Commenced in January 2007
Frequency: Monthly
Edition: International
Paper Count: 6821

Search results for: low temperature luminescence spectroscopy

6821 Low-Temperature Luminescence Spectroscopy of Violet Sr-Al-O:Eu2+ Phosphor Particles

Authors: Keiji Komatsu, Hayato Maruyama, Ariyuki Kato, Atsushi Nakamura, Shigeo Ohshio, Hiroki Akasaka, Hidetoshi Saitoh


Violet Sr–Al–O:Eu2+ phosphor particles were synthesized from a metal–ethylenediaminetetraacetic acid (EDTA) solution of Sr, Al, Eu, and particulate alumina via spray drying and sintering in a reducing atmosphere. The crystal structures and emission properties at 85–300 K were investigated. The composition of the violet Sr–Al–O:Eu2+ phosphor particles was determined from various Sr–Al–O:Eu2+ phosphors by their emission properties’ dependence on temperature. The highly crystalline SrAl12O19:Eu2+ emission phases were confirmed by their crystallite sizes and the activation energies for the 4f5d–8S7/2 transition of the Eu2+ ion. These results showed that the material identification for the violet Sr–Al–O:Eu2+ phosphor was accomplished by the low-temperature luminescence measurements.

Keywords: low temperature luminescence spectroscopy, material identification, strontium aluminates phosphor, emission properties

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6820 Silver Nanoparticles-Enhanced Luminescence Spectra of Silicon Nanocrystals

Authors: Khamael M. Abualnaja, Lidija Šiller, Benjamin R. Horrocks


Metal-enhanced luminescence of silicon nano crystals (SiNCs) was determined using two different particle sizes of silver nano particles (AgNPs). SiNCs have been characterized by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR) and X-ray photo electron spectroscopy (XPS). It is found that the SiNCs are crystalline with an average diameter of 65 nm and FCC lattice. AgNPs were synthesized using photochemical reduction of AgNO3 with sodium dodecyl sulphate (SDS). The enhanced luminescence of SiNCs by AgNPs was evaluated by confocal Raman microspectroscopy. Enhancement up to ×9 and ×3 times were observed for SiNCs that mixed with AgNPs which have an average particle size of 100 nm and 30 nm, respectively. Silver NPs-enhanced luminescence of SiNCs occurs as a result of the coupling between the excitation laser light and the plasmon bands of AgNPs; thus this intense field at AgNPs surface couples strongly to SiNCs.

Keywords: silver nanoparticles, surface enhanced raman spectroscopy (SERS), silicon nanocrystals, luminescence

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6819 Application of Laser Spectroscopy for Detection of Actinides and Lanthanides in Solutions

Authors: Igor Izosimov


This work is devoted to applications of the Time-resolved laser-induced luminescence (TRLIF) spectroscopy and time-resolved laser-induced chemiluminescence spectroscopy for detection of lanthanides and actinides. Results of the experiments on Eu, Sm, U, and Pu detection in solutions are presented. The limit of uranyl detection (LOD) in urine in our TRLIF experiments was up to 5 pg/ml. In blood plasma LOD was 0.1 ng/ml and after mineralization was up to 8pg/ml – 10pg/ml. In pure solution, the limit of detection of europium was 0.005ng/ml and samarium, 0.07ng/ml. After addition urine, the limit of detection of europium was 0.015 ng/ml and samarium, 0.2 ng/ml. Pu, Np, and some U compounds do not produce direct luminescence in solutions, but when excited by laser radiation, they can induce chemiluminescence of some chemiluminogen (luminol in our experiments). It is shown that multi-photon scheme of chemiluminescence excitation makes chemiluminescence not only a highly sensitive but also a highly selective tool for the detection of lanthanides/actinides in solutions.

Keywords: actinides/lanthanides detection, laser spectroscopy with time resolution, luminescence/chemiluminescence, solutions

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6818 Scientific Investigation for an Ancient Egyptian Polychrome Wooden Stele

Authors: Ahmed Abdrabou, Medhat Abdalla


The studied stele dates back to Third Intermediate Period (1075-664) B.C in an ancient Egypt. It is made of wood and covered with painted gesso layers. This study aims to use a combination of multi spectral imaging {visible, infrared (IR), Visible-induced infrared luminescence (VIL), Visible-induced ultraviolet luminescence (UVL) and ultraviolet reflected (UVR)}, along with portable x-ray fluorescence in order to map and identify the pigments as well as to provide a deeper understanding of the painting techniques. Moreover; the authors were significantly interested in the identification of wood species. Multispectral imaging acquired in 3 spectral bands, ultraviolet (360-400 nm), visible (400-780 nm) and infrared (780-1100 nm) using (UV Ultraviolet-induced luminescence (UVL), UV Reflected (UVR), Visible (VIS), Visible-induced infrared luminescence (VIL) and Infrared photography. False color images are made by digitally editing the VIS with IR or UV images using Adobe Photoshop. Optical Microscopy (OM), potable X-ray fluorescence spectroscopy (p-XRF) and Fourier Transform Infrared Spectroscopy (FTIR) were used in this study. Mapping and imaging techniques provided useful information about the spatial distribution of pigments, in particular visible-induced luminescence (VIL) which allowed the spatial distribution of Egyptian blue pigment to be mapped and every region containing Egyptian blue, even down to single crystals in some instances, is clearly visible as a bright white area; however complete characterization of the pigments requires the use of p. XRF spectroscopy. Based on the elemental analysis found by P.XRF, we conclude that the artists used mixtures of the basic mineral pigments to achieve a wider palette of hues. Identification of wood species Microscopic identification indicated that the wood used was Sycamore Fig (Ficus sycomorus L.) which is recorded as being native to Egypt and was used to make wooden artifacts since at least the Fifth Dynasty.

Keywords: polychrome wooden stele, multispectral imaging, IR luminescence, Wood identification, Sycamore Fig, p-XRF

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6817 Photoluminescence Spectroscopy to Probe Mixed Valence State in Eu-Doped Nanocrystalline Glass-Ceramics

Authors: Ruchika Bagga, Mauro Falconieri, Venu Gopal Achanta, José M. F. Ferreira, Ashutosh Goel, Gopi Sharma


Mixed valence Eu-doped nanocrystalline NaAlSiO4/NaY9Si6O26 glass-ceramics have been prepared by controlled crystallization of melt quenched bulk glasses. XRD and SEM techniques were employed to characterize the crystallization process of the precursor glass and their resultant glass-ceramics. Photoluminescence spectroscopy was used to analyze the formation of divalent europium (Eu2+) from Eu3+ ions during high temperature synthesis under ambient atmosphere and is explained on the basis of optical basicity model. The observed luminescence properties of Eu: NaY9Si6O26 are compared with that of well explored Eu: β-PbF2 nanocrystals and their marked differences are discussed.

Keywords: rare earth, oxyfluoride glasses, nano-crystalline glass-ceramics, photoluminescence spectroscopy

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6816 Structure and Optical Properties of Potassium Doped Zinc Oxide

Authors: Lila A. Alkhattaby, Norah A. Alsayegh, Mohammad S. Ansari, Mohammad O. Ansari


In this work, we doped zinc oxide ZnO with potassium K we have synthesized using the sol-gel method. Structural properties were depicted by X-ray diffractometer (XRD) and energy distribution spectroscopy, X-ray diffraction studies confirm the nanosized of the particles and favored orientations along the (100), (002), (101), (102), (110), (103), (200), and (112) planes confirm the hexagonal wurtzite structure of ZnO NPs. The optical properties study using the UV-Vis spectroscopy. The band gap decreases from 4.05 eV to 3.88 eV, the lowest band gap at 10% doped concentration. The photoluminescence (PL) spectroscopy results show two main peaks, a sharp peak at ≈ 384 nm in the UV region and a broad peak around 479 nm in the visible region. The highest intensity of the band-edge luminescence was for 2% doped concentration because of the combined effect of the decreased probability of nonradiative recombination and has better crystallinity.

Keywords: K doped ZnO, photoluminescence spectroscopy, UV-Vis spectroscopy, x-ray spectroscopy

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6815 Sol-Gel Erbium-Doped Silica-Hafnia Planar Waveguides

Authors: Mustapha El Mataouy, Abellatif Aaliti, Mouhamed Khaddor


Erbium actived silica-hafnia planar waveguides have been prepared by sol-gel route. The films were deposited on vitreous silica substrates using dip-coating technique. The parameters of preparation have been chosen to optimize the waveguides for operation in the near infrared (NIR) region, and to increase the luminescence efficiency of the metastable 4I13/2 state of Erbium ions. The waveguides properties were determined by m-lines spectroscopy, loss measurements. Waveguide Raman and luminescence spectroscopy were used to obtain information about the structure of the prepared films and about the dynamical process related to the emission in the C telecom band (1530nm-1565nm) of the Erbium ions. The results are discussed with the aim of comparing the structural and optical properties of Erbium activated silica-hafnia planar waveguides with different molar ratio of Si / Hf.

Keywords: erbium, optical amplifiers, silica-hafnia, sol-gel, waveguide

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6814 Enhancing the Luminescence of Alkyl-Capped Silicon Quantum Dots by Using Metal Nanoparticles

Authors: Khamael M. Abualnaja, Lidija Šiller, Ben R. Horrocks


Metal enhanced luminescence of alkyl-capped silicon quantum dots (C11-SiQDs) was obtained by mixing C11-SiQDs with silver nanoparticles (AgNPs). C11-SiQDs have been synthesized by galvanostatic method of p-Si (100) wafers followed by a thermal hydrosilation reaction of 1-undecene in refluxing toluene in order to extract alkyl-capped silicon quantum dots from porous Si. The chemical characterization of C11-SiQDs was carried out using X-ray photoemission spectroscopy (XPS). C11-SiQDs have a crystalline structure with a diameter of 5 nm. Silver nanoparticles (AgNPs) of two different sizes were synthesized also using photochemical reduction of silver nitrate with sodium dodecyl sulphate. The synthesized Ag nanoparticles have a polycrystalline structure with an average particle diameter of 100 nm and 30 nm, respectively. A significant enhancement up to 10 and 4 times in the luminescence intensities was observed for AgNPs100/C11-SiQDs and AgNPs30/C11-SiQDs mixtures, respectively using 488 nm as an excitation source. The enhancement in luminescence intensities occurs as a result of the coupling between the excitation laser light and the plasmon bands of Ag nanoparticles; thus this intense field at Ag nanoparticles surface couples strongly to C11-SiQDs. The results suggest that the larger Ag nanoparticles i.e.100 nm caused an optimum enhancement in the luminescence intensity of C11-SiQDs which reflect the strong interaction between the localized surface plasmon resonance of AgNPs and the electric field forming a strong polarization near C11-SiQDs.

Keywords: silicon quantum dots, silver nanoparticles (AgNPs), luminescence, plasmon

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6813 Study on Concentration and Temperature Measurement with 760 nm Diode Laser in Combustion System Using Tunable Diode Laser Absorption Spectroscopy

Authors: Miyeon Yoo, Sewon Kim, Changyeop Lee


It is important to measure the internal temperature or temperature distribution precisely in combustion system to increase energy efficiency and reduce the pollutants. Especially in case of large combustion systems such as power plant boiler and reheating furnace of steel making process, it is very difficult to measure those physical properties in detail. Tunable diode laser absorption spectroscopy measurement and analysis can be attractive method to overcome the difficulty. In this paper, TDLAS methods are used to measure the oxygen concentration and temperature distribution in various experimental conditions.

Keywords: tunable diode laser absorption Spectroscopy, temperature distribution, gas concentration

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6812 Optical Properties of Nanocrystalline Europium-Yttrium Titanate EuYTi2O7

Authors: J. Mrazek, R. Skala, S. Bysakh, Ivan Kasik


Lanthanide-doped yttrium titanium oxides, which crystallize in a pyrochlore structure with general formula (RExY1-x)2Ti2O7 (RE=rare earth element), have been extensively investigated in recent years for their interesting physical and chemical properties. Despite that the pure pyrochlore structure does not present luminescence ability, the presence of yttrium ions in the pyrochlore structure significantly improves the luminescence properties of the RE. Moreover, the luminescence properties of pyrochlores strongly depend on the size of formed nanocrystals. In this contribution, we present a versatile sol-gel synthesis of nanocrystalline EuYTi2O7pyrochlore. The nanocrystalline powders and thin films were prepared by the condensation of titanium(IV)butoxide with europium(III) chloride followed by the calcination. The introduced method leads to the formation of the highly-homogenous nanocrystalline EuYTi2O7 with tailored grain size ranging from 20 nm to 200 nm. The morphology and the structure of the formed nanocrystals are linked to the luminescence properties of Eu3+ ions incorporated into the pyrochlore lattice. The results of XRD and HRTEM analysis show that the Eu3+ and Y3+ ions are regularly distributed inside the lattice. The lifetime of Eu3+ ions in calcinated powders is regularly decreasing from 140 us to 68 us and the refractive index of prepared thin films regularly increases from 2.0 to 2.45 according to the calcination temperature. The shape of the luminescence spectra and the decrease of the lifetime correspond with the crystallinity of prepared powders. The results present fundamental information about the effect of the size of the nanocrystals to their luminescence properties. The promising application of prepared nanocrystals in the field of lasers and planar optical amplifiers is widely discussed in the contribution.

Keywords: europium, luminescence, nanocrystals, sol-gel

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6811 Synthesis of KCaVO4:Sm³⁺/PMMA Luminescent Nanocomposites and Their Optical Property Measurements

Authors: Sumara Khursheed, Jitendra Sharma


The present work reports synthesis of nanocomposites (NCs) of phosphor (KCaVO4:Sm3+) embedded poly(methylmethacrylate) (PMMA) using solution casting method and their optical properties measurements for their possible application in making flexible luminescent films. X-ray diffraction analyses were employed to obtain the structural parameters as crystallinity, shape and size of the obtained NCs. The emission and excitation spectra were obtained using Photoluminescence spectroscopy to quantify the spectral properties of these fluorescent polymer/phosphor films. Optical energy gap has been estimated using UV-VIS spectroscopy while differential scanning calorimetry (DSC) was exploited to measure the thermal properties of the NC films in terms of their thermal stability, glass transition temperature and degree of crystallinity etc.

Keywords: nanocomposites, luminescence, XRD, differential scanning calorimetry, PMMA

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6810 Unconventional Dating of Old Peepal Tree of Chandigarh (India) Using Optically Stimulated Luminescence

Authors: Rita Rani, Ramesh Kumar


The intend of the current study is to date an old grand Peepal tree that is still alive. The tree is situated in Kalibard village, Sector 9, Chandigarh (India). Due to its huge structure, it has got the status of ‘Heritage tree.’ Optically Stimulated Luminescence of sediments beneath the roots is used to determine the age of the tree. Optical dating is preferred over conventional dating methods due to more precession. The methodology includes OSL of quartz grain using SAR protocol for accumulated dose measurement. The age determination of an alive tree using sedimentary quartz is in close agreement with the approximated age provided by the related agency. This is the first attempt at using optically stimulated luminescence in the age determination of alive trees in this region. The study concludes that the Luminescence dating of alive trees is the nondestructive and more precise method.

Keywords: luminescence, dose rate, optical dating, sediments

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6809 Effect of Preparation Temperature on Producing Graphene Oxide by Chemical Oxidation Approach

Authors: Rashad Al-Gaashani, Muataz A. Atieh


In this study, the effect of preparation temperature, namely room temperature (RT), 40, 60, and 85°C, on producing of high-quality graphene oxide (GO) has been investigated. GO samples have been prepared by chemical oxidation of graphite via a safe improved chemical technique using a blend of two deferent acids: sulphuric acid (H₂SO₄) and phosphoric acid (H₃PO₄) with volume ratio 4:1, respectively. potassium permanganate (KMnO₄) and hydrogen peroxide (H₂O₂) were applied as oxidizing agents. In this work, sodium nitrate (NaNO₃) was excluded, so the emission of hazardous explosive gases such as NO₂ and N₂O₂ was shunned. Ice and oil baths were used to carefully control the temperature. Several characterization instruments including X-Ray diffraction, transmission electron microscopy, scanning electron microscopy, electron dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and UV-vis spectroscopy were used to study and compare the synthesized samples. The results indicated that GO can be prepared at RT with graphite oxide, and the purity of GO increased with rising of the solvent temperature. Optical properties of GO samples were studied using UV-vis absorption spectra.

Keywords: chemical method, graphite, graphene oxide, optical properties

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6808 Synthesis and Surface Engineering of Lanthanide Nanoparticles for NIR Luminescence Imaging and Photodynamic Therapy

Authors: Syue-Liang Lin, C. Allen Chang


Luminescence imaging is an important technique used in biomedical research and clinical diagnostic applications in recent years. Concurrently, the development of NIR luminescence probes / imaging contrast agents has helped the understanding of the structural and functional properties of cells and animals. Photodynamic therapy (PDT) is used clinically to treat a wide range of medical conditions, but the therapeutic efficacy of general PDT for deeper tumor was limited by the penetration of excitation source. The tumor targeting biomedical nanomaterials [email protected] (upconversion nanoparticle conjugated with photosensitizer) for photodynamic therapy and near-infrared imaging of cancer will be developed in our study. Synthesis and characterization of biomedical nanomaterials were completed in this studies. The spectrum of UCNP was characterized by photoluminescence spectroscopy and the morphology was characterized by Transmission Electron Microscope (TEM). TEM and XRD analyses indicated that these nanoparticles are about 20~50 nm with hexagonal phase. NaYF₄:Ln³⁺ (Ln= Yb, Nd, Er) upconversion nanoparticles (UCNPs) with core / shell structure, synthesized by thermal decomposition method in 300°C, have the ability to emit visible light (upconversion: 540 nm, 660 nm) and near-infrared with longer wavelength (downconversion: NIR: 980 nm, 1525 nm) by absorbing 800 nm NIR laser. The information obtained from these studies would be very useful for applications of these nanomaterials for bio-luminescence imaging and photodynamic therapy of deep tumor tissue in the future.

Keywords: Near Infrared (NIR), lanthanide, core-shell structure, upconversion, theranostics

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6807 Temperature Dependence of Photoluminescence Intensity of Europium Dinuclear Complex

Authors: Kwedi L. M. Nsah, Hisao Uchiki


Quantum computation is a new and exciting field making use of quantum mechanical phenomena. In classical computers, information is represented as bits, with values either 0 or 1, but a quantum computer uses quantum bits in an arbitrary superposition of 0 and 1, enabling it to reach beyond the limits predicted by classical information theory. lanthanide ion quantum computer is an organic crystal, having a lanthanide ion. Europium is a favored lanthanide, since it exhibits nuclear spin coherence times, and Eu(III) is photo-stable and has two stable isotopes. In a europium organic crystal, the key factor is the mutual dipole-dipole interaction between two europium atoms. Crystals of the complex were formed by making a 2 :1 reaction of Eu(fod)3 and bpm. The transparent white crystals formed showed brilliant red luminescence with a 405 nm laser. The photoluminescence spectroscopy was observed both at room and cryogenic temperatures (300-14 K). The luminescence spectrum of [Eu(fod)3(μ-bpm) Eu(fod)3] showed characteristic of Eu(III) emission transitions in the range 570–630 nm, due to the deactivation of 5D0 emissive state to 7Fj. For the application of dinuclear Eu3+ complex to q-bit device, attention was focused on 5D0 -7F0 transition, around 580 nm. The presence of 5D0 -7F0 transition at room temperature revealed that at least one europium symmetry had no inversion center. Since the line was unsplit by the crystal field effect, any multiplicity observed was due to a multiplicity of Eu3+ sites. For q-bit element, more narrow line width of 5D0 → 7F0 PL band in Eu3+ ion was preferable. Cryogenic temperatures (300 K – 14 K) was applicable to reduce inhomogeneous broadening and distinguish between ions. A CCD image sensor was used for low temperature Photoluminescence measurement, and a far better resolved luminescent spectrum was gotten by cooling the complex at 14 K. A red shift by 15 cm-1 in the 5D0 - 7F0 peak position was observed upon cooling, the line shifted towards lower wavenumber. An emission spectrum at the 5D0 - 7F0 transition region was obtained to verify the line width. At this temperature, a peak with magnitude three times that at room temperature was observed. The temperature change of the 5D0 state of Eu(fod)3(μ-bpm)Eu(fod)3 showed a strong dependence in the vicinity of 60 K to 100 K. Thermal quenching was observed at higher temperatures than 100 K, at which point it began to decrease slowly with increasing temperature. The temperature quenching effect of Eu3+ with increase temperature was caused by energy migration. 100 K was the appropriate temperature for the observation of the 5D0 - 7F0 emission peak. Europium dinuclear complex bridged by bpm was successfully prepared and monitored at cryogenic temperatures. At 100 K the Eu3+-dope complex has a good thermal stability and this temperature is appropriate for the observation of the 5D0 - 7F0 emission peak. Sintering the sample above 600o C could also be a method to consider but the Eu3+ ion can be reduced to Eu2+, reasons why cryogenic temperature measurement is preferably over other methods.

Keywords: Eu(fod)₃, europium dinuclear complex, europium ion, quantum bit, quantum computer, 2, 2-bipyrimidine

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6806 The Inversion of Helical Twist Sense in Liquid Crystal by Spectroscopy Methods

Authors: Anna Drzewicz, Marzena Tykarska


The chiral liquid crystal phases form the helicoidal structure, which is characterized by the helical pitch and the helical twist sense. In anticlinic smectic phase with antiferroelectric properties three types of helix temperature dependence have been obtained: increased helical pitch with temperature and right-handed helix, decreased helical pitch with temperature and left-handed helix and the inversion of both. The change of helical twist sense may be observed during the transition from one liquid crystal phase to another or within one phase for the same substance. According to Gray and McDonnell theory, the helical handedness depends on the absolute configuration of the assymetric carbon atom and its position related to the rigid core of the molecule. However, this theory does not explain the inversion of helical twist sense phenomenon. It is supposed, that it may be caused by the presence of different conformers with opposite handendess, which concentration may change with temperature. In this work, the inversion of helical twist sense in the chiral liquid crystals differing in the length of alkyl chain, in the substitution the benzene ring by fluorine atoms and in the type of helix handedness was tested by vibrational spectroscopy (infrared and raman spectroscopy) and by nuclear magnetic resonance spectroscopy. The results obtained from the vibrational spectroscopy confirm the presence of different conformers. Moreover, the analysis of nuclear magnetic resonance spectra is very useful to check, on which structural fragments the change of conformations are important for the change of helical twist sense.

Keywords: helical twist sense, liquid crystals, nuclear magnetic resonance spectroscopy, vibrational spectroscopy

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6805 Dielectric, Energy Storage and Impedance Spectroscopic Studies of Tin Doped Ba₀.₉₈Ca₀.₀₂TiO₃ Lead-Free Ceramics

Authors: Ramovatar, Neeraj Panwar


Lead free Ba₀.₉₈Ca₀.₀₂SnxTi₁₋ₓO₃ (x = 0.01 and 0.05 mole %) ferroelectric ceramics have been synthesized by the solid-state reaction method with sintering at 1400 °C for 2 h. The room temperature x-ray diffraction (XRD) patterns identified the tetragonal phase for x = 0.01 composition whereas co-existence of tetragonal and orthorhombic phases for x =0.05 composition. Raman spectroscopy results corroborated with the XRD results at room temperature. The maximum dielectric properties (ɛm ~ 8591, tanδ ~ 0.018) were obtained for the compound with x = 0.01 at 5 kHz. Further, the tetragonal to cubic (TC) transition temperature was observed at 122 °C and 102 °C for the ceramics with x =0.01 and x = 0.05, respectively. The temperature dependent P-E loops also revealed the existence of TC at these particular temperature values. The energy storage density (Ed) of both compounds was calculated from room temperature P – E loops at an applied electric field of 20 kV/cm. The maximum Ed ~ 224 kJ/m³ was achieved for the sample with x = 0.01 as compared to 164 kJ/m³ for the x =0.05 composition. The value of Ed is comparable to other BaTiO₃ based lead free ferroelectric systems. Impedance spectroscopy analysis exhibited the bulk and grain boundary contributions above 300 °C under the frequency range 100 Hz to 1 MHz. The above properties make these ceramics suitable for energy storage devices.

Keywords: dielectric properties, energy storage properties, impedance spectroscopy, lead free ceramics

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6804 Two-Photon Fluorescence in N-Doped Graphene Quantum Dots

Authors: Chi Man Luk, Ming Kiu Tsang, Chi Fan Chan, Shu Ping Lau


Nitrogen-doped graphene quantum dots (N-GQDs) were fabricated by microwave-assisted hydrothermal technique. The optical properties of the N-GQDs were studied. The luminescence of the N-GQDs can be tuned by varying the excitation wavelength. Furthermore, two-photon luminescence of the N-GQDs excited by near-infrared laser can be obtained. It is shown that N-doping play a key role on two-photon luminescence. The N-GQDs are expected to find application in biological applications including bioimaging and sensing.

Keywords: graphene quantum dots, nitrogen doping, photoluminescence, two-photon fluorescence

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6803 Thin Films of Copper Oxide Deposited by Sol-Gel Spin Coating Method: Effect of Annealing Temperature on Structural and Optical Properties

Authors: Touka Nassim, Tabli Dalila


In this study, CuO thin films synthesized via simple sol-gel method, have been deposited on glass substrates by the spin coating technique and annealed at various temperatures. Samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), Fourier-transform infrared (FT-IR) and Raman spectroscopy, and UV-visible spectroscopy. The structural characterization by XRD reveals that the as prepared films were tenorite phase and have a high level of purity and crystallinity. The crystallite size of the CuO films was affected by the annealing temperature and was estimated in the range 20-31.5 nm. SEM images show a homogeneous distribution of spherical nanoparticles over the surface of the annealed films at 350 and 450 °C. Vibrational Spectroscopy revealed vibration modes specific to CuO with monolithic structure on the Raman spectra at 289 cm−1 and on FT-IR spectra around 430-580 cm−1. Electronic investigation performed by UV–Visible spectroscopy showed that the films have high absorbance in the visible region and their optical band gap increases from 2.40 to 2.66 eV (blue shift) with increasing annealing temperature from 350 to 550 °C.

Keywords: Sol-gel, Spin coating method, Copper oxide, Thin films

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6802 In situ High Temperature Characterization of Diamond-Like Carbon Films

Authors: M. Rouhani, F. C. N. Hong, Y. R. Jeng


The tribological performance of DLC films is limited by graphitization at elevated temperatures. Despite of numerous studies on the thermal stability of DLC films, a comprehensive in-situ characterization at elevated temperature is still lacking. In this study, DLC films were deposited using filtered cathodic arc vacuum method. Thermal stability of the films was characterized in-situally using a synchronized technique integrating Raman spectroscopy and depth-sensing measurements. Tests were performed in a high temperature chamber coupled with feedback control to make it possible to study the temperature effects in the range of 21 – 450 ̊C. Co-located SPM and Raman microscopy maps at different temperature over a specific area on the surface of the film were prepared. The results show that the thermal stability of the DLC films depends on their sp3 content. Films with lower sp3 content endure graphitization during the temperature-course used in this study. The graphitization is accompanied with significant changes in surface roughness and Raman spectrum of the film. Surface roughness of the films start to change even before graphitization transformation could be detected using Raman spectroscopy. Depth-sensing tests (nanoindentation, nano-scratch and wear) endorse the surface roughness change seen before graphitization occurrence. This in-situ study showed that the surface of the films is more sensitive to temperature rise compared to the bulk. We presume the changes observed in films hardness, surface roughness and scratch resistance with temperature rise, before graphitization occurrence, is due to surface relaxation.

Keywords: DLC film, nanoindentation, Raman spectroscopy, thermal stability

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6801 Rare-Earth Ions Doped Lithium Niobate Crystals: Luminescence and Raman Spectroscopy

Authors: Ninel Kokanyan, Edvard Kokanyan, Anush Movsesyan, Marc D. Fontana


Lithium Niobate (LN) is one of the widely used ferroelectrics having a wide number of applications such as phase-conjugation, holographic storage, frequency doubling, SAW sensors. Furthermore, the possibility of doping with rare-earth ions leads to new laser applications. Ho and Tm dopants seem interesting due to laser emission obtained at around 2 µm. Raman spectroscopy is a powerful spectroscopic technique providing a possibility to obtain a number of information about physicochemical and also optical properties of a given material. Polarized Raman measurements were carried out on Ho and Tm doped LN crystals with excitation wavelengths of 532nm and 785nm. In obtained Raman anti-Stokes spectra, we detect expected modes according to Raman selection rules. In contrast, Raman Stokes spectra are significantly different compared to what is expected by selection rules. Additional forbidden lines are detected. These lines have quite high intensity and are well defined. Moreover, the intensity of mentioned additional lines increases with an increase of Ho or Tm concentrations in the crystal. These additional lines are attributed to emission lines reflecting the photoluminescence spectra of these crystals. It means that in our case we were able to detect, within a very good resolution, in the same Stokes spectrum, the transitions between the electronic states, and the vibrational states as well. The analysis of these data is reported as a function of Ho and Tm content, for different polarizations and wavelengths, of the incident laser beam. Results also highlight additional information about π and σ polarizations of crystals under study.

Keywords: lithium niobate, Raman spectroscopy, luminescence, rare-earth ions doped lithium niobate

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6800 Structural Investigation of Na2O–B2O3–SiO2 Glasses Doped with NdF3

Authors: M. S. Gaafar, S. Y. Marzouk


Sodium borosilicate glasses doped with different content of NdF3 mol % have been prepared by rapid quenching method. Ultrasonic velocities (both longitudinal and shear) measurements have been carried out at room temperature and at ultrasonic frequency of 4 MHz. Elastic moduli, Debye temperature, softening temperature and Poisson's ratio have been obtained as a function of NdF3 modifier content. Results showed that the elastic moduli, Debye temperature, softening temperature and Poisson's ratio have very slight change with the change of NdF3 mol % content. Based on FTIR spectroscopy and theoretical (Bond compression) model, quantitative analysis has been carried out in order to obtain more information about the structure of these glasses. The study indicated that the structure of these glasses is mainly composed of SiO4 units with four bridging oxygens (Q4), and with three bridging and one nonbridging oxygens (Q3).

Keywords: borosilicate glasses, ultrasonic velocity, elastic moduli, FTIR spectroscopy, bond compression model

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6799 Synthesis of Rare Earth Doped Nano-Phosphors through the Use of Isobutyl Nitrite and Urea Fuels: Study of Microstructure and Luminescence Properties

Authors: Seyed Mahdi Rafiaei


In this investigation, red emitting Eu³⁺ doped YVO₄ nano-phosphors have been synthesized via the facile combustion method using isobutyl nitrite and urea fuels, individually. Field-emission scanning electron microscope (FE-SEM) images, high resolution transmission electron microscope (TEM) images and X-ray diffraction (XRD) spectra reveal that the mentioned fuels can be used successfully to synthesis YVO₄: Eu³⁺ nano-particles. Interestingly, the fuels have a large effect on the size and morphology of nano-phosphors as well as luminescence properties. Noteworthy the use of isobutyl nitrite provides an average particle size of 65 nm, while the employment of urea, results in the formation of larger particles and also provides higher photoluminescence emission intensity. The improved luminescence performance is attributed to the condition of chemical reaction via the combustion synthesis and the size of synthesized phosphors.

Keywords: phosphors, combustion, fuels, luminescence, nanostructure

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6798 Spectroscopy Study of Jatropha curcas Seed Oil for Pharmaceutical Applications

Authors: Bashar Mudhaffar Abdullah, Hasniza Zaman Huri, Nany Hairunisa


This study was carried out to determine the thermal properties and spectroscopy study of Malaysian Jatropha curcas seed oil. The J. curcas seed oil physicochemical properties such as free fatty acid (FFA %), acid value, saponification value, iodine value, unsaponifiable matter, and viscosity (cp) gave values of 1.89±0.10%, 3.76±0.07, 203.36±0.36 mg/g, 4.90±0.25, 1.76±0.03%, and 32, respectively. Gas chromatography (GC) was used to determine the fatty acids (FAs) composition. J. curcas seed oil is consisting of saturated FAs (19.55%) such as palmitic (13.19%), palmitoleic (0.40%), and stearic (6.36%) acids and unsaturated FAs (80.42%) such as oleic (43.32%) and linoleic (36.70%) acids. The thermal properties using differential scanning calorimetry (DSC) showed that crystallized TAG was observed at -6.79°C. The melting curves displayed three major exothermic regions of J. curcas seed oil, monounsaturated (lower-temperature peak) at -31.69°C, di-unsaturated (medium temperature peak) at -20.23°C and tri-unsaturated (higher temperature peak) at -12.72°C. The results of this study showed that the J. curcas seed oil is a plausible source of polyunsaturated fatty acid (PUFA) to be developed in the future for pharmaceutical applications.

Keywords: Jatropha curcas seed oil, thermal properties, crystallization, melting, spectroscopy

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6797 Lanthanide-Mediated Aggregation of Glutathione-Capped Gold Nanoclusters Exhibiting Strong Luminescence and Fluorescence Turn-on for Sensing Alkaline Phosphatase

Authors: Jyun-Guo You, Wei-Lung Tseng


Herein, this study represents a synthetic route for producing highly luminescent AuNCs based on the integration of two concepts, including thiol-induced luminescence enhancement of ligand-insufficient GSH-AuNCs and Ce3+-induced aggregation of GSH-AuNCs. The synthesis of GSH-AuNCs was conducted by modifying the previously reported procedure. To produce more Au(I)-GSH complexes on the surface of ligand-insufficient GSH-AuNCs, the extra GSH is added to attach onto the AuNC surface. The formed ligand-sufficient GSH-AuNCs (LS-GSH-AuNCs) emit relatively strong luminescence. The luminescence of LS-GSH-AuNCs is further enhanced by the coordination of two carboxylic groups (pKa1 = 2 and pKa2 = 3.5) of GSH and lanthanide ions, which induce the self-assembly of LS-GSH-AuNCs. As a result, the quantum yield of the self-assembled LS-GSH-AuNCs (SA-AuNCs) was improved to be 13%. Interestingly, the SA-AuNCs were dissembled into LS-GSH-AuNCs in the presence of adenosine triphosphate (ATP) because of the formation of the ATP- lanthanide ion complexes. Our assay was employed to detect alkaline phosphatase (ALP) activity over the range of 0.1−10 U/mL with a limit of detection (LOD) of 0.03 U/mL.

Keywords: self-assembly, lanthanide ion, adenosine triphosphate, alkaline phosphatase

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6796 Structural and Magnetic Properties of NiFe2O4 Spinel Ferrite Nanoparticles Synthesized by Starch-Assisted Sol-Gel Auto-Combustion Method

Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, L. Kalina, M. Hajdúchová, V. Enev, J. Wasserbauer


Nickel spinel ferrite NiFe2O4 nanoparticles with different particle size at different annealing temperature were synthesized using the starch-assisted sol-gel auto-combustion method. The synthesized nanoparticles were characterized by conventional powder X-ray diffraction (XRD) spectroscopy, Raman Spectroscopy, Fourier Transform Infrared Spectroscopy, Field-Emission Scanning Electron Microscopy, X-ray Photoelectron Spectroscopy and Vibrating Sample Magnetometer. The XRD patterns confirmed the formation of NiFe2O4 spinel ferrite nanoparticles. Field-Emission Scanning Electron Microscopy revealed that particles are of spherical morphology with particle size 5-20 nm at lower annealing temperature. An infrared spectroscopy study showed the presence of two principal absorption bands in the frequency range around 525 cm-1 (ν1) and around 340 cm-1 (ν2); which indicate the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Raman spectroscopy study also indicated the change in octahedral and tetrahedral site related Raman modes in nickel ferrite nanoparticles with change of particle size. This change in magnetic behavior with change of particle size of NiFe2O4 nanoparticles was observed.

Keywords: nickel ferrite, nanoparticles, magnetic property, NiFe2O4

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6795 Phase Transition of Aqueous Ternary (THF + Polyvinylpyrrolidone + H2O) System as Revealed by Terahertz Time-Domain Spectroscopy

Authors: Hyery Kang, Dong-Yeun Koh, Yun-Ho Ahn, Huen Lee


Determination of the behavior of clathrate hydrate with inhibitor in the THz region will provide useful information about hydrate plug control in the upstream of the oil and gas industry. In this study, terahertz time-domain spectroscopy (THz-TDS) revealed the inhibition of the THF clathrate hydrate system with dosage of polyvinylpyrrolidone (PVP) with three different molecular weights. Distinct footprints of phase transition in the THz region (0.4–2.2 THz) were analyzed and absorption coefficients and real part of refractive indices are obtained in the temperature range of 253 K to 288 K. Along with the optical properties, ring breathing and stretching modes for different molecular weights of PVP in THF hydrate are analyzed by Raman spectroscopy.

Keywords: clathrate hydrate, terahertz spectroscopy, tetrahydrofuran, inhibitor

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6794 Use of Simultaneous Electron Backscatter Diffraction and Energy Dispersive X-Ray Spectroscopy Techniques to Characterize High-Temperature Oxides Formed on Nickel-Based Superalloys Exposed to Super-Critical Water Environment

Authors: Mohsen Sanayei, Jerzy Szpunar, Sami Penttilä


Exposure of Nickel-based superalloys to high temperature and harsh environment such as Super-Critical Water (SCW) environment leads to the formation of oxide scales composed of multiple and complex phases that are difficult to differentiate with conventional analysis techniques. In this study, we used simultaneous Electron Backscatter Diffraction (EBSD) and Energy Dispersive X-ray Spectroscopy (EDS) to analyze the complex oxide scales formed on several Nickel-based Superalloys exposed to high temperature SCW. Multi-layered structures of Iron, Nickel, Chromium and Molybdenum oxides and spinels were clearly identified using the simultaneous EBSD-EDS analysis technique. Furthermore, the orientation relationship between the oxide scales and the substrate has been investigated.

Keywords: electron backscatter diffraction, energy dispersive x-ray spectroscopy, superalloy, super-critical water

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6793 Particle Size Dependent Magnetic Properties of CuFe2O4 Spinel Ferrite Nanoparticles Synthesized by Starch-Assisted Sol-Gel Auto-Combustion Method

Authors: R. S. Yadav, J. Havlica, I. Kuřitka, Z. Kozakova, J. Masilko, L. Kalina, M. Hajdúchová, V. Enev, J. Wasserbauer


In this work, copper ferrite CuFe2O4 spinel ferrite nanoparticles with different particle size at different annealing temperature were synthesized using the starch-assisted sol-gel auto-combustion method. The synthesized nanoparticles were characterized by conventional powder X-ray diffraction (XRD) spectroscopy, Raman Spectroscopy, Fourier Transform Infrared Spectroscopy, Field-Emission Scanning Electron Microscopy, X-ray Photoelectron Spectroscopy, and Vibrating Sample Magnetometer. The XRD patterns confirmed the formation of CuFe2O4 spinel ferrite nanoparticles. Field-Emission Scanning Electron Microscopy revealed that particles are of spherical morphology with particle size 5-20 nm at lower annealing temperature. An infrared spectroscopy study showed the presence of two principal absorption bands in the frequency range around 530 cm-1 (ν1) and around 360 cm-1 (ν2); which indicate the presence of tetrahedral and octahedral group complexes, respectively, within the spinel ferrite nanoparticles. Raman spectroscopy study also indicated the change in octahedral and tetrahedral site related Raman modes in copper ferrite nanoparticles with change of particle size. This change in magnetic behavior with change of particle size of CuFe2O4 nanoparticles was also observed. The change in magnetic properties with change of particle size is due to cation redistribution, which was confirmed by X-Ray photoelectron study.

Keywords: copper ferrite, nanoparticles, magnetic property, CuFe2O4

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6792 Optical Characterization of Transition Metal Ion Doped ZnO Microspheres Synthesized via Laser Ablation in Air

Authors: Parvathy Anitha, Nilesh J. Vasa, M. S. Ramachandra Rao


ZnO is a semiconducting material with a direct wide band gap of 3.37 eV and a large exciton binding energy of 60 meV at room temperature. Microspheres with high sphericity and symmetry exhibit unique functionalities which makes them excellent omnidirectional optical resonators. Hence there is an advent interest in fabrication of single crystalline semiconductor microspheres especially magnetic ZnO microspheres, as ZnO is a promising material for semiconductor device applications. Also, ZnO is non-toxic and biocompatible, implying it is a potential material for biomedical applications. Room temperature Photoluminescence (PL) spectra of the fabricated ZnO microspheres were measured, at an excitation wavelength of 325 nm. The ultraviolet (UV) luminescence observed is attributed to the room-temperature free exciton related near-band-edge (NBE) emission in ZnO. Besides the NBE luminescence, weak and broad visible luminescence (~560nm) was also observed. This broad emission band in the visible range is associated with oxygen vacancies related to structural defects. In transition metal (TM) ion-doped ZnO, 3d levels emissions of TM ions will modify the inherent characteristic emissions of ZnO. A micron-sized ZnO crystal has generally a wurtzite structure with a natural hexagonal cross section, which will serve as a WGM (whispering gallery mode) lasing micro cavity due to its high refractive index (~2.2). But hexagonal cavities suffers more optical loss at their corners in comparison to spherical structures; hence spheres may be a better candidate to achieve effective light confinement. In our study, highly smooth spherical shaped micro particles with different diameters ranging from ~4 to 6 μm were grown on different substrates. SEM (Scanning Electron Microscopy) and AFM (Atomic Force Microscopy) images show the presence of uniform smooth surfaced spheres. Raman scattering measurements from the fabricated samples at 488 nm light excitation provide convincing supports for the wurtzite structure of the prepared ZnO microspheres. WGM lasing studies from TM-doped ZnO microparticles are in progress.

Keywords: laser ablation, microcavity, photoluminescence, ZnO microsphere

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