M. A. Ittyachen

Growth and micro-topographical studies of gel grown cholesterol crystals

Cholesterol (C27H46O) is the most abundant and best-known steroid in the animal kingdom. The in vitro crystallization of this important biomaterial has been attempted by few researchers. Here we are reporting crystallization of pure cholesterol monohydrate crystals in gel medium. It is found that the morphology of the crystals depends on various parameters. The effect of solvent has been studied in detail. The different morphologies observed are fibrous, needle, platelet, dendrite etc. Micro topographical studies have been made and it is found that the crystals grow, at least in the last stage, by spreading of layers. However, at initial stage microcrystals formed and developed into dendrite or needle forms. These one-dimensional crystals developed into platelets and finally thickened. Further studies reveal that micro impurities play a vital role in the development of these crystals as seen by dissolution figures on the crystals. These crystals are characterized by using the XRD and IR spectroscopic methods.

Some structural aspects of neodymium praseodymium oxalate single crystals grown in hydro silica gels

The mixed crystals of neodymium praseodymium oxalate are grown by the diffusion of a mixture of aqueous solutions of neodymium nitrate and praseodymium nitrate (as an upper reactant) into the set gel embedded with oxalic acid. By varying the concentration (by volume) of rare earth nitrates in the upper reactant, the incorporation of Nd and Pr in the mixed crystals has been studied. Tabular crystals with the well defined hexagonal basal planes are observed in the mixed crystals of varying concentrations. X-ray diffraction patterns of these powdered samples reveal that these mixed crystals are ‘isostructural’, while IR and FTIR spectra establish the presence of oxalate groups. TGA and DSC analyses show the correctness of the chemical formula for the mixed crystals, by the release of water molecules (endothermic) and of CO and CO2 (exothermic), with the rare earth oxides as the stable residue. X-ray fluorescence (XRF) and energy dispersive X-ray analyses (EDAX) establish the presence of heavy rare earth elements qualitatively and to a good extent quantitatively. X-ray photoelectron spectroscopic (XPS) studies confirm the presence of rare earth elements (Nd and Pr) as their respective oxides. The findings of these techniques of characterization are in excellent agreement with the proposed empirical structure for the mixed rare earth oxalates. The implications are discussed.

Structural studies and luminescence properties of CeO2:Eu3+ nanophosphors synthesized by oxalate precursor method

A novel synthesis strategy to prepare CeO2:Eu3+ nanophosphors and its luminescence behavior is reported. Different structural characterization techniques such as X-ray diffraction, transmission electron microscope and thermogravimetric analysis reveal that thermal decomposition of oxalate precursor is an effective pathway to produce rare earth oxide nanocrystals. Optical characterizations of the CeO2:Eu3+ were done by UV–Visible absorption, photoluminescence excitation and emission spectra. The presence of structural defects and their role on the band gap and luminescence were discussed on the basis of absorption and emission studies. Luminescence study of the CeO2:Eu3+ ensures that the strong charge transfer band of CeO2 makes it a suitable host material for efficiently exciting Eu3+ ions by subsequent energy transfer. The dependence of luminescence efficiency of the CeO2:Eu3+ with varying concentrations of Eu3+ was also studied and discussed. The results show that Eu3+-doped CeO2 nanophosphor is a potential candidate in ultraviolet-based LEDs.

Structural and spectral investigation of terbium molybdate nanophosphor

Terbium molybdate nanophosphors were synthesized through a facile sol-gel route. The structure of the phosphors was characterized by X-ray diffraction, Raman spectra and Fourier transform infrared spectroscopy analysis. The X-ray diffraction studies revealed that the structure of the nanophosphor gradually changes from monoclinic to orthorhombic phase as heated from 700 to 900 °C. High resolution transmission electron microscopy, SAED and EDS were also employed to characterize the size, crystallinity and composition of the samples. Detailed spectroscopic investigations were carried out by Judd-Ofelt analysis based on UV-Visible-NIR absorption and emission spectra. The luminescence spectra suggest that phosphors with orthorhombic structure have better luminescence properties than the monoclinic structure. The phosphors showed intense green emission under near-UV excitation due to the energy transfer from the host lattice to Tb(3+) ions. The CIE coordinates suggest enhanced color purity for green emission and short fluorescence decay values proposes the suitability for LED applications. These phosphors can be applied as promising candidates for blue and near-UV excited WLEDs.

Synthesis, structural and spectroscopic investigations of nanostructured samarium oxalate crystals.

Nanostructured samarium oxalate crystals were prepared via microwave assisted co-precipitation method. The crystal structure and morphology of the sample were analyzed using X-ray powder diffraction, Scanning electron microscopy and Transmission electron microscopy. The presence of functional groups is ascertained by Fourier transform infrared spectroscopy. Samarium oxalate nanocrystals of average size 20 nm were aggregated together to form nano-plate structure in sub-microrange. Detailed spectroscopic investigation of the prepared phosphor material was carried out by Judd-Ofelt analysis based on the UV-Visible-NIR absorption spectra and photoluminescence emission spectra. The analysis reveals that the transition from energy level (4)G5/2 to (6)H7/2 of Sm(3+) ion has maximum branching ratio and the corresponding orange emission can be used for display applications.

Growth and Optical Properties of NaY(WO4)2:Eu Crystals

Single crystals of mixed cerium lanthanum oxalate (CLO) are grown by gel method. Over the hydro-silica gel prepared by mixing oxalic acid and sodium meta silicate, a mixture of aqueous solutions of cerium nitrate and lanthanum nitrate are poured gently. Cerium and lanthanum ions diffuse into the gel and react with oxalic acid to give colorless, transparent cerium lanthanum oxalate crystals with in a few days. Different growth parameters give crystals of various dimensions. Infrared (IR) spectrum confirms the presence of water molecules and carboxylic acid. X-ray diffraction (XRD) pattern of these samples reveals the crystalline nature. Diffraction peaks are indexed. Unit cell parameters are determined. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) data support the presence of 9 H 2 O molecules attached to the CLO crystal lattice which are lost around 200°C as revealed by the endotherm record. Exothermic peak around 350°C-425°C shows the release of CO and CO 2 . Elemental analysis done by energy dispersive X-ray fluorescence analysis (EDXRF) for the mixed rare earth compound is almost in good agreement with experimental and theoretical values.

Lanthanum samarium oxalate : Its growth and structural characterization

Lanthanum samarium oxalate (LSO) single crystals are grown in silica gels by the diffusion of a mixture of aqueous solutions of lanthanum nitrate and samarium nitrate into the test tube having the set gel impregnated with oxalic acid. Tabular crystals of LSO having well defined hexagonal basal planes are observed at different depths inside the gel. LSO crystals grown by this method are colourless and transparent. Laue transmission X-ray diffraction pattern of LSO reveals well defined spots with two-fold symmetry along the horizontal axis. Thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) support that LSO loses water around 120°C, and CO and CO2 around 350–450°C. The infrared (IR) absorption spectrum of LSO establishes the presence of oxalate (C2 O4)2− ions. Energy dispersive X-ray analysis (EDAX) confirms the presence of La and Sm in the sample. X-ray photoelectron spectroscopic (XPS) studies of LSO confirm the presence of La and Sm in their respective oxide states. An empirical structure for LSO has been proposed on the basis of these findings.

Thermal Decomposition Studies of Neodymium Praseodymium Oxalate Decahydrate Crystals

Neodymium praseodymium oxalate decahydrate crystals were grown using silica gel technique by the controlled reaction of rare earth nitrates with oxalic acid. The grown crystal were characterized using X-ray powder diffraction and thermogravimetric analysis. The thermal decomposition process of the crystals is in good agreement with the proposed crystal structure.

Studies on Ce2(C2O4)3·nH2O crystals grown in hydro-silica gel

Single crystals of cerium oxalate are grown by the gel method. Ce(NO3)3 is allowed to diffuse into a gel in which oxalic acid is incorporated. Cerium oxalate crystals are formed by chemical reaction and the growth process is observed. Crystals are yellow-white in colour. Morphology and size of the crystals are highly influenced by the acidity of the feed solution. With 30% HNO3 long needle shaped, with 50% HNO3 thin hexagonal and with 100% HNO3, well developed crystals are obtained. Natural etch pits are observed on the grown crystals due to the presence of HNO3. Appearance of a single, large interfacial crystal is observed for 0·5 M cerium nitrate. IR spectrum confirms the presence of water molecules and carboxylic group. X-ray diffractogram gives well defined peaks. Peaks are indexed. Unit cell dimensions are determined. Thermal analysis of the samples done using TGA and DTA show the release of water molecules (endothermic) and of CO and CO2 (exothermic) with the rare earth oxide as stable residue.

The growth and thermodynamical feasibility of tungsten diselenide single crystals using chemical vapour transport technique

Thermodynamical feasibility study and the growth of layer structured transition metal dichalcogenide single crystals of WSe2, using iodine as transporting agent, has been reported in this paper. The characterization of the grown samples have been done by X-ray analysis.