochemical behavior and lithium diffusion properties were investigated by galvanostatic cycling, CV, electrochemical impedance, pulsed-discharge experiments, and ex-situ XAS analysis of cycled cathodes. Lithium based electrochemical cells containing S-Ag 1.4Mn 8O 16 delivered a capacity 15X higher than L-Ag 1.4Mn 8O 16 on cycle 1. Ex-situ XAS demonstrated structural change for S-Ag 1.4Mn 8O 16 and formation of Ag 0 on insertion of 3.8 Li + intercalation. However, the samples of L-Ag 1.4Mn 8O 16 were lithiated by a more limited 0.25 molar equivalents, where no significant structural changes were observed. Finally, the findings affirm crystallite size significantly impacts electrochemistry independent of cation occupancy of the α-MnO 2 type structure.« less
Phase Competition Induced Bio-Electrochemical Resistance and Bio-Compatibility Effect in Nanocrystalline Zr x -Cu100-x Thin Films.

PubMed

Badhirappan, Geetha Priyadarshini; Nallasivam, Vignesh; Varadarajan, Madhuri; Leobeemrao, Vasantha Priya; Bose, Sivakumar; Venugopal, Elakkiya; Rajendran, Selvakumar; Angleo, Peter Chrysologue

2018-07-01

Nano-crystalline Zrx-Cu100-x (x = 20-100 at.%) thin films with thickness ranging from 50 to 185 nm were deposited by magnetron co-sputtering with individual Zr and Cu targets. The as-sputtered thin films were characterized by Field Emission Scanning Electron Microscope (FE-SEM), Atomic Force Microscopy (AFM) and Glancing Incidence X-ray Diffraction (GIXRD) for structural and morphological properties. The crystallite size was found to decrease from 57 nm to 37 nm upon increasing the Zr content from 20 to 30 at.% with slight increase in the lattice strain from 0.17 to 0.33%. Further, increase in Zr content to 40 at.% leads to increase in the crystallite size to 57 nm due to stabilization of C10Zr7 phase along with the presence of nanocrystalline Cu-Zr phase. A bimodal distribution of grain size was observed from FE-SEM micrograph was attributed to the highest surface roughness in Zr30Cu70 thin films comprised of Cu10Zr7, Cu9Zr2, Cu-Zr intermetallic phases. In-vitro electrochemical behaviors of nano-crystalline Zrx-Cu100-x thin films in simulated body fluid (SBF) were investigated using potentiodynamic polarization studies. Electrochemical impedance spectroscopy (EIS) data fitting by equivalent electrical circuit fit model suggests that inner bulk layer contributes to high bio-corrosion resistance in Zrx-Cu100-x thin films with increase in Zr content. The results of cyto-compatibility assay suggested that Zr-Cu thin film did not introduce cytotoxicity to osteoblast cells, indicating its suitability as a bio-coating for minimally invasive medical devices.
High capacity Li-ion battery anodes: Impact of crystallite size, surface chemistry and PEG-coating

DOE PAGES

Minnici, Krysten; Kwon, Yo Han; Huie, Matthew M.; ...

2017-12-06

Battery electrodes are complex mesoscale systems comprised of an active material, conductive agent, current collector, and polymeric binder. Previous work showed that introduction of poly [3-(potassium-4-butanoate) thiophene] (PPBT) as a binder component coupled with a polyethylene glycol (PEG) surface coating on magnetite (Fe 3O 4) nanoparticles enhanced electron and ion transport in the high capacity anode system. Here, the impact of Fe 3O 4 crystallite size (10 nm vs. 20 nm) and surface chemistry were explored to evaluate their effects on interfacial interactions within the composite PEG/PPBT based electrodes and resultant battery performance. The Fe 3O 4 synthesis methods inevitablymore » lead to differences in surface chemistry. For instance, the Fe 3O 4 particles synthesized using ammonium hydroxide appeared more dispersed, and afforded improved rate capability performance. Notably, chemical interactions between the active nanoparticles and PPBT binder were only seen with particles synthesized using triethylamine. Capacity retention and cycling performance were unaffected. Thus, this study provides fundamental insights into the significant impact of active material synthesis on the design and fabrication of composite battery electrodes.« less
Multifunctional Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles synthesized by reverse micelle method

PubMed Central

Gavrilović, Tamara V.; Jovanović, Dragana J.; Lojpur, Vesna; Dramićanin, Miroslav D.

2014-01-01

Synthesis of Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles in reverse micelles and their multifunctional luminescence properties are presented. Using cyclohexane, Triton X-100, and n-pentanol as the oil, surfactant, and co-surfactant, respectively, crystalline nanoparticles with ~4 nm diameter are prepared at low temperatures. The particle size assessed using transmission electron microscopy is similar to the crystallite size obtained from X-ray diffraction measurements, suggesting that each particle comprises a single crystallite. Eu3+-doped GdVO4 nanoparticles emit red light through downconversion upon UV excitation. Er3+/Yb3+-doped GdVO4 nanoparticles exhibit several functions; apart from the downconversion of UV radiation into visible green light, they act as upconvertors, transforming near-infrared excitation (980 nm) into visible green light. The ratio of green emissions from 2H11/2 → 2I15/2 and 4S3/2 → 4I15/2 transitions is temperature dependent and can be used for nanoscale temperature sensing with near-infrared excitation. The relative sensor sensitivity is 1.11%K−1, which is among the highest sensitivities recorded for upconversion-luminescence-based thermometers. PMID:24572638

Multifunctional Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles synthesized by reverse micelle method

NASA Astrophysics Data System (ADS)

Gavrilović, Tamara V.; Jovanović, Dragana J.; Lojpur, Vesna; Dramićanin, Miroslav D.

2014-02-01

Synthesis of Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles in reverse micelles and their multifunctional luminescence properties are presented. Using cyclohexane, Triton X-100, and n-pentanol as the oil, surfactant, and co-surfactant, respectively, crystalline nanoparticles with ~4 nm diameter are prepared at low temperatures. The particle size assessed using transmission electron microscopy is similar to the crystallite size obtained from X-ray diffraction measurements, suggesting that each particle comprises a single crystallite. Eu3+-doped GdVO4 nanoparticles emit red light through downconversion upon UV excitation. Er3+/Yb3+-doped GdVO4 nanoparticles exhibit several functions; apart from the downconversion of UV radiation into visible green light, they act as upconvertors, transforming near-infrared excitation (980 nm) into visible green light. The ratio of green emissions from 2H11/2 --> 2I15/2 and 4S3/2 --> 4I15/2 transitions is temperature dependent and can be used for nanoscale temperature sensing with near-infrared excitation. The relative sensor sensitivity is 1.11%K-1, which is among the highest sensitivities recorded for upconversion-luminescence-based thermometers.
High capacity Li-ion battery anodes: Impact of crystallite size, surface chemistry and PEG-coating

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

Minnici, Krysten; Kwon, Yo Han; Huie, Matthew M.

Battery electrodes are complex mesoscale systems comprised of an active material, conductive agent, current collector, and polymeric binder. Previous work showed that introduction of poly [3-(potassium-4-butanoate) thiophene] (PPBT) as a binder component coupled with a polyethylene glycol (PEG) surface coating on magnetite (Fe 3O 4) nanoparticles enhanced electron and ion transport in the high capacity anode system. Here, the impact of Fe 3O 4 crystallite size (10 nm vs. 20 nm) and surface chemistry were explored to evaluate their effects on interfacial interactions within the composite PEG/PPBT based electrodes and resultant battery performance. The Fe 3O 4 synthesis methods inevitablymore » lead to differences in surface chemistry. For instance, the Fe 3O 4 particles synthesized using ammonium hydroxide appeared more dispersed, and afforded improved rate capability performance. Notably, chemical interactions between the active nanoparticles and PPBT binder were only seen with particles synthesized using triethylamine. Capacity retention and cycling performance were unaffected. Thus, this study provides fundamental insights into the significant impact of active material synthesis on the design and fabrication of composite battery electrodes.« less
Multifunctional Eu3+- and Er3+/Yb3+-doped GdVO4 nanoparticles synthesized by reverse micelle method.

PubMed

Gavrilović, Tamara V; Jovanović, Dragana J; Lojpur, Vesna; Dramićanin, Miroslav D

2014-02-27

Synthesis of Eu(3+)- and Er(3+)/Yb(3+)-doped GdVO4 nanoparticles in reverse micelles and their multifunctional luminescence properties are presented. Using cyclohexane, Triton X-100, and n-pentanol as the oil, surfactant, and co-surfactant, respectively, crystalline nanoparticles with ~4 nm diameter are prepared at low temperatures. The particle size assessed using transmission electron microscopy is similar to the crystallite size obtained from X-ray diffraction measurements, suggesting that each particle comprises a single crystallite. Eu(3+)-doped GdVO4 nanoparticles emit red light through downconversion upon UV excitation. Er(3+)/Yb(3+)-doped GdVO4 nanoparticles exhibit several functions; apart from the downconversion of UV radiation into visible green light, they act as upconvertors, transforming near-infrared excitation (980 nm) into visible green light. The ratio of green emissions from (2)H11/2 → (2)I15/2 and (4)S3/2 → (4)I15/2 transitions is temperature dependent and can be used for nanoscale temperature sensing with near-infrared excitation. The relative sensor sensitivity is 1.11%K(-1), which is among the highest sensitivities recorded for upconversion-luminescence-based thermometers.
Improved magnetic and electrical properties of Cu doped Fe-Ni invar alloys synthesized by chemical reduction technique

NASA Astrophysics Data System (ADS)

Ahmad, Sajjad; Ziya, Amer Bashir; Ashiq, Muhammad Naeem; Ibrahim, Ather; Atiq, Shabbar; Ahmad, Naseeb; Shakeel, Muhammad; Khan, Muhammad Azhar

2016-12-01

Fe-Ni-Cu invar alloys of various compositions (Fe65Ni35-xCux, x=0, 0.2, 0.6, 1, 1.4 and 1.8) were synthesized via chemical reduction route. These alloys were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and vibrating sample magnetometry (VSM) techniques. The XRD analysis revealed the formation of face centered cubic (fcc) structure. The lattice parameter and the crystallite size of the investigated alloys were calculated and the line broadening indicated the nano-crystallites size of alloy powder. The particle size was estimated from SEM and it decreases by the incorporation of Cu and found to be in the range of 24-40 nm. The addition of Cu in these alloys appreciably enhances the saturation magnetization and it increases from 99 to 123 emu/g. Electrical conductivity has been improved with Cu addition. The thermal conductivity was calculated using the Wiedemann-Franz law.
Damage creation in porous silicon irradiated by swift heavy ions

NASA Astrophysics Data System (ADS)

Canut, B.; Massoud, M.; Newby, P.; Lysenko, V.; Frechette, L.; Bluet, J. M.; Monnet, I.

2014-05-01

Mesoporous silicon (PS) samples were processed by anodising p+ Si wafers in (1:1) HF-ethanol solution. Different current densities were used to obtain three different porosities (41%, 56% and 75%). In all cases the morphology of the PS layer is columnar with a mean crystallite size between 12 nm (75% porosity) and 19 nm (41% porosity). These targets were irradiated at the GANIL accelerator, using different projectiles (130Xe ions of 91 MeV and 29 MeV, 238U ions of 110 MeV and 850 MeV) in order to vary the incident electronic stopping power Se. The fluences ranged between 1011 and 7 × 1013 cm-2. Raman spectroscopy and cross sectional SEM observations evidenced damage creation in the irradiated nanocrystallites, without any degradation of the PS layer morphology at fluences below 3 × 1012 cm-2. For higher doses, the columnar morphology transforms into a spongy-like structure. The damage cross sections, extracted from Raman results, increase with the electronic stopping power and with the sample porosity. At the highest Se (>10 keV nm-1) and the highest porosity (75%), the track diameter coincides with the crystallite diameter, indicating that a single projectile impact induces the crystallite amorphization along the major part of the ion path. These results were interpreted in the framework of the thermal spike model, taking into account the low thermal conductivity of the PS samples in comparison with that of bulk silicon.
Synthesis and characterization of nanocrystalline Co-Fe-Nb-Ta-B alloy

NASA Astrophysics Data System (ADS)

Raanaei, Hossein; Fakhraee, Morteza

2017-09-01

In this research work, structural and magnetic evolution of Co57Fe13Nb8Ta4B18 alloy, during mechanical alloying process, have been investigated by using, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, electron dispersive X-ray spectroscopy, differential thermal analysis and also vibrating sample magnetometer. It is observed that at 120 milling time, the crystallite size reaches to about 7.8 nm. Structural analyses show that, the solid solution of the initial powder mixture occurs at160 h milling time. The coercivity behavior demonstrates a rise, up to 70 h followed by decreasing tendency up to final stage of milling process. Thermal analysis of 160 h milling time sample reveals two endothermic peaks. The characterization of annealed milled sample for 160 h milling time at 427 °C shows crystallite size growth accompanied by increasing in saturation magnetization.
Environment friendly route of iron oxide nanoparticles from Zingiber officinale (ginger) root extract

NASA Astrophysics Data System (ADS)

Xin Hui, Yau; Yi Peng, Teoh; Wei Wen, Liu; Zhong Xian, Ooi; Peck Loo, Kiew

2016-11-01

Iron oxide nanoparticles were prepared from the reaction between the Zingiber officinale (ginger) root extracts and ferric chloride solution at 50°C for 2 h in mild stirring condition. The synthesized powder forms of nanoparticles were further characterized by using UV-Vis spectroscopy and X-ray Diffraction spectrometry. UV-Vis analysis shows the absorption peak of iron oxide nanoparticles is appeared at 370 nm. The calculation of crystallite size from the XRD showed that the average particle size of iron oxide nanoparticles was 68.43 nm. Therefore, this eco-friendly technique is low cost and large scale nanoparticles synthesis to fulfill the demand of various applications.
A bioactive coating with submicron-sized titania crystallites fabricated by induction heating of titanium after tensile deformations.

PubMed

Li, Ning-Bo; Xu, Wen-Hua; Xiao, Gui-Yong; Zhao, Jun-Han; Lu, Yu-Peng

2017-11-01

Thermal oxidation technology was widely investigated as one of effective surface modification method for improving the bioactivity and biocompatibility of titanium and its alloys. In this work, the induction heat oxidization method, a fast, efficient, economical and environmental protective technology, was applied to prepare the submicron-morphological oxide coating with variable rutile TiO 2 equiaxed crystallites on the surface of pure Ti substrates after cold-drawing with 10-20% deformations. The results showed the plastic-deformed Ti cylinders recrystallized during induction heating treatment (IHT) for 10-20s which resulted in evolution of microstructures as well as slight improvement of microhardness. The surface characteristics of TiO 2 crystallites in oxidation layers were determined by the microstructural evolutions of Ti substrate in terms of the nucleation and growth of TiO 2 crystallites. Specially, the oxidized surface with 50-75nm roughness and more uniform and finer equiaxed oxide grains remarkablely improved the apatite deposition after bioactive evaluation in 1.5 × SBF for 7 days. This work provided a potential method to create controlled bioactive oxide coatings with submicro-/nano-scaled TiO 2 crystallites on titanium substrate in terms of the role of metallographic microstructure in the formation process of titanium oxides. Copyright © 2017 Elsevier Ltd. All rights reserved.
Synthesis, self-assembly, and properties of Mn doped ZnO nanoparticles.

PubMed

Barick, K C; Bahadur, D

2007-06-01

We report here a novel process to prepare Mn doped ZnO nanoparticles by a soft chemical route at low temperature. The synthesis process is based on the hydrolysis of zinc acetate dihydrate and manganese acetate tetrahydrate heated under reflux to 160-175 degrees C using diethylene glycol as a solvent. X-ray diffraction analysis reveals that the Mn doped ZnO crystallizes in a wurtzite structure with crystal size of 15-25 nm. These nano size crystallites of Mn doped ZnO self-organize into polydisperse spheres in size ranging from 100-400 nm. Transmission Electron Microscopy image also shows that each sphere is made up of numerous nanocrystals of average diameter 15-25 nm. By means of X-ray photoelectron spectroscopy and electron spin resonance spectroscopy, we determined the valence state of Mn ions as 2+. These nanoparticles were found to be ferromagnetic at room temperature. Monodisperse porous spheres (approximately 250 nm) were obtained by size selective separation technique and then self-assembled in a closed pack periodic array through sedimentation with slow solvent evaporation, which gives strong opalescence in visible region.
Synthesis and characterization of nanocrystalline LaMnO3 modified BaTiO3 ferroelectric ceramics prepared by chemical route

NASA Astrophysics Data System (ADS)

Dhak, Prasanta; Adak, Mrinal Kanti; Dhak, Debasis

2016-02-01

Nanocrystalline Ba1-3xTi1-3xLa2xMn4xO3, [x = 0.006, 0.008, 0.01 and 0.05] (abbreviated hereafter as BTLM) by chemical route. The phase formation and purity were checked by X-ray diffraction (XRD) study and transmission electron microscopy (TEM). The grain morphology after sintering was studied by scanning electron microscopy (SEM). The crystallite sizes range from 21 nm to 30 nm, while the particle size ranges between 27 nm and 38 nm. The grain size 212 nm and grain density 96.8% were found to be maximum for BTLM x = 0.05 and x = 0.01, respectively. The temperature dependence of dielectric constants was found to be more diffused and the peak value of the dielectric constant was decreased and more flat with the increase of the substituent concentration. The tangent loss was found to be decreased and reached to the minimum value of 0.032 for BTLM x = 0.05. The remnant polarization Pr, was 10 μC/cm2 for BTLM x = 0.01.
Reproducible Crystallite Size of Mono-Dispersed and Scalable Biologically Produced Metal-Substituted Nanometer-Sized Magnetites

NASA Astrophysics Data System (ADS)

Moon, J.; Rawn, C.; Rondinone, A.; Love, L.; Roh, Y.; Lauf, R.; Phelps, T.

2008-12-01

Our previous research demonstrated that biosynthesized magnetite (biomagnetite) exhibited similar properties as chemically synthesized magnetite. To complement uses of the traditional chemically synthesized magnetite (chem-magnetite) biomagnetite must be exhibit highly reproducible sizes and be available in scalable qualities. Here we emphasize potentially advantageous properties of biomagnetite regarding size, reproducibility and scaling availability. Average crystallite size (ACS) of biomagnetites ranging from 10-100 nm was determined after varied 1) incubation times, 2) substitution of metal and lanthanide species, 3) degrees of congruent incorporation or retardation of substitution elements, 4) bacterial species with their varied ability to substitute elemental species, and 6) incubation temperature that can influence coalescence. The microbial production of biomagnetite has demonstrated capacity to make highly crystalline nanoscale particles of metal-substituted ferrites including compounds of Co, Ni, Cr, Mn, Zn and the rare earths in large quantity. Selected Zn-substituted magnetite (nominal composition of Zn0.6Fe2.4O4) has been recovered at over 1 kg (wet weight) in batches from 30 L fermentations. The massively produced extracellular magnetites were confirmed to exhibit good mono- dispersity via transmission electron microscopy (TEM). TEM also validated highly reproducible ACS of 13.1±0.8 nm size as determined through X-ray diffraction (N=7) at a 99 % confidence level. Based on the scale-up experiments performed using the 35 L reactor, the reduction in ACS variability and shorted incubation times of several days may be attributed to increases of electron donor input, and availability of divalent ions of the substitution metal with less ferrous ions in the case of doped magnetite, or a combination of the above. While costs of commercial nanometer sized magnetite (25-50 nm) may vary from 500/kg to > 1,000/kg, microbial mass production is likely capable of producing 13-90 nm magnetite or doped magnetites at a fraction of the cost of traditional chemical synthesis. While there are numerous approaches for the synthesis of nanoparticles, bacterial fermentation of magnetite or metal-substituted magnetite may represent a disruptive manufacturing technology with respect to yield, reproducibility and scalability.
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 %.
Gold nano-particle formation from crystalline AuCN: Comparison of thermal, plasma- and ion-beam activated decomposition

NASA Astrophysics Data System (ADS)

Beck, Mihály T.; Bertóti, Imre; Mohai, Miklós; Németh, Péter; Jakab, Emma; Szabó, László; Szépvölgyi, János

2017-02-01

In this work, in addition to the conventional thermal process, two non-conventional ways, the plasma and ion beam activations are described for preparing gold nanoparticles from microcrystalline AuCN precursor. The phase formation at plasma and ion beam treatments was compared with that at thermal treatments and the products and transformations were characterized by thermogravimetry-mass-spectrometry (TG-MS), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). TG-MS measurements in Ar atmosphere revealed that AuCN decomposition starts at 400 °C and completes at ≈700 °C with evolution of gaseous (CN)2. XPS and TEM show that in heat treatment at 450 °C for 1 h in Ar, loss of nitrogen and carbon occurs and small, 5-30 nm gold particles forms. Heating at 450 °C for 10 h in sealed ampoule, much larger, 60-200 nm size and well faceted Au particles develop together with a fibrous (CN)n polymer phase, and the Au crystallites are covered by a 3-5 nm thick polymer shell. Low pressure Ar plasma treatment at 300 eV energy results in 4-20 nm size Au particles and removes most of the nitrogen and part of carbon. During Ar+ ion bombardment with 2500 eV energy, 5-30 nm size Au crystallites form already in 10 min, with preferential loss of nitrogen and with increased amount of carbon residue. The results suggest that plasma and ion beam activation, acting similarly to thermal treatment, may be used to prepare Au nanoparticles from AuCN on selected surface areas either by depositing AuCN precursors on selected regions or by focusing the applied ionized radiation. Thus they may offer alternative ways for preparing tailor-made catalysts, electronic devices and sensors for different applications.
Tailoring the synthesis of supported Pd catalysts towards desired structure and size of metal particles.

PubMed

Suresh, Gatla; Radnik, Jörg; Kalevaru, Venkata Narayana; Pohl, Marga-Martina; Schneider, Matthias; Lücke, Bernhard; Martin, Andreas; Madaan, Neetika; Brückner, Angelika

2010-05-14

In a systematic study, the influence of different preparation parameters on phase composition and size of metal crystallites and particles in Pd-Cu/TiO(2) and Pd-Sb/TiO(2) catalyst materials has been explored. Temperature and atmosphere of thermal pretreatment (pure He or 10% H(2)/He), nature of metal precursors (chlorides, nitrates or acetates) as well as of ammonium additives (ammonium sulfate, nitrate, carbonate) and urea were varied with the aim of tailoring the synthesis procedure for the preferential formation of metal particles with similar size and structure as observed recently in active catalysts after long-term equilibration under catalytic reaction conditions in acetoxylation of toluene to benzylacetate. Among the metal precursors and additives, the chloride metal precursors and (NH(4))(2)SO(4) were most suitable. Upon thermal pretreatment of Pd-Sb or Pd-Cu precursors, chloroamine complexes of Pd and Cu are formed, which decompose above 220 degrees C to metallic phases independent of the atmosphere. In He, metallic Pd particles were formed with both the co-components. In H(2)/He flow, Pd-Cu precursors were converted to core-shell particles with a Cu shell and a Pd core, while Sb(1)Pd(1) and Sb(7)Pd(20) alloy phases were formed in the presence of Sb. Metal crystallites of about 40 nm agglomerate to particles of up to 150 nm in He and to even larger size in H(2)/He.
Surface spins disorder in uncoated and SiO2 coated maghemite nanoparticles

NASA Astrophysics Data System (ADS)

Zeb, F.; Nadeem, K.; Shah, S. Kamran Ali; Kamran, M.; Gul, I. Hussain; Ali, L.

2017-05-01

We studied the surface spins disorder in uncoated and silica (SiO2) coated maghemite (γ-Fe2O3) nanoparticles using temperature and time dependent magnetization. The average crystallite size for SiO2 coated and uncoated nanoparticles was about 12 and 29 nm, respectively. Scanning electron microscopy (SEM) showed that the nanoparticles are spherical in shape and well separated. Temperature scans of zero field cooled (ZFC)/field cooled (FC) magnetization measurements showed lower average blocking temperature (TB) for SiO2 coated maghemite nanoparticles as compared to uncoated nanoparticles. The saturation magnetization (Ms) of SiO2 coated maghemite nanoparticles was also lower than the uncoated nanoparticles and is attributed to smaller average crystallite size of SiO2 coated nanoparticles. For saturation magnetization vs. temperature data, Bloch's law (M(T)= M(0).(1- BTb)) was fitted well for both uncoated and SiO2 coated nanoparticles and yields: B =3×10-7 K-b, b=2.22 and B=0.0127 K-b, b=0.57 for uncoated and SiO2 coated nanoparticles, respectively. Higher value of B for SiO2 coated nanoparticles depicts decrease in exchange coupling due to enhanced surface spins disorder (broken surface bonds) as compared to uncoated nanoparticles. The Bloch's exponent b was decreased for SiO2 coated nanoparticles which is due to their smaller average crystallite size or finite size effects. Furthermore, a sharp increase of coercivity at low temperatures (<25 K) was observed for SiO2 coated nanoparticles which is also due to contribution of increased surface anisotropy or frozen surface spins in these smaller nanoparticles. The FC magnetic relaxation data was fitted to stretched exponential law which revealed slower magnetic relaxation for SiO2 coated nanoparticles. All these measurements revealed smaller average crystallite size and enhanced surface spins disorder in SiO2 coated nanoparticles than in uncoated γ-Fe2O3 nanoparticles.
Matrix Structure Evolution and Nanoreinforcement Distribution in Mechanically Milled and Spark Plasma Sintered Al-SiC Nanocomposites.

PubMed

Saheb, Nouari; Aliyu, Ismaila Kayode; Hassan, Syed Fida; Al-Aqeeli, Nasser

2014-09-19

Development of homogenous metal matrix nanocomposites with uniform distribution of nanoreinforcement, preserved matrix nanostructure features, and improved properties, was possible by means of innovative processing techniques. In this work, Al-SiC nanocomposites were synthesized by mechanical milling and consolidated through spark plasma sintering. Field Emission Scanning Electron Microscope (FE-SEM) with Energy Dispersive X-ray Spectroscopy (EDS) facility was used for the characterization of the extent of SiC particles' distribution in the mechanically milled powders and spark plasma sintered samples. The change of the matrix crystallite size and lattice strain during milling and sintering was followed through X-ray diffraction (XRD). The density and hardness of the developed materials were evaluated as function of SiC content at fixed sintering conditions using a densimeter and a digital microhardness tester, respectively. It was found that milling for 24 h led to uniform distribution of SiC nanoreinforcement, reduced particle size and crystallite size of the aluminum matrix, and increased lattice strain. The presence and amount of SiC reinforcement enhanced the milling effect. The uniform distribution of SiC achieved by mechanical milling was maintained in sintered samples. Sintering led to the increase in the crystallite size of the aluminum matrix; however, it remained less than 100 nm in the composite containing 10 wt.% SiC. Density and hardness of sintered nanocomposites were reported and compared with those published in the literature.
Structural and optical characterizations of Ca2Al2SiO7:Ce3+, Mn2+ nanoparticles produced via a hybrid route

NASA Astrophysics Data System (ADS)

Teixeira, V. C.; Montes, P. J. R.; Valerio, M. E. G.

2014-07-01

Pure, Ce3+ doped and Ce3+ and Mn2+ co-doped Ca2Al2SiO7 ceramic powders were prepared by two different methodologies which are the proteic sol-gel process and a new hybrid route combining the proteic sol-gel with solid state reaction processes. The second one is an eco-friendly method because it uses natural raw materials in replacement of the metal alkoxides used in the traditional sol-gel routes. X-ray diffraction showed that Ca2Al2SiO7 crystalline phase was obtained for both preparations. Differential thermal analysis indicated that the exothermic event around 850 °C, for sample produced by proteic sol-gel method, and around 927 °C, for ceramics prepared by hybrid synthesis, can be associated to crystallization of Ca2Al2SiO7. Transmission electron microscope indicates that regular and spherical nanoparticles were obtained with average sizes of about 12 nm. The Scherrer's method was used to determine the average crystallite sizes and it was shown that nanometric crystallites were obtained of about 74 nm for samples produced via hybrid route. For all the single phase samples, the crystallite sizes are about the same and that agrees with TEM results. Diffuse optical reflectance measurements were used to estimate the Ca2Al2SiO7 optical band gap and the obtained value is about 6 eV, photoluminescence (PL) spectra presented typical emissions of Ce3+ and Mn2+ ions. Upon excitation at 352 nm the emission spectra showed a broad band centered at 415 nm due to the Ce3+ 4f1 → 5d1 typical transition. This emission is resonant with Mn2+ excitation and it transfers energy to Mn ions generating a second broad emission band centered at 620 nm due to the Mn2+. The PL results were used to obtain, as a fist approach, the Ce3+ energy levels diagram and, using the Tanabe-Sugano diagrams, the transitions due to the Mn2+ were calculated. X-ray excited optical luminescence measurements showed the same emission spectra as the PL emission spectra. Luminescence lifetime decay constants were measured for Ce and Mn co-doped and for Ce doped samples and the results indicate Ca2Al2SiO7:Ce3+, Mn2+ showed quite fast responses with main time constants below 30 ns.
STRUCTURAL, SURFACE MORPHOLOGICAL AND MAGNETIC STUDIES OF Zn1-xFexS (x=0.00-0.10) DILUTED MAGNETIC SEMICONDUCTORS GROWN BY CO-PRECIPITATION METHOD

NASA Astrophysics Data System (ADS)

Hassan, M.; Ghazanfar, M.; Arooj, N.; Riaz, S.; Hussain, S. Sajjad; Naseem, S.

We have fabricated Zn1-xFexS (x=0.00, 0.02, 0.04, 0.06, 0.08 and 0.10) diluted magnetic semiconductors using co-precipitation method. X-ray diffraction patterns depict that Zn1-xFexS appears as a dominant phase with cubic zinc blende structure and nanoscale crystallite size. In addition, a secondary phase of rhombohedral ZnS also appears; however, no additional phase arises that primarily belongs to Fe dopant. Using Debye-Scherrer relation, the crystallite size is found to be in the range of 20-27nm, which is in good agreement with the crystallite size calculated using the Williamson-Hall (WH) plot method. The appearance of secondary phase provoked to study the residual strain using Stokes-Wilson equation, which is nearly consistent to that observed using WH plot method. The surface morphology, revealed using scanning electron microscopy, depicts non-uniform surface structure with a variety of grains and void dimensions. Hysteresis loops measured for Zn1-xFexS at room temperature (RT) illustrate a paramagnetic behavior at higher fields; however, small ferromagnetic behavior is evident due to the small openings of the measured hysteresis loops around the origin. The measured RT ferromagnetism reveals the potential spintronic device applications of the studied diluted magnetic semiconductors.
Crystallite size strain analysis of nanocrystalline La0.7Sr0.3MnO3 perovskite by Williamson-Hall plot method

NASA Astrophysics Data System (ADS)

Kumar, Dinesh; Verma, Narendra Kumar; Singh, Chandra Bhal; Singh, Akhilesh Kumar

2018-04-01

The nanocrystalline Sr-doped LaMnO3 (La0.7Sr0.3MnO3 = LSMO) perovskite manganites having different crystallite size were synthesized using the nitrate-glycine auto-combustion method. The phase purity of the manganites was checked by X-ray diffraction (XRD) measurement. The XRD patterns of the sample reveal that La0.7S0.3MnO3 crystallizes into rhombohedral crystal structure with space group R-3c. The size-dependence of structural lattice parameters have been investigated with the help of Rietveld refinement. The structural parameters increase as a function of crystallite size. The crystallite-size and internal strain as a function of crystallite-size have been calculated using Williamson-Hall plot.
Pre and post annealed low cost ZnO nanorods on seeded substrate

NASA Astrophysics Data System (ADS)

Nordin, M. N.; Kamil, Wan Maryam Wan Ahmad

2017-05-01

We wish to report the photonic band gap (where light is confined) in low cost ZnO nanorods created by two-step chemical bath deposition (CBD) method where the glass substrates were pre-treated with two different seeding thicknesses, 100 nm (sample a) and 150 nm (sample b), of ZnO using radio frequency magnetron sputtering. Then the samples were annealed at 600°C for 1 hour in air before and after immersed into the chemical solution for CBD process. To observe the presence of photonic band gap on the sample, UV-Visible-NIR spectrophotometer was utilized and showed that sample a and sample b both achieved wide band gap between 240 nm and 380 nm, within the UV range for typical ZnO, however sample b provided a better light confinement that may be attributed by the difference in average nanorods size. Field Emission Scanning Electron Microscope (FESEM) of the samples revealed better oriented nanorods uniformly scattered across the surface when substrates were coated with 100 nm of seeding layer whilst the 150 nm seeding sample showed a poor distribution of nanorods probably due to defects in the sample. Finally, the crystal structure of the ZnO crystallite is revealed by employing X-ray diffraction and both samples showed polycrystalline with hexagonal wurtzite structure that matched with JCPDS No. 36-1451. The 100 nm pre-seeded samples was recognized to have bigger average crystallite size, however sample b was suggested as having a higher crystalline quality. In conclusion, the sample b is recognized as a better candidate for future photonic applications due to its more apparent of photonic band gap and this may be contributed by more random distribution of the nanorods as observed in FESEM images as well as higher crystalline quality as suggested from XRD measurements.

Fabrication of nano ZrO2 dispersed novel W79Ni10Ti5Nb5 alloy by mechanical alloying and pressureless sintering

NASA Astrophysics Data System (ADS)

Sahoo, R. R.; Patra, A.; Karak, S. K.

2017-02-01

A high energy planetary ball-mill was employed to synthesize tungsten (W) based alloy with nominal composition of W79Ni10Ti5Nb5(ZrO2)1 (in wt. %) for 20 h with chrome steel as grinding media, toluene as process control agent (PCA) along with compaction at 500 MPa pressure for 5 mins and sintering at 1500°C for 2 h using Ar atmosphere. X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS), elemental mapping and Transmission electron microscopy (TEM) was used to study the phase formation, microstructure of both milled powder and consolidated alloy. The crystallite size of W in W79Ni10Ti5Nb5(ZrO2)1 powder was 37 nm, 14.7 nm at 10 h and 20 h of milling respectively and lattice strain enhances to 0.54% at 20 h of milling. The crystallite size reduction is more at 10 h of milling and the rate drop beyond 10 to 20 h of milling. The intense improvement in dislocation density was evident upto 10 h of milling and the rate decreases between 10 to 20 h of milling. Increase in the lattice parameter of tungsten in W79Ni10Ti5Nb5(ZrO2)1 alloy upto 0.09% was observed at 10 h of milling owing to severe stress assisted deformation followed by contraction upto 0.07% at 20 h of milling due to formation of solid solution. The large spherical particles at 0 h of milling transformed to elongated shape at 10 h of milling and finer morphology at 20 h of milling. The average particle size reduced from 100 µm to 4.5 µm with the progress of milling from 0 to 20 h. Formation of fine polycrystallites of W was revealed by bright field TEM analysis and the observed crystallite size from TEM study was well supported by the evaluated crystallite size from XRD. XRD pattern and SEM micrograph of sintered alloy revealed the formation of NbNi, Ni3Ti intermetallic phases. Densification of 91.5% was attained in the 20 h milled and sintered alloy. Mechanical behaviour of the sintered product was evaluated by hardness and wear study. W79Ni10Ti5Nb5(ZrO2)1 alloy showed increase in hardness with decreasing load. The wear rate increases with increasing load due to higher abrasion effect at higher load.
Electrical and magnetic properties of nano-sized magnesium ferrite

NASA Astrophysics Data System (ADS)

T, Smitha; X, Sheena; J, Binu P.; Mohammed, E. M.

2015-02-01

Nano-sized magnesium ferrite was synthesized using sol-gel techniques. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. Vibration Sample Magnetometer was used to record the magnetic measurements. XRD analysis reveals the prepared sample is single phasic without any impurity. Particle size calculation shows the average crystallite size of the sample is 19nm. FTIR analysis confirmed spinel structure of the prepared samples. Magnetic measurement study shows that the sample is ferromagnetic with high degree of isotropy. Hysterisis loop was traced at temperatures 100K and 300K. DC electrical resistivity measurements show semiconducting nature of the sample.
Optical properties of cerium oxide (CeO2) nanoparticles synthesized by hydroxide mediated method

NASA Astrophysics Data System (ADS)

Ali, Mawlood Maajal; Mahdi, Hadeel Salih; Parveen, Azra; Azam, Ameer

2018-05-01

The nanoparticles of cerium oxide have been successfully synthesized by hydroxide mediated method, using cerium nitrate and sodium hydroxide as precursors. The microstructural properties were analyzed by X-ray diffraction technique (XRD). The X-ray diffraction results show that the cerium oxide nanoparticles were in cubic structure. The optical absorption spectra of cerium oxide were recorded by UV-VIS spectrophotometer in the range of 320 to 600 nm and photoluminescence spectra in the range of 400-540 nm and have been presented. The energy band gap was determined by Tauc relationship. The crystallite size was determined from Debye-Scherer equation and came out to be 6.4 nm.
Synthesis and photoluminescence of ultra-pure germanium nanoparticles

NASA Astrophysics Data System (ADS)

Chivas, R.; Yerci, S.; Li, R.; Dal Negro, L.; Morse, T. F.

2011-09-01

We have used aerosol deposition to synthesize defect and micro-strain free, ultra-pure germanium nanoparticles. Transmission electron microscopy images show a core-shell configuration with highly crystalline core material. Powder X-ray diffraction measurements verify the presence of highly pure, nano-scale germanium with average crystallite size of 30 nm and micro-strain of 0.058%. X-ray photoelectron spectroscopy demonstrates that GeO x ( x ⩽ 2) shells cover the surfaces of the nanoparticles. Under optical excitation, these nanoparticles exhibit two separate emission bands at room temperature: a visible emission at 500 nm with 0.5-1 ns decay times and an intense near-infrared emission at 1575 nm with up to ˜20 μs lifetime.
Effect of La3+ Substitution on Electric, Dielectric and Magnetic Properties of Cobalt Nano-Ferrite

NASA Astrophysics Data System (ADS)

Kumar, Pawan; Singh, M.

2011-07-01

Ultrafine particles of CoLaxFe2-xO4 (x = 0, 0.20) were prepared by using co-precipitation method. X-ray diffraction studies show that the samples have cubic spinel structure and average crystallite size of x = 0 and x = 0.2 are 49.84 nm and 27.73 nm respectively. Dielectric and magnetic properties have been studied by impedance analyzer and magnetic properties of the ferrite system were studied using VSM respectively. La3+ ions modulate significantly the electric, dielectric and magnetic properties of cobalt spinel ferrites.
Effect of Cu Salt Molarity on the Nanostructure of CuO Prolate Spheroid

NASA Astrophysics Data System (ADS)

Sabeeh, Sabah H.; Hussein, Hashim Abed; Judran, Hadia Kadhim

Copper sulfate pentahydrate was used as a source of Cu ion with five different molarities (0.02, 0.05, 0.1, 0.15, 2 and 0.25M). XRD, FE-SEM and TEM techniques all showed that CuO samples have polycrystalline monoclinic structure. CuO prolate spheroid is assembled from nanoparticles as building units. It was demonstrated that the purity, morphology, size range of prolate spheroid and density of nano building units are significantly influenced by Cu precursor’s molarity. The pure phase of CuO prolate spheroid was produced via molarity of 0.2M with crystallite size of 15.1565nm while the particle size of building units ranges from 16nm to 21nm. The stability of CuO nanosuspension or nanofluid was evaluated by zeta potential analysis. The obtained properties of specific structure with large surface area of CuO prolate spheroid make it a promising candidate for wide range of potential applications as in nanofluids for cooling purposes.
Synthesis of nanometer-sized sodalite without adding organic additives.

PubMed

Fan, Wei; Morozumi, Kazumasa; Kimura, Riichiro; Yokoi, Toshiyuki; Okubo, Tatsuya

2008-06-01

Aggregates (80 nm) of sodalite nanocrystals with crystallite sizes ranging from 20 to 40 nm have been synthesized from a sodium aluminosilicate solution at low temperature, without adding any organic additives, while paying attention to the key factors for the synthesis of nanosized zeolite crystals. The physical properties of nanosized sodalite crystals were characterized by X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, 29Si solid-state magic-angle spinning (MAS) NMR, and N2 adsorption. As expected, the external surface area of nanosized sodalite crystals is significantly increased compared with that of microsized sodalite crystals. The size of synthesized sodalite crystals can be controlled from 20 nm to 10 microm. It is found that the preparation of a homogeneous aluminosilicate solution followed by the formation of an aluminosilicate hard gel by adjusting the initial composition, for example, SiO2/Al2O3 and Na2O/H2O ratios, is critical for synthesis.
Oligonucleotide flexibility dictates crystal quality in DNA-programmable nanoparticle superlattices.

PubMed

Senesi, Andrew J; Eichelsdoerfer, Daniel J; Brown, Keith A; Lee, Byeongdu; Auyeung, Evelyn; Choi, Chung Hang J; Macfarlane, Robert J; Young, Kaylie L; Mirkin, Chad A

2014-11-12

The evolution of crystallite size and microstrain in DNA-mediated nanoparticle superlattices is dictated by annealing temperature and the flexibility of the interparticle bonds. This work addresses a major challenge in synthesizing optical metamaterials based upon noble metal nanoparticles by enabling the crystallization of large nanoparticles (100 nm diameter) at high volume fractions (34% metal). © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
One-step rapid synthesis of ultrafine γ-Ga2O3 nanocrystals by microwave hydrothermal method in ammonium hydroxide medium

NASA Astrophysics Data System (ADS)

Cui, Lu; Wang, Hong; Xin, Baifu; Mao, Guijie

2017-10-01

Ultrafine nanocrystals of γ-gallium oxide (γ-Ga2O3) were rapidly synthesized via microwave hydrothermal method at 140 °C, in which Ga(NO3)3 was used as the gallium source and urea was the precipitant. The samples were characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), transmission electron microscopy (TEM), nitrogen physisorption and photoluminescence spectroscopy (PL). The crystallite size of ultrafine spinel γ-Ga2O3 was in the range from 4 to 5 nm and the optical bandgap was 4.61 eV. To improve the crystallinity, the ultrafine γ-Ga2O3 nanocrystals were calcined at 300-700 °C further. The ultrafine γ-Ga2O3 calcined at 500 °C (calcined-γ-Ga2O3) still remained the metastable γ-phase with relatively high crystallinity and the crystallite size around 5-7 nm. Photocatalytic performances of the synthesized samples were also evaluated by the degradation of rhodamine B (RhB). Results revealed that the ultrafine γ-Ga2O3 and the calcined-γ-Ga2O3 samples exhibited high photocatalytic efficiencies of 68.2 and 90.7%, respectively.
Biosynthesis of extracellular and intracellular gold nanoparticles by Aspergillus fumigatus and A. flavus.

PubMed

Gupta, Saurabh; Bector, Shruti

2013-05-01

Green chemistry is a boon for the development of safe, stable and ecofriendly nanostructures using biological tools. The present study was carried out to explore the potential of selected fungal strains for biosynthesis of intra- and extracellular gold nanostructures. Out of the seven cultures, two fungal strains (SBS-3 and SBS-7) were selected on the basis of development of dark pink colour in cell free supernatant and fungal beads, respectively indicative of extra- and intracellular gold nanoparticles production. Both biomass associated and cell free gold nanoparticles were characterized using X-ray diffractogram (XRD) analysis and transmission electron microscopy (TEM). XRD analysis confirmed crystalline, face-centered cubic lattice of metallic gold nanoparticles along with average crystallite size. A marginal difference in average crystallite size of extracellular (17.76 nm) and intracellular (26 and 22 nm) Au-nanostructures was observed using Scherrer equation. In TEM, a variety of shapes (triangles, spherical, hexagonal) were observed in both extra- and intracellular nanoparticles. 18S rRNA gene sequence analysis by multiple sequence alignment (BLAST) indicated 99 % homology of SBS-3 to Aspergillus fumigatus with 99 % alignment coverage and 98 % homology of SBS-7 to Aspergillus flavus with 98 % alignment coverage respectively. Native-PAGE and activity staining further confirmed enzyme linked synthesis of gold nanoparticles.
Cellulose polymorphy, crystallite size, and the Segal crystallinity index

USDA-ARS?s Scientific Manuscript database

The X-ray diffraction-based Segal Crystallinity Index (CI) was calculated for simulated different sizes of crystallites for cellulose I' and II. The Mercury software was used, and different crystallite sizes were based on different input peak widths at half of the maximum peak intensity (pwhm). The ...
DOE Office of Scientific and Technical Information (OSTI.GOV)

Ravikumar, Patta; Kisan, Bhagaban; Perumal, A., E-mail: perumal@iitg.ernet.in

We report systematic investigations of structural, vibrational, resonance and magnetic properties of nanoscale NiO powders prepared by ball milling process under different milling speeds for 30 hours of milling. Structural properties revealed that both pure NiO and as-milled NiO powders exhibit face centered cubic structure, but average crystallite size decreases to around 11 nm along with significant increase in strain with increasing milling speed. Vibrational properties show the enhancement in the intensity of one-phonon longitudinal optical (LO) band and disappearance of two-magnon band due to size reduction. In addition, two-phonon LO band exhibits red shift due to size-induced phonon confinementmore » effect and surface relaxation. Pure NiO powder exhibit antiferromagnetic nature, which transforms into induced ferromagnetic after size reduction. The average magnetization at room temperature increases with decreasing the crystallite size and a maximum moment of 0.016 μ{sub B}/f.u. at 12 kOe applied field and coercivity of 170 Oe were obtained for 30 hours milled NiO powders at 600 rotation per minute milling speed. The change in the magnetic properties is also supported by the vibrational properties. Thermomagnetization measurements at high temperature reveal a well-defined magnetic phase transition at high temperature (T{sub C}) around 780 K due to induced ferromagnetic phase. Electron paramagnetic resonance (EPR) studies reveal a good agreement between the EPR results and magnetic properties. The observed results are described on the basis of crystallite size variation, defect density, large strain, oxidation/reduction of Ni and interaction between uncompensated surfaces and particle core with lattice expansion. The obtained results suggest that nanoscale NiO powders with high T{sub C} and moderate magnetic moment at room temperature with cubic structure would be useful to expedite for spintronic devices.« less
Structural and magnetic properties of cobalt-doped iron oxide nanoparticles prepared by solution combustion method for biomedical applications.

PubMed

Venkatesan, Kaliyamoorthy; Rajan Babu, Dhanakotti; Kavya Bai, Mane Prabhu; Supriya, Ravi; Vidya, Radhakrishnan; Madeswaran, Saminathan; Anandan, Pandurangan; Arivanandhan, Mukannan; Hayakawa, Yasuhiro

2015-01-01

Cobalt-doped iron oxide nanoparticles were prepared by solution combustion technique. The structural and magnetic properties of the prepared samples were also investigated. The average crystallite size of cobalt ferrite (CoFe2O4) magnetic nanoparticle was calculated using Scherrer equation, and it was found to be 16±5 nm. The particle size was measured by transmission electron microscope. This value was found to match with the crystallite size calculated by Scherrer equation corresponding to the prominent intensity peak (311) of X-ray diffraction. The high-resolution transmission electron microscope image shows clear lattice fringes and high crystallinity of cobalt ferrite magnetic nanoparticles. The synthesized magnetic nanoparticles exhibited the saturation magnetization value of 47 emu/g and coercivity of 947 Oe. The anti-microbial activity of cobalt ferrite nanoparticles showed better results as an anti-bacterial agent. The affinity constant was determined for the nanoparticles, and the cytotoxicity studies were conducted for the cobalt ferrite nanoparticles at different concentrations and the results are discussed.
Structural and magnetic properties of cobalt-doped iron oxide nanoparticles prepared by solution combustion method for biomedical applications

PubMed Central

Venkatesan, Kaliyamoorthy; Rajan Babu, Dhanakotti; Kavya Bai, Mane Prabhu; Supriya, Ravi; Vidya, Radhakrishnan; Madeswaran, Saminathan; Anandan, Pandurangan; Arivanandhan, Mukannan; Hayakawa, Yasuhiro

2015-01-01

Cobalt-doped iron oxide nanoparticles were prepared by solution combustion technique. The structural and magnetic properties of the prepared samples were also investigated. The average crystallite size of cobalt ferrite (CoFe2O4) magnetic nanoparticle was calculated using Scherrer equation, and it was found to be 16±5 nm. The particle size was measured by transmission electron microscope. This value was found to match with the crystallite size calculated by Scherrer equation corresponding to the prominent intensity peak (311) of X-ray diffraction. The high-resolution transmission electron microscope image shows clear lattice fringes and high crystallinity of cobalt ferrite magnetic nanoparticles. The synthesized magnetic nanoparticles exhibited the saturation magnetization value of 47 emu/g and coercivity of 947 Oe. The anti-microbial activity of cobalt ferrite nanoparticles showed better results as an anti-bacterial agent. The affinity constant was determined for the nanoparticles, and the cytotoxicity studies were conducted for the cobalt ferrite nanoparticles at different concentrations and the results are discussed. PMID:26491320
Developpement d'un modele thermodynamique pour les cristallites de coke: Application aux systems carbone-hydrogene et carbone-soufre

NASA Astrophysics Data System (ADS)

Ouzilleau, Philippe

Carbon materials are essential components of multiple key industrial processes. One example of such a process is the production of aluminum using the Hall-Heroult process. It is well known that important quantities of carbon materials are regularily consumed by the operation of the Hall-Heroult process. In recent years, the increased impurity content of industrial carbon materials motivated the development of a better understanding for the high temperature behavior of these specific materials. The most common forms of carbon materials used in the industry are cokes. Cokes are carbon materials which, following heat treatment, present a crystalline structure similar to that observed in graphite. However, the observed crystallite size of cokes is usually much smaller than the one observed in graphite. For this reason, the chemical and thermodynamic properties of the ordered phase of cokes (i.e. coke crystallites) are very different than those of graphite (although coke crystallites of infinite size would possess properties almost identical to graphite). Coke crystallites consist of hexagonal planes of carbon atoms stacked one above the other. This particular aspect causes strong anisotropic properties in coke crystallites. No thermodynamic model was found for the production of a reliable correlation between the effect of crystallite size and chemical composition for the predictive calculations of the thermodynamic properties (and phase equilibriums) of coke crystallites. It is also difficult to produce predictive calculations that can be compared to experimental results using such a thermodynamic model. The goal of the present work is to propose a thermodynamic model designed to solve this problem. The present model is based on the well-defined geometrical properties of coke cristallites. This geometry allows the development of mathematical equations for the calculation of the mass balances of the crystallite (using a simplified geometry) using only the commonly used cristallite size parameters La (diameter of the crystallite) and Lc (height of the crystallite). The use of the Compound Energy Formalism is necessary to establish the methodology of the present model. Globally, the planar structure of the crystallites is divided into three sublattices on which individual chemical species are assumed to mix randomly. Appropriate thermodynamic paths are used to define the relative enthalpies and absolute entropies of these chemical species. The relative enthalpy and absolute entropy of the coke crystallites are derived for various values of La in the carbon/hydrogen and carbon/sulfur chemical systems. For the carbon/hydrogen system, the model parameters are based on the known values for the entropy of formation of simple hydrogenous organic compounds in the gaseous phase and known carbon/hydrogen bond enthalpies. Also, additional enthalpic properties of coke crystallites and graphitic structures are required for the definition of the thermodynamic paths (for example, the enthalpy associated with the delocalization of one electron in graphitic structures). Results for the carbon/hydrogen system are compared to experiments concerning the dehydrogenation of various cokes. A very satisfying agreement is obtained between the dehydrogenation curves predictively calculated by the model and the reported experimental results (obtained using slow heating rates). Most of the hydrogen content of coke crystallites (this content does not inclue the hydrogen in the condensed volatile matter phase) is predicted to leave the crystalline structure for temperatures between 1100 and 1300 K. Also, experimental measurements of the Gibbs energy of coke relative to graphite are reported. These measurements were obtained using a solid state electrochemical technique. A stabiliy of approximately 900 J g-1, relative to graphite, is reported for temperatures between 950 and 1250 K and for a crystallite size La of ˜10 nm. This value is in excellent agreement with the present thermodynamic model. Finally, an open discussion is made on the possible existance of a degraphitization behavior for coke crystallites heat treated above 2585 K. For the carbon/sulfur system, a modeling approach similar to the one developed for the carbon/hydrogen system is used. Approximately 75% of the model parameters of the carbon/hydrogen and carbon/sulfur systems are common to the two models. Predictive desulfurization curves using the current thermodynamic model are presented for temperatures above 1500 K. A very good agreement is obtained between the model calculations and the reported experimental data. Most of the sulfur content of coke crystallites is predicted to leave the crystallites for temperatures between 1600 and 1850 K. This temperature range is very similar to the puffing temperatures typically found during the desulfurization of petrochemical cokes. The good precision of the model for both studied systems (carbon/sulfur and carbon/hydrogen) combined with the transferability of the model parameters between the carbon/hydrogen and carbon/sulfur systems tend to validate the global approach developed so far.
One-dimensional nanoferroic rods; synthesis and characterization

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Seddik, U.; Okasha, N.; Imam, N. G.

2015-11-01

One-dimensional nanoferroic rods of BaTiO3 were synthesized by improved citrate auto-combustion technology using tetrabutyl titanate. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) have been used to characterize the prepared sample. The results indicated that the crystal structure of BaTiO3 is tetragonal phase with an average crystallite size of 47 nm. SEM image gives a cauliflower-like morphology of the agglomerated nanorods. The stoichiometry of the chemical composition of the BaTiO3 ceramic was confirmed by EDX. TEM micrograph exhibited that BaTiO3 nanoparticles have rod-like shape with an average length of 120 nm and width of 43 nm. AFM was used to investigate the surface topography and its roughness. The topography image in 3D showed that the BaTiO3 particles have a rod shape with an average particle size of 116 nm which in agreement with 3D TEM result.
Microstructure, hardness and modulus of carbon-ion-irradiated new SiC fiber (601-4)

NASA Astrophysics Data System (ADS)

Huang, Qing; Lei, Guanhong; Liu, Renduo; Li, Jianjian; Yan, Long; Li, Cheng; Liu, Weihua; Wang, Mouhua

2018-05-01

Two types of SiC fibers, one is low-oxygen and carbon-rich fiber denoted by 601-4 and the other is low-oxygen and near-stoichiometric Tyranno SA, were irradiated with 450 keV C+ ions at room temperature. The Raman spectra indicate that irradiation induced distortion and amorphization of SiC crystallites in fibers. TEM characterization of Tyranno SA suggests that SiC crystallites undergo a continued fragmentation into smaller crystalline islands and a continued increase of surrounding amorphous structure. The SiC nano-crystallites (<15 nm) in 601-4 fiber are more likely to be amorphized than larger crystallites (∼200 nm) in Tyranno SA. The hardness and modulus of 601-4 continuously decreases with increasing fluence, while that of Tyranno SA first increases and then decreases.
The effect of temperature deposited on the performance of ZnO-CNT-graphite for supercapacitors

NASA Astrophysics Data System (ADS)

Darari, Alfin; Hakim, Istajib S.; Priyono; Subagio, Agus; Pardoyo; Subhan, Achmad

2017-07-01

Carbon nanotubes (CNTs), graphite are now widely studied as the electrodes of supercapacitor, owing to their high conductivity, large surface area, chemical stability, etc. A lot of research has been focused on Carbon/metal oxide nanocomposite electrode for Electrode supercapacitor because it will increase the total capacitance. In this research, ZnO nanoparticles were deposited onto substrate CNT:Graphite in different temperatures such as 300°, 350°, and 400°C. The characterization of the crystal size using X-Ray Diffraction (XRD) patterns showed ZnO material peak was detected a ZnO crystallite. The size of ZnO crystallite in 300°, 350°, and 400°C consecutively is 101.1; 103.4; and 116.7 nm. The test results are Electrochemical impedance spectrometry (EIS) high electrical conductivity values obtained on the composition of ZnO-CNT-graphite with a temperature of 350°C 4.6 (S/m); and (2) the highest value of capacitance in 300°C is 1.23 F/g.
Synthesis, surface chemistry and pseudocapacitance mechanisms of VN nanocrystals derived by a simple two-step halide approach

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

Choi, Daiwon; Jampani, Prashanth H.; Jayakody, J. R. P.

Chloroamide precursors generated via a simple two-step ammonolysis reaction of transition metal chloride in the liquid phase at room temperature were heat treated in ammonia at moderate temperature to yield nano-sized VN crystallites. Grain growth inhibited by lowering the synthesis temperature (≈400°C) yielded agglomerated powders of spherical crystallites of cubic phase of VN with particle sizes as small as 6nm in diameter. X-ray diffraction, FTIR, mass spectroscopy (MS), and nuclear magnetic resonance (NMR) spectroscopy assessed the ammonolysis and nitridation reaction of the VCl 4-NH 3 system. X-ray Rietveld refinement, the BET technique and high-resolution transmission microscopy (HRTEM), energy dispersive x-raymore » (EDX) and thermogravimetric analysis (TGA) helped assess the crystallographic and microstructural nature of the VN nanocrystals. The surface chemistry and redox reaction leading to the gravimetric pseudo-capacitance value of (≈855 F/g) measured for the VN nanocrystals was determined and validated using FTIR, XPS and cyclic voltammetry analyses.« less
Frequency dependent dielectric properties of Sr doped NiO nanostructures

NASA Astrophysics Data System (ADS)

Siddique, M. Naseem; Ahmed, Ateeq; Ali, T.; Tripathi, P.

2018-05-01

Ni1-xSrxO (x=0.0, 0.02) nanoparticles have been synthesized using sol-gel method calcined at temperature 600 °C. The XRD analysis result revealed that the calcined sample has a cubic structure with single phase structure. We have calculated crystallite size of samples using both Debye-Sherrer and William Hall (W-H) method which are found to be 19.69 nm, 22.39 nm and 28.50 nm, 33.27 nm, respectively. TEM image reveals the formation of spherical shaped particles. In addition, dielectric properties have been studied using LCR measurement and found that ɛ', ɛ″ and tan δ are decreases with increase in frequency whereas ac conductivity increases with increase in frequency. This behavior may be explained using Maxwell-Wagner and Koop theory.

Facile microwave-assisted synthesis of Te-doped hydroxyapatite nanorods and nanosheets and their characterizations for bone cement applications.

PubMed

Yahia, I S; Shkir, Mohd; AlFaify, S; Ganesh, V; Zahran, H Y; Kilany, Mona

2017-03-01

In this work, the authors have fabricated the nanorods and nanosheets of pure and Te-doped HAp with different Te concentrations (0.04, 0.08, 0.16, 0.24wt%) by microwave-assisted technique at low temperature. The crystallite size, degree of crystallinity and lattice parameters are calculated. FE-SEM study confirms that the fabricated nanostructures are nanorods of diameter about 10nm in undoped and at low concentration of Te doping. However, at and higher concentration, it becomes nanosheets of about 5nm thickness. X-ray diffraction, FT-IR and FT-Raman studies shows that the prepared products are of HAp and Te has been successfully incorporated. From EDX the Ca/P molar ratio of the pure HAp is about 1.740, while this ratio for 0.04, 0.08, 0.16, 0.24 wt% Te doped is about 1.53, 1.678, 1.724, 1.792, respectively. Crystallite size was found to be increased with Te doping from 15nm to 62nm. The value of dielectric constant is found to be enhanced at higher concentrations of Te. The values of linear absorption coefficient were also determined and show that the prepared material with Te doping is more absorbable than pure and will be highly applicable in radiation detection applications. Furthermore, the antimicrobial potential of pure and Te doped HAp was examined against some Gram- negative and positive bacteria and fungi by agar disk diffusion method. The results demonstrated that the antimicrobial activity of Te doped HAp is stronger than that of pure HAp where it exhibited the highest activity against Bacillus subtilis>Candida albicans>Shigella dysenteriae. Copyright © 2016 Elsevier B.V. All rights reserved.
Microwave-Assisted Synthesis of Silver Vanadium Phosphorus Oxide, Ag 2VO 2PO 4 : Crystallite Size Control and Impact on Electrochemistry

DOE PAGES

Huang, Jianping; Marschilok, Amy C.; Takeuchi, Esther S.; ...

2016-03-07

We study silver vanadium phosphorus oxide, Ag 2VO 2PO 4, that is a promising cathode material for Li batteries due in part to its large capacity and high current capability. Herein, a new synthesis of Ag 2VO 2PO 4 based on microwave heating is presented, where the reaction time is reduced by approximately 100× relative to other reported methods, and the crystallite size is controlled via synthesis temperature, showing a linear correlation of crystallite size with temperature. Notably, under galvanostatic reduction, the Ag 2VO 2PO 4 sample with the smallest crystallite size delivers the highest capacity and shows the highestmore » loaded voltage. Further, pulse discharge tests show a significant resistance decrease during the initial discharge coincident with the formation of Ag metal. Thus, the magnitude of the resistance decrease observed during pulse tests depends on the Ag 2VO 2PO 4 crystallite size, with the largest resistance decrease observed for the smallest crystallite size. Additional electrochemical measurements indicate a quasi-reversible redox reaction involving Li + insertion/deinsertion, with capacity fade due to structural changes associated with the discharge/charge process. In summary, this work demonstrates a faster synthetic approach for bimetallic polyanionic materials which also provides the opportunity for tuning of electrochemical properties through control of material physical properties such as crystallite size.« less
Preparation and Scintillating Properties of Sol-Gel Eu3+, Tb3+ Co-Doped Lu2O3 Nanopowders

PubMed Central

de Jesús Morales Ramírez, Ángel; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Hernández, Margarita García; Palmerin, Joel Moreno; Guerrero, Rosario Ruiz

2011-01-01

Nanocrystalline Eu3+, Tb3+ co-doped Lu2O3 powders with a maximum size of 25.5 nm were prepared by the sol-gel process, using lutetium, europium and terbium nitrates as precursors, and ethanol as a solvent. Differential thermal analysis (DTA) and infrared spectroscopy (IR) were used to study the chemical changes during the xerogel annealing. After the sol evaporation at 100 °C, the formed gel was annealed from 300 to 900 °C for 30 min under a rich O2 atmosphere, and the yielded product was analyzed by X-ray diffraction (XRD) to characterize the microstructural behavior and confirm the crystalline structure. The results showed that Lu2O3 nanopowders start to crystallize at 400 °C and that the crystallite size increases along with the annealing temperature. A transmission electron microscopy (TEM) study of samples annealed at 700 and 900 °C was carried out in order to analyze the microstructure, as well as the size, of crystallites. Finally, in regard to scintillating properties, Eu3+ dopant (5 mol%), Tb3+ codoped Lu2O3 exhibited a typical red emission at 611 nm (D°→7F2), furthermore, the effect of Tb3+ molar content (0.01, 0.015 and 0.02% mol) on the Eu3+ radioluminiscence was analyzed and it was found that the higher emission intensity corresponds to the lower Tb3+ content. PMID:22016655
Surfactant-assisted morphological studies of α-Al2O3 nanoparticles

NASA Astrophysics Data System (ADS)

Shah, Janki; Ranjan, Mukesh; Gupta, Sanjeev K.; Sonvane, Yogesh

2018-05-01

The present study deals with the synthesis and characterization of aluminum oxide (Al2O3) nanopowders, it is very useful material as dielectric, ceramic and catalyst. The high-quality nanopowders were obtained by adding surfactants urea and sodium acetate. Further, all characterizations are done for with (urea and sodium acetate) and without surfactant. X-ray diffraction was used to characterize phase formation and the crystallite size of powder while, FTIR gives information about the particle composition and surface intermediates. X-ray diffraction spectra revealed the synthesized nanoparticles phase transformation were γ-Al2O3 to α-Al2O3 phase. Furthermore, the addition of urea and sodium acetate significantly reduced the crystalline size of α-Al2O3 nanoparticles from 43.94 nm to 35.12 nm respectively.
Platinum particle size and support effects in NO(x) mediated carbon oxidation over platinum catalysts.

PubMed

Villani, Kenneth; Vermandel, Walter; Smets, Koen; Liang, Duoduo; van Tendeloo, Gustaaf; Martens, Johan A

2006-04-15

Platinum metal was dispersed on microporous, mesoporous, and nonporous support materials including the zeolites Na-Y, Ba-Y, Ferrierite, ZSM-22, ETS-10, and AIPO-11, alumina, and titania. The oxidation of carbon black loosely mixed with catalyst powder was monitored gravimetrically in a gas stream containing nitric oxide, oxygen, and water. The carbon oxidation activity of the catalysts was found to be uniquely related to the Pt dispersion and little influenced by support type. The optimum dispersion is around 3-4% corresponding to relatively large Pt particle sizes of 20-40 nm. The carbon oxidation activity reflects the NO oxidation activity of the platinum catalyst, which reaches an optimum in the 20-40 nm Pt particle size range. The lowest carbon oxidation temperatures were achieved with platinum loaded ZSM-22 and AIPO-11 zeolite crystallites bearing platinum of optimum dispersion on their external surfaces.
On the formation of nanocrystalline active zinc oxide from zinc hydroxide carbonate

NASA Astrophysics Data System (ADS)

Moezzi, Amir; Cortie, Michael; Dowd, Annette; McDonagh, Andrew

2014-04-01

The decomposition of zinc hydroxide carbonate, Zn5(CO3)2(OH)6 (ZHC), into the high surface area form of ZnO known as "active zinc oxide" is examined. In particular, the nucleation and evolution of the ZnO nanocrystals is of interest as the size of these particles controls the activity of the product. The decomposition process was studied using X-ray diffraction, thermogravimetric analysis, scanning electron microscopy, transmission electron microscopy and BET surface area measurements. At about 240 °C ZHC decomposes to porous ZnO in a single step. The product material has a specific surface area in the range of 47-65 m2 g-1 and initially has a crystallite size that is of the order of 10 nm. A further increase in temperature, however, causes the particles to coarsen to over 25 nm in diameter. In principle, the coarsening phenomenon may be interrupted to control the particle size.
Ambient aging of rhenium filaments used in thermal ionization mass spectrometry: Growth of oxo-rhenium crystallites and anti-aging strategies.

PubMed

Mannion, Joseph M; Wellons, Matthew S; Shick, Charles R; Fugate, Glenn A; Powell, Brian A; Husson, Scott M

2017-01-01

Degassing is a common preparation technique for rhenium filaments used for thermal ionization mass spectrometric analysis of actinides, including plutonium. Although optimization studies regarding degassing conditions have been reported, little work has been done to characterize filament aging after degassing. In this study, the effects of filament aging after degassing were explored to determine a "shelf-life" for degassed rhenium filaments, and methods to limit filament aging were investigated. Zone-refined rhenium filaments were degassed by resistance heating under high vacuum before exposure to ambient atmosphere for up to 2 months. After degassing the nucleation and preferential growth of oxo-rhenium crystallites on the surface of polycrystalline rhenium filaments was observed by atomic force microscopy and scanning electron microscopy (SEM). Compositional analysis of the crystallites was conducted using SEM-Raman spectroscopy and SEM energy dispersive X-ray spectroscopy, and grain orientation at the metal surface was investigated by electron back-scatter diffraction mapping. Spectra collected by SEM-Raman suggest crystallites are composed primarily of perrhenic acid. The relative extent of growth and crystallite morphology were found to be grain dependent and affected by the dissolution of carbon into filaments during annealing (often referred to as carbonization or carburization). Crystallites were observed to nucleate in region specific modes and grow over time through transfer of material from the surface. Factors most likely to affect the rates of crystallite growth include rhenium substrate properties such as grain size, orientation, levels of dissolved carbon, and relative abundance of defect sites; as well as environmental factors such as length of exposure to oxygen and relative humidity. Thin (∼180 nm) hydrophobic films of poly(vinylbenzyl chloride) were found to slow the growth of oxo-rhenium crystallites on the filament surfaces and may serve as an alternative carbon source for filament carburization.
Role of surface states and defects in the ultrafast nonlinear optical properties of CuS quantum dots

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

Mary, K. A. Ann; Unnikrishnan, N. V., E-mail: nvu100@yahoo.com; Philip, Reji

2014-07-01

We report facile preparation of water dispersible CuS quantum dots (2–4 nm) and nanoparticles (5–11 nm) through a nontoxic, green, one-pot synthesis method. Optical and microstructural studies indicate the presence of surface states and defects (dislocations, stacking faults, and twins) in the quantum dots. The smaller crystallite size and quantum dot formation have significant effects on the high energy excitonic and low energy plasmonic absorption bands. Effective two-photon absorption coefficients measured using 100 fs laser pulses employing open-aperture Z-scan in the plasmonic region of 800 nm reveal that CuS quantum dots are better ultrafast optical limiters compared to CuS nanoparticles.
On the possibility of room temperature ferromagnetism on chunk-shape BaSnO3/ZnO core/shell nanostructures

NASA Astrophysics Data System (ADS)

Rajamanickam, N.; Jayakumar, K.; Ramachandran, K.

2018-04-01

Core/shell BaSnO3/ZnO (BS-ZO) nanostructures were prepared by oxalate precipitation method and wet-chemical method. BaSnO3 (BSO) cubic perovskite structure and ZnO hexagonal wurtzite structure were confirmed by X-ray diffraction (XRD). The crystallite sizes is 23 nm, 29 nm and 27 nm for BSO, ZnO and BS-ZO, respectively. Chunk-shape and cuboids morphology observed from scanning electron microscopy (SEM) analysis. The magnetic properties were studied by VSM for bare and core-shell nano systems and the room temperature ferromagnetism observed for core-shell nanostructures. The BSO/ZnO shows enhanced coercivity and saturated magnetization as compared with BSO and ZnO nanostructures.
Structure and morphology evolution of silica-modified pseudoboehmite aerogels during heat treatment

NASA Astrophysics Data System (ADS)

Pakharukova, V. P.; Shalygin, A. S.; Gerasimov, E. Yu.; Tsybulya, S. V.; Martyanov, O. N.

2016-01-01

Silica-modified pseudoboehmite aerogels (0, 10, 20 at% of Si) were prepared by sol-gel method followed by supercritical drying. The phase transformations, changes in structure and morphology upon calcination were thoroughly investigated by advanced X-Ray diffraction (XRD) techniques and high-resolution transmission electron microscopy (HRTEM). Obtained pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. The silica dopant drastically enhanced the crystallite anisotropy. Thus, the aerogel with Al:Si atomic ratio of 9:1 consisted of the pseudoboehmite nanosheets with thickness of one unit cell (average dimensions of 14.0×1.2×14.5 nm). The specific nanostructure caused remarkable features of experimental XRD patterns, including anisotropic peak broadening and appearance of forbidden reflection. Direct simulation of XRD patterns with using the Debye Scattering Equation allowed the size and morphology of pseudoboehmite crystallites to be determined. The silica addition strongly delayed formation of γ-alumina and further phase transformations upon calcinaton. Thermal stability of alumina was suggested to be affected by the particle morphology inherited from the pseudoboehmite precursor.
An insight into the influence of crystallite size on the performances of microsized spherical Li(Ni0.5Co0.2Mn0.3)O2 cathode material composed of aggregated nanosized particles

NASA Astrophysics Data System (ADS)

Fan, Guangxin; Wen, Yin; Liu, Baozhong; Yang, Wenpeng

2018-02-01

Relationships between the performance and the crystallite size of the microsized spherical Li(Ni0.5Co0.2Mn0.3)O2 cathode material composed of aggregated nanosized primary particles have been comprehensively studied. The cathode material was synthesized by a high-temperature solid-state method. The results obtained by XRD, Rietveld refinement, SEM, HR-TEM, DSC, and galvanostatic test show that the crystallite size (XS) of Li(Ni0.5Co0.2Mn0.3)O2 is greatly affected by the temperature in the range of 750 to 820 °C. Most of all, the crystallite size plays a unique role in the performance of the material. That is, the electrochemical characteristics of Li(Ni0.5Co0.2Mn0.3)O2, such as discharge capacity, rate performance, and thermal stability, are closely related to the crystallite size. Furthermore, the retention of discharge capacity is determined by that of crystallite size in Li(Ni0.5Co0.2Mn0.3)O2 after 100 cycles.
Microstructural evolution of diamond growth during HFCVD

NASA Technical Reports Server (NTRS)

Singh, J.

1994-01-01

High resolution transmission electron microscopy (HRTEM) was used to study the nucleation and growth mechanism of diamond by hot filament chemical vapor deposition (HFCVD) process. A novel technique has shown a direct evidence for the formation of the diamond-like carbon layer 8-14 nm thick in which small diamond micro-crystallites were embedded. These diamond micro-crystallites were formed as a result of transformation of diamond-like carbon into diamond. The diamond micro-crystallites present in the amorphous diamond-like carbon layer provided nucleation sites for diamond growth. Large diamond crystallites were observed to grow from these micro-crystallites. The mechanism of diamond growth will be presented based on experimental findings.
Effcet of acid stimulation on the photoresponse of single walled carbon nanotubes

NASA Astrophysics Data System (ADS)

Dhall, Shivani; Mehta, B. R.

2018-04-01

In this work, we have investigated the effect of acid treatment on the photoresponse of single walled carbon nanotubes (SWCNTs) and silicon (Si) interface. It was found that acid infiltration of SWCNTs proved helpful for the removal of impurities such as amhoporous carbon and improved the photoresponse at room temperature from 20 % to 42%. Raman analysis confirms that, the calculated crystallite size of the acids treated nanotubes is found to increase to 14.11 nm as compared to 13.7 nm for the pristine tubes. Furthermore, acid functionalized SWCNTs/Si interface shows better rectifying behavior as compared to pristine SWCNTs/ Si interface.
Investigation of photoluminescence and dielectric properties of pure and Fe doped nickel oxide nanoparticles

NASA Astrophysics Data System (ADS)

Gupta, Jhalak; Ahmad, Arham S.

2018-05-01

The nanocrystallites of pure and Fe doped Nickel Oxide (NiO) were synthesized by the cost effective co-precipitation method using nickel nitrate as the initial precursor. The synthesized nickel oxide nanoparticles were characterized by X-Ray Diffraction (XRD), Photoluminiscence Spectroscopy (PL), LCR meter. The crystallite size of synthesized pure Nickel Oxide nanoparticles obtained by XRD using Debye Scherer's formula was found to be 21.8nm and the size decreases on increasing the dopant concentration. The optical properties were analyzed by PL and dielectric ones by using LCR meter.
Reaction-diffusion-induced explosive crystallization in a metal-selenium nanometer film structure

NASA Astrophysics Data System (ADS)

Kogai, V. Ya.

2016-03-01

Experimental data for reaction-diffusion-induced explosive crystallization in a nanodimensional metal (Cu, Ag)/selenium structure are presented. It is found that after the metal layer has completely diffused into the amorphous Se film, the electrical potential rises from 0.14 to 1.21 V in the Cu(30 nm)/Se(140 nm) heterolayer and from 0.01 to 1.17 V in the Ag(30 nm)/Se(140 nm) heterolayer. The metals diffusing into the amorphous Se layer interact with Se, forming nuclei of a new phase (CuSe or Ag2Se). The intense growth of the CuSe and Ag2Se crystallization centers results in a considerable liberation of latent energy in the form of phase transformation heat and in explosive growth of CuSe and Ag2Se nanocrystalline particles. The mean size of CuSe and Ag2Se crystallites equals 25 and 50 nm, respectively.
TEM characterization of nanodiamond thin films.

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

Qin, L.-C.; Zhou, D.; Krauss, A. R.

The microstructure of thin films grown by microwave plasma-enhanced chemical vapor deposition (MPCVD) from fullerene C{sub 60} precursors has been characterized by scanning electron microscopy (SEM), selected-area electron diffraction (SAED), bright-field electron microscopy, high-resolution electron microscopy (HREM), and parallel electron energy loss spectroscopy (PEELS). The films are composed of nanosize crystallites of diamond, and no graphitic or amorphous phases were observed. The diamond crystallite size measured from lattice images shows that most grains range between 3-5 nm, reflecting a gamma distribution. SAED gave no evidence of either sp2-bonded glassy carbon or sp3-bonded diamondlike amorphous carbon. The sp2-bonded configuration found inmore » PEELS was attributed to grain boundary carbon atoms, which constitute 5-10% of the total. Occasionally observed larger diamond grains tend to be highly faulted.« less
Two-stage processed high-quality famatinite thin films for photovoltaics

NASA Astrophysics Data System (ADS)

Chalapathi, U.; Poornaprakash, B.; Cui, Hao; Park, Si-Hyun

2017-11-01

Famatinite (Cu3SbS4) thin films were prepared by annealing chemically grown Sb2S3-CuS stacks in a graphite box at 370-430 °C for 30 min under sulfur and N2 atmospheres. The films grown at 370 °C contain a minor CuSbS2 phase with dominant Cu3SbS4. Those films prepared at 400 °C and 430 °C are single-phase Cu3SbS4 with a tetragonal structure and lattice parameters a = 0.537 nm and b = 1.087 nm and a crystallite size of 25 nm. The grain size of the films increases as the annealing temperature is increased to 400 °C and subsequently decreases. The film morphology is compact and void-free with a grain size of 300-800 nm at 400 °C. The band gap of the films is 0.89 eV. The films exhibited p-type electrical conductivity and a relatively high hole mobility of 14.70 cm2V-1s-1 at 400 °C. Their attractive optoelectronic properties suggest that these films are suitable as solar cell absorber layers.
Synthesis and characterization of polyvinylimidazole-grafted superparamagnetic iron oxide nanoparticles (Si-PVIm-grafted SPION)

NASA Astrophysics Data System (ADS)

Erdemi, H.; Sözeri, H.; Şenel, M.; Baykal, A.

2012-08-01

Polyvinylimidazole (PVIm)-grafted superparamagnetic iron oxide nanoparticles (SPION) (Si-PVIm-grafted Fe3O4 NPs) were prepared by grafting of telomere of PVIm on the SPION. The product identified as magnetite, which has an average crystallite size of 9 ± 2 nm as estimated from X-ray line profile fitting. Particle size was estimated as 10.0 ± 0.5 nm from TEM micrographs. Mean particle size is found as 8.4 ± 1.0 nm which agrees well with the values calculated from XRD patterns (9 ± 2 nm). Vibrating Sample Magnetometer (VSM) analysis explained the superparamagnetic nature of the nanocomposite. Thermogravimetric analysis showed that the Si-Imi is 25 % of the Si-PVIm-grafted SPION, which means an inorganic content is about 75 %. Detailed electrical and dielectric properties of the properties of the product are also presented. The conductivity of the sample increases significantly with temperature and has the value in the range of 1.14 × 10-7-1.78 × 10-4 S cm-1. Analysis of the real and imaginary parts of the permittivities indicated temperature and frequency dependency representing interfacial polarization and temperature-assisted reorganization effects.
Nano crystalline Bi{sub 2}(VO{sub 5}) phases in lithium bismuth borate glasses containing mixed vanadium-nickel oxides

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

Yadav, Arti, E-mail: artidabhur@gmail.com; Khasa, S.; Dahiya, M. S.

2016-05-23

Glass composition 7V{sub 2}O{sub 5}·23Li{sub 2}O·20Bi{sub 2}O{sub 3}·50B{sub 2}O{sub 3} and x(2NiO·V{sub 2}O{sub 5})·(30-x)Li{sub 2}O·20Bi{sub 2}O{sub 3}·50B{sub 2}O{sub 3}, x=0, 2, 5, 7 and 10, were produced by conventional melt quenching technique. The quenched amorphous glass samples were annealed at temperatures 400°C and 500°C for 6 hours. The Bi{sub 2}(VO{sub 5}) crystallite were grown in all prepared glass matrix. Tn vanadium lithium bismuth borate glass (annealed), the some phrase of V{sub 2}O{sub 5}-crystal were observed along with the nano crystalline Bi{sub 2}(VO{sub 5}) phase. The sharp peaks in FTTR spectra of all annealed compositions were also compatible with the XRDmore » diffraction peaks of the system under investigation. Average crystalline size (D) of the Bi{sub 2}(VO{sub 5}) nano-crystallite was ~30 nm for samples annealed at 400°C and ~42 nm for samples annealed at 500°C. Lattice parameter and the lattice strain for all the samples was also calculated corresponding to the (113) plane of Bi{sub 2}(VO{sub 5}) crystallite.« less
Enhancement of luminescence emission from GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} phosphor by Li{sup +} co-doping

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

Gavrilović, Tamara V.; Jovanović, Dragana J., E-mail: draganaj@vinca.rs; Lojpur, Vesna M.

2014-09-15

This paper demonstrates the effects of Li{sup +} co-doping on the structure, morphology, and luminescence properties of GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} phosphor prepared using a high-temperature solid-state chemistry method. The GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} powders synthesized with the Li{sup +} co-dopant (in concentrations of 0, 5, 10, and 15 mol%) are characterized by X-ray powder diffraction, scanning electron microscopy, and photoluminescence spectroscopy. Structural analysis showed that powders co-doped with Li{sup +} have larger crystallite sizes and slightly smaller crystal lattice parameters than powders prepared without Li{sup +} ions. Photoluminescence down-conversion (345-nm excitation) and up-conversion (980-nm excitation) spectra show characteristic Er{supmore » 3+} emissions, with the most intense bands peaking at 525 nm ({sup 2}H{sub 11/2}→{sup 4}I{sub 15/2} transition) and 552 nm ({sup 4}S{sub 3/2}→{sup 4}I{sub 15/2}). The intensity of up-conversion emission from GdVO{sub 4}:Er{sup 3+}/Yb{sup 3+} is enhanced (by a factor of four) by co-doping with 5 mol% of Li{sup +} ions. The mechanisms responsible for this emission enhancement are discussed. - Graphical abstract: UC emission spectra for GdVO{sub 4}:1.5-mol% Er{sup 3+}/20-mol% Yb{sup 3+} powders co-doped with different concentrations of Li{sup +} ions, recorded under 980-nm excitation. - Highlights: • 5-mol% Li{sup +} co-doped powders have 400% enhanced up-conversion emission intensity. • 15-mol% Li{sup +} co-doping produces 40% higher emission in down-conversion. • Li{sup +} co-doped powders have larger crystallite size and smaller lattice parameters.« less

Low temperature molten-salt synthesis of nanocrystalline cubic Sr{sub 2}SbMnO{sub 6}

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

Baral, Antara; Varma, K.B.R., E-mail: kbrvarma@mrc.iisc.ernet.i

2009-12-15

Sr{sub 2}SbMnO{sub 6} (SSM) powders were successfully synthesized at reasonably low temperatures via molten-salt synthesis (MSS) method using eutectic composition of 0.635 Li{sub 2}SO{sub 4}-0.365 Na{sub 2}SO{sub 4} (flux). High-temperature cubic phase SSM was stabilized at room temperature by calcining the as-synthesized powders at 900 deg. C/10 h. The phase formation and morphology of these powders were characterized via X-ray powder diffraction and scanning electron microscopy, respectively. The SSM phase formation associated with {approx}60 nm sized crystallites was also confirmed by transmission electron microscopy. The activation energy associated with the particle growth was found to be 95+-5 kJ mol{sup -1}.more » The dielectric constant of the tetragonal phase of the ceramic (fabricated using this cubic phase powder) with and without the flux (sulphates) has been monitored as a function of frequency (100 Hz-1 MHz) at room temperature. Internal barrier layer capacitance (IBLC) model was invoked to rationalize the dielectric properties. - Graphical abstract: The as synthesized powders of Sr{sub 2}SbMnO{sub 6} calcined at 900 deg. C/10 h yielded a cubic phase ({approx}60 nm sized crystallites). Centrosymmetric tetragonal (I4/mcm) phase was obtained by increasing the calcination temperature to 1000 deg. C. Display Omitted« less
Structural and optoelectronic studies on Ag-CdS quantum dots

NASA Astrophysics Data System (ADS)

Ibrahim Mohammed S., M.; Gubari, Ghamdan M. M.; Huse, Nanasaheb P.; Dive, Avinash S.; Sharma, Ramphal

2018-05-01

In the present study, we have successfully deposited CdS quantum dot thin films and Ag doped CdS on a glass slide by simple and economical chemical bath deposition at room temperature. The X-ray diffraction method analysis reveals that CdS thin films exhibit hexagonal structure when compared with standard JCPDS data. The estimated average crystallite size of the quantum dots and resulted in the least crystallite size of ˜9 nm. a comparison between the optical and electrical properties of the films before and after doping Ag was made through measuring and analyzing the curves for UV and I-V. From UV absorption spectra we observed that the samples exhibited a band edge near ˜400 nm with a slight deviation with the presence of excitonic peak for both CdS and Ag doped CdS. The presence of excitonic peak may be referred to the formation of quantum dots. The calculated band gap energy of thin films was found to be 3.45 eV and 3.15 eV for both CdS and Ag doped CdS thin films respectively, where the optical absorption spectra of Ag doped CdS nanoparticles also exhibit shift with respect to that of CdS quantum dots thin films. The photosensitive of CdS thin films show an increase in photocurrent when Ag doped CdS.
Evolution of the atomic order and valence state of rare-earth atoms and uranium in a new carbon-metal composite—diphthalocyanine pyrolysate C64H32N16 Me ( Me = Y, La, Ce, Eu, and U)

NASA Astrophysics Data System (ADS)

Sovestnov, A. E.; Kapustin, V. K.; Tikhonov, V. I.; Fomin, E. V.; Chernenkov, Yu. P.

2014-08-01

The structure of a metal-carbon composite formed by the pyrolysis of diphthalocyanine of some rare-earth elements (Y, La, Ce, Eu) and uranium in the temperature range T ann = 800-1700°C has been investigated for the first time by the methods of X-ray diffraction analysis and X-ray line shift. It has been shown that, in the general case, the studied pyrolysates consist of three phases. One phase corresponds to the structure of graphite. The second phase corresponds to nitrides, carbides, and oxides of basic metal elements with a crystallite size ranging from 5 to 100 nm. The third phase is amorphous or consisting of crystallites with a size of ˜1 nm. It has been found that all the basic elements (Y, La, Ce, Eu, U) and incorporated iodine atoms in the third phase are in a chemically bound state. The previously unobserved electronic configurations have been revealed for europium. The possibility of including not only atoms of elements forming diphthalocyanine but also other elements (for example, iodine) in the composite structure is of interest, in particular, for the creation of a thermally, chemically, and radiation resistant metal-carbon matrix for the radioactive waste storage.
Mössbauer and magnetic studies of surfactant mediated Ca-Mg doped ferrihydrite nanoparticles.

PubMed

Layek, Samar; Mohapatra, M; Anand, S; Verma, H C

2013-03-01

Ultrafine (2-5 nm) particles of amorphous Ca-Mg co-doped ferrihydrite have been synthesized by surfactant mediated co-precipitation method. The evolution of the amorphous ferrihydrite by Ca-Mg co-doping is quite different from our earlier investigations on individual doping of Ca and Mg. Amorphous phase of ferrihydrite for the present study has been confirmed by X-ray diffraction (XRD) and Mössbauer spectroscopy at room temperature and low temperatures (40 K and 20 K). Hematite nanoparticles with crystallite size about 8, 38 and 70 nm were obtained after annealing the as-prepared samples at 400, 600 and 800 degrees C respectively in air atmosphere. Superparamagnetism has been found in 8 nm sized hematite nanoparticles which has been confirmed from the magnetic hysteresis loop with zero remanent magnetization and coercive field and also from the superparamagnetic doublet of its room temperature Mössbauer spectrum. The magnetic properties of the 38 and 70 nm sized particles have been studied by room temperature magnetic hysteresis loop measurements and Mössbauer spectroscopy. The coercive field in these hematite nanoparticles increases with increasing particle size. Small amount of spinel MgFe2O4 phase has been detected in the 800 degrees C annealed sample.
Nanocrystalline (U0.5Ce0.5)O2±x solid solutions through citrate gel-combustion

NASA Astrophysics Data System (ADS)

Maji, D.; Ananthasivan, K.; Venkata Krishnan, R.; Balakrishnan, S.; Amirthapandian, S.; Joseph, Kitheri; Dasgupta, Arup

2018-04-01

Nanocrystalline powders of (U0.5Ce0.5)O2±x solid solutions were synthesized in bulk (100-200 g) through the citrate gel combustion. The fuel (citric acid) to oxidant (nitrate) mole ratio (R) was varied from 0.1 to 1.0. Two independent lots of the products obtained through the gel-combustion were calcined at 973 K in air and in a mixture of argon containing 8% H2 respectively. All these powders were characterized for their bulk density, X-ray crystallite size, specific surface area, size distribution of the particles, porosity as well as residual carbon. The morphology and microstructures of these powders were studied by using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) respectively. Nanocrystalline single phase fluorite solid solutions having a typical crystallite size of about (7-15 nm) were obtained. These powders were highly porous comprising cuboidal flaky agglomerates. The combustion mixture with an 'R' value of 0.25 was found to undergo volume combustion and was found to yield a product that was distinctly different. The systematic investigation on synthesis and characterization of nanocrystalline UCeO2 is reported for the first time.
Size dependent exchange bias in single-phase Zn0.3Ni0.7Fe2O4 ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Mohan, Rajendra; Ghosh, Mritunjoy Prasad; Mukherjee, Samrat

2018-07-01

We report the microstructural and magnetic characterization of single phase nanocrystalline partially inverted Zn0.3Ni0.7Fe2O4 mixed spinel ferrite. The samples were annealed at 200 °C, 400 °C, 600 °C, 800 °C and 1000 °C. X-ray diffraction results indicate phase purity of all the samples and application of Debye- Scherrer yielded a crystallite size variation from 5 nm to 33 nm for the different samples. Magnetic measurements have revealed the freezing of interfacial spins which were the cause of the large horizontal M-H loop shift causing large exchange bias with high anisotropy. The magnetic measurements show a hysteresis loop with high effective anisotropy constant due to highly magnetically disordered surface spin at 5 K.
Study on photocatalytic activity of nanosized Co0.3Zn0.7Fe2O4 synthesized by hydrothermal method

NASA Astrophysics Data System (ADS)

Mondal, R.; Sarkar, K.; Dey, S.; Bhattacharjee, S.; Ghosh, C. K.; Kumar, S.

2018-04-01

We have reported the photocatalytic activity of nanosized Co0.3Zn0.7Fe2O4 (CZM) synthesized by hydrothermal method. Powder x-ray diffraction (PXRD), field emission and transmission electron microscopic techniques have been employed for structural and microstructural characterization of the sample. The Rietveld refinement of the PXRD pattern of CZM reveals that the sample is a single phase spinel ferrite of F d 3 ¯m symmetry having crystallite size ˜ 20 nm. The average particle size is ˜ 23 nm. The photocatalytic study suggests that CZM can be suitably used as an efficient (rate constant and % degradation are 7.4×10-2 min-1, 95.76 % at 40 min, respectively), magnetically separable, recyclable photocatalyst for removal of Congo Red from its aqueous solution.
A closer look at 40Ar/39Ar systematics of illite, recoil, retention ages, total gas ages, and a new correction method

NASA Astrophysics Data System (ADS)

Fitz-Diaz, E.; Hall, C. M.; van der Pluijm, B.

2013-12-01

One of the fundamentals of 40Ar-39Ar systematics of illite considers the effects of 39Ar recoil (ejection of 39Ar from tiny illite crystallites during the nuclear reaction 39K(n,p)39Ar), for which sample vacuum encapsulation prior to irradiation has been used since the 1990's. This technique separately measures the fraction of recoiled 39Ar and the Ar (39Ar and 40Ar) retained within illite crystals as they degas during step heating in vacuum. Total-gas ages (TGA) are calculated by using both recoiled and retained argon, while retention ages (RA) only involve retained Ar. Observations in numerous natural examples have shown that TGA fit stratigraphic constraints of geological processes when the average illite crystallite thickness (ICT) is smaller than 10nm, and that RA better matches these constrains for larger ICTs. Illite crystals with ICT >50nm show total gas and retention ages within a few My and they are identical, within analytical error, when ICT exceeds 150nm. We propose a new age correction that takes into account the average ICT and corresponding recoil for a sample , with such corrected ages (XCA) lying between the TGA and RA end-member ages. We apply this correction to samples containing one generation of illite and it particularly affects illite populations formed in the anchizone, with typical ICT values between 10-40nm. We analyzed bentonitic samples (S1, S2 and S3) from sites in Cretaceous carbonates in the front of the Monterrey salient in northern Mexico. Four size fractions (<0.05, 0.05-0.2, 0.2-1 & 1-2 μm) were separated, analyzed with XRD and dated by Ar-Ar. XRD analysis provides mineralogic characterization, illite polytype quantification, and illite crystallite thickness (ICT) determination using half-height peak width (illite crystallinity) and the Scherrer equation. All samples contain illite as the main mineral phase, ICT values between 8-27nm, from fine to coarser grain size fractions. Ages show a range in TGA among the different size fractions of S1, S2 and S3, respectively: 46-49, 36-43 and 40-52 My) and RA (54-64, 47-52 and 53-54 My. XCA calculations produce tighter constrained ranges (53-57, 45.5-48.5 and 49-52 My) with an overall average 51.1Ma×3.9 My. In the ICT vs. apparent age plot, authigenic illite grains show a greater slope that is in general slightly positive for TGA, slightly negative for RA, but close to zero for XCA. In the ICT vs. XCA plot thinner crystallites shows more dispersion than thicker ones. In order to test if such dispersion in the age of the finer/thinner illite is due to a different formation history in each site or the result of retention capability, degassing spectra were modeled for site XCA averages and overall XCA average. The modeling shows that local site ages best match the measured spectra, instead of a single age for the combined sites. The closeness between experimental and artificial degassing patterns also supports the hypothesis that each sample preserves a single age population. All illite grains in these samples grew progressively during folding in a time window that is constrained by the three sites. Small and large grains represent the same population in each sample, representing progressive degrees of grain growth (Ostwald ripening).
Changes in the mechanism of heat transfer in passing from microparticles to nanoparticles

NASA Astrophysics Data System (ADS)

Shakhov, F. M.; Meilakhs, A. P.; Eidelman, E. D.

2016-03-01

On the basis of experimental data on thermal conduction and sound velocity in composites obtained by sintering detonation nanodiamonds with the crystallite size of 4-5 nm and diamond micropowders with a grain size of about 10 μm at a high pressure (5-7 GPa) and high temperature (1200-1800°C), mechanisms of heat transfer in such structures are suggested. These mechanisms are shown to be different in composites of micro- and nanoparticles. In composites of micrometer particles, the conventional macroscopic mechanism of phonon propagation is active. In composites with a grain size of a few nanometers, the main contribution comes from thermal resistance on grain boundaries.
[Raman spectrum of nano-graphite synthesized by explosive detonation].

PubMed

Wen, Chao; Li, Xun; Sun, De-Yu; Guan, Jin-Qing; Liu, Xiao-Xin; Lin, Ying-Rui; Tang, Shi-Ying; Zhou, Gang; Lin, Jun-De; Jin, Zhi-Hao

2005-01-01

The nano-graphite powder synthesized by the detonation of explosives with negative oxygen balance is a new powder material with potential applications. In this work, the preparation of nano-graphite powder in steel chamber by pure TNT (trinitrotoluene) explosives has been introduced. In the synthesis process, the protective gases in the steel chamber are N2, CO2 and Ar, and the pressure is 0.25-2 atm. Raman spectrum of the nano-graphite was measured. The characteristic Raman band assigned to sp2 of graphite has been observed at about 1 585 cm(-1) with half-peak width of 22 cm(-1). The peak shifted to a higher frequency by 5 cm(-1) compared with that of bulk graphite. The authors explain this blue shift phenomenon by size effect. The average size of nanographite from Raman measurement is 2.97-3.97 nm. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to measure the structure and particle size of the nano-graphite. The crystallite size of nano-graphite estimated from XRD andTEM are 2.58 nm (acid untreated) and 1.86 nm (acid treated) respectively, which is in accord with the results of the measurement approximately.
Phase analysis of ZrO2-SiO2 systems synthesized through Ball milling mechanical activations

NASA Astrophysics Data System (ADS)

Nurlaila, Rizka; Musyarofah, Muwwaqor, Nibras Fuadi; Triwikantoro, Kuswoyo, Anton; Pratapa, Suminar

2017-01-01

Zircon powders have been produced from raw materials of amorphous zirconia and amorphous silica powders obtained from natural zircon sand of Kalimantan Tengah, Indonesia. Synthesis process was started with the extraction of zircon powder to produce sodium silicate solution and pure zircon powder. The amorphous zirconia and silica powders were prepared by alkali fusion and co-precipitation techniques. The powders were mixed using a planetary ball mill, followed by a calcination of various holding time of 3, 10, and 15 h. Phase characterization was done using X-Ray Diffraction (XRD) technique and analysis of the diffraction data was carried out using Rietica and MAUD software. The identified phases after the calcination were zircon, tetragonal zirconia, and cristobalite. The highest zircon content was obtained in the sample calcinated for15 hours - reaching 99.66 %wt. Crystallite size analysis revealed that the samples calcinated for 3, 10, and 15 h exhibited zircon crystal size of 176 (1) nm, 191 (1) nm and 233 (1) nm respectively.
Influence of deposition temperature on WTiN coatings tribological performance

NASA Astrophysics Data System (ADS)

Londoño-Menjura, R. F.; Ospina, R.; Escobar, D.; Quintero, J. H.; Olaya, J. J.; Mello, A.; Restrepo-Parra, E.

2018-01-01

WTiN films were grown on silicon and stainless-steel substrates using the DC magnetron sputtering technique. The substrate temperature was varied taking values of 100 °C, 200 °C, 300 °C, and 400 °C. X-ray diffraction analysis allowed us to identify a rock salt-type face centered cubic (FCC) structure, with a lattice parameter of approximately 4.2 nm, a relatively low microstrain (deformations at microscopy level, between 4.7% and 6.7%), and a crystallite size of a few nanometers (11.6 nm-31.5 nm). The C1s, N1s, O1s, Ti2p, W4s, W4p, W4d and W4f narrow spectra were obtained using X-ray photoelectron spectroscopy (XPS) and depending on the substrate temperature, the deconvoluted spectra presented different binding energies. Grain sizes and roughness (approximately 4 nm) of films were determined using atomic force microscopy. Scratch and pin on disc tests were conducted, showing better performance of the film grown at 200 °C. This sample exhibited a lower roughness, coefficient of friction, and wear rate.
Adsorption of Pb2+ ions on novel ternary nanocomposite of tin, iron and titania

NASA Astrophysics Data System (ADS)

Rehman, Mahfooz ur; Rehman, Wajid; Waseem, Muhammad; Haq, Sirajul; Hussain Shah, Khizar; Kang, Peng

2018-02-01

In this study, ternary nanocomposite (TNC) was synthesized by microemulsion method by taking Sn, Ti and Fe in (1:1:1) molar ratio. The BET surface area and pore size were measured by nitrogen adsorption method. The morphological features of TNC like particle size, elemental percentage and crystallite size were studied by scanning electron microscopy (SEM), energy dispersive x-rays (EDX) and x-rays diffraction (XRD) respectively, whereas the surface functional groups were detected by Fourier Transform Infrared (FTIR) spectroscopy. The crystallite size was found to be 11 nm, calculated from FWHM of diffraction peak with relative intensity 100%. For the thermal stability of TNC, thermogravimetric analysis (TGA) was performed. Batch adsorption tests were used for the removal of Pb2+ ions from aqueous solutions. The maximum adsorption capacity in this study was found to be 79.56 mg g-1 at 40 °C which is promising than the values reported in the literature. Based on the regression coefficient (r 2), the adsorption data was found well fitted to the Langmuir as compared to Freundlich model. The exchange of a single proton with every Pb2+ ion was calculated. Thermodynamic parameters were indicative for the sorption process to be endothermic and spontaneous.
High throughput, high resolution enzymatic lithography process: effect of crystallite size, moisture, and enzyme concentration.

PubMed

Mao, Zhantong; Ganesh, Manoj; Bucaro, Michael; Smolianski, Igor; Gross, Richard A; Lyons, Alan M

2014-12-08

By bringing enzymes into contact with predefined regions of a surface, a polymer film can be selectively degraded to form desired patterns that find a variety of applications in biotechnology and electronics. This so-called "enzymatic lithography" is an environmentally friendly process as it does not require actinic radiation or synthetic chemicals to develop the patterns. A significant challenge to using enzymatic lithography has been the need to restrict the mobility of the enzyme in order to maintain control of feature sizes. Previous approaches have resulted in low throughput and were limited to polymer films only a few nanometers thick. In this paper, we demonstrate an enzymatic lithography system based on Candida antartica lipase B (CALB) and poly(ε-caprolactone) (PCL) that can resolve fine-scale features, (<1 μm across) in thick (0.1-2.0 μm) polymer films. A Polymer Pen Lithography (PPL) tool was developed to deposit an aqueous solution of CALB onto a spin-cast PCL film. Immobilization of the enzyme on the polymer surface was monitored using fluorescence microscopy by labeling CALB with FITC. The crystallite size in the PCL films was systematically varied; small crystallites resulted in significantly faster etch rates (20 nm/min) and the ability to resolve smaller features (as fine as 1 μm). The effect of printing conditions and relative humidity during incubation is also presented. Patterns formed in the PCL film were transferred to an underlying copper foil demonstrating a "Green" approach to the fabrication of printed circuit boards.
Synthesis and structural characterization of nano-hydroxyapatite biomaterials prepared by microwave processing

NASA Astrophysics Data System (ADS)

Ramli, Rosmamuhamadani; Arawi, Ainaa Zafirah Omar; Talari, Mahesh Kumar; Mahat, Mohd Muzamir; Jais, Umi Sarah

2012-07-01

Synthetic hydroxyapatite, (HA, Ca10(PO4)6(OH)2), is an attractive and widely utilized bio-ceramic material for orthopedic and dental implants because of its close resemblance of native tooth and bone crystal structure. Synthetic HA exhibits excellent osteoconductive properties. Osteoconductivity means the ability to provide the appropriate scaffold or template for bone formation. Calcium phosphate biomaterials [(HA), tri-calcium phosphate (TCP) and biphasic calcium phosphate (HA/TCP)] with appropriate three-dimensional geometry are able to bind and concentrate endogenous bone morphogenetic proteins in circulation, and may become osteoinductive and can be effective carriers of bone cell seeds. This HA can be used in bio-implants as well as drug delivery application due to the unique properties of HA. Biomaterials synthesized from the natural species like mussel shells have additional benefits such as high purity, less expensive and high bio compatibility. In this project, HA-nanoparticles of different crystallite size were prepared by microwave synthesis of precursors. High purity CaO was extracted from the natural mussel shells for the synthesis of nano HA. Dried nano HA powders were analyzed using X-Ray Diffraction (XRD) technique for the determination of crystal structure and impurity content. Scanning Electron Microscopic (SEM) investigation was employed for the morphological investigation of nano HA powders. From the results obtained, it was concluded that by altering the irradiation time, nano HA powders of different crystallite sizes and morphologies could be produced. Crystallite sizes calculated from the XRD patterns are found to be in the range of 10-55 nm depending on the irradiation time.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Manaf, A., E-mail: azwar@ui.ac.id; Fahmi, Agam Aidil; Yustanti, Erlina

This paper describes the particle size characterization of mechanically alloyed Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} prepared with the aid of a high-power ultrasonic destruction. Analytical-grade BaCO{sub 3}, TiO{sub 2} and SrCO{sub 3} with a purity greater than 99 wt.% were used as precursors for Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3}. The mechanically powders were respectively sintered at 1200 °C for 3 hours to form crystalline powders. This work is aimed at studying the effect of diameter ratio between reactor and transducer of a high power sonicator on the Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} andmore » Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} nanoparticles formation. The presence of a single phase of the two materials was confirmed by X-Ray Diffraction (XRD). The concentration of the particles in demineralized water was 3.0 g / 100 mL which become the object of 3 hours ultrasonic destruction subjected to the application of transducer in which the ratio between the diameter of the reactor and the transducer (D/d) was fixed at 1.4, 1.6 and 1.8 respectively. It was found that the mean particle size before the ultrasonic destruction was 538 nm for Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and 480 nm for Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3}. With D/d of 1.8, the mean particle size of the two materials was found to decrease drastically to 38 nm and 24 nm, respectively. These mean particle sizes were respectively comparable with that of the crystallite size of the particles derived using the Whole Powder Pattern Modelling (WPPM) from which the mean crystallite size of 22 nm for Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and 14 nm for Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} were obtained. It is then confirmed single nanocrystallite Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} particles were already achieved. We can conclude that the ultrasonic destruction to mechanically milled crystalline particles would be one of an effective way to produce nanoparticles.« less
Naturally occurring clay nanoparticles in Latosols of Brazil central region: detection and characterization

NASA Astrophysics Data System (ADS)

Dominika Dybowska, Agnieszka; Luciene Maltoni, Katia; Piella, Jordi; Najorka, Jens; Puntes, Victor; Valsami-Jones, Eugenia

2015-04-01

Stability and reactivity of minerals change as a particle size function, which makes mineral nanoparticles (defined here as <100 nm) fundamentally distinct from the larger size materials. Naturally occurring mineral nanoparticles contribute to many biogeochemical processes, however much remains to be learnt about these materials, their size dependent behavior and environmental significance. Advances in analytical, imaging and spectroscopic techniques made it now possible to study such particles; however we still have limited knowledge of their chemical, structural and morphological identity and reactivity, in particular in soils. The aim of this research was to characterize the naturally occurring nanoparticles in three soils from Brazil central region. The samples were collected in the A horizon, treated with H2O2 to remove organic material, dispersed in ultrasonic bath and wet sieved (53 µm) to remove the sand fraction. The clay fraction was collected by siphoning the supernatant, conditioned in 1000 ml cylinder, according to the Stock's law. This fraction was further processed by re-suspension in water, sonication and repeated centrifugation, to separate the fraction smaller than 100nm. This material, called here the soil "nanofraction", was analyzed using a range of techniques: 1) nanoparticle size/morphology and crystallinity with Transmission Electron Microscopy (TEM operateing in scanning (HAADF-STEM) and High Resolution (HRTEM) mode), 2) size distribution in water with Dynamic Light Scattering (DLS) and surface charge estimated from electrophoretic mobility measurements 3) crystal phase and crystallite size with X-ray Diffraction (XRD) 4) Chemical composition by quantitative analysis of elements (e.g., Si, Fe, Al, Ti) and their spatial distribution with HRTEM/EDS elemental mappings. The nanofraction had an average hydrodynamic particle diameter ranging from 83 to 92nm with a low polydispersity index of 0.13-0.17 and was found highly stable in aqueous suspension (no change in average particle size up to several months of storage). Particle surface charge (in water) ranged from -31mV to -34.5mV (pH = 5.7 - 6.2), this reflects the predominantly negative surface charge of kaolinites in soil environment effectively screening the positive charge of Fe oxides. Kaolinites appeared as single crystals (pseudo hexagonal platelets) while Fe oxides occurred mostly as micro-aggregates, with individual particles often not morphologically distinct with particle size <10nm. In addition, several anatase (TiO2) nanoparticles were also found. Both kaolinites and Fe oxides nanoparticles were crystalline, as evidenced from XRD measurements and HRTEM imaging. Distinction between different crystalline forms of Fe oxides (mainly hematite and goethite) was only possible with XRD, which revealed also subtle differences in mineralogical composition of the clay fraction (<2µm) and nanofraction (<100nm). The kaolinite's crystallite size (calculated from XRD data) was found to range 14-17nm in the nanofraction and 26-50nm in the clay fraction. For hematite, it was 13nm in the nanofraction and ranged from 21-30nm in the clay fraction. Such small particles can be expected to play an important role in soil sorption processes with implications on nutrient and contaminant cycling. Identification and understanding of the properties of naturally occurring nanoparticles in soils can therefore help soil scientists to better understand retention/mobilization of nutrients and pollutants in soils.
Phase identification and morphology study of hematite (Fe2O3) with sintering time varitions

NASA Astrophysics Data System (ADS)

Yazirin, Cepi; Puspitasari, Poppy; Sasongko, Muhammad Ilman Nur; Tsamroh, Dewi Izzatus; Risdanareni, Puput

2017-09-01

Iron oxide has been the interest of many studies due to its applications in various scientific and industrial fields including in environment, corrosion, soil science, and exhaust emissions. Iron oxide (Fe2O3) has potential applications in catalytic reactions in electronic devices such as semiconductors, paint formulations, and lithium rechargeable batteries. Fe2O3 can be synthesized through the process of stirring, decomposition of organic iron, sol-gel, combustion, and evaporating solvents. Most of the methods used involve several steps and take a long time. The aim of this research was to investigate the phase and morphology characterization of iron oxide (Fe2O3) powder with solvent ethylene glycol after being sintered for 1 hour, 2 hours and 3 hours. The characterization tools utilized were XRD, SEM-EDX, and FTIR. The results of XRD analysis showed that the Fe2O3 sintered for 1 hour had the smallest crystallite size with a diameter of 21.05 nm. In the XRD test, the beam of X-ray was shot directly at the grain being tested. The results of SEM analysis showed thatthe Fe2O3 sintered for 1 hour produced the best result due to its crystallite size of 12.36 nm and hada shape of homogeneous nanosphere; the duration of sintering indeed had a great influence on the grain size of iron oxide (Fe2O3). In addition, the results of the elemental composition analysis indicate that the longer the sintering process, the higher the concentration of O but the lower the Fe.
Effect of Temperature, Precursor Type and Dripping Time on the Crystallite Size of Nano ZnO Obtained by One-Pot Synthesis: 2 k Full Factorial Design Analysis.

PubMed

Machado, Morgana de Medeiros; Savi, Bruna Martinello; Perucchi, Mariana Borges; Benedetti, Alessandro; Oliveira, Luis Felipe Silva; Bernardin, Adriano Michael

2018-06-01

The aim of this work was to determine the effect of temperature, precursor and dripping time on the crystallite size of ZnO nanoparticles synthesized by controlled precipitation according a 2k full factorial design. ZnCl2, Zn(NO3)2 and NaOH were used as precursors. After synthesis, the nano crystalline powder was characterized by XRD (Cu Kα), UV-Vis, and HR-TEM. The nano ZnO particles presented a crystallite size between 210 and 260 Å (HR-TEM and XRD). The results show that the crystallite size depends on the type of precursor and temperature of synthesis, but not on the dripping time.
Thermal decomposition of wood: influence of wood components and cellulose crystallite size.

PubMed

Poletto, Matheus; Zattera, Ademir J; Forte, Maria M C; Santana, Ruth M C

2012-04-01

The influence of wood components and cellulose crystallinity on the thermal degradation behavior of different wood species has been investigated using thermogravimetry, chemical analysis and X-ray diffraction. Four wood samples, Pinus elliottii (PIE), Eucalyptus grandis (EUG), Mezilaurus itauba (ITA) and Dipteryx odorata (DIP) were used in this study. The results showed that higher extractives contents associated with lower crystallinity and lower cellulose crystallite size can accelerate the degradation process and reduce the wood thermal stability. On the other hand, the thermal decomposition of wood shifted to higher temperatures with increasing wood cellulose crystallinity and crystallite size. These results indicated that the cellulose crystallite size affects the thermal degradation temperature of wood species. Copyright © 2012. Published by Elsevier Ltd.

Synthesis of nano-forsterite powder by making use of natural silica sand

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

Nurbaiti, Upik, E-mail: upik-nurbaiti@mail.unnes.ac.id; Department of Physics, Faculty of Mathematics and Natural Sciences Semarang State University Jl. Raya Sekaran GunungPati, Semarang 50221; Suud, Fikriyatul Azizah

2016-02-08

Nano-forsterite powder with natural silica sand and magnesium powder as the raw materials have been succesfully synthesized. The silica sand was purified followed by a coprecipitation process to obtain colloidal silica. The magnesium powder was dissolved in a chloric acid solution to obtain MgCl{sub 2} solution. The nanoforsterite powder was synthesised using a sol-gel method which included the mixing the colloidal silica and the MgCl{sub 2} solution with various aging and filtering processes. The samples were dried at 100 °C using a hot plate and then the dried powders were calcinated at 900 °C for 2 hours. The samples weremore » characetised for their elements and phase compositions using X-ray Flourescence (XRF) and X-ray Diffraction (XRD) methods, respectively. The diffraction data were qualitatively analyzed using Match!2 software and quantitatively using Rietica software. The crystallite size was verified using Transmission Electron Microscopy (TEM). Results of XRD data analysis showed that the forsterite content reached up to 90.5% wt. The TEM average crystallite size was approximately 53(6) nm.« less
Nanomorphology Characteristics of Thermally Annealed Pre Encapsulated P3HT:PCBM Thin Films Using Atomic Force Microscopy

DTIC Science & Technology

2014-10-30

fib- rils aggregate in bundles with the fullerene as the anneal- ing temperature increases. This bundle formation or grain features could indicate a...the diffusion lengths of charge carriers (∼10 nm). Past work on these fullerene networks have shown that trap distribution in devices is broader for...aver- age distance between polymer and fullerene molecules. The size of crystallites perhaps reach an upper limit in the range of 150 "C; beyond this
Rietveld analysis of the cubic crystal structure of Na-stabilized zirconia

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

Fagherazzi, G.; Canton, P.; Benedetti, A.

Using x-ray Rietveld analysis the fcc (fluorite-type) structure of a Na-containing nanocrystalline zirconia powder (9.5 nm estimated of crystallite size) obtained by precipitation and subsequent calcination has been confirmed. The result shows that using conventional x-ray diffraction techniques the cubic crystallographic form of ZrO{sub 2} from the tetragonal one in nanosized powders. These conclusions are supported by the findings of independent Raman scattering experiments. {copyright} {ital 1997 Materials Research Society.}
Structural and spectroscopic study of mechanically synthesized SnO2 nanostructures

NASA Astrophysics Data System (ADS)

Vij, Ankush; Kumar, Ravi

2016-05-01

We report the single step synthesis of SnO2 nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO2 nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A1g Raman mode towards lower wave number, which is correlated with the nanostructure formation.
Synthesis, Surface Modification and Optical Properties of Thioglycolic Acid-Capped ZnS Quantum Dots for Starch Recognition at Ultralow Concentration

NASA Astrophysics Data System (ADS)

Tayebi, Mahnoush; Tavakkoli Yaraki, Mohammad; Ahmadieh, Mahnaz; Mogharei, Azadeh; Tahriri, Mohammadreza; Vashaee, Daryoosh; Tayebi, Lobat

2016-11-01

In this research, water-soluble thioglycolic acid-capped ZnS quantum dots (QDs) are synthesized by the chemical precipitation method. The prepared QDs are characterized using x-ray diffraction and transmission electron microscopy. Results revealed that ZnS QDs have a 2.73 nm crystallite size, cubic zinc blende structure, and spherical morphology with a diameter less than 10 nm. Photoluminescence (PL) spectroscopy is performed to determine the presence of low concentrations of starch. Four emission peaks are observed at 348 nm, 387 nm, 422 nm, and 486 nm and their intensities are quenched by increasing concentration of starch. PL intensity variations in the studied concentrations range (0-100 ppm) are best described by a Michaelis-Menten model. The Michaelis constant ( K m) for immobilized α-amylase in this system is about 101.07 ppm. This implies a great tendency for the enzyme to hydrolyze the starch as substrate. Finally, the limit of detection is found to be about 6.64 ppm.
Structure and morphology evolution of silica-modified pseudoboehmite aerogels during heat treatment

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

Pakharukova, V.P., E-mail: verapakh@catalysis.ru; Novosibirsk State University, Pirogova Street 2, 630090 Novosibirsk; Research and Educational Center for Energy Efficient Catalysis, Novosibirsk State University, Novosibirsk 630090

Silica-modified pseudoboehmite aerogels (0, 10, 20 at% of Si) were prepared by sol–gel method followed by supercritical drying. The phase transformations, changes in structure and morphology upon calcination were thoroughly investigated by advanced X-Ray diffraction (XRD) techniques and high-resolution transmission electron microscopy (HRTEM). Obtained pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. The silica dopant drastically enhanced the crystallite anisotropy. Thus, the aerogel with Al:Si atomic ratio of 9:1 consisted of the pseudoboehmite nanosheets with thickness of one unit cell (average dimensions of 14.0×1.2×14.5 nm). The specific nanostructure caused remarkable features of experimental XRD patterns, includingmore » anisotropic peak broadening and appearance of forbidden reflection. Direct simulation of XRD patterns with using the Debye Scattering Equation allowed the size and morphology of pseudoboehmite crystallites to be determined. The silica addition strongly delayed formation of γ-alumina and further phase transformations upon calcinaton. Thermal stability of alumina was suggested to be affected by the particle morphology inherited from the pseudoboehmite precursor. - Graphical abstract: Pseudoboehmite samples had specific nanostructure: ultrathin two-dimensional (2D) crystallites were loosely packed. - Highlights: • Silica-doped boehmites were prepared by sol–gel method with supercritical drying. • Ultrathin two-dimensional crystallites of pseudoboehmite were obtained. • Changes in structure and morphology upon calcination were studied. • Simulation of XRD patterns was performed with use of the Debye Scattering Equation. • Thermal stability of alumina depended on morphology inherited from pseudoboehmite.« less
A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy

PubMed Central

Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

2017-01-01

Objective: Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. Materials and Methods: The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. Results: The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70–55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 (d10), 3.025 (d50), and 6.712 (d90) μm and average surface area of 2.71 m2/g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed Tmax at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λmax), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn–Cl stretching. Conclusions: These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications. PMID:28405577
A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy.

PubMed

Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

2017-01-01

Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70-55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 ( d 10 ), 3.025 ( d 50 ), and 6.712 ( d 90 ) μm and average surface area of 2.71 m 2 /g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed T max at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λ max ), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn-Cl stretching. These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications.
Structural and optical properties of ITO and Cu doped ITO thin films

NASA Astrophysics Data System (ADS)

Chakraborty, Deepannita; Kaleemulla, S.; Rao, N. Madhusudhana; Subbaravamma, K.; Rao, G. Venugopal

2018-04-01

(In0.95Sn0.05)2O3 and (In0.90Cu0.05Sn0.05)2O3 thin films were coated onto glass substrate by electron beam evaporation technique. The structural and optical properties of ITO and Cu doped ITO thin films have been studied by X-ray diffractometer (XRD) and UV-Vis-NIR spectrophotometer. The crystallite size obtained for ITO and Cu doped ITO thin films was in the range of 24 nm to 22 nm. The optical band gap of 4 eV for ITO thin film sample has been observed. The optical band gap decreases to 3.85 eV by doping Cu in ITO.
Investigation on structural and optical properties of ZnO film prepared by simple wet chemical method

NASA Astrophysics Data System (ADS)

Sholehah, Amalia; Mulyadi, Rendi; Haryono, Didied; Muttakin, Imamul; Rusbana, Tb Bahtiar; Mardiyanto

2018-04-01

ZnO thin layer has a broad potential application in electronic and optoelectronic devices. In this study, vertically align ZnO layers were deposited on ITO glass using wet chemistry method. The seed layers were prepared using electrodeposition technique at 3°C. The growing process was carried out using chemical bath deposition at 90°C. To improve the structural properties, two different hydrothermal treatment variations were applied separately. From the experiment, it is shown that the hydrothermal process using N2 gas has given the best result, with average diameter, crystallite size, and band-gap energy of 68.83 nm; 56.37 nm; and 3.16 eV, respectively.
Structural, Morphological, Differential Scanning Calorimetric and Thermogravimetric Studies of Ball Milled Fe Doped Nanoscale La0.67Sr0.33MnO3 Manganite

NASA Astrophysics Data System (ADS)

Astik, Nidhi; Jha, Prafulla K.; Pratap, Arun

2018-03-01

The ball milling route has been used to produce the La0.67Sr0.33Mn0.85Fe0.15O3 (LSMFO) nanocrystalline sample from oxide precursors. The sample was characterized using x-ray diffraction (XRD), a scanning electron microscope (SEM), energy dispersive x-ray spectroscopy (EDAX), differential scanning calorimetry (DSC) and thermogravimetric (TGA) measurements. The x-ray diffraction confirms the phase purity of sample and shows that the sample crystallizes in the rhombohedral perovskite structure with a R-3c space group. The scanning electron micrograph shows the presence of well-faceted crystallites of LSMFO. The EDAX spectrum demonstrates the molar ratio of different elements of nanocrystalline LSMFO. Furthermore, the crystallite size using the Debye-Scherrer formula and William-Hall analysis has been found as 24 nm and 29 nm, respectively. Our results support the idea that a good quality nanocrystalline LSMFO sample can be obtained using the ball milling route. We also discuss the DSC and TGA curves and analyse the results in terms of phase transition, calcination temperature and activation barrier energies.
Influence of Ba/Fe mole ratios on magnetic properties, crystallite size and shifting of X-ray diffraction peaks of nanocrystalline BaFe12O19 powder, prepared by sol gel auto combu

NASA Astrophysics Data System (ADS)

Suastiyanti, Dwita; Sudarmaji, Arif; Soegijono, Bambang

2012-06-01

Barium hexaferrite BaFe12O19 (BFO) is of great importance as permanent magnets, particularly for magnetic recording as well as in microwave devices. Nano-crystalline BFO powders were prepared by sol gel auto combustion method in citric acid - metal nitrates system. Hence the mole ratios of Ba/Fe were variated at 1:12; 1:11.5 and 1:11. Ratio of cation to fuel was fixed at 1:1. An appropriate amount of amonia solution was added dropwise to this solution with constant stirring until the PH reached 7 in all cases. Heating at 850oC for 10 hours for each sample to get final formation of BFO nanocrystalline. The data from XRD showing the lattice parameters a,c and the unit-cell volume V, confirm that BFO with ratio 1:12 has same crystall parameters with ratio 1:11. Ratio of Ba/Fe 1:12 and 1:11 have diffraction pattern similarly at almost each 2 θ for each samples. Ratio of Ba/Fe 1: 11.5 has the finest crystallite size 22 nm. Almost diffraction pattern peaks of Ba/Fe 1:11.5 move to the left from of Ba/Fe 1:12 then return to diffraction pattern of Ba/Fe 1:12 for Ba/Fe 1:11. SEM observations show the particle size less than 100 nm and the same shape for each sample. Ratio of Ba/Fe 1: 12 gives the highest intrinsic coercive Hc = 427.3 kA/m. The highest remanent magnetization is at ratio 1:11 with Mr = 0.170 T. BFO with mole ratio 1:11.5 has the finest grain 22 nm, good magnetic properties and the highest value of best FoM 89%.
Ion irradiation induced nucleation and growth of nanoparticles in amorphous silicon carbide at elevated temperatures

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

Zhang, Limin; Jiang, Weilin; Ai, Wensi

Ion irradiation induced crystallization in as-deposited amorphous SiC films is investigated using grazing-angle incidence x-ray diffraction (GIXRD), transmission electron microscopy (TEM) and Raman spectroscopy. Irradiation with 5 MeV Xe to fluence of 115 Xe/nm2 at 700 K results in a homogenous distribution of 3C-SiC grains with an average crystallite size of ~5.7 nm over the entire film thickness (~1 μm). The nucleation and growth processes exhibit a weak dependence on dose in displacements per atom (dpa) in the dose range from 6 to 20 dpa. A transformation of homonuclear C-C bonds from sp3 to sp2 hybridization is observed in themore » irradiated films, which may be partly responsible for the observed grain size saturation. The results from this study may have a significant impact on synthesis of nanograins in amorphous SiC and other similar materials with effective control of grain size and density by ion irradiation.« less
Synchrotron X-ray characterization of mackinawite and uraninite relevant to bio-remediation of groundwater contaminated with uranium

NASA Astrophysics Data System (ADS)

Carpenter, J.; Hyun, S.; Hayes, K. F.

2010-12-01

Uranium (U) originating from mining operations for weapon manufacturing and nuclear energy production is a significant radionuclide contaminant in groundwater local to uranium mining, uranium milling, and uranium mill tailing (UMT) storage sites. In the USA, the Department of Energy (DOE) is currently overseeing approximately 24 Uranium Mill Tailing Remediation Action (UMTRA) sites which have collectively processed over 27 million tons of uranium ore1,2. In-Situ microbial bio-reduction of the highly mobile U6+ ion into the dramatically less mobile U4+ ion has been demonstrated as an effective remedial process to inhibit uranium migration in the aqueous phase3. The resistance of this process to oxidization and possible remobilization of U when bioremediation stops (and oxidants such as oxygen from the air or nitrate in water diffuse into the formation) in the long term is not known. UMTRA site studies3 have shown that iron sulfide solids are produced by sulfate reducing bacteria (SRB) during U bioremediation, and some forms of these iron sulfide solids are known to be effective oxidant scavengers, potentially protecting against re-oxidation and thus remobilization of U. This work is investigating the role of iron sulfide solids in the long-term immobilization of reduced U compounds after bioremediation is completed in groundwater local to UMTRA sites. Re-oxidation tests are being performed in packed media columns loaded with both FeS and U solids. High quality mackinawite (FeS), and uraninite (UO2) have been synthesized in our laboratory via a wet chemistry approach. These synthetic materials are expected to mimic the naturally occurring and biogenic materials present in biologically stimulated UMTRA sites. In order to establish the initial conditions of the prepared experimental columns and to compare synthetic and biogenic FeS and UO2, these synthesized materials have been characterized with synchrotron radiation at the Stanford Synchrotron Radiation Lightsource using synchrotron x-ray powder diffraction (SXRD) and extended x-ray absorption fine structure (EXAFS). SXRD data were collected and analyzed with profile fitting to determine lattice parameters and crystallite size for comparison with published values for both biogenic and synthetic materials. This is particularly of interest for UO2, as there is very little information on particle size and lattice parameters for synthetic UO2 in the literature. Profile fitting of the SXRD data for FeS gives lattice parameters of a = b = 3.668 and a mean crystallite size of 5 to 8 nm. Both of these values are in good agreement with published values. For fresh UO2, lattice parameters were determined as a = b = c = 5.4 nm for both freshly synthesized and aged (3 months) UO2 and particle size was determined to be 3.5 nm for fresh UO2 and 5.83 nm for aged UO2. This suggests a growth mechanism for crystallites over time, and an inferred decrease in reactivity.
Quaternary M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4} (M = Ni, Zn, Co, Mn) ferrite oxides: Synthesis, characterization and magnetic properties

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

Ciocarlan, Radu George; Laboratory of Adsorption and Catalysis, Department of Chemistry, University of Antwerpen; Pui, Aurel, E-mail: aurel@uaic.ro

2016-09-15

Highlights: • Superparamagnetic quaternary nanoferrite (M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4,} where M = Mn, Zn, Co, Ni) were obtained. • C, O, H and metals were observed by XPS analysis. • Phases purity were confirmed by XRD diffraction and crystallite size (3–10 nm) were determind. - Abstract: We report the synthesis of M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4} (where M = Mn, Zn, Co, Ni) nanoparticles using the coprecipitation method in the presence of carboxymethyl cellulose (CMC) as the in-situ surfactant. The crystalline structure and surface morphology were examined by means of X-ray diffraction (XRD) and scanning electron microscopymore » (SEM) and it was established that the average diameter of the magnetic nanoparticles (MNPs) is in the range of 3–10 nm. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) show that the MNPs are activated by the hydrophilic groups of the surfactant, which coat them and enhance their stability. The vibrating sample magnetometry measurements show the superparamagnetic behavior of the nanoparticles. Due to their small crystallite size, which implies large surface area, and their functionalization with organic groups, the obtained nanoparticles could have medical and catalytic applications.« less
Elucidation of structural, vibrational and dielectric properties of transition metal (Co2+) doped spinel Mg-Zn chromites

NASA Astrophysics Data System (ADS)

Choudhary, Pankaj; Varshney, Dinesh

2018-05-01

Co2+ doped Mg-Zn spinel chromite compositions Mg0.5Zn0.5-xCoxCr2O4 (0.0 ≤ x ≤ 0.5) have been synthesized by the high-temperature solid state method. Synchrotron and X-ray diffraction (XRD) studies show single-phase crystalline nature. The structural analysis is validated by Rietveld refinement confirms the cubic structure with space group Fd3m. Crystallite size is estimated from Synchrotron XRD which was found to be 30-34 nm. Energy dispersive analysis confirms stoichiometric Mg0.5Zn0.5-xCoxCr2O4 composition. Average crystallite size distribution is estimated from imaging software (Image - J) of SEM is in the range of 100-250 nm. Raman spectroscopy reveals four active phonon modes, and a pronounced red shift is due to enhanced Co2+ concentration. Increased Co2+ concentration in Mg-Zn chromites shows a prominent narrowing of band gap from 3.46 to 2.97 eV. The dielectric response is attributed to the interfacial polarization, and the electrical modulus study supports non-Debye type of dielectric relaxation. Ohmic junctions (minimum potential drop) at electrode interface are active at lower levels of doping (x < 0.2) give rise to a low-frequency semicircle as evidenced from the complex impedance analysis. The low dielectric loss and high ac conductivity of Co2+ doped Mg-Zn spinel chromites are suitable for power transformer applications at high frequencies.
Optical absorption and photoluminescence studies of gold nanoparticles deposited on porous silicon

PubMed Central

2013-01-01

We present an investigation on a coupled system consists of gold nanoparticles and silicon nanocrystals. Gold nanoparticles (AuNPs) embedded into porous silicon (PSi) were prepared using the electrochemical deposition method. Scanning electron microscope images and energy-dispersive X-ray results indicated that the growth of AuNPs on PSi varies with current density. X-ray diffraction analysis showed the presence of cubic gold phases with crystallite sizes around 40 to 58 nm. Size dependence on the plasmon absorption was studied from nanoparticles with various sizes. Comparison with the reference sample, PSi without AuNP deposition, showed a significant blueshift with decreasing AuNP size which was explained in terms of optical coupling between PSi and AuNPs within the pores featuring localized plasmon resonances. PMID:23331761
Nanostructures of Indium Gallium Nitride Crystals Grown on Carbon Nanotubes.

PubMed

Park, Ji-Yeon; Man Song, Keun; Min, Yo-Sep; Choi, Chel-Jong; Seok Kim, Yoon; Lee, Sung-Nam

2015-11-16

Nanostructure (NS) InGaN crystals were grown on carbon nanotubes (CNTs) using metalorganic chemical vapor deposition. The NS-InGaN crystals, grown on a ~5-μm-long CNT/Si template, were estimated to be ~100-270 nm in size. Transmission electron microscope examinations revealed that single-crystalline InGaN NSs were formed with different crystal facets. The observed green (~500 nm) cathodoluminescence (CL) emission was consistent with the surface image of the NS-InGaN crystallites, indicating excellent optical properties of the InGaN NSs on CNTs. Moreover, the CL spectrum of InGaN NSs showed a broad emission band from 490 to 600 nm. Based on these results, we believe that InGaN NSs grown on CNTs could aid in overcoming the green gap in LED technologies.
Application of back-propagation artificial neural network (ANN) to predict crystallite size and band gap energy of ZnO quantum dots

NASA Astrophysics Data System (ADS)

Pelicano, Christian Mark; Rapadas, Nick; Cagatan, Gerard; Magdaluyo, Eduardo

2017-12-01

Herein, the crystallite size and band gap energy of zinc oxide (ZnO) quantum dots were predicted using artificial neural network (ANN). Three input factors including reagent ratio, growth time, and growth temperature were examined with respect to crystallite size and band gap energy as response factors. The generated results from neural network model were then compared with the experimental results. Experimental crystallite size and band gap energy of ZnO quantum dots were measured from TEM images and absorbance spectra, respectively. The Levenberg-Marquardt (LM) algorithm was used as the learning algorithm for the ANN model. The performance of the ANN model was then assessed through mean square error (MSE) and regression values. Based on the results, the ANN modelling results are in good agreement with the experimental data.
Effects of alcohol solvents on anatase TiO2 nanocrystals prepared by microwave-assisted solvothermal method

NASA Astrophysics Data System (ADS)

Wu, Yu-Chun; Tai, Yu-Chuen

2013-06-01

The effects of solvents on the anatase crystallite size prepared by sol-gel microwave-assisted solvothermal method were investigated in this study. Eight different alcohol solvents classified into two groups, i.e. primary and secondary/ternary alcohols, were used as reaction media and the effects of solvent properties, such as dielectric constant, boiling point, and internal pressure during the solvothermal process, on the crystallite size and shape were analyzed. According to the experimental results, selecting the solvent type allowed not only the alteration of the crystallite size but also the crystallite shape without the need of any additives. The boiling point of solvent was determined as the major factor influencing the crystallite size. Among the solvents with similar boiling points, the solvent with a higher carbon number produced the smaller crystallite size because of steric hindrance effect. In addition, the carboxyl groups dissociated from the alcohol solvent can play a role as a structural capping agent to retard the anatase crystal growth along the [001] direction and led to a rectangular crystallite shape with preferred development in {001} facets. On the other hand, the alcoholysis reaction was found easily occurred between the primary alcohol and isopropoxide that effectively limited the hydrolysis and condensation processes but also suppressed the structural capping effect. Therefore, the anatase crystals prepared in the primary alcohols became exceptionally small and showed spherical shape. Finally, the anatase crystals prepared using isopropanol demonstrated the highest photocatalytic activity due to its evident preferred crystallization in the {001} facets.

Time dependent rise and decay of photocurrent in zinc oxide nanoparticles in ambient and vacuum medium

NASA Astrophysics Data System (ADS)

C, Rajkumar; Srivastava, Rajneesh K.

2018-05-01

Zinc oxide (ZnO) nanoparticle has been synthesized by cost effective Co-precipitation method and studied its photo-response activity. The synthesized ZnO nanomaterial was characterized by using various analytical techniques such as x-ray diffraction (XRD), UV–visible spectroscopy, FTIR spectroscopy, photoluminescence (PL) spectroscopy, and Scanning Electron Microscopy (SEM). From the XRD results, it is confirmed that synthesized ZnO nanomaterial possess hexagonal wurtzite phase structure with an average crystallite size of ∼16–17 nm. The UV-Visible absorption spectrum shows that it has blue shift compared to their bulk counterparts. Photoluminescence spectra of ZnO nanoparticles have a strong violet band at 423 nm and three weak bands at 485 nm (blue), 506 nm (green), and 529 nm (green). The presence of hydroxyl group was confirmed by FTIR. The photo-response analysis was studied by the time-dependent rise and decay photocurrent of ZnO nanoparticle was tested in the air as well as vacuum medium.
Size distribution of magnetic iron oxide nanoparticles using Warren-Averbach XRD analysis

NASA Astrophysics Data System (ADS)

Mahadevan, S.; Behera, S. P.; Gnanaprakash, G.; Jayakumar, T.; Philip, J.; Rao, B. P. C.

2012-07-01

We use the Fourier transform based Warren-Averbach (WA) analysis to separate the contributions of X-ray diffraction (XRD) profile broadening due to crystallite size and microstrain for magnetic iron oxide nanoparticles. The profile shape of the column length distribution, obtained from WA analysis, is used to analyze the shape of the magnetic iron oxide nanoparticles. From the column length distribution, the crystallite size and its distribution are estimated for these nanoparticles which are compared with size distribution obtained from dynamic light scattering measurements. The crystallite size and size distribution of crystallites obtained from WA analysis are explained based on the experimental parameters employed in preparation of these magnetic iron oxide nanoparticles. The variation of volume weighted diameter (Dv, from WA analysis) with saturation magnetization (Ms) fits well to a core shell model wherein it is known that Ms=Mbulk(1-6g/Dv) with Mbulk as bulk magnetization of iron oxide and g as magnetic shell disorder thickness.
Characterization of nanostructured VO2 thin films grown by magnetron controlled sputtering deposition and post annealing method.

PubMed

Chen, Sihai; Lai, Jianjun; Dai, Jun; Ma, Hong; Wang, Hongchen; Yi, Xinjian

2009-12-21

By magnetron controlled sputtering system, a new nanostructured metastable monoclinic phase VO2 (B) thin film has been fabricated. The testing result shows that this nanostructured VO2 (B) thin film has high temperature coefficient of resistance (TCR) of -7%/K. Scanning electron microscopy measurement shows that the average grain diameter of the VO2 (B) crystallite is between 100 and 250 nm. After post annealed, VO2 (B) crystallite is changed into monoclinic (M) phase VO2 (M) crystallite with the average grain diameter between 20 and 50 nm. A set up of testing the thin film switching time is established. The test result shows the switching time is about 50 ms. With the nanostructured VO2 (B) and VO2 (M) thin films, optical switches and high sensitivity detectors will be presented.
Effect of magnetic anisotropy and particle size distribution on temperature dependent magnetic hyperthermia in Fe3O4 ferrofluids

NASA Astrophysics Data System (ADS)

Palihawadana Arachchige, Maheshika; Nemala, Humeshkar; Naik, Vaman; Naik, Ratna

Magnetic hyperthermia (MHT) has a great potential as a non-invasive cancer therapy technique. Specific absorption rate (SAR) which measures the efficiency of heat generation, mainly depends on magnetic properties of nanoparticles such as saturation magnetization (Ms) and magnetic anisotropy (K) which depend on the size and shape. Therefore, MHT applications of magnetic nanoparticles often require a controllable synthesis to achieve desirable magnetic properties. We have synthesized Fe3O4 nanoparticles using two different methods, co-precipitation (CP) and hydrothermal (HT) techniques to produce similar XRD crystallite size of 12 nm, and subsequently coated with dextran to prepare ferrofluids for MHT. However, TEM measurements show average particle sizes of 13.8 +/-3.6 nm and 14.6 +/-3.6 nm for HT and CP samples, implying the existence of an amorphous surface layer for both. The MHT data show the two samples have very different SAR values of 110 W/g (CP) and 40W/g (HT) at room temperature, although they have similar Ms of 70 +/-4 emu/g regardless of their different TEM sizes. We fitted the temperature dependent SAR using linear response theory to explain the observed results. CP sample shows a larger magnetic core with a narrow size distribution and a higher K value compared to that of HT sample.
Structure and mechanical properties of foils made of nanocrystalline beryllium

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

Zhigalina, O. M., E-mail: zhigal@ns.crys.ras.ru; Semenov, A. A.; Zabrodin, A. V.

2016-07-15

The phase composition and structural features of (45–90)-μm-thick foils obtained from nanocrystalline beryllium during multistep thermomechanical treatment have been established using electron microscopy, electron diffraction, electron backscattering diffraction, and energy-dispersive analysis. This treatment is shown to lead to the formation of a structure with micrometer- and submicrometer-sized grains. The minimum average size of beryllium grains is 352 nm. The inclusions of beryllium oxide (BeO) of different modifications with tetragonal (sp. gr. P4{sub 2}/mnm) and hexagonal (sp. gr. P6{sub 3}/mmc) lattices are partly ground during deformation to a size smaller than 100 nm and are located along beryllium grain boundaries inmore » their volume, significantly hindering migration during treatment. The revealed structural features of foils with submicrometer-sized crystallites provide the thermal stability of their structural state. Beryllium with this structure is a promising material for X-ray instrument engineering and for the production of ultrathin (less than 10 μm) vacuum-dense foils with very high physicomechanical characteristics.« less
Magnetic properties of Mn0.1Mg0.2TM0.7Fe2O4 (TM = Zn, Co, or Ni) prepared by hydrothermal processes: The effects of crystal size and chemical composition

NASA Astrophysics Data System (ADS)

Nhlapo, T. A.; Msomi, J. Z.; Moyo, T.

2018-02-01

Nano-crystalline Zn-, Co-, and Ni-substituted Mn-Mg ferrites were prepared by hydrothermal process and annealed at 1100 °C. Annealing conditions are critical on the crystalline phase. TEM and XRD data reveal particle sizes between 8 nm and 15 nm for the as-prepared fine powders, which increase to about 73 nm after sintering at 1100 °C. Mӧssbauer spectra show well resolved magnetic splitting in bulk samples. The as-prepared fine powders show weak hyperfine splitting and broad central doublets associated with fine particles. Magnetization data reveal a high coercive field at about 300 K of about 945 Oe in the Co-based nanosized oxide, which reduces to about 360 Oe after thermal annealing at 1100 °C. The magnetization curves of Zn- and Ni-based samples show much lower coercive fields indicative of superparamagnetic nanoparticles. The crystallite size and chemical composition have significant effects on the properties of Mn0.1Mg0.2(Zn,Co,Ni)0.7Fe2O4 investigated.
Structure and optical properties of ZnO with silver nanoparticles

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

Lyadov, N. M., E-mail: nik061287@mail.ru; Gumarov, A. I.; Kashapov, R. N.

Textured nanocrystalline ZnO thin films are synthesized by ion beam assisted deposition. According to X-ray diffraction data, the crystallite size is ∼25 nm. Thin (∼15 nm) ZnO layers containing Ag nanoparticles are formed in a thin surface region of the films by the implantation of Ag ions with an energy of 30 keV and a dose in the range (0.25–1) × 10{sup 17} ion/cm{sup 2}. The structure and optical properties of the layers are studied. Histograms of the size distribution of Ag nanoparticles are obtained. The average size of the Ag nanoparticles varies from 0.5 to 1.5–2 nm depending onmore » the Ag-ion implantation dose. The optical transmittance of the samples in the visible and ultraviolet regions increases, as the implantation dose is increased. The spectra of the absorption coefficient of the implanted films are calculated in the context of the (absorbing film)/(transparent substrate) model. It is found that the main changes in the optical-density spectra occur in the region of ∼380 nm, in which the major contribution to absorption is made by Ag nanoparticles smaller than 0.75 nm in diameter. In this spectral region, absorption gradually decreases, as the Ag-ion irradiation dose is increased. This is attributed to an increase in the average size of the Ag nanoparticles. It is established that the broad surface-plasmon-resonance absorption bands typical of nanocomposite ZnO films with Ag nanoparticles synthesized by ion implantation are defined by the fact that the size of the nanoparticles formed does not exceed 1.5–2 nm.« less
Further Improvement of the RITS Code for Pulsed Neutron Bragg-edge Transmission Imaging

NASA Astrophysics Data System (ADS)

Sato, H.; Watanabe, K.; Kiyokawa, K.; Kiyanagi, R.; Hara, K. Y.; Kamiyama, T.; Furusaka, M.; Shinohara, T.; Kiyanagi, Y.

The RITS code is a unique and powerful tool for a whole Bragg-edge transmission spectrum fitting analysis. However, it has had two major problems. Therefore, we have proposed methods to overcome these problems. The first issue is the difference in the crystallite size values between the diffraction and the Bragg-edge analyses. We found the reason was a different definition of the crystal structure factor. It affects the crystallite size because the crystallite size is deduced from the primary extinction effect which depends on the crystal structure factor. As a result of algorithm change, crystallite sizes obtained by RITS drastically approached to crystallite sizes obtained by Rietveld analyses of diffraction data; from 155% to 110%. The second issue is correction of the effect of background neutrons scattered from a specimen. Through neutron transport simulation studies, we found that the background components consist of forward Bragg scattering, double backward Bragg scattering, and thermal diffuse scattering. RITS with the background correction function which was developed through the simulation studies could well reconstruct various simulated and experimental transmission spectra, but refined crystalline microstructural parameters were often distorted. Finally, it was recommended to reduce the background by improving experimental conditions.
Preparation and characterization of nanocrystalline CuO powders with the different surfactants and complexing agent mediated precipitation method

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

Rajendran, V.; Gajendiran, J., E-mail: gaja.nanotech@gmail.com

2014-08-15

Highlights: • CuO nanostructures by surfactants mediated method. • Structural and optical properties of CuO nanostructures changes under the effect of surface modifier. • Citric acid assisted is the best, in terms of size, morphology and optical properties than that of CTAB, SDS and PEG-400. - Abstract: Nanostructures of copper oxide (CuO) was synthesized into crystallite sized ranging from 20 to 50 nm in the presence of different surfactants, and complex agent such as cityl tri methyl ammonium bromide (CTAB), sodium do decyl sulfate (SDS), poly ethylene glycol (PEG-400) and citric acid via a precipitation route. Variations in several parametersmore » and their effects on the structural and optical properties of CuO nanostructures (crystallite size, morphology and band gap) were investigated by XRD, FTIR, SEM and UV analysis. The UV–visible absorption spectra of the different surfactants and complexing agent assisted CuO nanostructures indicates that the estimated optical band gap energy value (1.94–1.98 eV) is higher than that of the bulk CuO value (1.4 eV), which is attributed to the quantum confinement effect. The formation mechanism of different surfactants and complexing agent assisted CuO nanostructures is also proposed.« less
Fabrication of mesoporous silica nanoparticles by sol gel method followed various hydrothermal temperature

NASA Astrophysics Data System (ADS)

Purwaningsih, Hariyati; Pratiwi, Vania Mitha; Purwana, Siti Annisa Bani; Nurdiansyah, Haniffudin; Rahmawati, Yenny; Susanti, Diah

2018-04-01

Rice husk is an agricultural waste that is potentially used as natural silica resources. Natural silica claimed to be safe in handling, cheap and can be generate from cheap resource. In this study mesoporous silica was synthesized using sodium silicate extracted from rice husk ash. This research's aim are to study the optimization of silica extraction from rice husk, characterizing mesoporous silica from sol-gel method and surfactant templating from rice husk and the effect of hydrothermal temperature on mesoporous silica nanoparticle (MSNp) formation. In this research, rice husk was extracted with sol-gel method and was followed by hydrothermal treatment; several of hydrothermal temperatures were 85°C, 100°C, 115°C, 130°C and 145° for 24 hours. X-ray diffraction analysis was identified of α-SiO2 phase and NaCl compound impurities. Scherer's analysis method for crystallite size have resulted 6.27-40.3 nm. FTIR results of silica from extraction and MSNp indicated Si-O-Si bonds on the sample. SEM result showed the morphology of the sample that has spherical shape and smooth surface. TEM result showed particle size ranged between 69,69-84,42 nm. BET showed that the pore size classified as mesoporous with pore diameter size is 19,29 nm.
Influence of Mg and Ni substitution on structural, microstructural and magnetic properties of Sr2Co2-xMgx/2Nix/2Fe12O22 (Co2Y) hexaferrite

NASA Astrophysics Data System (ADS)

Alizad Farzin, Y.; Mirzaee, O.; Ghasemi, A.

2014-12-01

In this study, Mg and Ni substituted Y-type hexaferrite particles with narrow size distribution have been prepared by using a sol-gel auto combustion method. The effects on structural, microstructure and magnetic properties have been investigated by substituting Mg2+ and Ni2+ at Co2+ sites. XRD patterns showed that Y-type hexaferrite phase formation has not been affected by substituting magnesium and nickel with cobalt in the range of 0.0≤x≤0.75. Various parameters such as lattice constants, cell volume and crystallite size have been calculated based on XRD data. The morphology and size distribution of the particles have been studied using high resolution field emission scanning electron microscopy (FESEM). It was also understood that the average crystallite size of particles increased from 45 to 63 nm with an increase of x content at Co2Y compound. Magnetic properties were determined using a vibrating sample magnetometer (VSM). The magnetic results revealed that by increasing the Mg and Ni in octahedral and tetrahedral sites, the coercivity was also increased from 949 to 1066 Oe, whereas saturation magnetization and Remnant magnetization were decreased from 47.98 to 40.78 emu/g and 23.05 to 20.99 emu/g, respectively.
Gas sensing performance of nano zinc oxide sensors

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

Sharma, Shiva, E-mail: shivasharmaau@gmail.com; Chauhan, Pratima, E-mail: mangu167@yahoo.co.in

We report nano Zinc Oxide (ZnO) synthesized by sol-gel method possessing the crystallite size which varies from 25.17 nm to 47.27 nm. The Scanning electron microscope (SEM) image confirms the uniform distribution of nanograins with high porosity. The Energy dispersion X-ray (EDAX) spectrum gives the atomic composition of Zn and O in ZnO powders and confirms the formation of nano ZnO particles. These factors reveals that Nano ZnO based gas sensors are highly sensitive to Ammonia gas (NH{sub 3}) at room temperature, indicating the maximum response 86.8% at 800 ppm with fast response time and recovery time of 36 sec and 23 secmore » respectively.« less
Preparation of silver nanoparticles at low temperature

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

Mishra, Mini, E-mail: mishramini5@gmail.com; Chauhan, Pratima, E-mail: mangu167@yahoo.co.in

Silver from ancient time is used as antimicrobial agent in the bulk form but now with the advancement in nanotechnology silver in the form of nanoparticles shown potential effect against microbes which make us easy to fight with many diseases plants and animals. In this work silver nanoparticles were synthesized by chemical routes using sodium borohydride as reducing agent at low temperature. The particles were characterized through UV-Visible spectroscopy as well as X-Ray Diffraction. The UV-visible spectra of silver nanoparticles exhibited absorption at 425 cm; the crystallite size of the particles is between 19nm to 39nm. EDAX graph shows two peaksmore » of silver and oxygen. Water absorbed by silver nanoparticles was removed by the calcinations.« less
Synthetic control of manganese birnessite: Impact of crystallite size on Li, Na, and Mg based electrochemistry

DOE PAGES

Yin, Jiefu; Takeuchi, Esther S.; Takeuchi, Kenneth J.; ...

2016-08-12

We demonstrated the synthesis and characterization of Mg-birnessite (Mg xMnO 2) with different crystallite sizes, prepared though low temperature precipitation and ion exchange. The influence of crystallite size on electrochemical performance of Mg-birnessite was studied for the first time, where material with smaller crystallite size was demonstrated to have enhanced capacity and rate capability in Li ion, Na ion, and Mg ion based electrolytes. Cation diffusion using GITT type testing demonstrated the ion diffusion coefficient of Mg 2+ was ~10× lower compared with Li + and Na +. This work illustrates that tuning of inorganic materials properties can lead tomore » significant enhancement of electrochemical performance in lithium, sodium as well as magnesium based batteries for materials such as Mg-birnessite and provides a deliberate approach to improve electrochemical performance.« less
Role of stacking disorder in ice nucleation

NASA Astrophysics Data System (ADS)

Lupi, Laura; Hudait, Arpa; Peters, Baron; Grünwald, Michael; Gotchy Mullen, Ryan; Nguyen, Andrew H.; Molinero, Valeria

2017-11-01

The freezing of water affects the processes that determine Earth’s climate. Therefore, accurate weather and climate forecasts hinge on good predictions of ice nucleation rates. Such rate predictions are based on extrapolations using classical nucleation theory, which assumes that the structure of nanometre-sized ice crystallites corresponds to that of hexagonal ice, the thermodynamically stable form of bulk ice. However, simulations with various water models find that ice nucleated and grown under atmospheric temperatures is at all sizes stacking-disordered, consisting of random sequences of cubic and hexagonal ice layers. This implies that stacking-disordered ice crystallites either are more stable than hexagonal ice crystallites or form because of non-equilibrium dynamical effects. Both scenarios challenge central tenets of classical nucleation theory. Here we use rare-event sampling and free energy calculations with the mW water model to show that the entropy of mixing cubic and hexagonal layers makes stacking-disordered ice the stable phase for crystallites up to a size of at least 100,000 molecules. We find that stacking-disordered critical crystallites at 230 kelvin are about 14 kilojoules per mole of crystallite more stable than hexagonal crystallites, making their ice nucleation rates more than three orders of magnitude higher than predicted by classical nucleation theory. This effect on nucleation rates is temperature dependent, being the most pronounced at the warmest conditions, and should affect the modelling of cloud formation and ice particle numbers, which are very sensitive to the temperature dependence of ice nucleation rates. We conclude that classical nucleation theory needs to be corrected to include the dependence of the crystallization driving force on the size of the ice crystallite when interpreting and extrapolating ice nucleation rates from experimental laboratory conditions to the temperatures that occur in clouds.
Role of stacking disorder in ice nucleation.

PubMed

Lupi, Laura; Hudait, Arpa; Peters, Baron; Grünwald, Michael; Gotchy Mullen, Ryan; Nguyen, Andrew H; Molinero, Valeria

2017-11-08

The freezing of water affects the processes that determine Earth's climate. Therefore, accurate weather and climate forecasts hinge on good predictions of ice nucleation rates. Such rate predictions are based on extrapolations using classical nucleation theory, which assumes that the structure of nanometre-sized ice crystallites corresponds to that of hexagonal ice, the thermodynamically stable form of bulk ice. However, simulations with various water models find that ice nucleated and grown under atmospheric temperatures is at all sizes stacking-disordered, consisting of random sequences of cubic and hexagonal ice layers. This implies that stacking-disordered ice crystallites either are more stable than hexagonal ice crystallites or form because of non-equilibrium dynamical effects. Both scenarios challenge central tenets of classical nucleation theory. Here we use rare-event sampling and free energy calculations with the mW water model to show that the entropy of mixing cubic and hexagonal layers makes stacking-disordered ice the stable phase for crystallites up to a size of at least 100,000 molecules. We find that stacking-disordered critical crystallites at 230 kelvin are about 14 kilojoules per mole of crystallite more stable than hexagonal crystallites, making their ice nucleation rates more than three orders of magnitude higher than predicted by classical nucleation theory. This effect on nucleation rates is temperature dependent, being the most pronounced at the warmest conditions, and should affect the modelling of cloud formation and ice particle numbers, which are very sensitive to the temperature dependence of ice nucleation rates. We conclude that classical nucleation theory needs to be corrected to include the dependence of the crystallization driving force on the size of the ice crystallite when interpreting and extrapolating ice nucleation rates from experimental laboratory conditions to the temperatures that occur in clouds.
Optical and dielectric properties of poly(vinyl-alcohol) - Cobalt oxide nanocomposite film

NASA Astrophysics Data System (ADS)

Das, Amit Kumar; Tripathi, Himadri Sekhar; Meikap, Ajit Kumar

2018-04-01

Highly crystalline cobalt oxide (Co3O4) have been synthesized via calcination method. The crystallite size of the nanoparticles is 28.5 nm. Two direct band gap of Co3O4 is observed. The temperature dependent dielectric spectroscopy of PVA-Co3O4 composite film shows ferroelectric behavior. The dielectric constant of the composite film is almost 2.5 times compare to pure PVA at a 1kHz frequency and room temperature. From the Nyquist plot grain and grain boundary effects are identified.
Synthesis of nanocrystalline rare earth oxides by glycothermal method

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

Hosokawa, Saburo; Iwamoto, Shinji; Inoue, Masashi

2008-11-03

The reaction of yttrium acetate hydrate in 1,2-propanediol at 300 deg. C yielded a product containing acetate groups and glycol moieties. From this product, Y{sub 2}O{sub 3} was directly crystallized at 400 deg. C without the formation of a carbonate oxide phase. The thus-obtained Y{sub 2}O{sub 3} samples had a small crystallite size (2.2 nm) and significantly large surface area (280 m{sup 2}/g). Other nanocrystalline rare earth (Gd-Yb) oxides were also obtained by this method.
Structural and spectroscopic study of mechanically synthesized SnO{sub 2} nanostructures

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

Vij, Ankush, E-mail: vij-anx@yahoo.com; Kumar, Ravi; Presently at Beant College of Engineering and Technology, Gurdaspur-143521

2016-05-23

We report the single step synthesis of SnO{sub 2} nanostructures using high energy mechanical attrition method. X-ray diffraction (XRD) pattern reveals the single phase rutile structure with appreciable broadening of diffraction peaks, which is a signature of nanostructure formation. The average crystallite size of SnO{sub 2} nanostructures has been calculated to be ~15 nm. The micro-Raman study reveals the shifting of A{sub 1g} Raman mode towards lower wave number, which is correlated with the nanostructure formation.
Synthesis, EPR and luminescent properties of YAlO3:Fe3+ (0.1-0.9mol%) nanopowders.

PubMed

Premkumar, H B; Nagabhushana, H; Sharma, S C; Daruka Prasad, B; Nagabhushana, B M; Rao, J L; Chakradhar, R P S

2014-05-21

A simple and inexpensive combustion method was used to prepare Fe(3+) doped YAlO3 perovskite within few minutes at low temperature (400±10°C). This might be useful in lowering the cost of the material. The final products were well characterized by various spectroscopic techniques such as PXRD, SEM, TEM, FTIR and UV-Visible. The average crystallite size was estimated from the broadening of the PXRD peaks and found to be in the range 45-90nm, the results were in good agreement with the W-H plots and TEM. The crystallites show dumbbell shape, agglomerated particles with different size. The TL glow curves of 1-5kGy γ-irradiated YAlO3:Fe(3+) (0.1mol%) nanopowder warmed at a heating rate of 3°Cs(-1) records a single glow peak at ∼260°C. The kinetic parameters namely activation energy (E), order of kinetics (b) and frequency factor (s) were determined at different gamma doses using the Chens glow peak shape method and the results were discussed in detail. The photoluminescence spectra for Fe(3+) (0.1-0.9mol%) doped YAlO3 records the lower energy band at 720nm ((4)T1 (4G)→(6)A1 (6S)) and the intermediate band located at 620nm ((4)T2 ((4)G)→(6)A1 (6S)) with the excitation of 378nm. The higher energy band located at 514nm was associated to (4)E+(4)A1 ((4)G)→(6)A1 (6S) transition. The resonance signals at g values 7.6, 4.97, 4.10, 2.94, 2.33 and 1.98 were observed in EPR spectra of Fe(3+) (0.1-0.9mol%) doped YAlO3 recorded at room temperature. The g values indicate that the iron ions were in trivalent state and distorted octahedral site symmetry was observed. Copyright © 2014 Elsevier B.V. All rights reserved.

Sonochemical method for producing titanium metal powder.

PubMed

Halalay, Ion C; Balogh, Michael P

2008-07-01

We demonstrate a sonochemical method for producing titanium metal powder. The method uses low intensity ultrasound in a hydrocarbon solvent at near-ambient temperatures to first create a colloidal suspension of liquid sodium-potassium alloy in the solvent and then to reduce liquid titanium tetrachloride to titanium metal under cavitation conditions. XRD data collected for the reaction products after the solvent removal show only NaCl and KCl, with no diffraction peaks attributable to titanium metal or other titanium compounds, indicating either the formation of amorphous metal or extremely small crystallite size. TEM micrographs show that hollow spheres formed of halide salts and titanium metal, with diameters with diameters ranging from 100 to 500 nm and a shell thickness of 20 to 40 nm form during the synthesis, suggesting that the sonochemical reaction occurs inside the liquid shell surrounding the cavitation bubbles. Metal particle sizes are estimated to be significantly smaller than 40 nm from TEM data. XRD data of the powder after annealing and prior to removal of the alkali chloride salts provides direct evidence that titanium metal was formed during the sonochemical synthesis.
Fe K-Edge X-ray absorption near-edge spectroscopy (XANES) and X-ray diffraction (XRD) analyses of LiFePO4 and its base materials

NASA Astrophysics Data System (ADS)

Latif, C.; Negara, V. S. I.; Wongtepa, W.; Thamatkeng, P.; Zainuri, M.; Pratapa, S.

2018-03-01

XANES analysis has been performed with the aim of knowing the Fe oxidation state in a synthesized LiFePO4 and its base materials. XANES measurements were performed at SLRI on energy around Fe K-edge. An XRD analysis has also been performed with the aim of knowing the phase composition, lattice parameters and crystallite size of the LiFePO4 as well as the base materials. From the XRD analysis, it was found that the dominating phase in the iron sand sample was Fe3O4 and the only phase found after calcination was LiFePO4. The latter phase exhibited crystallite size of 100 nm and lattice parameters a = 10.169916 Å, b = 5.919674 Å, c = 4.627893 Å. Qualitative analysis of XANES data revealed that the oxidation number of Fe in the sample before calcination was greater than that after calcination and Fe in the natural iron sand, indicated by the E0 values of 7129.2 eV, 7120.6 eV and 7124.4 eV respectively.
Investigation on the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ manganites

NASA Astrophysics Data System (ADS)

Arun, B.; Athira, M.; Akshay, V. R.; Sudakshina, B.; Mutta, Geeta R.; Vasundhara, M.

2018-02-01

We have investigated the structural, magnetic and magnetocaloric properties of nanocrystalline Pr-deficient Pr1-xSrxMnO3-δ Perovskite manganites. Rietveld refinement of the X-ray powder diffraction patterns confirms that all the studied compounds have crystallized into an orthorhombic structure with Pbnm space group. Transmission electron microscopy analysis reveals nanocrystalline compounds with crystallite size less than 50 nm. The selected area electron diffraction patterns reveal the highly crystalline nature of the compounds and energy dispersive X-ray spectroscopic analysis shows that the obtained compositions are nearly identical with the nominal one. The oxygen stoichiometry is estimated by iodometric titration method and stoichiometric compositions are confirmed by X-ray Fluorescence Spectrometry analysis. A large bifurcation is observed in the ZFC/FC curves and Arrott plots not show a linear relation but have a convex curvature nature. The temperature dependence of inverse magnetic susceptibility at higher temperature confirms the existence of ferromagnetic clusters. The experimental results reveal that the reduction of crystallite size to nano metric scale in Pr-deficient manganites adversely influences structural, magnetic and magnetocaloric properties as compared to its bulk counterparts reported earlier.
Thermal stability and chemical resistance of (Ti,Al)N-Cu and (Ti,Al)N-Ni metal-ceramic nanostructured coatings

NASA Astrophysics Data System (ADS)

Belov, D. S.; Blinkov, I. V.; Volkhonskii, A. O.; Kuznetsov, D. V.; Kiryukhantsev-Korneev, F. V.; Pustov, Yu. A.; Sergevnin, V. S.

2016-12-01

This work represents the results of research on thermal stability, oxidation resistance at temperatures of up to 800 °C and electrochemical behaviour of (Ti,Al)N-(∼3 at.%)Cu and (Ti,Al)N-(∼8 at.%)Ni nanocrystalline coatings in acidic and alkaline media. The coatings were deposited by the arc-PVD method with a thickness of approximately 4 μm and crystallite size of less than 20 nm. It has been demonstrated that the composition and properties of the coating structures do not change when the coatings are heated in 10-4 Pa vacuum at temperatures of 600, 700 °C for 1.5 h. Heating up to 800 °C caused an increase of crystallite size and reduction microstrain in the crystal lattice of the ceramic phase. The process is accompanied by deterioration of the coating hardness from 48 to 52 to 33-36 GPa. The (Ti,Al)N-Cu and (Ti,Al)N-Ni metal-ceramic nanostructured coatings are characterized by heat resistance up to the temperatures of 700 and 800 °C respectively. The coatings under study have tendency for self-passivation and resistance to pitting corrosion.
Synthesis and characterization of mesoporous ZnS with narrow size distribution of small pores

NASA Astrophysics Data System (ADS)

Nistor, L. C.; Mateescu, C. D.; Birjega, R.; Nistor, S. V.

2008-08-01

Pure, nanocrystalline cubic ZnS forming a stable mesoporous structure was synthesized at room temperature by a non-toxic surfactant-assisted liquid liquid reaction, in the 9.5 10.5 pH range of values. The appearance of an X-ray diffraction (XRD) peak in the region of very small angles (˜ 2°) reveals the presence of a porous material with a narrow pore size distribution, but with an irregular arrangement of the pores, a so-called worm hole or sponge-like material. The analysis of the wide angle XRD diffractograms shows the building blocks to be ZnS nanocrystals with cubic structure and average diameter of 2 nm. Transmission electron microscopy (TEM) investigations confirm the XRD results; ZnS crystallites of 2.5 nm with cubic (blende) structure are the building blocks of the pore walls with pore sizes from 1.9 to 2.5 nm, and a broader size distribution for samples with smaller pores. Textural measurements (N2 adsorption desorption isotherms) confirm the presence of mesoporous ZnS with a narrow range of small pore sizes. The relatively lower surface area of around 100 m2/g is attributed to some remaining organic molecules, which are filling the smallest pores. Their presence, confirmed by IR spectroscopy, seems to be responsible for the high stability of the resulting mesoporous ZnS as well.
Interaction of Se{sup 0} nanoparticles stabilized by poly(vinylpyrrolidone) with gel films of cellulose Acetobacter xylinum

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

Baklagina, Yu. G.; Khripunov, A. K.; Tkachenko, A. A.

2006-07-15

The sorption and desorption of poly(vinylpyrrolidone)-Se{sup 0} (PVP-Se{sup 0}) nanoparticles on gel films of cellulose Acetobacter xylinum (CAX) are investigated. It is revealed that the hydrodynamic radius R{sub h} of PVP-Se{sup 0} nanoparticles decreases from 57 nm in the initial solution (without CAX gel films) to 25 nm after the sorption of nanostructures on gel films and then increases to approximately 100 nm after the desorption of nanoparticles with water from dry samples of the CAX gel film-PVP-Se{sup 0} nanocomposite. It is found that selenium atoms do not penetrate into crystallites of the cellulose nanofibrils and replace water molecules sorbedmore » by the primary hydroxyl groups of their walls. Poly(vinylpyrrolidone)-Se{sup 0} nanoclusters differ in the number and size upon their sorption inside the cellulose gel film and on the film surface.« less
Optical and electrical properties of mechanochemically synthesized nanocrystalline delafossite CuAlO2.

PubMed

Prakash, T; Prasad, K Padma; Ramasamy, S; Murty, B S

2008-08-01

Nanocrystalline p-type semiconductor copper aluminum oxide (CuAlO2) has been synthesized by mechanical alloying using freshly prepared Cu2O and alpha-AlO2O3 nanocrystals in toluene medium. A study on structural property performed with different alloying and post annealing durations, by X-ray diffraction (XRD) reveals the formation of single phase with average crystallite size approximately 45 nm. Optical absorbance onset at 364.5 nm confirms its wide band gap nature (E(g) = 3.4 eV) and the fluorescence emission behaviour (390 nm) confirms its direct band type transition. The activation energy for electrical conduction has been calculated by Arrhenius plots using impedance measurement. Both grain and grain boundary conductivity takes place with almost equal activation energies of approximately 0.45 eV. The paper discusses synthesis, structural, optical and electrical properties of delafossite CuAlO2 in detail.
A facile growth mechanism, structural, optical, dielectric and electrical properties of ZnSe nanosphere via hydrothermal process

NASA Astrophysics Data System (ADS)

Javed, Qurat-Ul-Ain; Baqi, Sabah; Abbas, Hussain; Bibi, Maryam

2017-02-01

Hydrothermal method was chosen as a convenient method to fabricate zinc selenide (ZnSe) nanoparticle materials. The prepared nanospheres were characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM), where its different properties were observed using UV-visible spectroscopy and LCR meter. It was found that the pure ZnSe nanoparticles have a Zinc blende structure with crystallite size 10.91 nm and in a spherical form with average diameter of 35 nm (before sonication) and 18 nm (after sonication) with wide band gap of 4.28 eV. It was observed that there is inverse relation of frequency with dielectric constant and dielectric loss while AC conductivity grows up by increasing frequency. Such nanostructures were determined to be effectively used in optoelectronic devices as UV detector and in those devices where high-dielectric constant materials are required.
Structural and electromagnetic properties of NiAlxFe2-xO4/SiO2 nanocomposite films deposited using a sol-gel spin-coating method

NASA Astrophysics Data System (ADS)

Wang, Li; Li, Xuejian; Li, Ji; Liu, Mei; Xu, Shichong; Li, Haibo

2017-12-01

NiAlxFe2-xO4/SiO2 (0 ≤ x ≤ 1.0) nanocomposite films deposited on Si(1 0 0) substrates were prepared by a sol-gel spin-coating method. The influences of Al3+ content and annealing temperature on the structural and electromagnetic properties of the nanocomposite films were investigated. The results indicated that NiAlxFe2-xO4 in the nanocomposite films crystallized after annealing at 1073 K and above. When the doping content x increased from 0 to 1.0, the lattice constants and the average crystallite sizes of the NiAlxFe2-xO4 nanoparticles decreased. The saturation magnetization and coercivity of the films were inversely proportional to the Al3+ content. The maximum value of saturation magnetization (361.6 emu/cm3) and the minimum value of coercivity (18.6 kA/m) were obtained for x of 0.2. When the annealing temperature increased from 1073 to 1473 K, the lattice constant and the average crystallite size of the NiAl0.2Fe1.8O4 nanoparticles increased from 0.8322 to 0.8349 nm and 4 to 28 nm, respectively, and the saturation magnetization and coercivity of the films increased from 214.8 to 464.5 emu/cm3 and 8.2 to 26.9 kA/m, respectively. Moreover, the DC resistivity of the films increased with increasing Al3+ content and annealing temperature.
Structural and growth aspects of electron beam physical vapor deposited NiO-CeO{sub 2} nanocomposite films

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

Kuanr, Sushil Kumar; K, Suresh Babu, E-mail: sureshbabu.nst@pondiuni.edu.in

2016-03-15

Deposition of composite materials as thin film by electron beam physical vapor deposition technique (EB-PVD) still remains as a challenge. Here, the authors report the deposition of NiO-CeO{sub 2} (30/70 wt. %) composites on quartz substrate by EB-PVD. Two NiO-CeO{sub 2} nanocomposite targets—one as green compact and the other after sintering at 1250 °C—were used for the deposition. Though the targets varied with respect to physical properties such as crystallite size (11–45 nm) and relative density (44% and 96%), the resultant thin films exhibited a mean crystallite size in the range of 20–25 nm underlining the role of physical nature of deposition. In spitemore » of the crystalline nature of the targets and similar elemental concentration, a transformation from amorphous to crystalline structure was observed in thin films on using sintered target. Postannealing of the as deposited film at 800 °C resulted in a polycrystalline structure consisting of CeO{sub 2} and NiO. Deposition using pure CeO{sub 2} or NiO as target resulted in the preferential orientation toward (111) and (200) planes, respectively, showing the influence of adatoms on the evaporation and growth process of NiO-CeO{sub 2} composite. The results demonstrate the influence of electron beam gun power on the adatom energy for the growth process of composite oxide thin films.« less
Investigation of nanocrystalline zinc chromite obtained by two soft chemical routes

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

Gingasu, Dana; Mindru, Ioana, E-mail: imandru@yahoo.com; Culita, Daniela C.

2014-01-01

Graphical abstract: - Highlights: • Two soft chemical routes to synthesize zinc chromites are described. • Glycine is used as chelating agent (precursor method) and fuel (solution combustion method). • The synthesized chromites have crystallite size in the range of 18–27 nm. • An antiferromagnetic (AFM) transition is observed at about T{sub N} ∼ 18 K. - Abstract: Zinc chromite (ZnCr{sub 2}O{sub 4}) nanocrystalline powders were obtained by two different chemical routes: the precursor method and the solution combustion method involving glycine-nitrates. The complex compound precursors, [ZnCr{sub 2}(NH{sub 2}CH{sub 2}COO){sub 8}]·9H{sub 2}O and [ZnCr{sub 2}(NH{sub 2}CH{sub 2}COOH){sub 4.5}]·(NO{sub 3}){sub 8}·6H{submore » 2}O, were characterized by chemical analysis, infrared spectroscopy (IR), ultraviolet–visible spectroscopy (UV–vis) and thermal analysis. The structure, morphology, surface chemistry and magnetic properties of ZnCr{sub 2}O{sub 4} powders were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), infrared and Raman spectroscopy (RS), ultraviolet–visible spectroscopy (UV–vis) and magnetic measurements. X-ray diffraction patterns indicated the chromite spinel phase with good crystallinity and an average crystallite size of approximately 18–27 nm. The band gap values ranged between 3.31 and 3.33 eV. The magnetic measurements indicated an antiferromagnetic transition at T{sub N} ∼ 17.5/18 K.« less
Nanostructure investigation of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} synthesized by sol-gel method

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

Pransisco, Prengki, E-mail: prengkipransisco@gmail.com; Badan Lingkungan Hidup Derah Kabupaten Empat Lawang South of Sumatera; Shafie, Afza, E-mail: afza@petronas.com.my

2015-07-22

Magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} was successfully prepared by using sol-gel method. Heat treatment on material is always giving defect on properties of material. This paper investigates the effect of heat treatment on nanostructure of magnetic nanomaterial Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4}. According to thermo gravimetric analysis (TGA) that after 600°C there is no more weight loss detected and it was decided as minimum calcination temperature. Intensity, crystallite size, structure, lattice parameter and d-spacing of the material were investigated by using X-ray diffraction (XRD). High resolution transmission electron microscope (HRTEM) was used to examine nanostructure, nanosize,more » shape and distribution particle of magnetic material Ni{sub 0.5}Zn{sub 0.3}Cu{sub 0.2}Fe{sub 2}O{sub 4} and variable pressure field emission scanning electron microscope (VP-FESEM) was used to investigate the surface morphology and topography of the material. The XRD result shows single-phase cubic spinel structure with average crystallite size in the range of 25.6-95.9 nm, the value of the intensity of the material was increased with increasing temperature, and followed by lattice parameter was increased with increasing calcination temperature, value of d-spacing was relatively decreased with accompanied increasing temperature. From HRTEM result the distribution of particles was tend to be agglomerates with particle size of 7.8-17.68 nm. VP-FESEM result shows that grain size of the material increases with increasing calcination temperature and the surface morphology shows that the material is in hexagonal shape and it was also proved by mapping result which showing the presence each of constituents inside the compound.« less
Magnon-induced interband spin-flip scattering contribution to resistivity and magnetoresistance in a nanocrystalline itinerant-electron ferromagnet: Effect of crystallite size

NASA Astrophysics Data System (ADS)

Madduri, P. V. Prakash; Kaul, S. N.

2017-05-01

We report the results of an exhaustive study of `zero-field' electrical resistivity ρ (T ) and magnetoresistance (MR) (in magnetic fields up to 90 kOe) over the temperature range 1.8-300 K in nanocrystalline (nc-) Ni with average crystallite size d ranging from 10 nm to 40 nm. A quantitative comparison of our results with the predictions of the recent self-consistent calculations permits us to unambiguously identify the scattering mechanisms responsible for ρ (T ) and MR in different temperature ranges and accurately determine their relative magnitudes in nc-Ni samples of different d . Like in bulk 3 d transition metal ferromagnets, ρ varies with temperature as T2 at T ≲15 K. Contrary to the widely-held view that the T2 variation of ρ at low temperatures arises from the electron-magnon (e -m ) scattering, this contribution to ρ (T ) is shown to originate from the electron-electron (Baber) scattering. In the temperature range 15 K≤T ≤300 K, the phonon-induced non-spin-flip (NSF) intraband [i.e., s↑↓-s↑↓ , d↑↓-d↑↓ electron-phonon (e -p )] scattering and magnon-induced spin-flip (SF) interband (i.e., s↑↓-d↓↑e -m ) scattering contributions completely account for the intrinsic resistivity. The former contribution dominates over the latter at T >T whereas the reverse is true at temperatures 15 K ≤T T , ρe -m(T ,H =0 ) becomes comparable in magnitude to ρe -p(T ,H =0 ) for d ≥25 nm. By contrast, the MR in nc-Ni is entirely due to the s↑↓-d↓↑e -m scattering. The present work clearly brings out the importance of the thermal renormalization of magnon mass (caused mainly by the magnon-magnon interactions) over the temperature range 15 K≤T ≤300 K. Irrespective of the value of d (including the bulk, d =∞ ), phonon-induced s↑↓-s↑↓ , d↑↓-d↑↓ transitions are more frequent than the e -p s↑↓-d↑↓ transitions over the entire temperature range 1.8 K≤T ≤300 K. The saturation magnetization at 0 K, spin wave stiffness at 0 K, Debye temperature as well as the parameters that are a direct measure of the strength of e -p coupling, e -m coupling, and level of suppression of e -m scattering by external magnetic field, all exhibit power law variations with d . The power law behavior asserts that the average crystallite size is the dominant length scale so far as the magnetism, electrical transport, and magnetotransport in nc-Ni are concerned.
Influence of Dispersant and Heat Treatment on the Morphology of Nanocrystalline Hydroxyapatite

NASA Astrophysics Data System (ADS)

Pan, Yusong; Xiong, Dangsheng

2010-10-01

Natural biological hard tissues are biocomposites of proteins and hydroxyapatite (HA) with superior strength. Nanometer scale HAp is the key material to manufacture bone substitute. In this work, nano-sized HA particles were synthesized by a wet method using orthophosphoric acid and calcium hydroxide as raw materials. The prepared nanocrystalline HAp was characterized for its phase purity and nano-scale morphological structure by XRD, TEM, and FTIR. The influences of heat treatment temperature and dispersant on the properties of HAp were also investigated. The results indicated that nano-particles were pure single-phase HAp with a diameter of 25-70 nm and length of 50-180 nm depending on heat treatment temperature. The morphology and crystallite size of HAp change with heat treatment temperature. After heat treating, the crystallinity of these nano-particles increased and its morphology transformed from needle-like to sphere-like structure. The dispersant is beneficial to prevent the growth of HA particles and provide a uniform particle size distribution. Moreover, the HAp tends to form small agglomerates in the absence of dispersant.
Modeling of the Structure of Disordered Metallic Alloys and Its Transformation Under Thermal Forcing

NASA Astrophysics Data System (ADS)

Cress, Ryan Paul

The morphology of disordered binary metallic alloys is investigated. The structure of disordered binary metallic alloys is modeled as a randomly close packed (RCP) assembly of atoms. It was observed through a 2-D binary hard sphere experiment that RCP structure can be modeled as a mixture of nano-crystallites and glassy matter. We define the degree of crystallinity as the fraction of atoms contained in nano-crystallites in an RCP medium. Nano-crystallites by size in a crystallite size distribution were determined experimentally to define the morphology of the RCP medium. Both the degree of crystallinity and the crystallite size distribution have been found to be determined by the composition of a given binary mixture. A 2-D Monte Carlo simulation was developed in order to replicate the RCP structure observed in the experiment which is then extended to cases of arbitrary composition. Crystallites were assumed to be spherical with isotropic cross sections. The number of atoms in an individual crystallite in 2-D is simply transformed into the number of atoms in 3-D; we then obtain the crystallite size distribution in 3-D. This experiment accounts for the contribution from the repulsive core of the inter-atomic potential. The attractive part of the potential is recovered by constructing spherical nano-crystallites of a given radius from a crystalline specimen of each given alloy. A structural model of a disordered alloy is thus obtained. With the basic structure of the RCP medium defined, the response to heating would be in the form of changes to the crystallite size distribution. This was first investigated in a hard sphere mechanical oven experiment. The experimental setup consists of a 2-D cell which is driven by two independent stepper motors. The motors drive a binary RCP bed of spheres on a slightly tilted plane according to a chaotic algorithmm. The motors are driven at four different speed settings. The RCP medium was analyzed using a sequence of digital images taken of the beds. The bursts of images provide a Gaussian distribution of particle speeds in x and y directions thus giving rise to the notion of "temperature." This temperature scales with the motor speed settings. The measured average degree of crystallinity is found to decrease as the effective temperature was raised suggesting that nano-crystallites dissociate under thermal forcing. The evolution of a specimen's structure is calculated rigorously by means of the law of mass action formalism. A system of thermal dissociation reaction equations is written out for the set of nano-crystallites according to the 3-D crystallite size distribution. The equilibrium treatment is justified because the energy differences between metastable RCP structures fall within kT. Thermal dissociation of one surface atom at a time is assumed because the energy cost in dissociation of a surface atom on a nano-crystallite is significantly less than that of a multi atom cluster. The full set of reaction equations cover all possible dissociation steps, which may amount to several thousand for a disordered alloy specimen. The primary determining factor in each of these dissociation equations is the dissociation potential or the amount of attractive energy needed to remove a surface atom on a nano-crystallite of a given size. The attractive potential between atoms is calculated using a Lennard-Jones potential between a pair of atoms for which quantum chemistry calculations exist in the literature. All interactions impinged on the surface atom by all other atoms in a crystallite are summed. As the nano-crystallites dissociate due to heating, the structure of the alloy changes, and this leads to modifications of alloy's transport properties. The model is found to predict the melting temperature of various disordered binary alloys as well as refractory metals in good agreement with known data. The structure model for disordered binary alloys gives an excellent characterization of the alloy morphology. It therefore provides fruitful avenues for making predictions about how thermophysical properties of disordered binary alloys change as the alloy temperature is raised by heating.
The optical and structural properties of graphene nanosheets and tin oxide nanocrystals composite

NASA Astrophysics Data System (ADS)

Farheen, Parveen, Azra; Azam, Ameer

2018-05-01

A nanocomposite material consisting of metal oxide and reduced graphene oxide was prepared via simple, economic, and effective chemical reduction method. The synthesis strategy was based on the reduction of GO with Sn2+ ion that combines tin oxidation and GO reduction in one step, which provides a simple, low-cost and effective way to prepare graphene nanosheets/SnO2 nanocrystals composites because no additional chemicals were needed. SEM and TEM images shows the uniform distribution of the SnO2 nanocrystals on the Graphene nanosheets (GNs) surface and transmission electron microscope shows an average particle size of 2-4 nm. The mean crystallite size was calculated by Debye Scherrer formula and was found to be about 4.0 nm. Optical analysis was done by using UV-Visible spectroscopy technique and the band gap energy of the GNs/SnO2 nanocomposite was calculated by Tauc relation and came out to be 3.43eV.
Highly transparent ceramics with disordered crystal structure

NASA Astrophysics Data System (ADS)

Osipov, V. V.; Khasanov, O. L.; Solomonov, V. I.; Shitov, V. A.; Orlov, A. N.; Platonov, V. V.; Spirina, A. V.; Luk'yashin, K. E.; Dvilis, E. S.

2010-08-01

A highly transparent ceramic has been synthesized from Nd3+:Y2O3 to which 6 mol. % ZrO2 and 25 mol. % Sc2O3 or Lu2O3 were added for disordering the crystal structure. Nanopowders with an average particle size of 10-15 nm served as an initial material. They were compacted by the method of uniaxial static pressing combined with ultrasonic action on nanoparticles. The compacting pressure was 200 MPa; the power of the ultrasonic generator was 1.5 kW. It has been shown that the replacement of Y by isovalent Sc and Lu ions and by heterovalent Zr ions reduces the content of pores and the sizes of crystallites. The transparency of the Nd3+:Y2O3 ceramic with these additives reaches a maximum of 82.2%, and the 40% intensity level spectral band corresponding to the 4F3/2 → 4I11/2 transition widens from 11.4 to 40 nm.
Influence the dopant concentration on the photocatalytic activity: Dy3+, Eu3+ doped TiO2

NASA Astrophysics Data System (ADS)

Zikriya, Mohamed; Nadaf, Y. F.; Pramod, A. G.; Renuka, C. G.

2018-05-01

Titanium dioxide (TiO2) nanoparticles were synthesis by means of hydrothermal process from metatitanic acid. The impacts reaction temperature, stirring process and aging time on the morphology, the transfer of nanoparticles particles were characterized. The morphology of the nanoparticles was described in detail with scanning electron microscopy. In the dynamic of hydrothermal method, stirring can cut down the reaction time of change from particles to nanoparticles. As can be seen from the XRD patterns, the diffraction peaks get broadened as the Eu3+ focus is increased, proposing an orderly abatement in the grain size. The Crystallite size was calculated for pure, Dy3+ and Eu3+ doped TiO2 from diffraction plane by Sherrer's formula and it was found that 13 nm to 18 nm. From SEM images the majorities of TiO2 particles are oblate spheroid or spheroid and look looser, and some macropores could be seen on a few particles.
Thermo-responsive magnetic liposomes for hyperthermia-triggered local drug delivery.

PubMed

Dai, Min; Wu, Cong; Fang, Hong-Ming; Li, Li; Yan, Jia-Bao; Zeng, Dan-Lin; Zou, Tao

2017-06-01

We prepared and characterised thermo-responsive magnetic liposomes, which were designed to combine features of magnetic targeting and thermo-responsive control release for hyperthermia-triggered local drug delivery. The particle size and zeta-potential of the thermo-responsive magnetic ammonium bicarbonate (MagABC) liposomes were about 210 nm and -14 mV, respectively. The MagABC liposomes showed encapsulation efficiencies of about 15% and 82% for magnetic nanoparticles (mean crystallite size 12 nm) and doxorubicin (DOX), respectively. The morphology of the MagABC liposomes was visualised using transmission electron microscope (TEM). The MagABC liposomes showed desired thermo-responsive release. The MagABC liposomes, when physically targeted to tumour cells in culture by a permanent magnetic field yielded a substantial increase in intracellular accumulation of DOX as compared to non-magnetic ammonium bicarbonate (ABC) liposomes. This resulted in a parallel increase in cytotoxicity for DOX loaded MagABC liposomes over DOX loaded ABC liposomes in tumour cells.
Post-annealing effect on optical absorbance of hydrothermally grown zinc oxide nanorods

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

Mohar, Rahmat Setiawan; Djuhana, Dede; Imawan, Cuk

In this study, the optical absorbance of zinc oxide (ZnO) nanorods was investigated. The ZnO thin film were deposited on indium tin oxide (ITO) layers using ultrasonic spray pyrolysis (USP) method and then grown by hydrothermal method. In order to improve the optical absorbance, the ZnO nanorods were then post-annealed for one hour at three different of temperatures, namely 250, 400, and 500 °C. The X-ray diffraction (XRD) spectra and FESEM images show that the ZnO nanorods have the hexagonal wurtzite crystal structure and the increasing of post-annealing temperature resulted in the increasing of crystallite size from 38.2 nm to 48.4 nm.more » The UV-vis spectra shows that all samples of ZnO nanorods exhibited the identical sharp absorption edge at 390 nm indicating that all samples have the same bandgap. The post-annealing process seemed to decrease the optical absorbance in the region of 300-550 nm and increase the optical absorbance in the region of 550-700 nm..« less

Kinetic and microstructural study of titanium nitride deposited by laser chemical vapor deposition

NASA Astrophysics Data System (ADS)

Egland, Keith Maynard

Titanium nitride (TiN) films were deposited onto Ti-6Al-4V substrates by laser chemical vapor deposition using a cw COsb2 laser and TiClsb4,\\ Nsb2, and Hsb2 reactant gases. In-situ laser induced fluorescence (LIF) and multi-wavelength pyrometry determined relative titanium gas phase atomic number density and deposition temperature, respectively. Deposited films were yellow to gold in color. Transmission electron microscopy on one sample revealed a face-centered cubic structure with a lattice parameter (0.4237 nm) expected for TiN. Auger electron spectroscopy found substoichiometric compositions with a N/Ti ratio between 0.7 and 0.9. Variables decreasing grain size (lower temperature, higher TiClsb4 input) decreased the N/Ti ratio. Higher Nsb2 input increased stoichiometry, while larger Hsb2 input decreased stoichiometry. The deposit substoichiometry is believed to be caused by diffusion of nitrogen through TiN grain boundaries to the titanium alloy substrate. The morphology starts as a dense polycrystalline structure evolving into a columnar structure having facets or nodules at the surface with crystallite sizes ranging from 10-1000 nm. TiClsb4 input had a inverse correlation with crystallite size, while Nsb2:Hsb2 ratio had minimal effect; the crystallite size (G) varied exponentially with temperature (T) for a given irradiation time, i.e., G = C exp (-28000/T), with constant C reflecting substrate roughness and gas composition. Microhardness tests revealed substrate contributions; nevertheless, films appeared to have a minimum hardness of 2000 Hsbv. The deposition apparent activation energy was calculated as 122 ± 9 kJ/mole using growth rates measured by film height and 117 ± 23 kJ/mole using growth rates measured by LIF signals. This puts the process in the surface kinetic growth regime over the temperature range 1370-1610 K. Above Nsb2 and Hsb2 levels of 1.25% and below TiClsb4 input of 4.5%, the growth rate has a half-order dependence on nitrogen and a linear dependence on hydrogen and is approximated by$r = {{kPsb{TiClsb4}Psb{Hsb2}Psbsp{Nsb2}{1/2}exp≤ft({{-}Esb{a}/ {RT}right)}/{1 + Psb{Ar}}}}.Since nitrogen positively affects growth rate (when added to a TiClsb4+Hsb2 mixture), stepwise reduction of TiClsb4 to Ti by hydrogen does not occur. NHsb{x} complexes are clearly involved in the growth mechanism; a likely combination of rate determining steps is the formation of NH and the initial reduction of TiClsb4$ by hydrogen.
Fabrication and Characterization of novel W80Ni10Nb10 alloy produced by mechanical alloying

NASA Astrophysics Data System (ADS)

Saxena, R.; Patra, A.; Karak, S. K.; Pattanaik, A.; Mishra, S. C.

2016-02-01

Nanostructured tungsten (W) based alloy with nominal composition of W80Ni10Nb10 (in wt. %) was synthesized by mechanical alloying of elemental powders of tungsten (W), nickel (Ni), niobium (Nb) in a high energy planetary ball-mill for 20 h using chrome steel as grinding media and toluene as process control agent followed by compaction at 500 MPa pressure for 5 mins and sintering at 1500°C for 2 h in Ar atmosphere. The phase evolution and the microstructure of the milled powder and consolidated product were investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). The crystallite size of W in W80Ni10Nb10 powder was reduced from 100 μm at 0 h to 45.6 nm at 10 h and 34.1 nm at 20 h of milling whereas lattice strain increases to 35% at 20 h of milling. The dislocation density shows sharp increase up to 5 h of milling and the rate of increase drops beyond 5 to 20 h of milling. The lattice parameter of tungsten in W80Ni10Nb10 expanded upto 0.04% at 10 h of milling and contracted upto 0.02% at 20 h of milling. The SEM micrograph revealed the presence of spherical and elongated particles in W80Ni10Nb10 powders at 20 h of milling. The particle size decreases from 100 μm to 2 μm with an increase in the milling time from 0 to 20 hours. The crystallite size of W in milled W80Ni10Nb10 alloy as evident from bright field TEM image was in well agreement with the measured crystallite size from XRD. Structure of W in 20 h milled W80Ni10Nb10 alloy was identified by indexing of selected area diffraction (SAD) pattern. Formation of NbNi intermetallic was evident from XRD pattern and SEM micrograph of sintered alloy. Maximum sinterability of 90.8% was achieved in 20 h milled sintered alloy. Hardness and wear study was also conducted to investigate the mechanical behaviour of the sintered product. Hardness of W80Ni10Nb10 alloy reduces with increasing load whereas wear rate increases with increasing load. The evaluated hardness value in the present study for all loads is lower than the literature reported hardness of nanostructured W.
The gas-sensing potential of nanocrystalline SnO2 produced by a mechanochemical milling via centrifugal action

NASA Astrophysics Data System (ADS)

Kersen, Ü.

In this work, the synthesis of undoped nanocrystalline tin dioxide powders and the subsequent preparation of SnO2 thick-films were studied. An initial mixture of SnCl2 and Ca(OH)2 was sealed in a vial for milling in an air atmosphere. Heat treatment of the milled powder resulted in the formation of tetragonal and orthorhombic SnO2 phases, which was confirmed by X-ray diffraction (XRD) analysis. It was found that crystallite size could be controlled by varying the milling time, the rotation speed and the temperature used for the heat treatment. Crystallite sizes in the range 20 to 30 nm (determined by XRD measurements) were obtained. The total pore volume was 0.22 ml/g for a measured particle size of 37 m2/g. No contamination of the powder during milling was found. The response of the prepared thick-films to H2S gas in the concentration range 0.5 to 10 ppm in air was investigated as a function of the preparation conditions. The advantage of mechanochemical synthesis of powder is its relative simplicity, low cost and possibility of obtaining isolated, unagglomerated nanosized grains. It is shown that chemical reactions, which usually occur in the vibratory mill to produce the SnO phase, can also be initiated during a short processing time in the centrifugal mill.
Synthesis and characterization of arsenic-doped cysteine-capped thoria-based nanoparticles

NASA Astrophysics Data System (ADS)

Pereira, F. J.; Díez, M. T.; Aller, A. J.

2013-09-01

Thoria materials have been largely used in the nuclear industry. Nonetheless, fluorescent thoria-based nanoparticles provide additional properties to be applied in other fields. Thoria-based nanoparticles, with and without arsenic and cysteine, were prepared in 1,2-ethanediol aqueous solutions by a simple precipitation procedure. The synthesized thoria-based nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (ED-XRS), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy and fluorescence microscopy. The presence of arsenic and cysteine, as well as the use of a thermal treatment facilitated fluorescence emission of the thoria-based nanoparticles. Arsenic-doped and cysteine-capped thoria-based nanoparticles prepared in 2.5 M 1,2-ethanediol solutions and treated at 348 K showed small crystallite sizes and strong fluorescence. However, thoria nanoparticles subjected to a thermal treatment at 873 K also produced strong fluorescence with a very narrow size distribution and much smaller crystallite sizes, 5 nm being the average size as shown by XRD and TEM. The XRD data indicated that, even after doping of arsenic in the crystal lattice of ThO2, the samples treated at 873 K were phase pure with the fluorite cubic structure. The Raman and FT-IR spectra shown the most characteristics vibrational peaks of cysteine together with other peaks related to the bonds of this molecule to thoria and arsenic when present.
Laser-synthesized Y2O3:Eu3+ nanophosphors and their stabilization in water suspensions

NASA Astrophysics Data System (ADS)

Ivanov, M. G.; Krutikova, I. V.; Kynast, U.; Lezhnina, M.; Puzyrev, I. S.

2017-12-01

Europium doped yttrium oxide nanophosphors (Y2O3 doped with 5% Eu3+), which consists of spherical single-phase monoclinic particles with an average size of 17 nm, was prepared by laser synthesis. While the monoclinic material has a low efficiency of only 19% of a μm-sized commercial Y2O3:Eu product, the cubic phase after calcination at 900 °C achieves 68% despite the remaining hydroxo-groups at the surface and still small crystallite size (56 nm). An ethanolammonium salt of citric acid (Dolapix CE64) was used as a dispersant in water suspension. To estimate the stability of the dispersed phase, the electrokinetic potential and agglomerate sizes were measured as a function of pH. With this dispersant, a 30 wt% nanopowder water suspension, showing a Newtonian viscosity of about 6 mPa × s, was obtained. Maximum content of the nanopowder of about 60 wt% can be accomplished in the slurry, still fluid enough to be used to cast a highly uniform and dense ceramic green body to sinter nanostructured Y2O3:Eu3+ phosphors ceramics.
Structural and photoluminescence properties of Ni doped CdS nanoparticles synthesis by sol gel method

NASA Astrophysics Data System (ADS)

Mahdi, Hadeel Salih; Parveen, Azra; Azam, Ameer

2018-05-01

Ni doped CdS nanoparticles have been successfully synthesized by sol-gel method. Nickel nitrate, cadmium nitrate, sodium sulfide has been used as precursors for the preparation of these Ni-doped CdS nanoparticles. The structural properties were studied by X-ray diffraction analysis. Surface morphology and the composition of the samples were studied by scanning electron microscope (SEM). The X-ray diffraction results revealed that the Ni-doped CdS nanoparticles were in hexagonal structure. The crystallite size was determined from Debye-Scherer equation and showed that the particle size increases with the doping of Ni. Optical absorption spectra of Ni doped CdS also was studied by Photoluminescence spectroscopy in the range of 200-600 nm.
Bio-active synthesis of tin oxide nanoparticles using eggshell membrane for energy storage application

NASA Astrophysics Data System (ADS)

Celina Selvakumari, J.; Nishanthi, S. T.; Dhanalakshmi, J.; Ahila, M.; Pathinettam Padiyan, D.

2018-05-01

Nano-sized tin oxide (SnO2) particles were synthesized using eggshell membrane (ESM), a natural bio-waste from the chicken eggshell. The crystallization of SnO2 into the tetragonal structure was confirmed from powder X-ray diffraction and the crystallite size ranged from 13 to 40 nm. Various shapes including rod, hexagonal and spherical SnO2 nanoparticles were observed from the morphological studies. The electrochemical impedance study revealed a lower charge transfer resistance (Rct) of 8.565 Ω and the presence of a constant phase element which arised due to surface roughness and porosity. Capacitive behavior seen in the cyclic voltammetry curve of the prepared SnO2 nanoparticles, find future applications in supercapacitors.
X-ray peak broadening analysis of AA 6061{sub 100-x} - x wt.% Al{sub 2}O{sub 3} nanocomposite prepared by mechanical alloying

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

Sivasankaran, S., E-mail: sivasankarangs1979@gmail.com; Sivaprasad, K., E-mail: ksp@nitt.edu; Narayanasamy, R., E-mail: narayan@nitt.edu

2011-07-15

Nanocrystalline AA 6061 alloy reinforced with alumina (0, 4, 8, and 12 wt.%) in amorphized state composite powder was synthesized by mechanical alloying and consolidated by conventional powder metallurgy route. The as-milled and as-sintered (573 K and 673 K) nanocomposites were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The peaks corresponding to fine alumina was not observed by XRD patterns due to amorphization. Using high-resolution transmission electron microscope, it is confirmed that the presence of amorphized alumina observed in Al lattice fringes. The crystallite size, lattice strain, deformation stress, and strain energy density of AA 6061 matrixmore » were determined precisely from the first five most intensive reflection of XRD using simple Williamson-Hall models; uniform deformation model, uniform stress deformation model, and uniform energy density deformation model. Among the developed models, uniform energy density deformation model was observed to be the best fit and realistic model for mechanically alloyed powders. This model evidenced the more anisotropic nature of the ball milled powders. The XRD peaks of as-milled powder samples demonstrated a considerable broadening with percentage of reinforcement due to grain refinement and lattice distortions during same milling time (40 h). The as-sintered (673 K) unreinforced AA 6061 matrix crystallite size from well fitted uniform energy density deformation model was 98 nm. The as-milled and as-sintered (673 K) nanocrystallite matrix sizes for 12 wt.% Al{sub 2}O{sub 3} well fitted by uniform energy density deformation model were 38 nm and 77 nm respectively, which indicate that the fine Al{sub 2}O{sub 3} pinned the matrix grain boundary and prevented the grain growth during sintering. Finally, the lattice parameter of Al matrix in as-milled and as-sintered conditions was also investigated in this paper. Research highlights: {yields} Integral breadth methods using various Williamson-Hall models were investigated for line profile analysis. {yields} Uniform energy density deformation model is observed to the best realistic model. {yields} The present analysis is used for understanding the stress and the strain present in the nanocomposites.« less
Electrical transport properties of nanoplates shaped tungsten oxide embedded poly(vinyl-alcohol) film

NASA Astrophysics Data System (ADS)

Das, Amit Kumar; Chatterjee, Piyali; Meikap, Ajit Kumar

2018-04-01

Tungsten oxide (WO3) nanoplates have been synthesized via hydrothermal method. The average crystallite size of the nanoplates is 28.9 ± 0.5 nm. The direct and indirect band gap of WO3 is observed. The AC conductivity of PVA-WO3 composite film has been observed and carrier transport mechanism follows correlated barrier hopping model. The maximum barrier height of the composite film is 0.1 eV. The electric modulus reflects the non-Debye type behaviour of relaxation time which is simulated by Kohlrausch-Willims-Watts (KWW) function.
Composition and phase analysis of nanocrystalline Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} (x = 1.0; 0.6; and 0.4) by using general structure analysis system

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

Gunanto, Y. E., E-mail: yohanes.gunanto@uph.edu; Jobiliong, E., E-mail: eric.jobiliong@uph.edu; Adi, Wisnu Ari, E-mail: dwisnuaa@batan.go.id

2016-03-11

Single phase of nanocrystalline Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} (x = 1.0; 0.6; and 0.4) was successfully synthesized by mechanical milling method and thermal process. Stoichiometric quantities of analytical-grade SrCO{sub 3}, BaCO{sub 3}, and Fe{sub 2}O{sub 3}, were mixed and milled using a high-energy milling. The mixture of all precursors was sintered at a temperature of 1000 °C for 10 hours. The refinement of x-ray diffraction trace for all samples confirmed a single phase material with a hexagonal structure. The increase of the amount of strontium content in the barium atoms in the Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} system canmore » decrease the lattice parameter which have been successfully substituted into the barium atoms. The calculation result of cationic distribution showed that the Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} (x = 0.6) and (x = 0.4) samples have nominal composition of Ba{sub 0,61}Sr{sub 0,39}Fe{sub 12}O{sub 19} and Ba{sub 0,37}Sr{sub 0,63}Fe{sub 12}O{sub 19}, respectively. Results of the mean of crystallite size evaluation for respective powder materials showed that the Ba{sub x}Sr{sub 1-x}Fe{sub 12}O{sub 19} (x = 1.0; 0.6; and 0.4) samples have the crystallite size of 22 nm, 25 nm and 34 nm, respectively. We concluded that the cationic distribution of barium atoms was successfully substituted by strontium atoms approaching the nominal stoichiometric composition.« less
Method of controlling crystallite size in nuclear-reactor fuels

DOEpatents

Lloyd, Milton H.; Collins, Jack L.; Shell, Sam E.

1985-01-01

Improved spherules for making enhanced forms of nuclear-reactor fuels are prepared by internal gelation procedures within a sol-gel operation and are accomplished by first boiling the concentrated HMTA-urea feed solution before engaging in the spherule-forming operation thereby effectively controlling crystallite size in the product spherules.
THE EFFECT OF SATELLITE LINES FROM THE X-RAY SOURCE ON X-RAY DIFFRACTION PEAKS

EPA Science Inventory

The article discusses the development of a method for relating reactivity to crystallite size and strain parameters obtained by the Warren-Averbach technique. EPA has been using crystallite size and strain data obtained from x-ray diffraction (XRD) peak profile analysis to predic...
Method of controlling crystallite size in nuclear-reactor fuels

DOEpatents

Lloyd, M.H.; Collins, J.L.; Shell, S.E.

Improved spherules for making enhanced forms of nuclear-reactor fuels are prepared by internal gelation procedures within a sol-gel operation and are accomplished by first boiling the concentrated HMTA-urea feed solution before engaging in the spherule-forming operation thereby effectively controlling crystallite size in the product spherules.
Effect of annealing on particle size, microstructure and gas sensing properties of Mn substituted CoFe2O4 nanoparticles

NASA Astrophysics Data System (ADS)

Kumar, E. Ranjith; Kamzin, A. S.; Janani, K.

2016-11-01

Microstructure, morphological and gas sensor studies of Mn substituted cobalt ferrite nanoparticles synthesized by a simple evaporation method and auto- combustion method. The influence of heat treatment on phase and particle size of spinel ferrite nanoparticles were determined by X-ray diffraction and Mossbauer spectroscopy. The XRD study reveals that the lattice constant and crystallite size of the samples increases with the increase of annealing temperature. Last one was confirmed by Mossbauer data. The lowest size of particles of MnCoFe2O4 (~3 nm) is obtained by auto combustion method. The spherical shaped nanoparticles are recorded by TEM. Furthermore, conductance response of Mn-Co ferrite nanomaterial was measured by exposing the material to reducing gas like liquefied petroleum gas (LPG) which showed a sensor response of ~0.19 at an optimum operating temperature of 250 °C.
Neoteric environmental detoxification of organic pollutants and pathogenic microbes via green synthesized ZnO nanoparticles.

PubMed

Jaffri, Shaan Bibi; Ahmad, Khuram Shahzad

2018-06-13

Present study has for the first time reported Prunus cerasifera leaf extract mediated zinc oxide nanoparticles in a green and one pot synthetic mode without utilization of any chemical reducing agents. Synthesized nanoparticles were analyzed by ultraviolet-visible (UV-Vis) spectroscopy, X-ray diffraction (XRD), fourier transmission infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). UV-Vis peak was detected at 380 nm due to surface plasmon resonance (SPR). Variety of biomolecules were revealed by FTIR involved in reduction cum stabilization of zinc oxide nanoparticles. Wurtzite hexagonal geometry with an average crystallite size of 12 nm was obtained from XRD diffraction pattern. SEM exhibited size ranges of 80-100 nm and 60- 100 nm for 200 ℃ and 600 ℃ calcination temperatures. Synthesized nanoparticles were used as bio-cleaning photocatalysts against organic pollutants i.e. bromocresol green, bromophenol blue, methyl red and methyl blue, which yielded pseudo first order reaction kinetics (R 2 = 0.98, 0.92, 0.92, 0.90 respectively). Pollutants expressed higher degradation percentages in less than 14 min in direct solar irradiance. Moreover, synthesized nanoparticles were tested against resistant microbes i.e. Aspergillus niger, Aspergillus flavus, Aspergillus fumigatus, Aspergillus terreus, Penicillium chrysogenum, Fusarium solani, Lasiodiplodia theobromae, Xanthomonas axonopodis pv. citri and Psuedomonas syringae for development of new generation of antimicrobial agents.
Influence of Substrate, Additives, and Pulse Parameters on Electrodeposition of Gold Nanoparticles from Potassium Dicyanoaurate

NASA Astrophysics Data System (ADS)

Vahdatkhah, Parisa; Sadrnezhaad, Sayed Khatiboleslam

2015-12-01

Gold nanoparticles (AuNPs) of less than 50 nm diameter were electrodeposited from cyanide solution by pulsating electric current on modified copper and indium tin oxide (ITO) films coated on glass. Morphology, size, and composition of the deposited AuNPs were studied by X-ray photoelectron spectroscopy, atomic force microscopy, and field emission scanning electron microscopy. Effects of peak current density, pulse frequency, potassium iodide and cysteine on grain size, and morphology of the AuNPs were determined. Experiments showed that cathode current efficiency increases with the pulse frequency and the iodide ion. Size of the AuNPs increased with the current density. The number of nucleation sites was larger on ITO than on Cu layer; while the average diameter of the crystallites on ITO was smaller than on Cu layer.
Citrus maxima (Pomelo) juice mediated eco-friendly synthesis of ZnO nanoparticles: Applications to photocatalytic, electrochemical sensor and antibacterial activities

NASA Astrophysics Data System (ADS)

Pavithra, N. S.; Lingaraju, K.; Raghu, G. K.; Nagaraju, G.

2017-10-01

In the present work, Zinc oxide nanoparticles (ZnO Nps) have been successfully prepared through a simple, effective and low cost solution combustion method using Zn (NO3)2·6H2O as an oxidizer, chakkota (Common name = Pomelo) fruit juice as novel fuel. X-ray diffraction pattern indicates the hexagonal wurtzite structure with average crystallite size of 22 nm. ZnO Nps were characterized with the aid of different spectroscopic techniques such as Raman spectroscopy, Fourier Transform Infrared spectroscopy, Photoluminescence and UV-Visible spectroscopy. FTIR shows characteristic ZnO vibrational mode at 393 cm- 1. SEM images show that the particles are agglomerated. TEM image shows the size of the particles are about 10-20 nm. Further, in order to establish practical applicability of the synthesized ZnO Nps, photocatalytic degradation of methylene blue (MB) dye as a model system was studied in presence of UV (665 nm) light. In addition to this, the antibacterial activity was screen against 3 bacterial strains and electrochemical sensor performance towards the quantification of dopamine at nano molar concentrations was also explored.
CoO doping effects on the ZnO films through EBPDV technique

NASA Astrophysics Data System (ADS)

Inês Basso Bernardi, Maria; Queiroz Maia, Lauro June; Antonelli, Eduardo; Mesquita, Alexandre; Li, Maximo Siu; Gama, Lucianna

2014-03-01

Nanometric Zn1-xCo xO (x = 0.020, 0.025 and 0.030 in mol.%) nanopowders were obtained from low temperature calcination of a resin prepared using the Pechini's method. Firing the Zn1-xCoxO resin at 400 °C/2 h a powder with hexagonal structure was obtained as measured by X-ray diffraction (XRD). The powder presented average particle size of 40 nm observed by field emission scanning electronic microscopy (FE-SEM) micrographs and average crystallite size of 10 nm calculated from the XRD using Scherrer's equation. Nanocrystalline Zn1-xCo xO films with good homogeneity and optical quality were obtained with 280-980 nm thicknesses by electron beam physical vapour deposition (EBPVD) under vacuum onto silica substrate at 25 °C. Scanning electron microscopy with field emission gun showed that the film microstructure is composed by spherical grains and some needles. In these conditions of deposition the films presented only hexagonal phase observed by XRD. The UV-visible-NIR and diffuse reflectance properties of the films were measured and the electric properties were calculated using the reflectance and transmittance spectra.
Structure and luminescence of nanocrystalline gallium nitride synthesized by a novel polymer pyrolysis route

NASA Astrophysics Data System (ADS)

Garcia, Rafael; Hirata, Gustavo A.; Thomas, Alan C.; Ponce, Fernando A.

2006-10-01

Thermal decomposition in a horizontal quartz tube reactor of a polymer [-(CH 6N 4O) 3Ga(NO 3) 3-] in a nitrogen atmosphere, yield directly nano-structured gallium nitride (GaN) powder. The polymer was obtained by the reaction between high purity gallium nitrate (Ga(NO 3) 3) dissolved in toluene and carbohydrazide as an azotic ligand. The powder synthesized by this method showed a yellow color and elemental analysis suggested that the color is due to some carbon and oxygen impurities in the as-synthesized powder. Electron microscopy showed that the as-synthesized powders consist of a mixture of various porous particles containing nanowires and nano-sized platelets. The size of the crystallites can be controlled by annealing processes under ammonia. Photoluminescence analysis at 10 K on as-synthesized powders showed a broad red luminescence around 668 nm under UV laser excitation (He-Cd laser, 325 nm). However after annealing process the red luminescence disappears and the typical band edge emission of GaN around 357 nm (3.47 eV) and the UV band were the dominant emissions in the PL spectra.
Magnetic properties of Ni nanoparticles embedded in silica matrix (KIT-6) synthesized via novel chemical route

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

Dalavi, Shankar B.; Panda, Rabi N., E-mail: rnp@goa.bits-pilani.ac.in; Raja, M. Manivel

2015-06-24

Thermally stable Ni nanoparticles have been embedded in mesoporous silica matrix (KIT-6) via novel chemical reduction method by using superhydride as reducing agent. X-ray diffraction (XRD) study confirms that pure and embedded Ni nanoparticles crystallize in face centered cubic (fcc) structure. Crystallite sizes of pure Ni, 4 wt% and 8 wt% Ni in silica were estimated to be 6.0 nm, 10.4 nm and 10.5 nm, respectively. Morphology and dispersion of Ni in silica matrix were studied by scanning electron microscopy (SEM). Magnetic study shows enhancement of magnetic moments of Ni nanoparticles embedded in silica matrix compared with that of pure Ni. The resultmore » has been interpreted on the basis of size reduction and magnetic exchange effects. Saturation magnetization values for pure Ni, 4 wt% and 8 wt% Ni in silica were found to be 15.77 emu/g, 5.08 emu/g and 2.00 emu/g whereas coercivity values were 33.72 Oe, 92.47 Oe and 64.70 Oe, respectively. We anticipate that the observed magnetic properties may find application as soft magnetic materials.« less

Structure and magnetic properties of mechanically alloyed Co and Co-Ni

NASA Astrophysics Data System (ADS)

Guessasma, S.; Fenineche, N.

The influence of milling process on magnetic properties of Co and Co-Ni materials is studied. Coercivity, squareness ratio and crystallite size of mechanically alloyed Co-Ni material were related to milling time. For Co material, coercivity, cubic phase ratio and crystallite size were related to milling energy considering the vial and plateau rotation velocities. An artificial neural network (ANN) combining the parameters for both materials is used to predict magnetic and structure results versus milling conditions. Predicted results showed that milling energy is mostly dependent on the ratio vial to plateau rotation velocities and that milling times larger than 40 h do not add significant change to both structure and magnetic responses. Magnetic parameters were correlated to crystallite size and the D 6 law was only valid for small sizes.
Magnetic and critical properties of Pr0.6Sr0.4MnO3 nanocrystals prepared by a combination of the solid state reaction and the mechanical ball milling methods

NASA Astrophysics Data System (ADS)

Dung, Nguyen Thi; Linh, Dinh Chi; Huyen Yen, Pham Duc; Yu, Seong Cho; Van Dang, Nguyen; Dang Thanh, Tran

2018-06-01

Influence of the crystallite size on the magnetic and critical properties of nanocrystals has been investigated. The results show that Curie temperature and magnetization slightly decrease with decreasing average crystallite size . Based on the mean-field theory and the magnetic-field dependences of magnetization at different temperatures , we pointed out that the ferromagnetic-paramagnetic phase transition in the samples undergoes the second-order phase transition with the critical exponents (, , and ) close to those of the mean-field theory. However, there is a small deviation from those expected for the mean-field theory of the values of , and obtained for the samples. It means that short-range ferromagnetic interactions appear in the smaller particles. In other words, nanocrystals become more magnetically inhomogeneous with smaller crystallite sizes that could be explained by the presence of surface-related effects, lattice strain and distortions, which lead the strength of ferromagnetic interaction is decreased in the small crystallite sizes.
Effects of Eu3+ concentration on structural, optical and vibrational properties of multifunctional Ce(1-x)Eu(x)O2-delta) nanoparticles synthesized by thermolysis of 2,4-pentanedione complexes.

PubMed

Kremenovic, A; Bozanic, D K; Welsch, A M; Jancar, B; Nikolic, A S; Boskovic, M; Colomban, Ph; Fabian, Martin; Antic, B

2012-12-01

The 5-10 nm Ce(1-x)Eu(x)O(2-delta) (0 < or = x < or = 0.30) nanoparticles with fluorite structure were synthesized by thermal decomposition of Eu- and Ce-2,4-pentanedione complexes mixtures. X-ray line broadening analysis of mixed samples Ce(1-x)Eu(x)O(2-delta) (0.05 < or = x < or = 0.30) showed that the crystallite size was lower and root mean square strain higher than in pure ceria. However, within mixed samples Ce(1-x)Eu(x)O(2-delta) (0.05 < or = x < or = 0.30) crystallite size and root mean square strain were independent of Eu3+ concentration. Raman spectroscopy results indicated that europium ions yield disorder by breaking the phonon propagation and therefore making the non-centre Brillouin zone modes Raman active. The absorption bands in the spectra of mixed oxides were blue-shifted in comparison to pure CeO(2-delta) nanopowder. The samples show red emission typical for Eu ions. The biggest photoluminescent intensity was observed for the highest Eu3+ concentration (x = 0.30) and further enhanced with the increase in crystallinity.
Spin reorientation transition and hard magnetic properties of MnBi intermetallic compound

NASA Astrophysics Data System (ADS)

Suzuki, K.; Wu, X.; Ly, V.; Shoji, T.; Kato, A.; Manabe, A.

2012-04-01

The effects of mechanical grinding (MG) on the crystallite size, the spin reorientation transition temperature (TSR) and the hard magnetic properties in melt-spun low temperature phase (LTP) MnBi have been investigated in order to understand the origin of magnetic hardening induced by MG. The room-temperature coercive field (μ0Hcj) is enhanced dramatically from 0.08 T before MG to 1.5 T after MG for 43.2 ks while TSR is concurrently suppressed from 110 to 38 K. The coercive force exhibits positive temperature dependence approximately 50-60 K above TSR and the lowered TSR after MG could result in magnetic hardening at room temperature. The room-temperature coercive force of LTP-MnBi is highly dependent on the crystallite size (D) and is found to be described phenomenologically by the following relationship: μ0Hcj = μ0Ha(δ/D)n, where μ0Ha is ˜ 4 T, the Bloch wall width δ is 7 nm, and the exponent n is approximately 0.7. Our results suggest that the grain refinement is the primary origin of the hardening effect induced by MG with a possible minor hardening effect due to the suppression of the spin reorientation transition temperature.
Highly active lanthanum doped ZnO nanorods for photodegradation of metasystox.

PubMed

Korake, P V; Dhabbe, R S; Kadam, A N; Gaikwad, Y B; Garadkar, K M

2014-01-05

La-doped ZnO nanorods with different La contents were synthesized by microwave assisted method and characterized by various sophisticated techniques such as XRD, UV-Vis., EDS, XPS, SEM and TEM. The XRD patterns of the La-doped ZnO indicate hexagonal crystal structure with an average crystallite size of 30nm. It was found that the crystallite size of La-doped ZnO is much smaller as compared to pure ZnO and decreases with increasing La content. The photocatalytic activity of 0.5mol% La-doped ZnO in the degradation of metasystox was studied. It was observed that degradation efficiency of metasystox over La-doped ZnO increases up to 0.5mol% doping then decreases for higher doping levels. Among the catalyst studied, the 0.5mol% La-doped ZnO was the most active, showing high photocatalytic activity for the degradation of metasystox. The maximum reduction of concentration of metasystox was observed under static condition at pH 8. Reduction in the Chemical Oxygen Demand (COD) of metasystox was observed after 150min. The cytotoxicological studies of meristematic root tip cells of Allium cepa were studied. The results obtained indicate that photocatalytically degraded products of metasystox were less toxic as compared to metasystox. Copyright © 2013 Elsevier B.V. All rights reserved.
Solid State Reduction of MoO3 with Carbon via Mechanical Alloying to Synthesize Nano-Crystaline MoO2

NASA Astrophysics Data System (ADS)

Saghafi, M.; Ataie, A.; Heshmati-Manesh, S.

In this research, effect of milling time on solid state reduction of MoO3 with carbon has been investigated. It was found that mechanical activation of a mixture of MoO3 and carbon at ambient temperature by high energy ball milling was not able to reduce MoO3 to metallic molybdenum. MoO3 was converted to MoO2 at the first stage of reduction and peaks of the latter phase in X-ray diffraction patterns were detected when the milling time exceeded from 50 hours. The main effect of increased milling time at this stage was decreasing of MoO3 peak intensities and significant peak broadening due to decrease in size of crystallites. After prolonged milling, MoO3 was fully reduced to nano-crystalline MoO2 and its mean crystallite size was calculated using Williamson-Hall technique and found to be 17.5 nm. Thermodynamic investigations also confirm the possibility of reduction of MoO3 to MoO2 during the milling operation at room temperature. But, further reduction to metallic molybdenum requires thermal activation at higher temperature near 1100 K. XRD and SEM techniques were employed to evaluate the powder particles characteristics.
Effect of reaction atmosphere on structural and optical properties of hexagonal molybdenum oxide (h-MoO{sub 3})

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

Doss, V. Arumai; Chithambararaj, A.; Bose, A. Chandra, E-mail: acbose@nitt.edu

2016-05-23

The present work aims to synthesize single phase h-MoO{sub 3} nanocrytals by chemical precipitation method exposed under different reaction atmospheres. The reaction atmosphere have been successfully tuned as air, nitrogen and argon and studied its effects on structural, functional, morphology and optical properties by using X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and diffuse reflectance spectroscopy (DRS) measurements. The XRD result indicates that the sample exhibits characteristic hexagonal phase of MoO{sub 3}. The crystallite size is estimated by well known Scherrer’s method. The crystallite size is relative small in the case of sample prepared atmore » argon atmosphere. The functional groups such as Mo-O, N-H and O-H are identified from FT-IR spectroscopy. The particle exhibits rod like morphology with perfect hexagonal cross-section. The optical absorption observed at 420-450 nm corresponds to fundamental optical absorption by h-MoO{sub 3}. The band gap values are estimated using Kublka-Munk (K-M) function and found to be 2. 87 eV, 2.93 eV and 2.97 eV for samples synthesized under air, nitrogen and argon, respectively.« less
The Importance of Nanometric Passivating Films on Cathodes forLi - Air Batteries

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

Adams, Brian D.; Black, Robert; Radtke, Claudio

2014-12-23

Recently, there has been a transition from fully carbonaceous positive electrodes for the aprotic lithium oxygen battery to alternative materials and the use of redox mediator additives, in an attempt to lower the large electrochemical overpotentials associated with the charge reaction. However, the stabilizing or catalytic effect of these materials can become complicated due to the presence of major side-reactions observed during dis(charge). Here, we isolate the charge reaction from the discharge by utilizing electrodes prefilled with commercial lithium peroxide with a crystallite size of about 200-800 nm. Using a combination of S/TEM, online mass spectrometry, XPS, and electrochemical methodsmore » to probe the nature of surface films on carbon and conductive Ti-based nanoparticles, we show that oxygen evolution from lithium peroxide is strongly dependent on their surface properties. Insulating TiO2 surface layers on TiC and TiN - even as thin as 3 nm*can completely inhibit the charge reaction under these conditions. On the other hand, TiC, which lacks this oxide film, readily facilitates oxidation of the bulk Li2O2 crystallites, at a much lower overpotential relative to carbon. Since oxidation of lithium oxygen battery cathodes is inevitable in these systems, precise control of the surface chemistry at the nanoscale becomes of upmost importance.« less
Self-assembled mesoporous Co and Ni-ferrite spherical clusters consisting of spinel nanocrystals prepared using a template-free approach.

PubMed

Yu, Byong Yong; Kwak, Seung-Yeop

2011-10-21

Based on a self-assembly strategy, spherical mesoporous cobalt and nickel ferrite nanocrystal clusters with a large surface area and narrow size distribution were successfully synthesized for the first time via a template-free solvothermal process in ethylene glycol and subsequent heat treatment. In this work, the mesopores in the ferrite clusters were derived mainly from interior voids between aggregated primary nanoparticles (with crystallite size of less than 7 nm) and disordered particle packing domains. The concentration of sodium acetate is shown herein to play a crucial role in the formation of mesoporous ferrite spherical clusters. These ferrite clusters were characterized in detail using wide-angle X-ray diffraction, thermogravimetric-differential thermal analysis, (57)Fe Mössbauer spectroscopy, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy, standard and high-resolution transmission electron microscopy, and other techniques. The results confirmed the formation of both pure-phase ferrite clusters with highly crystalline spinel structure, uniform size (about 160 nm) and spherical morphology, and worm-like mesopore structures. The BET specific surface areas and mean pore sizes of the mesoporous Co and Ni-ferrite clusters were as high as 160 m(2) g(-1) and 182 m(2) g(-1), and 7.91 nm and 6.87 nm, respectively. A model for the formation of the spherical clusters in our system is proposed on the basis of the results. The magnetic properties of both samples were investigated at 300 K, and it was found that these materials are superparamagnetic. This journal is © The Royal Society of Chemistry 2011
Magneto-optical properties of α-Fe2O3@ZnO nanocomposites prepared by the high energy ball-milling technique

NASA Astrophysics Data System (ADS)

Chaudhury, Chandana Roy; Roychowdhury, Anirban; Das, Anusree; Das, Dipankar

2016-05-01

Magnetic-fluorescent nanocomposites (NCs) with 10 wt% of α-Fe2O3 in ZnO have been prepared by the high energy ball-milling. The crystallite sizes of α-Fe2O3 and ZnO in the NCs are found to vary from 65 nm to 20 nm and 47 nm to 15 nm respectively as milling time is increased from 2 to 30 h. XRD analysis confirms presence of α-Fe2O3 and ZnO in pure form in all the NCs. UV-vis study of the NCs shows a continuous blue-shift of the absorption peak and a steady increase of band gap of ZnO with increasing milling duration that are assigned to decreasing particle size of ZnO in the NCs. Photoluminescence (PL) spectra of the NCs reveal three weak emission bands in the visible region at 421, 445 and 485 nm along with the strong near band edge emission at 391 nm. These weak emission bands are attributed to different defect - related energy levels e.g. Zn-vacancy, Zn interstitial and oxygen vacancy. Dc and ac magnetization measurements show presence of weakly interacting superparamagnetic (SPM) α-Fe2O3 particles in the NCs. 57Fe-Mössbauer study confirms presence of SPM hematite in the sample milled for 30 h. Positron annihilation lifetime measurements indicate presence of cation vacancies in ZnO nanostructures confirming results of PL studies.
Comparison of 20 nm silver nanoparticles synthesized with and without a gold core: Structure, dissolution in cell culture media, and biological impact on macrophages

PubMed Central

Munusamy, Prabhakaran; Wang, Chongmin; Engelhard, Mark H.; Baer, Donald R.; Smith, Jordan N.; Liu, Chongxuan; Kodali, Vamsi; Thrall, Brian D.; Chen, Shu; Porter, Alexandra E.; Ryan, Mary P.

2015-01-01

Widespread use of silver nanoparticles raises questions of environmental and biological impact. Many synthesis approaches are used to produce pure silver and silver-shell gold-core particles optimized for specific applications. Since both nanoparticles and silver dissolved from the particles may impact the biological response, it is important to understand the physicochemical characteristics along with the biological impact of nanoparticles produced by different processes. The authors have examined the structure, dissolution, and impact of particle exposure to macrophage cells of two 20 nm silver particles synthesized in different ways, which have different internal structures. The structures were examined by electron microscopy and dissolution measured in Rosewell Park Memorial Institute media with 10% fetal bovine serum. Cytotoxicity and oxidative stress were used to measure biological impact on RAW 264.7 macrophage cells. The particles were polycrystalline, but 20 nm particles grown on gold seed particles had smaller crystallite size with many high-energy grain boundaries and defects, and an apparent higher solubility than 20 nm pure silver particles. Greater oxidative stress and cytotoxicity were observed for 20 nm particles containing the Au core than for 20 nm pure silver particles. A simple dissolution model described the time variation of particle size and dissolved silver for particle loadings larger than 9 μg/ml for the 24-h period characteristic of many in-vitro studies. PMID:26178265
Comparison of 20 nm silver nanoparticles synthesized with and without a gold core: Structure, dissolution in cell culture media, and biological impact on macrophages.

PubMed

Munusamy, Prabhakaran; Wang, Chongmin; Engelhard, Mark H; Baer, Donald R; Smith, Jordan N; Liu, Chongxuan; Kodali, Vamsi; Thrall, Brian D; Chen, Shu; Porter, Alexandra E; Ryan, Mary P

2015-09-15

Widespread use of silver nanoparticles raises questions of environmental and biological impact. Many synthesis approaches are used to produce pure silver and silver-shell gold-core particles optimized for specific applications. Since both nanoparticles and silver dissolved from the particles may impact the biological response, it is important to understand the physicochemical characteristics along with the biological impact of nanoparticles produced by different processes. The authors have examined the structure, dissolution, and impact of particle exposure to macrophage cells of two 20 nm silver particles synthesized in different ways, which have different internal structures. The structures were examined by electron microscopy and dissolution measured in Rosewell Park Memorial Institute media with 10% fetal bovine serum. Cytotoxicity and oxidative stress were used to measure biological impact on RAW 264.7 macrophage cells. The particles were polycrystalline, but 20 nm particles grown on gold seed particles had smaller crystallite size with many high-energy grain boundaries and defects, and an apparent higher solubility than 20 nm pure silver particles. Greater oxidative stress and cytotoxicity were observed for 20 nm particles containing the Au core than for 20 nm pure silver particles. A simple dissolution model described the time variation of particle size and dissolved silver for particle loadings larger than 9 μg/ml for the 24-h period characteristic of many in-vitro studies.
Influence of Zn doping on structural, optical and dielectric properties of LaFeO3

NASA Astrophysics Data System (ADS)

Manzoor, Samiya; Husain, Shahid

2018-05-01

The effect of Zn doping on structural, optical and dielectric properties of nano-crystalline LaFe1‑xZnxO3 (0.0 ≤ x ≤ 0.3) samples have been investigated. These samples are synthesized using conventional solid state reaction route. X-ray diffraction patterns with Rietveld analysis confirm the single phase nature of samples. Further, the sample formation has been confirmed by FTIR spectroscopy. All the samples are formed in orthorhombic crystal symmetry with Pbnm space group. The average crystallite sizes, calculated from the Scherer’s formula, lie in the range below 50 nm. Rietveld refinement technique is used to determine lattice parameters, bond lengths and unit cell volume. Williamson-Hall analysis has been performed to calculate the crystallite size and lattice strain. Crystallite sizes are found to be of nanometer range while the strain is of the order of 10‑3. Zn doping leads to the expansion of volume due to the tensile strain. Optical bandgap has been determined from Kubelka-Munk function using Tauc’s relation. Zinc doping in LaFeO3 leads to decrease in optical bandgap. Dielectric constant as a function of frequency is measured in the frequency range of 75 kHz–5 MHz. The dielectric behavior has been investigated by analyzing ‘universal dielectric response’ (UDR) model. The dielectric constant (ε‧) shows colossal value with Zn doping in the whole frequency range. However, the imaginary part (ε″) shows relaxational behavior which may be attributed to the strong correlation that exists between conduction mechanism and dielectric behavior in ferrites. Cole-Cole analysis has been done that confirms the dielectric material does not follow the ideal Debye theory but shows distribution of relaxation times. The a.c conductivity increases with frequency and with Zn doping due to the increased polaron hopping.
Study of energy versus misorientation for grain boundaries in gold by crystallite rotation method. I. (001) twist boundaries

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

Chan, S.W.; Balluffi, R.W.

1984-11-01

Small gold crystallites (approx. 50 to 80 nm dia) were welded to thin film (001) single crystal gold substrates at a series of predetermined (001) twist angles in the range 0 to 45/sup 0/. A pure (001) twist boundary therefore existed in each welded neck region which could be observed directly by transmission electron microscopy at normal incidence. Upon annealing, the crystallites rotated around (001) when the boundary energy varied with theta. The crystallites rotated into three misorientations corresponding to the special ..sigma..1 and ..sigma..5 misorientations and a symmetry related misorientation at theta=45/sup 0/. These results indicate the existence ofmore » grain boundary dislocation (GBD) related cusps on the boundary energy versus theta curve at ..sigma..1 and ..sigma..« less
Role of oxygen on microstructure and thermoelectric properties of silicon nanocomposites

NASA Astrophysics Data System (ADS)

Schierning, G.; Theissmann, R.; Stein, N.; Petermann, N.; Becker, A.; Engenhorst, M.; Kessler, V.; Geller, M.; Beckel, A.; Wiggers, H.; Schmechel, R.

2011-12-01

Phosphorus-doped silicon nanopowder from a gas phase process was compacted by DC-current sintering in order to obtain thermoelectrically active, nanocrystalline bulk silicon. A density between 95% and 96% compared to the density of single crystalline silicon was achieved, while preserving the nanocrystalline character with an average crystallite size of best 25 nm. As a native surface oxidation of the nanopowder usually occurs during nanopowder handling, a focus of this work is on the role of oxygen on microstructure and transport properties of the nanocomposite. A characterization with transmission electron microscopy (TEM) showed that the original core/shell structure of the nanoparticles was not found within the sintered nanocomposites. Two different types of oxide precipitates could be identified by energy filtered imaging technique. For a detailed analysis, 3-dimensional tomography with reconstruction was done using a needle-shaped sample prepared by focused ion beam (FIB). The 3-dimensional distribution of silicon dioxide precipitates confirmed that the initial core/shell structure breaks down and precipitates are formed. It is further found that residual pores are exclusively located within oxide precipitates. Thermoelectric characterization was done on silicon nanocomposites sintered between 960 °C and 1060 °C with varying oxygen content between room temperature and 950 °C. The higher sintering temperature led to a better electrical activation of the phosphorus dopant. The oxidic precipitates support densification and seem to be able to reduce the thermal conductivity therefore enhancing thermoelectric properties. A peak figure of merit, zT, of 0.5 at 950 °C was measured for a sample sintered at 1060 °C with a mean crystallite size of 46 nm.
Models for Amorphous Calcium Carbonate

NASA Astrophysics Data System (ADS)

Sinha, Sourabh

Many species e.g. sea urchin form amorphous calcium carbonate (ACC) precursor phases that subsequently transform into crystalline CaCO3. It is certainly possible that the biogenic ACC might have more than 10 wt% Mg and ˜3 wt% of water. The structure of ACC and the mechanisms by which it transforms to crystalline phase are still poorly understood. In this dissertation our goal is to determine an atomic structure model that is consistent with diffraction and IR measurements of ACC. For this purpose a calcite supercell with 24 formula units, containing 120 atoms, was constructed. Various configurations with substitution of Ca by 6 Mg ions (6 wt.%) and insertion of 3-5 H 2O molecules (2.25-3.75 wt.%) in the interstitial positions of the supercell, were relaxed using a robust density function code VASP. The most noticeable effects were the tilts of CO3 groups and the distortion of Ca sub-lattice, especially in the hydrated case. The distributions of Ca-Ca nearest neighbor distance and CO3 tilts were extracted from various configurations. The same methods were also applied to aragonite. Sampling from the calculated distortion distributions, we built models for amorphous calcite/aragonite of size ˜ 1700 nm3 based on a multi-scale modeling scheme. We used these models to generate diffraction patterns and profiles with our diffraction code. We found that the induced distortions were not enough to generate a diffraction profile typical of an amorphous material. We then studied the diffraction profiles from several nano-crystallites as recent studies suggest that ACC might be a random array of nano-cryatallites. It was found that the generated diffraction profile from a nano-crystallite of size ˜ 2 nm3 is similar to that from the ACC.
Micro structural analysis and magnetic characteristics of rare earth substituted cobalt ferrite

NASA Astrophysics Data System (ADS)

Tapdiya, Swati; Singh, Sarika; Kulshrestha, Shobha; Shrivastava, A. K.

2018-05-01

A series of ultrafine nanoparticles of Gd3+ doped Co-ferrites CoGdxFe2-xO4 (x=0.0, 0.05 and 0.10) were prepared by wet chemical co-precipitation method using nitrates of respective metal ions. Structural and morphology studies were performed using XRD, SEM and EDAX. Indexed XRD patterns confirm the formation of cubic spinel phase. Average crystallite sizes found to be decreases with trivalent rare earth ion substitution. Lattice constant (a) and lattice strain increases with increase in Gd3+ concentration due to large ionic radii (0.94nm) of Gd3+ replacing Fe3+ (0.64nm). SEM images show the spherical morphology and uniform growth of nanoparticles. Magnetic studies show that magnetization (Ms), decreases with increase in Gd3+ concentration from 50.16 emu/gm to 31.26 emu/gm.
Near band edge emission characteristics of sputtered nano-crystalline ZnO films

NASA Astrophysics Data System (ADS)

Kunj, Saurabh; Sreenivas, K.

2016-05-01

Sputtered zinc oxide (ZnO) thin films deposited on unheated glass substrate under different sputtering gas mixtures (Ar+O2) have been investigated using X-ray diffraction and photo luminescence spectroscopy. Earlier reported studies on ZnO films prepared by different techniques exhibit either a sharp/broad near band edge (NBE) emission peak depending on the crystalline quality of the film. In the present study zinc oxide films, grown on unheated substrates, are seen to possess a preferred (002) orientation with a microstructure consisting of clustered nano-sized crystallites. The splitting in the near band edge emission (NBE) into three characteristic peaks is attributed to quantum confinement effect, and is observed specifically under an excitation of 270 nm. Deep level emission (DLE) in the range 400 to 700 nm is not observed indicating absence of deep level radiative defects.
Effect of aging heat time and annealing temperature on the properties of nanocrystalline tin dioxide thin films

NASA Astrophysics Data System (ADS)

Kadhim, Imad H.; Abu Hassan, H.

2017-04-01

Nanocrystalline tin dioxide (SnO2) thin films have been successfully prepared by sol-gel spin-coating technique on p-type Si (100) substrates. A stable solution was prepared by mixing tin(II) chloride dihydrate, pure ethanol, and glycerin. Temperature affects the properties of SnO2 thin films, particularly the crystallite size where the crystallization of SnO2 with tetragonal rutile structure is achieved when thin films that prepared under different aging heat times are annealed at 400∘C. By increasing aging heat time in the presence of annealing temperatures the FESEM images indicated that the thickness of the fabricated film was directly proportional to solution viscosity, increasing from approximately 380 nm to 744 nm, as well as the crystallization of the thin films improved and reduced defects.
Inverse opal photonic crystals with photonic band gaps in the visible and near-infrared

NASA Astrophysics Data System (ADS)

Jarvis, Brandon C.; Gilleland, Cody L.; Renfro, Tim; Gutierrez, Jose; Parikh, Kunjal; Glosser, R.; Landon, Preston B.

2005-08-01

Colloidal silica spheres with 200nm, 250nm, and 290nm diameters were self-assembled with single crystal crystallites 4-5mm wide and 10-15mm long. Larger spheres with diameters between 1000-2300nm were self-assembled with single crystal crystallites up to 1.5mm wide and 2mm long. The silica opals self-assembled vertically along the [100] direction of the face centered cubic lattice resulting in self-templated opals. Inverse opal photonic crystals with a partial band gap possessing a maximum in the near infrared at 3.8μm were constructed from opal templates composed of 2300nm diameter spheres with chalcogenide Ge33As12Se55 (AMTIR-1), a transparent glass in the near infrared with high refractive index. Inverse gold and gold/ polypropylene composite photonic crystals were fabricated from synthetic opal templates composed of 200-290nm silica spheres. The reflectance spectra and electrical conductance of the resulting structures is presented. Gold was infiltrated into opal templates as gold chloride and heat converted to metallic gold. Opals partially infiltrated with gold were co-infiltrated with polypropylene plastic for mechanical support prior to removal of the silica template with hydrofluoric acid.

Optical and Morphological Properties of P3HT and P3HT: PCBM Thin Films Used in Photovoltaic Applications

NASA Astrophysics Data System (ADS)

Hrostea, L.; Girtan, M.; Mallet, R.; Leontie, L.

2018-06-01

This work is focused on the study of some physical properties of poly(3-hexylthiophene-2,5-diyl) (P3HT) and poly(e-hexylthiophene-2,5-diyl): Methanolfullerene Phenyl-C61-Butyric-Accid-Methyl-Ester (PCBM) blend thin films. Knowing the polymer advantages, such as ease of processing, high thermal stability, strong interaction with light, its properties have captured the attention regarding the changes that can occur in a polymer:fullerene blend in term of them. Polymer and polymer:fullerene blend (1:0.1, 1:0.2, 1:0.4 and 1:0.8 ratios) were deposited by spin coating on glass and SnO2:F (FTO) coated glass. The optical properties were emphasized using spectrophotometry (300 – 2200 nm wavelength range) and spectroscopic ellipsometry models, to obtain the refractive index, extinction coefficient and the transmission (found higher than 80%). According to X-ray diffraction analysis, as-obtained films are amorphous. Investigation of the surface morphology of thin-film samples using Atomic Force Microscopy revealed a crystallite-like surface morphology with crystallite size in the nanometer range.
One-step synthesis and characterizations of cerium oxide nanoparticles in an ambient temperature via Co-precipitation method

NASA Astrophysics Data System (ADS)

Pujar, Malatesh S.; Hunagund, Shirajahammad M.; Desai, Vani R.; Patil, Shivaprasadgouda; Sidarai, Ashok H.

2018-04-01

We report the simple Co-precipitation method for the synthesis of Cerium oxide (CeO2) nanoparticles (NPs) in an ambient temperature. We have taken the Cerium (III) nitrate hexahydrate (Ce(NO3)3.6H2O) and Sodium hydroxide (NaOH) as the precursors. The obtained NPs were analyzed using the UV-Vis spectrophotometer, Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The obtained results signify that UV-Vis spectrum exhibited a well-defined absorption peak at 274 nm and the estimated energy gap (Eg) is 4.05 eV. The FT-IR analysis provides the supporting evidence for the presence of bonding of O-H, nitrates, alcohols and O-Ce-O vibrations. The XRD result reveals that the synthesized CeO2 NPs was crystallite with cubic phase structure and the estimated average crystallite size of CeO2 NPs using Scherer's and W-H method was significantly different due to their assumptions. Further, it is purposed to study their photocatalytic biological activities.
Novel Synthesis and Structural Analysis of Ferrihydrite

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

Smith, Stacey J.; Page, Katharine; Kim, Hyunjeong

2012-07-25

Naturally occurring ferrihydrite is both impure and difficult to isolate, so the numerous applications and interesting properties of ferrihydrite have spurred the development of various synthetic techniques. Nearly all techniques are based on the hydrolysis of an iron salt and require careful control of temperature, pH, and concentration. In this Article, we report a new synthetic method which does not require such control and is perhaps the fastest and simplest route to synthesizing ferrhydrite. XRD, TEM, BET, and chemical purity characterizations show that the chemically pure, 2-line ferrihydrite product consists of crystallites 2-6 nm in diameter which aggregate to formmore » mesoporous, high surface area agglomerates that are attractive candidates for the many adsorption applications of ferrihydrite. X-ray PDF data were also collected for the ferrihydrite product and refined against the hexagonal structural model recently proposed by Michel et al. These analyses suggest that ferrihydrite has a consistent, repeatable structure independent of variation in the synthetic method, water content of the sample, or particle size of the crystallites, and this structure can be adequately described by the proposed hexagonal model.« less
Novel synthesis and structural analysis of ferrihydrite.

PubMed

Smith, Stacey J; Page, Katharine; Kim, Hyunjeong; Campbell, Branton J; Boerio-Goates, Juliana; Woodfield, Brian F

2012-06-04

Naturally occurring ferrihydrite is both impure and difficult to isolate, so the numerous applications and interesting properties of ferrihydrite have spurred the development of various synthetic techniques. Nearly all techniques are based on the hydrolysis of an iron salt and require careful control of temperature, pH, and concentration. In this Article, we report a new synthetic method which does not require such control and is perhaps the fastest and simplest route to synthesizing ferrhydrite. XRD, TEM, BET, and chemical purity characterizations show that the chemically pure, 2-line ferrihydrite product consists of crystallites 2-6 nm in diameter which aggregate to form mesoporous, high surface area agglomerates that are attractive candidates for the many adsorption applications of ferrihydrite. X-ray PDF data were also collected for the ferrihydrite product and refined against the hexagonal structural model recently proposed by Michel et al. These analyses suggest that ferrihydrite has a consistent, repeatable structure independent of variation in the synthetic method, water content of the sample, or particle size of the crystallites, and this structure can be adequately described by the proposed hexagonal model.
Physicochemical characterizations of nano-palm oil fuel ash

NASA Astrophysics Data System (ADS)

Rajak, Mohd Azrul Abdul; Majid, Zaiton Abdul; Ismail, Mohammad

2015-07-01

Palm Oil Fuel Ash (POFA) is known as a good supplementary cementing material due to its siliceous-rich content. The application of nanotechnology in the pozzolanic materials could invent new functions in the efficiency of physical and chemical properties of materials. Thus, the present study aims to generate nano-sized POFA and characterize the physicochemical properties of nano-palm oil fuel ash (nPOFA). The nPOFA was prepared by mechanically grinding micro POFA using a high intensity ball milling for 6 hours. The physicochemical properties of nPOFA were characterized via X-Ray Fluoresence (XRF), Scanning Emission microscopy- Energy Dispersive X-Ray (SEM-EDX), Transmission Electron Microscope (TEM) and X-Ray Diffraction (XRD). The particle size of nPOFA acquired from TEM analysis was in the range of 20 nm to 90 nm, while the average crystallite size calculated from XRD diffractogram was 61.5 nm. The resulting nPOFA has a BET surface area of 145.35 m2/g, which is more than 85% increment in surface area compared to micro-sized POFA. The morphology and elemental studies showed the presence of spherical as well as irregularly shaped and fine nPOFA particles contains with high silicon content. The presence of α-quartz as the major phase of the nPOFA was identified through XRD analysis. The study concludes that nPOFA has the potential as a supplementary cementing material due to the high silica content, high surface area and the unique behaviors of nano-structured particles.
Microstructural, optical and electrical transport properties of Cd-doped SnO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ahmad, Naseem; Khan, Shakeel; Mohsin Nizam Ansari, Mohd

2018-03-01

We have successfully investigated the structural, optical and dielectric properties of Cd assimilated SnO2 nanoparticles synthesized via very convenient precipitation route. The structural properties were studied by x-ray diffraction method (XRD) and Fourier Transform Infrared (FTIR) Spectroscopy. As-synthesized samples in the form of powder were examined for its morphology and average particle size by Transmission electron microscopy (TEM). The optical properties were studied by diffuse reflectance spectroscopy. Dielectric properties such that complex dielectric constant and ac conductivity were investigated by LCR meter. Average crystallite size calculated by XRD and average particle size obtained from TEM were found to be consistent and below 50 nm for all samples. The optical band gap of as-synthesized powder samples from absorption study was found in the range of 3.76 to 3.97 eV. The grain boundary parameters such that Rgb, Cgb and τ were evaluated using impedance spectroscopy.
Correlating sampling and intensity statistics in nanoparticle diffraction experiments

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

Öztürk, Hande; Yan, Hanfei; Hill, John P.

2015-07-28

It is shown in a previous article [Öztürk, Yan, Hill & Noyan (2014).J. Appl. Cryst.47, 1016–1025] that the sampling statistics of diffracting particle populations within a polycrystalline ensemble depended on the size of the constituent crystallites: broad X-ray peak breadths enabled some nano-sized particles to contribute more than one diffraction spot to Debye–Scherrer rings. Here it is shown that the equations proposed by Alexander, Klug & Kummer [J. Appl. Phys.(1948),19, 742–753] (AKK) to link diffracting particle and diffracted intensity statistics are not applicable if the constituent crystallites of the powder are below 10 nm. In this size range, (i) themore » one-to-one correspondence between diffracting particles and Laue spots assumed in the AKK analysis is not satisfied, and (ii) the crystallographic correlation between Laue spots originating from the same grain invalidates the assumption that all diffracting plane normals are randomly oriented and uncorrelated. Such correlation produces unexpected results in the selection of diffracting grains. For example, three or more Laue spots from a given grain for a particular reflection can only be observed at certain wavelengths. In addition, correcting the diffracted intensity values by the traditional Lorentz term, 1/cos θ, to compensate for the variation of particles sampled within a reflection band does not maintain fidelity to the number of poles contributing to the diffracted signal. A new term, cos θ B/cos θ, corrects this problem.« less
Finely Tuned SnO2 Nanoparticles for Efficient Detection of Reducing and Oxidizing Gases: The Influence of Alkali Metal Cation on Gas-Sensing Properties.

PubMed

Lee, Szu-Hsuan; Galstyan, Vardan; Ponzoni, Andrea; Gonzalo-Juan, Isabel; Riedel, Ralf; Dourges, Marie-Anne; Nicolas, Yohann; Toupance, Thierry

2018-03-28

Tin dioxide (SnO 2 ) nanoparticles were straightforwardly synthesized using an easily scaled-up liquid route that involves the hydrothermal treatment, either under acidic or basic conditions, of a commercial tin dioxide particle suspension including potassium counterions. After further thermal post-treatment, the nanomaterials have been thoroughly characterized by Fourier transform infrared and Raman spectroscopy, powder X-ray diffraction, transmission electron microscopy, X-ray photoelectron spectroscopy, and nitrogen sorption porosimetry. Varying pH conditions and temperature of the thermal treatment provided cassiterite SnO 2 nanoparticles with crystallite sizes ranging from 7.3 to 9.7 nm and Brunauer-Emmett-Teller surface areas ranging from 61 to 106 m 2 ·g -1 , acidic conditions favoring potassium cation removal. Upon exposure to a reducing gas (H 2 , CO, and volatile organic compounds such as ethanol and acetone) or oxidizing gas (NO 2 ), layers of these SnO 2 nanoparticles led to highly sensitive, reversible, and reproducible responses. The sensing results were discussed in regard to the crystallite size, specific area, valence band energy, Debye length, and chemical composition. Results highlight the impact of the counterion residuals, which affect the gas-sensing performance to an extent much higher than that of size and surface area effects. Tin dioxide nanoparticles prepared under acidic conditions and calcined in air showed the best sensing performances because of lower amount of potassium cations and higher crystallinity, despite the lower surface area.
Optical, electrical and magnetic properties of nanostructured Mn3O4 synthesized through a facile chemical route

NASA Astrophysics Data System (ADS)

Bose, Vipin C.; Biju, V.

2015-02-01

Nanostructured Mn3O4 sample with an average crystallite size of ˜15 nm is synthesized via the reduction of potassium permanganate using hydrazine. The average particle size obtained from the Transmission Electron Microscopy analysis is in good agreement with the average crystallite size estimated from X-ray diffraction analysis. The presence of Mn4+ ions at the octahedral sites is inferred from the results of Raman, UV-visible absorption and X-ray photoelectron spectroscopy analyzes. DC electrical conductivity of the sample in the temperature range 313-423 K, is about five orders of magnitude larger than that reported for single crystalline Mn3O4 sample. The dominant conduction mechanism is identified to be of the polaronic hopping of holes between cations in the octahedral sites. The zero field cooled and field cooled magnetization of the sample is studied in the range 20-300 K. The Curie temperature for the sample is about 45 K, below which the sample is ferrimagnetic. A blocking temperature of 35 K is observed in the field cooled curve. It is observed that the sample shows hysteresis at temperatures below the Curie temperature with no saturation, even at an applied field (20 kOe). The presence of an ordered core and disordered surface of spin arrangements is observed from the magnetization studies. Above the Curie temperature, the sample shows linear dependence of magnetization on applied field with no hysteresis characteristic of paramagnetic phase.
Mössbauer study of Cu1-xZnxFe2O4 catalytic materials

NASA Astrophysics Data System (ADS)

Koleva, K.; Velinov, N.; Tsoncheva, T.; Mitov, I.

2014-04-01

Copper zinc ferrites (Cu1-xZnxFe2O4) with different composition (x = 1; 0.2; 0.5; 0.8) were prepared by conventional thermal method. Formation of well crystallized ferrite phase with cubic structure and crystallites size of about 19.08-24.39 nm was observed by Powder X-ray diffraction and Mössbauer spectroscopy. The ferrite materials were tested as catalysts in methanol decomposition to CO and H2. A strong dependence of the catalytic behaviour of Cu1-xZnxFe2O4 ferrites of their composition and the phase transformations which occurred under the reaction medium was established.
Nickel antimony oxide (NiSb2O6): A fascinating nanostructured material for gas sensing application

NASA Astrophysics Data System (ADS)

Singh, Archana; Singh, Ajendra; Singh, Satyendra; Tandon, Poonam

2016-02-01

Fabrication of nanocrystalline NiSb2O6 thin films via sol-gel spin coating method towards the development of liquefied petroleum gas (LPG) sensor operable at room temperature (25 °C) is being reported. Nanostructural, surface morphological and optical properties of trirutile-type NiSb2O6 have been investigated in order to explore the parameters of interest. The crystallite size has been found to be 19 nm. A detailed sensing performance (sensitivity, sensor response, response and recovery times, reproducibility and long term stability) of NiSb2O6 nanostructures grown on alumina substrate has been investigated.
Iron Oxide Nanoparticles: Tunable Size Synthesis and Analysis in Terms of the Core-Shell Structure and Mixed Coercive Model

NASA Astrophysics Data System (ADS)

Phong, P. T.; Oanh, V. T. K.; Lam, T. D.; Phuc, N. X.; Tung, L. D.; Thanh, Nguyen T. K.; Manh, D. H.

2017-04-01

Iron oxide nanoparticles (NPs) are currently a very active research field. To date, a comprehensive study of iron oxide NPs is still lacking not only on the size dependence of structural phases but also in the use of an appropriate model. Herein, we report on a systematic study of the structural and magnetic properties of iron oxide NPs prepared by a co-precipitation method followed by hydrothermal treatment. X-ray diffraction and transmission electron microscopy reveal that the NPs have an inverse spinel structure of iron oxide phase (Fe3O4) with average crystallite sizes ( D XRD) of 6-19 nm, while grain sizes ( D TEM) are of 7-23 nm. In addition, the larger the particle size, the closer the experimental lattice constant value is to that of the magnetite structure. Magnetic field-dependent magnetization data and analysis show that the effective anisotropy constants of the Fe3O4 NPs are about five times larger than that of their bulk counterpart. Particle size ( D) dependence of the magnetization and the non-saturating behavior observed in applied fields up to 50 kOe are discussed using the core-shell structure model. We find that with decreasing D, while the calculated thickness of the shell of disordered spins ( t ˜ 0.3 nm) remains almost unchanged, the specific surface areas S a increases significantly, thus reducing the magnetization of the NPs. We also probe the coercivity of the NPs by using the mixed coercive Kneller and Luborsky model. The calculated results indicate that the coercivity rises monotonously with the particle size, and are well matched with the experimental ones.
THE CHARACTERIZATION OF A SOLID SORBENT WITH CRYSTALLITE SIZE AND STRAIN DATA FROM X-RAY DIFFRACTION LINE BROADENING

EPA Science Inventory

The paper gives results of the characterization of a solid sorbent with crystallite size and strain data from x-ray diffraction line broadening, as part of an EPA investigation of the injection of dry Ca(OH)2 into coal-fired electric power plant burners for the control of SO2 emi...
Thin Film Research. Volume 1

DTIC Science & Technology

1985-05-30

Order (FECO) ......... 23 3. X -Ray Diffraction ............................... 26 4. Transmission Electron Microscopy (TEM) ............... 26 5...remained amorphous after bombardment, as evidenced by X - ray diffraction, and showed no other changes. 0 (2) For Sb203, the crystallite size was reduced...main effect on MgF2 was the reduction in crystallite size. The films were too thir. for meaningful x - ray diffraction analysis. Durability and
Effect of sample moisture content on XRD-estimated cellulose crystallinity index and crystallite size

Treesearch

Umesh P. Agarwal; Sally A. Ralph; Carlos Baez; Richard S. Reiner; Steve P. Verrill

2017-01-01

Although X-ray diffraction (XRD) has been the most widely used technique to investigate crystallinity index (CrI) and crystallite size (L200) of cellulose materials, there are not many studies that have taken into account the role of sample moisture on these measurements. The present investigation focuses on a variety of celluloses and cellulose...
Synthesis of Ag-Cu-Pd alloy thin films by DC-magnetron sputtering: Case study on microstructures and optical properties

NASA Astrophysics Data System (ADS)

Rezaee, Sahar; Ghobadi, Nader

2018-06-01

The present study aims to investigate optical properties of Ag-Cu-Pd alloy thin films synthesized by DC-magnetron sputtering method. The thin films are deposited on the glass and silicon substrates using Argon gas and Ag-Cu-Pd target. XRD analysis confirms the successful growth of Ag, Cu, and Pd NPs with FCC crystalline structure. Moreover, UV-visible absorption spectroscopy is applied to determine optical properties of the prepared samples which are affected by changes in surface morphology. The existence of single surface plasmon resonance (SPR) peak near 350 nm proves the formation of silver nanoparticles with a slight red shift through increasing deposition time. Ineffective thickness method (ITM) and Derivation of ineffective thickness method (DITM) are applied to extract optical band gap and transition type via absorption spectrum. SEM and AFM analyses show the distribution of near-spherical nanoparticles covering the surface of thin films. Furthermore, thickness variation affects the grain size. In addition, TEM image reveals the uniform size distribution of nanoparticles with an average particle size of about 15 nm. The findings show that increasing grain size and crystallite order along with the decrease of structural defect and disorders decrease optical band gap from 3.86 eV to 2.58 eV.
On the peculiarities of galvanomagnetic effects in high magnetic fields in twisting bicrystals of the 3D topological insulator Bi{sub 1–x}Sb{sub x} (0.07 ≤ x ≤ 0.2)

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

Muntyanu, F. M., E-mail: muntean-teodor@yahoo.com; Gheorghitsa, E. I.; Gilewski, A.

2017-04-15

Galvanomagnetic effects in twisting bicrystals of Bi{sub 1–x}Sb{sub x} alloys (0.07 ≤ x ≤ 0.2) at low temperatures and in magnetic fields up to 40 T are studied. It is found that, at small crystallite misorientation angles, the semiconductor–semimetal transition is induced in the central layer (~60-nm-thick) and two adjacent layers (each ~20-nm-thick) of the interface at different values of ultraquantum magnetic field. Bicrystals with large misorientation angles, being located in strong magnetic fields, exhibit quantum oscillations of the magnetoresistance and the Hall effect, thus indicating that the density of states is higher and charge carriers are heavier in themore » adjacent layers of the interfaces than in the crystallites. Our results show also that twisting bicrystals contain regions with different densities of quantum electronic states, which are determined by the crystallite misorientation angle and magnetic-field strength.« less
Synthesis of antimony-doped tin oxide (ATO) nanoparticles by the nitrate-citrate combustion method

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

Zhang Jianrong; Gao Lian

2004-12-02

Antimony-doped tin oxide (ATO) nanoparticles having rutile structure have been synthesized by the combustion method using citric acid (CA) as fuel and nitrate as an oxidant, the metal sources were granulated tin and Sb{sub 2}O{sub 3}. The influence of citric acid (fuel) to metal ratio on the average crystallite size, specific surface area and morphology of the nanoparticles has been investigated. X-ray diffraction showed the tin ions were reduced to elemental tin during combustion reaction. The average ATO crystallite size increased with the increase of citric acid (fuel). Powder morphology and the comparison of crystallite size and grain size showsmore » that the degree of agglomeration of the powder decreased with an increase of the ratio. The highest specific surface area was 37.5 m{sup 2}/g when the citric acid to tin ratio was about 6.« less
Studying the morphological features of plasma treated silver and PEGylated silver nanoparticles: antibacterial activity

NASA Astrophysics Data System (ADS)

Waseem, M.; Awan, T.; Yasin, H. M.; Rehman, N. U.

2018-03-01

A strategy to treat the silver and PEGylated silver nanoparticles with plasma was being purposed. Oil in water (o/w) microemulsion method was used for the synthesis of Ag nanoparticles (AgNPs). Polyethylene glycol (PEG) having molecular weight 600 was used to coat the surface of AgNPs. Optical emission spectroscopy (OES) was used to characterize the plasma and it is noted that plasma treatment is useful to modify the structural characteristic of silver nanoparticles. The nanoparticles were treated with helium-oxygen mixture plasma, generated in plasma needle at atmospheric pressure. Both AgNPs and PEGylated AgNPs before and after plasma treatment were characterized by x-rays diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared (FTIR) spectroscopy. The crystallite size of silver nanoparticles after the treatment of plasma decreases from 71 nm to 27 nm. The SEM micrographs show that the size of Ag nanoparticles was nearly 118 nm whereas the thickness of the silver needle was around 135 nm. All the characteristics IR bands associated to the silver nanoparticles were detected. The FTIR spectrum also support the accumulation of OH radicals in the plasma treated samples. The samples before and after plasma treatment were screened against Gram positive (Bacillus Subtilis and Staphylococcus Aureus) and Gram negative (Escherichia Coli and Pseudomonas Aeruginosa) bacteria. The promising response was detected when plasma treated PEGylated AgNPs was tested against bacterial strains.
Comparative study of Ni and Cu doped ZnO nanoparticles: Structural and optical properties

NASA Astrophysics Data System (ADS)

Thakur, Shaveta; Thakur, Samita; Sharma, Jyoti; Kumar, Sanjay

2018-05-01

Nanoparticles of undoped and doped (0.1 M Ni2+ and Cu2+) ZnO are synthesized using chemical precipitation method. The crystallite size, morphology, chemical bonding and optical properties of as prepared nanoparticles are determined by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectroscopy and UV-visible spectra. XRD analysis shows that the prepared samples are single phase and have hexagonal wurtzite structure. The crystallite size of the doped and undoped nanoparticles is determined using Scherrer method. The crystallite size is found to be increased with concentration of nickel and copper. All stretching and vibrational bands are observed at their specific positions through FTIR. The increase in band gap can be attributed to the different chemical nature of dopant and host cation.

Structural and electrical properties of nickel substituted cadmium ferrite

NASA Astrophysics Data System (ADS)

Chethan, B.; Raj Prakash, H. G.; Vijayakumari, S. C.; Ravikiran, Y. T.

2018-05-01

Spinal nano-sized Cadmium ferrite (CD) and Nickel substituted cadmium ferrite (NSCF) were fabricated by sol-gel auto combustion method. The formation of spinal structure of ferrite materials was confirmed by X-ray diffraction (XRD) analysis. The crystallites size of CF and NSCF as determined by Scherrer's formula were found to be 24.73 nm and 17.70 nm respectively. comparative study of Fourier transform infrared spectroscopy (FTIR) of CF and NSCF revealed tetrahedral absorption bands shifted slightly towards higher frequency where as octahedral bands shifted towards lower frequency side confirming interfacial interaction between Ni and CF. The AC conductivity (σ), loss tangent (tan δ) and complex plane impedance plots for both CF and NSCF are determined at various frequencies ranging from 50 kHz to 5 MHz and comparatively analyzed. The increase in AC conductivity of the NSCF nano particles as compared to CF was explained in the light of hopping model. The impedance measurement of NSCF show presence of a semi-circle corresponding to the grain boundary resistance and hence shows that the conductivity takes place largely through grain boundaries.
One-pot green synthesis of zinc oxide nano rice and its application as sonocatalyst for degradation of organic dye and synthesis of 2-benzimidazole derivatives

NASA Astrophysics Data System (ADS)

Paul, Bappi; Vadivel, Sethumathavan; Dhar, Siddhartha Sankar; Debbarma, Shyama; Kumaravel, M.

2017-05-01

In this paper, we report novel and green approach for one-pot biosynthesis of zinc oxide (ZnO) nanoparticles (NPs). Highly stable and hexagonal phase ZnO nanoparticles were synthesized using seeds extract from the tender pods of Parkia roxburghii and characterized by XRD, FT-IR, EDX, TEM, and N2 adsorption-desorption (BET) studies. The present method of synthesis of ZnO NPs is very efficient and cost effective. The powder XRD pattern furnished evidence for the formation of hexagonal close packing structure of ZnO NPs having average crystallite size 25.6 nm. The TEM image reveals rice shapes ZnO NPs are with an average diameter of 40-60 nm. The as-synthesized ZnO NPs has proved to be an excellent sonocatalysts for degradation of organic dye and synthesis of 2-benzimidazole derivatives.
Spectroscopic studies on some fluorescent mixed-ligand titanium(IV) complexes.

PubMed

Baranwal, Balram Prasad; Singh, Alok Kumar; Varma, Anand

2011-12-15

A novel route to synthesize some titanium(IV) complexes containing acetylacetone, straight chain carboxylic acid and hydroxycarboxylic acid ligands has been investigated. Complexes with the general formula [Ti(acac)Cl(2-n)(OOCR*)(n)(OOCC(15)H(31))] (where Hacac=acetylacetone, R*COOH=hydroxycarboxylic acids and n=1 or 2) have been isolated and characterized. Molecular weight determinations indicated mononuclear nature of the complexes. LMCT bands were observed in the electronic spectra. Infrared spectra suggested bidentate nature of the ligands. Fluorescent behaviour of the complexes was noticed on the basis of fluorescence spectra. Powder XRD indicated them to be semi-crystalline having the crystallite size in 136-185 nm range. Transmission electron microscopy (TEM) indicated spherical particles of ~ 200 nm diameter. On the basis of physico-chemical studies, it is suggested that titanium is having coordination number 7 or 8 in these complexes. Copyright © 2011 Elsevier B.V. All rights reserved.
Structural analysis of nanocrystalline ZnTe alloys synthesized by melt quenching technique

NASA Astrophysics Data System (ADS)

Singh, Harinder; Singh, Tejbir; Thakur, Anup; Sharma, Jeewan

2018-05-01

Nanocrystalline ZnxTe100-x (x=0, 5, 20, 30, 40, 50) alloys have been synthesized using melt quenching technique. Energy-dispersive X-Ray spectroscopy (EDS) has been used to verify the elemental composition of samples. Various absorption modes are recorded from Fourier transform infrared spectroscopy (FTIR) confirming the formation of ZnTe. The structural study has been performed using X-Ray Diffraction (XRD) method. All synthesized samples have been found to be nanocrystalline in nature with average crystallite size in the range from 49.3 nm to 77.1 nm. Results have shown that Zn0Te100 exhibits hexagonal phase that transforms into a cubic ZnTe phase as the amount of zinc is increased. Pure ZnTe phase has been obtained for x = 50. The texture coefficient (Tc) has been calculated to find the prominent orientations of different planes.
Study of Zn-Cu Ferrite Nanoparticles for LPG Sensing

PubMed Central

Jain, Anuj; Baranwal, Ravi Kant; Bharti, Ajaya; Vakil, Z.; Prajapati, C. S.

2013-01-01

Nanostructured zinc-copper mixed ferrite was synthesized using sol-gel method. XRD patterns of different compositions of zinc-copper ferrite, Zn(1−x)CuxFe2O4 (x = 0.0, 0.25, 0.50, 0.75), revealed single phase inverse spinel ferrite in all the samples synthesized. With increasing copper concentration, the crystallite size was found to be increased from 28 nm to 47 nm. The surface morphology of all the samples studied by the Scanning Electron Microscopy there exhibits porous structure of particles throughout the samples. The pellets of the samples are prepared for LPG sensing characteristics. The sensing is carried out at different operating temperatures (200, 225, and 250°C) with the variation of LPG concentrations (0.2, 0.4, and 0.6 vol%). The maximum sensitivity of 55.33% is observed at 250°C operating for the 0.6 vol% LPG. PMID:23864833
Nanoscale arrays of antimony telluride single crystals by selective chemical vapor deposition

PubMed Central

Huang, Ruomeng; Benjamin, Sophie L.; Gurnani, Chitra; Wang, Yudong; Hector, Andrew L.; Levason, William; Reid, Gillian; De Groot, C. H. (Kees)

2016-01-01

Arrays of individual single nanocrystals of Sb2Te3 have been formed using selective chemical vapor deposition (CVD) from a single source precursor. Crystals are self-assembled reproducibly in confined spaces of 100 nm diameter with pitch down to 500 nm. The distribution of crystallite sizes across the arrays is very narrow (standard deviation of 15%) and is affected by both the hole diameter and the array pitch. The preferred growth of the crystals in the <1 1 0> orientation along the diagonal of the square holes strongly indicates that the diffusion of adatoms results in a near thermodynamic equilibrium growth mechanism of the nuclei. A clear relationship between electrical resistivity and selectivity is established across a range of metal selenides and tellurides, showing that conductive materials result in more selective growth and suggesting that electron donation is of critical importance for selective deposition. PMID:27283116
Synthesis characterization and luminescence studies of gamma irradiated nanocrystalline yttrium oxide

NASA Astrophysics Data System (ADS)

Shivaramu, N. J.; Lakshminarasappa, B. N.; Nagabhushana, K. R.; Singh, Fouran

2016-02-01

Nanocrystalline Y2O3 is synthesized by solution combustion technique using urea and glycine as fuels. X-ray diffraction (XRD) pattern of as prepared sample shows amorphous nature while annealed samples show cubic nature. The average crystallite size is calculated using Scherrer's formula and is found to be in the range 14-30 nm for samples synthesized using urea and 15-20 nm for samples synthesized using glycine respectively. Field emission scanning electron microscopy (FE-SEM) image of 1173 K annealed Y2O3 samples show well separated spherical shape particles and the average particle size is found to be in the range 28-35 nm. Fourier transformed infrared (FTIR) and Raman spectroscopy reveals a stretching of Y-O bond. Electron spin resonance (ESR) shows V- center, O2- and Y2 + defects. A broad photoluminescence (PL) emission with peak at 386 nm is observed when the sample is excited with 252 nm. Thermoluminescence (TL) properties of γ-irradiated Y2O3 nanopowder are studied at a heating rate of 5 K s- 1. The samples prepared by using urea show a prominent and well resolved peak at 383 K and a weak one at 570 K. It is also found that TL glow peak intensity (Im1) at 383 K increases with increase in γ-dose up to 6.0 kGy and then decreases with increase in dose. However, glycine used Y2O3 shows a prominent TL glow with peaks at 396 K and 590 K. Among the fuels, urea used Y2O3 shows simple and well resolved TL glows. This might be due to fuel and hence particle size effect. The kinetic parameters are calculated by Chen's glow curve peak shape method and results are discussed in detail.
Microwave assisted scalable synthesis of titanium ferrite nanomaterials

NASA Astrophysics Data System (ADS)

Shukla, Abhishek; Bhardwaj, Abhishek K.; Singh, S. C.; Uttam, K. N.; Gautam, Nisha; Himanshu, A. K.; Shah, Jyoti; Kotnala, R. K.; Gopal, R.

2018-04-01

Titanium ferrite magnetic nanomaterials are synthesized by one-step, one pot, and scalable method assisted by microwave radiation. Effects of titanium content and microwave exposure time on size, shape, morphology, yield, bonding nature, crystalline structure, and magnetic properties of titanium ferrite nanomaterials are studied. As-synthesized nanomaterials are characterized by X-ray diffraction (XRD), ultraviolet-visible absorption spectroscopy (UV-Vis), attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), Raman spectroscopy, transmission electron microscopy (TEM), and vibrating sample magnetometer measurements. XRD measurements depict the presence of two phases of titanium ferrite into the same sample, where crystallite size increases from ˜33 nm to 37 nm with the increase in titanium concentration. UV-Vis measurement showed broad spectrum in the spectral range of 250-600 nm which reveals that its characteristic peaks lie between ultraviolet and visible region; ATR-FTIR and Raman measurements predict iron-titanium oxide structures that are consistent with XRD results. The micrographs of TEM and selected area electron diffraction patterns show formation of hexagonal shaped particles with a high degree of crystallinity and presence of multi-phase. Energy dispersive spectroscopy measurements confirm that Ti:Fe compositional mass ratio can be controlled by tuning synthesis conditions. Increase of Ti defects into titanium ferrite lattice, either by increasing titanium precursor or by increasing exposure time, enhances its magnetic properties.
Improved conversion efficiency of dye sensitized solar cell using Zn doped TiO2-ZrO2 nanocomposite

NASA Astrophysics Data System (ADS)

Tomar, Laxmi J.; Bhatt, Piyush J.; Desai, Rahul K.; Chakrabarty, B. S.; Panchal, C. J.

2016-05-01

TiO2-ZrO2 and Zn doped TiO2-ZrO2 nanocomposites were prepared by hydrothermal method for dye sensitized solar cell (DSSC) application. The structural and optical properties were investigated by X -ray diffraction (XRD) and UV-Visible spectroscopy respectively. XRD results revealed the formation of material in nano size. The average crystallite size is 22.32 nm, 17.41 nm and 6.31 nm for TiO2, TiO2-ZrO2 and Zn doped TiO2-ZrO2 nanocomposites respectively. The optical bandgap varies from 2.04 eV to 3.75 eV. Dye sensitized solar cells were fabricated using the prepared material. Pomegranate juice was used as a sensitizer and graphite coated conducting glass plate was used as counter electrode. The I - V characteristics were recorded to measure photo response of DSSC. Photovoltaic parameter like open circuit voltage, power conversion efficiency, and fill factor were evaluated for fabricated solar cell. The power conversion efficiency of DSSC fabricated with TiO2, TiO2-ZrO2 and Zn doped TiO2-ZrO2 nanocomposites were found 0.71%, 1.97% and 4.58% respectively.
Effect of film thickness on structural and mechanical properties of AlCrN nanocompoite thin films deposited by reactive DC magnetron sputtering

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

Prakash, Ravi; Kaur, Davinder, E-mail: dkaurfph@iitr.ac.in

2016-05-06

In this study, the influence of film thickness on the structural, surface morphology and mechanical properties of Aluminum chromium nitride (AlCrN) thin films has been successfully investigated. The AlCrN thin films were deposited on silicon (100) substrate using dc magnetron reactive co-sputtering at substrate temperature 400° C. The structural, surface morphology and mechanical properties were studied using X-ray diffraction, field-emission scanning electron microscopy and nanoindentation techniques respectively. The thickness of these thin films was controlled by varying the deposition time therefore increase in deposition time led to increase in film thickness. X-ray diffraction pattern of AlCrN thin films with differentmore » deposition time shows the presence of (100) and (200) orientations. The crystallite size varies in the range from 12.5 nm to 36.3 nm with the film thickness due to surface energy minimization with the higher film thickness. The hardness pattern of these AlCrN thin films follows Hall-Petch relation. The highest hardness 23.08 Gpa and young modulus 215.31 Gpa were achieved at lowest grain size of 12.5 nm.« less
Photoconductivity in reactively evaporated copper indium selenide thin films

NASA Astrophysics Data System (ADS)

Urmila, K. S.; Asokan, T. Namitha; Pradeep, B.; Jacob, Rajani; Philip, Rachel Reena

2014-01-01

Copper indium selenide thin films of composition CuInSe2 with thickness of the order of 130 nm are deposited on glass substrate at a temperature of 423 ±5 K and pressure of 10-5 mbar using reactive evaporation, a variant of Gunther's three temperature method with high purity Copper (99.999%), Indium (99.999%) and Selenium (99.99%) as the elemental starting materials. X-ray diffraction (XRD) studies shows that the films are polycrystalline in nature having preferred orientation of grains along the (112) plane. The structural type of the film is found to be tetragonal with particle size of the order of 32 nm. The structural parameters such as lattice constant, particle size, dislocation density, number of crystallites per unit area and strain in the film are also evaluated. The surface morphology of CuInSe2 films are studied using 2D and 3D atomic force microscopy to estimate the grain size and surface roughness respectively. Analysis of the absorption spectrum of the film recorded using UV-Vis-NIR Spectrophotometer in the wavelength range from 2500 nm to cutoff revealed that the film possess a direct allowed transition with a band gap of 1.05 eV and a high value of absorption coefficient (α) of 106 cm-1 at 570 nm. Photoconductivity at room temperature is measured after illuminating the film with an FSH lamp (82 V, 300 W). Optical absorption studies in conjunction with the good photoconductivity of the prepared p-type CuInSe2 thin films indicate its suitability in photovoltaic applications.
Effect of Front-Side Silver Metallization on Underlying n+-p Junction in Multicrystalline Silicon Solar Cells: Preprint

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

Jiang, C. S.; Li, Z. G.; Moutinho, H. R.

2012-06-01

We report on the effect of front-side Ag metallization on the underlying n+-p junction of multicrystalline Si solar cells. The junction quality beneath the contacts was investigated by characterizing the uniformities of the electrostatic potential and doping concentration across the junction, using scanning Kelvin probe force microscopy and scanning capacitance microscopy. We investigated cells with a commercial Ag paste (DuPont PV159) and fired at furnace setting temperatures of 800 degrees, 840 degrees, and 930 degrees C, which results in actual cell temperatures ~100 degrees C lower than the setting temperature and the three cells being under-, optimal-, and over-fired. Wemore » found that the uniformity of the junction beneath the Ag contact was significantly degraded by the over-firing, whereas the junction retained good uniformity with the optimal- and under-fire temperatures. Further, Ag crystallites with widely distributed sizes from <100 nm to several μm were found at the Ag/Si interface of the over-fired cell. Large crystallites were imaged as protrusions into Si deeper than the junction depth. However, the junction was not broken down; instead, it was reformed on the entire front of the crystallite/Si interface. We propose a mechanism of the junction-quality degradation, based on emitter Si melting at the temperature around the Ag-Si eutectic point during firing, and subsequent recrystallization with incorporation of impurities in the Ag paste and with formation of crystallographic defects during quenching.« less
Hierarchically 3D assembled strontium titanate nanomaterials for water splitting application

NASA Astrophysics Data System (ADS)

Moniruddin, Md; Afroz, Khurshida; Shabdan, Yerkin; Bizri, Baraa; Nuraje, Nurxat

2017-10-01

Water splitting is an important technique to store solar energy in the simple form of chemical energy, such as hydrogen. Strontium titanate (SrTiO3) is one of the most promising photocatalysts to produce hydrogen gas from water splitting. In this research, an electrospinning technique in combination with sol-gel method was developed to synthesize 3D porous SrTiO3 nanostructures. Different crystallite sizes of SrTiO3-nanofibers (STO-NFs) were produced by varying the synthesis parameters including precursor concentration and calcination temperature. The synthesized nanofibers were characterized using DSC, TGA, XRD, SEM, and TEM. The crystallite size of STO-NFs decreases with increasing precursor concentration (3.03-15.78 vol.%) and gradually increases as the calcination temperature increases within the range of 600-800 °C. The photocatalytic activity of different STO-NFs (based on crystallite size) was also evaluated by the amount of H2 production from water splitting under UV irradiation. The H2 evolution study demonstrated that the photocatalytic activity of the STO-NFs strongly depends on the crystallite size of the nanofibers, precursor concentration, and calcination temperature. The H2 production rate increases with increasing crystallite size and temperature, whereas it decreases with increasing precursor concentration. The photocatalytic performance of the STO-NFs was also compared with the commercial SrTiO3 nanoparticles (STO-NPs) after Pt addition as a cocatalyst, where the synthesized nanofibers showed 2 times higher H2 production rate (1.14 mmol/g-h) than that of the nanoparticles. This synthesis technique provides a good example to produce other inorganic photocatalytic 3D porous structure materials.
Ex-Situ Synthesis of Polyvinyl alcohol(PVA)-coated Fe3O4 Nanoparticles by Coprecipitation-Ultrasonication Method

NASA Astrophysics Data System (ADS)

Riva'i, Imam; Oktavia Wulandari, Ika; Sulistyarti, Hermin; Sabarudin, Akhmad

2018-01-01

In this study, the synthesis of Fe3O4 nanoparticles was done with surface modification using PVA with coprecipitation-ultrasonication method. Time variations and PVA concentrations were added to determine the effect on crystallite size and lattice parameters on the synthesis of Fe3O4-PVA nanoparticles. Fe3O4 characterization was done using X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR) instruments. FTIR was employed to determine PVA coating on the surface of Fe3O4 nanoparticles. The crystallite size and lattice parameters were analyzed using XRD. From the FTIR data, it is known that the interaction between PVA and Fe3O4 nanoparticles is characterized by Fe-O-C group at 1100 cm-1 region which is characteristic of Fe3O4-PVA nanoparticles, C-H groups of PVA in the range of 2950 cm-1 wave number, C-C of PVA regions of wave number 1405 cm-1, Fe3O4 and Fe3O4-PVA samples are in the range of 565 cm-1. In addition, the variation of ultrasonication time and the addition of PVA concentration have an effect on the crystallite size change and the lattice parameter observed from the XRD data. The use of ultrasonication time will affect the size of the crystallite become smaller and the grating lattice parameters obtained are wider. The effect of addition of PVA showed that higher concentration of PVA resulted in smaller crystallite size and larger lattice parameters. These results indicated that ultrasonication time and addition of PVA concentration greatly affect the characteristics of nanoparticles.
Gold nano-particle formation from crystalline AuCN: Comparison of thermal, plasma- and ion-beam activated decomposition

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

Beck, Mihály T.; Bertóti, Imre, E-mail: bertoti.imre@ttk.mta.hu; Mohai, Miklós

In this work, in addition to the conventional thermal process, two non-conventional ways, the plasma and ion beam activations are described for preparing gold nanoparticles from microcrystalline AuCN precursor. The phase formation at plasma and ion beam treatments was compared with that at thermal treatments and the products and transformations were characterized by thermogravimetry-mass-spectrometry (TG-MS), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). TG-MS measurements in Ar atmosphere revealed that AuCN decomposition starts at 400 °C and completes at ≈700 °C with evolution of gaseous (CN){sub 2}. XPS and TEM show that in heat treatment at 450 °C formore » 1 h in Ar, loss of nitrogen and carbon occurs and small, 5–30 nm gold particles forms. Heating at 450 °C for 10 h in sealed ampoule, much larger, 60–200 nm size and well faceted Au particles develop together with a fibrous (CN){sub n} polymer phase, and the Au crystallites are covered by a 3–5 nm thick polymer shell. Low pressure Ar plasma treatment at 300 eV energy results in 4–20 nm size Au particles and removes most of the nitrogen and part of carbon. During Ar{sup +} ion bombardment with 2500 eV energy, 5–30 nm size Au crystallites form already in 10 min, with preferential loss of nitrogen and with increased amount of carbon residue. The results suggest that plasma and ion beam activation, acting similarly to thermal treatment, may be used to prepare Au nanoparticles from AuCN on selected surface areas either by depositing AuCN precursors on selected regions or by focusing the applied ionized radiation. Thus they may offer alternative ways for preparing tailor-made catalysts, electronic devices and sensors for different applications. - Graphical abstract: Proposed scheme of the decomposition mechanism of AuCN samples: heat treatment in Ar flow (a) and in sealed ampoule (b); Ar{sup +} ion treatment at 300 eV (c) and at 2500 eV (d). Cross section sketches illustrate the Au phase formation and the corresponding TEM micrographs are shown as top views. The dotted lines represent the original boundaries of the AuCN crystals. - Highlights: • AuCN decomposes between 400 and 700 °C with evolution of gaseous (CN){sub 2}. • Epitaxial relationship is established between Au and parent AuCN crystals. • Ar plasma treatment results in similar phase transition than the thermal treatment. • Plasma and ion-beam activation offer alternative way for preparing Au nanocrystals. • Reaction mechanisms of Au particle formation at the three treatments are proposed.« less
Modelling and validation of particle size distributions of supported nanoparticles using the pair distribution function technique

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

Gamez-Mendoza, Liliana; Terban, Maxwell W.; Billinge, Simon J. L.

The particle size of supported catalysts is a key characteristic for determining structure–property relationships. It is a challenge to obtain this information accurately andin situusing crystallographic methods owing to the small size of such particles (<5 nm) and the fact that they are supported. In this work, the pair distribution function (PDF) technique was used to obtain the particle size distribution of supported Pt catalysts as they grow under typical synthesis conditions. The PDF of Pt nanoparticles grown on zeolite X was isolated and refined using two models: a monodisperse spherical model (single particle size) and a lognormal size distribution.more » The results were compared and validated using scanning transmission electron microscopy (STEM) results. Both models describe the same trends in average particle size with temperature, but the results of the number-weighted lognormal size distributions can also accurately describe the mean size and the width of the size distributions obtained from STEM. Since the PDF yields crystallite sizes, these results suggest that the grown Pt nanoparticles are monocrystalline. This work shows that refinement of the PDF of small supported monocrystalline nanoparticles can yield accurate mean particle sizes and distributions.« less
Structural and electromagnetic characterization of Co-Mn doped Ni-Sn ferrites fabricated via micro-emulsion route

NASA Astrophysics Data System (ADS)

Ali, Rajjab; Azhar Khan, Muhammad; Manzoor, Alina; Shahid, Muhammad; Farooq Warsi, Muhammad

2017-11-01

Ni0.5Sn0.5CoxMnxFe2-2xO4 ferrites with x = 0.0-0.8 have been prepared by the micro-emulsion method, using CTAB as a surfactant material. X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR) and vibrational sample magnetometer (VSM) were used to investigate the effects of Co and Mn substitutions on cationic distribution, crystallite size, lattice constant, spectral, magnetic and dielectric properties. Lattice constant and crystallite size were found to increase from 7.4 to 9.25 Å and from 11.8 to 19.7 nm respectively with increasing substitution of Co and Mn ions. Saturation magnetization (MS) gradually increased from 20.5 to 47.6 emu/g with increase in the value of x. However, Coercivity increased from 152.7 to 462.4 Oe up to x = 0.4 and then it decreased thereafter. The dielectric constant, complex dielectric constant and tan loss (tanδ) were observed to decrease with increase in frequency, depicting the semiconductor behavior of the ferrites. Dc resistivity was observed to decrease considerably upon addition of Co and Mn content. The outcome for the tunable magnetic properties and achieved modification of the synthesized nanocrystallites may be chosen for tremendous applications; such as miniaturized memory devices that are based on the energy storage principles and capacitive components.
Kinetic and catalytic analysis of mesoporous Co3O4 on the oxidation of morin

NASA Astrophysics Data System (ADS)

Xaba, Morena. S.; Meijboom, Reinout

2017-11-01

Herein we report on the synthesis, characterization and catalytic evaluation of mesoporous cobalt oxides on the oxidation of morin. These mesoporous cobalt oxides were synthesized using an inverse surfactant micelle method, they are connected, well-defined with intra-particle voids. These materials were calcined to different final heating temperatures of 150, 250, 350, 450 and 550 °C, and each mesoporous cobalt oxide catalyst showed unique physical properties and catalytic behavior. Morin oxidation was used as a model reaction in the presence of hydrogen peroxide to evaluate the kinetic and catalytic activity of calcined mesoporous cobalt oxides. The adsorption-desorption equilibrium rate constants of morin and hydrogen peroxide were found to be inversely proportional to the crystallite size of the mesoporous cobalt oxide, and the characteristic path length in which the mass transfer takes place was found to be directly proportional to the crystallite size. The materials were characterized using powder X-Ray Diffraction (p-XRD), N2-sorption isotherms (BET), hydrogen temperature programmed reduction (H2-TPR) and High Resolution-Transmission Electron Microscopy (HR-TEM). UV-vis spectrophotometry was used to monitor the time-resolved absorbance of morin at λmax = 410 nm. The surface reaction in this system is described in terms of the well-established Langmuir-Hinshelwood model. The thermodynamic parameters, EA, ΔH#, ΔS# and ΔG# were calculated and catalyst recycling and reusability is demonstrated.
High hardness BaCb-(BxOy/BN) composites with 3D mesh-like fine grain-boundary structure by reactive spark plasma sintering.

PubMed

Vasylkiv, Oleg; Borodianska, Hanna; Badica, Petre; Grasso, Salvatore; Sakka, Yoshio; Tok, Alfred; Su, Liap Tat; Bosman, Michael; Ma, Jan

2012-02-01

Boron carbide B4C powders were subject to reactive spark plasma sintering (also known as field assisted sintering, pulsed current sintering or plasma assisted sintering) under nitrogen atmosphere. For an optimum hexagonal BN (h-BN) content estimated from X-ray diffraction measurements at approximately 0.4 wt%, the as-prepared BaCb-(BxOy/BN) ceramic shows values of Berkovich and Vickers hardness of 56.7 +/- 3.1 GPa and 39.3 +/- 7.6 GPa, respectively. These values are higher than for the vacuum SPS processed B4C pristine sample and the h-BN -mechanically-added samples. XRD and electronic microscopy data suggest that in the samples produced by reactive SPS in N2 atmosphere, and containing an estimated amount of 0.3-1.5% h-BN, the crystallite size of the boron carbide grains is decreasing with the increasing amount of N2, while for the newly formed lamellar h-BN the crystallite size is almost constant (approximately 30-50 nm). BN is located at the grain boundaries between the boron carbide grains and it is wrapped and intercalated by a thin layer of boron oxide. BxOy/BN forms a fine and continuous 3D mesh-like structure that is a possible reason for good mechanical properties.
Native Cellulose: Structure, Characterization and Thermal Properties

PubMed Central

Poletto, Matheus; Ornaghi Júnior, Heitor L.; Zattera, Ademir J.

2014-01-01

In this work, the relationship between cellulose crystallinity, the influence of extractive content on lignocellulosic fiber degradation, the correlation between chemical composition and the physical properties of ten types of natural fibers were investigated by FTIR spectroscopy, X-ray diffraction and thermogravimetry techniques. The results showed that higher extractive contents associated with lower crystallinity and lower cellulose crystallite size can accelerate the degradation process and reduce the thermal stability of the lignocellulosic fibers studied. On the other hand, the thermal decomposition of natural fibers is shifted to higher temperatures with increasing the cellulose crystallinity and crystallite size. These results indicated that the cellulose crystallite size affects the thermal degradation temperature of natural fibers. This study showed that through the methods used, previous information about the structure and properties of lignocellulosic fibers can be obtained before use in composite formulations. PMID:28788179

Surface morphology and molecular bonding of CaCO3 nanocrystallites by gas diffusion method

NASA Astrophysics Data System (ADS)

Sulimai, N. H.; Rani, Rozina Abdul; Khusaimi, Z.; Abdullah, S.; Salifairus, M. J.; Alrokayan, Salman; Khan, Haseeb; Rusop, M.

2018-05-01

Calcium carbonate with the chemical formula of (CaCO3) is the most abundant element in the world. Its usage on certain applications is largely affected by its properties. The best means to control its properties is through controlled preparation of CaCO3. This study uses diffusion method between the precursors Calcium Chloride and Ammonium Carbonate. Instead of using water, ethanol was used to prepare the salt. Reaction was done in room temperature (RT) for 6h-24h. Smallest average crystallite size measured by FESEM micrograph is 500nm produced by synthesis of CaCO3 reacted for 168 hours. From energy-dispersive X-ray spectrum also indicated the smallest particle size is by CaCO3 reacted for 168 hours. Changes was seen for element Ca at 3.7keV.
A chemical reduction approach to the synthesis of copper nanoparticles

NASA Astrophysics Data System (ADS)

Khan, Ayesha; Rashid, Audil; Younas, Rafia; Chong, Ren

2016-11-01

Development of improved methods for the synthesis of copper nanoparticles is of high priority for the advancement of material science and technology. Herein, starch-protected zero-valent copper (Cu) nanoparticles have been successfully synthesized by a novel facile route. The method is based on the chemical reduction in aqueous copper salt using ascorbic acid as reducing agent at low temperature (80 °C). X-ray diffraction, scanning electron microscopy and energy-dispersive X-ray spectroscopy measurements were taken to investigate the size, structure and composition of synthesized Cu nanocrystals, respectively. Average crystallite size of Cu nanocrystals calculated from the major diffraction peaks using the Scherrer formula is about 28.73 nm. It is expected that the outcomes of the study take us a step closer toward designing rational strategies for the synthesis of nascent Cu nanoparticles without inert gas protection.
Effect of Zn2+, Fe3+ and Cr3+ addition to hydroxyapatite for its application as an active constituent of sunscreens

NASA Astrophysics Data System (ADS)

de Araujo, T. S.; de Souza, S. O.; de Sousa, E. M. B.

2010-11-01

Biocompatible phosphate materials are used in different applications like bone and dental implants, drug delivery systems and others, but could also be applied in inorganic sunscreens. Using sunscreens is extremely necessary, because long time exposure to sun can cause skin cancer. In this work chemical precipitation method has been used to produce hydroxyapatite. Cr3+, Zn2+ and Fe3+ doped samples were characterized using powder X-Ray Diffraction (XRD) and Optical Absorption techniques. X-ray diffraction measurements confirmed the materials were in the expected crystalline structures. The crystallite size as measured from the X-ray pattern was 23-27 nm (±1). The absorption spectra in the ultraviolet and visible ranges indicate that appropriately doped and sized hydroxyapatite particles may have potential applications as active constituents of sunscreens.
Polymorphism influences singlet fission rates in tetracene thin films

DOE PAGES

Arias, Dylan H.; Ryerson, Joseph L.; Cook, Jasper D.; ...

2015-11-06

Here, we report the effect of crystal structure and crystallite grain size on singlet fission (SF) in polycrystalline tetracene, one of the most widely studied SF and organic semiconductor materials. SF has been comprehensively studied in one polymoprh (Tc I), but not in the other, less stable polymorph (Tc II). Using carefully controlled thermal evaporation deposition conditions and high sensitivity ultrafast transient absorption spectroscopy, we found that for large crystallite size samples, SF in nearly pure Tc II films is significantly faster than SF in Tc I films. We also discovered that crystallite size has a minimal impact on themore » SF rate in Tc II films, but a significant influence in Tc I films. Large crystallites exhibit SF times of 125 ps and 22 ps in Tc I and Tc II, respectively, whereas small crystallites have SF times of 31 ps and 33 ps. Our results demonstrate first, that attention must be paid to polymorphism in obtaining a self-consistent rate picture for SF in tetracene and second, that control of polymorphism can play a significant role towards achieving a mechanistic understanding of SF in polycrystalline systems. In this latter context we show that conventional theory based on non-covalent tetracene couplings is insufficient, thus highlighting the need for models that capture the delocalized and highly mobile nature of excited states in elucidating the full photophysical picture.« less
Thermal-induced SPR tuning of Ag-ZnO nanocomposite thin film for plasmonic applications

NASA Astrophysics Data System (ADS)

Singh, S. K.; Singhal, R.

2018-05-01

The formation of silver (Ag) nanoparticles in a ZnO matrix were successfully synthesized by RF-magnetron sputtering at room temperature. As prepared Ag-ZnO nanocomposite (NCs) thin films were annealed in vacuum at three different temperatures of 300 °C, 400 °C and 500 °C, respectively. The structural modifications for as-deposited and annealed films were estimated by X-ray diffraction and TEM techniques. The crystalline behavior preferably along the c-axis of the hexagonal wurtzite structure was observed in as-deposited Ag-ZnO film and improved significantly with increasing the annealing temperature. The crystallite size of as-deposited film was measured to be 13.6 nm, and increases up to 28.5 nm at higher temperatures. The chemical composition and surface structure of the as-deposited films were estimated by X-ray photoelectron spectroscopy. The presence of Ag nanoparticles with average size of 8.2 ± 0.2 nm, was confirmed by transmission electron microscopy. The strong surface plasmon resonance (SPR) band was observed at the wavelength of ∼565 nm for as-deposited film and a remarkable red shift of ∼22 nm was recorded after the annealing treatment as confirmed by UV-visible spectroscopy. Atomic force microscopy confirmed the grain growth from 60.38 nm to 79.42 nm for as-deposited and higher temperature annealed film respectively, with no significant change in the surface roughness. Thermal induced modifications such as disordering and lattice defects in Ag-ZnO NCs thin films were carried out by Raman spectroscopy. High quality Ag-ZnO NCs thin films with minimum strain and tunable optical properties could be useful in various plasmonic applications.
Demagnetizing fields of crystallites and a method for measuring the thermodynamic fields of quasi-single-crystal and polycrystalline thin YBa{sub 2}Cu{sub 3}O{sub 7-x} disks

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

Rostami, Kh. R.

The role of the demagnetizing fields of crystallites in HTSC samples is studied. An increase in the crystallite size is shown to suppress the intra-and intercrystalline critical currents of the sample in lower fields. The demagnetizing fields of crystallites are shown to be one of the main causes of the fact that the Bean model is invalid for HTSC samples. A method is proposed to measure the thermodynamic field of a superconductor; this method allows the first thermodynamic critical magnetic fields of the sample and its crystallites and 'subcrystallites' to be measured with a high accuracy. The first thermodynamic criticalmore » magnetic fields are used to estimate the critical current density J{sub c} of the sample, crystallites, and subcrystallites.« less
XRD-based 40Ar/39Ar age correction for fine-grained illite, with application to folded carbonates in the Monterrey Salient (northern Mexico)

NASA Astrophysics Data System (ADS)

Fitz-Díaz, Elisa; Hall, Chris M.; van der Pluijm, Ben A.

2016-05-01

Due to their minute size, 40Ar/39Ar analysis of illite faces significant analytical challenges, including mineral characterization and, especially, effects of grain size and crystallography on 39Ar recoil. Quantifying the effects of 39Ar recoil requires the use of sample vacuum encapsulation during irradiation, which permits the measurement of the fraction of recoiled 39Ar as well as the 39Ar and 40Ar∗ retained within illite crystals that are released during step heating. Total-Gas Ages (TGA) are calculated by using both recoiled and retained argon, which is functionally equivalent to K-Ar ages, while Retention Ages (RA) only involve retained Ar in the crystal. Natural applications have shown that TGA fits stratigraphic constraints of geological processes when the average illite crystallite thickness (ICT) is smaller than 10 nm, and that RA matches these constraints for ICTs larger than 50 nm. We propose a new age correction method that takes into account the average ICT and corresponding recoiled 39Ar for a sample, with X-ray Corrected Ages (XCA) lying between Total-Gas and Retention Ages depending on ICT. This correction is particularly useful in samples containing authigenic illite formed in the anchizone, with typical ICT values between 10 and 50 nm. In three samples containing authigenic illite from Cretaceous carbonates in the Monterrey Salient in northern Mexico, there is a range in TGAs among the different size-fractions of 46-49, 36-43 and 40-52 Ma, while RAs range from 54-64, 47-52 and 53-54 Ma, respectively. XCA calculations produce tighter age ranges for these samples of 52.5-56, 45.5-48.5 and 49-52.5 Ma, respectively. In an apparent age vs ICT or %2M 1illite plot, authigenic illite grains show a slope that is in general slightly positive for TGA, slightly negative for RA, but close to zero for XCA, with thinner crystallites showing more dispersion than thicker ones. In order to test if dispersion is due to a different formation history or the result of retention capability, degassing spectra were modeled for site XCA averages and overall XCA average. Modeling shows that local site age average best match the measured spectra, instead of a global average age, indicating that illite growth reflects local deformation, and is not the result of regional metamorphism. Modeling also shows that Ar-degassing spectra are very sensitive to grain size, such that age interpretation based on Ar-plateaus is meaningless for most fine-grained clays.
Physicochemical characterizations of nano-palm oil fuel ash

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

Rajak, Mohd Azrul Abdul, E-mail: azrulrajak88@gmail.com; Preparatory Centre of Science and Technology, Universiti Malaysia Sabah, Jalan UMS, 88400, Kota Kinabalu, Sabah; Majid, Zaiton Abdul, E-mail: zaiton@kimia.fs.utm.my

2015-07-22

Palm Oil Fuel Ash (POFA) is known as a good supplementary cementing material due to its siliceous-rich content. The application of nanotechnology in the pozzolanic materials could invent new functions in the efficiency of physical and chemical properties of materials. Thus, the present study aims to generate nano-sized POFA and characterize the physicochemical properties of nano-palm oil fuel ash (nPOFA). The nPOFA was prepared by mechanically grinding micro POFA using a high intensity ball milling for 6 hours. The physicochemical properties of nPOFA were characterized via X-Ray Fluoresence (XRF), Scanning Emission microscopy- Energy Dispersive X-Ray (SEM-EDX), Transmission Electron Microscope (TEM)more » and X-Ray Diffraction (XRD). The particle size of nPOFA acquired from TEM analysis was in the range of 20 nm to 90 nm, while the average crystallite size calculated from XRD diffractogram was 61.5 nm. The resulting nPOFA has a BET surface area of 145.35 m{sup 2}/g, which is more than 85% increment in surface area compared to micro-sized POFA. The morphology and elemental studies showed the presence of spherical as well as irregularly shaped and fine nPOFA particles contains with high silicon content. The presence of α-quartz as the major phase of the nPOFA was identified through XRD analysis. The study concludes that nPOFA has the potential as a supplementary cementing material due to the high silica content, high surface area and the unique behaviors of nano-structured particles.« less
Structural, optical and dielectric properties of pure and chromium (Cr) doped nickel oxide nanoparticles

NASA Astrophysics Data System (ADS)

Gupta, Jhalak; Ahmed, Arham S.

2018-05-01

The pure and Cr doped nickel oxide (NiO) nanoparticles have been synthesized by cost effective co-precipitation method having nickel nitrate as initial precursor. The synthesized samples were characterized by X-Ray diffraction (XRD), UV-Visible Spectroscopy(UV-Vis) and LCR meter for structural, optical and dielectric properties respectively. The crystallite size of pure nickel oxide nanoparticles characterized by XRD using Debye Scherer's formula was found to be 21.7nm and the same decreases on increasing Cr concentration whereas optical and dielectric properties were analyzed by UV-Vis and LCR meter respectively. The energy band gaps were determined by UV-Vis using Tauc relation.
Synthesis of Nano-Crystalline Cu-Cr Alloy by Mechanical Alloying

NASA Astrophysics Data System (ADS)

Sheibani, S.; Heshmati-Manesh, S.; Ataie, A.

In this paper, the influence of toluene as the process control agent (PCA) and pre-milling on the extension of solid solubility of 7 wt.% Cr in Cu by mechanical alloying in a high energy ball mill was investigated. The structural evolution and microstructure were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques, respectively. The solid solution formation at different conditions was analyzed by copper lattice parameter change during the milling process. It was found that both the presence of PCA and pre-milling of Cr powder lead to faster dissolution of Cr. The mean crystallite size was also calculated and showed to be about 10 nm after 80 hours of milling.
Report on cascade energy relaxation from PVP to Tb3+:Bi2SiO5 nanophosphor through salicylic acid in composite polymeric film

NASA Astrophysics Data System (ADS)

Kumari, Pushpa; Dwivedi, Y.

2018-05-01

The present article reports structural and spectroscopic properties of Tb:Bi2SiO5 nanophosphors dispersed in Polyvinylpyrrolidone polymer film, in presence of Salicylic acid (SA) molecule, which acts as a sensitizer. Detailed structural and spectroscopic characterizations were carried out using X-ray diffraction patterns, Scanning Electron Microscope, Fourier Transform Infrared and Excitation and photoluminescence techniques. The mean crystallite size of Tb3+:Bi2SiO5 nanophosphor and Tb3+:Bi2SiO5 in Polyvinylpyrrolidone polymer composite was estimated ∼22 nm and ∼28 nm, respectively. We have report atleast two times enhancement in Tb3+ ions emission intensity due to the efficient energy transfer from salicylic acid molecule to Tb ions. In addition to energy transfer from salicylic acid, the Polyvinylpyrrolidone polymeric host was also reported to serve as a sensitizer for SA molecule and Tb3+ ions through a cascade energy relaxation process while exciting with 248 nm photons. On 248 nm photon excitation, atleast five improvements in Tb3+ ion emission intensity are reported. Presence of SA molecule facilitates precise colour tuning as obvious from the CIE coordinates.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Garcia-Mateo, Carlos, E-mail: cgm@cenim.csic.es

Since the major strengthening mechanisms in nanocrystalline bainitic steels arise from the exceptionally small size of the bainitc ferrite plate, accurate determination of this parameter is fundamental for quantitative relating the microstructure to the mechanical properties. In this work, the thickness of the bainitic ferrite subunits obtained by different bainitic heat treatments was determined in two steels, with carbon contents of 0.3 and 0.7 wt.%, from SEM and TEM micrographs. As these measurements were made on 2D images taken from random sections, the method includes some stereological correction factors to obtain accurate information. Finally, the determined thicknesses of bainitic ferritemore » plates were compared with the crystallite size calculated from the analysis of X-ray diffraction peak broadening. Although in some case the values obtained for crystallite size and plate thickness can be similar, this study confirms that indeed they are two different parameters. - Highlights: •Bainitic microstructure in a nanostructured and sub-micron steel •Bainitic ferrite plate thickness measured by SEM and TEM •Crystallite size determined by X-ray analysis.« less
Study on the corrosion properties of nanocrystalline nickel electrodepositied by reverse pulse current

NASA Astrophysics Data System (ADS)

Cheng, Wen; Ge, Wen; Yang, Qian; Qu, Xinxin

2013-07-01

Nanocrystalline nickel coatings were produced by the method of reverse pulse electrodepositing on the surface of steel sheets. The crystallite size of nanocrystalline nickel coatings was determined by X-ray diffraction (XRD). The effect of saccharin concentration on the crystallite size of the coatings was studied. The average crystallite sizes were diminished as a result of increasing saccharin concentration. CHI660C electrochemical workstation was used to determine the Tafel polarization curves and electrochemical impedance spectroscopy (EIS) of the coatings. The value of corrosion potential, natural corrosion current density, polarizaiton resistance and impedance was calculated, the results suggested that smaller grain size led to higher polarization resistance. EIS gave the charge transfer resistance Rct and pore resistance Rpo variation trend from beginning to 30 min. Scanning electron microscopy (SEM) examination showed the surface morphology of the nickel coatings after the neutral salt spray (NSS) test or bathing in 10% HCl. The images indicated that the corrosion behavior of nanocrystalline nickel coatings was pitting corrosion, the mechanism was also discussed.
Micro Structural, Optical and Magnetic Properties of Co-SiO2 Nanocomposite Synthesized by Sol-Gel Technique

NASA Astrophysics Data System (ADS)

Saha, Mrinal; Mukherjee, Soumya; Gayen, Arup; Mukherjee, Siddhartha

2017-04-01

Co-SiO2 nano composite has been synthesized via sol-gel technique using dextrose [C6H12O6] as a reducer and tetraethyl orthosilicate [Si(OCH2CH3)4] as oxide forming agent, respectively. The dried gel has been subsequently calcined at different temperature (850 and 900 °C) for 30 min in an inert atmosphere by N2 purging. The synthesized materials have been characterized by X-ray diffraction, high resolution transmission microscope, Fourier transform infrared spectroscopy, UV-Vis spectroscopy, scanning electron microscope, field emission microscope, atomic force microscope and physical property measurement system. The crystallite sizes of the face centered cubic cobalt nano composite materials have been found to be in the range of 14-28 nm. The crystallite size of the material found to be increased at higher calcination temperature due to the grain growth. The surface morphology of the obtained material has been found to be agglomerated but spherical in nature. This agglomeration tendency could be attributed to magnetic interaction between particles, large surface area as well as high surface energy. The band gap value of the obtained material has been determined to be 1.92 eV. The saturation magnetization (Ms) and the coercivity (Hc) of the composite material were found to be 29.45 emu g-1and 23.2 Oe, respectively. This technique has thus been found to be a convenient and effective method to prepare pure metallic cobalt nanoparticles with uniform size and homogeneous distribution throughout the matrix.
Structural elucidation and magnetic behavior evaluation of Cu-Cr doped BaCo-X hexagonal ferrites

NASA Astrophysics Data System (ADS)

Azhar Khan, Muhammad; Hussain, Farhat; Rashid, Muhammad; Mahmood, Asif; Ramay, Shahid M.; Majeed, Abdul

2018-04-01

Ba2-xCuxCo2CryFe28-yO46 (x = 0.0, 0.1, 0.2, 0.3, 0.4, y = 0.0, 0.2, 0.4, 0.6, 0.8) X-type hexagonal ferrites were synthesized via micro-emulsion route. The techniques which were applied to characterize the prepared samples are as follows: X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Dielectric measurements and vibrating sample magnetometer (VSM). The structural parameters i.e. lattice constant (a, c), cell volume (V), X-ray density, bulk density and crystallite size of all the prepared samples were obtained using XRD analysis. The lattice parameters 'a' and 'c' increase from 5.875 Å to 5.934 Å and 83.367 Å to 83.990 Å respectively. The crystallite size of investigated samples lies in the range of 28-32 nm. The magnetic properties of all samples have been calculated by vibrating sample magnetometer (VSM) analysis. The increase in coercivity (Hc) was observed with the increase of doping contents. It was observed that the coercivity (Hc) of all prepared samples is inversely related to the crystalline size which reflects that all materials are super-paramagnetic. The dielectric parameters i.e. dielectric constant, dielectric loss, tangent loss etc were obtained in the frequency range of 1 MHz-3 GHz and followed the Maxwell-Wagner's model. The significant variation the dielectric parameters are observed with increasing frequency. The maximum Q value is obtained at ∼2 GHz due to which these materials are used for high frequency multilayer chip inductors.
Analytical characterization of engineered ZnO nanoparticles relevant for hazard assessment

NASA Astrophysics Data System (ADS)

Bragaru, Adina; Kusko, Mihaela; Vasile, Eugeniu; Simion, Monica; Danila, Mihai; Ignat, Teodora; Mihalache, Iuliana; Pascu, Razvan; Craciunoiu, Florea

2013-01-01

The optoelectronic properties of zinc oxide nanoparticles (ZnO-NPs) have determined development of novel applications in catalysis, paints, wave filters, UV detectors, transparent conductive films, solar cells, or sunscreens. While the immediate advantages of using nano-ZnO in glass panel coatings and filter screens for lamps, as protecting products against bleaching, have been demonstrated, the potential environmental effect of the engineered NPs and the associated products was not fully estimated; this issue being of utmost importance, as these materials will be supplied to the market in quantities of tons per year, equating to thousands of square meters. In this study, ZnO-NPs with commercial name Zincox™ have been subjected to a comprehensive characterization, relevant for hazard assessment, using complementary physico-chemical methods. Therefore, the morphological investigations have been corroborated with XRD pattern analyses and UV-Vis absorption related properties resulting an excellent correlation between the geometrical sizes revealed by microscopy (8.0-9.0 nm), and, respectively, the crystallite size (8.2-9.5 nm) and optical size (7.8 nm) calculated from the last two techniques' data. Furthermore, the hydrodynamic diameter of ZnO-NPs and stability of aqueous dispersions with different concentration of nanoparticles have been analyzed as function of significant solution parameters, like concentration, pH and solution ionic strength. The results suggest that solution chemistry exerts a strong influence on ZnO dissolution stability, the complete set of analyses providing useful information toward better control of dosage during biotoxicological tests.
Structure and corrosion behavior of sputter deposited cerium oxide based coatings with various thickness on Al 2024-T3 alloy substrates

NASA Astrophysics Data System (ADS)

Liu, Yuanyuan; Huang, Jiamu; Claypool, James B.; Castano, Carlos E.; O'Keefe, Matthew J.

2015-11-01

Cerium oxide based coatings from ∼100 to ∼1400 nm in thickness were deposited onto Al 2024-T3 alloy substrates by magnetron sputtering of a 99.99% pure CeO2 target. The crystallite size of CeO2 coatings increased from 15 nm to 46 nm as the coating thickness increased from ∼100 nm to ∼1400 nm. The inhomogeneous lattice strain increased from 0.36% to 0.91% for the ∼100 nm to ∼900 nm thick coatings and slightly decreased to 0.89% for the ∼1400 nm thick coating. The highest adhesion strength to Al alloy substrates was for the ∼210 nm thick coating, due to a continuous film coverage and low internal stress. Electrochemical measurements indicated that sputter deposited crystalline CeO2 coatings acted as physical barriers that provide good cathodic inhibition for Al alloys in saline solution. The ∼900 nm thick CeO2 coated sample had the best corrosion performance that increased the corrosion resistance by two orders magnitude and lowered the cathodic current density 30 times compared to bare Al 2024-T3 substrates. The reduced defects and exposed surface, along with suppressed charge mobility, likely accounts for the improved corrosion performance as coating thickness increased from ∼100 nm to ∼900 nm. The corrosion performance decreased for ∼1400 nm thick coatings due in part to an increase in coating defects and porosity along with a decrease in adhesion strength.
Control of crystallite and particle size in the synthesis of layered double hydroxides: Macromolecular insights and a complementary modeling tool.

PubMed

Galvão, Tiago L P; Neves, Cristina S; Caetano, Ana P F; Maia, Frederico; Mata, Diogo; Malheiro, Eliana; Ferreira, Maria J; Bastos, Alexandre C; Salak, Andrei N; Gomes, José R B; Tedim, João; Ferreira, Mário G S

2016-04-15

Zinc-aluminum layered double hydroxides with nitrate intercalated (Zn(n)Al-NO3, n=Zn/Al) is an intermediate material for the intercalation of different functional molecules used in a wide range of industrial applications. The synthesis of Zn(2)Al-NO3 was investigated considering the time and temperature of hydrothermal treatment. By examining the crystallite size in two different directions, hydrodynamic particle size, morphology, crystal structure and chemical species in solution, it was possible to understand the crystallization and dissolution processes involved in the mechanisms of crystallite and particle growth. In addition, hydrogeochemical modeling rendered insights on the speciation of different metal cations in solution. Therefore, this tool can be a promising solution to model and optimize the synthesis of layered double hydroxide-based materials for industrial applications. Copyright © 2016 Elsevier Inc. All rights reserved.
Characterization of X80 and X100 Microalloyed Pipeline Steel Using Quantitative X-ray Diffraction

NASA Astrophysics Data System (ADS)

Wiskel, J. B.; Li, X.; Ivey, D. G.; Henein, H.

2018-06-01

Quantitative X-ray diffraction characterization of four (4) X80 and three (3) X100 microalloyed steels was undertaken. The effect of through-thickness position, processing parameters, and composition on the measured crystallite size, microstrain, and J index (relative magnitude of crystallographic texture) was determined. Microstructure analysis using optical microscopy, scanning electron microscopy, transmission electron microscopy, and electron-backscattered diffraction was also undertaken. The measured value of microstrain increased with increasing alloy content and decreasing cooling interrupt temperature. Microstructural features corresponding to crystallite size in the X80 steels were both above and below the detection limit for quantitative X-ray diffraction. The X100 steels consistently exhibited microstructure features below the crystallite size detection limit. The yield stress of each steel increased with increasing microstrain. The increase in microstrain from X80 to X100 is also associated with a change in microstructure from predominantly polygonal ferrite to bainitic ferrite.
Crystal growth in zinc borosilicate glasses

NASA Astrophysics Data System (ADS)

Kullberg, Ana T. G.; Lopes, Andreia A. S.; Veiga, João P. B.; Monteiro, Regina C. C.

2017-01-01

Glass samples with a molar composition (64+x)ZnO-(16-x)B2O3-20SiO2, where x=0 or 1, were successfully synthesized using a melt-quenching technique. Based on differential thermal analysis data, the produced glass samples were submitted to controlled heat-treatments at selected temperatures (610, 615 and 620 °C) during various times ranging from 8 to 30 h. The crystallization of willemite (Zn2SiO4) within the glass matrix was confirmed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). Under specific heat-treatment conditions, transparent nanocomposite glass-ceramics were obtained, as confirmed by UV-vis spectroscopy. The influence of temperature, holding time and glass composition on crystal growth was investigated. The mean crystallite size was determined by image analysis on SEM micrographs. The results indicated an increase on the crystallite size and density with time and temperature. The change of crystallite size with time for the heat-treatments at 615 and 620 °C depended on the glass composition. Under fixed heat-treatment conditions, the crystallite density was comparatively higher for the glass composition with higher ZnO content.

Zn(1-x)Cu(x)O (0.02 ≤ x ≤ 0.1) Nanomaterials Prepared by Ball Milling, Citrate Sol Gel, and Molten Salt Flux Methods.

PubMed

Balamurugan, S; Melba, K

2015-06-01

The Cu doped ZnO, (Zn(1-x)Cu(x))O (x = 0.02, 0.04, 0.06, 0.08, and 0.1) nanomaterials were prepared by ball milling technique (BMT), citrate sol gel (CSG), and molten salt flux (MSF) methods. The various as-prepared (Zn(1-x)Cu(x))O materials were analyzed by powder X-ray diffraction (pXRD), FT-IR, and SEM-EDX measurements in order to check the phase formation, purity, surface morphology and elements present in the annealed materials. Due to the preparation methods as well as doping of 'x' slight variations in cell parameters are seen. The average crystalline size of CSG method shows smaller size (25-35 nm) than BMT and MSF approaches. The materials obtained by MSF technique reveal the average crystalline size in the range of 32-72 nm whereas the BMT materials exhibit 36-50 nm for the composition, 0.02 ≤ x ≤ 0.1. The presence of functional groups and the chemical bonding in (Zn(1-x)Cu(x))O system is confirmed through FT-IR measurements. It is evident from the FT-IR data that bands seen at 400-500 cm(-1) are characteristics of M-O (M = metal ion) bonding in the studied materials. The micro images observed by SEM exhibiting polycrystalline character as compared with the crystallite size obtained from XRD. Among the three approaches employed in the present investigations, in terms of average particle size the CSG method may be concluded as an efficient method for the preparation of Zn(1-x)Cu(x)O nanomaterials.
Ultrasonically assisted synthesis of lead oxide nanoflowers using ball milling

NASA Astrophysics Data System (ADS)

Bangi, Uzma K. H.; Park, Hyung-Ho; Han, Wooje; Prakshale, Vipul M.; Deshmukh, Lalasaheb P.

2017-05-01

The experimental results on the ultrasonically assisted synthesis of lead oxide nanoflowers using ball milling have been reported in the present work. Lead oxide nanoflowers were prepared employing mixed ligands by subjecting the formed precipitate to ultrasonication and grinding/ball milling. The effect of ball milling as well as fine grinding in agate mortar on the microstructure and surface morphology of the lead oxide was studied. The characteristics of synthesized PbO were studied using X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy and field emission scanning electron microscopy techniques. XRD results demonstrated the tetragonal phase of PbO with crystallite size of around 25 nm and strain of 3.6 × 10-3 calculated from Williamson-Hall plot. FESEM images manifested the formation of nanodiscs and nanoflowers with a diameter of around 300 nm and thickness of 50 nm. XPS spectra revealed the formation of PbO with photoelectron peak of Pb 4f and O 1 s lied at 137.68 and 529.96 eV. Moreover, FTIR spectrum exhibited Pb-O bond peak in the range of 400-530 cm-1.
Effects of the synthesis temperature on the crystalline structure and the magnetic properties of cobalt ferrite nanoparticles prepared via coprecipitation

NASA Astrophysics Data System (ADS)

Hutamaningtyas, Evangelin; Utari; Suharyana; Purnama, Budi; Wijayanta, Agung Tri

2016-08-01

The effects of the synthesis temperature on the crystalline structure and the magnetic properties of cobalt ferrite (CoFe2O4) nanoparticles prepared via coprecipitation are discussed. The synthesis was conducted at temperatures of 75 °C, 85 °C and 95 °C. Fourier transform infrared spectroscopy characterization related to a stretching vibration at a wavenumber of 590 cm-1 indicated the formation of a CoFe2O4 metal oxide. In addition, powder X ray diffraction (XRD) characterization proved that the metal oxide was CoFe2O4. Crystallite sizes calculated using the Scherer formula at the strongest peak of the XRD spectra of the samples synthesized at 75 °C, 85 °C and 95 °C were 32 nm, 43 nm and 50.4 nm, respectively. Finally, the results of the vibrating sample magnetometer characterization showed that the saturation magnetization decreased with increasing synthesis temperature, which is related to the dominant preference of Co2+ over Fe3+ cations at the octahedral sites.
About the optical properties of oxidized black silicon structures

NASA Astrophysics Data System (ADS)

Pincik, E.; Brunner, R.; Kobayashi, H.; Mikula, M.; Kučera, M.; Švec, P.; Greguš, J.; Vojtek, P.; Zábudlá, Z.; Imamura, K.; Zahoran, M.

2017-02-01

The paper deals with the optical and morphological properties of thermally oxidized black silicon (OBSi) nano-crystalline specimens produced by the surface structure chemical transfer method (SSCT). This method can produce a nano-crystalline Si black color layer on c-Si with a range of thickness of ∼50 nm to ∼300 nm by the contact of c-Si immersed in chemical solutions HF + H2O2 with a catalytic mesh. We present and discuss mainly the photoluminescence properties of both polished c-Si and OBSi structures, respectively. The similar photoluminescence (PL) behaviors recorded at liquid helium (6 K) and room temperatures on both polished crystalline Si and OBSi samples, respectively, indicate the similar origin of recorded luminescence light. As the positions of PL maxima of OBSi structures are mainly related to the size of Si nanocrystallites and SiO(x), we therefore suppose that the size of the dominant parts of the luminated OBSi nanostructure is pre-determined by the used polishing Si procedure, and/or the distribution function of the number of formed crystallites on their size is very similar. The blue shift of both PL spectra reaching almost value of 0.40 eV observed after the decrease of the sample temperature to 6 K we relate also with the change of the semiconductor band gap width.
Reciprocal-space mapping of epitaxic thin films with crystallite size and shape polydispersity.

PubMed

Boulle, A; Conchon, F; Guinebretière, R

2006-01-01

A development is presented that allows the simulation of reciprocal-space maps (RSMs) of epitaxic thin films exhibiting fluctuations in the size and shape of the crystalline domains over which diffraction is coherent (crystallites). Three different crystallite shapes are studied, namely parallelepipeds, trigonal prisms and hexagonal prisms. For each shape, two cases are considered. Firstly, the overall size is allowed to vary but with a fixed thickness/width ratio. Secondly, the thickness and width are allowed to vary independently. The calculations are performed assuming three different size probability density functions: the normal distribution, the lognormal distribution and a general histogram distribution. In all cases considered, the computation of the RSM only requires a two-dimensional Fourier integral and the integrand has a simple analytical expression, i.e. there is no significant increase in computing times by taking size and shape fluctuations into account. The approach presented is compatible with most lattice disorder models (dislocations, inclusions, mosaicity, ...) and allows a straightforward account of the instrumental resolution. The applicability of the model is illustrated with the case of an yttria-stabilized zirconia film grown on sapphire.
Synthesis, Characterization, and Self-Controlled Orthorhombic to Tetragonal Polymorphic Transformation in BaTiO3 Nanoparticles

NASA Astrophysics Data System (ADS)

Ram, S.; Jana, A.; Kundu, T. K.

The phase formation and thermal-induced phase transformation are studied in BaTiO3 nanoparticles. 2 h of heating a polymer precursor at 550°C in air formed a single phase BaTiO3 of 15 nm average crystallite size D. The X-ray diffraction peaks are analyzed assuming a Pnma orthorhombic (o) crystal structure of lattice parameters a = 0.6435 nm, b = 0.5306 nm, and c = 0.8854 nm. The lattice volume V = 0.3023 nm3, with z = 4 formula units, yields a density ρ = 5.124 g/cm3. This is a new polymorph in comparison to well-known Pm3m tetragonal (t) structure, V = 0.0644 nm3 or ρ = 6.016 g/cm3 (z = 1). An o ↦ t transformation appears on heating at temperature as high as 650°C in air. A proposed model explains the transformation above a certain D value in terms of the Gibbs free energy. Unless heating above 750°C, the two phases coexist in a composite structure (D≤27 nm), with as much residual o-phase trace as ~28 vol%. As a function of temperature both the phases decrease in the V values up to 0.2975 and 0.0643 nm3 at 750°C respectively (0.0650 nm3 at 650°C). This is an important parameter for designing useful ferroelectric and other properties in a hybrid composite structure.
DOE Office of Scientific and Technical Information (OSTI.GOV)

Salili, S.M.; School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran; Ataie, A., E-mail: aataie@ut.ac.ir

This research aimed to synthesize nanostructured strontium-doped lanthanum manganite, La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSMO), with its Curie temperature (T{sub c}) adjusted to the therapeutic range, through a mechanothermal route. In order to investigate the effect of heat treatment temperature and duration on the resulting crystallite size, morphology, magnetic behavior and Curie temperature, the starting powder mixture was milled in a planetary ball mill before being subsequently heat treated at distinct temperatures for different time lengths. The composition, morphology, and magnetic behavior were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopymore » (HRTEM), selected area electron diffraction (SAED) and vibrating sample magnetometer (VSM). In addition, magnetic properties were further investigated using an alternating current (AC) susceptometer and thermo-magnetic analyzer. 20 h of milling produced a crystallite size reduction leading to a decrease in the heat treatment temperature of LSMO synthesis to 800 °C. Moreover, SEM analysis has shown the morphology of a strong agglomeration of fine nanoparticles. HRTEM showed clear lattice fringes of high crystallinity. The mean crystallite and particle size of 20-hour milled sample heat treated at 1100 °C for 10 h are relatively 69 and 100 nm, respectively. The VSM data at room temperature, indicated a paramagnetic behavior for samples heat treated at 800 °C. However, by increasing heat treatment temperature to 1100 °C, LSMO indicates a ferromagnetic behavior with well-adjusted Curie temperature of 320 K, suitable for hyperthermia applications. Also, reentrant spin glass (RSG) behavior has been found in heat treated samples. The particles are coated with (3-aminopropyl) triethoxysilane (APTES) for biocompatibility purposes; Fourier transform infrared spectroscopy (FTIR) and thermo-gravimetric analysis (TGA) are used for further confirmation of APTES coating. - Highlights: • La{sub 0.8}Sr{sub 0.2}MnO{sub 3} nanoparticles were synthesized via a mechanothermal route. • We report a significant reduction in the heat treatment temperature. • The Curie temperature was tuned within the therapeutic range. • The particles were coated with (3-aminopropyl) triethoxysilane for biocompatibility purposes.« less
Effect of X-ray Line Spectra Profile Fitting with Pearson VII, Pseudo-Voigt and Generalized Fermi Functions on Asphalt Binder Aromaticity and Crystallite Parameters

NASA Astrophysics Data System (ADS)

Gebresellasie, K.; Shirokoff, J.; Lewis, J. C.

2012-12-01

X-ray line spectra profile fitting using Pearson VII, pseudo-Voigt and generalized Fermi functions was performed on asphalt binders prior to the calculation of aromaticity and crystallite size parameters. The effects of these functions on the results are presented and discussed in terms of the peak profile fit parameters, the uncertainties in calculated values that can arise owing to peak shape, peak features in the pattern and crystallite size according to the asphalt models (Yen, modified Yen or Yen-Mullins) and theories. Interpretation of these results is important in terms of evaluating the performance of asphalt binders widely used in the application of transportation systems (roads, highways, airports).
Molecular dynamics modeling of PPTA crystallite mechanical properties in the presence of defects

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

Mercer, Brian; Zywicz, Edward; Papadopoulos, Panayiotis

Here, the mechanical properties of PPTA crystallites, the fundamental building blocks of aramid polymer fibers such as Kevlar® and Twaron®, are studied here using molecular dynamics simulations. The ReaxFF interatomic potential is employed to study crystallite failure via covalent and hydrogen bond rupture in constant strain-rate tensile loading simulations. Emphasis is placed on analyzing how chain-end defects in the crystallite influence its mechanical response and fracture strength. Chain-end defects are found to affect the behavior of nearby chains in a region of the PPTA crystallite that is small relative to the typical crystallite size in manufactured aramid fibers. The centralmore » Csingle bondN bond along the backbone chain is identified as the weakest in the PPTA polymer chain backbone in dynamic strain-to-failure simulations of the crystallite. It is found that clustering of chain-ends leads to reduced crystallite strength and crystallite failure via hydrogen bond rupture and chain sliding, whereas randomly scattered defects impact the strength less and failure is by covalent bond rupture and chain scission. The axial crystallite modulus increases with increasing chain length and is independent of chain-end defect locations. On the basis of these findings, a theoretical model is proposed to predict the axial modulus as a function of chain length.« less
Molecular dynamics modeling of PPTA crystallite mechanical properties in the presence of defects

DOE PAGES

Mercer, Brian; Zywicz, Edward; Papadopoulos, Panayiotis

2017-03-11

Here, the mechanical properties of PPTA crystallites, the fundamental building blocks of aramid polymer fibers such as Kevlar® and Twaron®, are studied here using molecular dynamics simulations. The ReaxFF interatomic potential is employed to study crystallite failure via covalent and hydrogen bond rupture in constant strain-rate tensile loading simulations. Emphasis is placed on analyzing how chain-end defects in the crystallite influence its mechanical response and fracture strength. Chain-end defects are found to affect the behavior of nearby chains in a region of the PPTA crystallite that is small relative to the typical crystallite size in manufactured aramid fibers. The centralmore » Csingle bondN bond along the backbone chain is identified as the weakest in the PPTA polymer chain backbone in dynamic strain-to-failure simulations of the crystallite. It is found that clustering of chain-ends leads to reduced crystallite strength and crystallite failure via hydrogen bond rupture and chain sliding, whereas randomly scattered defects impact the strength less and failure is by covalent bond rupture and chain scission. The axial crystallite modulus increases with increasing chain length and is independent of chain-end defect locations. On the basis of these findings, a theoretical model is proposed to predict the axial modulus as a function of chain length.« less
Imaging of electrical response of NiO x under controlled environment with sub-25-nm resolution

DOE PAGES

Jacobs, Christopher B.; Ievlev, Anton V.; Collins, Liam F.; ...

2016-07-19

The spatially resolved electrical response of rf-sputtered polycrystalline NiO x films composed of 40 nm crystallites was investigated under different relative humidity levels (RH). The topological and electrical properties (surface potential and resistance) were characterized using Kelvin probe force microscopy (KPFM) and conductive scanning probe microscopy at 0%, 50%, and 80% relative humidity with sub 25nm resolution. The surface potential of NiO x decreased by about 180 mV and resistance decreased in a nonlinear fashion by about 2 G when relative humidity was increased from 0% to 80%. The dimensionality of surface features obtained through autocorrelation analysis of topological, surfacemore » potential and resistance maps increased linearly with increased relative humidity as water was adsorbed onto the film surface. Spatially resolved surface potential and resistance of the NiO x films were found to be heterogeneous, with distinct features that grew in size from about 60 nm to 175 nm between 0% and 80% RH levels, respectively. Here, we find that the changes in the heterogeneous character of the NiO films are consistent through the topological, surface potential, and resistance measurements, suggesting that the nanoscale surface potential and resistance properties converge with the mesoscale properties as water is adsorbed onto the NiO x film.« less
The fracture strength of cryomilled 99.7 Al nanopowders consolidated by high frequency induction sintering

NASA Astrophysics Data System (ADS)

El-Danaf, Ehab A.; Baig, Muneer; Almajid, Abdulhakim A.; Soliman, Mahmoud S.

2014-08-01

Mechanical Attrition of metallic powders induces severe plastic deformation and consequently reduces the average grain size. Powders of 99.7 Al (45μm particle size), cryomilled for 7 hrs having a crystal size of ~ 20 nm, were consolidated by high frequency induction sintering under a constant pressure of 50 MPa and at two temperatures of 500 and 550 °C for two sintering dwell times of 1 and 3 minutes at a constant heating rate of 400 °C/min. The bright field TEM image and X-ray line broadening technique, for the cryomilled powders, were used to measure-the crystallite size. Simple compression at an initial strain rate of 10-4 s-1 was conducted at room temperature, 373 and 473 K, and the yield strength was documented and correlated with the sintering parameters. The as-received 99.7 Al powders-consolidated using one of the sintering parameters was used as a reference material to compare the mechanical properties. Hardness, density and crystal size of the consolidated sample, that gave the highest yield and fracture strength, were measured.
Phosphate-enhanced cytotoxicity of zinc oxide nanoparticles and agglomerates.

PubMed

Everett, W Neil; Chern, Christina; Sun, Dazhi; McMahon, Rebecca E; Zhang, Xi; Chen, Wei-Jung A; Hahn, Mariah S; Sue, H-J

2014-02-10

Zinc oxide (ZnO) nanoparticles (NPs) have been found to readily react with phosphate ions to form zinc phosphate (Zn3(PO4)2) crystallites. Because phosphates are ubiquitous in physiological fluids as well as waste water streams, it is important to examine the potential effects that the formation of Zn3(PO4)2 crystallites may have on cell viability. Thus, the cytotoxic response of NIH/3T3 fibroblast cells was assessed following 24h of exposure to ZnO NPs suspended in media with and without the standard phosphate salt supplement. Both particle dosage and size have been shown to impact the cytotoxic effects of ZnO NPs, so doses ranging from 5 to 50 μg/mL were examined and agglomerate size effects were investigated by using the bioinert amphiphilic polymer polyvinylpyrrolidone (PVP) to generate water-soluble ZnO ranging from individually dispersed 4 nm NPs up to micron-sized agglomerates. Cell metabolic activity measures indicated that the presence of phosphate in the suspension media can led to significantly reduced cell viability at all agglomerate sizes and at lower ZnO dosages. In addition, a reduction in cell viability was observed when agglomerate size was decreased, but only in the phosphate-containing media. These metabolic activity results were reflected in separate measures of cell death via the lactate dehydrogenase assay. Our results suggest that, while higher doses of water-soluble ZnO NPs are cytotoxic, the presence of phosphates in the surrounding fluid can lead to significantly elevated levels of cell death at lower ZnO NP doses. Moreover, the extent of this death can potentially be modulated or offset by tuning the agglomerate size. These findings underscore the importance of understanding how nanoscale materials can interact with the components of surrounding fluids so that potential adverse effects of such interactions can be controlled. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.
Change in structural morphology on addition of ZnO and its effect on fluorescence of Yb³⁺/Er³⁺ doped Y₂O₃.

PubMed

Yadav, R V; Verma, R K; Kaur, G; Rai, S B

2013-02-15

Yb(3+)/Er(3+) codoped Y(2)O(3) phosphor and its composite with ZnO have been synthesized by combustion method. Morphology of the materials has been investigated using X-ray diffraction pattern (XRD) and scanning electron microscopy (SEM) techniques. XRD confirms the constituents as Y(2)O(3) and ZnO, with average crystallite size of 112 nm. On addition of ZnO, a small shifting in XRD pattern of Y(2)O(3) is observed. SEM pattern suggests that the average particle size lies in micro-range (0.5 μm). A dumble like structure is observed for hybrid material on annealing at 1473 K. A strong green (525, 546 nm) with weak blue (411 nm) and red (657 nm) emissions through upconversion has been observed from the phosphor on excitation with 976 nm diode laser. The observed emissions involve (2)H(9/2)→(4)I(15/2), (2)H(11/2)→(4)I(15/2), (4)S(3/2)→(4)I(15/2) and (4)F(9/2)→(4)I(15/2) electronic transitions, respectively. The upconversion process has been confirmed by power dependence measurements and its slope value was found to be 1.85, 1.72 for green and red emissions, respectively. On addition of ZnO, the intensity of these emissions is enhanced several times. The reason behind the enhancement is discussed with the help of the emitting level lifetime. An interesting dual mode property (upconversion and downconversion) to the same material has been observed on excitation with 532 nm laser source. Copyright © 2012 Elsevier B.V. All rights reserved.
Impact of crystalline defects and size on X-ray line broadening: A phenomenological approach for tetragonal SnO{sub 2} nanocrystals

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

Muhammed Shafi, P.; Chandra Bose, A., E-mail: acbose@nitt.edu

2015-05-15

Nanocrystalline tin oxide (SnO{sub 2}) powders with different grain size were prepared by chemical precipitation method. The reaction was carried out by varying the period of hydrolysis and the as-prepared samples were annealed at different temperatures. The samples were characterized using X-ray powder diffractometer and transmission electron microscopy. The microstrain and crystallite size were calculated for all the samples by using Williamson-Hall (W-H) models namely, isotropic strain model (ISM), anisotropic strain model (ASM) and uniform deformation energy density model (UDEDM). The morphology and particle size were determined using TEM micrographs. The directional dependant young’s modulus was modified as an equationmore » relating elastic compliances (s{sub ij}) and Miller indices of the lattice plane (hkl) for tetragonal crystal system and also the equation for elastic compliance in terms of stiffness constants was derived. The changes in crystallite size and microstrain due to lattice defects were observed while varying the hydrolysis time and the annealing temperature. The dependence of crystallite size on lattice strain was studied. The results were correlated with the available studies on electrical properties using impedance spectroscopy.« less
Structural, magnetic and impedance spectroscopic analysis of LaFeO3 nano-particles

NASA Astrophysics Data System (ADS)

Rao, T. Lakshmana; Pradhan, M. K.; Dash, S.

2018-04-01

Physical properties are known to be drastically varied with crystallite size and in a multifunctional material this size reduction is seem to be interesting. One such material is chosen as LaFeO3 nanoparticles which have been prepared by wet-chemical route. The average particle size found to be in the order of 45nm in which the chemical content of the unit cell has been verified. A distorted orthorhombic structure with Pbnm space group is possessed by this nanoparticle. From the bifurcation of ZFC and FC in low field, behavior of inverse susceptibility and the small hysteresis loop favors the material to be in a weak FM state well below the Neel temperature. The electrical behavior and the conduction mechanism above room temperature have been studied by cole-cole plot of the Impedance spectra. The high frequency depressed semi circles represent the grain conduction while the intermediate frequency semi circles appear may be due to grain boundary effect.
Synthesis and Characterization of Zirconium Substituted Cobalt Ferrite Nanopowders

DOE PAGES

Rus, S. F.; Vlazan, P.; Herklotz, A.

2016-01-01

Nanocrystalline ferrites; CoFe 2O 4 (CFO) and CoFe 1.9Zr 0.1O 4 (CFZO) have been synthesized through chemical coprecipitation method. Moreover, the role played by the zirconium ions in improving the magnetic and structural properties is analyzed. X-ray diffraction revealed a single-phase cubic spinel structure for both materials, where the crystallite size increases and the lattice parameter decreases with substitution of Zr. The average sizes of the nanoparticles are estimated to be 16-19 nm. These sizes are small enough to achieve the suitable signal to noise ratio in the high density recording media. An increase in the saturation magnetization with themore » substitution of Zr suggests the preferential occupation of Zr 4+ ions in the tetrahedral sites. A decrease in the coercivity values indicates the reduction of magneto-crystalline anisotropy. We investigated spinel ferrites can be used also in recoding media due to the large value of coercivity 1000 Oe which is comparable to those of hard magnetic materials.« less
Effect of size and shape dependent anisotropy on superparamagnetic property of CoFe2O4 nanoparticles and nanoplatelets

NASA Astrophysics Data System (ADS)

Chandekar, Kamlesh V.; Kant, K. Mohan

2017-09-01

Superparamagnetic cobalt ferrite (CoFe2O4) spherical nanoparticles and rhomboidal nanoplatelets were synthesized by co-precipitation at 80 °C (S1) and hydrothermal route at 150 °C (S2). X-ray diffraction (XRD) pattern confirms formation of cubic inverse spinel structure of as prepared cobalt ferrite samples (S1 and S2) with average crystallite size of 13 nm and 18.7 nm for S1 and S2 respectively. Transmission electron microscopy (TEM) reveals spherical and rhomboidal shaped with average particle size 16.7 nm (S1) and 19.8 nm (S2). The zero field cooled magnetization MZFCvs. T exhibit a broad maxima at 400 K and 510 K for S1 and S2 respectively. The blocking temperature TB is obtained as 310 K and 341 K for S1 and S2 respectively, by fitting coercive field at different temperatures to T 1 / 2 law. The morphology of S1 and S2 corresponds to shape dependence of continuum approach. The effective demagnetization factors estimated as ΔN1 = 0 and ΔN2 = 0 . 749 for S1 and S2 samples respectively. The uniaxial anisotropy and shape anisotropy observed to be dominant in spherical shaped and rhomboidal shaped CoFe2O4 nanoparticles respectively. The uniaxial anisotropy constant of S1 sample is estimated as 56 (kJ/m3) at TB = 310 K whereas the effective anisotropy constant for S2 sample is 627 (kJ/m3) at TB = 341 K , in which shape anisotropy constant 605 (kJ/m3) dominates over contribution from uniaxial anisotropy constant 22 (kJ/m3) in S2 sample.
Effect of vacuum annealing and substrate temperature on structural and optical properties of ZnIn2Se4 thin films

NASA Astrophysics Data System (ADS)

El-Nahass, M. M.; Attia, A. A.; Salem, G. F.; Ali, H. A. M.; Ismail, M. I.

2013-09-01

Zinc indium selenide (ZnIn2Se4) thin films were prepared by the thermal evaporation technique with high deposition rate. The effect of thermal annealing in vacuum on the crystallinity of the as-deposited films was studied at different temperatures (523, 573 and 623 K). The effect of substrate temperature (623 K) for different thickness values (173, 250, 335 and 346 nm) on the optical parameters of ZnIn2Se4 was also studied. The structural studies showed nanocrystalline nature of the room temperature (300 K) deposited films with crystallite size of about a few nanometers. The crystallite size increased up to 31 nm with increasing the annealing temperature in vacuum. From the reflection and transmission data, the refractive index n and the extinction coefficient k were estimated for ZnIn2Se4 thin films and they were found to be independent of film thickness. Analysis of the absorption coefficient data of the as-deposited films revealed the existence of allowed direct and indirect transitions with optical energy gaps of 2.21 eV and 1.71 eV, respectively. These values decreased with increasing annealing temperature. At substrate temperature of 623 K, the direct band gap increased to 2.41 eV whereas the value of indirect band gap remained nearly unchanged. The dispersion analysis showed that the values of the oscillator energy Eo, dispersion energy Ed, dielectric constant at infinite frequency ε∞, and lattice dielectric constant εL were changed appreciably under the effect of annealing and substrate temperature. The covalent nature of structure was studied as a function of the annealing and substrate temperature using an empirical relation for the dispersion energy Ed. Generalized Miller's rule and linear refractive index were used to estimate the nonlinear susceptibility and nonlinear refractive index of the thin films.
Cytotoxicity evaluation of ZnO-eugenol (ZOE) using different ZnO structure on human gingival fibroblast

NASA Astrophysics Data System (ADS)

Bakhori, Siti Khadijah Mohd; Mahmud, Shahrom; Masudi, Sam'an Malik; Seeni, Azman; Mohamad, Dasmawati; Ann, Ling Chuo; Sirelkhatim, Amna

2017-07-01

Application of ZnO is widely used in many industries, such as in optoelectronic devices, automotive, textile, cosmetics, medical and dentistry. In this study, emphasis was given on ZnO-eugenol (ZOE) that has been used in dental restoration. ZOE contained 80% ZnO and 20% eugenol. ZOE exhibited selective toxicity that could kill bacteria but safe on human cells. The safety of ZOE on humans is critically important. Two types of ZnO with different morphology, namely ZnO-A and ZnO-K were used to make ZOE (ZOE-A and ZOE-K) and the cytotoxicity level on human gingival fibroblast (HGF) cell line were evaluated. Both ZnO were characterized for its morphology and structural using Field Emission Scanning Electron Microscopy (FESEM) and X-ray Diffraction (XRD), respectively. The cytotoxicity level was evaluated using CCK-8 assay where the percentage of viable cells after 72 h were observed. The result showed ZnO-A, containing mostly rod-like shape with a crystallite size of 37.5 nm, had a higher percentage of viable cells after 72 h. Sample ZnO-K, containing irregular shape morphology with bigger crystallite size of 42.2 nm, had a lower percentage of viable cells after 72 h. The HGF cell line was treated with extract dilution of ZOE-A and ZOE-K at 5, 10 and 15%, respectively. At 15% of extracts dilution, 97.3% of the HGF cells survived (for ZOE-A) while the survival percentage of ZOE-K was only 88.1%. This fact was probably due to the larger surface-to-volume ratio of ZnO-A that gave better interlocking bond in ZOE-A. This interlocking bond can prevent the ZnO and eugenol elements leaching out from the ZOE matrix thereby decrease in cytotoxicity effects on HGF.

Investigation of microstructure, micro-mechanical and optical properties of HfTiO{sub 4} thin films prepared by magnetron co-sputtering

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

Mazur, Michal, E-mail: michal.mazur@pwr.edu.pl; Wojcieszak, Damian; Domaradzki, Jaroslaw

2015-12-15

Highlights: • HfTiO{sub 4} thin films were deposited by magnetron co-sputtering. • As-prepared and annealed at 800 °C thin films were nanocrystalline. • Optical properties and hardness were investigated in relation to thin films structure. • Hardness was 3-times higher in the case of as-deposited thin films. • HfTiO{sub 4} thin films are suitable for use as optical coatings with protective properties. - Abstract: Titania (TiO{sub 2}) and hafnium oxide (HfO{sub 2}) thin films are in the focus of interest to the microelectronics community from a dozen years. Because of their outstanding properties like, among the others, high stability, highmore » refractive index, high electric permittivity, they found applications in many optical and electronics domains. In this work discussion on the hardness, microstructure and optical properties of as-deposited and annealed HfTiO{sub 4} thin films has been presented. Deposited films were prepared using magnetron co-sputtering method. Performed investigations revealed that as-deposited coatings were nanocrystalline with HfTiO{sub 4} structure. Deposited films were built from crystallites of ca. 4–12 nm in size and after additional annealing an increase in crystallites size up to 16 nm was observed. Micro-mechanical properties, i.e., hardness and elastic modulus were determined using conventional load-controlled nanoindentation testing. the annealed films had 3-times lower hardness as-compared to as-deposited ones (∼9 GPa). Based on optical investigations real and imaginary components of refractive index were calculated, both for as-deposited and annealed thin films. The real refractive index component increased after annealing from 2.03 to 2.16, while extinction coefficient increased by an order from 10{sup −4} to 10{sup −3}. Structure modification was analyzed together with optical energy band-gap, Urbach energy and using Wemple–DiDomenico model.« less
Synthesis and magnetic properties of NiFe2-xSmxO4 nanopowder

NASA Astrophysics Data System (ADS)

Hassanzadeh-Tabrizi, S. A.; Behbahanian, Shahrzad; Amighian, Jamshid

2016-07-01

NiFe2-xSmxO4 (x=0.00, 0.05, 0.10 and 0.15) nanopowders were synthesized via a sol-gel combustion route. The structural studies were carried out by X-ray diffractometer, Fourier transform infrared spectroscopy, scanning electron microscopy and transmission electron microscopy. The XRD results confirmed the formation of single-phase spinel cubic structure. The crystallite size decreased with an increase of samarium ion concentration, while lattice parameter and lattice strain increased with samarium substitution. TEM micrographs showed that agglomerated nanoparticles with particle sizes ranging from 35 to 90 nm were obtained. The magnetic studies were carried out using vibrating sample magnetometer. Magnetic measurements revealed that the saturation magnetization (Ms) of NiFe2-xSmxO4 nanoparticles decreases with increasing Sm3+substitution. The reduction of saturation magnetization is attributed to the dilution of the magnetic interaction. The coercivity (Hc) of samples increases by adding samarium.
Structural, Optical, and Electronic Characterization of Fe-Doped Alumina Nanoparticles

NASA Astrophysics Data System (ADS)

Heiba, Zein K.; Mohamed, Mohamed Bakr; Wahba, Adel Maher; Imam, N. G.

2018-01-01

The effects of iron doping on the structural, optical, and electronic properties of doped alumina have been studied. Single-phase iron-doped alumina Al2- x Fe x O3 ( x = 0.00 to 0.30) nanoparticles were synthesized via citrate-precursor method. Formation of single-phase hexagonal corundum structure with no other separate phases was demonstrated by x-ray diffraction (XRD) analysis and Fourier-transform infrared spectroscopy. The effects of iron doping on the α-Al2O3 structural parameters, viz. atomic coordinates, lattice parameters, crystallite size, and microstrain, were estimated from XRD data by applying the Rietveld profile fitting method. Transmission electron microscopy further confirmed the nanosize nature of the prepared samples with size ranging from 12 nm to 83 nm. The electronic band structure was investigated using density functional theory calculations to explain the decrease in the energy gap of Al2- x Fe x O3 as the amount of Fe was increased. The colored emission peaks in the visible region (blue, red, violet) of the electromagnetic spectrum obtained for the Fe-doped α-Al2O3 nanoparticles suggest their potential application as ceramic nanopigments.
EXAFS/XANES studies of plutonium-loaded sodalite/glass waste forms

NASA Astrophysics Data System (ADS)

Richmann, Michael K.; Reed, Donald T.; Kropf, A. Jeremy; Aase, Scott B.; Lewis, Michele A.

2001-09-01

A sodalite/glass ceramic waste form is being developed to immobilize highly radioactive nuclear wastes in chloride form, as part of an electrochemical cleanup process. Two types of simulated waste forms were studied: where the plutonium was alone in an LiCl/KCl matrix and where simulated fission-product elements were added representative of the electrometallurgical treatment process used to recover uranium from spent nuclear fuel also containing plutonium and a variety of fission products. Extended X-ray absorption fine structure spectroscopy (EXAFS) and X-ray absorption near-edge spectroscopy (XANES) studies were performed to determine the location, oxidation state, and particle size of the plutonium within these waste form samples. Plutonium was found to segregate as plutonium(IV) oxide with a crystallite size of at least 4.8 nm in the non-fission-element case and 1.3 nm with fission elements present. No plutonium was observed within the sodalite in the waste form made from the plutonium-loaded LiCl/KCl eutectic salt. Up to 35% of the plutonium in the waste form made from the plutonium-loaded simulated fission-product salt may be segregated with a heavy-element nearest neighbor other than plutonium or occluded internally within the sodalite lattice.
Preparation, characterization and electroluminescence studies of ZnO nanorods for optoelectronic device applications

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

Singh, Anju, E-mail: singh-nk24@yahoo.com; Vishwakarma, H. L., E-mail: horilal5@yahoo.com

2015-07-31

In this work, ZnO nanorods were achieved by a simple chemical precipitation method in the presence of capping agent Poly Vinyl Pyrrolidone (PVP) at room temperature. X-Ray Diffraction (XRD) result indicates that the synthesized undoped ZnO nanorods have wurtzite hexagonal structure without any impurities. It has been seen that the growth orientation of the prepared ZnO nanorods were (101). XRD analysis revealed that the nanorods having the crystallite size 49 nm. The Scanning Electron Microscopy (SEM) image confirmed the size and shape of these nanorods. The diameter of nanorods has been found that 1.52 µm to 1.61 µm and the lengthmore » of about 4.89 µm. It has also been found that at room temperature Ultra Violet Visible (UV-VIS) absorption band is around 355 nm (blue shifted as compared to bulk). Electroluminescence (EL) studies show that emission of light is possible at very small threshold voltage and increases rapidly with increasing applied voltage. It is seen that smaller ZnO nanoparticles give higher electroluminescence brightness starting at lower threshold voltage. The brightness is also affected by increasing the frequency of AC signal.« less
Synthesis and characterization of carbon-coated cobalt ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Bakhshi, Hamed; Shokuhfar, Ali; Vahdati, Nima

2016-09-01

Cobalt ferrite nanoparticles (CFNPs) were prepared via a reverse micelle method. The CFNPs were subsequently coated with carbon shells by means of thermal chemical vapor deposition (TCVD). In this process, acetylene gas (C2H2) was used as a carbon source and the coating was carried out for 1, 2, or 3 h at 750°C. The Ar/C2H2 ratio was 10:1. Heating during the TCVD process resulted in a NP core size that approached 30 nm; the thickness of the shell was less than 10 nm. The composition, structure, and morphology of the fabricated composites were characterized using X-ray diffraction, simultaneous thermal analysis, transmission electron microscopy, high-resolution transmission electron microscopy, and selected-area diffraction. A vibrating sample magnetometer was used to survey the samples' magnetic properties. The deposited carbon shell substantially affected the growth and magnetic properties of the CFNPs. Micro-Raman spectroscopy was used to study the carbon coating and revealed that the deposited carbon comprised graphite, multiwalled carbon nanotubes, and diamond- like carbon. With an increase in coating time, the intensity ratio between the amorphous and ordered peaks in the Raman spectra decreased, which indicated an increase in crystallite size.
Synthesis and characterization of struvite nano particles

NASA Astrophysics Data System (ADS)

Rathod, K. R.; Jogiya, B. V.; Chauhan, C. K.; Joshi, M. J.

2015-06-01

Struvite, Ammonium Magnesium Phosphate Hexahydrate [(AMPH) - (NH4)MgPO4.6(H2O)], is one of the fascinating inorganic phosphate minerals. Struvite is one of the components of the urinary stones. Struvite occurs as crystallites in urine and grows as a type of kidney stone. In this study, struvite nano particles were synthesized by wet chemical technique. The aqueous solutions containing dissolved Mg(CH3COO)2.4H2O and (NH4)H2PO4 mixed at the Mg/P molar ratio of 1.00. The synthesized struvite nano particles were characterized by XRD, FT-IR, Thermal Analysis and TEM. From XRD, crystal structure of the nano particle was found to be orthorhombic and crystalline size was found to be within 11 to 26 nm. The FT-IR spectrum for the struvite nano particles confirmed the presence of a water molecule and metal-oxygen stretching vibration, O-H stretching and bending, N-H bending and stretching, P-O bending and stretching vibrations. The Thermal Analysis was carried out from room temperature to 900°C. From TEM analysis, particle size was 23 to 30 nm. All the results were compared with bulk struvite.
An investigation on the preparation of nanocrystalline hydrous zirconia from zirconium tungstate

NASA Astrophysics Data System (ADS)

Antunes, M.; Perottoni, C. A.; Gouvêa, D.; Machado, G.; Zorzi, J. E.

2018-02-01

Hydrous nanocrystalline zirconia was prepared from an unusual precursor—the bimetallic oxide zirconium tungstate (ZrW2O8)—in alkaline medium. Different experimental conditions (NaOH concentration, time and temperature) were used to investigate the effects on crystallographic, morphological, chemical and thermal characteristics of the products. The resulting materials are composed of particles with a crystal structure similar to that of cubic ZrO2 (or a mixture of tetragonal and cubic phases, depending on the synthesis conditions), with particle size around 5 nm and crystallites around 3 nm in diameter. These particles form high surface area agglomerates, exhibiting mesoporosity and capacity for adsorption of water and carbon dioxide. The synthesis mechanism appears to be constituted, first, by a chemical substitution reaction between the WO4 tetrahedra and hydroxyl ions, with subsequent solubilization of the structure. Indeed, excess hydroxyls in the medium form colloidal zirconium ions which polymerize/condense, generating crystalline nuclei in a process facilitated by heterogeneous nucleation and supersaturation. The presence of residual tungsten in all samples appears to be a key element for stabilizing the size and crystalline structure of the materials produced.
Structural and magnetic properties of sol-gel Co2xNi0.5-x Zn0.5-xFe2O4 thin films

NASA Astrophysics Data System (ADS)

Rebrov, Evgeny V.; Gao, Pengzhao; Verhoeven, Tiny M. W. G. M.; Schouten, Jaap C.; Kleismit, Richard; Turgut, Zafer; Kozlowski, Gregory

2011-03-01

Nanocrystalline Co2xNi0.5-xZn0.5-xFe2O4 (x=0-0.5) thin films have been synthesized with various grain sizes by a sol-gel method on polycrystalline silicon substrates. The morphology as well as magnetic and microwave absorption properties of the films calcined at 1073 K were studied using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and vibrating sample magnetometry. All films were uniform without microcracks. The Co content in the Co-Ni-Zn films resulted in a grain size ranging from 15 to 32 nm while it ranged from 33 to 49 nm in the corresponding powders. Saturation and remnant magnetization increased with increase in grain size, while coercivity demonstrated a drop due to multidomain behavior of crystallites for a given value of x. Saturation magnetization increased and remnant magnetization had a maximum as a function of grain size independent of x. In turn, coercivity increased with x independent of grain size. Complex permittivity of the Co-Ni-Zn ferrite films was measured in the frequency range 2-15 GHz. The highest hysteretic heating rate in the temperature range 315-355 K was observed in CoFe2O4. The maximum absorption band shifted from 13 to 11 GHz as cobalt content increased from x=0.1 to 0.2.
Oxidant effect of La(NO3)3·6H2O solution on the crystalline characteristics of nanocrystalline ZrO2 films grown by atomic layer deposition

NASA Astrophysics Data System (ADS)

Oh, Nam Khen; Kim, Jin-Tae; Kang, Goru; An, Jong-Ki; Nam, Minwoo; Kim, So Yeon; Park, In-Sung; Yun, Ju-Young

2017-02-01

Nanocrystalline ZrO2 films were synthesized by atomic layer deposition method using CpZr[N(CH3)2]3 (Cp = C5H5) as the metal precursor and La(NO3)3·6H2O solution as the oxygen source. La element in the deposited ZrO2 films could not be detected as its content was below the resolution limit of the X-ray photoelectron spectroscopy. The alternative introduction of La(NO3)3·6H2O solution to conventionally used H2O as the oxidant effectively altered the crystalline structure, grain size, and surface roughness of the grown ZrO2 films. Specifically, the crystalline structure of the ZrO2 film changed from a mixture of tetragonal and monoclinic phases to monoclinic phase. The average grain size also increased, and the resulting film surface became rougher. The average grain sizes of the ZrO2 films prepared from La(NO3)3·6H2O solution at concentrations of 10, 20, 30, and 40% were 280, 256, 208, and 200 nm, respectively, whereas that prepared using H2O oxidant was 142 nm. However, the concentration of La(NO3)3·6H2O solution minimally influenced the crystalline characteristics of the nanocrystalline ZrO2 films i.e., the crystalline structure, grain size, and surface roughness except for crystallite size.
Vapor-phase photo-oxidation of methanol over nanosize titanium dioxide clusters dispersed in MCM-41 host material part 1: synthesis and characterization.

PubMed

Bhattacharya, K; Tripathi, A K; Dey, G K; Gupta, N M

2005-05-01

Nanosize clusters of titania were dispersed in mesoporous MCM-41 silica matrix with the help of the incipient wet-impregnation route, using an isopropanol solution of titanium isopropoxide as precursor. The clusters thus formed were of pure anatase phase and their size depended upon the titania loading. In the case of low (< 15 wt %) loadings, the TiO2 particles were X-ray and laser-Raman amorphous, confirming very high dispersion. These particles were mostly of < or = 2 nm size. On the other hand, larger size clusters (2-15 nm) were present in a sample with a higher loading of approximately 21 wt %. These particles of titania, irrespective of their size, exhibited an absorbance behavior similar to that of bulk TiO2. Powder X-ray diffraction, N2-adsorption and transmission electron microscopy results showed that while smaller size particles were confined mostly inside the pore system, the larger size particles occupied the external surface of the host matrix. At the same time, the structural integrity of the host was maintained even though some deformation in the pore system was noticed in the case of the sample having highest loading. The core level X-ray photoelectron spectroscopy results revealed a + 4 valence state of Ti in all the samples. A positive binding energy shift and the increase of the width of Ti 2p peaks were observed, however, with the decrease in the particle size of supported titania crystallites, indicative of a microenvironment for surface sites that is different from that of the bulk.
In-vitro efficacy of different morphology zinc oxide nanopowders on Streptococcus sobrinus and Streptococcus mutans.

PubMed

Mohd Bakhori, Siti Khadijah; Mahmud, Shahrom; Ling, Chuo Ann; Sirelkhatim, Amna Hassan; Hasan, Habsah; Mohamad, Dasmawati; Masudi, Sam'an Malik; Seeni, Azman; Abd Rahman, Rosliza

2017-09-01

ZnO with two different morphologies were used to study the inhibition of Streptococcus sobrinus and Streptococcus mutans which are closely associated with tooth cavity. Rod-like shaped ZnO-A and plate-like shaped ZnO-B were produced using a zinc boiling furnace. The nanopowders were characterized using energy filtered transmission electron microscopy (EFTEM), X-ray diffraction (XRD), photoluminescence (PL) spectroscopy, Raman spectroscopy and dynamic light scattering (DLS) to confirm the properties of the ZnO polycrystalline wurtzite structures. XRD results show that the calculated crystallite sizes of ZnO-A and ZnO-B were 36.6 and 39.4nm, respectively, whereas DLS revealed particle size distributions of 21.82nm (ZnO-A) and 52.21nm (ZnO-B). PL spectra showed ion vacancy defects related to green and red luminescence for both ZnO particles. These defects evolved during the generation of reactive oxygen species which contributed to the antibacterial activity. Antibacterial activity was investigated using microdilution technique towards S. sobrinus and S. mutans at different nanopowder concentrations. Results showed that ZnO-A exhibited higher inhibition on both bacteria compared with ZnO-B. Moreover, S. mutans was more sensitive compared with S. sobrinus because of its higher inhibition rate. Copyright © 2017 Elsevier B.V. All rights reserved.
Structural, morphological, and optical characterizations of Mo, CrN and Mo:CrN sputtered coatings for potential solar selective applications

NASA Astrophysics Data System (ADS)

Ibrahim, Khalil; Mahbubur Rahman, M.; Taha, Hatem; Mohammadpour, Ehsan; Zhou, Zhifeng; Yin, Chun-Yang; Nikoloski, Aleksandar; Jiang, Zhong-Tao

2018-05-01

Mo, CrN, and Mo:CrN sputtered coatings synthesized onto silicon Si(100) substrates were investigated as solar selective surfaces and their potential applications in optical devices. These coatings were characterized using XRD, SEM, UV-vis, and FTIR techniques. XRD investigation, showed a change in CrN thin film crystallite characteristic due to Mo doping. Compared to the CrN coating, the Mo:CrN film has a higher lattice parameter and lower grain size of 4.19 nm and 106.18 nm, respectively. FESEM morphology confirmed the decrement in Mo:CrN crystal size due to Mo doping. Optical analysis showed that in the visible range of the solar spectrum, the CrN coatings exhibit the highest solar absorptance of 66% while the lowest thermal emittance value of 5.67 was recorded for the CrN coating doped with Mo. Consequently, the highest solar selectivity of 9.6, and the energy band-gap of 2.88 eV were achieved with the Mo-doped CrN coatings. Various optical coefficients such as optical absorption coefficient, refractive index, extinction coefficient, real and imaginary parts of dielectric constants, and energy loss functions of these coatings were also estimated from the optical reflectance data recorded in the wavelength range of 190-2300 nm.
Improved conversion efficiency of dye sensitized solar cell using Zn doped TiO{sub 2}-ZrO{sub 2} nanocomposite

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

Tomar, Laxmi J., E-mail: laxmi-tomar86@yahoo.com; Bhatt, Piyush J.; Desai, Rahul K.

TiO{sub 2}-ZrO{sub 2} and Zn doped TiO{sub 2}-ZrO{sub 2} nanocomposites were prepared by hydrothermal method for dye sensitized solar cell (DSSC) application. The structural and optical properties were investigated by X –ray diffraction (XRD) and UV-Visible spectroscopy respectively. XRD results revealed the formation of material in nano size. The average crystallite size is 22.32 nm, 17.41 nm and 6.31 nm for TiO{sub 2}, TiO{sub 2}-ZrO{sub 2} and Zn doped TiO{sub 2}-ZrO{sub 2} nanocomposites respectively. The optical bandgap varies from 2.04 eV to 3.75 eV. Dye sensitized solar cells were fabricated using the prepared material. Pomegranate juice was used as a sensitizer and graphitemore » coated conducting glass plate was used as counter electrode. The I – V characteristics were recorded to measure photo response of DSSC. Photovoltaic parameter like open circuit voltage, power conversion efficiency, and fill factor were evaluated for fabricated solar cell. The power conversion efficiency of DSSC fabricated with TiO{sub 2}, TiO{sub 2}-ZrO{sub 2} and Zn doped TiO{sub 2}-ZrO{sub 2} nanocomposites were found 0.71%, 1.97% and 4.58% respectively.« less
Synthesis and Characterization of CeO2 Nanoparticles via Solution Combustion Method for Photocatalytic and Antibacterial Activity Studies

PubMed Central

Ravishankar, Thammadihalli Nanjundaiah; Ramakrishnappa, Thippeswamy; Nagaraju, Ganganagappa; Rajanaika, Hanumanaika

2015-01-01

CeO2 nanoparticles have been proven to be competent photocatalysts for environmental applications because of their strong redox ability, nontoxicity, long-term stability, and low cost. We have synthesized CeO2 nanoparticles via solution combustion method using ceric ammonium nitrate as an oxidizer and ethylenediaminetetraacetic acid (EDTA) as fuel at 450 °C. These nanoparticles exhibit good photocatalytic degradation and antibacterial activity. The obtained product was characterized by various techniques. X-ray diffraction data confirms a cerianite structure: a cubic phase CeO2 having crystallite size of 35 nm. The infrared spectrum shows a strong band below 700 cm−1 due to the Ce−O−Ce stretching vibrations. The UV/Vis spectrum shows maximum absorption at 302 nm. The photoluminescence spectrum shows characteristic peaks of CeO2 nanoparticles. Scanning electron microscopy (SEM) images clearly show the presence of a porous network with a lot of voids. From transmission electron microscopy (TEM) images, it is clear that the particles are almost spherical, and the average size of the nanoparticles is found to be 42 nm. CeO2 nanoparticles exhibit photocatalytic activity against trypan blue at pH 10 in UV light, and the reaction follows pseudo first-order kinetics. Finally, CeO2 nanoparticles also reduce CrVI to CrIII and show antibacterial activity against Pseudomonas aeruginosa. PMID:25969812
Luminescence variations in hydroxyapatites doped with Eu2+ and Eu3+ ions.

PubMed

Graeve, Olivia A; Kanakala, Raghunath; Madadi, Abhiram; Williams, Brandon C; Glass, Katelyn C

2010-05-01

We present a detailed analysis of the luminescence behavior of europium-doped hydroxyapatite (HAp) and calcium-deficient hydroxyapatite (Ca-D HAp) nanopowders. The results show that, while both powders are similar in crystallite size, particle size, and morphology, the luminescence behavior differs significantly. For the HAp:Eu powders, the emission is clearly from Eu(3+) ions and corresponds to typical (5)D(0) --> (7)F(J) emissions, whereas for the Ca-D HAp:Eu powders, we also see a broad emission with two peaks at 420 and 445 nm, corresponding to the 4f(6)5d(1) --> 4f(7) ((8)S(7/2)) transition of Eu(2+). The powders are weakly luminescent in the as-synthesized state, as expected for combustion-synthesized materials and have higher emission intensities as the heat treatment temperature is increased. Luminescence spectra obtained using an excitation wavelength of 254 nm are weak for all samples. Excitation wavelengths of 305, 337, and 359 nm, are better at promoting the Eu(3+) and Eu(2+) emissions in hydroxyapatites. We propose that fluorescence measurements are an excellent way of qualitatively determining the phase composition of europium-doped hydroxyapatite powders, since powders that exhibit a blue emission contain substantial amounts of Ca-D HAp, allowing the determination of the presence of this phase in mixed-phase hydroxyapatites. Copyright (c) 2010 Elsevier Ltd. All rights reserved.
The effect of temperature on the structure and magnetic properties of Co0.5Ni0.5Fe2O4 spinel nanoferrite

NASA Astrophysics Data System (ADS)

Abdallah, Hafiz M. I.; Moyo, Thomas; Ngema, Nokwanda

2015-11-01

Nanocrystalline Co0.5Ni05Fe2O4 ferrite with average crystallite size of 7.6 nm and lattice constant of 0.8372 nm was synthesized via a glycol-thermal process. The structure parameters and morphology of the as-synthesized sample and annealed samples were characterized by XRD, EDX, FTIR, HRSEM and HRTEM. The hyperfine interactions, iron distribution on the tetrahedral and octahedral sites for the as-synthesized sample and samples annealed at 500 °C were deduced by Mössbauer spectroscopy measurements at 300 K. The magnetization measurements for the as-synthesized and annealed samples (300-900 °C) were obtained by a vibrating sample magnetometer on a cryogen free measurement system at different isothermal temperatures (4-300 K) in external applied magnetic fields of ±5 T. The temperature dependence of the magnetic properties such as coercive field, saturation magnetization, remanent magnetization and squareness of hysteresis loops were investigated. The sample transformed from single-domain to multi-domain configuration at particle size of about 31 nm. At 300 K, the sample annealed at 700 °C exhibits a maximum coercivity. The as-prepared sample shows a substantial increase in coercivity from 0.182 kOe at 300 K to 6.018 kOe at 4 K.
Crystallinity of the epitaxial heterojunction of C60 on single crystal pentacene

NASA Astrophysics Data System (ADS)

Tsuruta, Ryohei; Mizuno, Yuta; Hosokai, Takuya; Koganezawa, Tomoyuki; Ishii, Hisao; Nakayama, Yasuo

2017-06-01

The structure of pn heterojunctions is an important subject in the field of organic semiconductor devices. In this work, the crystallinity of an epitaxial pn heterojunction of C60 on single crystal pentacene is investigated by non-contact mode atomic force microscopy and high-resolution grazing incidence x-ray diffraction. Analysis shows that the C60 molecules assemble into grains consisting of single crystallites on the pentacene single crystal surface. The in-plane mean crystallite size exceeds 0.1 μm, which is at least five time larger than the size of crystallites deposited onto polycrystalline pentacene thin films grown on SiO2. The results indicate that improvement in the crystal quality of the underlying molecular substrate leads to drastic promotion of the crystallinity at the organic semiconductor heterojunction.
Modelling and validation of particle size distributions of supported nanoparticles using the pair distribution function technique

DOE PAGES

Gamez-Mendoza, Liliana; Terban, Maxwell W.; Billinge, Simon J. L.; ...

2017-04-13

The particle size of supported catalysts is a key characteristic for determining structure–property relationships. It is a challenge to obtain this information accurately and in situ using crystallographic methods owing to the small size of such particles (<5 nm) and the fact that they are supported. In this work, the pair distribution function (PDF) technique was used to obtain the particle size distribution of supported Pt catalysts as they grow under typical synthesis conditions. The PDF of Pt nanoparticles grown on zeolite X was isolated and refined using two models: a monodisperse spherical model (single particle size) and a lognormalmore » size distribution. The results were compared and validated using scanning transmission electron microscopy (STEM) results. Both models describe the same trends in average particle size with temperature, but the results of the number-weighted lognormal size distributions can also accurately describe the mean size and the width of the size distributions obtained from STEM. Since the PDF yields crystallite sizes, these results suggest that the grown Pt nanoparticles are monocrystalline. As a result, this work shows that refinement of the PDF of small supported monocrystalline nanoparticles can yield accurate mean particle sizes and distributions.« less
Modelling and validation of particle size distributions of supported nanoparticles using the pair distribution function technique

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

Gamez-Mendoza, Liliana; Terban, Maxwell W.; Billinge, Simon J. L.

The particle size of supported catalysts is a key characteristic for determining structure–property relationships. It is a challenge to obtain this information accurately and in situ using crystallographic methods owing to the small size of such particles (<5 nm) and the fact that they are supported. In this work, the pair distribution function (PDF) technique was used to obtain the particle size distribution of supported Pt catalysts as they grow under typical synthesis conditions. The PDF of Pt nanoparticles grown on zeolite X was isolated and refined using two models: a monodisperse spherical model (single particle size) and a lognormalmore » size distribution. The results were compared and validated using scanning transmission electron microscopy (STEM) results. Both models describe the same trends in average particle size with temperature, but the results of the number-weighted lognormal size distributions can also accurately describe the mean size and the width of the size distributions obtained from STEM. Since the PDF yields crystallite sizes, these results suggest that the grown Pt nanoparticles are monocrystalline. As a result, this work shows that refinement of the PDF of small supported monocrystalline nanoparticles can yield accurate mean particle sizes and distributions.« less

Correlating Sampling and Intensity Statistics in Nanoparticle Diffraction Experiments

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

Ozturk, Hande; Yan, Hanfei; Hill, John P.

2015-08-01

In this article, [Öztürk, Yan, Hill & Noyan (2014). J. Appl. Cryst. 47, 1016-1025] it was shown that the sampling statistics of diffracting particle populations within a polycrystalline ensemble depended on the size of the constituent crystallites: broad X-ray peak breadths enabled some nano-sized particles to contribute more than one diffraction spot to Debye-Scherrer rings. Here it is shown that the equations proposed by Alexander, Klug & Kummer [J. Appl. Phys. (1948), 19, 742-753] (AKK) to link diffracting particle and diffracted intensity statistics are not applicable if the constituent crystallites of the powder are below 10 nm. In this sizemore » range, (i) the one-to-one correspondence between diffracting particles and Laue spots assumed in the AKK analysis is not satisfied, and (ii) the crystallographic correlation between Laue spots originating from the same grain invalidates the assumption that all diffracting plane normals are randomly oriented and uncorrelated. Such correlation produces unexpected results in the selection of diffracting grains. Three or more Laue spots from a given grain for a particular reflection can only be observed at certain wavelengths. In addition, correcting the diffracted intensity values by the traditional Lorentz term, 1/cos [theta], to compensate for the variation of particles sampled within a reflection band does not maintain fidelity to the number of poles contributing to the diffracted signal. A new term, cos [theta]B/cos [theta], corrects this problem.« less
Xenon-ion irradiation of Co/Si bilayers: Magnetic and structural properties

NASA Astrophysics Data System (ADS)

Novaković, M.; Popović, M.; Zhang, K.; Čubrović, V.; Bibić, N.; Rakočević, Z.

2018-07-01

Evolution of the structure of cobalt-silicon films during Xe ions irradiation has been studied and the same is correlated with magnetic properties. The polycrystalline cobalt films were deposited by electron beam evaporation method to a thickness of 50 nm on crystalline silicon (c-Si) and silicon with pre-amorphized surface (a-Si). After deposition the layers were irradiated with 400 keV Xe ions to the fluences in the range of 2-30 × 1015 ions/cm2. Structural analysis was done by means of transmission electron microscopy, atomic force microscopy (AFM) and X-ray diffraction (XRD), while the magnetic properties were analyzed by using magneto-optical Kerr effect (MOKE) technique. For the both types of substrate the AFM and XRD results show that after Xe ions irradiation the layers become more rough and the grain size of the crystallites increases; the effects being more evidenced for all fluences for the layers deposited on pre-amorphized Si. The MOKE measurements provided the in-plane azimuthal angular dependence of the hysteresis loops and the change of magnetization with the structural parameters. Although the coercive field is influenced by the surface roughness, in the case of c-Si substrate we found it is much more determined by the size of the crystallites. Additionally, independently on the substrate used the magnetic anisotropy in the Co films disappeared as the Xe ion fluence increased, indicating that the changes of magnetization in both systems occur for similar reasons.
Homocomposites of Polylactide (PLA) with Induced Interfacial Stereocomplex Crystallites

PubMed Central

2015-01-01

The demand for “green” degradable composite materials increases with growing environmental awareness. The key challenge is achieving the preferred physical properties and maintaining their eco-attributes in terms of the degradability of the matrix and the filler. Herein, we have designed a series of “green” homocomposites materials based purely on polylactide (PLA) polymers with different structures. Film-extruded homocomposites were prepared by melt-blending PLA matrixes (which had different degrees of crystallinity) with PLLA and PLA stereocomplex (SC) particles. The PLLA and SC particles were spherical and with 300–500 nm size. Interfacial crystalline structures in the form of stereocomplexes were obtained for certain particulate-homocomposite formulations. These SC crystallites were found at the particle/matrix interface when adding PLLA particles to a PLA matrix with d-lactide units, as confirmed by XRD and DSC data analyses. For all homocomposites, the PLLA and SC particles acted as nucleating agents and enhanced the crystallization of the PLA matrixes. The SC particles were more rigid and had a higher Young’s modulus compared with the PLLA particles. The mechanical properties of the homocomposites varied with particle size, rigidity, and the interfacial adhesion between the particles and the matrix. An improved tensile strength in the homocomposites was achieved from the interfacial stereocomplex formation. Hereafter, homocomposites with tunable crystalline arrangements and subsequently physical properties, are promising alternatives in strive for eco-composites and by this, creating materials that are completely degradable and sustainable. PMID:26523245
Viscoelastic Properties of Core-Shell-Structured, Hemicellulose-Rich Nanofibrillated Cellulose in Dispersion and Wet-Film States.

PubMed

Tanaka, Reina; Saito, Tsuguyuki; Hänninen, Tuomas; Ono, Yuko; Hakalahti, Minna; Tammelin, Tekla; Isogai, Akira

2016-06-13

We report the viscoelastic properties of core-shell-structured, hemicellulose-rich nanofibrillated cellulose (NFC) in dispersion and wet-film states. The hemicellulose-rich NFC (hemicellulose neutral sugars 23%, carboxylate 0.2 mmol g(-1)), prepared from Japanese persimmons, had a core crystallite thickness of 2.3 nm and unit fibril thickness of 4.2 nm. A carboxylate-rich NFC (hemicellulose neutral sugars 7%, carboxylate 0.9 mmol g(-1)) with crystallite and fibril widths of 2.5 and 3.3 nm, respectively, was used as a reference. The solid-concentration dependencies of the storage moduli of gel-like water dispersions of the hemicellulose-rich NFC were weaker than those of carboxylate-rich NFC, and the dispersions were loosely flocculated even at high salt concentrations and low pH values. The viscoelastic properties of wet NFC films were similar to those of their dispersions; the hemicellulose-rich NFC films were significantly less sensitive to salt concentration and pH and were soft and swollen at high salt concentrations and low pH values.
Green synthesis of magnetite (Fe3O4) nanoparticles using Graptophyllum pictum leaf aqueous extract

NASA Astrophysics Data System (ADS)

Sari, I. P.; Yulizar, Y.

2017-04-01

Magnetite nanoparticles (MNPs) attracted the attention of many researchers due to their unique properties. In this research, nanoscale magnetite particles have been successfully synthesized through an environmentally friendly method using aqueous extract of Graptophyllum pictum leaf (GPLE). In MNPs formation, GPLE acted as a base source and capping agent. Alkaloids in GPLE were hydrolyzed in water and hydroxilated Fe2+ to form Fe3O4 nanoparticles powder through calcination. After the addition of leaf extract, MNPs formation was observed by color change from pale yellow to dark brown. The synthesized nanoparticles were characterized using UV-Vis spectrophotometer, X-Ray diffraction (XRD), and Fourier transform infra red (FTIR) spectroscopy. The results confirmed that MNPs formation indicated the surface plasmon resonance at a maximum wavelength, λmax 291 nm. The average crystallite size is 23.17 nm. The formed MNPs through green synthesis method promise in various medical applications such as drug carrier and targeted therapy.
Synthesis of Diopside by Solution Combustion Process Using Glycine Fuel

NASA Astrophysics Data System (ADS)

Sherikar, Baburao N.; Umarji, A. M.

Nano ceramic Diopside (CaMgSi2O6) powders are synthesized by Solution Combustion Process(SCS) using Calcium nitrate, Magnesium nitrate as oxidizer and glycine as fuel, fumed silica as silica source. Ammonium nitrate (AN) is used as extra oxidizer. Effect of AN on Diopside phase formation is investigated. The adiabatic flame temperatures are calculated theoretically for varying amount of AN according to thermodynamic concept and correlated with the observed flame temperatures. A “Multi channel thermocouple setup connected to computer interfaced Keithley multi voltmeter 2700” is used to monitor the thermal events during the process. An interpretation based on maximum combustion temperature and the amount of gases produced during reaction for various AN compositions has been proposed for the nature of combustion and its correlation with the characteristics of as synthesized powder. These powders are characterized by XRD, SEM showing that the powders are composed of polycrystalline oxides with crystallite size of 58nm to 74nm.
Study of lattice strain and optical properties of nanocrystalline SnO2

NASA Astrophysics Data System (ADS)

Ahmad, Naseem; Khan, Shakeel; Bhargava, Richa; Ansari, Mohd Mohsin Nizam

2018-05-01

Nanocrystalline SnO2 has been synthesized by co-precipitation method by using two solvents (water and ethylene glycol). The structure and surface morphology were investigated using XRD and scanning electron microscope (SEM). The optical properties were studied using diffused reflectance spectroscopy (DRS). From the XRD analysis, the prepared materials are found to be pure crystalline with tetragonal rutile structure. The lattice strain and crystallite size, were calculated using Williamson-Hall method, are found to be 0.00413 & 16.3 nm in water assisted SnO2 and 0.00495 & 35.6 nm for EG assisted SnO2. Study of surface morphology of the samples was carried out using SEM. It has been seen that the solvents which are used in synthesis can also alter the optical properties of the materials. The optical band gap of the water based SnO2 and EG based SnO2 are found to be 3.92eV and 3.86eV respectively.
Preparation and characterization of polyol assisted ultrafine Cu-Ni-Mg-Ca mixed ferrite via co-precipitation method

NASA Astrophysics Data System (ADS)

Boobalan, T.; Pavithradevi, S.; Suriyanarayanan, N.; Manivel Raja, M.; Ranjith Kumar, E.

2017-04-01

Nanocrystalline spinel ferrite of composition Cu0.2Ni0.2Mg0.2Ca0.4Fe2O4 is synthesized by wet hydroxyl co-precipitation method in ethylene glycol as chelating agent and sodium hydroxide as precipitator at pH 8. Ethylene glycol is utilized as the medium which serves as the dissolvable and in addition a complexing specialist. The synthesized particles are annealed at various temperatures. Thermogravimetric investigation affirms that at 280 °C ethylene glycol is dissipated totally and stable phase arrangement happens over 680 °C. FTIR spectra of as synthesized and annealed at 1050 °C recorded between 400 cm-1 and 4000 cm-1. Structural characterizations of all the samples are carried out by X-ray diffraction (XRD) technique. Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) affirm that the particles are spherical and cubic shape with the crystallite size of 12 nm to 32 nm. Magnetic measurements are performed utilizing vibrating sample magnetometer at room temperature.
Tailoring the structure of biphasic calcium phosphate via synthesis procedure

NASA Astrophysics Data System (ADS)

Mansour, S. F.; El-dek, S. I.; Ahmed, M. K.

2017-12-01

Nano calcium phosphate ceramics (CaPC) were synthesized using simple co-precipitation method at different preparation conditions. The selected Ca/P ratio with a variation of pH value lead to formation of dicalcium phosphate dihydrate (DCPD) at pH 5 and 6 while, hydroxyapatite (HAP) nano particles were formed at pH 9 and 12 at room temperature. The crystallite size was in the range of 15-55 nm depending on the obtained crystalline phase. The study displayed variation of decomposition depending on the annealing temperature. The significant note is the different transformation trend of each phase depending on the starting pH value. The HRTEM illustrated that the DCPD phase was formed as fibers with diameter around 4-6 nm, while HAP was formed in rod shape. The aspect ratio decreased from 6.6 at pH 9 to 4 at pH 12 which refer to the great influence of pH value on the morphology of calcium phosphates.
Thermal stability and electrochemical properties of PVP-protected Ru nanoparticles synthesized at room temperature

NASA Astrophysics Data System (ADS)

Kumar, Manish; Devi, Pooja; Shivling, V. D.

2017-08-01

Stable ruthenium nanoparticles (RuNPs) have been synthesized by the chemical reduction of ruthenium trichloride trihydrate (RuCl3 · 3H2O) using sodium borohydride (NaBH4) as a reductant and polyvinylpyrrolidone (PVP) as a protecting agent in the aqueous medium at room temperature. The nanoparticles thus prepared were characterized by their morphology and structural analysis from transmission electron microscopy (TEM), X-ray powder diffraction (XRD), UV-vis spectroscopy, Fourier transformation infrared and thermogravimetric analysis (TGA) techniques. The TEM image suggested a homogeneous distribution of PVP-protected RuNPs having a small average diameter of 2-4 nm with a chain-like network structure. The XRD pattern also confirmed that a crystallite size is around 2 nm of PVP-protected RuNPs having a single broad peak. The thermal stability studied using TGA, indicated good stability and the electrochemical properties of these nanoparticles revealed that saturation current increases for PVP-protected RuNPs/GC.
Investigation of structural, morphological and opto-electronic properties of CdS quantum dot thin film

NASA Astrophysics Data System (ADS)

Ibrahim Mohammed S., M.; Gubari, Ghamdan M. M.; Huse, Nanasaheb P.; Dive, Avinash S.; Sharma, Ramphal

2018-05-01

We have successfully deposited CdS quantum dot thin film on the glass substrate by simple and economic chemical bath deposition method at ˜50 ˚C. The X-ray diffraction study confirms the formation of CdS when compared with standard JCPDS data with average crystallite size ˜3 nm. The morphology of the film was studied by FE-SEM, which suggests the homogeneous and uniform deposition of the CdS material over the entire glass substrate with a porous structure. From UV absorption spectra we observed that the sample exhibited a band edge near ˜400 nm with a slight deviation with the presence of excitonic peak for the sample. The presence of excitonic peak may be attributed to the formation of quantum dots. The calculated band gap energy of CdS quantum dot thin film was found to be ˜3.136 eV. The thin film further characterized to study electrical parameters and the sample show a drastic increase in current after light illumination.
The preparation of BP single crystals by high pressure flux method

NASA Technical Reports Server (NTRS)

Kumashiro, Y.; Misawa, S.; Gonda, S.

1984-01-01

Single crystals of BP, a III-V compound semiconductor, were obtained by the high pressure flux method. Cu3P and Ni12P5 powders were used as the flux, and mixed with BP powder. Two kinds of mixtures were prepared: (1) 1.8g (BP) + 35 G (Cu3P) and (2) 1.7 g (BP) + 25 g (Ni12P5). They were compressed into pellets, heated at 1300 C for 24 h in an induction furnace under a pressure of 1 MPa using Ar-P2 gas, and slowly cooled to room temperature. In case (1), BP single crystals grew along the (III) plane, and in case (2) they grew as an aggregate of crystallites. The cathodoluminescence spectra of the synthetic BP crystals showed peaks near 680 nm (1.82 eV) for case (1), and 500 nm (2.47 eV) for case (2). By using the high pressure flux method conventional sized crystals were obtained in a relatively short time.
Nano-sized ZnO powders prepared by co-precipitation method with various pH

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

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro,

2016-04-19

In this work, nano-sized ZnO powders have been synthesized by the co-precipitation method with Zn(CH3COOH)2.2H2O, HCl, and NH3.H2O as raw materials in various pH ranging from 8 to 10. The purity, microstructure, chemical group analysis, morphology of the prepared ZnO powders were studied by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), energy dispersive X-ray spectrometry (EDX), and scanning electron microscope (SEM), respectively. Rietveld refinement of XRD data showed that ZnO crystallizes in the wurtzite structure with high purity. The obtained powders were nano-sized particles with the average crystallite size about 17.9 ± 2.1 nm synthesized with pH of 9.5, atmore » 85°C, and stirring time of 6 h. The SEM results have visualied the morphology of ZnO nanoparticles with spherical-like shape. The effect of processing conditions on morphology of ZnO was also discussed.« less
Anomalous behavior of B{sub 1g} mode in highly transparent anatase nano-crystalline Nb-doped Titanium Dioxide (NTO) thin films

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

Gautam, Subodh K., E-mail: subodhkgtm@gmail.com, E-mail: fouran@gmail.com; Ojha, S.; Singh, Fouran, E-mail: subodhkgtm@gmail.com, E-mail: fouran@gmail.com

2015-12-15

The effect of Niobium doping and size of crystallites on highly transparent nano-crystalline Niobium doped Titanium Dioxide (NTO) thin films with stable anatase phase are reported. The Nb doping concentration is varied within the solubility limit in TiO{sub 2} lattice. Films were annealed in controlled environment for improving the crystallinity and size of crystallites. Elemental and thickness analysis were carried out using Rutherford backscattering spectrometry and cross sectional field emission scanning electron microscopy. Structural characteristics reveal a substitutional incorporation of Nb{sup +5} in the TiO{sub 2} lattice which inhibits the anatase crystallites growth with increasing the doping percentage. The micro-Ramanmore » (MR) spectra of films with small size crystallites shows stiffening of about 4 cm{sup −1} for the E{sub g(1)} mode and is ascribed to phonon confinement and non-stoichiometry. In contrast, B{sub 1g} mode exhibits a large anomalous softening of 20 cm{sup −1} with asymmetrical broadening; which was not reported for the case of pure TiO{sub 2} crystallites. This anomalous behaviour is explained by contraction of the apical Ti-O bonds at the surface upon substitutional Nb{sup 5+} doping induced reduction of Ti{sup 4+} ions also known as hetero-coordination effect. The proposed hypotheses is manifested through studying the electronic structure and phonon dynamics by performing the near edge x-ray absorption fine structure (NEXAFS) and temperature dependent MR down to liquid nitrogen temperature on pure and 2.5 at.% doped NTO films, respectively.« less
Protein-free formation of bone-like apatite: New insights into the key role of carbonation

PubMed Central

Deymier, Alix C.; Nair, Arun K.; Depalle, Baptiste; Qin, Zhao; Arcot, Kashyap; Drouet, Christophe; Yoder, Claude H.; Buehler, Markus J.; Thomopoulos, Stavros; Genin, Guy M.; Pasteris, Jill D.

2017-01-01

The nanometer-sized plate-like morphology of bone mineral is necessary for proper bone mechanics and physiology. However, mechanisms regulating the morphology of these mineral nanocrystals remain unclear. The dominant hypothesis attributes the size and shape regulation to organic-mineral interactions. Here, we present data supporting the hypothesis that physicochemical effects of carbonate integration within the apatite lattice control the morphology, size, and mechanics of bioapatite mineral crystals. Carbonated apatites synthesized in the absence of organic molecules presented plate-like morphologies and nanoscale crystallite dimensions. Experimentally-determined crystallite size, lattice spacing, solubility and atomic order were modified by carbonate concentration. Molecular dynamics (MD) simulations and density functional theory (DFT) calculations predicted changes in surface energy and elastic moduli with carbonate concentration. Combining these results with a scaling law predicted the experimentally observed scaling of size and energetics with carbonate concentration. The experiments and models describe a clear mechanism by which crystal dimensions are controlled by carbonate substitution. Furthermore, the results demonstrate that carbonate substitution is sufficient to drive the formation of bone-like crystallites. This new understanding points to pathways for biomimetic synthesis of novel, nanostructured biomaterials. PMID:28279923
Study of energy vs misorientation for grain boundaries in gold by crystallite rotation method - I. (001) twist boundaries

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

Chan, S-W; Balluffi, R.W.

1985-06-01

Small gold crystallites ( about50-80 nm dia) were welded to thin film (001) single crystal gol substrates at a series of predetermined (001) twist angles in the range 0.45/sup 0/. A pure (001) twist boundary therefore existed in each welded neck region which could be observed directly by transmission electron microscopy at normal incidence. Upon annealing, the crystallites rotated around (001) when the boundary energy varied with theta. The crystallites rotated into three misorientations corresponding to the special ..sigma..1 and ..sigma..5 misorientations and a symmetry related misorientation at theta = 45/sup 0/. These results indicate the existence of grain boundarymore » dislocation (GBD) related cusps on the boundary energy vs theta curve a ..sigma..1 and ..sigma..5. The rotations occurred conservatively by the motion of screw GBDs which could be observed directly by the transmission microscopy in certain regimes of theta. The results are relevant to recent calculations of the energies of (001) twist boundaries and the applicability of the GBD/structural unit model for grain boundaries.« less
Dip coated TiO2 nanostructured thin film: synthesis and application

NASA Astrophysics Data System (ADS)

Vanaraja, Manoj; Muthukrishnan, Karthika; Boomadevi, Shanmugam; Karn, Rakesh Kumar; Singh, Vijay; Singh, Pramod K.; Pandiyan, Krishnamoorthy

2016-02-01

TiO2 thin film was fabricated by dip coating method using titanium IV chloride as precursor and sodium carboxymethyl cellulose as thickening as well as capping agent. Structural and morphological features of TiO2 thin film were characterized by X-ray diffractometer and field emission scanning electron microscope, respectively. Crystallinity of the film was confirmed with high-intensity peak at (101) plane, and its average crystallite size was found to be 28 nm. The ethanol-sensing properties of TiO2 thin film was studied by the chemiresistive method. Furthermore, various gases were tested in order to verify the selectivity of the sensor. Among the several gases, the fabricated TiO2 sensor showed very high selectivity towards ethanol at room temperature.
Influence of Mn doping on structural, dielectric and optical properties of neodymium orthoferrite

NASA Astrophysics Data System (ADS)

Somvanshi, Anand; Manzoor, Samiya; Husain, Shahid

2018-05-01

We report the study of structural, dielectric and optical properties of nanocrystalline samples of NdFe1-xMnxO3 (x=0, 0.1 and 0.2) synthesized using solid state reaction route. X-ray diffraction (XRD) patterns are recorded to confirm phase purity. These samples conform in orthorhombic crystal symmetry with Pbnm space group. The lattice parameters are determined using Rietveld refinement. The crystallite size is calculated using Scherrer formula and that is found to lie in the range of 40-50 nm. The dielectric constant (ɛ') decreases with the increase in frequency as well as Mn doping concentration. Energy bandgap (Eg) as determined using UV-Vis. absorption spectra, is found to decrease with the increase in Mn doping.
SrFe 12O 19 prepared by the proteic sol-gel process

NASA Astrophysics Data System (ADS)

Brito, P. C. A.; Gomes, R. F.; Duque, J. G. S.; Macêdo, M. A.

2006-10-01

Powders of strontium hexaferrite (SrFe 12O 19) were prepared by the proteic sol-gel process using coconut water as a precursor. X-ray diffraction (XRD) measurement showed the formation of SrFe 12O 19 with a small amount of the hematite for the sample calcined at 1000 °C with Fe/Sr=12. Rietveld refinement disclosed that this sample had 87.56% of the SrFe 12O 19 and 12.44% of Fe 2O 3 and the values for Rp, Rwp and χ2 were 4.28%, 5.93% and 1.71, respectively. The magnetic properties were Ms=64 emu/g, Mr/ Ms=0.55 and Hc=1.4 kOe for a crystallite size of 57 nm.
Group 12 dithiocarbamate complexes: Synthesis, spectral studies and their use as precursors for metal sulfides nanoparticles and nanocomposites

NASA Astrophysics Data System (ADS)

Ajibade, Peter A.; Ejelonu, Benjamin C.

2013-09-01

Zn(II), Cd(II) and Hg(II) dithiocarbamate complexes have been synthesized and characterized by elemental analysis, thermogravimetric analysis, UV-Vis, FTIR, 1H- and 13C NMR spectroscopy. The complexes were thermolysed at 180 °C and used as single molecule precursors for the synthesis of HDA capped ZnS, CdS and HgS nanoparticles and polymethylmethacrylate (PMMA) nanocomposites. The optical and structural properties of the nanoparticles and nanocomposites were studied by UV-Vis, PL, XRD and SEM. The crystallites sizes of the nanoparticles varied between 3.03 and 23.45 nm. SEM and EDX analyses of the nanocomposites confirmed the presence of the nanoparticles in the polymer matrix.

On the Nature of Disorder in Solid 4He

NASA Astrophysics Data System (ADS)

Krainyukova, N. V.

2010-02-01

We apply a modified Debye approach to calculate the Gibbs free energy for different structural phases and crystallite sizes in 4He. Atoms are assumed to interact via the Aziz potential. We have found that some intermediate (between hcp and bcc) phase predicted previously is more favorable than hcp at low temperatures and for small sizes. We show that it can exist in a wide pressure range up to 60 bar in 4He for crystallite sizes about 3,000 atoms. For larger sizes (10,000 atoms or more) this phase becomes unfavorable. In multidomain structures the intermediate phase competes with hcp and metastable fcc that can be a reason for disorder in solid 4He.
Strain and grain size of TiO2 nanoparticles from TEM, Raman spectroscopy and XRD: The revisiting of the Williamson-Hall plot method

NASA Astrophysics Data System (ADS)

Kibasomba, Pierre M.; Dhlamini, Simon; Maaza, Malik; Liu, Chuan-Pu; Rashad, Mohamed M.; Rayan, Diaa A.; Mwakikunga, Bonex W.

2018-06-01

The Williamson-Hall (W-H) equation, which has been used to obtain relative crystallite sizes and strains between samples since 1962, is revisited. A modified W-H equation is derived which takes into account the Scherrer equation, first published in 1918, (which traditionally gives more absolute crystallite size prediction) and strain prediction from Raman spectra. It is found that W-H crystallite sizes are on average 2.11 ± 0.01 times smaller than the sizes from Scherrer equation. Furthermore the strain from the W-H plots when compared to strain obtained from Raman spectral red-shifts yield factors whose values depend on the phases in the materials - whether anatase, rutile or brookite. Two main phases are identified in the annealing temperatures (350 °C-700 °C) chosen herein - anatase and brookite. A transition temperature of 550 °C has been found for nano-TiO2 to irreversibly transform from brookite to anatase by plotting the Raman peak shifts against the annealing temperatures. The W-H underestimation on the strain in the brookite phase gives W-H/Raman factor of 3.10 ± 0.05 whereas for the anatase phase, one gets 2.46 ± 0.03. The new βtot2cos2θ-sinθ plot and when fitted with a polynomial yield less strain but much better matching with experimental TEM crystallite sizes and the agglomerates than both the traditional Williamson-Hall and the Scherrer methods. There is greater improvement in the model when linearized - that is the βtotcos2θ-sinθ plot rather than the βtot2cos2θ-sinθ plot.
Optimization of reaction parameters in hydrothermal synthesis: a strategy towards the formation of CuS hexagonal plates

PubMed Central

2013-01-01

Background For decades, copper sulphide has been renowned as the superior optical and semiconductor materials. Its potential applications can be ranged from solar cells, lithium-ion batteries, sensors, and catalyst systems. The synthesis methodologies of copper sulphide with different controlled morphology have been widely explored in the literature. Nevertheless, the understanding on the formation chemistry of CuS is still limited. The ultimate approach undertaking in this article is to investigate the formation of CuS hexagonal plates via the optimization of reaction parameters in hydrothermal reaction between copper (II) nitrate and sodium thiosulphate without appending any assistant agent. Results Covellite (CuS) hexagonal plates were formed at copper ion: thiosulphate ion (Cu2+:S2O32−) mole ratio of 1:2 under hydrothermal treatment of 155°C for 12 hours. For synthesis conducted at reaction temperature lower than 155°C, copper sulphate (CuSO4), krohnite (NaCu2(SO4)(H2O)2] and cyclooctasulphur (S8) were present as main impurities with covellite (CuS). When Cu2+:S2O32− mole ratio was varied to 1: 1 and 1: 1.5, phase pure plate-like natrochalcite [NaCu2(SO4)(H2O)] and digenite (Cu9S5) were produced respectively. Meanwhile, mixed phases of covellite (CuS) and cyclooctasulphur (S8) were both identified when Cu2+:S2O32− mole ratio was varied to 1: 2.5, 1: 3 and 1: 5 as well as when reaction time was shortened to 1 hour. Conclusions CuS hexagonal plates with a mean edge length of 1 μm, thickness of 100 nm and average crystallite size of approximately (45 ± 2) nm (Scherrer estimation) were successfully synthesized via assisting agent- free hydrothermal method. Under a suitable Cu2+:S2O32− mole ratio, we evidenced that the formation of covellite (CuS) is feasible regardless of the reaction temperature applied. However, a series of impurities were attested with CuS if reaction temperature was not elevated high enough for the additional crystallite phase decomposition. It was also identified that Cu2+:S2O32− mole ratio plays a vital role in controlling the amount of cyclooctasulphur (S8) in the final powder obtained. Finally, reaction time was recognized as an important parameter in impurity decomposition as well as increasing the crystallite size and crystallinity of the CuS hexagonal plates formed. PMID:23575312
Microstructural evolution and thermal stability of Fe-Zr metastable alloys developed by mechanical alloying followed by annealing

NASA Astrophysics Data System (ADS)

Sooraj, S.; Muthaiah, V. M. Suntharavel; Kang, P. C.; Koch, Carl C.; Mula, Suhrit

2016-09-01

The effect of Zr (up to 1 at.%) addition on the formation of Fe-Zr metastable alloys and their thermal stability were investigated for their possible nuclear applications. Fe-xZr (x = 0.25, 0.5, 1%) alloys were synthesised by mechanical alloying under a high-purity argon atmosphere using stainless steel grinding media in a SPEX 8000M high energy mill. The milling was conducted for 20 h with a ball-to-powder weight ratio of 10:1. The formation of metastable solid solutions after milling was confirmed from the change in the Gibbs free energy analysis as per Miedema's model. The microstructural characterisation was carried out by analysis of X-ray diffraction, atomic force microscopy and transmission electron microscopy. The effect of Zr on the thermal stability of Fe-Zr alloys was investigated by extensive annealing experiments followed by microstructural analysis and microhardness measurements. The stabilisation was found to occur at 800 °C and thereafter, no significant change in the crystallite size was observed for the samples annealed between 800 and 1200 °C. The supersaturated solid solution, especially 1% Zr alloy, found to be highly stable up to 800 °C and the microhardness value of the same measured to be as high as 8.8 GPa corresponding to a crystallite size of 57 nm. The stabilisation effect has been discussed in the light of both the thermodynamic and kinetic mechanisms and the grain size stabilisation is attributed to the grain boundary segregation of Zr atoms and/or Zener pinning by nanoscale precipitation of the Fe2Zr phase.
Preparation of highly ordered mesoporous Al2O3/TiO2 and its application in dye-sensitized solar cells.

PubMed

Kim, Jae-Yup; Kang, Soon Hyung; Kim, Hyun Sik; Sung, Yung-Eun

2010-02-16

Highly ordered mesoporous Al(2)O(3)/TiO(2) was prepared by sol-gel reaction and evaporation-induced self-assembly (EISA) for use in dye-sensitized solar cells. The prepared materials had two-dimensional, hexagonal pore structures with anatase crystalline phases. The average pore size of mesoporous Al(2)O(3)/TiO(2) remained uniform and in the range of 6.33-6.58 nm while the Brunauer-Emmett-Teller (BET) surface area varied from 181 to 212 m(2)/g with increasing the content of Al(2)O(3). The incorporation of Al content retarded crystallite growth, thereby decreasing crystallite size while simultaneously improving the uniformity of pore size and volume. The thin Al(2)O(3) layer was located mostly on the mesopore surface, as confirmed by X-ray photoelectron spectroscopy (XPS). The Al(2)O(3) coating on the mesoporous TiO(2) film contributes to the essential energy barrier which blocks the charge recombination process in dye-sensitized solar cells. Mesoporous Al(2)O(3)/TiO(2) (1 mol % Al(2)O(3)) exhibited enhanced power conversion efficiency (V(oc) = 0.74 V, J(sc) = 15.31 mA/cm(2), fill factor = 57%, efficiency = 6.50%) compared to pure mesoporous TiO(2) (V(oc) = 0.72 V, J(sc) = 16.03 mA/cm(2), fill factor = 51%, efficiency = 5.88%). Therefore, the power conversion efficiency was improved by approximately 10.5%. In particular, the increase in V(oc) and fill factor resulted from the inhibition of charge recombination and the improvement of pore structure.
Role of Cu in engineering the optical properties of SnO2 nanostructures: Structural, morphological and spectroscopic studies

NASA Astrophysics Data System (ADS)

Kumar, Virender; Singh, Kulwinder; Jain, Megha; Manju; Kumar, Akshay; Sharma, Jeewan; Vij, Ankush; Thakur, Anup

2018-06-01

We have carried out a systematic study to investigate the effect of Cu doping on the optical properties of SnO2 nanostructures synthesized by chemical route. Synthesized nanostructures were characterized using X-ray diffraction (XRD), Field emission scanning electron microscopy (FE-SEM), High resolution transmission electron microscopy (HR-TEM), Energy dispersive X-ray spectroscopy, Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy, UV-visible and Photoluminescence (PL) spectroscopy. The Rietveld refinement analysis of XRD patterns of Cu-doped SnO2 samples confirmed the formation of single phase tetragonal rutile structure, however some localized distortion was observed for 5 mol% Cu-doped SnO2. Crystallite size was found to decrease with increase in dopant concentration. FE-SEM images indicated change in morphology of samples with doping. HR-TEM images revealed that synthesized nanostructures were nearly spherical and average crystallite size was in the range 12-21 nm. Structural defects, crystallinity and size effects on doping were investigated by Raman spectroscopy and results were complemented by FTIR spectroscopy. Optical band gap of samples was estimated from reflectance spectra. We have shown that band gap of SnO2 can be engineered from 3.62 to 3.82 eV by Cu doping. PL emission intensity increased as the doping concentration increased, which can be attributed to the development of defect states in the forbidden transition region of band gap of SnO2 with doping. We have also proposed a band model owing to defect states in SnO2 to explain the observed PL in Cu doped SnO2 nanostructures.
Enhanced photo-response of porous silicon photo-detectors by embeddingTitanium-dioxide nano-particles

NASA Astrophysics Data System (ADS)

Ali, Hiba M.; Makki, Sameer A.; Abd, Ahmed N.

2018-05-01

Porous silicon (n-PS) films can be prepared by photoelectochemical etching (PECE) Silicon chips n - types with 15 (mA / cm2), in 15 minutes etching time on the fabrication nano-sized pore arrangement. By using X-ray diffraction measurement and atomic power microscopy characteristics (AFM), PS was investigated. It was also evaluated the crystallites size from (XRD) for the PS nanoscale. The atomic force microscopy confirmed the nano-metric size chemical fictionalization through the electrochemical etching that was shown on the PS surface chemical composition. The atomic power microscopy checks showed the roughness of the silicon surface. It is also notified (TiO2) preparation nano-particles that were prepared by pulse laser eradication in ethanol (PLAL) technique through irradiation with a Nd:YAG laser pulses TiO2 target that is sunk in methanol using 400 mJ of laser energy. It has been studied the structural, optical and morphological of TiO2NPs. It has been detected that through XRD measurement, (TiO2) NPs have been Tetragonal crystal structure. While with AFM measurements, it has been realized that the synthesized TiO2 particles are spherical with an average particle size in the (82 nm) range. It has been determined that the energy band gap of TiO2 NPs from optical properties and set to be in (5eV) range.The transmittance and reflectance spectra have determined the TiO2 NPs optical constants. It was reported the effectiveness of TiO2 NPs expansion on the PS Photodetector properties which exposes the benefits in (Al/PS/Si/Al). The built-in tension values depend on the etching time current density and laser flounce. Al/TiO2/PS/Si/Al photo-detector heterojunction have two response peaks that are situated at 350 nm and (700 -800nm) with max sensitivity ≈ 0.7 A/W. The maximum given detectivity is 9.38at ≈ 780 nm wavelength.
Synthesis characterization and luminescence studies of gamma irradiated nanocrystalline yttrium oxide.

PubMed

Shivaramu, N J; Lakshminarasappa, B N; Nagabhushana, K R; Singh, Fouran

2016-02-05

Nanocrystalline Y2O3 is synthesized by solution combustion technique using urea and glycine as fuels. X-ray diffraction (XRD) pattern of as prepared sample shows amorphous nature while annealed samples show cubic nature. The average crystallite size is calculated using Scherrer's formula and is found to be in the range 14-30 nm for samples synthesized using urea and 15-20 nm for samples synthesized using glycine respectively. Field emission scanning electron microscopy (FE-SEM) image of 1173 K annealed Y2O3 samples show well separated spherical shape particles and the average particle size is found to be in the range 28-35 nm. Fourier transformed infrared (FTIR) and Raman spectroscopy reveals a stretching of Y-O bond. Electron spin resonance (ESR) shows V(-) center, O2(-) and Y(2+) defects. A broad photoluminescence (PL) emission with peak at ~386nm is observed when the sample is excited with 252 nm. Thermoluminescence (TL) properties of γ-irradiated Y2O3 nanopowder are studied at a heating rate of 5 K s(-1). The samples prepared by using urea show a prominent and well resolved peak at ~383 K and a weak one at ~570 K. It is also found that TL glow peak intensity (I(m1)) at ~383 K increases with increase in γ-dose up to ~6.0 kGy and then decreases with increase in dose. However, glycine used Y2O3 shows a prominent TL glow with peaks at 396 K and 590 K. Among the fuels, urea used Y2O3 shows simple and well resolved TL glows. This might be due to fuel and hence particle size effect. The kinetic parameters are calculated by Chen's glow curve peak shape method and results are discussed in detail. Copyright © 2015. Published by Elsevier B.V.
Comparison of 20 nm silver nanoparticles synthesized with and without a gold core. Structure, dissolution in cell culture media, and biological impact on macrophages

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

Munusamy, Prabhakaran; Wang, Chongmin; Engelhard, Mark H.

Widespread use of silver nanoparticles raises questions of environmental impact and toxicity. Both silver particles and silver ions formed by particle dissolution may impact biological systems. Therefore it is important to understand the characteristics of silver nanoparticles and their stability in relevant media. The synthesis route can impact physical and chemical characteristics of the particles and we report the characterization and solution stability of three types of silver nanoparticles (20 nm particles with and without gold cores and 110 nm particles with gold cores) in cell culture media with serum proteins: FBS10%/RPMI. These nanoparticles were synthesized in aqueous solution andmore » characterized using both in situ and ex situ analysis methods. Dissolution studies were carried at particle concentrations from 1 µg/ml to 50 µg/ml. Particles with gold cores had smaller crystallite size and higher apparent solubility than pure silver particles. A dissolution model was found to describe the time variation of particle size and amount of dissolved silver for particle loadings above 9 µg/ml. An effective solubility product obtained from fitting the data was higher for the 20 nm gold core particles in comparison to the pure silver or 110 nm particles. Dissolution of the nanoparticles was enhanced by presence of serum proteins contained in fetal bovine serum. In addition, the protocol of the dispersion in the medium was found to influence particle agglomeration and dissolution. Results show that particle structure can impact the concentration of dissolved silver and the dose to which cells would be exposed during in vitro studies.« less
Comparison of 20 nm silver nanoparticles synthesized with and without a gold core. Structure, dissolution in cell culture media, and biological impact on macrophages

DOE PAGES

Munusamy, Prabhakaran; Wang, Chongmin; Engelhard, Mark H.; ...

2015-07-15

Widespread use of silver nanoparticles raises questions of environmental impact and toxicity. Both silver particles and silver ions formed by particle dissolution may impact biological systems. Therefore it is important to understand the characteristics of silver nanoparticles and their stability in relevant media. The synthesis route can impact physical and chemical characteristics of the particles and we report the characterization and solution stability of three types of silver nanoparticles (20 nm particles with and without gold cores and 110 nm particles with gold cores) in cell culture media with serum proteins: FBS10%/RPMI. These nanoparticles were synthesized in aqueous solution andmore » characterized using both in situ and ex situ analysis methods. Dissolution studies were carried at particle concentrations from 1 µg/ml to 50 µg/ml. Particles with gold cores had smaller crystallite size and higher apparent solubility than pure silver particles. A dissolution model was found to describe the time variation of particle size and amount of dissolved silver for particle loadings above 9 µg/ml. An effective solubility product obtained from fitting the data was higher for the 20 nm gold core particles in comparison to the pure silver or 110 nm particles. Dissolution of the nanoparticles was enhanced by presence of serum proteins contained in fetal bovine serum. In addition, the protocol of the dispersion in the medium was found to influence particle agglomeration and dissolution. Results show that particle structure can impact the concentration of dissolved silver and the dose to which cells would be exposed during in vitro studies.« less
Preparation and Characterization of Chitosan-coated Fe3O4 Nanoparticles using Ex-Situ Co-Precipitation Method and Tripolyphosphate/Sulphate as Dual Crosslinkers

NASA Astrophysics Data System (ADS)

Wulandari, Ika O.; Mardila, Vita T.; Santjojo, D. J. Djoko H.; Sabarudin, Akhmad

2018-01-01

The unique properties of nanomaterial provide great opportunities to develop in several fields. Several types of nanoparticles have been proven beneficial for biomedical and therapeutic agent development. Particularly for clinical use, nanoparticles must be biocompatible and non-toxic. Iron oxide nanoparticles consist of either magnetite (Fe3O4) or maghemite (γ-Fe2O3) was eligible to use for in vivo application including targeting drug delivery. Due to their distinct properties, these nanoparticles could be directed to the specific target under external magnetic field. However, nanoparticles have a tendency to form agglomeration. Therefore, surface modification was required to reduce the agglomeration. In this study, nanoparticles of Fe3O4 were produced and coated by biomaterial (chitosan) using ex-situ co-precipitation method. Nanoparticles of Fe3O4 were synthesized by adding ammonia water into iron ferric and ferrous solution. Synthesis process of Fe3O4 was conducted prior to adding chitosan. Chitosan was then cross-linked by a combination of tripolyphosphate/sulphate. The different composition ratio and crosslinking time provide the different physical and magnetic characteristics of nanoparticles. Particle and crystallite size was determined by using Scanning Electron Microscopy (SEM) and X-Ray Diffraction (XRD) respectively, whereas magnetic characteristic was determined by Electron Spin Resonance (ESR). The results showed that the ratio enhancement between chitosan: Fe3O4 increase the particle size, while decreased the crystallite size. Morphology and particle size were influenced by the ratio of crosslinkers. It was found that the higher tripolyphosphate content was contributed to the small size and more spherical morphology. In addition, the influence of crosslinking time toward crystallite size was determined by altering stirring time. The longer duration of crosslinking time, provide the larger crystallite size of chitosan-Fe3O4. There was an interesting correlation between particle size and amount of Fe3O4 phase with ESR curve.
Investigation of temperature dependent magnetic hyperthermia in Fe3O4 ferrofluids

NASA Astrophysics Data System (ADS)

Nemala, Humeshkar Bhaskar

Magnetic nanoparticles (MNPs) of Fe3O4 and gamma-Fe2O3 have been exploited in the biomedical fields for imaging, targeted drug delivery and magnetic hyperthermia. Magnetic hyperthermia (MHT), the production of heat using ferrofluids, colloidal suspensions of MNPs, in an external AC magnetic field (amplitude, 100-500 Oe and frequency 50 kHz -1MHz), has been explored by many researchers, both in vitro and in vivo, as an alternative viable option to treat cancer. The heat energy generated by Neel and Brownian relaxation processes of the internal magnetic spins could be used to elevate local tissue temperature to about 46 ˚C to arrest cancerous growth. MHT, due to its local nature of heating, when combined with other forms of treatment such as chemotherapy and/or radiation therapy, it could become an effective therapy for cancer treatment. The efficiency of heat production in MHT is quantified by specific absorption rate (SAR), defined as the power output per gram of the MNPs used. In this thesis, ferrofluids consisting of Fe3O4 MNPs of three different sizes (˜ 10 - 13 nm) coated with two different biocompatible surfactants, dextran and polyethylene glycol (PEG), have been investigated. The structural and magnetic characterization of the MNPs were done using XRD, TEM, and DC magnetization measurements. While XRD revealed the crystallite size, TEM provided the information about morphology and physical size distribution of the MNPs. Magnetic measurements of M-vs-H curves for ferrofluids provided information about the saturation magnetization (Ms) and magnetic core size distribution of MNPs. Using MHT measurements, the SAR has been studied as a function of temperature, taking into account the heat loss due to non-adiabatic nature of the experimental set-up. The observed SAR values have been interpreted using the theoretical framework of linear response theory (LRT). We found the SAR values depend on particle size distribution of MNPs, Ms (65-80 emu/g) and the magnetic anisotropy energy density (K: 12-20 KJ/m3), as well as the amplitude and frequency of the applied AC field (amplitude, 150-250 Oe and frequency, 180-380 kHz). In general, Ms and magnetic core diameter of MNPs increased with the increase in particle size. However, our detailed analysis of MHT data show that although SAR increased with the particle size, the polydispersity of the particles as well as the magnetic anisotropy energy density significantly affected the SAR values. Dextran and PEG coatings essentially yielded similar SAR values ~ 100 W/g using ferrofluids of Fe3O4 MNPs with an average crystallite size of 11.6 +/- 2.1 nm, in AC field of 245 Oe and 375 KHz.
Electron-beam irradiation induced transformation of Cu2(OH)3NO3 nanoflakes into nanocrystalline CuO

NASA Astrophysics Data System (ADS)

Padhi, S. K.; Gottapu, S. N.; Krishna, M. Ghanashyam

2016-05-01

The transmission electron microscope electron-beam (TEM e-beam) as a material modification tool has been demonstrated. The material modification is realised in the high-resolution TEM mode (largest condenser aperture, 150 μm, and 200 nm spot size) at a 200 keV beam energy. The Cu2(OH)3NO3 (CHN) nanoflakes used in this study were microwave solution processed that were layered single crystals and radiation sensitive. The single domain CHN flakes disintegrate into a large number of individual CuO crystallites within a 90 s span of time. The sequential bright-field, dark-field, and selected area electron diffraction modes were employed to record the evolved morphology, microstructural changes, and structural transformation that validate CHN modification. High-resolution transmission electron microscopy imaging of e-beam irradiated regions unambiguously supports the growth of CuO nanoparticles (11.8(3.2) nm in diameter). This study demonstrates e-beam irradiation induced CHN depletion, subsequent nucleation and growth of nanocrystalline CuO regions well embedded in the parent burnt porous matrix which can be useful for miniaturized sensing applications. NaBH4 induced room temperature reduction of CHN to elemental Cu and its printability on paper was also demonstrated.The transmission electron microscope electron-beam (TEM e-beam) as a material modification tool has been demonstrated. The material modification is realised in the high-resolution TEM mode (largest condenser aperture, 150 μm, and 200 nm spot size) at a 200 keV beam energy. The Cu2(OH)3NO3 (CHN) nanoflakes used in this study were microwave solution processed that were layered single crystals and radiation sensitive. The single domain CHN flakes disintegrate into a large number of individual CuO crystallites within a 90 s span of time. The sequential bright-field, dark-field, and selected area electron diffraction modes were employed to record the evolved morphology, microstructural changes, and structural transformation that validate CHN modification. High-resolution transmission electron microscopy imaging of e-beam irradiated regions unambiguously supports the growth of CuO nanoparticles (11.8(3.2) nm in diameter). This study demonstrates e-beam irradiation induced CHN depletion, subsequent nucleation and growth of nanocrystalline CuO regions well embedded in the parent burnt porous matrix which can be useful for miniaturized sensing applications. NaBH4 induced room temperature reduction of CHN to elemental Cu and its printability on paper was also demonstrated. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr02572b
Novel and facile microwave-assisted synthesis of Mo-doped hydroxyapatite nanorods: Characterization, gamma absorption coefficient, and bioactivity.

PubMed

Abutalib, M M; Yahia, I S

2017-09-01

In the current work, the authors report the microwave-assisted synthesis Molybdenum-doped (from 0.05 to 5wt%) hydroxyapatite (HAp) for the first time. The morphology of Mo-doped HAp is nanorods of diameter in the range of 25-70nm and length in the range of 25nm to 200nm. The good crystalline nature was confirmed from X-ray diffraction patterns and also lattice parameters, grain size, strain and dislocation density were determined. The crystallite size was found to be in the range 16 to 30nm and crystallinity was found to be enhanced from 0.5 to 0.7 with doping. The field emission SEM micrographs show that the morphology of the synthesized nanostructures of pure and Mo-doped HAp are nanorods of few nanometers. The vibrational modes were identified using the FT-Raman and FT-IR spectroscopy. The dielectric properties were studied and the AC electrical conductivity was found to be increased with increasing the concentration of Mo ions doping in HAp. Moreover, antimicrobial studies were also carried out to understand the anti-bacterial and anti-fungi properties. The results suggest that it may be a good bio-ceramics material for bio-medical applications. Mo-doped HAp was subjected to the gamma irradiation produced from Cs-137 (662keV) and its related parameters such as linear absorption coefficient, the half-value layer (HVL) and the tenth value layer TVL were calculated and analyzed. Copyright © 2017 Elsevier B.V. All rights reserved.
Development of Nanomaterials for Nuclear Energetics

NASA Astrophysics Data System (ADS)

Petrunin, V. F.

Structure and properties peculiarities of the nanocrystalline powders give the opportunity to design new and to develop a modernization of nuclear energy industry materials. It was shown experimentally, that addition of 5-10% uranium dioxide nanocrystalline powder to traditional coarse powder allows to decrease the sintering temperature or to increase the fuel tablets size of grain. Similar perspectives for the technology of neutron absorbing tablets of control-rod modernization are shown by nanopowder of dysprosium hafnate changing instead now using boron carbide. It is powders in nanocrystalline state get an opportunity to sinter them and to receive compact tablet with 8,2-8,4 g/cm2 density for automatic defence system of nuclear reactor. Resource of dysprosium hafnate ceramics can be 18-20 years instead 4-5 years for boron carbide. To step up the radiation-damage stability of fuel element jacket material was suggested to strengthen a heat-resistant ferrite-martensite steel by Y2O3 nanocrystalline powder addition. Nanopowder with size of particles 560 nm and crystallite size 9 nm was prepeared by chemical coprecipitation method. To make lighter the container for transport and provisional disposal of exposed fuel from nuclear reactor a new boron-aluminium alloy called as boral was developed. This composite armed with nanopowders of boron-containing materials and heavy metals oxides can replace succesburnt-up corrosion-resistant steels.
Spectral features and antibacterial properties of Cu-doped ZnO nanoparticles prepared by sol-gel method

NASA Astrophysics Data System (ADS)

Alireza, Samavati; A, F. Ismail; Hadi, Nur; Z, Othaman; M, K. Mustafa

2016-07-01

Zn1-x Cu x O (x = 0.00, 0.01, 0.03, and 0.05) nanoparticles are synthesized via the sol-gel technique using gelatin and nitrate precursors. The impact of copper concentration on the structural, optical, and antibacterial properties of these nanoparticles is demonstrated. Powder x-ray diffraction investigations have illustrated the organized Cu doping into ZnO nanoparticles up to Cu concentration of 5% (x = 0.05). However, the peak corresponding to CuO for x = 0.01 is not distinguishable. The images of field emission scanning electron microscopy demonstrate the existence of a nearly spherical shape with a size in the range of 30-52 nm. Doping Cu creates the Cu-O-Zn on the surface and results in a decrease in the crystallite size. Photoluminescence and absorption spectra display that doping Cu causes an increment in the energy band gap. The antibacterial activities of the nanoparticles are examined against Escherichia coli (Gram negative bacteria) cultures using optical density at 600 nm and a comparison of the size of inhibition zone diameter. It is found that both pure and doped ZnO nanoparticles indicate appropriate antibacterial activity which rises with Cu doping. Project supported by the Universiti Teknologi Malaysia (UTM) (Grant No. R. J1300000.7809.4F626). Dr. Samavati is thankful to RMC for postdoctoral grants.
Structural changes during milling of aluminum oxide powders

NASA Technical Reports Server (NTRS)

Ziepler, G.

1984-01-01

The mechanical activation of four fused corundum powders and a calcined Al2O3 powder was studied. The milled powders were characterized by their structural properties, crystallite size, and lattice distortions. Structural changes during milling, detected by X-ray line broadening analysis, gave information about the enhanced activity of the powders caused by the lattice distortions and by the decreasing crystallite size during milling. The structural changes during milling, under the same milling conditions, can be quite different for the same ceramic material, but with different characteristics in the as received state.
Blue light emitting Y2O3:Tm3 + nanophosphors with tunable morphology obtained by bio-surfactant assisted sonochemical route

NASA Astrophysics Data System (ADS)

Venkatachalaiah, K. N.; Nagabhushana, H.; Darshan, G. P.; Basavaraj, R. B.; Daruka Prasad, B.; Sharma, S. C.

2017-09-01

Modified sonochemical route was used to prepare Y2O3:Tm3+ (1-11 mol%) nanophosphor using Mimosa pudica (M.P.) leaves extract as bio-surfactant. The prepared samples were exhibited high crystalline nature with various morphologies. This was due to sonochemical experimental reaction took place between cavitation bubbles and nearby solution. The average crystallite sizes of the prepared samples were about 15 nm to 21 nm as obtained from PXRD and TEM analysis. The ultraviolet visible absorption spectra showed prominent bands with an energy gap varied from 5.73 eV to 5.84 eV. Photoluminescence (PL) emission spectra shows the prominent blue light emission peak at 456 nm attributed to 1D2 → 3F4 transitions of Tm3+ ions. Judd-Ofelt intensity parameters were estimated by using PL emission spectra. The photometric characteristics of the prepared compounds were very close to the blue color of NTSC standards. So the results were fruitful in making use of Y2O3:Tm3 + nanophosphor as an alternative material for effective blue component in WLED's.
Facile synthesis of cobalt ferrite nanotubes using bacterial nanocellulose as template.

PubMed

Menchaca-Nal, S; Londoño-Calderón, C L; Cerrutti, P; Foresti, M L; Pampillo, L; Bilovol, V; Candal, R; Martínez-García, R

2016-02-10

A facile method for the preparation of cobalt ferrite nanotubes by use of bacterial cellulose nanoribbons as a template is described. The proposed method relays on a simple coprecipitation operation, which is a technique extensively used for the synthesis of nanoparticles (either isolated or as aggregates) but not for the synthesis of nanotubes. The precursors employed in the synthesis are chlorides, and the procedure is carried out at low temperature (90 °C). By the method proposed a homogeneous distribution of cobalt ferrite nanotubes with an average diameter of 217 nm in the bacterial nanocellulose (BC) aerogel (3%) was obtained. The obtained nanotubes are formed by 26-102 nm cobalt ferrite clusters of cobalt ferrite nanoparticles with diameters in the 9-13 nm interval. The nanoparticles that form the nanotubes showed to have a certain crystalline disorder, which could be attributed in a greater extent to the small crystallite size, and, in a lesser extent, to microstrains existing in the crystalline lattice. The BC-templated-CoFe2O4 nanotubes exhibited magnetic behavior at room temperature. The magnetic properties showed to be influenced by a fraction of nanoparticles in superparamagnetic state. Copyright © 2015 Elsevier Ltd. All rights reserved.
Nanostructured CdO-NiO composite for multifunctional applications

NASA Astrophysics Data System (ADS)

Karthik, K.; Dhanuskodi, S.; Gobinath, C.; Prabukumar, S.; Sivaramakrishnan, S.

2018-01-01

In this study, CdO, NiO, and CdO-NiO nanocomposites (NCs) were synthesized and investigated by X-ray diffraction (XRD), scanning electron microscopy, and Fourier transform-infrared spectroscopy. XRD detected cubic structures with average crystallite sizes of 45 nm for CdO, 25 nm for NiO, and 30 nm for CdO-NiO. The band gap was estimated based on the ultraviolet-visible spectra. The near band edge emission was determined according to the luminescence spectrum. The antibacterial activities were tested against seven foodborne pathogens and the zones of inhibition with the Gram-negative bacterium Bacillus subtilis measured as 30 mm with CdO, 20 mm NiO, and 27 mm with CdO-NiO. The death of the bacterial cells was confirmed by confocal laser scanning microscope analysis. Cytotoxicity assays indicated the non-toxic effects of the NCs on normal healthy red blood cells. Furthermore, the in vitro cytotoxic effects of the CdO, NiO, and CdO-NiO NCs were examined using the human MCF-7 breast cancer cell line based on 3-[4,5-dimethylthiazol-2-yl]2,5-diphenyltetrazolium bromide assays with normal mouse embryonic fibroblasts (NH3T3) under identical conditions.

Exothermic low temperature sintering of Cu nanoparticles

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

Mittal, Jagjiwan; Lin, Kwang-Lung, E-mail: matkllin@mail.ncku.edu.tw

2015-11-15

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

NASA Astrophysics Data System (ADS)

Xu, Wei

Structure and properties of carbon black particles were investigated using atomic force microscopy, gas adsorption, Raman spectroscopy, and X-ray diffraction. Supplementary information was obtained using TEM and neutron scattering. The AFM imaging of carbon black aggregates provided qualitative visual information on their morphology, complementary to that obtained by 3-D modeling based on TEM images. Our studies showed that carbon black aggregates were relatively flat. The surface of all untreated carbon black particles was found to be rough and its fractal dimension was 2.2. Heating reduced the roughness and fractal dimension for all samples heat treated at above 1300 K to 2.0. Once the samples were heat treated rapid cooling did not affect the surface roughness. However, rapid cooling reduced crystallite sizes, and different Raman spectra were obtained for carbon blacks of various history of heat treatment. By analyzing the Raman spectra we determined the crystallite sizes and identified amorphous carbon. The concentration of amorphous carbon depends on hydrogen content. Once hydrogen was liberated at increased temperature, the concentration of amorphous carbon was reduced and crystallites started to grow. Properties of carbon blacks at high pressure were also studied. Hydrostatic pressure did not affect the size of the crystallites in carbon black particles. The pressure induced shift in Raman frequency of the graphitic component was a result of increased intermolecular forces and not smaller crystallites. Two methods of determining the fractal dimension, the FHH model and the yardstick technique based on the BET theory were used in the literature. Our study proved that the FHH model is sensitive to numerous assumptions and leads to wrong conclusions. On the other hand the yardstick method gave correct results, which agreed with the AFM results.
The growth process of first water layer and crystalline ice on the Rh(111) surface

NASA Astrophysics Data System (ADS)

Beniya, Atsushi; Sakaguchi, Yuji; Narushima, Tetsuya; Mukai, Kozo; Yamashita, Yoshiyuki; Yoshimoto, Shinya; Yoshinobu, Jun

2009-01-01

The adsorption states and growth process of the first layer and multilayer of water (D2O) on Rh(111) above 135K were investigated using infrared reflection absorption spectroscopy (IRAS), temperature programed desorption, spot-profile-analysis low-energy electron diffraction, and scanning tunneling microscopy (STM). At the initial stage, water molecules form commensurate (√3×√3)R30° islands, whose size is limited for several hexagonal units; the average diameter is ˜2.5nm. This two-dimensional (2D) island includes D-down species, and free OD species exist at the island edge. With increasing coverage, the D-up species starts to appear in IRAS. At higher coverages, the 2D islands are connected in STM images. By the titration of Xe adsorption we estimated that the D-down domain occupies about 55% on Rh(111) at the saturation coverage. Further adsorption of water molecules forms three-dimensional ice crystallites on the first water layer; thus, the growth mode of crystalline water layers on Rh(111) is a Stranski-Krastanov type. We have found that an ice crystallite starts to grow on D-down domains and the D-down species do not reorient upon the formation of a crystalline ice.
Sulfonated poly(ether ether ketone)/poly(vinyl alcohol) sensitizing system for solution photogeneration of small Ag, Au, and Cu crystallites.

PubMed

Korchev, A S; Shulyak, T S; Slaten, B L; Gale, W F; Mills, G

2005-04-28

Illumination of air-free aqueous solutions containing sulfonated poly(ether ether ketone) and poly(vinyl alcohol) with 350 nm light results in benzophenone ketyl radicals of the polyketone. The polymer radicals form with a quantum yield 0.02 and decay with a second-order rate constant 6 orders of magnitude lower than that of typical alpha-hydroxy radicals. Evidence is presented that the polymeric benzophenone ketyl radicals reduce Ag+, Cu2+, and AuCl4- to metal particles of nanometer dimensions. Decreases in the reduction rates with increasing Ag(I), Cu(II), and Au(III) concentrations are explained using a kinetic model in which the metal ions quench the excited state of the polymeric benzophenone groups, which forms the macromolecular radicals. Quenching is fastest for Ag+, whereas Cu2+ and AuCl4- exhibit similar rate constants. Particle formation becomes more complex as the number of equivalents needed to reduce the metal ions increases; the Au(III) system is an extreme case where the radical reactions operate in parallel with secondary light-initiated and thermal reduction channels. For each metal ion, the polymer-initiated photoreactions produce crystallites possessing distinct properties, such as a very strong plasmon in the Ag case or the narrow size distribution exhibited by Au particles.
XRD and FTIR analysis heat treated lithium bismo-borate glasses doped with 1.0 mol% copper ferrite

NASA Astrophysics Data System (ADS)

Yadav, Arti; Narwal, P.; Dahiya, Manjeet S.; Dahiya, T.; Agarwal, A.; Khasa, S.

2018-05-01

Glasses of compositions of 20Li20 • xBi2O3• (79-x)B2O3 + (1.0 mol%) CuFe2O4, with 0 ≤ x ≤ 40 were prepared by melt-quench technique. To obtain the glass-ceramics the controlled heat treatment were given to the prepared glasses. Two nano crystalline phases, i.e., Li2B4O7 and LiB3O5 were observed from X-ray diffraction patterns of the prepared glass- ceramic samples. We investigated the change in coordination number of network formers B2O3 and Bi2O3 and network modifiers Bi2O3, Li2O and CuFe2O4. Crystallites size (lies in range ˜47-50nm) and lattice strain (ɛ) were calculated for major phases for all prepared samples. FT-IR study revealed the de-polymerization of borate groups that change with heat treatment and Bi2O3 content. Deconvolution of IR absorption spectra resolves the overlapped and hidden peaks in IR spectra. Sharp and more intense FTIR peaks confirm the vibrations due to crystallites Li2B4O7 and LiB3O5 and change in coordination of network forming borate units.
Effect of 60Co γ-irradiation on structural and optical properties of thin films of Ga10Se80Hg10

NASA Astrophysics Data System (ADS)

Ahmad, Shabir; Asokan, K.; Shahid Khan, Mohd.; Zulfequar, M.

2015-08-01

Thin films of Ga10Se80Hg10 have been deposited onto a chemically cleaned Al2O3 substrates by thermal evaporation technique under vacuum. The investigated thin films are irradiated by 60Co γ-rays in the dose range of 50-150 kGy. X-ray diffraction patterns of the investigated thin films confirm the preferred crystallite growth occurs in the tetragonal phase structure. It also shows, the average crystallite size increases after γ-exposure, which indicates the crystallinity of the material increases after γ-irradiation. These results were further supported by surface morphological analysis carried out by scanning electron microscope and atomic force microscope which also shows the crystallinity of the material increases with increasing the γ-irradiation dose. The optical transmission spectra of the thin films at normal incidence were investigated in the spectral range from 190 to 1100 nm. Using the transmission spectra, the optical constants like refractive index (n) and extinction coefficient (k) were calculated based on Swanepoel's method. The optical band gap (Eg) was also estimated using Tauc's extrapolation procedure. The optical analysis shows: the value of optical band gap of investigated thin films decreases and the corresponding absorption coefficient increases continuously with increasing dose of γ-irradiation.
Structural characterization of ZnO thin films grown on various substrates by pulsed laser deposition

NASA Astrophysics Data System (ADS)

Novotný, M.; Čížek, J.; Kužel, R.; Bulíř, J.; Lančok, J.; Connolly, J.; McCarthy, E.; Krishnamurthy, S.; Mosnier, J.-P.; Anwand, W.; Brauer, G.

2012-06-01

ZnO thin films were grown by pulsed laser deposition on three different substrates: sapphire (0 0 0 1), MgO (1 0 0) and fused silica (FS). The structure and morphology of the films were characterized by x-ray diffraction and scanning electron microscopy and defect studies were carried out using slow positron implantation spectroscopy (SPIS). Films deposited on all substrates studied in this work exhibit the wurtzite ZnO structure and are characterized by an average crystallite size of 20-100 nm. However, strong differences in the microstructure of films deposited on various substrates were found. The ZnO films deposited on MgO and sapphire single-crystalline substrates exhibit local epitaxy, i.e. a well-defined relation between film crystallites and the substrate. Domains with different orientation relationships with the substrate were found in both films. On the other hand, the film deposited on the FS substrate exhibits fibre texture with random lateral orientation of crystallites. Extremely high compressive in-plane stress of σ ˜ 14 GPa was determined in the film deposited on the MgO substrate, while the film deposited on sapphire is virtually stress-free, and the film deposited on the FS substrate exhibits a tensile in-plane stress of σ ˜ 0.9 GPa. SPIS investigations revealed that the concentration of open-volume defects in the ZnO films is substantially higher than that in a bulk ZnO single crystal. Moreover, the ZnO films deposited on MgO and sapphire single-crystalline substrates exhibit a significantly higher density of defects than the film deposited on the amorphous FS substrate.
Line profile analysis of ODS steels Fe20Cr5AlTiY milled powders at different Y2O3 concentrations

NASA Astrophysics Data System (ADS)

Afandi, A.; Nisa, R.; Thosin, K. A. Z.

2017-04-01

Mechanical properties of material are largely dictated by constituent microstructure parameters such as dislocation density, lattice microstrain, crystallite size and its distribution. To develop ultra-fine grain alloys such as Oxide Dispersion Strengthened (ODS) alloys, mechanical alloying is crucial step to introduce crystal defects, and refining the crystallite size. In this research the ODS sample powders were mechanically alloyed with different Y2O3 concentration respectively of 0.5, 1, 3, and 5 wt%. MA process was conducted with High Energy Milling (HEM) with the ball to powder ratio of 15:1. The vial and the ball were made of alumina, and the milling condition is set 200 r.p.m constant. The ODS powders were investigated by X-Ray Diffractions (XRD), Bragg-Brentano setup of SmartLab Rigaku with 40 KV, and 30 mA, step size using 0.02°, with scanning speed of 4°min-1. Line Profile Analysis (LPA) of classical Williamson-Hall was carried out, with the aim to investigate the different crystallite size, and microstrain due to the selection of the full wide at half maximum (FWHM) and integral breadth.
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
Crystallographic Analysis of a Japanese Sword by using Bragg Edge Transmission Spectroscopy

NASA Astrophysics Data System (ADS)

Shiota, Yoshinori; Hasemi, Hiroyuki; Kiyanagi, Yoshiaki

Neutron imaging using a pulsed neutron source can give crystallographic information over wide area of a sample by analysing position dependent transmission spectra. With the use of a Bragg edge imaging method we non-destructively obtained crystallographic information of a Japanese sword, signed by Bishu Osafune Norimitsu, in order to know position dependent crystallographic characteristics and to check usefulness of the method for the Japanese sword investigation. Strong texture appeared on the back side. On the other hand in the middle area almost isotropic feature appeared and edge side showed feature between them. Rather isotropic area in the centre area gradually reduced from the grip side to the tip side. The crystallite size was smaller near the edge and became larger towards the back side. The smaller crystallite size will be due to quenching around the edge and this trend disappeared in the grip (nakago) area. The larger crystallite size will be due to strong hammering. Coarse grains were also observed directly as transmission images with the use of a high spatial resolution detector. The spatial distribution of the grains was not uniform but the reason have not been understood. Furthermore, a white area around a tip area was proved to be a void by looking at the Brag edge transmission spectra. This void may be formed during forging process of two kinds of steel. It is suggested that consideration on differences in the texture and the crystallite size depending on position will give information to clarify the manufacturing process, and Bragg edge analysis will be a profitable tool for research of Japanese sword.
Pseudocapacitance of Co doped NiO nanoparticles and its room temperature ferromagnetic behavior

NASA Astrophysics Data System (ADS)

Bharathy, G.; Raji, P.

2018-02-01

Co doped NiO nanoparticles CoxNi1-xO (x = 0.0, 0.1, 0.2, 0.3, 0.4) were synthesized by the Sol-gel technique. The impact of Co doping concentration on structural, functional and magnetic properties of NiO nanoparticles was analyzed by X-ray diffraction (XRD), FESEM with EDAX, FTIR and VSM. The average crystallite size was measured to be 34 nm and 11 nm for NiO and Co doped NiO nanoparticles respectively. FESEM reveals that particles are spherical in shape with average size around 30 nm. The elemental composition was analyzed by EDAX. FTIR spectra reveal the existence of NiO peaks in the prepared samples, room temperature ferromagnetism was observed for pure and Co doped NiO nanoparticles by VSM. Pure NiO particles shows ferromagnetic behavior with low coercivity and it increases gradually when doping ratio increases. Higher saturation magnetization was obtained for the sample 0.1 M of Co doped NiO nanoparticle as 22.09 emu/gm. An attempt has been made to study the pseudocapacitance behavior of pure and Co doped NiO nano particles in various scan rates. Electrochemical studies show that 0.4 M Co doped sample gives better charge storage capacity with maximum specific capacitance of 379 Fg-1 at a scan rate of 20 mVs-1. It reveals that it is a promising electrode material for super capacitor applications.
Magnetic and dielectric properties of Fe3BO6 nanoplates prepared through self-combustion method

NASA Astrophysics Data System (ADS)

Kumari, Kalpana

In the present investigation, a facile synthesis method is explored involving a self-combustion of a solid precursor mixture of iron oxide Fe2O3 and boric acid (H3BO3) using camphor (C10H16O) as fuel in ambient air in order to form a single phase Fe3BO6 crystallites. X-ray diffraction (XRD), Field emission electron microscopy (FESEM), magnetic, and dielectric properties of as prepared sample are studied. From XRD pattern, a single phase compound is observed with an orthorhombic crystal structure (Pnma space group), with average crystallite size of 42nm. A reasonably uniform size distribution of the plates and self-assemblies is retained in the sample. A magnetic transition is observed in dielectric permittivity (at ˜445K) and power loss (at ˜435K) when plotted against temperature. A weak peak occurs near 330K due to the charge reordering in the sample. For temperatures above the transition temperature, a sharp increase of the dielectric loss is observed which occurs due to the presence of thermally activated charge carriers. A canted antiferromagnetic Fe3+ ordering in a Fe3BO6 lattice with a localized charge surface layer is an apparent source of exhibiting a ferroelectric feature in this unique example of a centrosymmetric compound. An induced spin current over the Fe sites thus could give rise to a polarization hysteresis loop. Due to the presence of both ferromagnetic as well as polarization ordering, Fe3BO6 behaves like a single phase multiferroic ceramics.
Study of morphology and magnetic properties of the HoNi{sub 3} crystalline and ball-milled compound

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

Bajorek, Anna, E-mail: anna.bajorek@us.edu.pl; Silesian Center for Education and Interdisciplinary Research, University of Silesia, 75 Pułku Piechoty 1A, 41-500 Chorzów; Skornia, Paweł

2015-03-15

The morphology and magnetic properties of the HoNi{sub 3} crystalline and ball-milled intermetallic compounds are presented. The polycrystalline HoNi{sub 3} bulk compound crystallizes in the rhombohedral PuNi{sub 3} — type of crystal structure and indicates ferrimagnetic arrangement with the Curie temperature of T{sub C} = 57 ± 2 K, the helimagnetic temperature T{sub h} = 23 ± 2 K with the total saturation magnetic moment of 6.84 μ{sub B}/f.u. at 2 K. The use of the ball-milling method leads to the formation of HoNi{sub 3} nanoflakes with typical thickness of less than 100 nm prone to agglomeration upon milling. Themore » increase of grinding duration leads to the reduction in crystallite size, which was confirmed by various complementary microscopical and diffraction studies. Moreover, the increase in milling duration results in the emergence of the relatively small coercivity (H{sub C}), remanence (M{sub r}) and a variation of the saturation magnetization (M{sub S}). - Graphical abstract: Display Omitted - Highlights: • The ball-milling method exhibits significant potential for producing RT{sub 3} nanopowders. • The AFM method was used for the first time in analysis of R–T nanoflakes morphology. • HoNi{sub 3} compound forms polycrystalline and textured nanoflakes evolving upon milling. • The decrease in crystallite size via grinding is confirmed by XRD, TEM and AFM. • The magnetic parameters were sensitive to the extension of pulverization b.« less
Visible photoassisted room-temperature oxidizing gas-sensing behavior of Sn2S3 semiconductor sheets through facile thermal annealing.

PubMed

Liang, Yuan-Chang; Lung, Tsai-Wen; Wang, Chein-Chung

2016-12-01

Well-crystallized Sn 2 S 3 semiconductor thin films with a highly (111)-crystallographic orientation were grown using RF sputtering. The surface morphology of the Sn 2 S 3 thin films exhibited a sheet-like feature. The Sn 2 S 3 crystallites with a sheet-like surface had a sharp periphery with a thickness in a nanoscale size, and the crystallite size ranged from approximately 150 to 300 nm. Postannealing the as-synthesized Sn 2 S 3 thin films further in ambient air at 400 °C engendered roughened and oxidized surfaces on the Sn 2 S 3 thin films. Transmission electron microscopy analysis revealed that the surfaces of the Sn 2 S 3 thin films transformed into a SnO 2 phase, and well-layered Sn 2 S 3 -SnO 2 heterostructure thin films were thus formed. The Sn 2 S 3 -SnO 2 heterostructure thin film exhibited a visible photoassisted room-temperature gas-sensing behavior toward low concentrations of NO 2 gases (0.2-2.5 ppm). By contrast, the pure Sn 2 S 3 thin film exhibited an unapparent room-temperature NO 2 gas-sensing behavior under illumination. The suitable band alignment at the interface of the Sn 2 S 3 -SnO 2 heterostructure thin film and rough surface features might explain the visible photoassisted room-temperature NO 2 gas-sensing responses of the heterostructure thin film on exposure to NO 2 gas at low concentrations in this work.
Influence of solution deposition rate on properties of V2O5 thin films deposited by spray pyrolysis technique

NASA Astrophysics Data System (ADS)

Abd-Alghafour, N. M.; Ahmed, Naser M.; Hassan, Zai; Mohammad, Sabah M.

2016-07-01

Vanadium oxide (V2O5) thin films were deposited on glass substrates by using a cost-efficient spray pyrolysis technique. The films were grown at 350° through thermal decomposition of VCl3 in deionized water with different solution spray rates. The high resolution X-ray diffraction results revealed the formation of nanocrystalline films having orthorhombic structures with preferential orientation along (101) direction. The spray rate influenced the surface morphology and crystallite size of the films. The crystallite size was found to increase whereas the micro-strain was decreased by increasing the spray deposition rates. The increase in crystallite size and decrease in the macrostrain resulted in an improvement in the films' crystallinity. The UV-Visible spectroscopy analysis indicated that the average transmittance of all films lies in the range 75-80 %. The band gap of V2O5 film was decreased from 2.65 to 2.46 eV with increase of the spray deposition rate from 5 ml/min to 10 ml/min. first, second, and third level headings (first level heading).
Fabrication of hydroxyapatite and TiO 2 nanorods on microarc-oxidized titanium surface using hydrothermal treatment

NASA Astrophysics Data System (ADS)

Song, Ho-Jun; Kim, Ji-Woo; Kook, Min-Suk; Moon, Won-Jin; Park, Yeong-Joon

2010-09-01

AC-type microarc oxidation (MAO) and hydrothermal treatment techniques were used to enhance the bioactivity of commercially pure titanium (CP-Ti). The porous TiO 2 layer fabricated by the MAO treatment had a dominant anatase structure and contained Ca and P ions. The MAO-treated specimens were treated hydrothermally to form HAp crystallites on the titanium oxide layer in an alkaline aqueous solution (OH-solution) or phosphorous-containing alkaline solution (POH-solution). A small number of micro-sized hydroxyapatite (HAp) crystallites and a thin layer composed of nano-sized HAps were formed on the Ti-MAO-OH group treated hydrothermally in an OH-solution, whereas a large number of micro-sized HAp crystallites and dense anatase TiO 2 nanorods were formed on the Ti-MAO-POH group treated hydrothermally in a POH-solution. The layer of bone-like apatite that formed on the surface of the POH-treated sample after soaking in a modified simulated body fluid was thicker than that on the OH-treated samples.
Fabrication and enhanced photoluminescence properties of Sm3+-doped ZnO-Al2O3-B2O3-SiO2 glass derived willemite glass-ceramic nanocomposites

NASA Astrophysics Data System (ADS)

Tarafder, Anal; Molla, Atiar Rahaman; Mukhopadhyay, Sunanda; Karmakar, Basudeb

2014-07-01

The transparent willemite, Zn2SiO4 (ZS) glass-ceramic nanocomposites were prepared from melt-quench derived ZnO-Al2O3-B2O3-SiO2 (ZABS) precursor glass by an isothermal heat-treatment process. The generation of willemite crystal phase, size and morphology with increase in heat-treatment time was examined by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) techniques. The average calculated crystallite size obtained from XRD is found to be in the range 80-120 nm. The decreased refractive index with increase in heat-treatment time attributed to partial replacement of ZnO4 units of willemite nanocrystals by AlO4 units and simultaneous generation of vacancies in the Zn-site. Fourier transform infrared (FTIR) reflection spectroscopy exhibits the structural evolution of willemite glass-ceramics. The photoluminescence spectra of Sm3+ ions exhibit emission transitions of 4G5/2 → 6HJ (J = 5/2, 7/2, 9/2, 11/2) and its excitation spectra shows an intense absorption band at 402 nm. These spectra reveal that the luminescence performance of the glass-ceramic nanocomposites is enhanced up to 14-fold with crystallization into willemite.
Fabrication of NIR-responsive NaYF4:Yb,Tm/anatase TiO2 composite aerogel

NASA Astrophysics Data System (ADS)

Li, Fu-Chih; Kitamoto, Yoshitaka

2018-01-01

3-dimensional interconnected network structure of TiO2 aerogel has attracted considerable attention to solve environmental issues due to an advanced oxidation process which uses abundant sunlight for the complete minimization of toxic pollutants. The TiO2 aerogel with high specific surface area, large pores, and low density has a potential to be used as photocatalyst for air and water purification. Nonetheless, due to the larger band gap, TiO2 semiconductor photocatalysts possess high oxidizing properties under UV light only which occupies 5% of solar energy. To expand the absorption spectrum of TiO2 aerogel under solar irradiation, the NaYF4:Yb,Tm nanoparticles (NPs) are introduced into the TiO2 aerogel matrix structure. The morphology and crystal structure of the composite aerogel are investigated by transmission electron microscopy and X-ray diffraction, respectively. The particle size of NaYF4:Yb,Tm NPs is approximately 40 nm and the crystallite size of TiO2 is around 10 nm. In addition, the NaYF4:Yb,Tm NPs are enclosed by anatase phase of TiO2 aerogel. The NaYF4:Yb,Tm NPs which exist in the TiO2 aerogel has a capability of transferring NIR light to UV region.
Adsorption of Cd2+ ions on plant mediated SnO2 nanoparticles

NASA Astrophysics Data System (ADS)

Haq, Sirajul; Rehman, Wajid; Waseem, Muhammad; Shahid, Muhammad; Mahfooz-ur-Rehman; Hussain Shah, Khizar; Nawaz, Mohsan

2016-10-01

Plant mediated SnO2 nanoparticles were synthesized by using SnCl4.5H2O as a precursor material. The nanoparticles were then characterized for BET surface area measurements, energy dispersive x-rays (EDX), scanning electron microscopy (SEM), UV-vis diffuse reflectance (DRS) spectra and x-rays diffraction (XRD) analysis. The successful synthesis of SnO2 nanoparticles was confirmed by EDX analysis. The particle sizes were in the range 19-27 nm whereas the crystallite size computed from XRD measurement was found to be 19.9 nm. Batch adsorption technique was employed for the removal of Cd2+ ions from aqueous solution. The sorption studies of Cd2+ ions were performed at pHs 4 and 6. The equilibrium concentration of Cd2+ ions was determined by atomic absorption spectrometer (flame mode). The uptake of Cd2+ ions was affected by initial concentration, pH and temperature of the electrolytic solution. It was observed that the adsorption of Cd2+ ions enhanced with increase in the initial concentration of Cd2+ ions whereas a decrease in the percent adsorption was detected. From the thermodynamic parameters, the adsorption process was found spontaneous and endothermic in nature. The n values confirmed 2:1 exchange mechanism between surface protons and Cd2+ ions.
Effect of synthesis route on the uptake of Ni and Cd by MgFe2O4 nanopowders

NASA Astrophysics Data System (ADS)

Al-Najar, B.; Khezami, L.; Judith Vijaya, J.; Lemine, O. M.; Bououdina, M.

2017-01-01

In this study, MgFe2O4 nanopowders were synthesized through two different methods, sol-gel method (SG) and modified sol-gel with Ammonia (MSG-A). The influence of synthesis route was investigated in terms of phase stability, pores size and surface area, magnetic properties and uptake of Ni and Cd metals from aqueous solution. Rietveld refinements of x-ray diffraction patterns confirmed the formation of single spinel phase for SG sample, while minor impurity was detected for SGM-A sample (few amount of MgO). The crystallite size was found to be sensitive to the preparation method; it ranges from 4 nm for SG to 15 nm for MSG-A. Magnetization experiment at room temperature showed ferromagnetic behavior with a saturation magnetization ( M s) ranging from 5.39 emu/g for SG to 9.93 emu/g for MSG-A. Preliminary results showed that SG and MSG-A samples are efficient adsorbent for Ni and Cd metal ions from aqueous solution. Maximum quantity of 62.67 and 61.2 mg of Ni(II) and 36.49 and 32.84 mg of Cd(II) was adsorbed per gram of MgFe2O4 synthesized by SG and MSG-A, respectively.

Optimised synthesis of ZnO-nano-fertiliser through green chemistry: boosted growth dynamics of economically important L. esculentum.

PubMed

Jabeen, Nyla; Maqbool, Qaisar; Bibi, Tahira; Nazar, Mudassar; Hussain, Syed Z; Hussain, Talib; Jan, Tariq; Ahmad, Ishaq; Maaza, Malik; Anwaar, Sadaf

2018-06-01

Mounting-up economic losses to annual crops yield due to micronutrient deficiency, fertiliser inefficiency and increasing microbial invasions (e.g. Xanthomonas cempestri attack on tomatoes) are needed to be solved via nano-biotechnology. So keeping this in view, the authors' current study presents the new horizon in the field of nano-fertiliser with highly nutritive and preservative effect of green fabricated zinc oxide-nanostructures (ZnO-NSs) during Lycopersicum esculentum (tomato) growth dynamics. ZnO-NS prepared via green chemistry possesses highly homogenous crystalline structures well-characterised through ultraviolet and visible spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction and scanning electron microscope. The ZnO-NS average size was found as small as 18 nm having a crystallite size of 5 nm. L. esculentum were grown in different concentrations of ZnO-NS to examine the different morphological parameters includes time of seed germination, germination percentage, the number of plant leaves, the height of the plant, average number of branches, days count for flowering and fruiting time period along with fruit quantity. Promising results clearly predict that bio-fabricated ZnO-NS at optimum concentration resulted as growth booster and dramatically triggered the plant yield.
Photoluminescent properties of spider silk coated with Eu-doped nanoceria

NASA Astrophysics Data System (ADS)

Dmitrović, Svetlana; Nikolić, Marko G.; Jelenković, Branislav; Prekajski, Marija; Rabasović, Mihailo; Zarubica, Aleksandra; Branković, Goran; Matović, Branko

2017-02-01

Spider dragline silk was coated with pure as well as Eu-doped ceria nanopowders at the room temperature. The treatment was done by immersion of the spider silk mesh into aqueous solutions of cerium nitrate (Ce(NO3)3) and ammonium hydroxide (NH4OH). Depending on the relationship between Ce3+ ion and ammonium hydroxide concentration, coated fibers exhibited a different thickness. Obtained materials were studied by means of FESEM. It was found that ceria nanoparticles of average size of 3 nm were coated along spider thread. X-ray diffraction (XRD) and selected-area electron diffraction (SAED) confirmed crystal nature of nanoparticle coating of spider silk. By using Williamson-Hall plots, crystallite size and strain were estimated. EDS measurement confirmed the presence of Eu in spider-Eu-doped ceria composite, and according to FTIR analysis, the interaction between CeO2 and spider silk was proposed. The morphology of obtained composite was observed by TEM. The photoluminescence emission spectra of spider silk coated with Eu-doped ceria were measured with two different excitations of 385 and 466 nm. The two-photon excited auto-fluorescence of spider silk coated with Eu-doped ceria was detected using a nonlinear laser scanning microscope. Obtained composite has a potential as a fluorescent labeling material in diverse applications.
Effect of various surfactants on changes in the emission color chromaticity in upconversion YVO4: Yb3+, Er3+ nanoparticles

NASA Astrophysics Data System (ADS)

Woźny, Przemysław; Szczeszak, Agata; Lis, Stefan

2018-02-01

YVO4: Yb3+,Er3+ upconverting nanocrystals were synthesized via a hydrothermal method using different compounds as surfactants. Structure and morphology of the nanocrystals were investigated by X-ray diffraction and transmission electron microscopy. Tetragonal crystal structure of the nanocrystals appeared irrespective of the type of surfactant used. The average crystallite size was estimated by TEM images. The obtained products were composed of small nanoparticles, in the size range of 10-60 nm, depending on the surfactant used. The morphology of the nanoparticles was also regulated by the type of surfactant. Spectroscopic analysis of the materials obtained was carried out by measuring the emission and excitation spectra and the intensity of luminescence as a function of laser energy and luminescence decays. The nanocrystals prepared exhibited a green upconversion emission attributed to the 2H11/2 → 4I15/2 and 4S3/2 → 4I15/2 transitions of Er3+, under NIR (985 nm) pulse laser irradiation, and their emission lifetimes were in the range 3.84-4.90 μs. On the basis of the spectroscopic investigation, the upconversion mechanism was proposed and chromaticity coordinates were calculated. Surfactants were found to influence on chromaticity of luminescence.
Enhancement of Energy Conversion Efficiency for Dye Sensitized Solar Cell Using Zinc Oxide Photoanode

NASA Astrophysics Data System (ADS)

Jamalullail, N.; Smohamad, I.; Nnorizan, M.; Mahmed, N.

2018-06-01

Dye sensitized solar cell (DSSC) is a third generation solar cell that is well known for its low cost, simple fabrication process and promised reasonable energy conversion efficiency. Basic structure of DSSC is composed of photoanode, dye sensitizer, electrolyte that is sandwiched together in between two transparent conductive oxide (TCO) glasses. Each of the components in the DSSC contributes important role that affect the energy conversion efficiency. In this research, the commonly used titanium dioxide (TiO2) photoanode has previously reported to have high recombination rate and low electron mobility which caused efficiency loss had been compared with the zinc oxide (ZnO) photoanode with high electron mobility (155 cm2V-1s-1). Both of these photoanodes had been deposited through doctor blade technique. The electrical performance of the laboratory based DSSCs were tested using solar cell simulator and demonstrated that ZnO is a better photoanode compared to TiO2 with the energy conversion efficiency of 0.34% and 0.29% respectively. Nanorods shape morphology was observed in ZnO photoanode with average particle size of 41.60 nm and average crystallite size of 19.13 nm. This research proved that the energy conversion efficiency of conventional TiO2 based photoanode can be improved using ZnO material.
Effect of ph Value and Calcination Temperature on Structure and Magnetic Properties of Strontium Hexaferrite Thin Film

NASA Astrophysics Data System (ADS)

Shanaghi, A.

2012-02-01

Strontium hexaferrite was widely used in the fabrication of commercial permanent magnets and certain microwave devices. In this study, the strontium hexaferrite nanoparticle coatings were prepared by sol-gel method and using spin coating process on silicon substrate, then the effect of pH value, such as 5, 7 and 9, and calcination temperatures, such as 600°C, 800°C, and 1000°C, on structural and magnetic properties of strontium hexaferrite thin films were investigated by XRD, SEM and VSM measurements. The maximum saturation magnetization value of 57.43 emu/g and coercivity value of 3908 Oe were achieved for the thin film with crystallite size approximately 41 nm, prepared at pH value of 7 and calcinations temperature of 800°C.
Non-equilibrium nitrogen DC-arc plasma treatment of TiO2 nanopowder.

PubMed

Suzuki, Yoshikazu; Gonzalez-Aguilar, José; Traisnel, Noel; Berger, Marie-Hélène; Repoux, Monique; Fulcheri, Laurent

2009-01-01

Non-equilibrium nitrogen DC-arc plasma treatment of a commercial TiO2 anatase nanopowder was examined to obtain nitrogen-doped TiO2. By using a non-thermal discharge at low current (150 mA) and high voltage (1200 V) using pure N2 gas, light yellowish-gray TiO2 powder was successfully obtained within a short period of 5-10 min. XPS and TEM-EELS studies confirmed the existence of doped nitrogen. Due to the relatively mild conditions (plasma power of 180 W), metastable anatase structure and fine crystallite size of TiO2 (ca. 10 nm) were maintained after the plasma treatment. The in-flight powder treatment system used in this study is promising for various type of powder treatment.
Synthesis of ultrafine ZrB2 powders by sol-gel process

NASA Astrophysics Data System (ADS)

Yang, Li-Juan; Zhu, Shi-Zhen; Xu, Qiang; Yan, Zhen-Yu; Liu, Ling

2010-09-01

Ultrafine zirconium diboride (ZrB2) powders have been synthesized by sol-gel process using zirconium oxychloride (ZrOCl2·8H2O), boric acid (H3BO3) and phenolic resin as sources of zirconia, boron oxide and carbon, respectively. The effects of the reaction temperature, B/Zr ratio, holding time, and EtOH/H2O ratio on properties of the synthesized ZrB2 powders were investigated. It was revealed that ultrafine (average crystallite size between 100 and 400 nm) ZrB2 powders can be synthesized with the optimum processing parameters as follows: (i) the ratio of B/Zr is 4; (ii) the solvent is pure ethanol; (iii) the condition of carbothermal reduction heat treatment is at 1550°C for 20 min.
Group 12 dithiocarbamate complexes: synthesis, spectral studies and their use as precursors for metal sulfides nanoparticles and nanocomposites.

PubMed

Ajibade, Peter A; Ejelonu, Benjamin C

2013-09-01

Zn(II), Cd(II) and Hg(II) dithiocarbamate complexes have been synthesized and characterized by elemental analysis, thermogravimetric analysis, UV-Vis, FTIR, (1)H- and (13)C NMR spectroscopy. The complexes were thermolysed at 180 °C and used as single molecule precursors for the synthesis of HDA capped ZnS, CdS and HgS nanoparticles and polymethylmethacrylate (PMMA) nanocomposites. The optical and structural properties of the nanoparticles and nanocomposites were studied by UV-Vis, PL, XRD and SEM. The crystallites sizes of the nanoparticles varied between 3.03 and 23.45 nm. SEM and EDX analyses of the nanocomposites confirmed the presence of the nanoparticles in the polymer matrix. Copyright © 2013 Elsevier B.V. All rights reserved.
Suppression of the commensurate magnetic phase in nanosized hübnerite MnW O 4

DOE PAGES

Zajdel, P.; G?gor, A.; Pajerowski, D. M.; ...

2017-05-18

Magnetic structures of nanosized (20 to 70 nm) powders of MnWO 4 and MnWO 4:Mo were studied using neutron powder diffraction (NPD). Sizes and shapes of the crystallites calculated from anisotropic peak broadening of diffraction peaks were found to be orthogonal parallelepipedlike with the longest edge along the c axis and the shortest along the b axis. SQUID measurements indicate the presence of two magnetic transitions around 8 and 12 K. Rietveld refinement of the NPD data below the magnetic transition was consistent with the presence of an incommensurate spiral-like (ac-AF2) phase. Finally, a commensurate phase AF1 was not observedmore » down to 2.5 K for all of the samples.« less
Deposition of Size-Selected Cu Nanoparticles by Inert Gas Condensation

PubMed Central

2010-01-01

Nanometer size-selected Cu clusters in the size range of 1–5 nm have been produced by a plasma-gas-condensation-type cluster deposition apparatus, which combines a grow-discharge sputtering with an inert gas condensation technique. With this method, by controlling the experimental conditions, it was possible to produce nanoparticles with a strict control in size. The structure and size of Cu nanoparticles were determined by mass spectroscopy and confirmed by atomic force microscopy (AFM) and scanning electron transmission microscopy (STEM) measurements. In order to preserve the structural and morphological properties, the energy of cluster impact was controlled; the energy of acceleration of the nanoparticles was in near values at 0.1 ev/atom for being in soft landing regime. From SEM measurements developed in STEM-HAADF mode, we found that nanoparticles are near sized to those values fixed experimentally also confirmed by AFM observations. The results are relevant, since it demonstrates that proper optimization of operation conditions can lead to desired cluster sizes as well as desired cluster size distributions. It was also demonstrated the efficiency of the method to obtain size-selected Cu clusters films, as a random stacking of nanometer-size crystallites assembly. The deposition of size-selected metal clusters represents a novel method of preparing Cu nanostructures, with high potential in optical and catalytic applications. PMID:20652132
Structure, morphology and optical properties of undoped and MN-doped ZnO(1-x)Sx nano-powders prepared by precipitation method

NASA Astrophysics Data System (ADS)

Dejene, F. B.; Onani, M. O.; Koao, L. F.; Wako, A. H.; Motloung, S. V.; Yihunie, M. T.

2016-01-01

The undoped and Mn-doped ZnO(1-x)Sx nano-powders were successfully synthesized by precipitation method without using any capping agent. Its structure, morphology, elemental analysis, optical and luminescence properties were determined by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), UV-vis spectroscopy (UV) and photoluminescence spectroscopy (PL). A typical SEM image of the un-doped ZnO(1-x)Sx nanoparticles exhibit flake like structures that changes to nearly spherical particles with Mn-doping. The XRD of undoped and Mn doped ZnO(1-x)Sx pattern reveals the formation of a product indexed to the hexagonal wurtzite phase of ZnS. The nanopowders have crystallite sizes estimated from XRD measurements were in the range of 10-20 nm. All the samples showed absorption maximum of ZnO(1-x)Sx at 271 nm and high transmittance in UV and visible region, respectively. The undoped ZnO(1-x)Sx nanoparticles show strong room-temperature photoluminescence with four emission bands centering at 338 nm, 384 nm, 448 nm and 705 nm that may originate to the impurity of ZnO(1-x)Sx, existence of oxide related defects. The calculated bandgap of the nanocrystalline ZnO(1-x)Sx showed a blue-shift with respect to the Mn-doping. The PL spectra of the Mn-doped samples exhibit a strong orange emission at around 594 nm attributed to the 4T1-6A1 transition of the Mn2+ ions.
One-Pot Process in Scalable Bath for Water-Dispersed ZnS Nanocrystals with the Tailored Size

DOE PAGES

Jung, Hyunsung; Phelps, Tommy J.; Rondinone, Adam J.; ...

2017-05-01

Well-dispersed ZnS nanocrystals with tailored size in aqueous solutions were synthesized by employing cysteine-sulfur (Cys-S) complexes with low molecular weight in a scalable anoxic vessel. High yield production of water-dispersed ZnS nanocrystals on a 10-L scale was demonstrated in an aqueous solution process. The average crystallite size of ZnS was controlled by changing the ratio of the cysteine to sulfide in the applied Cys-S complexes. A decrease in the crystallite size of ZnS likely resulted in both the blue shift of peak positions and the relative variation of peak intensities in the photoluminescence properties. In addition, the pH-dependent stability againstmore » aggregation of ZnS nanocrystals was investigated to reduce agglomeration.« less
Electron-Beam Deposition of Superconducting Molybdenum Thin Films for the Development of Mo/Au TES X-Ray Microcalorimeter

NASA Technical Reports Server (NTRS)

Finkbeiner, Fred Michael; Adams, Joseph S.; Bandler, Simon R.; Betancour-Martinez, Gabriele L.; Brown, Ari David; Chang, Meng-Ping; Chervenak, James A.; Chiao, Meng P.; Datesman, Aaron; Eckart, Megan E.;

2016-01-01

We are exploring the properties of electron-beam evaporated molybdenum thin films on silicon nitride coated silicon wafers at substrate temperatures between room temperature and 650 C. The temperature dependence of film stress, transition temperature, and electrical properties are presented. X-ray diffraction measurements are performed to gain information on molybdenum crystallite size and growth. Results show the dominant influence of the crystallite size on the intrinsic properties of our films. Wafer-scale uniformity, wafer yield, and optimal thermal bias regime for TES fabrication are discussed.

Grain size effect on activation energy in spinel CoFe{sub 2}O{sub 4} ceramic

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

Supriya, Sweety, E-mail: sweety@iitp.ac.in; Kumar, Sunil; Kar, Manoranjan

2016-05-23

Cobalt ferrite of different average crystallites (from nanocrystallite to micro crystallites) has been prepared by the Sol-Gel Method. The X-ray diffraction (XRD) analysis confirms the cubic spinel phase with no trace of impurity phases. The effect of annealing temperature on micro structure and electric transport properties as a function of frequency and temperature has been studied. It is observed that the electric impedance and conductivity are strongly dependent on grain size. The impedance spectroscopic study is employed to understand the electrical transport properties of cobalt ferrite.
Effects of Palladium Loading on the Response of a Thick Film Flame-made ZnO Gas Sensor for Detection of Ethanol Vapor

PubMed Central

Liewhiran, Chaikarn; Phanichphant, Sukon

2007-01-01

ZnO nanoparticles doped with 0-5 mol% Pd were successfully produced in a single step by flame spray pyrolysis (FSP) using zinc naphthenate and palladium (II) acetylacetonate dissolved in toluene-acetonitrile (80:20 vol%) as precursors. The effect of Pd loading on the ethanol gas sensing performance of the ZnO nanoparticles and the crystalline sizes were investigated. The particle properties were analyzed by XRD, BET, AFM, SEM (EDS line scan mode), TEM, STEM, EDS, and CO-pulse chemisorption measurements. A trend of an increase in specific surface area of samples and a decrease in the dBET with increasing Pd concentrations was noted. ZnO nanoparticles were observed as particles presenting clear spheroidal, hexagonal and rod-like morphologies. The sizes of ZnO spheroidal and hexagonal particle crystallites were in the 10-20 nm range. ZnO nanorods were in the range of 10-20 nm in width and 20-50 nm in length. The size of Pd nanoparticles increased and Pd-dispersion% decreased with increasing Pd concentrations. The sensing films were produced by mixing the particles into an organic paste composed of terpineol and ethyl cellulose as a vehicle binder. The paste was doctor-bladed onto Al2O3 substrates interdigitated with Au electrodes. The film morphology was analyzed by SEM and EDS analyses. The gas sensing of ethanol (25-250 ppm) was studied in dry air at 400°C. The oxidation of ethanol on the sensing surface of the semiconductor was confirmed by MS. A well-dispersed of 1 mol%Pd/ZnO films showed the highest sensitivity and the fastest response time (within seconds).
Conventional and microwave combustion synthesis of optomagnetic CuFe2O4 nanoparticles for hyperthermia studies

NASA Astrophysics Data System (ADS)

Kombaiah, K.; Vijaya, J. Judith; Kennedy, L. John; Bououdina, M.; Al-Najar, Basma

2018-04-01

Nanosized copper ferrite (CuFe2O4) nanoparticles have been prepared by conventional (CCM) and microwave (MCM) combustion methods using Hibiscus rosa sinensis plant extract as a fuel. XRD and rietveld analysis confirmed the formation of single cubic phase and with crystallite size varying from 25 to 62 nm owing to grain growth after calcination. FT-IR analysis confirms the modes of the cubic CuFe2O4 phase, due to the stretching and bending vibrations. Spherical shaped particles are observed by scanning electron microscopy and the average particle size is found to be in the range of 50-200 nm. The chemical composition is confirmed by energy dispersive X-ray analysis. The optical band gap energy estimated using Kubelka-Munk function with the help of UV-Visible diffused reflectance spectroscopy, is found to be 2.34 and 2.22 eV for CCM and MCM respectively. Photoluminescence analysis indicates that both samples absorb light in the UV-visible region and exhibit emissions at 360, 376, and 412 nm. Magnetic measurements indicate a ferromagnetic behavior, where both magnetic properties very much influenced by the preparation method and calcination temperature: both saturation magnetization and coercivity are found higher when using CCM and MCM; from 29.40 to 34.09 emu/g while almost double from 224.4 to 432.2 Oe. The observed changes in physical properties are mainly associated with crystallinity, particle size, better chemical homogeneity, and cations distribution among tetrahedral/octahedral sites. The maximum specific absorption rate obtained was 14.63 W/g, which can be considered suitable and favorable for magnetic hyperthermia. This study highlighted the benefits of green synthesis of CuFe2O4 nanoparticles providing better magnetic properties for the platform of hyperthermia application.
Immobilized TiO2 nanoparticles produced by flame spray for photocatalytic water remediation

NASA Astrophysics Data System (ADS)

Bettini, Luca Giacomo; Diamanti, Maria Vittoria; Sansotera, Maurizio; Pedeferri, Maria Pia; Navarrini, Walter; Milani, Paolo

2016-08-01

Anatase/rutile mixed-phase titanium dioxide (TiO2) photocatalysts in the form of nanostructured powders with different primary particle size, specific surface area, and rutile content were produced from the gas-phase by flame spray pyrolysis (FSP) starting from an organic solution containing titanium (IV) isopropoxide as Ti precursor. Flame spray-produced TiO2 powders were characterized by means of X-ray diffraction, Raman spectroscopy, and BET measurements. As-prepared powders were mainly composed of anatase crystallites with size ranging from 7 to 15 nm according to the synthesis conditions. TiO2 powders were embedded in a multilayered fluoropolymeric matrix to immobilize the nanoparticles into freestanding photocatalytic membranes. The photocatalytic activity of the TiO2-embedded membranes toward the abatement of hydrosoluble organic pollutants was evaluated employing the photodegradation of rhodamine B in aqueous solution as test reaction. The photoabatement rate of best performing membranes significantly overcomes that of membranes produced by the same method and incorporating commercial P25-TiO2.
Ultrasound-Assisted Synthesis of Titania Nanoparticles, Characterization of Their Thin Films, and Activity in Photooxidation of β-Naphthol

NASA Astrophysics Data System (ADS)

Hurain, Syyeda Sana; Habib, Amir; Hussain, Syed Muzammil; Ul-Haq, Noaman

2015-11-01

Nanosized titania (TiO2) films and powders were prepared from titanium isopropoxide by ultrasonication then ultrasonic aerosol-assisted chemical vapor deposition (UAACVD). X-ray diffraction (XRD), used to study the crystal structure, phase, and crystallite size of TiO2 samples annealed at 500°C, revealed anatase was the main crystalline phase. Scanning electron microscopy and atomic force microscopy revealed the quasi-spherical morphology of the TiO2 nanoparticles; average size distribution was in the range 20-35 nm. Ultraviolet-visible spectroscopy was used to evaluate the photocatalytic activity of the anatase TiO2, on the basis of efficiency of degradation of β-naphthol. Pure TiO2 nanoparticles synthesized by use of sonication-UAACVD then calcination at 500°C enabled effective photodegradation under UV light. This method of synthesis of TiO2 is superior to the reflux-UAACVD method with titanium isopropoxide as precursor.
Anti-ferromagnetic/ferromagnetic transition in half-metallic Co9Se8 nanoparticles

NASA Astrophysics Data System (ADS)

Singh, Jai; Kumar, Pushpendra

2015-09-01

The size, shape and defects of the half-metallic Co9Se8 nanoparticles (NPs) play a crucial role in the magnetic transition at the local magnetic regime at low temperatures. A general, non-injection, one-pot reaction route without toxic reagents, such as TOPO/TOPSe, surfactant and/or chelating agent, were used to synthesize gram scale of well-dispersed, high-quality Co9Se8 NPs. The calculated mean crystallite size of the NPs was ∼10 nm, which is consistent with the transmission electron microscope data. This study reveals an unusual anti-ferromagnetic/ferromagnetic transition with some super-paramagnetic character in the low temperature region of Co9Se8 NPs. These investigations are expected not only to help the observed phenomenon, but also help in identifying new half-metallic magnetic NPs for spintronics devices. The outcome provides better understanding of the occurrence of superparamagnetism at low temperatures in the nano-regime, for half-metallic systems.
Multiferroics BiMn1-xAlxO3 nanoparticles: Synthesis, characterization and evaluation of various structural, physical, electrical and dielectric parameters

NASA Astrophysics Data System (ADS)

Ahmad, Bashir; Raissat, Rabia; Mumtaz, Saleem; Ahmad, Zahoor; Sadiq, Imran; Ashiq, Muhammad Naeem; Najam-ul-Haq, Muhammad

2017-07-01

The aluminium substituted bismuth based manganates with nominal composition BiMn1-xAlxO3 (x = 0.0, 0.2, 0.4, 0.6 and 0.8) were prepared by the simple microemulsion method. The alteration in their structural, electrical and dielectric parameters due to Al substitution has been investigated. The X-ray diffraction analysis (XRD) confirms the formation of single phase orthorhombic with crystallite size ranges from 32 to 52 nm. The morphological features and particle size were determined by using scanning electron microscopy (SEM). The dc electrical resistivity increased from 6 × 108 to 8 × 109 Ω cm with the increase in substituent concentration. The dielectric constant, dielectric loss tangent and dielectric loss factor decreased with the increase in frequency. The increase in electrical resistivity makes the synthesized materials paramount over other materials and can be useful for technological applications in microwave devices.

Ion irradiation induced nucleation and growth of nanoparticles in amorphous silicon carbide at elevated temperatures

NASA Astrophysics Data System (ADS)

Zhang, Limin; Jiang, Weilin; Ai, Wensi; Chen, Liang; Wang, Tieshan

2018-07-01

Ion irradiation induced crystallization in as-deposited amorphous SiC films is investigated using grazing-angle incidence x-ray diffraction (GIXRD), transmission electron microscopy (TEM) and Raman spectroscopy. Irradiation with 5 MeV Xe to fluence of 1.15 × 1016 Xe/cm2 at 700 K results in a homogenous distribution of 3C-SiC grains with an average crystallite size of ∼5.7 nm over the entire film thickness (∼1 μm). The nucleation and growth processes exhibit a weak dependence on dose in displacements per atom (dpa) in the range from ∼6 dpa at the film surface to ∼20 dpa at the SiC/Si interface. A transformation of homonuclear C-C bonds from sp3 to sp2 hybridization is observed in the irradiated films, which may be partly responsible for the observed grain size saturation. The results from this study may have a significant impact on applications of SiC as structural components of advanced nuclear energy systems.
Optical, electrochemical and thermal properties of Mn2+ doped CdS nanoparticles

NASA Astrophysics Data System (ADS)

Muruganandam, S.; Anbalagan, G.; Murugadoss, G.

2015-08-01

Mn2+ doped (1-5 and 10 %) CdS nanoparticles have been synthesized by the chemical precipitation method using polyvinylpyrrolidone as a capping agent. The particle size, morphology and optical properties have been studied by X-ray powder diffraction, transmission electron microscopy, UV-Visible and photoluminescence spectroscopy. Powder diffraction data have confirmed that the crystallite size is around 2-5 nm. The band gap of the nanoparticles has been calculated using UV-Visible absorption spectra. An optimum concentration, Mn2+ (3 %) has been selected by optical study. The functional groups of the capping agent have been identified by fourier transform infrared spectroscopy study. The presence of dopant (Mn2+) has been confirmed by electron paramagnetic resonance spectroscopy. Thermal properties of CdS:Mn2+ have been analyzed using thermogravimetric-differential thermal analyser. The electrochemical properties of the undoped and doped samples have been studied by cyclic voltammetry for electrode applications. In addition, magnetic properties of Mn2+ doped CdS have been studied using a vibrating sample magnetometer.
Effect of solvent volume on the physical properties of aluminium doped nanocrystalline zinc oxide thin films deposited using a simplified spray pyrolysis technique

NASA Astrophysics Data System (ADS)

Jabena Begum, N.; Mohan, R.; Ravichandran, K.

2013-01-01

Aluminium doped zinc oxide (AZO) thin films were deposited by employing a low cost and simplified spray technique using a perfume atomizer from starting solutions having different volumes (10, 20, … , 50 mL) of solvent. The effect of solvent volume on the structural, electrical, optical, photoluminescence (PL) and surface morphological properties was studied. The electrical resistivity of the AZO films is remarkably influenced by the variation in the solvent volume. The X-ray diffraction profiles clearly showed that all the films have preferential orientation along the (0 0 2) plane irrespective of the solvent volume. The crystallite size was found to be in the nano range of 35-46 nm. The optical transmittance in the visible region is desirably high (>85%). The AFM images show columnar morphology with varying grain size. The PL studies revealed that the AZO film deposited from 50 mL of solvent volume has good quality with lesser defect density.
Single step, phase controlled, large scale synthesis of ferrimagnetic iron oxide polymorph nanoparticles by thermal plasma route and their rheological properties

NASA Astrophysics Data System (ADS)

Raut, Suyog A.; Mutadak, Pallavi R.; Kumar, Shiv; Kanhe, Nilesh S.; Huprikar, Sameer; Pol, Harshawardhan V.; Phase, Deodatta M.; Bhoraskar, Sudha V.; Mathe, Vikas L.

2018-03-01

In this paper we report single step large scale synthesis of highly crystalline iron oxide nanoparticles viz. magnetite (Fe3O4) and maghemite (γ-Fe2O3) via gas phase condensation process, where micron sized iron metal powder was used as a precursor. Selective phases of iron oxide were obtained by variation of gas flow rate of oxygen and hence partial pressure of oxygen inside the plasma reactor. Most of the particles were found to possesses average crystallite size of about 20-30 nm. The DC magnetization curves recorded indicate almost super-paramagnetic nature of the iron oxide magnetic nanoparticles. Further, iron oxide nanoparticles were analyzed using Raman spectroscopy, X-ray photoelectron spectroscopy and Mossbauer spectroscopy. In order to explore the feasibility of these nanoparticles for magnetic damper application, rheological studies have been carried out and compared with commercially available Carbonyl Iron (CI) particles. The nanoparticles obtained by thermal plasma route show improved dispersion which is useful for rheological applications.
Eco-friendly synthesis of silver nanoparticles and its larvicidal property against fourth instar larvae of Aedes aegypti.

PubMed

Ali, Zainal Abidin; Roslan, Muhammad Aidil; Yahya, Rosiyah; Wan Sulaiman, Wan Yusoff; Puteh, Rustam

2017-03-01

In this study, larvicidal activity of silver nanoparticles (AgNPs) synthesised using apple extract against fourth instar larvae of Aedes aegypti was determined. As a result, the AgNPs showed moderate larvicidal effects against Ae. aegypti larvae (LC 50 = 15.76 ppm and LC 90 = 27.7 ppm). In addition, comparison of larvicidal activity performance of AgNPs at high concentration prepared using two different methods showed that Ae. aegypti larvae was fully eliminated within the duration of 2.5 h. From X-ray diffraction, the AgNP crystallites were found to exhibit face centred cubic structure. The average size of these AgNPs as estimated by particle size distribution was in the range of 50-120 nm. The absorption maxima of the synthesised Ag showed characteristic Ag surface plasmon resonance peak. This green synthesis provides an economic, eco-friendly and clean synthesis route to Ag.
Cation distribution of Ni-Zn-Mn ferrite nanoparticles

NASA Astrophysics Data System (ADS)

Parvatheeswara Rao, B.; Dhanalakshmi, B.; Ramesh, S.; Subba Rao, P. S. V.

2018-06-01

Mn substituted Ni-Zn ferrite nanoparticles, Ni0.4Zn0.6-xMnxFe2O4 (x = 0.00-0.25 in steps of 0.05), using metal nitrates were prepared by sol-gel autocombustion in citric acid matrix. The samples were examined by X-ray diffraction and vibrating sample magnetometer techniques. Rietveld structural refinements using the XRD data were performed on the samples to consolidate various structural parameters like phase (spinel), crystallite size (24.86-37.43 nm), lattice constant (8.3764-8.4089 Å) etc and also to determine cation distributions based on profile matching and integrated intensity ratios. Saturation magnetization values (37.18-68.40 emu/g) were extracted from the measured M-H loops of these nanoparticles to estimate their magnetic moments. Experimental and calculated magnetic moments and lattice constants were used to confirm the derived cation distributions from Rietveld analysis. The results of these ferrite nanoparticles are discussed in terms of the compositional modifications, particle sizes and the corresponding cation distributions as a result of Mn substitutions.
Thickness Dependent Nanostructural, Morphological, Optical and Impedometric Analyses of Zinc Oxide-Gold Hybrids: Nanoparticle to Thin Film

PubMed Central

Perumal, Veeradasan; Hashim, Uda; Gopinath, Subash C. B.; Haarindraprasad, R.; Liu, Wei-Wen; Poopalan, P.; Balakrishnan, S. R.; Thivina, V.; Ruslinda, A. R.

2015-01-01

The creation of an appropriate thin film is important for the development of novel sensing surfaces, which will ultimately enhance the properties and output of high-performance sensors. In this study, we have fabricated and characterized zinc oxide (ZnO) thin films on silicon substrates, which were hybridized with gold nanoparticles (AuNPs) to obtain ZnO-Aux (x = 10, 20, 30, 40 and 50 nm) hybrid structures with different thicknesses. Nanoscale imaging by field emission scanning electron microscopy revealed increasing film uniformity and coverage with the Au deposition thickness. Transmission electron microscopy analysis indicated that the AuNPs exhibit an increasing average diameter (5–10 nm). The face center cubic Au were found to co-exist with wurtzite ZnO nanostructure. Atomic force microscopy observations revealed that as the Au content increased, the overall crystallite size increased, which was supported by X-ray diffraction measurements. The structural characterizations indicated that the Au on the ZnO crystal lattice exists without any impurities in a preferred orientation (002). When the ZnO thickness increased from 10 to 40 nm, transmittance and an optical bandgap value decreased. Interestingly, with 50 nm thickness, the band gap value was increased, which might be due to the Burstein-Moss effect. Photoluminescence studies revealed that the overall structural defect (green emission) improved significantly as the Au deposition increased. The impedance measurements shows a decreasing value of impedance arc with increasing Au thicknesses (0 to 40 nm). In contrast, the 50 nm AuNP impedance arc shows an increased value compared to lower sputtering thicknesses, which indicated the presence of larger sized AuNPs that form a continuous film, and its ohmic characteristics changed to rectifying characteristics. This improved hybrid thin film (ZnO/Au) is suitable for a wide range of sensing applications. PMID:26694656
Thickness Dependent Nanostructural, Morphological, Optical and Impedometric Analyses of Zinc Oxide-Gold Hybrids: Nanoparticle to Thin Film.

PubMed

Perumal, Veeradasan; Hashim, Uda; Gopinath, Subash C B; Haarindraprasad, R; Liu, Wei-Wen; Poopalan, P; Balakrishnan, S R; Thivina, V; Ruslinda, A R

2015-01-01

The creation of an appropriate thin film is important for the development of novel sensing surfaces, which will ultimately enhance the properties and output of high-performance sensors. In this study, we have fabricated and characterized zinc oxide (ZnO) thin films on silicon substrates, which were hybridized with gold nanoparticles (AuNPs) to obtain ZnO-Aux (x = 10, 20, 30, 40 and 50 nm) hybrid structures with different thicknesses. Nanoscale imaging by field emission scanning electron microscopy revealed increasing film uniformity and coverage with the Au deposition thickness. Transmission electron microscopy analysis indicated that the AuNPs exhibit an increasing average diameter (5-10 nm). The face center cubic Au were found to co-exist with wurtzite ZnO nanostructure. Atomic force microscopy observations revealed that as the Au content increased, the overall crystallite size increased, which was supported by X-ray diffraction measurements. The structural characterizations indicated that the Au on the ZnO crystal lattice exists without any impurities in a preferred orientation (002). When the ZnO thickness increased from 10 to 40 nm, transmittance and an optical bandgap value decreased. Interestingly, with 50 nm thickness, the band gap value was increased, which might be due to the Burstein-Moss effect. Photoluminescence studies revealed that the overall structural defect (green emission) improved significantly as the Au deposition increased. The impedance measurements shows a decreasing value of impedance arc with increasing Au thicknesses (0 to 40 nm). In contrast, the 50 nm AuNP impedance arc shows an increased value compared to lower sputtering thicknesses, which indicated the presence of larger sized AuNPs that form a continuous film, and its ohmic characteristics changed to rectifying characteristics. This improved hybrid thin film (ZnO/Au) is suitable for a wide range of sensing applications.
Structural and magnetic properties of Gd3+ ion substituted magnesium ferrite nanopowders

NASA Astrophysics Data System (ADS)

Elkady, Ashraf S.; Hussein, Shaban I.; Rashad, Mohamed M.

2015-07-01

Nanocrystalline MgGdxFe2-xO4 powders (where x=0, 0.05, 0.1, 0.2, 0.25, 0.3) have been synthesized by the ethylene diamine tetraacetic acid (EDTA)-based sol-gel combustion method. X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, high resolution transmission electron microscopy (HRTEM) and vibrating sample magnetometer (VSM) were applied in order to study the effect of variation of Gd3+ ion substitution and its impact on crystal structure, crystallite size, lattice parameters, nanostructure and magnetic properties of the formed powders. XRD indicated that, after doping and calcination at 400 °C for 2 h, all samples have two spinel ferrite structures namely cubic and tetragonal phases, which are dependent on Gd3+ ion concentration. The cubic phase is found to increase with increasing the Gd3+ ion molar ratio up to 0.1, compared to pure MgFe2O4 and higher Gd3+ content samples. Indeed, with increasing Gd3+ ion, the crystallite size was almost unchanged whereas the lattice parameter was found to increase. FT-IR spectrum showed broadening of the ν2 band and the presence of another band in the range (465-470 cm-1) upon adding Gd3+ ion, which confirm the presence of Gd3+ ion in addition to Fe3+ ion at octahedral site. Besides, these bands were assigned to the formation of (Gd3+-O2-) complexes at B-sites. HRTEM images showed that the studied samples consist of nanocrystallites having average particle sizes around 9 nm for pure MgFe2O4 up to 27 and 42 nm for the Gd3+ ion substituted MgFe2O4 of molar ratio 0.05 and 0.30, respectively. An examination of the magnetic properties revealed an increase in saturation magnetization with increasing Gd concentration incorporation up to x=0.1, as a result of the change of cubic and tetragonal spinel ratio and lattice parameters. Meanwhile, the formed powders exhibited superparamagnetic characteristics. Therefore, such newly synthesized superparamagnetic nanoparticles, containing Gd3+ ion can be considered as a promising candidate for use in several potential applications including neutron capture therapy (NCT), magnetic hyperthermia, ferrofluids and magnetic resonance imaging (MRI).
Characteristics of nano-sized yttria powder synthesized by a polyvinyl alcohol solution route at low temperature.

PubMed

Lee, Sang-Jin; Jung, Choong-Hwan

2012-01-01

Nano-sized yttria (Y2O3) powders were successfully synthesized at a low temperature of 400 degrees C by a simple polymer solution route. PVA polymer, as an organic carrier, contributed to an atom-scale homogeneous precursor gel and it resulted in fully crystallized, nano-sized yttria powder with high specific surface area through the low temperature calcination. In this process, the content of PVA, calcination temperature and heating time affected the microstructure and crystallization behavior of the powders. The development of crystalline phase and the final particle size were strongly dependant on the oxidation reaction from the polymer burn-out step and the PVA content. In this paper, the PVA solution technique for the fabrication of nano-sized yttria powders is introduced. The effects of PVA content and holding time on the powder morphology and powder specific surface area are also studied. The characterization of the synthesized powders is examined by using XRD, DTA/TG, SEM, TEM and nitrogen gas adsorption. The yttria powder synthesized from the PVA content of 3:1 ratio and calcined at 400 degrees C had a crystallite size of about 20 nm or less with a high surface areas of 93.95-120.76 m2 g(-1).
Morphological evolution of carbon nanofibers encapsulating SnCo alloys and its effect on growth of the solid electrolyte interphase layer.

PubMed

Shin, Jungwoo; Ryu, Won-Hee; Park, Kyu-Sung; Kim, Il-Doo

2013-08-27

Two distinctive one-dimensional (1-D) carbon nanofibers (CNFs) encapsulating irregularly and homogeneously segregated SnCo nanoparticles were synthesized via electrospinning of polyvinylpyrrolidone (PVP) and polyacrylonitrile (PAN) polymers containing Sn-Co acetate precursors and subsequent calcination in reducing atmosphere. CNFs synthesized with PVP, which undergoes structural degradation of the polymer during carbonization processes, exhibited irregular segregation of heterogeneous alloy particles composed of SnCo, Co3Sn2, and SnO with a size distribution of 30-100 nm. Large and exposed multiphase SnCo particles in PVP-driven amorphous CNFs (SnCo/PVP-CNFs) kept decomposing liquid electrolyte and were partly detached from CNFs during cycling, leading to a capacity fading at the earlier cycles. The closer study of solid electrolyte interphase (SEI) layers formed on the CNFs reveals that the gradual growth of fiber radius due to continuous increment of SEI layer thickness led to capacity fading. In contrast, SnCo particles in PAN-driven CNFs (SnCo/PAN-CNFs) showed dramatically reduced crystallite sizes (<10 nm) of single phase SnCo nanoparticles which were entirely embedded in dense, semicrystalline, and highly conducting 1-D carbon matrix. The growth of SEI layer was limited and saturated during cycling. As a result, SnCo/PAN-CNFs showed much improved cyclability (97.9% capacity retention) and lower SEI layer thickness (86 nm) after 100 cycles compared to SnCo/PVP-CNFs (capacity retention, 71.9%; SEI layer thickness, 593 nm). This work verifies that the thermal behavior of carbon precursor is highly responsible for the growth mechanism of SEI layer accompanied with particles detachment and cyclability of alloy particle embedded CNFs.
A comparison investigation of optical, structural and luminescence properties of CdOxTe1-x and CdTexSe1-x nanoparticles prepared by a simple one pot method

NASA Astrophysics Data System (ADS)

Kiprotich, Sharon; Onani, Martin O.; Dejene, Francis B.

2018-04-01

We present L-cysteine capped CdOXTe1-X and CdTeXSe1-X nanoparticles (NPs) prepared in one pot. The as-prepared CdOXTe1-X NPs were found to have a hexagonal crystal structure of CdTe with a cubic phase of CdO. There was, however, change in phase to cubic type when 2 mM of Se was introduced into the CdTe at 60 min of reaction time. The average crystallite sizes obtained from X-ray diffraction analysis for CdOXTe1-X and CdTeXSe1-X NPs were in the range of 10-36 nm. The diffraction peaks shifted to higher diffraction angle with longer growth time. Scanning electron microscope images display change in shape and size as reaction progress. Photoluminescence (PL) emission was observed to shift from 510-566 nm and 620-653 nm for CdOXTe1-X and CdTeXSe1-X NPs respectively followed by variation in the peak intensities. The emission spectra displayed a good symmetry and a narrow full width at half maximum ranging from 41 to 100 nm in both cases. The absorbance analysis of the as-prepared NPs displayed well-resolved absorption bands. The optical band gaps of the as-prepared NPs were found to decrease with increase in reaction time. Reaction parameters such as pH, reaction time, reaction temperature and the molar concentration could have major effects on the optical properties of the as-prepared nanoparticles hence their need to control them.
Structural and Magnetic Properties of Dilute Ca²⁺ Doped Iron Oxide Nanoparticles.

PubMed

Samar Layek; Rout, K; Mohapatra, M; Anand, S; Verma, H C

2016-01-01

Undoped and calcium substituted hematite (α-Fe₂O₃) nanoparticles are synthesized by surfactant-directed co-precipitation and post annealing method. The annealed nanoparticles were found to be in single phase in nature and crystallize in the rhombohedral structure with space group R3c as confirmed by Rietveld refinement of the X-ray diffraction (XRD) data. Average crystallite sizes are calculated to be 20 to 30 nm and 50 to 60 nm for the nanoparticles annealed at 400 and 600 °C respectively. Mössbauer spectra for all the nanoparticles could be fitted with a sextet corresponding to the single magnetic state of the iron atoms in its Fe³⁺ state in the hematite matrix. The FTIR and Raman spectra of all the samples correspond to specific modes of α-Fe₂O₃. UV-Vis spectra of annealed samples showed broad peaks in the range of 525-630 nm resulting from spin-forbidden ligand field transition together with the spin-flip transition among the 2t₂g states. The estimated band gap energies were in the range of 1.6 to 1.9 eV which are much lower than the reported values for nano hematite. From the room temperature magnetic hysteresis loop measurements, weak ferromagnetic behavior is observed in all undoped and Ca²⁺ doped hematite samples. Morin temperature (T(M)) is calculated to be 257 and 237 K for 1.45% doped samples with particle size 54 and 27 nm respectively. The sample with Ca content of 1.45 wt% when annealed at 400 °C showed that the particles were of different shapes which included both quasi spherical and rod shaped. On annealing the same sample at 600 °C, the nanorods collapsed to form bigger spherical and ellipsoidal particles.
Low temperature synthesis and enhanced electrical properties by substitution of Al3+ and Cr3+ in Co-Ni nanoferrites

NASA Astrophysics Data System (ADS)

Pervaiz, Erum; Gul, I. H.

2013-10-01

Aluminum and chromium substituted Co-Ni spinel nanoferrites were prepared by sol-gel auto combustion method. Structural parameters along with electrical and magnetic properties have been investigated in the present work. Crystallite sizes of nano ferrite estimated from the peak (311) lies in the range of 13-21 nm ±2 nm and compared with crystallite sizes calculated from Williamsons-Hall plots. DC electrical resistivity variations due to the concentration of aluminum and chromium in the host ferrite have been measured from 368 K to 573 K. Increase in the room temperature DC electrical resistivity was observed up to a concentration x=0.2 and then decreases for x >0.2. Dielectric parameters (real and imaginary part of complex permittivity, dielectric loss tangent) were studied as a function of frequency (20 Hz-5 MHz) and a decrease in the dielectric parameters was observed due to substitution of nickel, aluminum and chromium ions in cobalt nanoferrites. AC conductivity, complex impedance and complex electrical modulus were studied as a function of frequency for the conduction and relaxation mechanisms in the present ferrite system. Saturation magnetization, coercivity, canting angles and magneto crystalline anisotropy variations with composition were observed and presented for the present ferrites under an applied magnetic field of 10 kOe at room temperature. It was found that both magnetization and coercivity decreases with increase in the concentration of aluminum and chromium along with a decrease in the anisotropy parameters. High DC resistivity with low dielectric parameters of the present nanoferrites make them suitable for high frequency and electromagnetic wave absorbing devices. High purity mixed Co-Ni-Al-Cr nanoferrites have been prepared by sol-gel auto combustion method. DC electrical resistivity increases due to substitution of Al3+ and Cr3+. Complex permittivity decrease for Co-Ni-Al-Cr nanoferrites. Detailed AC response analysis has been presented for mixed Co-Ni-Al-Cr nanoferrites. Magnetization and coercively reduces for Al3+ and Cr3+ doped Co-Ni ferrite nanoparticles showing that material is becoming soft magnetic.
Synthesis, characterization and photocatalytic properties of Mg1-xZnxAl2O4 spinel nanoparticles

NASA Astrophysics Data System (ADS)

Li, Hui; Liu, Yuqin; Tang, Junkai; Deng, Yanxi

2016-08-01

Mg1-xZnxAl2O4 spinel nanoparticles with x = 0, 0.05, 0.10, 0.15 and 0.20 were prepared via the chemical coprecipitation method. The obtained samples were characterised by thermal gravimetric and differential scanning calorimetry, X-ray diffraction, Fourier transform infrared spectroscopy, UV-Vis diffuse reflection spectrum, transmission electron microscopy and 27Al MAS-NMR spectroscopy. Mg1-xZnxAl2O4 spinel powders with the mean crystallite size of around 11 nm-14 nm were obtained. The crystallinity of the MgAl2O4 samples increases with the increase in the calcination temperature. At the same calcination temperature, higher amount of Zn2+ substitution leads to the higher level of crystallinity, but has no apparent influence on the mean crystallite size of the samples. The photocatalytic activity of the obtained Mg1-xZnxAl2O4 spinel nanoparticles was evaluated by monitoring the degradation of methylene blue under UV light. The degradation rates of methylene blue using the MgAl2O4 nanoparticles prepared at the calcination temperatures of 700 °C and 800 °C are much higher than those prepared at 900 °C and 1000 °C. The photocatalytic activities of the spinel powders with lower level of Zn2+ substitution such as Mg0.95Zn0.05Al2O4 are inferior to that of MgAl2O4. Results of 27Al MAS-NMR spectroscopy analysis and the first principle total density of state calculations reveal that this is probably due to the substitutions of Zn2+ decreasing the degree of Al3+ ions inversion over the sites of tetrahedral and octahedral coordination. With the increase in the amounts of Zn2+ substitution, the effects of Zn2+ additions on the photocatalytic activities become gradually predominant, leading to the increases in the degradation rates. The methylene blue degraded by 99% within 4 h using the Mg0.8Zn0.2Al2O4 spinel powders.
Effect of electrode material on characteristics of non-volatile resistive memory consisting of Ag{sub 2}S nanoparticles

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

Jang, Jaewon, E-mail: j1jang@knu.ac.kr

2016-07-15

In this study, Ag{sub 2}S nanoparticles are synthesized and used as the active material for two-terminal resistance switching memory devices. Sintered Ag{sub 2}S films are successfully crystallized on plastic substrates with synthesized Ag{sub 2}S nanoparticles, after a relatively low-temperature sintering process (200 °C). After the sintering process, the crystallite size is increased from 6.8 nm to 80.3 nm. The high ratio of surface atoms to inner atoms of nanoparticles reduces the melting point temperature, deciding the sintering process temperature. In order to investigate the resistance switching characteristics, metal/Ag{sub 2}S/metal structures are fabricated and tested. The effect of the electrode materialmore » on the non-volatile resistive memory characteristics is studied. The bottom electrochemically inert materials, such as Au and Pt, were critical for maintaining stable memory characteristics. By using Au and Pt inert bottom electrodes, we are able to significantly improve the memory endurance and retention to more than 10{sup 3} cycles and 10{sup 4} sec, respectively.« less
Pulsed UV laser-induced modifications in optical and structural characteristics of alpha-irradiated PM-355 SSNTD.

PubMed

Alghamdi, S S; Farooq, W A; Baig, M R; Algarawi, M S; Alrashidi, Talal Mohammed; Ali, Syed Mansoor; Alfaramawi, K

2017-10-01

Pre- and postalpha-exposed PM-355 detectors were irradiated using UV laser with different number of pulses (100, 150, 200, 300, and 400). UV laser beam energy of 20mJ per pulse with a pulse width of 9ns was incident on an area of 19.6mm 2 of the samples. XRD spectra indicated that for both reference and UV-irradiated samples, the structure is amorphous, but the crystallite size increases upon UV irradiation. The same results were obtained from SEM analysis. Optical properties of PM-355 polymeric solid-state nuclear track detectors were also investigated. Absorbance measurements for all PM-355 samples in the range of 200-400nm showed that the absorption edge had a blue shift up to a certain value, and then, it had an oscillating behavior. Photoluminescence spectra of PM-355 at 250nm revealed a decrease in the broadband peak intensity as a function of the number of UV pulses, while the wavelengths corresponding to the peaks had random shifts. Copyright © 2017 Elsevier Ltd. All rights reserved.
Structural and optical properties of chromium doped zinc oxide nanoparticles synthesized by sol-gel method

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

Naqvi, Syed Mohd. Adnan, E-mail: adiaks2004@yahoo.co.in; Irshad, Kashif, E-mail: alig.kashif@gmail.com; Soleimani, Hassan, E-mail: hassan.soleimani@petronas.com.my, E-mail: noorhana-yahya@petronas.com.my

2014-10-24

Nanosized Cr-doped ZnO nano particles were synthesized by facile sol-gel auto combustion method. The structural and optical properties of Cr-doped ZnO nanoparticles have been investigated by XRD and UV-Vis spectroscopy at room temperature for 0% to 8% concentration. X-ray diffraction analysis reveals that the Cr-doped ZnO crystallizes in a single phase polycrystalline nature with wurtzite lattice. With every % of doping, the peaks are shifting scarcely and doping of Cr is possible up to 7%. After that, the last peak vanishes, that signifies its structure is transmuted from 8% doping. The average crystallite size decreases with increase in Cr concentrationmore » (i.e. 28.9 nm for 0% to 25.8 nm for 8%). The UV-Vis spectra of the nanoparticles betoken an incrementation in the band gap energy from 3.401, 3.415, 3.431, 3.437,3.453, 3.514,3.521, 3.530 and 3.538 eV respectively, for 0,1, 2, 3, 4, 5, 6, 7 and 8 % doping concentration.« less
A Fast Responsive Ultraviolet Sensor from mSILAR-Processed Sn-ZnO

NASA Astrophysics Data System (ADS)

Thomas, Deepu; Vijayalakshmi, K. A.; Sadasivuni, Kishor Kumar; Thomas, Ajith; Ponnamma, Deepalekshmi; Cabibihan, John-John

2017-11-01

Microwave-assisted successive ionic layer adsorption and reaction was employed to synthesize Sn-ZnO (tin-doped zinc oxide), and its sensitivity to ultraviolet radiation is compared with zinc oxide (ZnO). The sensing films were made by the dip-coated method on an indium titanium oxide glass substrate, and the sensing performance was monitored using the 300-700 nm wavelength of UV-Vis light. Excellent sensitivity and recovery were observed for the Sn-doped ZnO sensor device, especially at 380 nm wavelength of ultraviolet (UV) light (response and recovery time 2.26 s and 8.63 s, respectively, at 5 V bias voltage). The variation in photocurrent with respect to dark and light illumination atmosphere was well illustrated based on the Schottky and inter-particle network effects. Doping of Sn on ZnO nanoparticles varied the surface roughness and crystallite size as observed from scanning electron microscopic and x-ray diffraction studies. Here, we demonstrate a simple and economical fabrication technique for designing a high-performance UV light sensor. The developed device works at room temperature with high durability and stability.
Fabrication of microporous calcite block from calcium hydroxide compact under carbon dioxide atmosphere at high temperature.

PubMed

Otsu, Akihiro; Tsuru, Kanji; Maruta, Michito; Munar, Melvin L; Matsuya, Shigeki; Ishikawa, Kunio

2012-01-01

Effects of carbonation temperature and compacting pressure on basic properties of calcite block were studied using Ca(OH)2 compact made with 0.2-2.0 MPa and their carbonation at 200-800ºC for 1 h. Microporous calcite was obtained only when carbonated at 600ºC using Ca(OH)2 compact made with 0.2 MPa even though thermogravimetry analysis showed that calcite powder was stable up to 920ºC under CO2 atmosphere. CaO formed by carbonation at 700ºC and 800ºC is thought to be caused by the limited CO2 diffusion interior to the Ca(OH)2 compact. Also, unreacted Ca(OH)2 was found for Ca(OH)2 compact prepared with 0.5 MPa or higher pressure even when carbonated at 600ºC. As a result of high temperature carbonation, crystallite size of the calcite, 58.0 nm, was significantly larger when compared to that of calcite prepared at room temperature, 35.5 nm. Porosity and diametral tensile strength of the microporous calcite were 39.5% and 6.4 MPa.

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