Synthesis, characterization and spectroscopic investigation of Cr3+ doped wollastonite nanophosphor

This work explores the preparation of nanocrystalline Cr3+ (1-5 mol%) doped CaSiO3 phosphors by solution combustion process and study of its photoluminescence (PL) behavior. The nanopowders are well characterized by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and Fourier transform infra-red (FTIR) spectroscopy. PXRD results confirm monoclinic phase upon calcination at 950 degrees C for 3 h. SEM micrographs indicates that the powder is highly porous and agglomerated. The TEM images show the powder to consist of spherical shaped particles of size similar to 30-60 nm. Upon 323 nm excitation, the emission profile of CaSiO3:Cr3+ exhibits a narrow red emission peak at 641 nm due to E-2 -> (4)A(2) transition and broad band at 722 nm due to T-4(2g) -> (4)A(2g). It is observed that PL intensity increases with increase in Cr3+ concentration and highest PL intensity is observed for 3 mol% doped sample. The PL intensity decreases with further increase in Cr3+ doping. This decrease in PL intensity beyond 3 mol% is ascribed to concentration quenching. Racah parameters are calculated to describe the effects of electron-electron repulsion within the crystal lattice. The parameters show 21% reduction in the Racah parameter of free ion and the complex, indicating the moderate nephelauxetic effect in the lattice. (C) 2014 Elsevier B.V. All rights reserved.

Photo-induced optical bleaching in Ge12Sb25S63 amorphous chalcogenide thin films: effect of 532 nm laser illumination

The photo-induced effects of Ge12Sb25S63 films illuminated with 532 nm laser light are investigated from transmission spectra measured by FTIR spectroscopy. The material exhibits photo-bleaching (PB) when exposed to band gap light for a prolonged time in a vacuum. The PB is ascribed to structural changes inside the film as well as surface photooxidation. The amorphous nature of thin films was detected by x-ray diffraction. The chemical composition of the deposited thin films was examined by energy dispersive x-ray analysis (EDAX). The refractive indices of the films were obtained from the transmission spectra based on an inverse synthesis method and the optical band gaps were derived from optical absorption spectra using the Tauc plot. The dispersion of the refractive index is discussed in terms of the single-oscillator Wemple-DiDomenico model. It was found that the mechanism of the optical absorption follows the rule of the allowed non-direct transition. Raman and x-ray photoelectron spectra (XPS) were measured and decomposed into several peaks that correspond to the different structural units which support the optical changes.

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

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

Piezoelectric properties of individual nanocrystallites of Ba0.85Ca0.15Zr0.1Ti0.9O3 obtained by oxalate precursor route

Nanocrystalline Ba0.85Ca0.15Zr0.1Ti0.9O3 (BCZT) powder was synthesized via the complex oxalate precursor route at a relatively low temperature (800 degrees C/5 h). The phase formation temperature of BCZT at nanoscale was confirmed by thermogravimetric (TG), differential thermal analysis (DTA) followed by X-ray powder diffraction (XRD) studies. Fourier transform infrared (FTIR) spectroscopy was carried out to confirm the complete decomposition of oxalate precursor into BCZT phase. The XRD and profile fitting revealed the coexistence of cubic and tetragonal phases and was corroborated by Raman study. Transmission electron microscopy (TEM) carried out on 800 degrees C and 1000 degrees C/5 h heat treated BCZT powder revealed the crystallite size to be in the range of 20-50 nm and 40-200 nm respectively. The optical band gap for BCZT nanocrystalline powder was obtained using Kubelka Munk function and was found to be around 3.12 +/- 0.02 eV and 3.03 +/- 0.02 eV respectively for 800 degrees C (20-50 nm) and 1000 degrees C/5 h (40-200 nm) heat treated samples. The piezoelectric properties were studied for two different crystallite sizes (30 and 70 nm) using a piezoresponse force microscope (PFM). The d(33) coefficients obtained for 30 nm and 70 nm sized crystallites were 4 pm V-1 and 47 pm V-1 respectively. These were superior to that of BaTiO3 nanocrystal (approximate to 50 nm) and promising from a technological/industrial applications viewpoint.

Observation of phase transformations in cement during hydration

We report the phase transformations in Portland cement before and after hydration. The hydration mechanism was studied in detail by using a full Rietveld refinement of the X-ray diffraction (XRD) patterns, Fourier Transformed Infra-Red (FTIR) spectroscopy, Thermogravimetric Analysis (TGA) and Mossbauer spectroscopy at room temperature. From the Rietveld refinement of XRD data, alite, belite, celite, brown-millerite and low quartz phases were detected and quantified as major phases in dry cement powder. After hydration, calcium carbonate, portlandite and ettringite phases were found to form. A large reduction in the amounts of alite and belite phases were observed suggesting the formation of amorphous C-S-H phase and emphasizing the role of alite phase in flash setting of cement, as justified by the XRD and FTIR spectroscopy. Mossbauer spectra of all the unset samples showed quadrupole split doublets corresponding to the brownmillerite phase which remains unchanged even after about one week of hydration, suggesting that brownmillerite did not transform to other phases during initial stage of hydration process. (C) 2015 Elsevier Ltd. All rights reserved.

Molecular profiling of sepsis in mice using Fourier Transform Infrared Microspectroscopy

Sepsis is a life threatening condition resulting from a high burden of infection. It is a major health care problem and associated with inflammation, organ dysfunction and significant mortality. However, proper understanding and delineating the changes that occur during this complex condition remains a challenge. A comparative study involving intra-peritoneal injection of BALB/c mice with Salmonella Typhimurium (infection), lipopolysaccharide (endotoxic shock) or thioglycollate (sterile peritonitis) was performed. The changes in organs and sera were profiled using immunological assays and Fourier Transform Infrared (FTIR) micro-spectroscopy. There is a rapid rise in inflammatory cytokines accompanied with lowering of temperature, respiratory rate and glucose amounts in mice injected with S. Typhimurium or lipopolysaccharide. FTIR identifies distinct changes in liver and sera: decrease in glycogen and protein/lipid ratio and increase in DNA and cholesteryl esters. These changes were distinct from the pattern observed in mice treated with thioglycollate and the differences in the data obtained between the three models are discussed. The combination of FTIR spectroscopy and other biomarkers will be valuable in monitoring molecular changes during sepsis. GRAPHICS] Intra-peritoneal infection with high dose of Salmonella Typhimurium leads to rapid increase in inflammatory cytokines, e.g. Tnf alpha (A). FTIR analysis of liver (B) and sera (C) identifies several metabolic changes: glycogen, protein/lipid, cholesteryl esters and DNA.

Electrochemical, spectroscopic and SPM evidence for the controlled formation of self-assembled monolayers and organised multilayers of ferrocenyl alkyl thiols on Au(111)

Organised multilayers were formed from the controlled self-assembly of ferrocene alkyl thiols on Au(111) surfaces. The control was accomplished by increasing the concentration of the thiol solutions used for the assembly. Cyclic voltammetry, ellipsometry, scanning probe microscopy (STM and AFM) and in situ FTIR spectroscopy were used to probe the differences between mono- and multilayers of the same compounds. Electrochemical desorption studies confirmed that the multilayer structure is attached to the surface via one monolayer. The electrochemical behaviour of the multilayers indicated the presence of more than one controlling factor during the oxidation step, whereas the reduction was kinetically controlled which contrasts with the behaviour of monolayers, which exhibit kinetic control for the oxidation and reduction steps. Conventional and imaging ellipsometry confirmed that multilayers with well-defined increments in thickness could be produced. However, STM indicated that at the monolayer stage, the thiols used promote the mobility of Au atoms on the surface. It is very likely that the multilayer structure is held together through hydrogen bonding. To the best of out knowledge, this is the first example of a controlled one-step growth of multilayers of ferrocenyl alkyl thiols using self-assembly techniques.

Amorphous carbon-silicon alloys prepared by a high plasma density source

The addition of silicon to hydrogenated amorphous carbon can have the advantageous effect of lowering the compressive stress, improving the thermal stability of its hydrogen and maintaining a low friction coefficient up to high humidity. Most experiments to date have been on a-C1-xSix:H alloys deposited by RF plasma enhanced chemical vapour deposition (PECVD). This method gives alloys with considerable hydrogen content and only moderate hardness. Here, we use a high plasma density source, the electron cyclotron wave resonance (ECWR) source, to prepare films with a high deposition rate. The composition and bonding in the alloys is determined by XPS, visible and UV Raman and FTIR spectroscopy. We find that it is possible to produce hard, low stress, low friction, almost humidity insensitive a-C1-xSix:H alloys with a good optical transparency and a band gap over 2 eV.

The diphasic nc-Si/a-Si : H thin film with improved medium-range order

A series of silicon film samples were prepared by plasma enhanced chemical vapor deposition (PECVD) near the threshold from amorphous to nanocrystalline state by adjusting the plasma parameters and properly increasing the reactions between the hydrogen plasma and the growing surface. The microstucture of the films was studied by micro-Raman and Fourier transform infrared (FTIR) spectroscopy. The influences of the hydrogen dilution ratio of silane (R-H = [H-2]/[SiH4]) and the substrate temperature (T-s) on the microstructural and photoelectronic properties of silicon films were investigated in detail. With the increase of RH from 10 to 100, a notable improvement in the medium-range order (MRO) of the films was observed, and then the phase transition from amorphous to nanocrystalline phase occurred, which lead to the formation of diatomic hydrogen complex, H-2* and their congeries. With the increase of T-s from 150 to 275 degreesC, both the short-range order and the medium range order of the silicon films are obviously improved. The photoconductivity spectra and the light induced changes of the films show that the diphasic nc-Si/a-Si:H films with fine medium-range order present a broader light spectral response range in the longer wavelength and a lower degradation upon illumination than conventional a-Si:H films. (C) 2004 Elsevier B.V. All rights reserved.

Effect of rapid thermal annealing and hydrogen plasma treatment on the microstructure and light-emission of silicon-rich oxide film

Silicon-rich silicon oxide (SRSO) films are prepared by plasma-enhanced chemical vapor deposition method at the substrate temperature of 200degreesC. The effect of rapid thermal annealing and hydrogen plasma treatment on tire microstructure and light-emission of SRSO films are investigated in detail using micro-Raman spectroscopy, Fourier transform infrared (FTIR) spectroscopy and photoluminescence (PL) spectra. It is found that the phase-separation degree of the films decreases with increasing annealing temperature from 300 to 600degreesC, while it increases with increasing annealing temperature from 600 to 900degreesC. The light-emission of the films are enhanced with increasing annealing temperature up to 500degreesC, while it is rapidly reduced when the annealing temperature exceeds 600degreesC. The peak position of the PL spectrum blueshifts by annealing at the temperature of 300degreesC, then it red-shifts with further raising annealing temperature. The following hydrogen plasma treatment results in a disproportionate increase of the PL intensity and a blueshift or redshift of the peak positions, depending on the pristine annealing temperature. It is thought that the size of amorphous silicon clusters, surface structure of the clusters and the distribution of hydrogen in the films can be changed during the annealing procedure. The results indicate that not only cluster size but also surface state of the clusters plays an important role in the determination of electronic structure of the amorphous silicon cluster and recombination process of light-generated carriers.

Structural evaluation of polycrystalline silicon thin films by hot-wire-assisted PECVD

Tungsten wires were introduced into a plasma-enhanced chemical vapor deposition (PECVD) system as a catalyzer: we name this technique 'hot-wire-assisted PECVD' (HW-PECVD). Under constant deposition pressure (p(g)), gas flow ratio and catalyzer position, the effects of the hot wire temperature (T-f) on the structural properties of the poly-Si films have been characterized by X-ray diffraction (XRD), Raman scattering and Fourier-transform infrared (FTIR) spectroscopy. Compared with conventional PECVD, the grain size, crystalline volume fraction (X-e) and deposition rate were all enhanced when a high T-f was used. The best poly-Si film exhibits a preferential (220) orientation, with a full width at half-maximum (FWHM) of 0.2 degrees. The Si-Si TO peak of the Raman scattering spectrum is located at 519.8 cm(-1) with a FWHM of 7.1 cm(-1). The X-c is 0.93. These improvements are mainly the result of promotion of the dissociation of SiH4 and an increase in the atomic H concentration in the gas phase. (C) 2001 Elsevier Science B.V. All rights reserved.

Comparative study of the surface passivation on crystalline silicon by silicon thin films with different structures

Si thin films with different structures were deposited by plasma enhanced chemical vapor deposition (PECVD), and characterized via Raman spectroscopy and Fourier transform infrared (FTIR) spectroscopy. The passivation effect of such different Si thin films on crystalline Si surface was investigated by minority carrier lifetime measurement via a method, called microwave photoconductive decay (mu PCD), for the application in HIT (heterojunction with intrinsic thin-layer) solar cells. The results show that amorphous silicon (a-Si:H) has a better passivation effect due to its relative higher H content, compared with microcrystalline (mu c-Si) silicon and nanocrystalline silicon (nc-Si). Further, it was found that H atoms in the form of Si-H bonds are more preferred than those in the form of Si-H-2 bonds to passivate the crystalline Si surface. (C) 2009 Elsevier B.V. All rights reserved.

The diphasic nc-Si/a-Si : H thin film with improved medium-range order

A series of silicon film samples were prepared by plasma enhanced chemical vapor deposition (PECVD) near the threshold from amorphous to nanocrystalline state by adjusting the plasma parameters and properly increasing the reactions between the hydrogen plasma and the growing surface. The microstucture of the films was studied by micro-Raman and Fourier transform infrared (FTIR) spectroscopy. The influences of the hydrogen dilution ratio of silane (R-H = [H-2]/[SiH4]) and the substrate temperature (T-s) on the microstructural and photoelectronic properties of silicon films were investigated in detail. With the increase of RH from 10 to 100, a notable improvement in the medium-range order (MRO) of the films was observed, and then the phase transition from amorphous to nanocrystalline phase occurred, which lead to the formation of diatomic hydrogen complex, H-2* and their congeries. With the increase of T-s from 150 to 275 degreesC, both the short-range order and the medium range order of the silicon films are obviously improved. The photoconductivity spectra and the light induced changes of the films show that the diphasic nc-Si/a-Si:H films with fine medium-range order present a broader light spectral response range in the longer wavelength and a lower degradation upon illumination than conventional a-Si:H films. (C) 2004 Elsevier B.V. All rights reserved.

Structural evaluation of polycrystalline silicon thin films by hot-wire-assisted PECVD

Tungsten wires were introduced into a plasma-enhanced chemical vapor deposition (PECVD) system as a catalyzer: we name this technique 'hot-wire-assisted PECVD' (HW-PECVD). Under constant deposition pressure (p(g)), gas flow ratio and catalyzer position, the effects of the hot wire temperature (T-f) on the structural properties of the poly-Si films have been characterized by X-ray diffraction (XRD), Raman scattering and Fourier-transform infrared (FTIR) spectroscopy. Compared with conventional PECVD, the grain size, crystalline volume fraction (X-e) and deposition rate were all enhanced when a high T-f was used. The best poly-Si film exhibits a preferential (220) orientation, with a full width at half-maximum (FWHM) of 0.2 degrees. The Si-Si TO peak of the Raman scattering spectrum is located at 519.8 cm(-1) with a FWHM of 7.1 cm(-1). The X-c is 0.93. These improvements are mainly the result of promotion of the dissociation of SiH4 and an increase in the atomic H concentration in the gas phase. (C) 2001 Elsevier Science B.V. All rights reserved.

Biosorption of uranium by chemically modified Rhodotorula glutinis

The present paper reports the biosorption of uranium onto chemically modified yeast cells, Rhodotorula glutinis, in order to study the role played by various functional groups in the cell wall. Esterification of the carboxyl groups and methylation of the amino groups present in the cells were carried out by methanol and formaldehyde treatment, respectively. The uranium sorption capacity increased 31% for the methanol-treated biomass and 11% for the formaldehyde-treated biomass at an initial uranium concentration of 140 mg/L The enhancement of uranium sorption capacity was investigated by Fourier transform infrared (FTIR) spectroscopy analysis, with amino and carboxyl groups were determined to be the important functional groups involved in uranium binding. The biosorption isotherms of uranium onto the raw and chemically modified biomass were also investigated with varying uranium concentrations. Langmuir and Freundlich models were well able to explain the sorption equilibrium data with satisfactory correlation coefficients higher than 0.9. (C) 2010 Elsevier Ltd. All rights reserved.