Oxalate Single Crystals Research Articles

INVESTIGATIONS ON THE GROWTH AND CHARACTERIZATION OF MAGNESIUM SULFATE DOPED L-LEUCINIUM OXALATE CRYSTALS

Magnesium Sulfate-doped L-Leucinium oxalate (MSLO) single crystal was grown using slow evaporation method. Structure of the crystal was determined by single-crystal X-Ray Diffraction (XRD). Lattice parameters of MSLO crystal were determined. Optical transmittance study was done to find various linear optical parameters like band gap, reflectance, refractive index, absorption coefficient, extinction coefficient, optical conductivity. Vickers Micro hardness study was carried out to find mechanical properties such as hardness, work hardening coefficient, brittleness index and fracture toughness of the grown MSLO crystal. Kurtz-Perry powder technique with Nd: YAG laser was applied to study the second harmonic generation (SHG) competency. By using Z-scan technique, third-order NLO efficiency of MSLO crystal was calculated. LDT study was also done for MSLO crystal. It is observed that magnesium sulfate-doped L-leucinium oxalate (MSLO) crystal has the superior properties compared to that of undoped L-leucinium oxalate crystal. EDS studies were conducted for MSLO crystal to check the elements present in the crystal.

White light emitting dysprosium doped lanthanum oxalate single crystals

Single crystals of Lanthanum oxalate [La2 (C2O4)3]1OH2O and Dy3+ doped Lanthanum oxalate [La2-xDyx (C2O4)3]10H2O with x=0.1, 0.15, 0.2 were grown by gel method and characterised by X-ray powder diffraction analysis. Thermal stability of sample was investigated by thermo gravimetric analysis. UV-Visible absorption and photo-luminescent studies were also conducted. The emission spectrum on exciting at 271nm and 364 nm were recorded in which Dy3+ ions showed four emission bands at positions 458nm (blue), 478 nm (blue), 572 nm (yellow) and 655 nm (red) corresponding to transitions 4I15/2→ 6H15/2, 4F9/2→ 6H15/2, 4F9/2→ 6H13/2 and 4F9/2→ 6H11/2 respectively. The CIE coordinates, colour purity and CCT values were calculated, and all these parameters show that Dy3+ doped lanthanum oxalate single crystals are suitable candidates for white light emitting applications.

Growth Kinetics, Optical studies of Pure and Mg2+ Doped Nickel Cadmium Oxalate Single Crystals

Growth of pure (nickel cadmium oxalate) and Mg2+ doped nickel cadmium oxalate (MNCO) single crystals were grown by the single diffusion gel method at room temperature, by optimizing the various growth parameters such as specific gravity of sodium meta silicate (SMS), gel pH, gel temperature, gel aging, concentration of supernatant solution and concentration of oxalic acid. The morphology and composition of elements present in the crystals were identified using SEM-EDX analysis. The FTIR study shows that the occurrences of C=O, C-O, C-C, O-H and M-O bonding within the crystal lattice. The triclinic crystal system with P-1 space group were identified using, X-ray diffraction method. The absorbance, transmittance, energy gap, refractive index (n), reflectance (R) and insulating behaviour of the grown crystals were analysed using UV-Visible spectrophotometer.

Growth, spectral, optical, electrical and computational analysis of sodium oxalate single crystals

Single crystals of Sodium Oxalate (SO) were grown by adopting the slow evaporation solution growth approach from aqueous solution. The prominent functional groups seen in the SO crystal were distinctly detected with Fourier transform infrared and FT-Raman spectral analysis. The cut-off wavelength of 230 nm was measured using Ultraviolet -visible spectral analysis. Theoretical quantum chemical computations were done by DFT using Gaussian software package. The different properties such as structural, vibrational and electronic properties of SO was studied at the B3LYP/LanL2DZ level. The chemical activity of SO molecule was revealed by HOMO-LUMO energies. From Topology analysis the chemical significance of the molecules has been enunciated. The electron density centered on local reactivity descriptors like Mulliken atomic charges and Fukui function were calculated to describe the chemical reactivity of the SO compound. The mechanical property of the grown crystal was disclosed from Vicker's micro hardness test carried out on the grown SO crystals and the test confirms the soft nature of the crystal. The dielectric behavior of SO crystal was completely investigated for different temperatures and the activation energies were calculated for different frequencies.

Comments on the paper “Growth, structural, optical and thermal studies of semi-organic nonlinear optical potassium hydrogen oxalate single crystal”

The authors of the title paper (Appl Phys A 126:394, 2020) report to have grown a new nonlinear optical potassium hydrogen oxalate (KHO) single crystal, which exhibits second harmonic generation response. In this comment, it is shown that these claims are erroneous since KHO is a well-known solid which crystallizes in the centrosymmetric P21/c space group.

L-Valine doped oxalate single crystals for optoelectronic applications

L-Valine doped potassium hydrogen oxalate (KHO) and potassium boro oxalate (KBO) single crystals are grown by slow evaporation solution growth technique at room temperature. The presence of l-valine in the crystal lattices has not altered the structure of the KHO and KBO as evidenced by Single Crystal X – ray diffraction analysis. The grown crystals are characterized by FT-IR and UV–Vis-NIR analysis. The major elements present in the crystals are identified by Energy Dispersive X-ray spectrometry. Thermo-gravimetric – Differential Thermal analysis has been enforced to evaluate the melting point of the grown crystals and the nonlinear optical property is estimated by Kurtz – Perry test.

Dielectric, Magnetic and Spectral studies of gel grown Mg2+ Doped Copper Cadmium Oxalate Single Crystals

Mg2+ doped Copper Cadmium oxalate (MCuCO) single crystals were grown by a single diffusion method in silica hydrogel at room temperature. Powder X-ray diffraction (XRD) studies show the triclinic nature of the crystals. The dielectric constant, ac resistivity and ac conductivity have been measured as a function of frequency. The dielectric constant of MCuCO crystal decreases as the frequency of applied field increases; at the end it gives the diminishing value of dielectric constant. AC conductivity increases with the increase of frequency. Absorbance, transmittance, reflectance, refractive index, and energy gap of MCuCO crystal were determined by UV-Visible spectroscopy. A high bandgap corresponds to the dielectric behavior of the crystal.

Synthesis and Investigation on Structural, Thermal, Mechanical, Linear Optical, and Nonlinear Optical Nature of Potassium Sulphato Oxalate Single Crystals

AbstractThe new semiorganic potassium sulphato oxalate (KSO) single crystals are grown at room temperature by a slow evaporation method using an aqueous solution. The Fourier transform infrared spectroscopy is used to ascertain the various functional groups present in the grown KSO sample. The single crystal X‐ray diffractometer (XRD) results confirm the grown KSO crystal is a triclinic structure with lattice parameters a = 6.37 Å; b = 7.03 Å; c = 10.61 Å; and space group P1. Powder XRD study proves the crystallinity and purity of the grown crystal. The optical behaviors of KSO are analyzed by UV–vis‐near infrared reflectance (NIR) spectrophotometer. Photoluminescence (PL) studies of KSO reveal its strong green emission at 576 nm. The laser damage threshold (LDT) of the title compound is measured to be 6.135 GW/cm2. The thermo gravimetric and differential thermal analysis indicated that KSO is stable up to 103 °C. From the Vickers microhardness tester, the mechanical behaviors of the title compound are studied. The frequency conversion property of KSO crystal is analyzed using Kurtz–Perry method, and it is found to be 1.16 times higher than that of the reference potassium dihydrogen phosphate which indicates KSO is well suited for optoelectronic device fabrication.

Growth and Characterization of Pure and Magnesium Doped Copper Cadmium Oxalate Single Crystals

Single crystals of Pure (CCO) and Magnesium Doped Copper Cadmium Oxalate (MDCCO) having size of 0.30×0.15×0.10 were grown by the single-diffusion reaction method in the silica gel medium at 23°C temperature. Optimum condition for growth was established by varying gel parameters such as specific gravity, pH, gel ageing, concentration of the reactants and ratio of supernatant solutions of Cadmium chloride and Cupric chloride. The crystals were characterized by using the methods such as Powder X-Ray Diffraction (PXRD), Fourier-Transform Infrared (FT-IR)Spectroscopy, UV-Visible spectral studies, Scanning Electron Microscopy-Energy Dispersive X-ray Analysis (SEM-EDAX), Thermo Gravimetric Analysis /Differential thermal analysis (TGA / DTA).

Thermal Phases in Gel-Grown Cadmium Oxalate Single Crystals

Thermogravimetric (TG) and Differential thermal (DT) analysis carried out for studying thermal kinetics and mechanism of phase changes of gel-grown crystals of cadmium oxalate (CdC2O4.3H2O). The material turns out to be trihydrated. The obtained experimental data show that the material is thermally stable up to 64°C, beyond which it exhibits marked tendency to structural decomposition. The process occurs in three phases until, ultimately, cadmium oxide is obtained. The energies of the reactions involved and the mechanism of phase change at each stage have been examined. The kinetic parameters such as activation energy, order of reaction, frequency factor and entropy are evaluated from non-mechanistic equation for thermal dehydration.

Molecular structure, vibrational spectroscopic (FT-IR, FT-Raman), NBO, HOMO and LUMO analysis of morpholinium oxalate by density functional method

A new organic nonlinear optical morpholinium oxalate (MO) single crystal was grown from low temperature solution growth method. Single crystal XRD was utilized to calculate the lattice constants, the molecular arrangements and the formation of hydrogen bonds in the MO compound. Vibrational analysis was utilized to identify the assorted functional groups existing in the compound. The optimized structure, electronic properties and frontier energy gap was scrutinized by DFT (density functional theory). The DFT supports to construe the charge transfer from oxalic acid to morpholine in the compound. NBO (natural bond orbital) computations were utilized to evaluate the stabilities occurs from charge delocalization and intermolecular interactions in the MO crystal. The 1H and 13C NMR spectrum confirms the protonation of the compound. The first-order hyperpolarizability was estimated to be 8.31 × 10−31 esu.

Morphological and FTIR Studies of Barium Oxalate Single Crystals

Abstract The conditions for the gel growth of barium oxalate single crystals in silica gels were studied in this paper. We describe the growth mechanism, effect concentration of feed solution, interchanging of the reactants, the effect of temperature and detailed study of microstructures of barium oxalate single crystals. At higher concentration of feed solution dense fibers were observed. With interchanged feed solution precipitate and spherulites have been obtained. The effect of temperature on growth barium oxalate crystals showed that there was a decrease in nucleation density at higher temperature. The crystals growth were observed under the electron microscope which revealed that the crystal have needle and spherulites structures. We also report the FTIR studies of barium oxalate crystals.

Structural, optical, mechanical and density functional theory studies of 1H-pyrazol-2-ium hydrogen oxalate crystal

In the present work, we have grown 1H- pyrazol-2-ium hydrogen oxalate single crystal by slow evaporation solution growth technique. The lattice parameters are determined from single crystal X ray diffraction studies. The functional groups present in the compound are confirmed by Fourier transform infrared spectroscopy. UV-Vis analysis shows that the crystal has a wide transparency window. Vicker's hardness test has been carried out to estimate the stiffness constant, fracture toughness, brittleness index and yield strength of the crystal. Density functional study B3LYP method at 6-31 G (d, p) has been performed to study the optimized structure, HOMO-LUMO energy gap, hyperpolarizability and thermodynamic properties.

Investigation on growth and characteristics of undoped and Mn doped glycinium oxalate single crystals

This work aims at investigating the undoped Glycinium Oxalate (GO) and Manganese doped Glycinium Oxalate (Mn:GO) single crystals that were prepared via slow evaporation method. The single crystals grown were characterized for its structural, vibrational, optical, topographical, electrical and mechanical properties. Single and Powder X-ray diffraction suggests that the grown crystals are crystallized in the monoclinic structure. The functional groups and the effect of moisture on the undoped and doped GO crystals can be analyzed with the help of FTIR spectrum. The undoped and doped GO single crystal shows low absorption in the entire visible and IR region, which is suitable for optical device applications. The emission of green light with the use of Nd:YAG laser (λ = 1064 nm) confirmed the second harmonic generation properties of the grown crystals. Dielectric measurements were carried to the wide range of frequency (50 Hz–5 MHz) at different temperatures. The determined Vickers hardness number and work hardening coefficient of the grown crystals ascertains the soft nature of the crystal.

Growth and characterization of Sm3+ doped cerium oxalate single crystals

Single crystals of Sm3+ doped cerium oxalate decahydrate were synthesized using single diffusion gel technique and the conditions influencing the size, morphology, nucleation density and quality of the crystals were optimized. Highly transparent single crystals of average size 3mm×2mm×1mm with well-defined hexagonal morphology were grown during a time period of two weeks. X-ray powder diffraction analysis revealed that the grown crystals crystallize in the monoclinic system with space group P21/c as identical with the pure cerium oxalate. The various functional groups of the oxalate ligand and the water of crystallization were identified by Fourier transform infrared spectroscopy. The photoluminescence spectrum of the Sm3+ doped cerium oxalate indicated that the Sm3+ ions are optically active in the cerium oxalate matrix. The crystal has a strong and efficient orange red emission with a wavelength peak at 595nm and hence can be effectively used for optical amplification. Microhardness measurements of the crystal revealed that they belong to the soft material category.

Vibrational spectroscopic studies of L-Alaninium oxalate

An organic crystal of L-Alaninium oxalate single crystal, belongs to the amino acid group, was grown by the slow evaporation solution growth technique at room temperature. The grown crystal had been subjected to single-crystal X-ray diffraction technique and cell parameters of the crystal were determined. The quantitative analysis on the crystal had been carried out using Fourier transform infrared (FTIR) and Fourier transform Raman (FTRaman) spectral measurements. The molecular structures, vibrational wave numbers were calculated using Density Functional Theory method. The calculated Thermodynamic properties were performed.

Crystal growth methods dedicated to low solubility actinide oxalates

Two novel crystal growth syntheses dedicated to low solubility actinide-oxalate systems and adapted to glove box handling are described. These methods based on the use of precursors of either actinide metal or oxalic acid have been optimized on lanthanide systems (analogue of actinides(III)) and then assessed on real actinide systems. They allow the synthesis of several actinide oxalate single crystals, Am2(C2O4)3(H2O)3·xH2O, Th(C2O4)2·6H2O, M2+x[PuIV2−xPuIIIx(C2O4)5]·nH2O and M1−x[PuIII1−xPuIVx(C2O4)2·H2O]·nH2O. It is the first time that these well-known compounds are formed by crystal growth methods, thus enabling direct structural studies on transuranic element systems and acquisition of basic data beyond deductions from isomorphic (or not) lanthanide compounds. Characterizations by X-ray diffraction, UV–visible solid spectroscopy, demonstrate the potentialities of these two crystal growth methods to obtain oxalate compounds.

Growth, optical, mechanical and electrical studies of nonlinear optical crystal: l-Valinium oxalate

l-Valinium oxalate (LVO) single crystal has been grown by solution growth technique at room temperature. The crystal structure and lattice parameters were determined for the grown crystal by single crystal X-ray diffraction studies. Optical constants like band gap, refractive index, reflectance, extinction coefficient and electric susceptibility were determined from UV–vis–NIR spectrum. The microhardness studies reveal the mechanical strength of the grown crystal. The dielectric constant, dielectric loss and AC conductivity of the compound were calculated at different temperatures and frequencies to analyze the electrical properties. Nonlinear optical property was discussed to confirm the SHG efficiency of the grown crystal.

Growth and spectroscopic properties of samarium oxalate single crystals

Single crystals of samarium oxalate decahydrate were synthesized using single diffusion gel technique and the conditions influencing the size, shape and quality were optimized. Highly transparent crystals of size 3×2×1mm3 with a well defined hexagonal morphology were grown during a time period of two weeks. X ray powder diffraction analysis revealed that the grown crystals crystallize in the monoclinic system with space group P21/c and the proposed chemical formula and linkage of water molecules were confirmed using thermogravimetric analysis. The various functional groups of the oxalate ligand and the water of crystallization were identified by Fourier transform infrared spectroscopy. Spectroscopic investigations such as electric dipole transition probability, magnetic dipole transition probability and branching ratios of all possible transitions from 4G5/2 level of Sm3+ ions were estimated from the absorption spectra using JO theory. The spectroscopic analysis suggested that the crystal has a strong and efficient orange red emission. This is confirmed from the photoluminescence spectrum with a wavelength peak at 595nm and hence this promising emission can be effectively used for optical amplification.

Growth and Structural Characterization of Gadolinium Neodymium Oxalate Crystals Grown in Hydro-Silica Gel

Gadolinium Neodymium Oxalate (GNO) single crystals were grown in hydrosilica gel by the diffusion of a mixture of aqueous solutions of the respective rare earth nitrates into a gel, impregnated with oxalic acid, in a test tube. Pink, transparent, hexagonal GNO crystals were obtained on optimization of growth parameters. The crystals are found to be monoclinic by the XRD analysis. The presence of water of hydration and carboxylic group in the grown crystals was confirmed by IR analysis. EDAX analysis confirmed the presence of Gd and Nd in the grown samples. The thermal decomposition behavior of the grown crystals were studied by thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The thermal analysis results concur with the proposed crystal structure.